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Variable-temperature X-ray crystal structure determinations (80–330 K) on compounds {Fe[tren(6-Mepy)3]}(ClO4)2 (1-Fe) {tren(6-Mepy)3 is tris[3-aza-4-(6-methyl-2-pyridyl)but-3-enyl]amine} and {Zn[tren(6-Mepy)3]}(ClO4)2 (1-Zn) {tren(6-Mepy)3 is tris[3-aza-4-(6-methyl-2-pyridyl)but-3-enyl]amine} were carried out together with a detailed analysis of the unit-cell volume and parameters in the spin transition region for (1-Fe). Both compounds crystallize in the monoclinic system and retained the space group P21/c at all measured temperatures. The Fe and Zn atoms are surrounded by six N atoms belonging to imine groups and pyridine groups of the trifurcated ligand, adopting a pseudo-octahedral symmetry. The average Fe—N bond lengths of 2.013 (1) Å (80 K) and 2.216 (2) Å (330 K) are consistent with a low-spin (LS) and a high-spin (HS) state for the iron(II) ions. In contrast to (1-Fe), the structures of (1-Zn) at low and high temperatures are similar and repeat the structural features of the high-spin structure of (1-Fe). The volume of the unit cell increases on heating from 80 to 330 K for (1-Fe) and (1-Zn). On the other hand, while the a, b and c cell parameters increase for (1-Fe), they show less variation for (1-Zn). For (1-Fe), variation of the unit-cell volume with temperature recalculated per Fe atom shows a change ΔV = 27.16 Å3 during the spin crossover process. Magnetic susceptibility and Mössbauer spectroscopy studies performed on (1-Fe) reveal an inversion temperature, T1/2 of 233 K, where the molar fractions of LS and HS sites are both equal to 0.5. The variation in metal–ligand bond lengths, the distortion parameters and the cell parameters are very close to the character of the magnetic curve and the curve of γHS (the molar fraction of HS molecules) derived from the Mössbauer data; this result shows the correlation between structure and physical properties in (1-Fe).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889807048571/aj5096sup1.cif
Contains datablocks 1-Fe_80, 1-Fe_130, 1-Fe_150, 1-Fe_170, 1-Fe_190, 1-Fe_210, 1-Fe_230, 1-Fe_250, 1-Fe_270, 1-Fe_290, 1-Fe_310, 1-Fe_330, 1-Zn_80, 1-Zn_130, 1-Zn_170, 1-Zn_210, 1-Zn_230, 1-Zn_250, 1-Zn_270, 1-Zn_290, 1-Zn_310, 1-Zn_330, text

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Fe_130sup2.fcf
Contains datablock 1-Fe_130

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Fe_170sup3.fcf
Contains datablock 1-Fe_170

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Fe_210sup4.fcf
Contains datablock 1-Fe_210

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Fe_230sup5.fcf
Contains datablock 1-Fe_230

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Fe_250sup6.fcf
Contains datablock 1-Fe_250

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Fe_270sup7.fcf
Contains datablock 1-Fe_270

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Fe_290sup8.fcf
Contains datablock 1-Fe_290

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Fe_310sup9.fcf
Contains datablock 1-Fe_310

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Fe_330sup10.fcf
Contains datablock 1-Fe_330

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Fe_80sup11.fcf
Contains datablock 1-Fe_80

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Zn_130sup12.fcf
Contains datablock 1-Zn_130

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Zn_170sup13.fcf
Contains datablock 1-Zn_170

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Zn_210sup14.fcf
Contains datablock 1-Zn_210

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Zn_230sup15.fcf
Contains datablock 1-Zn_230

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Zn_250sup16.fcf
Contains datablock 1-Zn_250

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Zn_270sup17.fcf
Contains datablock 1-Zn_270

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Zn_290sup18.fcf
Contains datablock 1-Zn_290

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Zn_310sup19.fcf
Contains datablock 1-Zn_310

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Zn_330sup20.fcf
Contains datablock 1-Zn_330

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0021889807048571/aj50961-Zn_80sup21.fcf
Contains datablock 1-Zn_80

CCDC references: 671633; 671634; 671635; 671636; 671637; 671638; 671639; 671640; 671641; 671642; 671643; 671644; 671645; 671646; 671647; 671648; 671649; 671650; 671651; 671652; 671653; 671654

Computing details top

For all compounds, data collection: CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28); cell refinement: CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28); data reduction: CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
(1_80) top
Crystal data top
C27H33Cl2FeN7O8Z = 4
Mr = 710.35F(000) = 1472
Monoclinic, P21/cDx = 1.623 Mg m3
a = 10.1545 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 19.0923 (6) ŵ = 0.77 mm1
c = 15.0033 (5) ÅT = 80 K
β = 91.566 (3)°Polyhedron, dark red
V = 2907.65 (16) Å30.48 × 0.32 × 0.12 mm
Data collection top
KM4_CCD_Sapphire3
diffractometer
9683 independent reflections
Radiation source: fine-focus sealed tube7773 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
Detector resolution: 16.0328 pixels mm-1θmax = 32.8°, θmin = 2.9°
θ–scanh = 1415
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 2819
Tmin = 0.859, Tmax = 0.915l = 2022
27924 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.033Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.104H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.077P)2]
where P = (Fo2 + 2Fc2)/3
9683 reflections(Δ/σ)max = 0.002
409 parametersΔρmax = 1.17 e Å3
0 restraintsΔρmin = 0.92 e Å3
Crystal data top
C27H33Cl2FeN7O8V = 2907.65 (16) Å3
Mr = 710.35Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.1545 (3) ŵ = 0.77 mm1
b = 19.0923 (6) ÅT = 80 K
c = 15.0033 (5) Å0.48 × 0.32 × 0.12 mm
β = 91.566 (3)°
Data collection top
KM4_CCD_Sapphire3
diffractometer
9683 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
7773 reflections with I > 2σ(I)
Tmin = 0.859, Tmax = 0.915Rint = 0.019
27924 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0330 restraints
wR(F2) = 0.104H-atom parameters constrained
S = 1.01Δρmax = 1.17 e Å3
9683 reflectionsΔρmin = 0.92 e Å3
409 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.690211 (17)0.070335 (9)0.738786 (12)0.00889 (5)
Cl11.36072 (3)0.317743 (16)0.53965 (2)0.01442 (7)
Cl21.22109 (3)0.148594 (17)0.70315 (2)0.01646 (7)
N10.59931 (11)0.08996 (6)0.62485 (7)0.0119 (2)
N20.82478 (11)0.14027 (5)0.68762 (7)0.0113 (2)
N30.76396 (11)0.05570 (6)0.86826 (7)0.0112 (2)
N40.61402 (11)0.15266 (5)0.79509 (7)0.0110 (2)
N50.55423 (10)0.00608 (6)0.77560 (7)0.01085 (19)
N60.75700 (11)0.02024 (5)0.67705 (7)0.01080 (19)
N70.34716 (12)0.11171 (6)0.72605 (8)0.0149 (2)
O11.33356 (14)0.30786 (6)0.63242 (8)0.0293 (3)
O21.43983 (11)0.25958 (5)0.50878 (8)0.0229 (2)
O31.23813 (11)0.31988 (6)0.48836 (8)0.0237 (2)
O71.15883 (17)0.20914 (6)0.66589 (8)0.0427 (4)
O51.3114 (2)0.12212 (14)0.64010 (10)0.0885 (9)
O61.12703 (18)0.09646 (9)0.72134 (12)0.0588 (5)
O41.43043 (11)0.38259 (5)0.52781 (9)0.0247 (2)
O81.29242 (15)0.16424 (8)0.78461 (8)0.0424 (4)
C10.56030 (13)0.05679 (7)0.74537 (9)0.0130 (2)
H110.49830.09150.76170.016*
C20.66589 (13)0.07258 (6)0.68528 (9)0.0119 (2)
C30.67355 (14)0.13750 (7)0.64368 (9)0.0154 (2)
H130.60590.17130.65030.018*
C40.78173 (15)0.15198 (7)0.59231 (10)0.0169 (3)
H140.79000.19560.56260.020*
C50.87706 (14)0.10074 (7)0.58589 (9)0.0148 (2)
H150.95340.10990.55260.018*
C60.86338 (13)0.03514 (7)0.62776 (9)0.0128 (2)
C70.65953 (13)0.13179 (7)0.57233 (9)0.0136 (2)
H170.62430.14250.51460.016*
C80.78315 (13)0.16194 (7)0.60447 (9)0.0131 (2)
C90.85223 (14)0.20825 (7)0.55183 (10)0.0169 (3)
H190.81970.22070.49400.020*
C100.96994 (15)0.23601 (7)0.58552 (10)0.0194 (3)
H1101.02010.26770.55140.023*
C111.01183 (14)0.21611 (7)0.67022 (10)0.0180 (3)
H1111.09110.23510.69510.022*
C120.93884 (13)0.16806 (7)0.72018 (9)0.0137 (2)
C130.64740 (13)0.16306 (7)0.87705 (9)0.0134 (2)
H1130.62250.20460.90720.016*
C140.72457 (13)0.10914 (7)0.92198 (9)0.0128 (2)
C150.74646 (13)0.11163 (7)1.01357 (9)0.0154 (2)
H1150.72010.15121.04710.018*
C160.80780 (14)0.05494 (8)1.05493 (9)0.0162 (3)
H1160.82440.05451.11760.019*
C170.84424 (13)0.00103 (7)1.00225 (9)0.0155 (2)
H1170.88310.04121.02960.019*
C180.82487 (12)0.00050 (7)0.90929 (9)0.0129 (2)
C190.52123 (13)0.20338 (6)0.75491 (9)0.0129 (2)
H1190.53870.20860.69070.015*
H2190.53370.24960.78380.015*
C200.37916 (13)0.17848 (7)0.76650 (9)0.0136 (2)
H1200.36240.17540.83110.016*
H2200.31880.21430.74080.016*
C210.44603 (13)0.02260 (7)0.83490 (9)0.0129 (2)
H1210.47610.05780.87940.015*
H2210.42040.02020.86740.015*
C220.32538 (13)0.05135 (7)0.78174 (10)0.0145 (2)
H1220.28970.01320.74350.017*
H2220.25670.06350.82470.017*
C230.47012 (13)0.06281 (7)0.59391 (9)0.0144 (2)
H1230.46240.01320.61240.017*
H2230.46520.06430.52790.017*
C240.35324 (13)0.10451 (7)0.63083 (9)0.0153 (2)
H1240.35500.15210.60460.018*
H2240.27080.08180.60920.018*
C300.87636 (14)0.05917 (7)0.85555 (9)0.0154 (2)
H1300.80230.08550.82900.023*
H2300.92920.09020.89430.023*
H3300.93130.04090.80820.023*
C310.97310 (14)0.01704 (7)0.61955 (10)0.0171 (3)
H1310.94320.05610.58180.026*
H2311.04890.00570.59260.026*
H3310.99880.03470.67880.026*
C320.99303 (14)0.14653 (7)0.81003 (10)0.0166 (3)
H1320.94100.16830.85660.025*
H2321.08490.16180.81650.025*
H3320.98860.09540.81560.025*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.00930 (9)0.00897 (9)0.00846 (9)0.00018 (6)0.00173 (6)0.00010 (6)
Cl10.01709 (15)0.01223 (13)0.01417 (14)0.00057 (10)0.00453 (11)0.00128 (10)
Cl20.01672 (15)0.01946 (15)0.01319 (14)0.00193 (11)0.00049 (11)0.00028 (11)
N10.0130 (5)0.0116 (5)0.0111 (5)0.0005 (4)0.0012 (4)0.0006 (4)
N20.0114 (5)0.0100 (4)0.0128 (5)0.0004 (4)0.0038 (4)0.0008 (4)
N30.0096 (5)0.0136 (5)0.0106 (5)0.0018 (4)0.0008 (4)0.0005 (4)
N40.0099 (5)0.0111 (5)0.0123 (5)0.0003 (4)0.0033 (4)0.0004 (4)
N50.0100 (5)0.0126 (5)0.0100 (5)0.0002 (4)0.0009 (4)0.0019 (4)
N60.0119 (5)0.0108 (4)0.0097 (5)0.0007 (4)0.0010 (4)0.0007 (4)
N70.0172 (6)0.0137 (5)0.0139 (5)0.0010 (4)0.0013 (4)0.0015 (4)
O10.0434 (7)0.0293 (6)0.0159 (5)0.0131 (5)0.0110 (5)0.0074 (4)
O20.0237 (6)0.0174 (5)0.0283 (6)0.0038 (4)0.0114 (4)0.0012 (4)
O30.0188 (5)0.0251 (5)0.0270 (6)0.0008 (4)0.0022 (4)0.0053 (4)
O70.0888 (12)0.0182 (6)0.0214 (6)0.0189 (7)0.0037 (7)0.0054 (5)
O50.0697 (12)0.182 (2)0.0147 (7)0.0845 (14)0.0120 (7)0.0108 (10)
O60.0632 (11)0.0530 (9)0.0582 (10)0.0433 (8)0.0371 (9)0.0330 (8)
O40.0237 (6)0.0158 (5)0.0347 (6)0.0062 (4)0.0027 (5)0.0027 (4)
O80.0540 (9)0.0568 (9)0.0158 (6)0.0339 (7)0.0099 (6)0.0063 (6)
C10.0115 (6)0.0137 (5)0.0137 (6)0.0017 (4)0.0004 (4)0.0014 (4)
C20.0126 (6)0.0116 (5)0.0115 (6)0.0001 (4)0.0003 (4)0.0004 (4)
C30.0170 (6)0.0124 (5)0.0168 (6)0.0012 (5)0.0004 (5)0.0020 (5)
C40.0202 (7)0.0136 (6)0.0169 (6)0.0014 (5)0.0013 (5)0.0038 (5)
C50.0175 (6)0.0144 (6)0.0128 (6)0.0025 (5)0.0035 (5)0.0015 (5)
C60.0142 (6)0.0133 (5)0.0109 (5)0.0014 (4)0.0028 (4)0.0007 (4)
C70.0159 (6)0.0148 (5)0.0103 (5)0.0013 (5)0.0022 (4)0.0012 (4)
C80.0153 (6)0.0119 (5)0.0122 (6)0.0011 (4)0.0037 (4)0.0005 (4)
C90.0211 (7)0.0147 (6)0.0153 (6)0.0006 (5)0.0066 (5)0.0035 (5)
C100.0200 (7)0.0156 (6)0.0229 (7)0.0014 (5)0.0086 (5)0.0026 (5)
C110.0143 (6)0.0159 (6)0.0240 (7)0.0025 (5)0.0048 (5)0.0013 (5)
C120.0121 (6)0.0118 (5)0.0172 (6)0.0007 (4)0.0030 (5)0.0001 (4)
C130.0125 (6)0.0138 (5)0.0141 (6)0.0007 (4)0.0025 (4)0.0023 (4)
C140.0118 (6)0.0160 (6)0.0108 (5)0.0024 (4)0.0020 (4)0.0013 (4)
C150.0126 (6)0.0218 (6)0.0118 (6)0.0024 (5)0.0019 (4)0.0030 (5)
C160.0125 (6)0.0266 (7)0.0095 (6)0.0045 (5)0.0004 (4)0.0012 (5)
C170.0118 (6)0.0208 (6)0.0140 (6)0.0028 (5)0.0002 (4)0.0039 (5)
C180.0094 (5)0.0154 (6)0.0139 (6)0.0025 (4)0.0001 (4)0.0020 (4)
C190.0124 (6)0.0105 (5)0.0159 (6)0.0011 (4)0.0020 (4)0.0008 (4)
C200.0122 (6)0.0132 (5)0.0156 (6)0.0015 (4)0.0022 (4)0.0014 (4)
C210.0117 (6)0.0138 (5)0.0134 (6)0.0007 (4)0.0044 (4)0.0015 (4)
C220.0113 (6)0.0139 (5)0.0186 (6)0.0008 (4)0.0033 (5)0.0032 (5)
C230.0148 (6)0.0168 (6)0.0114 (6)0.0015 (5)0.0023 (4)0.0010 (4)
C240.0138 (6)0.0175 (6)0.0145 (6)0.0006 (5)0.0023 (5)0.0014 (5)
C300.0153 (6)0.0146 (6)0.0162 (6)0.0015 (5)0.0008 (5)0.0017 (5)
C310.0157 (6)0.0128 (6)0.0232 (7)0.0003 (5)0.0086 (5)0.0009 (5)
C320.0125 (6)0.0176 (6)0.0197 (7)0.0021 (5)0.0008 (5)0.0016 (5)
Geometric parameters (Å, º) top
Fe1—N51.9387 (11)C9—C101.390 (2)
Fe1—N41.9541 (11)C9—H190.9500
Fe1—N11.9566 (11)C10—C111.382 (2)
Fe1—N22.0729 (11)C10—H1100.9500
Fe1—N32.0815 (11)C11—C121.4082 (19)
Fe1—N62.0840 (11)C11—H1110.9500
Cl1—O11.4387 (12)C12—C321.4995 (19)
Cl1—O41.4395 (10)C13—C141.4489 (19)
Cl1—O31.4460 (12)C13—H1130.9500
Cl1—O21.4538 (10)C14—C151.3868 (18)
Cl2—O61.4113 (14)C15—C161.387 (2)
Cl2—O71.4245 (12)C15—H1150.9500
Cl2—O51.4277 (15)C16—C171.385 (2)
Cl2—O81.4349 (13)C16—H1160.9500
N1—C71.2880 (17)C17—C181.4034 (18)
N1—C231.4738 (17)C17—H1170.9500
N2—C121.3530 (17)C18—C301.4981 (19)
N2—C81.3702 (17)C19—C201.5333 (18)
N3—C181.3607 (16)C19—H1190.9900
N3—C141.3668 (16)C19—H2190.9900
N4—C131.2821 (17)C20—H1200.9900
N4—C191.4689 (16)C20—H2200.9900
N5—C11.2852 (16)C21—C221.5444 (19)
N5—C211.4669 (16)C21—H1210.9900
N6—C61.3558 (16)C21—H2210.9900
N6—C21.3696 (16)C22—H1220.9900
N7—C241.4383 (18)C22—H2220.9900
N7—C221.4440 (17)C23—C241.5444 (19)
N7—C201.4452 (17)C23—H1230.9900
C1—C21.4513 (18)C23—H2230.9900
C1—H110.9500C24—H1240.9900
C2—C31.3909 (18)C24—H2240.9900
C3—C41.387 (2)C30—H1300.9800
C3—H130.9500C30—H2300.9800
C4—C51.381 (2)C30—H3300.9800
C4—H140.9500C31—H1310.9800
C5—C61.4098 (18)C31—H2310.9800
C5—H150.9500C31—H3310.9800
C6—C311.5021 (18)C32—H1320.9800
C7—C81.4513 (19)C32—H2320.9800
C7—H170.9500C32—H3320.9800
C8—C91.3885 (18)
N5—Fe1—N495.30 (4)C10—C11—C12121.01 (13)
N5—Fe1—N192.72 (5)C10—C11—H111119.5
N4—Fe1—N192.33 (5)C12—C11—H111119.5
N5—Fe1—N2174.27 (4)N2—C12—C11121.41 (13)
N4—Fe1—N285.11 (4)N2—C12—C32120.43 (12)
N1—Fe1—N281.55 (5)C11—C12—C32118.14 (12)
N5—Fe1—N383.69 (4)N4—C13—C14117.49 (12)
N4—Fe1—N380.86 (4)N4—C13—H113121.3
N1—Fe1—N3171.95 (4)C14—C13—H113121.3
N2—Fe1—N3102.01 (4)N3—C14—C15124.63 (12)
N5—Fe1—N681.05 (4)N3—C14—C13114.80 (11)
N4—Fe1—N6175.67 (4)C15—C14—C13120.44 (12)
N1—Fe1—N685.53 (4)C16—C15—C14118.33 (12)
N2—Fe1—N698.28 (4)C16—C15—H115120.8
N3—Fe1—N6100.97 (4)C14—C15—H115120.8
O1—Cl1—O4109.88 (8)C17—C16—C15118.06 (12)
O1—Cl1—O3109.49 (8)C17—C16—H116121.0
O4—Cl1—O3109.21 (7)C15—C16—H116121.0
O1—Cl1—O2109.29 (7)C16—C17—C18121.24 (13)
O4—Cl1—O2109.86 (7)C16—C17—H117119.4
O3—Cl1—O2109.10 (7)C18—C17—H117119.4
O6—Cl2—O7110.65 (11)N3—C18—C17121.02 (12)
O6—Cl2—O5109.19 (15)N3—C18—C30120.43 (12)
O7—Cl2—O5108.26 (10)C17—C18—C30118.53 (12)
O6—Cl2—O8108.10 (8)N4—C19—C20110.13 (10)
O7—Cl2—O8111.94 (9)N4—C19—H119109.6
O5—Cl2—O8108.65 (11)C20—C19—H119109.6
C7—N1—C23117.31 (11)N4—C19—H219109.6
C7—N1—Fe1115.64 (9)C20—C19—H219109.6
C23—N1—Fe1127.04 (9)H119—C19—H219108.1
C12—N2—C8116.75 (11)N7—C20—C19115.30 (11)
C12—N2—Fe1133.27 (9)N7—C20—H120108.4
C8—N2—Fe1109.97 (9)C19—C20—H120108.4
C18—N3—C14116.62 (11)N7—C20—H220108.4
C18—N3—Fe1132.35 (9)C19—C20—H220108.4
C14—N3—Fe1110.27 (9)H120—C20—H220107.5
C13—N4—C19116.19 (11)N5—C21—C22111.10 (11)
C13—N4—Fe1116.22 (9)N5—C21—H121109.4
C19—N4—Fe1127.58 (9)C22—C21—H121109.4
C1—N5—C21117.31 (11)N5—C21—H221109.4
C1—N5—Fe1116.69 (9)C22—C21—H221109.4
C21—N5—Fe1126.00 (8)H121—C21—H221108.0
C6—N6—C2116.51 (11)N7—C22—C21116.78 (11)
C6—N6—Fe1133.66 (9)N7—C22—H122108.1
C2—N6—Fe1109.66 (8)C21—C22—H122108.1
C24—N7—C22120.66 (11)N7—C22—H222108.1
C24—N7—C20119.09 (11)C21—C22—H222108.1
C22—N7—C20119.82 (11)H122—C22—H222107.3
N5—C1—C2117.16 (12)N1—C23—C24113.07 (11)
N5—C1—H11121.4N1—C23—H123109.0
C2—C1—H11121.4C24—C23—H123109.0
N6—C2—C3124.29 (12)N1—C23—H223109.0
N6—C2—C1114.64 (11)C24—C23—H223109.0
C3—C2—C1121.01 (12)H123—C23—H223107.8
C4—C3—C2118.81 (13)N7—C24—C23117.37 (11)
C4—C3—H13120.6N7—C24—H124108.0
C2—C3—H13120.6C23—C24—H124108.0
C5—C4—C3117.69 (12)N7—C24—H224108.0
C5—C4—H14121.2C23—C24—H224108.0
C3—C4—H14121.2H124—C24—H224107.2
C4—C5—C6121.35 (13)C18—C30—H130109.5
C4—C5—H15119.3C18—C30—H230109.5
C6—C5—H15119.3H130—C30—H230109.5
N6—C6—C5121.27 (12)C18—C30—H330109.5
N6—C6—C31120.62 (11)H130—C30—H330109.5
C5—C6—C31118.05 (12)H230—C30—H330109.5
N1—C7—C8117.60 (12)C6—C31—H131109.5
N1—C7—H17121.2C6—C31—H231109.5
C8—C7—H17121.2H131—C31—H231109.5
N2—C8—C9124.20 (13)C6—C31—H331109.5
N2—C8—C7115.17 (11)H131—C31—H331109.5
C9—C8—C7120.62 (13)H231—C31—H331109.5
C8—C9—C10118.61 (13)C12—C32—H132109.5
C8—C9—H19120.7C12—C32—H232109.5
C10—C9—H19120.7H132—C32—H232109.5
C11—C10—C9118.00 (13)C12—C32—H332109.5
C11—C10—H110121.0H132—C32—H332109.5
C9—C10—H110121.0H232—C32—H332109.5
(1_130) top
Crystal data top
C27H33Cl2FeN7O8Z = 4
Mr = 710.35F(000) = 1472
Monoclinic, P21/cDx = 1.617 Mg m3
a = 10.1834 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 19.0720 (5) ŵ = 0.76 mm1
c = 15.0304 (4) ÅT = 130 K
β = 91.467 (3)°Polyhedron, dark red
V = 2918.21 (14) Å30.34 × 0.29 × 0.10 mm
Data collection top
KM4_CCD_Sapphire3
diffractometer
9866 independent reflections
Radiation source: fine-focus sealed tube7674 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
Detector resolution: 16.0328 pixels mm-1θmax = 32.8°, θmin = 2.9°
θ–scanh = 1515
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 2821
Tmin = 0.913, Tmax = 0.930l = 2221
28510 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.108H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.077P)2]
where P = (Fo2 + 2Fc2)/3
9866 reflections(Δ/σ)max = 0.001
409 parametersΔρmax = 0.96 e Å3
0 restraintsΔρmin = 0.90 e Å3
Crystal data top
C27H33Cl2FeN7O8V = 2918.21 (14) Å3
Mr = 710.35Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.1834 (3) ŵ = 0.76 mm1
b = 19.0720 (5) ÅT = 130 K
c = 15.0304 (4) Å0.34 × 0.29 × 0.10 mm
β = 91.467 (3)°
Data collection top
KM4_CCD_Sapphire3
diffractometer
9866 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
7674 reflections with I > 2σ(I)
Tmin = 0.913, Tmax = 0.930Rint = 0.019
28510 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0340 restraints
wR(F2) = 0.108H-atom parameters constrained
S = 1.00Δρmax = 0.96 e Å3
9866 reflectionsΔρmin = 0.90 e Å3
409 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.690194 (18)0.070631 (9)0.738984 (12)0.01215 (5)
Cl11.35960 (4)0.317568 (17)0.53966 (2)0.02135 (8)
Cl21.22187 (4)0.147864 (19)0.70178 (2)0.02436 (8)
N10.60041 (12)0.09032 (6)0.62508 (8)0.0164 (2)
N20.82476 (11)0.14067 (6)0.68822 (8)0.0157 (2)
N30.76317 (11)0.05579 (6)0.86822 (8)0.0151 (2)
N40.61381 (11)0.15264 (6)0.79526 (8)0.0147 (2)
N50.55433 (11)0.00653 (6)0.77539 (7)0.0148 (2)
N60.75697 (11)0.01981 (6)0.67721 (7)0.0144 (2)
N70.34861 (13)0.11176 (6)0.72533 (9)0.0212 (2)
O11.33103 (17)0.30785 (8)0.63173 (9)0.0480 (4)
O21.43939 (13)0.26003 (6)0.50936 (9)0.0350 (3)
O31.23805 (13)0.31945 (7)0.48820 (10)0.0381 (3)
O71.1604 (2)0.20824 (7)0.66475 (10)0.0569 (5)
O51.3108 (2)0.12124 (17)0.63961 (11)0.1193 (12)
O61.1269 (2)0.09715 (11)0.72124 (15)0.0827 (7)
O41.42766 (14)0.38232 (6)0.52789 (10)0.0388 (3)
O81.29317 (17)0.16250 (9)0.78276 (10)0.0549 (4)
C10.56066 (14)0.05608 (7)0.74540 (9)0.0177 (3)
H110.49880.09080.76160.021*
C20.66627 (14)0.07205 (7)0.68549 (9)0.0164 (2)
C30.67449 (16)0.13669 (7)0.64407 (10)0.0223 (3)
H130.60730.17070.65080.027*
C40.78226 (17)0.15089 (8)0.59269 (10)0.0246 (3)
H140.79050.19450.56280.030*
C50.87658 (15)0.10000 (7)0.58637 (10)0.0213 (3)
H150.95270.10920.55300.026*
C60.86323 (14)0.03458 (7)0.62806 (9)0.0176 (2)
C70.66077 (15)0.13217 (7)0.57302 (9)0.0193 (3)
H170.62600.14300.51540.023*
C80.78379 (14)0.16223 (7)0.60527 (9)0.0184 (3)
C90.85269 (16)0.20865 (8)0.55301 (10)0.0247 (3)
H190.82060.22120.49530.030*
C100.96933 (17)0.23632 (8)0.58677 (12)0.0283 (3)
H1101.01950.26810.55280.034*
C111.01077 (16)0.21638 (8)0.67140 (12)0.0258 (3)
H1111.08980.23540.69630.031*
C120.93794 (14)0.16856 (7)0.72111 (10)0.0189 (3)
C130.64631 (14)0.16280 (7)0.87717 (9)0.0183 (3)
H1130.62100.20420.90740.022*
C140.72284 (13)0.10896 (7)0.92194 (9)0.0175 (2)
C150.74480 (14)0.11132 (8)1.01323 (10)0.0214 (3)
H1150.71780.15071.04680.026*
C160.80676 (15)0.05527 (9)1.05452 (10)0.0233 (3)
H1160.82350.05491.11700.028*
C170.84363 (14)0.00033 (8)1.00178 (10)0.0215 (3)
H1170.88290.04041.02890.026*
C180.82440 (13)0.00112 (7)0.90909 (9)0.0175 (2)
C190.52160 (14)0.20332 (7)0.75499 (10)0.0178 (2)
H1190.53990.20880.69100.021*
H2190.53350.24960.78400.021*
C200.37980 (14)0.17839 (7)0.76561 (10)0.0195 (3)
H1200.36200.17540.82990.023*
H2200.32000.21420.73950.023*
C210.44585 (13)0.02294 (7)0.83423 (9)0.0180 (3)
H1210.47540.05820.87870.022*
H2210.42020.01990.86660.022*
C220.32608 (14)0.05156 (8)0.78108 (10)0.0208 (3)
H1220.29060.01330.74300.025*
H2220.25740.06400.82380.025*
C230.47187 (15)0.06313 (7)0.59398 (10)0.0204 (3)
H1230.46420.01350.61230.025*
H2230.46740.06470.52810.025*
C240.35519 (14)0.10445 (8)0.63040 (10)0.0216 (3)
H1240.35660.15200.60410.026*
H2240.27330.08150.60880.026*
C300.87639 (15)0.05824 (8)0.85548 (10)0.0212 (3)
H1300.80290.08490.82920.032*
H2300.92960.08910.89410.032*
H3300.93070.03970.80800.032*
C310.97215 (15)0.01746 (8)0.61996 (11)0.0241 (3)
H1310.94190.05700.58320.036*
H2311.04730.00500.59210.036*
H3310.99870.03450.67930.036*
C320.99155 (15)0.14705 (8)0.81062 (11)0.0236 (3)
H1320.93830.16800.85710.035*
H2321.08250.16320.81770.035*
H3320.98890.09580.81570.035*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.01313 (9)0.01160 (9)0.01179 (9)0.00024 (6)0.00187 (6)0.00018 (6)
Cl10.02606 (17)0.01719 (15)0.02112 (16)0.00130 (12)0.00661 (13)0.00186 (11)
Cl20.02579 (18)0.02477 (17)0.02245 (17)0.00202 (13)0.00119 (13)0.00121 (13)
N10.0190 (5)0.0161 (5)0.0142 (5)0.0010 (4)0.0010 (4)0.0007 (4)
N20.0161 (5)0.0131 (5)0.0180 (5)0.0009 (4)0.0047 (4)0.0006 (4)
N30.0131 (5)0.0178 (5)0.0144 (5)0.0018 (4)0.0011 (4)0.0003 (4)
N40.0133 (5)0.0136 (5)0.0174 (5)0.0004 (4)0.0035 (4)0.0010 (4)
N50.0135 (5)0.0160 (5)0.0148 (5)0.0008 (4)0.0007 (4)0.0020 (4)
N60.0168 (5)0.0128 (5)0.0135 (5)0.0004 (4)0.0012 (4)0.0009 (4)
N70.0236 (6)0.0186 (5)0.0213 (6)0.0018 (4)0.0002 (5)0.0026 (4)
O10.0740 (11)0.0454 (8)0.0255 (6)0.0237 (7)0.0193 (7)0.0134 (6)
O20.0373 (7)0.0247 (6)0.0439 (7)0.0044 (5)0.0178 (6)0.0003 (5)
O30.0316 (7)0.0391 (7)0.0433 (8)0.0011 (5)0.0041 (6)0.0103 (6)
O70.1101 (15)0.0282 (7)0.0324 (7)0.0263 (8)0.0032 (8)0.0079 (6)
O50.1108 (18)0.225 (3)0.0226 (8)0.117 (2)0.0156 (10)0.0140 (13)
O60.0834 (14)0.0748 (12)0.0872 (15)0.0553 (11)0.0479 (12)0.0435 (11)
O40.0368 (7)0.0237 (6)0.0561 (9)0.0091 (5)0.0050 (6)0.0039 (6)
O80.0645 (11)0.0722 (11)0.0272 (7)0.0313 (9)0.0112 (7)0.0073 (7)
C10.0166 (6)0.0167 (6)0.0200 (6)0.0024 (5)0.0009 (5)0.0021 (5)
C20.0184 (6)0.0142 (5)0.0164 (6)0.0010 (5)0.0004 (5)0.0001 (4)
C30.0260 (7)0.0154 (6)0.0256 (7)0.0025 (5)0.0005 (6)0.0029 (5)
C40.0315 (8)0.0178 (6)0.0245 (7)0.0030 (6)0.0008 (6)0.0066 (5)
C50.0264 (7)0.0187 (6)0.0190 (6)0.0043 (5)0.0045 (5)0.0027 (5)
C60.0210 (6)0.0164 (6)0.0155 (6)0.0021 (5)0.0033 (5)0.0009 (4)
C70.0240 (7)0.0194 (6)0.0146 (6)0.0025 (5)0.0024 (5)0.0018 (5)
C80.0221 (7)0.0158 (6)0.0178 (6)0.0016 (5)0.0065 (5)0.0016 (5)
C90.0324 (8)0.0202 (7)0.0221 (7)0.0001 (6)0.0099 (6)0.0060 (5)
C100.0300 (8)0.0222 (7)0.0332 (8)0.0026 (6)0.0130 (7)0.0058 (6)
C110.0213 (7)0.0218 (7)0.0346 (8)0.0042 (5)0.0075 (6)0.0014 (6)
C120.0169 (6)0.0157 (6)0.0245 (7)0.0003 (5)0.0053 (5)0.0010 (5)
C130.0177 (6)0.0183 (6)0.0191 (6)0.0013 (5)0.0040 (5)0.0035 (5)
C140.0155 (6)0.0224 (6)0.0147 (6)0.0031 (5)0.0018 (5)0.0019 (5)
C150.0178 (6)0.0305 (7)0.0160 (6)0.0038 (5)0.0021 (5)0.0045 (5)
C160.0185 (7)0.0376 (8)0.0137 (6)0.0063 (6)0.0007 (5)0.0021 (5)
C170.0159 (6)0.0295 (7)0.0189 (6)0.0027 (5)0.0007 (5)0.0062 (5)
C180.0131 (6)0.0215 (6)0.0177 (6)0.0030 (5)0.0003 (5)0.0034 (5)
C190.0177 (6)0.0132 (5)0.0227 (6)0.0018 (5)0.0029 (5)0.0013 (5)
C200.0175 (6)0.0175 (6)0.0237 (7)0.0022 (5)0.0032 (5)0.0017 (5)
C210.0161 (6)0.0186 (6)0.0195 (6)0.0000 (5)0.0057 (5)0.0026 (5)
C220.0159 (6)0.0202 (6)0.0266 (7)0.0009 (5)0.0041 (5)0.0047 (5)
C230.0229 (7)0.0217 (6)0.0165 (6)0.0020 (5)0.0044 (5)0.0000 (5)
C240.0186 (7)0.0246 (7)0.0215 (7)0.0007 (5)0.0042 (5)0.0025 (5)
C300.0221 (7)0.0196 (6)0.0218 (7)0.0028 (5)0.0025 (5)0.0026 (5)
C310.0233 (7)0.0174 (6)0.0322 (8)0.0004 (5)0.0129 (6)0.0015 (5)
C320.0171 (6)0.0245 (7)0.0293 (8)0.0050 (5)0.0007 (6)0.0019 (6)
Geometric parameters (Å, º) top
Fe1—N51.9357 (11)C9—C101.384 (2)
Fe1—N41.9494 (11)C9—H190.9500
Fe1—N11.9565 (12)C10—C111.383 (2)
Fe1—N22.0732 (11)C10—H1100.9500
Fe1—N32.0812 (11)C11—C121.403 (2)
Fe1—N62.0814 (11)C11—H1110.9500
Cl1—O41.4293 (12)C12—C321.496 (2)
Cl1—O11.4335 (13)C13—C141.445 (2)
Cl1—O31.4432 (14)C13—H1130.9500
Cl1—O21.4460 (12)C14—C151.3852 (19)
Cl2—O61.4036 (16)C15—C161.381 (2)
Cl2—O51.4126 (18)C15—H1150.9500
Cl2—O71.4177 (14)C16—C171.382 (2)
Cl2—O81.4287 (15)C16—H1160.9500
N1—C71.2852 (18)C17—C181.4022 (19)
N1—C231.4730 (18)C17—H1170.9500
N2—C121.3515 (18)C18—C301.494 (2)
N2—C81.3677 (18)C19—C201.533 (2)
N3—C181.3542 (17)C19—H1190.9900
N3—C141.3659 (17)C19—H2190.9900
N4—C131.2814 (18)C20—H1200.9900
N4—C191.4675 (17)C20—H2200.9900
N5—C11.2785 (17)C21—C221.541 (2)
N5—C211.4665 (17)C21—H1210.9900
N6—C61.3553 (17)C21—H2210.9900
N6—C21.3663 (17)C22—H1220.9900
N7—C241.4368 (19)C22—H2220.9900
N7—C201.4396 (18)C23—C241.538 (2)
N7—C221.4432 (18)C23—H1230.9900
C1—C21.4526 (19)C23—H2230.9900
C1—H110.9500C24—H1240.9900
C2—C31.3847 (19)C24—H2240.9900
C3—C41.385 (2)C30—H1300.9800
C3—H130.9500C30—H2300.9800
C4—C51.371 (2)C30—H3300.9800
C4—H140.9500C31—H1310.9800
C5—C61.4044 (19)C31—H2310.9800
C5—H150.9500C31—H3310.9800
C6—C311.496 (2)C32—H1320.9800
C7—C81.450 (2)C32—H2320.9800
C7—H170.9500C32—H3320.9800
C8—C91.3862 (19)
N5—Fe1—N495.05 (5)C10—C11—C12121.03 (15)
N5—Fe1—N192.71 (5)C10—C11—H111119.5
N4—Fe1—N192.46 (5)C12—C11—H111119.5
N5—Fe1—N2174.24 (5)N2—C12—C11121.22 (14)
N4—Fe1—N285.27 (4)N2—C12—C32120.61 (12)
N1—Fe1—N281.53 (5)C11—C12—C32118.12 (13)
N5—Fe1—N383.74 (4)N4—C13—C14117.57 (12)
N4—Fe1—N380.85 (5)N4—C13—H113121.2
N1—Fe1—N3172.09 (5)C14—C13—H113121.2
N2—Fe1—N3101.98 (5)N3—C14—C15124.50 (13)
N5—Fe1—N681.18 (5)N3—C14—C13114.77 (12)
N4—Fe1—N6175.55 (5)C15—C14—C13120.64 (13)
N1—Fe1—N685.38 (5)C16—C15—C14118.71 (13)
N2—Fe1—N698.24 (4)C16—C15—H115120.6
N3—Fe1—N6101.00 (4)C14—C15—H115120.6
O4—Cl1—O1110.02 (10)C15—C16—C17117.66 (13)
O4—Cl1—O3108.92 (8)C15—C16—H116121.2
O1—Cl1—O3109.16 (10)C17—C16—H116121.2
O4—Cl1—O2109.79 (8)C16—C17—C18121.45 (14)
O1—Cl1—O2109.61 (8)C16—C17—H117119.3
O3—Cl1—O2109.34 (8)C18—C17—H117119.3
O6—Cl2—O5110.31 (19)N3—C18—C17121.13 (13)
O6—Cl2—O7109.99 (13)N3—C18—C30120.27 (12)
O5—Cl2—O7108.45 (12)C17—C18—C30118.58 (12)
O6—Cl2—O8107.15 (10)N4—C19—C20110.32 (11)
O5—Cl2—O8108.25 (13)N4—C19—H119109.6
O7—Cl2—O8112.67 (10)C20—C19—H119109.6
C7—N1—C23117.41 (12)N4—C19—H219109.6
C7—N1—Fe1115.59 (10)C20—C19—H219109.6
C23—N1—Fe1126.99 (9)H119—C19—H219108.1
C12—N2—C8116.91 (12)N7—C20—C19115.37 (12)
C12—N2—Fe1133.19 (10)N7—C20—H120108.4
C8—N2—Fe1109.88 (9)C19—C20—H120108.4
C18—N3—C14116.44 (12)N7—C20—H220108.4
C18—N3—Fe1132.64 (9)C19—C20—H220108.4
C14—N3—Fe1110.20 (9)H120—C20—H220107.5
C13—N4—C19116.32 (11)N5—C21—C22111.19 (11)
C13—N4—Fe1116.24 (9)N5—C21—H121109.4
C19—N4—Fe1127.43 (9)C22—C21—H121109.4
C1—N5—C21117.22 (11)N5—C21—H221109.4
C1—N5—Fe1116.58 (10)C22—C21—H221109.4
C21—N5—Fe1126.20 (9)H121—C21—H221108.0
C6—N6—C2116.69 (11)N7—C22—C21116.58 (12)
C6—N6—Fe1133.61 (9)N7—C22—H122108.1
C2—N6—Fe1109.53 (9)C21—C22—H122108.1
C24—N7—C20119.20 (12)N7—C22—H222108.1
C24—N7—C22120.76 (12)C21—C22—H222108.1
C20—N7—C22119.65 (12)H122—C22—H222107.3
N5—C1—C2117.33 (12)N1—C23—C24113.26 (12)
N5—C1—H11121.3N1—C23—H123108.9
C2—C1—H11121.3C24—C23—H123108.9
N6—C2—C3124.02 (13)N1—C23—H223108.9
N6—C2—C1114.62 (11)C24—C23—H223108.9
C3—C2—C1121.31 (13)H123—C23—H223107.7
C2—C3—C4118.87 (14)N7—C24—C23117.34 (12)
C2—C3—H13120.6N7—C24—H124108.0
C4—C3—H13120.6C23—C24—H124108.0
C5—C4—C3117.84 (13)N7—C24—H224108.0
C5—C4—H14121.1C23—C24—H224108.0
C3—C4—H14121.1H124—C24—H224107.2
C4—C5—C6121.48 (14)C18—C30—H130109.5
C4—C5—H15119.3C18—C30—H230109.5
C6—C5—H15119.3H130—C30—H230109.5
N6—C6—C5121.03 (13)C18—C30—H330109.5
N6—C6—C31120.71 (12)H130—C30—H330109.5
C5—C6—C31118.21 (13)H230—C30—H330109.5
N1—C7—C8117.68 (12)C6—C31—H131109.5
N1—C7—H17121.2C6—C31—H231109.5
C8—C7—H17121.2H131—C31—H231109.5
N2—C8—C9124.16 (14)C6—C31—H331109.5
N2—C8—C7115.26 (12)H131—C31—H331109.5
C9—C8—C7120.57 (14)H231—C31—H331109.5
C10—C9—C8118.54 (15)C12—C32—H132109.5
C10—C9—H19120.7C12—C32—H232109.5
C8—C9—H19120.7H132—C32—H232109.5
C11—C10—C9118.10 (14)C12—C32—H332109.5
C11—C10—H110120.9H132—C32—H332109.5
C9—C10—H110120.9H232—C32—H332109.5
(1_150) top
Crystal data top
C27H33Cl2FeN7O8Z = 4
Mr = 710.35F(000) = 1472
Monoclinic, P21/cDx = 1.612 Mg m3
a = 10.1952 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 19.0901 (7) ŵ = 0.76 mm1
c = 15.0429 (6) ÅT = 150 K
β = 91.451 (4)°Polyhedron, dark red
V = 2926.8 (2) Å30.48 × 0.32 × 0.12 mm
Data collection top
KM4_CCD_Sapphire3
diffractometer
9709 independent reflections
Radiation source: fine-focus sealed tube7234 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
Detector resolution: 16.0328 pixels mm-1θmax = 32.8°, θmin = 2.9°
θ–scanh = 1514
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 2919
Tmin = 0.847, Tmax = 0.918l = 2220
27839 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.123H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.087P)2]
where P = (Fo2 + 2Fc2)/3
9709 reflections(Δ/σ)max = 0.001
409 parametersΔρmax = 1.14 e Å3
0 restraintsΔρmin = 1.09 e Å3
Crystal data top
C27H33Cl2FeN7O8V = 2926.8 (2) Å3
Mr = 710.35Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.1952 (4) ŵ = 0.76 mm1
b = 19.0901 (7) ÅT = 150 K
c = 15.0429 (6) Å0.48 × 0.32 × 0.12 mm
β = 91.451 (4)°
Data collection top
KM4_CCD_Sapphire3
diffractometer
9709 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
7234 reflections with I > 2σ(I)
Tmin = 0.847, Tmax = 0.918Rint = 0.019
27839 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0380 restraints
wR(F2) = 0.123H-atom parameters constrained
S = 1.01Δρmax = 1.14 e Å3
9709 reflectionsΔρmin = 1.09 e Å3
409 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.69008 (2)0.070773 (10)0.739033 (14)0.01446 (6)
Cl11.35921 (4)0.31745 (2)0.53970 (3)0.02509 (9)
Cl21.22219 (4)0.14755 (2)0.70110 (3)0.02915 (10)
N10.60068 (13)0.09047 (7)0.62512 (9)0.0192 (3)
N20.82469 (13)0.14081 (7)0.68851 (9)0.0187 (3)
N30.76266 (12)0.05587 (7)0.86830 (9)0.0175 (2)
N40.61365 (13)0.15259 (7)0.79528 (9)0.0174 (2)
N50.55447 (12)0.00673 (7)0.77522 (8)0.0172 (2)
N60.75687 (13)0.01963 (6)0.67739 (8)0.0167 (2)
N70.34922 (15)0.11184 (7)0.72486 (10)0.0246 (3)
O11.3302 (2)0.30807 (9)0.63146 (11)0.0574 (5)
O21.43906 (15)0.26009 (7)0.50966 (10)0.0407 (4)
O31.23818 (16)0.31940 (8)0.48798 (12)0.0462 (4)
O71.1616 (2)0.20778 (8)0.66404 (11)0.0637 (6)
O51.3103 (3)0.1212 (2)0.63961 (13)0.1371 (16)
O61.1270 (2)0.09737 (13)0.72128 (18)0.0951 (9)
O41.42616 (16)0.38216 (7)0.52783 (13)0.0468 (4)
O81.2934 (2)0.16168 (11)0.78202 (12)0.0615 (5)
C10.56084 (16)0.05585 (8)0.74523 (11)0.0208 (3)
H110.49900.09050.76140.025*
C20.66638 (16)0.07172 (8)0.68559 (11)0.0191 (3)
C30.67469 (18)0.13627 (9)0.64420 (12)0.0259 (3)
H130.60760.17030.65090.031*
C40.78217 (19)0.15046 (9)0.59295 (12)0.0283 (4)
H140.79040.19410.56320.034*
C50.87634 (18)0.09973 (9)0.58644 (11)0.0251 (3)
H150.95230.10890.55300.030*
C60.86298 (16)0.03423 (8)0.62822 (10)0.0204 (3)
C70.66109 (17)0.13228 (8)0.57336 (11)0.0227 (3)
H170.62650.14320.51580.027*
C80.78403 (17)0.16240 (8)0.60578 (11)0.0215 (3)
C90.85260 (19)0.20883 (9)0.55362 (13)0.0288 (4)
H190.82050.22140.49600.035*
C100.9688 (2)0.23644 (10)0.58744 (14)0.0333 (4)
H1101.01900.26810.55350.040*
C111.01018 (18)0.21669 (9)0.67207 (14)0.0298 (4)
H1111.08890.23580.69700.036*
C120.93768 (16)0.16889 (8)0.72159 (12)0.0224 (3)
C130.64544 (16)0.16261 (8)0.87728 (11)0.0215 (3)
H1130.61950.20380.90760.026*
C140.72226 (15)0.10886 (8)0.92182 (11)0.0202 (3)
C150.74386 (16)0.11118 (9)1.01316 (11)0.0245 (3)
H1150.71630.15041.04670.029*
C160.80602 (17)0.05546 (10)1.05428 (11)0.0265 (3)
H1160.82270.05521.11670.032*
C170.84330 (16)0.00003 (10)1.00172 (11)0.0248 (3)
H1170.88270.04001.02890.030*
C180.82427 (15)0.00133 (8)0.90902 (10)0.0202 (3)
C190.52175 (16)0.20328 (8)0.75501 (11)0.0209 (3)
H1190.54040.20890.69110.025*
H2190.53350.24940.78420.025*
C200.37997 (16)0.17839 (8)0.76516 (12)0.0230 (3)
H1200.36170.17540.82940.028*
H2200.32040.21420.73890.028*
C210.44589 (15)0.02304 (8)0.83391 (11)0.0210 (3)
H1210.47520.05830.87840.025*
H2210.42020.01980.86610.025*
C220.32615 (16)0.05166 (9)0.78062 (13)0.0245 (3)
H1220.29070.01350.74250.029*
H2220.25750.06420.82320.029*
C230.47264 (17)0.06338 (9)0.59376 (11)0.0238 (3)
H1230.46500.01370.61180.029*
H2230.46850.06510.52800.029*
C240.35589 (17)0.10448 (9)0.63011 (12)0.0257 (3)
H1240.35710.15200.60380.031*
H2240.27420.08140.60850.031*
C300.87626 (17)0.05792 (9)0.85548 (12)0.0246 (3)
H1300.80290.08440.82890.037*
H2300.92900.08880.89410.037*
H3300.93100.03940.80830.037*
C310.97178 (18)0.01783 (9)0.62010 (13)0.0278 (4)
H1310.94170.05710.58300.042*
H2311.04710.00470.59270.042*
H3310.99770.03510.67930.042*
C320.99094 (17)0.14725 (9)0.81075 (13)0.0274 (4)
H1320.93740.16780.85720.041*
H2321.08170.16360.81810.041*
H3320.98870.09610.81550.041*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.01545 (11)0.01416 (10)0.01385 (11)0.00023 (7)0.00229 (7)0.00017 (7)
Cl10.0304 (2)0.02076 (18)0.02448 (19)0.00191 (14)0.00800 (15)0.00194 (14)
Cl20.0302 (2)0.0287 (2)0.0284 (2)0.00211 (16)0.00160 (17)0.00208 (16)
N10.0215 (6)0.0190 (6)0.0171 (6)0.0004 (5)0.0009 (5)0.0005 (5)
N20.0187 (6)0.0160 (5)0.0217 (6)0.0006 (5)0.0062 (5)0.0008 (5)
N30.0150 (6)0.0207 (6)0.0168 (6)0.0022 (5)0.0009 (5)0.0006 (5)
N40.0158 (6)0.0174 (6)0.0192 (6)0.0004 (4)0.0043 (5)0.0012 (5)
N50.0156 (6)0.0184 (6)0.0175 (6)0.0002 (4)0.0015 (5)0.0030 (5)
N60.0193 (6)0.0153 (5)0.0157 (6)0.0004 (4)0.0016 (5)0.0007 (4)
N70.0270 (7)0.0218 (6)0.0248 (7)0.0017 (5)0.0004 (6)0.0030 (5)
O10.0878 (14)0.0546 (10)0.0310 (8)0.0291 (9)0.0227 (9)0.0157 (7)
O20.0431 (9)0.0297 (7)0.0503 (9)0.0045 (6)0.0207 (7)0.0007 (6)
O30.0365 (8)0.0490 (9)0.0529 (10)0.0010 (7)0.0053 (7)0.0127 (8)
O70.1189 (18)0.0340 (8)0.0382 (9)0.0292 (10)0.0033 (10)0.0091 (7)
O50.136 (2)0.251 (4)0.0261 (10)0.136 (3)0.0177 (13)0.0150 (16)
O60.0945 (17)0.0869 (15)0.1011 (19)0.0619 (14)0.0523 (15)0.0497 (14)
O40.0445 (9)0.0275 (7)0.0687 (12)0.0104 (6)0.0075 (8)0.0049 (7)
O80.0708 (13)0.0808 (13)0.0323 (8)0.0295 (10)0.0116 (8)0.0082 (9)
C10.0190 (7)0.0198 (7)0.0236 (8)0.0023 (5)0.0007 (6)0.0026 (6)
C20.0209 (7)0.0165 (6)0.0198 (7)0.0008 (5)0.0005 (6)0.0003 (5)
C30.0292 (9)0.0184 (7)0.0301 (9)0.0026 (6)0.0000 (7)0.0039 (6)
C40.0350 (9)0.0214 (8)0.0284 (9)0.0027 (7)0.0004 (7)0.0077 (6)
C50.0305 (9)0.0232 (8)0.0219 (8)0.0051 (6)0.0056 (6)0.0030 (6)
C60.0242 (8)0.0201 (7)0.0170 (7)0.0027 (6)0.0044 (6)0.0007 (5)
C70.0280 (8)0.0228 (7)0.0175 (7)0.0030 (6)0.0032 (6)0.0018 (6)
C80.0251 (8)0.0190 (7)0.0206 (7)0.0019 (6)0.0071 (6)0.0021 (6)
C90.0364 (10)0.0242 (8)0.0263 (8)0.0003 (7)0.0119 (7)0.0068 (7)
C100.0348 (10)0.0250 (8)0.0407 (11)0.0027 (7)0.0160 (8)0.0061 (7)
C110.0248 (8)0.0249 (8)0.0400 (10)0.0052 (7)0.0085 (7)0.0021 (7)
C120.0189 (7)0.0188 (7)0.0298 (8)0.0000 (6)0.0062 (6)0.0013 (6)
C130.0207 (7)0.0215 (7)0.0224 (8)0.0014 (6)0.0044 (6)0.0049 (6)
C140.0177 (7)0.0256 (7)0.0172 (7)0.0035 (6)0.0022 (5)0.0023 (6)
C150.0202 (8)0.0355 (9)0.0178 (7)0.0043 (6)0.0026 (6)0.0045 (6)
C160.0204 (8)0.0442 (10)0.0150 (7)0.0072 (7)0.0008 (6)0.0015 (7)
C170.0187 (7)0.0340 (9)0.0217 (8)0.0037 (6)0.0006 (6)0.0065 (6)
C180.0155 (7)0.0247 (7)0.0204 (7)0.0033 (5)0.0001 (5)0.0026 (6)
C190.0200 (7)0.0166 (6)0.0261 (8)0.0019 (5)0.0033 (6)0.0009 (6)
C200.0196 (7)0.0204 (7)0.0291 (8)0.0030 (6)0.0031 (6)0.0027 (6)
C210.0192 (7)0.0224 (7)0.0219 (8)0.0001 (6)0.0067 (6)0.0034 (6)
C220.0176 (7)0.0235 (7)0.0327 (9)0.0009 (6)0.0054 (6)0.0049 (6)
C230.0262 (8)0.0261 (8)0.0188 (7)0.0023 (6)0.0052 (6)0.0008 (6)
C240.0215 (8)0.0287 (8)0.0265 (8)0.0016 (6)0.0057 (6)0.0025 (7)
C300.0250 (8)0.0235 (7)0.0251 (8)0.0039 (6)0.0026 (6)0.0027 (6)
C310.0278 (9)0.0204 (7)0.0360 (10)0.0011 (6)0.0150 (7)0.0008 (7)
C320.0196 (8)0.0288 (8)0.0337 (9)0.0051 (6)0.0009 (7)0.0017 (7)
Geometric parameters (Å, º) top
Fe1—N51.9341 (13)C9—C101.382 (3)
Fe1—N41.9483 (13)C9—H190.9500
Fe1—N11.9570 (13)C10—C111.383 (3)
Fe1—N22.0740 (13)C10—H1100.9500
Fe1—N62.0819 (13)C11—C121.401 (2)
Fe1—N32.0825 (13)C11—H1110.9500
Cl1—O41.4248 (14)C12—C321.493 (3)
Cl1—O11.4303 (16)C13—C141.445 (2)
Cl1—O31.4425 (17)C13—H1130.9500
Cl1—O21.4438 (14)C14—C151.387 (2)
Cl2—O51.399 (2)C15—C161.377 (3)
Cl2—O61.402 (2)C15—H1150.9500
Cl2—O71.4132 (16)C16—C171.381 (3)
Cl2—O81.4271 (17)C16—H1160.9500
N1—C71.283 (2)C17—C181.403 (2)
N1—C231.471 (2)C17—H1170.9500
N2—C121.354 (2)C18—C301.494 (2)
N2—C81.365 (2)C19—C201.533 (2)
N3—C181.354 (2)C19—H1190.9900
N3—C141.363 (2)C19—H2190.9900
N4—C131.282 (2)C20—H1200.9900
N4—C191.467 (2)C20—H2200.9900
N5—C11.279 (2)C21—C221.543 (2)
N5—C211.467 (2)C21—H1210.9900
N6—C61.3548 (19)C21—H2210.9900
N6—C21.3641 (19)C22—H1220.9900
N7—C241.436 (2)C22—H2220.9900
N7—C201.439 (2)C23—C241.538 (2)
N7—C221.445 (2)C23—H1230.9900
C1—C21.450 (2)C23—H2230.9900
C1—H110.9500C24—H1240.9900
C2—C31.384 (2)C24—H2240.9900
C3—C41.382 (3)C30—H1300.9800
C3—H130.9500C30—H2300.9800
C4—C51.369 (3)C30—H3300.9800
C4—H140.9500C31—H1310.9800
C5—C61.408 (2)C31—H2310.9800
C5—H150.9500C31—H3310.9800
C6—C311.497 (2)C32—H1320.9800
C7—C81.452 (2)C32—H2320.9800
C7—H170.9500C32—H3320.9800
C8—C91.385 (2)
N5—Fe1—N495.04 (5)C10—C11—C12120.95 (17)
N5—Fe1—N192.72 (6)C10—C11—H111119.5
N4—Fe1—N192.51 (6)C12—C11—H111119.5
N5—Fe1—N2174.27 (5)N2—C12—C11121.20 (16)
N4—Fe1—N285.30 (5)N2—C12—C32120.50 (14)
N1—Fe1—N281.55 (6)C11—C12—C32118.25 (16)
N5—Fe1—N681.12 (5)N4—C13—C14117.45 (14)
N4—Fe1—N6175.51 (5)N4—C13—H113121.3
N1—Fe1—N685.39 (5)C14—C13—H113121.3
N2—Fe1—N698.29 (5)N3—C14—C15124.48 (15)
N5—Fe1—N383.72 (5)N3—C14—C13114.92 (14)
N4—Fe1—N380.82 (5)C15—C14—C13120.49 (15)
N1—Fe1—N3172.10 (5)C16—C15—C14118.70 (16)
N2—Fe1—N3101.97 (5)C16—C15—H115120.7
N6—Fe1—N3100.96 (5)C14—C15—H115120.7
O4—Cl1—O1109.95 (12)C15—C16—C17117.75 (15)
O4—Cl1—O3108.42 (10)C15—C16—H116121.1
O1—Cl1—O3109.18 (12)C17—C16—H116121.1
O4—Cl1—O2110.04 (9)C16—C17—C18121.44 (16)
O1—Cl1—O2109.83 (9)C16—C17—H117119.3
O3—Cl1—O2109.40 (9)C18—C17—H117119.3
O5—Cl2—O6110.9 (2)N3—C18—C17120.97 (15)
O5—Cl2—O7108.27 (14)N3—C18—C30120.34 (14)
O6—Cl2—O7110.08 (15)C17—C18—C30118.67 (15)
O5—Cl2—O8108.09 (15)N4—C19—C20110.38 (13)
O6—Cl2—O8106.51 (12)N4—C19—H119109.6
O7—Cl2—O8112.98 (12)C20—C19—H119109.6
C7—N1—C23117.39 (14)N4—C19—H219109.6
C7—N1—Fe1115.51 (11)C20—C19—H219109.6
C23—N1—Fe1127.10 (11)H119—C19—H219108.1
C12—N2—C8116.83 (14)N7—C20—C19115.32 (14)
C12—N2—Fe1133.26 (11)N7—C20—H120108.4
C8—N2—Fe1109.89 (11)C19—C20—H120108.4
C18—N3—C14116.55 (14)N7—C20—H220108.4
C18—N3—Fe1132.62 (11)C19—C20—H220108.4
C14—N3—Fe1110.16 (10)H120—C20—H220107.5
C13—N4—C19116.24 (13)N5—C21—C22111.20 (13)
C13—N4—Fe1116.33 (11)N5—C21—H121109.4
C19—N4—Fe1127.42 (10)C22—C21—H121109.4
C1—N5—C21117.14 (13)N5—C21—H221109.4
C1—N5—Fe1116.62 (11)C22—C21—H221109.4
C21—N5—Fe1126.24 (10)H121—C21—H221108.0
C6—N6—C2116.79 (13)N7—C22—C21116.41 (14)
C6—N6—Fe1133.50 (11)N7—C22—H122108.2
C2—N6—Fe1109.54 (10)C21—C22—H122108.2
C24—N7—C20119.30 (14)N7—C22—H222108.2
C24—N7—C22120.73 (14)C21—C22—H222108.2
C20—N7—C22119.62 (15)H122—C22—H222107.3
N5—C1—C2117.27 (14)N1—C23—C24113.28 (13)
N5—C1—H11121.4N1—C23—H123108.9
C2—C1—H11121.4C24—C23—H123108.9
N6—C2—C3123.99 (15)N1—C23—H223108.9
N6—C2—C1114.70 (13)C24—C23—H223108.9
C3—C2—C1121.26 (15)H123—C23—H223107.7
C4—C3—C2118.92 (16)N7—C24—C23117.36 (14)
C4—C3—H13120.5N7—C24—H124108.0
C2—C3—H13120.5C23—C24—H124108.0
C5—C4—C3117.94 (15)N7—C24—H224108.0
C5—C4—H14121.0C23—C24—H224108.0
C3—C4—H14121.0H124—C24—H224107.2
C4—C5—C6121.37 (16)C18—C30—H130109.5
C4—C5—H15119.3C18—C30—H230109.5
C6—C5—H15119.3H130—C30—H230109.5
N6—C6—C5120.94 (15)C18—C30—H330109.5
N6—C6—C31120.77 (14)H130—C30—H330109.5
C5—C6—C31118.24 (15)H230—C30—H330109.5
N1—C7—C8117.78 (15)C6—C31—H131109.5
N1—C7—H17121.1C6—C31—H231109.5
C8—C7—H17121.1H131—C31—H231109.5
N2—C8—C9124.31 (16)C6—C31—H331109.5
N2—C8—C7115.22 (14)H131—C31—H331109.5
C9—C8—C7120.47 (16)H231—C31—H331109.5
C10—C9—C8118.42 (18)C12—C32—H132109.5
C10—C9—H19120.8C12—C32—H232109.5
C8—C9—H19120.8H132—C32—H232109.5
C9—C10—C11118.25 (16)C12—C32—H332109.5
C9—C10—H110120.9H132—C32—H332109.5
C11—C10—H110120.9H232—C32—H332109.5
(1_170) top
Crystal data top
C27H33Cl2FeN7O8Z = 4
Mr = 710.35F(000) = 1472
Monoclinic, P21/cDx = 1.606 Mg m3
a = 10.2122 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 19.1179 (6) ŵ = 0.76 mm1
c = 15.0573 (5) ÅT = 170 K
β = 91.420 (3)°Polyhedron, dark red
V = 2938.82 (16) Å30.34 × 0.29 × 0.10 mm
Data collection top
KM4_CCD_Sapphire3
diffractometer
9889 independent reflections
Radiation source: fine-focus sealed tube7336 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
Detector resolution: 16.0328 pixels mm-1θmax = 32.9°, θmin = 2.9°
θ–scanh = 1515
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 2821
Tmin = 0.892, Tmax = 0.928l = 2221
28521 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.130H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0918P)2]
where P = (Fo2 + 2Fc2)/3
9889 reflections(Δ/σ)max = 0.002
409 parametersΔρmax = 1.41 e Å3
0 restraintsΔρmin = 1.27 e Å3
Crystal data top
C27H33Cl2FeN7O8V = 2938.82 (16) Å3
Mr = 710.35Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.2122 (3) ŵ = 0.76 mm1
b = 19.1179 (6) ÅT = 170 K
c = 15.0573 (5) Å0.34 × 0.29 × 0.10 mm
β = 91.420 (3)°
Data collection top
KM4_CCD_Sapphire3
diffractometer
9889 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
7336 reflections with I > 2σ(I)
Tmin = 0.892, Tmax = 0.928Rint = 0.020
28521 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0400 restraints
wR(F2) = 0.130H-atom parameters constrained
S = 1.01Δρmax = 1.41 e Å3
9889 reflectionsΔρmin = 1.27 e Å3
409 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.69007 (2)0.070934 (11)0.739112 (14)0.01593 (7)
Cl11.35888 (5)0.31737 (2)0.53973 (3)0.02822 (10)
Cl21.22249 (5)0.14711 (2)0.70021 (3)0.03350 (11)
N10.60134 (14)0.09081 (7)0.62519 (9)0.0217 (3)
N20.82464 (14)0.14115 (7)0.68887 (9)0.0206 (3)
N30.76222 (13)0.05584 (7)0.86833 (9)0.0192 (3)
N40.61332 (13)0.15258 (7)0.79547 (9)0.0194 (3)
N50.55448 (13)0.00676 (7)0.77503 (9)0.0193 (3)
N60.75675 (13)0.01942 (7)0.67744 (9)0.0187 (2)
N70.35024 (16)0.11189 (8)0.72436 (11)0.0281 (3)
O11.3290 (2)0.30816 (11)0.63110 (12)0.0678 (6)
O21.43898 (17)0.26034 (8)0.50985 (11)0.0464 (4)
O31.23812 (18)0.31924 (10)0.48802 (13)0.0547 (5)
O71.1623 (3)0.20721 (9)0.66330 (13)0.0710 (7)
O51.3093 (4)0.1208 (2)0.63930 (15)0.160 (2)
O61.1268 (3)0.09788 (15)0.7214 (2)0.1065 (11)
O41.42480 (18)0.38220 (8)0.52801 (14)0.0546 (5)
O81.2938 (2)0.16066 (12)0.78080 (13)0.0684 (6)
C10.56092 (17)0.05566 (9)0.74515 (12)0.0233 (3)
H110.49920.09030.76120.028*
C20.66655 (17)0.07142 (8)0.68560 (11)0.0215 (3)
C30.67539 (19)0.13584 (9)0.64444 (13)0.0291 (4)
H130.60890.17000.65140.035*
C40.7825 (2)0.14980 (10)0.59299 (13)0.0320 (4)
H140.79070.19320.56290.038*
C50.8760 (2)0.09941 (9)0.58678 (12)0.0284 (4)
H150.95200.10870.55360.034*
C60.86274 (17)0.03400 (8)0.62827 (11)0.0228 (3)
C70.66181 (18)0.13260 (9)0.57364 (11)0.0255 (3)
H170.62750.14350.51610.031*
C80.78418 (18)0.16272 (9)0.60615 (11)0.0241 (3)
C90.8527 (2)0.20921 (10)0.55435 (13)0.0325 (4)
H190.82080.22190.49680.039*
C100.9685 (2)0.23678 (10)0.58831 (15)0.0374 (5)
H1101.01870.26860.55450.045*
C111.0093 (2)0.21691 (10)0.67251 (15)0.0339 (4)
H1111.08790.23600.69740.041*
C120.93709 (17)0.16911 (9)0.72198 (12)0.0251 (3)
C130.64493 (17)0.16235 (9)0.87735 (11)0.0239 (3)
H1130.61900.20350.90770.029*
C140.72123 (16)0.10877 (9)0.92196 (11)0.0223 (3)
C150.74295 (17)0.11092 (10)1.01294 (11)0.0278 (4)
H1150.71520.15001.04650.033*
C160.80539 (18)0.05549 (11)1.05406 (12)0.0301 (4)
H1160.82200.05531.11640.036*
C170.84302 (17)0.00029 (10)1.00153 (11)0.0277 (4)
H1170.88270.03951.02870.033*
C180.82400 (16)0.00157 (9)0.90901 (11)0.0222 (3)
C190.52199 (17)0.20327 (8)0.75512 (12)0.0241 (3)
H1190.54110.20890.69140.029*
H2190.53350.24930.78440.029*
C200.38042 (17)0.17840 (9)0.76478 (13)0.0262 (3)
H1200.36160.17540.82890.031*
H2200.32110.21410.73830.031*
C210.44566 (16)0.02319 (9)0.83339 (11)0.0237 (3)
H1210.47480.05830.87790.028*
H2210.41970.01960.86550.028*
C220.32689 (17)0.05182 (10)0.78008 (13)0.0278 (4)
H1220.29150.01370.74200.033*
H2220.25820.06440.82250.033*
C230.47343 (18)0.06360 (9)0.59367 (12)0.0271 (3)
H1230.46590.01400.61170.032*
H2230.46940.06540.52790.032*
C240.35694 (18)0.10451 (10)0.62984 (12)0.0289 (4)
H1240.35800.15190.60350.035*
H2240.27550.08130.60830.035*
C300.87646 (19)0.05751 (9)0.85550 (12)0.0277 (4)
H1300.80340.08480.83010.042*
H2300.93100.08770.89380.042*
H3300.92930.03880.80750.042*
C310.97097 (19)0.01810 (9)0.62033 (14)0.0314 (4)
H1310.94020.05780.58440.047*
H2311.04570.00400.59180.047*
H3310.99800.03460.67960.047*
C320.99022 (18)0.14749 (10)0.81105 (13)0.0312 (4)
H1320.93620.16770.85750.047*
H2321.08050.16420.81860.047*
H3320.98880.09640.81560.047*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.01740 (11)0.01491 (11)0.01556 (11)0.00025 (7)0.00218 (7)0.00026 (7)
Cl10.0343 (2)0.02305 (19)0.0277 (2)0.00234 (15)0.00864 (17)0.00220 (15)
Cl20.0345 (2)0.0310 (2)0.0349 (2)0.00247 (17)0.00291 (18)0.00325 (18)
N10.0261 (7)0.0207 (6)0.0182 (6)0.0012 (5)0.0004 (5)0.0005 (5)
N20.0212 (6)0.0171 (6)0.0239 (6)0.0012 (5)0.0060 (5)0.0003 (5)
N30.0172 (6)0.0222 (6)0.0182 (6)0.0020 (5)0.0011 (5)0.0010 (5)
N40.0176 (6)0.0180 (6)0.0227 (6)0.0001 (5)0.0044 (5)0.0013 (5)
N50.0175 (6)0.0199 (6)0.0205 (6)0.0011 (5)0.0007 (5)0.0035 (5)
N60.0226 (6)0.0159 (5)0.0177 (6)0.0008 (5)0.0015 (5)0.0012 (4)
N70.0305 (8)0.0244 (7)0.0292 (8)0.0023 (6)0.0007 (6)0.0035 (6)
O10.1039 (17)0.0639 (12)0.0368 (9)0.0358 (11)0.0279 (10)0.0192 (8)
O20.0502 (10)0.0330 (7)0.0571 (10)0.0049 (7)0.0245 (8)0.0001 (7)
O30.0444 (10)0.0575 (11)0.0617 (11)0.0006 (8)0.0076 (8)0.0166 (9)
O70.129 (2)0.0393 (9)0.0447 (10)0.0325 (11)0.0030 (11)0.0102 (8)
O50.169 (3)0.282 (5)0.0295 (11)0.161 (3)0.0194 (15)0.0188 (18)
O60.102 (2)0.0984 (18)0.116 (2)0.0674 (16)0.0553 (17)0.0541 (17)
O40.0515 (10)0.0317 (8)0.0811 (14)0.0115 (7)0.0091 (9)0.0056 (8)
O80.0758 (14)0.0899 (16)0.0387 (9)0.0260 (12)0.0115 (9)0.0105 (10)
C10.0217 (8)0.0208 (7)0.0275 (8)0.0031 (6)0.0004 (6)0.0029 (6)
C20.0244 (8)0.0179 (7)0.0223 (7)0.0007 (6)0.0010 (6)0.0004 (5)
C30.0332 (9)0.0193 (7)0.0349 (9)0.0029 (7)0.0002 (7)0.0040 (6)
C40.0412 (11)0.0228 (8)0.0319 (9)0.0038 (7)0.0003 (8)0.0085 (7)
C50.0361 (10)0.0248 (8)0.0246 (8)0.0054 (7)0.0065 (7)0.0031 (6)
C60.0270 (8)0.0215 (7)0.0200 (7)0.0030 (6)0.0041 (6)0.0010 (6)
C70.0320 (9)0.0249 (8)0.0198 (7)0.0034 (7)0.0025 (6)0.0022 (6)
C80.0282 (8)0.0208 (7)0.0237 (8)0.0024 (6)0.0080 (6)0.0019 (6)
C90.0421 (11)0.0263 (8)0.0298 (9)0.0006 (8)0.0132 (8)0.0078 (7)
C100.0403 (11)0.0278 (9)0.0450 (12)0.0031 (8)0.0179 (9)0.0082 (8)
C110.0284 (9)0.0275 (9)0.0461 (11)0.0061 (7)0.0098 (8)0.0027 (8)
C120.0218 (8)0.0208 (7)0.0331 (9)0.0002 (6)0.0076 (7)0.0011 (6)
C130.0224 (8)0.0241 (7)0.0254 (8)0.0015 (6)0.0048 (6)0.0058 (6)
C140.0194 (7)0.0286 (8)0.0189 (7)0.0042 (6)0.0027 (6)0.0029 (6)
C150.0231 (8)0.0410 (10)0.0194 (7)0.0051 (7)0.0029 (6)0.0057 (7)
C160.0241 (8)0.0494 (11)0.0167 (7)0.0080 (8)0.0013 (6)0.0017 (7)
C170.0205 (8)0.0390 (10)0.0235 (8)0.0035 (7)0.0013 (6)0.0073 (7)
C180.0172 (7)0.0270 (8)0.0224 (7)0.0039 (6)0.0002 (6)0.0044 (6)
C190.0238 (8)0.0173 (7)0.0313 (9)0.0027 (6)0.0033 (6)0.0007 (6)
C200.0216 (8)0.0233 (8)0.0337 (9)0.0029 (6)0.0029 (7)0.0029 (7)
C210.0213 (8)0.0243 (7)0.0257 (8)0.0003 (6)0.0078 (6)0.0038 (6)
C220.0204 (8)0.0259 (8)0.0373 (10)0.0012 (6)0.0050 (7)0.0057 (7)
C230.0304 (9)0.0286 (8)0.0219 (8)0.0020 (7)0.0065 (7)0.0004 (6)
C240.0256 (9)0.0319 (9)0.0289 (9)0.0012 (7)0.0069 (7)0.0028 (7)
C300.0288 (9)0.0258 (8)0.0282 (9)0.0044 (7)0.0033 (7)0.0034 (6)
C310.0311 (9)0.0225 (8)0.0416 (10)0.0005 (7)0.0173 (8)0.0015 (7)
C320.0228 (8)0.0332 (9)0.0375 (10)0.0060 (7)0.0013 (7)0.0018 (7)
Geometric parameters (Å, º) top
Fe1—N51.9370 (13)C9—C101.382 (3)
Fe1—N41.9504 (13)C9—H190.9500
Fe1—N11.9572 (14)C10—C111.378 (3)
Fe1—N22.0771 (14)C10—H1100.9500
Fe1—N32.0834 (13)C11—C121.401 (2)
Fe1—N62.0836 (13)C11—H1110.9500
Cl1—O41.4235 (15)C12—C321.493 (3)
Cl1—O11.4274 (17)C13—C141.443 (2)
Cl1—O21.4416 (15)C13—H1130.9500
Cl1—O31.4425 (19)C14—C151.383 (2)
Cl2—O51.386 (2)C15—C161.376 (3)
Cl2—O61.399 (2)C15—H1150.9500
Cl2—O71.4107 (17)C16—C171.379 (3)
Cl2—O81.4235 (19)C16—H1160.9500
N1—C71.283 (2)C17—C181.402 (2)
N1—C231.474 (2)C17—H1170.9500
N2—C121.351 (2)C18—C301.494 (2)
N2—C81.366 (2)C19—C201.532 (2)
N3—C181.353 (2)C19—H1190.9900
N3—C141.367 (2)C19—H2190.9900
N4—C131.280 (2)C20—H1200.9900
N4—C191.466 (2)C20—H2200.9900
N5—C11.278 (2)C21—C221.538 (2)
N5—C211.468 (2)C21—H1210.9900
N6—C61.355 (2)C21—H2210.9900
N6—C21.363 (2)C22—H1220.9900
N7—C241.433 (2)C22—H2220.9900
N7—C201.440 (2)C23—C241.535 (3)
N7—C221.445 (2)C23—H1230.9900
C1—C21.451 (2)C23—H2230.9900
C1—H110.9500C24—H1240.9900
C2—C31.383 (2)C24—H2240.9900
C3—C41.382 (3)C30—H1300.9800
C3—H130.9500C30—H2300.9800
C4—C51.361 (3)C30—H3300.9800
C4—H140.9500C31—H1310.9800
C5—C61.406 (2)C31—H2310.9800
C5—H150.9500C31—H3310.9800
C6—C311.495 (2)C32—H1320.9800
C7—C81.450 (3)C32—H2320.9800
C7—H170.9500C32—H3320.9800
C8—C91.384 (2)
N5—Fe1—N495.03 (6)C10—C11—C12121.18 (19)
N5—Fe1—N192.81 (6)C10—C11—H111119.4
N4—Fe1—N192.50 (6)C12—C11—H111119.4
N5—Fe1—N2174.26 (6)N2—C12—C11121.07 (18)
N4—Fe1—N285.29 (5)N2—C12—C32120.59 (15)
N1—Fe1—N281.46 (6)C11—C12—C32118.29 (17)
N5—Fe1—N383.70 (5)N4—C13—C14117.71 (15)
N4—Fe1—N380.86 (6)N4—C13—H113121.1
N1—Fe1—N3172.17 (6)C14—C13—H113121.1
N2—Fe1—N3101.99 (5)N3—C14—C15124.29 (16)
N5—Fe1—N680.97 (6)N3—C14—C13114.86 (14)
N4—Fe1—N6175.37 (6)C15—C14—C13120.76 (15)
N1—Fe1—N685.39 (6)C16—C15—C14118.94 (17)
N2—Fe1—N698.45 (5)C16—C15—H115120.5
N3—Fe1—N6100.92 (5)C14—C15—H115120.5
O4—Cl1—O1109.86 (14)C15—C16—C17117.64 (16)
O4—Cl1—O2110.25 (10)C15—C16—H116121.2
O1—Cl1—O2110.12 (10)C17—C16—H116121.2
O4—Cl1—O3108.18 (12)C16—C17—C18121.52 (17)
O1—Cl1—O3108.85 (14)C16—C17—H117119.2
O2—Cl1—O3109.54 (11)C18—C17—H117119.2
O5—Cl2—O6111.6 (3)N3—C18—C17120.98 (16)
O5—Cl2—O7108.33 (16)N3—C18—C30120.32 (15)
O6—Cl2—O7109.74 (17)C17—C18—C30118.68 (15)
O5—Cl2—O8107.94 (18)N4—C19—C20110.33 (13)
O6—Cl2—O8105.86 (14)N4—C19—H119109.6
O7—Cl2—O8113.36 (14)C20—C19—H119109.6
C7—N1—C23117.46 (15)N4—C19—H219109.6
C7—N1—Fe1115.58 (12)C20—C19—H219109.6
C23—N1—Fe1126.96 (11)H119—C19—H219108.1
C12—N2—C8116.89 (15)N7—C20—C19115.25 (15)
C12—N2—Fe1133.26 (12)N7—C20—H120108.5
C8—N2—Fe1109.83 (11)C19—C20—H120108.5
C18—N3—C14116.52 (14)N7—C20—H220108.5
C18—N3—Fe1132.78 (11)C19—C20—H220108.5
C14—N3—Fe1110.05 (11)H120—C20—H220107.5
C13—N4—C19116.44 (14)N5—C21—C22111.26 (14)
C13—N4—Fe1116.19 (11)N5—C21—H121109.4
C19—N4—Fe1127.37 (11)C22—C21—H121109.4
C1—N5—C21117.19 (14)N5—C21—H221109.4
C1—N5—Fe1116.74 (12)C22—C21—H221109.4
C21—N5—Fe1126.07 (11)H121—C21—H221108.0
C6—N6—C2116.74 (14)N7—C22—C21116.51 (14)
C6—N6—Fe1133.49 (11)N7—C22—H122108.2
C2—N6—Fe1109.60 (10)C21—C22—H122108.2
C24—N7—C20119.45 (15)N7—C22—H222108.2
C24—N7—C22120.71 (15)C21—C22—H222108.2
C20—N7—C22119.52 (16)H122—C22—H222107.3
N5—C1—C2117.19 (15)N1—C23—C24113.24 (14)
N5—C1—H11121.4N1—C23—H123108.9
C2—C1—H11121.4C24—C23—H123108.9
N6—C2—C3123.88 (16)N1—C23—H223108.9
N6—C2—C1114.75 (14)C24—C23—H223108.9
C3—C2—C1121.31 (16)H123—C23—H223107.7
C4—C3—C2118.98 (17)N7—C24—C23117.32 (15)
C4—C3—H13120.5N7—C24—H124108.0
C2—C3—H13120.5C23—C24—H124108.0
C5—C4—C3117.91 (16)N7—C24—H224108.0
C5—C4—H14121.0C23—C24—H224108.0
C3—C4—H14121.0H124—C24—H224107.2
C4—C5—C6121.58 (17)C18—C30—H130109.5
C4—C5—H15119.2C18—C30—H230109.5
C6—C5—H15119.2H130—C30—H230109.5
N6—C6—C5120.84 (16)C18—C30—H330109.5
N6—C6—C31120.58 (15)H130—C30—H330109.5
C5—C6—C31118.53 (15)H230—C30—H330109.5
N1—C7—C8117.83 (15)C6—C31—H131109.5
N1—C7—H17121.1C6—C31—H231109.5
C8—C7—H17121.1H131—C31—H231109.5
N2—C8—C9124.20 (17)C6—C31—H331109.5
N2—C8—C7115.25 (15)H131—C31—H331109.5
C9—C8—C7120.55 (17)H231—C31—H331109.5
C10—C9—C8118.47 (19)C12—C32—H132109.5
C10—C9—H19120.8C12—C32—H232109.5
C8—C9—H19120.8H132—C32—H232109.5
C11—C10—C9118.16 (17)C12—C32—H332109.5
C11—C10—H110120.9H132—C32—H332109.5
C9—C10—H110120.9H232—C32—H332109.5
(1_190) top
Crystal data top
C27H33Cl2FeN7O8Z = 4
Mr = 710.35F(000) = 1472
Monoclinic, P21/cDx = 1.598 Mg m3
a = 10.2327 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 19.1464 (7) ŵ = 0.76 mm1
c = 15.0753 (6) ÅT = 190 K
β = 91.402 (4)°Polyhedron, dark red
V = 2952.7 (2) Å30.48 × 0.32 × 0.12 mm
Data collection top
KM4_CCD_Sapphire3
diffractometer
9686 independent reflections
Radiation source: fine-focus sealed tube7065 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
Detector resolution: 16.0328 pixels mm-1θmax = 32.8°, θmin = 2.9°
θ–scanh = 1415
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 2919
Tmin = 0.845, Tmax = 0.916l = 2022
27639 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.156H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.115P)2]
where P = (Fo2 + 2Fc2)/3
9686 reflections(Δ/σ)max = 0.002
409 parametersΔρmax = 1.57 e Å3
0 restraintsΔρmin = 1.44 e Å3
Crystal data top
C27H33Cl2FeN7O8V = 2952.7 (2) Å3
Mr = 710.35Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.2327 (4) ŵ = 0.76 mm1
b = 19.1464 (7) ÅT = 190 K
c = 15.0753 (6) Å0.48 × 0.32 × 0.12 mm
β = 91.402 (4)°
Data collection top
KM4_CCD_Sapphire3
diffractometer
9686 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
7065 reflections with I > 2σ(I)
Tmin = 0.845, Tmax = 0.916Rint = 0.019
27639 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0450 restraints
wR(F2) = 0.156H-atom parameters constrained
S = 1.00Δρmax = 1.57 e Å3
9686 reflectionsΔρmin = 1.44 e Å3
409 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.69024 (2)0.071134 (12)0.739252 (16)0.01865 (8)
Cl11.35861 (5)0.31728 (3)0.53973 (3)0.03263 (12)
Cl21.22282 (6)0.14667 (3)0.69927 (4)0.03961 (14)
N10.60219 (16)0.09121 (9)0.62516 (11)0.0252 (3)
N20.82519 (16)0.14153 (8)0.68944 (11)0.0243 (3)
N30.76184 (15)0.05600 (8)0.86868 (10)0.0224 (3)
N40.61339 (15)0.15257 (8)0.79581 (11)0.0227 (3)
N50.55459 (15)0.00676 (8)0.77462 (10)0.0226 (3)
N60.75671 (15)0.01930 (8)0.67750 (10)0.0220 (3)
N70.35191 (19)0.11199 (9)0.72380 (13)0.0331 (4)
O11.3283 (3)0.30848 (13)0.63036 (15)0.0802 (8)
O21.4388 (2)0.26056 (9)0.51023 (14)0.0533 (5)
O31.2386 (2)0.31921 (12)0.48774 (17)0.0650 (6)
O71.1633 (3)0.20652 (11)0.66224 (15)0.0802 (8)
O51.3084 (5)0.1207 (3)0.63907 (18)0.181 (3)
O61.1268 (3)0.09826 (18)0.7220 (2)0.1196 (14)
O41.4233 (2)0.38203 (10)0.52806 (18)0.0659 (6)
O81.2942 (3)0.15982 (15)0.77956 (15)0.0769 (8)
C10.56130 (19)0.05551 (10)0.74492 (14)0.0270 (4)
H110.49960.09010.76090.032*
C20.6672 (2)0.07128 (9)0.68565 (13)0.0255 (4)
C30.6763 (2)0.13545 (11)0.64449 (16)0.0341 (4)
H130.61000.16960.65150.041*
C40.7827 (3)0.14927 (11)0.59308 (15)0.0370 (5)
H140.79050.19260.56290.044*
C50.8762 (2)0.09917 (11)0.58683 (14)0.0331 (4)
H150.95200.10850.55370.040*
C60.8629 (2)0.03375 (10)0.62850 (13)0.0269 (4)
C70.6624 (2)0.13310 (11)0.57392 (13)0.0302 (4)
H170.62800.14420.51650.036*
C80.7849 (2)0.16307 (10)0.60658 (13)0.0288 (4)
C90.8528 (2)0.20973 (11)0.55526 (16)0.0380 (5)
H190.82100.22260.49790.046*
C100.9685 (3)0.23719 (12)0.58953 (18)0.0440 (6)
H1101.01870.26890.55590.053*
C111.0090 (2)0.21737 (12)0.67355 (18)0.0395 (5)
H1111.08720.23650.69870.047*
C120.9367 (2)0.16950 (10)0.72256 (15)0.0293 (4)
C130.64400 (19)0.16222 (10)0.87803 (14)0.0281 (4)
H1130.61730.20300.90860.034*
C140.72055 (18)0.10868 (10)0.92212 (13)0.0260 (4)
C150.7419 (2)0.11071 (12)1.01331 (13)0.0322 (4)
H1150.71360.14961.04700.039*
C160.8049 (2)0.05548 (13)1.05421 (14)0.0348 (5)
H1160.82170.05531.11650.042*
C170.8429 (2)0.00051 (12)1.00173 (14)0.0324 (4)
H1170.88290.03911.02880.039*
C180.82388 (18)0.00172 (10)0.90917 (13)0.0257 (4)
C190.52212 (19)0.20334 (10)0.75560 (14)0.0280 (4)
H1190.54180.20950.69210.034*
H2190.53300.24910.78540.034*
C200.3810 (2)0.17825 (10)0.76429 (15)0.0307 (4)
H1200.36130.17520.82810.037*
H2200.32200.21380.73750.037*
C210.44555 (19)0.02308 (11)0.83258 (14)0.0283 (4)
H1210.47440.05810.87730.034*
H2210.41940.01970.86450.034*
C220.3272 (2)0.05186 (11)0.77917 (16)0.0327 (4)
H1220.29190.01390.74090.039*
H2220.25850.06450.82140.039*
C230.4746 (2)0.06412 (11)0.59321 (14)0.0323 (4)
H1230.46700.01450.61090.039*
H2230.47090.06610.52760.039*
C240.3582 (2)0.10491 (12)0.62942 (15)0.0338 (4)
H1240.35920.15230.60330.041*
H2240.27690.08180.60790.041*
C300.8761 (2)0.05711 (11)0.85583 (15)0.0318 (4)
H1300.80340.08530.83210.048*
H2300.93300.08630.89360.048*
H3300.92630.03840.80670.048*
C310.9707 (2)0.01836 (11)0.62064 (17)0.0364 (5)
H1310.94060.05750.58350.055*
H2311.04610.00390.59350.055*
H3310.99610.03570.67980.055*
C320.9897 (2)0.14767 (12)0.81146 (16)0.0362 (5)
H1320.93630.16800.85790.054*
H2321.08010.16400.81880.054*
H3320.98760.09660.81600.054*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.02030 (13)0.01789 (13)0.01785 (13)0.00033 (8)0.00235 (9)0.00037 (8)
Cl10.0394 (3)0.0276 (2)0.0313 (2)0.00320 (18)0.0097 (2)0.00232 (18)
Cl20.0399 (3)0.0356 (3)0.0431 (3)0.0026 (2)0.0038 (2)0.0043 (2)
N10.0289 (8)0.0247 (7)0.0221 (7)0.0016 (6)0.0004 (6)0.0009 (6)
N20.0243 (7)0.0204 (7)0.0285 (8)0.0017 (6)0.0070 (6)0.0006 (6)
N30.0200 (7)0.0263 (7)0.0209 (7)0.0031 (5)0.0011 (5)0.0011 (6)
N40.0210 (7)0.0216 (7)0.0257 (7)0.0000 (5)0.0049 (6)0.0016 (6)
N50.0199 (7)0.0238 (7)0.0242 (7)0.0009 (5)0.0009 (6)0.0043 (6)
N60.0259 (7)0.0200 (6)0.0202 (7)0.0000 (5)0.0011 (6)0.0015 (5)
N70.0374 (10)0.0281 (8)0.0336 (9)0.0030 (7)0.0023 (8)0.0041 (7)
O10.123 (2)0.0748 (15)0.0443 (12)0.0437 (15)0.0330 (13)0.0223 (11)
O20.0586 (12)0.0376 (9)0.0651 (13)0.0059 (8)0.0282 (10)0.0000 (8)
O30.0514 (12)0.0707 (14)0.0723 (15)0.0008 (10)0.0100 (11)0.0201 (12)
O70.143 (3)0.0455 (12)0.0519 (13)0.0363 (14)0.0052 (14)0.0131 (10)
O50.199 (4)0.314 (6)0.0330 (13)0.180 (5)0.0228 (19)0.021 (2)
O60.114 (3)0.111 (2)0.131 (3)0.073 (2)0.057 (2)0.060 (2)
O40.0617 (13)0.0358 (10)0.1007 (18)0.0128 (9)0.0130 (12)0.0067 (11)
O80.0838 (18)0.101 (2)0.0450 (12)0.0226 (14)0.0113 (12)0.0116 (12)
C10.0254 (9)0.0246 (8)0.0308 (10)0.0036 (7)0.0002 (7)0.0041 (7)
C20.0290 (9)0.0209 (8)0.0264 (9)0.0018 (7)0.0020 (7)0.0014 (6)
C30.0389 (11)0.0226 (9)0.0406 (12)0.0026 (8)0.0028 (9)0.0046 (8)
C40.0473 (13)0.0276 (10)0.0360 (11)0.0030 (9)0.0001 (10)0.0087 (8)
C50.0413 (12)0.0300 (10)0.0283 (10)0.0062 (8)0.0064 (8)0.0034 (8)
C60.0327 (10)0.0251 (8)0.0230 (9)0.0031 (7)0.0054 (7)0.0015 (7)
C70.0370 (11)0.0301 (9)0.0237 (9)0.0045 (8)0.0028 (8)0.0020 (7)
C80.0341 (10)0.0256 (9)0.0271 (9)0.0032 (7)0.0089 (8)0.0028 (7)
C90.0481 (13)0.0315 (10)0.0350 (11)0.0014 (9)0.0156 (10)0.0082 (9)
C100.0467 (14)0.0330 (11)0.0533 (15)0.0021 (10)0.0225 (12)0.0089 (10)
C110.0337 (11)0.0315 (10)0.0539 (14)0.0060 (9)0.0119 (10)0.0015 (10)
C120.0255 (9)0.0247 (8)0.0379 (11)0.0006 (7)0.0075 (8)0.0011 (8)
C130.0267 (9)0.0275 (9)0.0302 (10)0.0019 (7)0.0062 (7)0.0069 (7)
C140.0226 (9)0.0336 (9)0.0219 (8)0.0043 (7)0.0030 (7)0.0037 (7)
C150.0270 (10)0.0474 (12)0.0224 (9)0.0057 (8)0.0034 (7)0.0067 (8)
C160.0280 (10)0.0572 (13)0.0194 (9)0.0091 (9)0.0016 (7)0.0010 (9)
C170.0244 (9)0.0453 (12)0.0275 (10)0.0043 (8)0.0000 (7)0.0081 (8)
C180.0199 (8)0.0311 (9)0.0260 (9)0.0043 (7)0.0004 (7)0.0035 (7)
C190.0269 (9)0.0212 (8)0.0361 (10)0.0021 (7)0.0043 (8)0.0016 (7)
C200.0268 (10)0.0272 (9)0.0383 (11)0.0036 (7)0.0037 (8)0.0024 (8)
C210.0245 (9)0.0299 (9)0.0308 (10)0.0003 (7)0.0090 (7)0.0060 (7)
C220.0238 (9)0.0301 (9)0.0443 (12)0.0015 (7)0.0051 (8)0.0069 (9)
C230.0359 (11)0.0342 (10)0.0265 (9)0.0016 (8)0.0088 (8)0.0026 (8)
C240.0302 (10)0.0358 (11)0.0348 (11)0.0012 (8)0.0087 (8)0.0026 (8)
C300.0323 (10)0.0296 (9)0.0333 (10)0.0060 (8)0.0037 (8)0.0032 (8)
C310.0356 (11)0.0268 (9)0.0476 (13)0.0013 (8)0.0190 (10)0.0013 (8)
C320.0264 (10)0.0386 (11)0.0436 (12)0.0063 (8)0.0021 (9)0.0016 (9)
Geometric parameters (Å, º) top
Fe1—N51.9406 (15)C9—C101.384 (4)
Fe1—N41.9517 (15)C9—H190.9500
Fe1—N11.9601 (16)C10—C111.376 (4)
Fe1—N22.0829 (16)C10—H1100.9500
Fe1—N32.0876 (16)C11—C121.400 (3)
Fe1—N62.0878 (15)C11—H1110.9500
Cl1—O11.418 (2)C12—C321.493 (3)
Cl1—O41.4184 (19)C13—C141.442 (3)
Cl1—O21.4379 (18)C13—H1130.9500
Cl1—O31.441 (2)C14—C151.387 (3)
Cl2—O51.370 (3)C15—C161.377 (3)
Cl2—O61.399 (3)C15—H1150.9500
Cl2—O71.407 (2)C16—C171.378 (3)
Cl2—O81.421 (2)C16—H1160.9500
N1—C71.281 (3)C17—C181.404 (3)
N1—C231.474 (3)C17—H1170.9500
N2—C121.345 (3)C18—C301.491 (3)
N2—C81.370 (3)C19—C201.531 (3)
N3—C181.355 (2)C19—H1190.9900
N3—C141.364 (2)C19—H2190.9900
N4—C131.284 (3)C20—H1200.9900
N4—C191.469 (2)C20—H2200.9900
N5—C11.276 (2)C21—C221.540 (3)
N5—C211.468 (2)C21—H1210.9900
N6—C61.357 (2)C21—H2210.9900
N6—C21.360 (2)C22—H1220.9900
N7—C241.432 (3)C22—H2220.9900
N7—C201.436 (3)C23—C241.536 (3)
N7—C221.448 (3)C23—H1230.9900
C1—C21.453 (3)C23—H2230.9900
C1—H110.9500C24—H1240.9900
C2—C31.381 (3)C24—H2240.9900
C3—C41.377 (3)C30—H1300.9800
C3—H130.9500C30—H2300.9800
C4—C51.360 (3)C30—H3300.9800
C4—H140.9500C31—H1310.9800
C5—C61.409 (3)C31—H2310.9800
C5—H150.9500C31—H3310.9800
C6—C311.494 (3)C32—H1320.9800
C7—C81.453 (3)C32—H2320.9800
C7—H170.9500C32—H3320.9800
C8—C91.381 (3)
N5—Fe1—N495.09 (6)C10—C11—C12121.0 (2)
N5—Fe1—N192.82 (7)C10—C11—H111119.5
N4—Fe1—N192.59 (7)C12—C11—H111119.5
N5—Fe1—N2174.26 (7)N2—C12—C11121.3 (2)
N4—Fe1—N285.31 (6)N2—C12—C32120.52 (18)
N1—Fe1—N281.45 (7)C11—C12—C32118.1 (2)
N5—Fe1—N383.81 (6)N4—C13—C14117.35 (17)
N4—Fe1—N380.70 (6)N4—C13—H113121.3
N1—Fe1—N3172.17 (7)C14—C13—H113121.3
N2—Fe1—N3101.89 (6)N3—C14—C15124.21 (19)
N5—Fe1—N680.72 (6)N3—C14—C13115.20 (17)
N4—Fe1—N6175.23 (6)C15—C14—C13120.49 (18)
N1—Fe1—N685.36 (6)C16—C15—C14118.9 (2)
N2—Fe1—N698.62 (6)C16—C15—H115120.6
N3—Fe1—N6101.01 (6)C14—C15—H115120.6
O1—Cl1—O4109.69 (18)C15—C16—C17117.71 (19)
O1—Cl1—O2110.36 (12)C15—C16—H116121.1
O4—Cl1—O2110.50 (13)C17—C16—H116121.1
O1—Cl1—O3108.86 (18)C16—C17—C18121.6 (2)
O4—Cl1—O3107.72 (15)C16—C17—H117119.2
O2—Cl1—O3109.65 (13)C18—C17—H117119.2
O5—Cl2—O6112.7 (3)N3—C18—C17120.81 (19)
O5—Cl2—O7108.1 (2)N3—C18—C30120.44 (17)
O6—Cl2—O7109.7 (2)C17—C18—C30118.74 (18)
O5—Cl2—O8107.8 (2)N4—C19—C20110.41 (16)
O6—Cl2—O8104.97 (17)N4—C19—H119109.6
O7—Cl2—O8113.71 (16)C20—C19—H119109.6
C7—N1—C23117.25 (17)N4—C19—H219109.6
C7—N1—Fe1115.74 (14)C20—C19—H219109.6
C23—N1—Fe1127.00 (13)H119—C19—H219108.1
C12—N2—C8116.90 (17)N7—C20—C19115.28 (17)
C12—N2—Fe1133.44 (14)N7—C20—H120108.5
C8—N2—Fe1109.64 (13)C19—C20—H120108.5
C18—N3—C14116.70 (16)N7—C20—H220108.5
C18—N3—Fe1132.63 (13)C19—C20—H220108.5
C14—N3—Fe1110.04 (12)H120—C20—H220107.5
C13—N4—C19116.15 (16)N5—C21—C22111.38 (17)
C13—N4—Fe1116.43 (13)N5—C21—H121109.4
C19—N4—Fe1127.40 (13)C22—C21—H121109.4
C1—N5—C21117.13 (16)N5—C21—H221109.4
C1—N5—Fe1116.87 (14)C22—C21—H221109.4
C21—N5—Fe1125.99 (13)H121—C21—H221108.0
C6—N6—C2116.72 (16)N7—C22—C21116.09 (17)
C6—N6—Fe1133.29 (13)N7—C22—H122108.3
C2—N6—Fe1109.83 (12)C21—C22—H122108.3
C24—N7—C20119.47 (18)N7—C22—H222108.3
C24—N7—C22120.68 (18)C21—C22—H222108.3
C20—N7—C22119.66 (19)H122—C22—H222107.4
N5—C1—C2117.21 (17)N1—C23—C24113.15 (17)
N5—C1—H11121.4N1—C23—H123108.9
C2—C1—H11121.4C24—C23—H123108.9
N6—C2—C3123.92 (19)N1—C23—H223108.9
N6—C2—C1114.68 (16)C24—C23—H223108.9
C3—C2—C1121.36 (19)H123—C23—H223107.8
C4—C3—C2119.1 (2)N7—C24—C23117.09 (18)
C4—C3—H13120.4N7—C24—H124108.0
C2—C3—H13120.4C23—C24—H124108.0
C5—C4—C3118.1 (2)N7—C24—H224108.0
C5—C4—H14121.0C23—C24—H224108.0
C3—C4—H14121.0H124—C24—H224107.3
C4—C5—C6121.4 (2)C18—C30—H130109.5
C4—C5—H15119.3C18—C30—H230109.5
C6—C5—H15119.3H130—C30—H230109.5
N6—C6—C5120.74 (19)C18—C30—H330109.5
N6—C6—C31120.63 (17)H130—C30—H330109.5
C5—C6—C31118.59 (18)H230—C30—H330109.5
N1—C7—C8117.78 (18)C6—C31—H131109.5
N1—C7—H17121.1C6—C31—H231109.5
C8—C7—H17121.1H131—C31—H231109.5
N2—C8—C9124.1 (2)C6—C31—H331109.5
N2—C8—C7115.35 (17)H131—C31—H331109.5
C9—C8—C7120.5 (2)H231—C31—H331109.5
C8—C9—C10118.3 (2)C12—C32—H132109.5
C8—C9—H19120.8C12—C32—H232109.5
C10—C9—H19120.8H132—C32—H232109.5
C11—C10—C9118.3 (2)C12—C32—H332109.5
C11—C10—H110120.8H132—C32—H332109.5
C9—C10—H110120.8H232—C32—H332109.5
(1_210) top
Crystal data top
C27H33Cl2FeN7O8Z = 4
Mr = 710.35F(000) = 1472
Monoclinic, P21/cDx = 1.584 Mg m3
a = 10.2747 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 19.2019 (6) ŵ = 0.75 mm1
c = 15.1011 (5) ÅT = 210 K
β = 91.399 (3)°Polyhedron, dark red
V = 2978.46 (18) Å30.34 × 0.29 × 0.10 mm
Data collection top
KM4_CCD_Sapphire3
diffractometer
9941 independent reflections
Radiation source: fine-focus sealed tube6795 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
Detector resolution: 16.0328 pixels mm-1θmax = 32.9°, θmin = 2.9°
θ–scanh = 1515
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 2821
Tmin = 0.903, Tmax = 0.934l = 2221
28574 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.155H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.105P)2]
where P = (Fo2 + 2Fc2)/3
9941 reflections(Δ/σ)max < 0.001
409 parametersΔρmax = 1.29 e Å3
0 restraintsΔρmin = 1.44 e Å3
Crystal data top
C27H33Cl2FeN7O8V = 2978.46 (18) Å3
Mr = 710.35Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.2747 (4) ŵ = 0.75 mm1
b = 19.2019 (6) ÅT = 210 K
c = 15.1011 (5) Å0.34 × 0.29 × 0.10 mm
β = 91.399 (3)°
Data collection top
KM4_CCD_Sapphire3
diffractometer
9941 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
6795 reflections with I > 2σ(I)
Tmin = 0.903, Tmax = 0.934Rint = 0.020
28574 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0470 restraints
wR(F2) = 0.155H-atom parameters constrained
S = 1.01Δρmax = 1.29 e Å3
9941 reflectionsΔρmin = 1.44 e Å3
409 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.69147 (3)0.071352 (13)0.739572 (17)0.02162 (8)
Cl11.35871 (6)0.31736 (3)0.53957 (4)0.03740 (13)
Cl21.22316 (6)0.14609 (3)0.69809 (5)0.04660 (15)
N10.60480 (18)0.09230 (9)0.62453 (12)0.0314 (4)
N20.82687 (17)0.14257 (8)0.69006 (12)0.0298 (3)
N30.76215 (16)0.05587 (9)0.87007 (11)0.0266 (3)
N40.61399 (16)0.15278 (8)0.79725 (11)0.0271 (3)
N50.55538 (16)0.00616 (9)0.77401 (11)0.0281 (3)
N60.75846 (17)0.01960 (8)0.67738 (11)0.0271 (3)
N70.3571 (2)0.11175 (10)0.72259 (14)0.0422 (5)
O11.3276 (3)0.30839 (15)0.62956 (16)0.0918 (10)
O21.4388 (2)0.26111 (10)0.50998 (15)0.0617 (6)
O31.2393 (2)0.31931 (13)0.48796 (18)0.0776 (7)
O71.1642 (3)0.20587 (12)0.66065 (16)0.0887 (9)
O51.3044 (5)0.1196 (3)0.63862 (19)0.196 (3)
O61.1268 (4)0.09900 (19)0.7227 (3)0.1309 (15)
O41.4221 (2)0.38221 (10)0.52840 (19)0.0755 (7)
O81.2955 (3)0.15927 (16)0.77766 (16)0.0869 (8)
C10.5629 (2)0.05570 (11)0.74413 (15)0.0329 (4)
H110.50220.08990.75960.040*
C20.6691 (2)0.07146 (10)0.68519 (14)0.0311 (4)
C30.6786 (3)0.13558 (12)0.64415 (17)0.0412 (5)
H130.61350.16940.65110.049*
C40.7843 (3)0.14908 (12)0.59326 (17)0.0444 (6)
H140.79220.19180.56340.053*
C50.8774 (3)0.09913 (12)0.58703 (15)0.0399 (5)
H150.95220.10830.55440.048*
C60.8641 (2)0.03394 (11)0.62848 (13)0.0323 (4)
C70.6654 (2)0.13438 (12)0.57438 (14)0.0369 (5)
H170.63210.14570.51760.044*
C80.7870 (2)0.16425 (11)0.60756 (14)0.0343 (4)
C90.8553 (3)0.21061 (12)0.55688 (18)0.0453 (6)
H190.82460.22330.50000.054*
C100.9703 (3)0.23820 (14)0.5916 (2)0.0531 (7)
H1101.01970.26980.55880.064*
C111.0098 (3)0.21807 (13)0.6752 (2)0.0476 (6)
H1111.08690.23670.70030.057*
C120.9375 (2)0.17033 (11)0.72364 (16)0.0350 (4)
C130.6442 (2)0.16178 (11)0.87950 (14)0.0331 (4)
H1130.61770.20180.91000.040*
C140.72022 (19)0.10829 (11)0.92347 (13)0.0305 (4)
C150.7416 (2)0.10998 (13)1.01420 (14)0.0379 (5)
H1150.71350.14821.04750.046*
C160.8042 (2)0.05535 (14)1.05495 (15)0.0411 (5)
H1160.82020.05511.11650.049*
C170.8430 (2)0.00055 (13)1.00253 (14)0.0377 (5)
H1170.88300.03841.02920.045*
C180.82386 (19)0.00188 (11)0.91045 (13)0.0303 (4)
C190.5232 (2)0.20353 (10)0.75727 (16)0.0340 (4)
H1190.54390.21050.69490.041*
H2190.53240.24830.78780.041*
C200.3836 (2)0.17762 (11)0.76401 (17)0.0365 (5)
H1200.36260.17400.82680.044*
H2200.32520.21250.73730.044*
C210.4457 (2)0.02237 (12)0.83113 (15)0.0348 (5)
H1210.47340.05660.87590.042*
H2210.41870.02000.86190.042*
C220.3297 (2)0.05161 (12)0.77688 (18)0.0402 (5)
H1220.29540.01450.73830.048*
H2220.26100.06410.81780.048*
C230.4778 (2)0.06538 (12)0.59222 (16)0.0401 (5)
H1230.47010.01630.60930.048*
H2230.47420.06770.52740.048*
C240.3624 (2)0.10580 (13)0.62860 (16)0.0403 (5)
H1240.36360.15290.60350.048*
H2240.28200.08330.60720.048*
C300.8763 (2)0.05662 (12)0.85685 (16)0.0364 (5)
H1300.80470.08480.83380.055*
H2300.93320.08520.89390.055*
H3300.92490.03790.80800.055*
C310.9708 (2)0.01849 (12)0.62099 (18)0.0428 (6)
H1310.93960.05800.58660.064*
H2311.04420.00250.59180.064*
H3310.99800.03400.67970.064*
C320.9894 (2)0.14836 (13)0.81258 (17)0.0419 (5)
H1320.93570.16790.85830.063*
H2321.07810.16490.82060.063*
H3320.98820.09790.81660.063*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.02410 (14)0.01974 (13)0.02110 (13)0.00033 (9)0.00231 (9)0.00033 (9)
Cl10.0446 (3)0.0315 (2)0.0365 (3)0.0038 (2)0.0107 (2)0.00255 (19)
Cl20.0466 (3)0.0396 (3)0.0533 (4)0.0031 (2)0.0050 (3)0.0058 (3)
N10.0363 (9)0.0290 (8)0.0290 (8)0.0029 (7)0.0017 (7)0.0033 (7)
N20.0315 (9)0.0246 (7)0.0335 (9)0.0035 (6)0.0069 (7)0.0008 (6)
N30.0235 (8)0.0298 (8)0.0266 (8)0.0032 (6)0.0034 (6)0.0001 (6)
N40.0243 (8)0.0242 (7)0.0332 (8)0.0001 (6)0.0056 (6)0.0007 (6)
N50.0228 (8)0.0305 (8)0.0309 (8)0.0023 (6)0.0010 (6)0.0070 (6)
N60.0318 (8)0.0243 (7)0.0253 (8)0.0021 (6)0.0009 (6)0.0029 (6)
N70.0550 (13)0.0315 (9)0.0397 (10)0.0050 (8)0.0069 (9)0.0039 (8)
O10.138 (3)0.0883 (17)0.0513 (13)0.0499 (17)0.0390 (15)0.0256 (12)
O20.0672 (14)0.0431 (10)0.0763 (14)0.0075 (9)0.0338 (11)0.0009 (9)
O30.0619 (15)0.0859 (17)0.0840 (17)0.0006 (12)0.0140 (13)0.0257 (14)
O70.154 (3)0.0517 (13)0.0607 (14)0.0383 (15)0.0048 (15)0.0149 (11)
O50.234 (5)0.320 (6)0.0363 (14)0.181 (5)0.025 (2)0.027 (3)
O60.123 (3)0.123 (3)0.144 (3)0.077 (2)0.055 (2)0.061 (2)
O40.0703 (15)0.0417 (11)0.115 (2)0.0125 (10)0.0163 (14)0.0066 (12)
O80.0902 (19)0.115 (2)0.0548 (14)0.0237 (16)0.0133 (13)0.0146 (14)
C10.0287 (10)0.0314 (10)0.0387 (11)0.0053 (8)0.0009 (8)0.0068 (8)
C20.0343 (10)0.0265 (9)0.0324 (10)0.0033 (8)0.0042 (8)0.0041 (7)
C30.0474 (13)0.0276 (10)0.0483 (13)0.0053 (9)0.0049 (11)0.0035 (9)
C40.0589 (16)0.0313 (11)0.0430 (13)0.0022 (10)0.0017 (11)0.0096 (9)
C50.0506 (14)0.0361 (11)0.0332 (11)0.0061 (10)0.0063 (10)0.0025 (9)
C60.0397 (11)0.0301 (10)0.0272 (9)0.0021 (8)0.0036 (8)0.0031 (7)
C70.0449 (13)0.0375 (11)0.0282 (10)0.0086 (9)0.0016 (9)0.0003 (8)
C80.0421 (12)0.0299 (10)0.0315 (10)0.0060 (9)0.0101 (9)0.0024 (8)
C90.0583 (16)0.0365 (12)0.0419 (13)0.0042 (11)0.0166 (11)0.0079 (10)
C100.0598 (17)0.0388 (13)0.0621 (17)0.0008 (12)0.0270 (14)0.0110 (12)
C110.0398 (13)0.0374 (12)0.0661 (17)0.0049 (10)0.0123 (12)0.0009 (11)
C120.0312 (10)0.0304 (10)0.0438 (12)0.0026 (8)0.0079 (9)0.0029 (8)
C130.0318 (10)0.0329 (10)0.0348 (11)0.0026 (8)0.0072 (8)0.0076 (8)
C140.0253 (9)0.0388 (11)0.0277 (9)0.0049 (8)0.0047 (7)0.0056 (8)
C150.0310 (11)0.0549 (14)0.0282 (10)0.0076 (10)0.0052 (8)0.0083 (9)
C160.0318 (11)0.0670 (15)0.0246 (10)0.0102 (11)0.0033 (8)0.0004 (10)
C170.0267 (10)0.0538 (13)0.0326 (10)0.0048 (9)0.0004 (8)0.0092 (9)
C180.0236 (9)0.0368 (10)0.0304 (9)0.0055 (8)0.0012 (7)0.0047 (8)
C190.0329 (11)0.0233 (9)0.0458 (12)0.0028 (8)0.0044 (9)0.0020 (8)
C200.0309 (11)0.0322 (10)0.0465 (13)0.0034 (8)0.0051 (9)0.0020 (9)
C210.0281 (10)0.0375 (10)0.0393 (11)0.0014 (8)0.0110 (8)0.0101 (9)
C220.0276 (10)0.0349 (11)0.0582 (15)0.0029 (8)0.0036 (10)0.0094 (10)
C230.0436 (13)0.0413 (12)0.0347 (11)0.0006 (10)0.0124 (9)0.0068 (9)
C240.0369 (12)0.0421 (12)0.0412 (12)0.0014 (9)0.0107 (10)0.0029 (9)
C300.0362 (11)0.0347 (10)0.0381 (11)0.0054 (9)0.0046 (9)0.0038 (9)
C310.0421 (13)0.0306 (10)0.0567 (15)0.0004 (9)0.0225 (11)0.0010 (10)
C320.0316 (11)0.0443 (12)0.0495 (14)0.0073 (9)0.0020 (10)0.0012 (10)
Geometric parameters (Å, º) top
Fe1—N51.9566 (16)C9—C101.386 (4)
Fe1—N41.9675 (16)C9—H190.9400
Fe1—N11.9742 (18)C10—C111.372 (4)
Fe1—N22.1013 (18)C10—H1100.9400
Fe1—N32.1046 (17)C11—C121.398 (3)
Fe1—N62.1064 (17)C11—H1110.9400
Cl1—O11.414 (2)C12—C321.494 (3)
Cl1—O41.417 (2)C13—C141.442 (3)
Cl1—O21.4355 (19)C13—H1130.9400
Cl1—O31.438 (3)C14—C151.383 (3)
Cl2—O51.342 (3)C15—C161.369 (4)
Cl2—O61.398 (3)C15—H1150.9400
Cl2—O71.410 (2)C16—C171.381 (3)
Cl2—O81.420 (3)C16—H1160.9400
N1—C71.279 (3)C17—C181.400 (3)
N1—C231.476 (3)C17—H1170.9400
N2—C121.344 (3)C18—C301.493 (3)
N2—C81.367 (3)C19—C201.524 (3)
N3—C181.353 (3)C19—H1190.9800
N3—C141.366 (3)C19—H2190.9800
N4—C131.285 (3)C20—H1200.9800
N4—C191.469 (3)C20—H2200.9800
N5—C11.274 (3)C21—C221.535 (3)
N5—C211.469 (3)C21—H1210.9800
N6—C61.356 (3)C21—H2210.9800
N6—C21.362 (3)C22—H1220.9800
N7—C241.426 (3)C22—H2220.9800
N7—C201.434 (3)C23—C241.530 (3)
N7—C221.448 (3)C23—H1230.9800
C1—C21.456 (3)C23—H2230.9800
C1—H110.9400C24—H1240.9800
C2—C31.383 (3)C24—H2240.9800
C3—C41.371 (4)C30—H1300.9700
C3—H130.9400C30—H2300.9700
C4—C51.360 (4)C30—H3300.9700
C4—H140.9400C31—H1310.9700
C5—C61.408 (3)C31—H2310.9700
C5—H150.9400C31—H3310.9700
C6—C311.495 (3)C32—H1320.9700
C7—C81.453 (3)C32—H2320.9700
C7—H170.9400C32—H3320.9700
C8—C91.377 (3)
N5—Fe1—N495.23 (7)C10—C11—C12121.1 (3)
N5—Fe1—N193.11 (7)C10—C11—H111119.4
N4—Fe1—N192.81 (7)C12—C11—H111119.4
N5—Fe1—N2174.05 (7)N2—C12—C11121.2 (2)
N4—Fe1—N285.35 (7)N2—C12—C32120.5 (2)
N1—Fe1—N280.95 (8)C11—C12—C32118.3 (2)
N5—Fe1—N383.87 (7)N4—C13—C14117.68 (18)
N4—Fe1—N380.32 (7)N4—C13—H113121.2
N1—Fe1—N3172.18 (7)C14—C13—H113121.2
N2—Fe1—N3102.05 (7)N3—C14—C15123.9 (2)
N5—Fe1—N680.30 (7)N3—C14—C13115.34 (18)
N4—Fe1—N6175.12 (7)C15—C14—C13120.70 (19)
N1—Fe1—N685.52 (7)C16—C15—C14119.3 (2)
N2—Fe1—N698.89 (6)C16—C15—H115120.4
N3—Fe1—N6101.03 (6)C14—C15—H115120.4
O1—Cl1—O4109.68 (19)C15—C16—C17117.7 (2)
O1—Cl1—O2110.63 (13)C15—C16—H116121.1
O4—Cl1—O2110.82 (13)C17—C16—H116121.1
O1—Cl1—O3108.29 (19)C16—C17—C18121.3 (2)
O4—Cl1—O3107.53 (16)C16—C17—H117119.3
O2—Cl1—O3109.80 (14)C18—C17—H117119.3
O5—Cl2—O6112.9 (3)N3—C18—C17121.0 (2)
O5—Cl2—O7108.0 (2)N3—C18—C30120.24 (18)
O6—Cl2—O7109.5 (2)C17—C18—C30118.76 (19)
O5—Cl2—O8108.2 (2)N4—C19—C20110.21 (17)
O6—Cl2—O8104.44 (18)N4—C19—H119109.6
O7—Cl2—O8113.90 (18)C20—C19—H119109.6
C7—N1—C23117.68 (19)N4—C19—H219109.6
C7—N1—Fe1115.73 (15)C20—C19—H219109.6
C23—N1—Fe1126.58 (15)H119—C19—H219108.1
C12—N2—C8117.08 (19)N7—C20—C19115.29 (19)
C12—N2—Fe1133.26 (15)N7—C20—H120108.5
C8—N2—Fe1109.64 (14)C19—C20—H120108.5
C18—N3—C14116.72 (17)N7—C20—H220108.5
C18—N3—Fe1132.66 (14)C19—C20—H220108.5
C14—N3—Fe1110.00 (13)H120—C20—H220107.5
C13—N4—C19116.37 (17)N5—C21—C22111.13 (18)
C13—N4—Fe1116.37 (14)N5—C21—H121109.4
C19—N4—Fe1127.24 (14)C22—C21—H121109.4
C1—N5—C21117.37 (18)N5—C21—H221109.4
C1—N5—Fe1116.89 (15)C22—C21—H221109.4
C21—N5—Fe1125.73 (14)H121—C21—H221108.0
C6—N6—C2116.68 (18)N7—C22—C21115.76 (19)
C6—N6—Fe1133.30 (14)N7—C22—H122108.3
C2—N6—Fe1109.84 (13)C21—C22—H122108.3
C24—N7—C20119.56 (19)N7—C22—H222108.3
C24—N7—C22120.8 (2)C21—C22—H222108.3
C20—N7—C22119.6 (2)H122—C22—H222107.4
N5—C1—C2117.61 (18)N1—C23—C24112.97 (18)
N5—C1—H11121.2N1—C23—H123109.0
C2—C1—H11121.2C24—C23—H123109.0
N6—C2—C3123.9 (2)N1—C23—H223109.0
N6—C2—C1114.68 (18)C24—C23—H223109.0
C3—C2—C1121.4 (2)H123—C23—H223107.8
C4—C3—C2119.0 (2)N7—C24—C23116.53 (19)
C4—C3—H13120.5N7—C24—H124108.2
C2—C3—H13120.5C23—C24—H124108.2
C5—C4—C3118.3 (2)N7—C24—H224108.2
C5—C4—H14120.9C23—C24—H224108.2
C3—C4—H14120.9H124—C24—H224107.3
C4—C5—C6121.4 (2)C18—C30—H130109.5
C4—C5—H15119.3C18—C30—H230109.5
C6—C5—H15119.3H130—C30—H230109.5
N6—C6—C5120.7 (2)C18—C30—H330109.5
N6—C6—C31120.19 (19)H130—C30—H330109.5
C5—C6—C31119.1 (2)H230—C30—H330109.5
N1—C7—C8118.1 (2)C6—C31—H131109.5
N1—C7—H17120.9C6—C31—H231109.5
C8—C7—H17120.9H131—C31—H231109.5
N2—C8—C9123.9 (2)C6—C31—H331109.5
N2—C8—C7115.49 (19)H131—C31—H331109.5
C9—C8—C7120.6 (2)H231—C31—H331109.5
C8—C9—C10118.6 (3)C12—C32—H132109.5
C8—C9—H19120.7C12—C32—H232109.5
C10—C9—H19120.7H132—C32—H232109.5
C11—C10—C9118.1 (2)C12—C32—H332109.5
C11—C10—H110120.9H132—C32—H332109.5
C9—C10—H110120.9H232—C32—H332109.5
(1_230) top
Crystal data top
C27H33Cl2FeN7O8Z = 4
Mr = 710.35F(000) = 1472
Monoclinic, P21/cDx = 1.562 Mg m3
a = 10.3663 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 19.2603 (6) ŵ = 0.74 mm1
c = 15.1373 (5) ÅT = 230 K
β = 91.432 (3)°Polyhedron, dark red
V = 3021.34 (18) Å30.34 × 0.29 × 0.10 mm
Data collection top
KM4_CCD_Sapphire3
diffractometer
10014 independent reflections
Radiation source: fine-focus sealed tube6362 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
Detector resolution: 16.0328 pixels mm-1θmax = 32.8°, θmin = 2.9°
θ–scanh = 1515
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 2821
Tmin = 0.892, Tmax = 0.925l = 2221
28711 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.149H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.0945P)2]
where P = (Fo2 + 2Fc2)/3
10014 reflections(Δ/σ)max = 0.001
409 parametersΔρmax = 1.03 e Å3
0 restraintsΔρmin = 1.16 e Å3
Crystal data top
C27H33Cl2FeN7O8V = 3021.34 (18) Å3
Mr = 710.35Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.3663 (4) ŵ = 0.74 mm1
b = 19.2603 (6) ÅT = 230 K
c = 15.1373 (5) Å0.34 × 0.29 × 0.10 mm
β = 91.432 (3)°
Data collection top
KM4_CCD_Sapphire3
diffractometer
10014 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
6362 reflections with I > 2σ(I)
Tmin = 0.892, Tmax = 0.925Rint = 0.020
28711 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0470 restraints
wR(F2) = 0.149H-atom parameters constrained
S = 1.00Δρmax = 1.03 e Å3
10014 reflectionsΔρmin = 1.16 e Å3
409 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.69498 (3)0.071374 (13)0.740110 (17)0.02622 (8)
Cl11.35954 (6)0.31774 (3)0.53925 (4)0.04402 (14)
Cl21.22325 (7)0.14610 (3)0.69698 (5)0.05437 (17)
N10.6118 (2)0.09533 (10)0.62168 (13)0.0430 (4)
N20.83295 (19)0.14510 (9)0.69083 (12)0.0390 (4)
N30.76378 (16)0.05498 (9)0.87417 (11)0.0329 (4)
N40.61594 (16)0.15324 (9)0.80204 (12)0.0353 (4)
N50.55747 (17)0.00281 (10)0.77127 (12)0.0386 (4)
N60.76346 (18)0.02199 (9)0.67616 (11)0.0363 (4)
N70.3740 (3)0.11039 (11)0.71979 (15)0.0600 (6)
O11.3273 (3)0.30759 (14)0.62829 (15)0.0970 (9)
O21.4383 (2)0.26197 (10)0.50892 (15)0.0728 (6)
O31.2410 (3)0.31970 (13)0.48832 (18)0.0863 (7)
O71.1660 (3)0.20551 (12)0.65812 (17)0.0984 (9)
O51.2991 (5)0.1172 (3)0.6381 (2)0.197 (3)
O61.1275 (3)0.10034 (19)0.7243 (2)0.1346 (14)
O41.4222 (2)0.38255 (11)0.5289 (2)0.0865 (7)
O81.2964 (3)0.16076 (17)0.77537 (17)0.1014 (9)
C10.5676 (2)0.05784 (12)0.74110 (17)0.0445 (5)
H110.50730.09230.75530.053*
C20.6749 (2)0.07356 (11)0.68346 (15)0.0410 (5)
C30.6852 (3)0.13743 (13)0.64240 (19)0.0539 (6)
H130.62080.17130.64880.065*
C40.7910 (3)0.15043 (13)0.59222 (19)0.0569 (7)
H140.79970.19300.56260.068*
C50.8821 (3)0.10080 (13)0.58630 (16)0.0512 (6)
H150.95630.10970.55370.061*
C60.8684 (2)0.03602 (11)0.62791 (14)0.0407 (5)
C70.6735 (3)0.13791 (13)0.57422 (15)0.0478 (6)
H170.64160.15030.51770.057*
C80.7939 (3)0.16710 (12)0.60861 (15)0.0440 (5)
C90.8632 (3)0.21329 (14)0.55939 (19)0.0576 (7)
H190.83390.22620.50250.069*
C100.9764 (3)0.24051 (15)0.5947 (2)0.0668 (8)
H1101.02580.27220.56250.080*
C111.0150 (3)0.21982 (14)0.6789 (2)0.0610 (7)
H1111.09100.23810.70480.073*
C120.9424 (2)0.17235 (12)0.72531 (17)0.0440 (5)
C130.6461 (2)0.16056 (12)0.88344 (15)0.0405 (5)
H1130.61980.20010.91450.049*
C140.7213 (2)0.10712 (12)0.92732 (14)0.0380 (5)
C150.7420 (2)0.10823 (14)1.01797 (15)0.0477 (6)
H1150.71330.14601.05160.057*
C160.8044 (2)0.05392 (16)1.05778 (16)0.0513 (6)
H1160.82050.05371.11920.062*
C170.8435 (2)0.00052 (15)1.00606 (15)0.0467 (6)
H1170.88310.03941.03270.056*
C180.8249 (2)0.00126 (12)0.91451 (14)0.0377 (4)
C190.5255 (2)0.20399 (11)0.76260 (18)0.0449 (5)
H1190.54860.21330.70140.054*
H2190.53070.24770.79560.054*
C200.3890 (2)0.17556 (12)0.76489 (18)0.0462 (5)
H1200.36490.16960.82660.055*
H2200.32980.20950.73770.055*
C210.4462 (2)0.01823 (14)0.82634 (17)0.0517 (6)
H1210.47210.05090.87320.062*
H2210.41640.02460.85430.062*
C220.3362 (2)0.04968 (14)0.7701 (2)0.0563 (7)
H1220.30300.01430.72900.068*
H2220.26590.06270.80890.068*
C230.4863 (3)0.06961 (14)0.58731 (19)0.0573 (7)
H1230.47850.02010.60100.069*
H2230.48270.07470.52290.069*
C240.3735 (3)0.10859 (14)0.62660 (18)0.0540 (6)
H1240.37400.15640.60450.065*
H2240.29290.08690.60550.065*
C300.8766 (2)0.05660 (12)0.85977 (16)0.0436 (5)
H1300.80590.08590.83920.065*
H2300.93700.08400.89520.065*
H3300.92040.03750.80940.065*
C310.9728 (3)0.01721 (12)0.62131 (19)0.0519 (6)
H1310.94110.05640.58690.078*
H2311.04650.00310.59260.078*
H3310.99850.03280.68010.078*
C320.9908 (2)0.14948 (14)0.81429 (18)0.0509 (6)
H1320.93290.16600.85900.076*
H2321.07640.16840.82560.076*
H3320.99470.09920.81610.076*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.03025 (15)0.02314 (13)0.02533 (13)0.00086 (10)0.00197 (10)0.00038 (9)
Cl10.0518 (3)0.0369 (3)0.0440 (3)0.0043 (2)0.0124 (2)0.0026 (2)
Cl20.0562 (4)0.0461 (3)0.0606 (4)0.0038 (3)0.0042 (3)0.0068 (3)
N10.0472 (11)0.0396 (10)0.0420 (10)0.0076 (8)0.0077 (8)0.0091 (8)
N20.0435 (10)0.0324 (9)0.0414 (10)0.0088 (7)0.0052 (8)0.0025 (7)
N30.0287 (8)0.0363 (8)0.0342 (9)0.0049 (6)0.0063 (7)0.0019 (7)
N40.0301 (9)0.0294 (8)0.0467 (10)0.0003 (6)0.0071 (7)0.0013 (7)
N50.0287 (9)0.0456 (10)0.0415 (10)0.0024 (7)0.0012 (7)0.0164 (8)
N60.0419 (10)0.0326 (8)0.0342 (9)0.0067 (7)0.0044 (7)0.0079 (7)
N70.0922 (18)0.0366 (10)0.0505 (13)0.0124 (11)0.0140 (12)0.0056 (9)
O10.138 (2)0.0970 (18)0.0583 (14)0.0456 (17)0.0376 (14)0.0250 (12)
O20.0812 (15)0.0495 (11)0.0896 (16)0.0076 (10)0.0411 (12)0.0010 (10)
O30.0748 (16)0.0918 (18)0.0917 (18)0.0023 (13)0.0139 (13)0.0233 (14)
O70.166 (3)0.0569 (13)0.0725 (15)0.0316 (15)0.0008 (16)0.0169 (11)
O50.258 (5)0.288 (6)0.0450 (15)0.155 (5)0.033 (2)0.031 (2)
O60.130 (3)0.134 (3)0.137 (3)0.077 (2)0.046 (2)0.060 (2)
O40.0769 (16)0.0488 (12)0.135 (2)0.0155 (11)0.0175 (15)0.0052 (13)
O80.105 (2)0.133 (2)0.0654 (15)0.0349 (18)0.0192 (14)0.0187 (15)
C10.0350 (11)0.0437 (12)0.0542 (14)0.0098 (9)0.0064 (10)0.0167 (10)
C20.0436 (12)0.0359 (10)0.0430 (12)0.0089 (9)0.0104 (9)0.0094 (9)
C30.0630 (17)0.0362 (12)0.0617 (16)0.0128 (11)0.0122 (13)0.0002 (11)
C40.0766 (19)0.0393 (12)0.0544 (15)0.0026 (12)0.0064 (14)0.0085 (11)
C50.0675 (17)0.0453 (13)0.0408 (13)0.0020 (12)0.0025 (11)0.0006 (10)
C60.0501 (13)0.0382 (11)0.0339 (11)0.0016 (9)0.0021 (9)0.0055 (8)
C70.0602 (16)0.0496 (13)0.0334 (11)0.0157 (11)0.0021 (10)0.0036 (10)
C80.0564 (14)0.0370 (11)0.0390 (11)0.0129 (10)0.0114 (10)0.0014 (9)
C90.077 (2)0.0465 (13)0.0505 (15)0.0124 (13)0.0195 (14)0.0080 (11)
C100.078 (2)0.0492 (15)0.075 (2)0.0044 (14)0.0338 (17)0.0109 (14)
C110.0545 (16)0.0486 (14)0.081 (2)0.0025 (12)0.0173 (14)0.0018 (14)
C120.0422 (12)0.0366 (11)0.0537 (14)0.0054 (9)0.0083 (10)0.0072 (9)
C130.0370 (11)0.0391 (11)0.0461 (12)0.0029 (9)0.0119 (9)0.0126 (9)
C140.0306 (10)0.0477 (12)0.0361 (11)0.0066 (9)0.0079 (8)0.0096 (9)
C150.0356 (12)0.0700 (17)0.0379 (12)0.0110 (11)0.0094 (9)0.0137 (11)
C160.0366 (12)0.0853 (19)0.0321 (11)0.0135 (12)0.0052 (9)0.0002 (11)
C170.0333 (12)0.0672 (16)0.0396 (12)0.0078 (11)0.0005 (9)0.0088 (11)
C180.0282 (10)0.0463 (12)0.0385 (11)0.0070 (8)0.0008 (8)0.0044 (9)
C190.0405 (12)0.0276 (10)0.0667 (15)0.0030 (9)0.0035 (11)0.0008 (10)
C200.0385 (12)0.0420 (12)0.0585 (15)0.0051 (9)0.0074 (10)0.0006 (10)
C210.0348 (12)0.0609 (15)0.0602 (15)0.0045 (11)0.0163 (11)0.0255 (12)
C220.0350 (12)0.0422 (12)0.091 (2)0.0053 (10)0.0036 (13)0.0197 (13)
C230.0568 (16)0.0590 (16)0.0548 (15)0.0061 (12)0.0224 (12)0.0194 (12)
C240.0514 (15)0.0550 (15)0.0548 (15)0.0090 (12)0.0175 (12)0.0029 (12)
C300.0433 (12)0.0408 (11)0.0465 (13)0.0041 (9)0.0064 (10)0.0059 (9)
C310.0513 (15)0.0373 (11)0.0682 (17)0.0004 (10)0.0256 (12)0.0008 (11)
C320.0406 (13)0.0533 (14)0.0585 (15)0.0069 (11)0.0041 (11)0.0001 (12)
Geometric parameters (Å, º) top
Fe1—N52.0080 (18)C9—C101.380 (5)
Fe1—N42.0186 (17)C9—H190.9400
Fe1—N12.0233 (19)C10—C111.385 (5)
Fe1—N32.1574 (18)C10—H1100.9400
Fe1—N22.161 (2)C11—C121.386 (4)
Fe1—N62.1700 (19)C11—H1110.9400
Cl1—O11.410 (2)C12—C321.492 (4)
Cl1—O41.418 (2)C13—C141.443 (3)
Cl1—O21.432 (2)C13—H1130.9400
Cl1—O31.435 (3)C14—C151.384 (3)
Cl2—O51.325 (3)C15—C161.363 (4)
Cl2—O61.397 (3)C15—H1150.9400
Cl2—O71.411 (2)C16—C171.376 (4)
Cl2—O81.420 (3)C16—H1160.9400
N1—C71.273 (3)C17—C181.395 (3)
N1—C231.474 (3)C17—H1170.9400
N2—C121.344 (3)C18—C301.496 (3)
N2—C81.366 (3)C19—C201.518 (3)
N3—C181.351 (3)C19—H1190.9800
N3—C141.367 (3)C19—H2190.9800
N4—C131.272 (3)C20—H1200.9800
N4—C191.471 (3)C20—H2200.9800
N5—C11.260 (3)C21—C221.530 (3)
N5—C211.470 (3)C21—H1210.9800
N6—C61.352 (3)C21—H2210.9800
N6—C21.359 (3)C22—H1220.9800
N7—C241.411 (3)C22—H2220.9800
N7—C201.435 (3)C23—C241.523 (4)
N7—C221.454 (3)C23—H1230.9800
C1—C21.462 (4)C23—H2230.9800
C1—H110.9400C24—H1240.9800
C2—C31.384 (3)C24—H2240.9800
C3—C41.373 (4)C30—H1300.9700
C3—H130.9400C30—H2300.9700
C4—C51.348 (4)C30—H3300.9700
C4—H140.9400C31—H1310.9700
C5—C61.406 (3)C31—H2310.9700
C5—H150.9400C31—H3310.9700
C6—C311.496 (3)C32—H1320.9700
C7—C81.454 (4)C32—H2320.9700
C7—H170.9400C32—H3320.9700
C8—C91.375 (4)
N5—Fe1—N496.08 (8)C10—C11—C12120.5 (3)
N5—Fe1—N193.93 (8)C10—C11—H111119.7
N4—Fe1—N193.69 (8)C12—C11—H111119.7
N5—Fe1—N384.42 (7)N2—C12—C11121.7 (3)
N4—Fe1—N378.82 (7)N2—C12—C32119.8 (2)
N1—Fe1—N3172.08 (7)C11—C12—C32118.5 (2)
N5—Fe1—N2173.17 (7)N4—C13—C14118.95 (19)
N4—Fe1—N285.81 (7)N4—C13—H113120.5
N1—Fe1—N279.37 (8)C14—C13—H113120.5
N3—Fe1—N2102.40 (7)N3—C14—C15123.4 (2)
N5—Fe1—N678.57 (7)N3—C14—C13115.57 (19)
N4—Fe1—N6174.60 (7)C15—C14—C13120.9 (2)
N1—Fe1—N686.02 (7)C16—C15—C14119.1 (2)
N3—Fe1—N6101.20 (6)C16—C15—H115120.4
N2—Fe1—N699.42 (7)C14—C15—H115120.4
O1—Cl1—O4110.35 (18)C15—C16—C17118.5 (2)
O1—Cl1—O2110.68 (13)C15—C16—H116120.8
O4—Cl1—O2111.02 (14)C17—C16—H116120.8
O1—Cl1—O3107.27 (18)C16—C17—C18120.8 (2)
O4—Cl1—O3107.83 (16)C16—C17—H117119.6
O2—Cl1—O3109.58 (15)C18—C17—H117119.6
O5—Cl2—O6111.8 (3)N3—C18—C17121.3 (2)
O5—Cl2—O7108.1 (2)N3—C18—C30119.38 (19)
O6—Cl2—O7109.9 (2)C17—C18—C30119.3 (2)
O5—Cl2—O8109.4 (3)N4—C19—C20109.64 (18)
O6—Cl2—O8104.25 (18)N4—C19—H119109.7
O7—Cl2—O8113.41 (19)C20—C19—H119109.7
C7—N1—C23118.0 (2)N4—C19—H219109.7
C7—N1—Fe1115.94 (17)C20—C19—H219109.7
C23—N1—Fe1126.08 (18)H119—C19—H219108.2
C12—N2—C8117.4 (2)N7—C20—C19113.2 (2)
C12—N2—Fe1133.01 (16)N7—C20—H120108.9
C8—N2—Fe1109.55 (16)C19—C20—H120108.9
C18—N3—C14116.82 (19)N7—C20—H220108.9
C18—N3—Fe1132.65 (14)C19—C20—H220108.9
C14—N3—Fe1110.01 (14)H120—C20—H220107.7
C13—N4—C19117.30 (19)N5—C21—C22110.4 (2)
C13—N4—Fe1116.34 (15)N5—C21—H121109.6
C19—N4—Fe1126.35 (16)C22—C21—H121109.6
C1—N5—C21117.8 (2)N5—C21—H221109.6
C1—N5—Fe1117.31 (16)C22—C21—H221109.6
C21—N5—Fe1124.89 (17)H121—C21—H221108.1
C6—N6—C2116.9 (2)N7—C22—C21113.8 (2)
C6—N6—Fe1133.08 (15)N7—C22—H122108.8
C2—N6—Fe1109.88 (15)C21—C22—H122108.8
C24—N7—C20119.6 (2)N7—C22—H222108.8
C24—N7—C22120.6 (2)C21—C22—H222108.8
C20—N7—C22118.8 (2)H122—C22—H222107.7
N5—C1—C2118.7 (2)N1—C23—C24112.1 (2)
N5—C1—H11120.7N1—C23—H123109.2
C2—C1—H11120.7C24—C23—H123109.2
N6—C2—C3123.6 (2)N1—C23—H223109.2
N6—C2—C1115.0 (2)C24—C23—H223109.2
C3—C2—C1121.4 (2)H123—C23—H223107.9
C4—C3—C2118.8 (2)N7—C24—C23114.7 (2)
C4—C3—H13120.6N7—C24—H124108.6
C2—C3—H13120.6C23—C24—H124108.6
C5—C4—C3118.6 (2)N7—C24—H224108.6
C5—C4—H14120.7C23—C24—H224108.6
C3—C4—H14120.7H124—C24—H224107.6
C4—C5—C6121.4 (3)C18—C30—H130109.5
C4—C5—H15119.3C18—C30—H230109.5
C6—C5—H15119.3H130—C30—H230109.5
N6—C6—C5120.7 (2)C18—C30—H330109.5
N6—C6—C31119.5 (2)H130—C30—H330109.5
C5—C6—C31119.8 (2)H230—C30—H330109.5
N1—C7—C8119.1 (2)C6—C31—H131109.5
N1—C7—H17120.4C6—C31—H231109.5
C8—C7—H17120.4H131—C31—H231109.5
N2—C8—C9123.2 (3)C6—C31—H331109.5
N2—C8—C7116.0 (2)H131—C31—H331109.5
C9—C8—C7120.8 (2)H231—C31—H331109.5
C8—C9—C10119.1 (3)C12—C32—H132109.5
C8—C9—H19120.4C12—C32—H232109.5
C10—C9—H19120.4H132—C32—H232109.5
C9—C10—C11118.0 (3)C12—C32—H332109.5
C9—C10—H110121.0H132—C32—H332109.5
C11—C10—H110121.0H232—C32—H332109.5
(1_250) top
Crystal data top
C27H33Cl2FeN7O8Z = 4
Mr = 710.35F(000) = 1472
Monoclinic, P21/cDx = 1.538 Mg m3
a = 10.4678 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 19.3228 (7) ŵ = 0.73 mm1
c = 15.1695 (6) ÅT = 250 K
β = 91.501 (3)°Polyhedron, dark red
V = 3067.2 (2) Å30.34 × 0.29 × 0.10 mm
Data collection top
KM4_CCD_Sapphire3
diffractometer
10160 independent reflections
Radiation source: fine-focus sealed tube5998 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
Detector resolution: 16.0328 pixels mm-1θmax = 32.8°, θmin = 2.9°
θ–scanh = 1515
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 2921
Tmin = 0.914, Tmax = 0.929l = 2221
29034 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.134H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.0765P)2]
where P = (Fo2 + 2Fc2)/3
10160 reflections(Δ/σ)max = 0.001
409 parametersΔρmax = 0.89 e Å3
0 restraintsΔρmin = 0.90 e Å3
Crystal data top
C27H33Cl2FeN7O8V = 3067.2 (2) Å3
Mr = 710.35Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.4678 (4) ŵ = 0.73 mm1
b = 19.3228 (7) ÅT = 250 K
c = 15.1695 (6) Å0.34 × 0.29 × 0.10 mm
β = 91.501 (3)°
Data collection top
KM4_CCD_Sapphire3
diffractometer
10160 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
5998 reflections with I > 2σ(I)
Tmin = 0.914, Tmax = 0.929Rint = 0.021
29034 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0440 restraints
wR(F2) = 0.134H-atom parameters constrained
S = 1.00Δρmax = 0.89 e Å3
10160 reflectionsΔρmin = 0.90 e Å3
409 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.69829 (2)0.071078 (12)0.740454 (16)0.03019 (8)
Cl11.36036 (6)0.31807 (3)0.53915 (4)0.05008 (14)
Cl21.22314 (6)0.14686 (3)0.69602 (4)0.06039 (17)
N10.61993 (19)0.09890 (10)0.61725 (12)0.0489 (4)
N20.83994 (17)0.14758 (8)0.69099 (11)0.0420 (4)
N30.76553 (15)0.05365 (9)0.87879 (11)0.0371 (4)
N40.61835 (16)0.15358 (8)0.80709 (12)0.0411 (4)
N50.55955 (16)0.00168 (10)0.76775 (12)0.0437 (4)
N60.76904 (17)0.02502 (8)0.67378 (11)0.0400 (4)
N70.3922 (2)0.10823 (10)0.71719 (14)0.0622 (6)
O11.3281 (3)0.30701 (13)0.62795 (14)0.1015 (8)
O21.4376 (2)0.26289 (10)0.50812 (15)0.0833 (7)
O31.2428 (2)0.32001 (12)0.48877 (16)0.0925 (7)
O71.1681 (3)0.20558 (11)0.65602 (16)0.1040 (8)
O51.2979 (5)0.1175 (2)0.63783 (19)0.202 (2)
O61.1290 (3)0.10167 (17)0.7250 (2)0.1373 (12)
O41.4216 (2)0.38287 (10)0.52978 (18)0.0934 (7)
O81.2964 (3)0.16264 (16)0.77347 (16)0.1134 (9)
C10.5732 (2)0.06154 (11)0.73677 (16)0.0504 (5)
H110.51400.09650.74960.060*
C20.6812 (2)0.07661 (10)0.68084 (15)0.0451 (5)
C30.6929 (3)0.14004 (12)0.63980 (19)0.0603 (6)
H130.62940.17400.64550.072*
C40.7987 (3)0.15260 (13)0.59059 (18)0.0651 (7)
H140.80840.19510.56140.078*
C50.8884 (3)0.10268 (12)0.58493 (16)0.0560 (6)
H150.96220.11100.55260.067*
C60.8730 (2)0.03875 (11)0.62658 (13)0.0445 (5)
C70.6831 (3)0.14199 (12)0.57293 (14)0.0530 (6)
H170.65300.15580.51670.064*
C80.8024 (2)0.17013 (11)0.60930 (14)0.0481 (5)
C90.8724 (3)0.21651 (13)0.56138 (18)0.0656 (7)
H190.84450.22990.50450.079*
C100.9843 (3)0.24309 (14)0.5981 (2)0.0737 (8)
H1101.03370.27500.56700.088*
C111.0214 (3)0.22152 (13)0.6815 (2)0.0669 (7)
H1111.09710.23890.70780.080*
C120.9479 (2)0.17430 (11)0.72678 (16)0.0489 (5)
C130.6480 (2)0.15897 (11)0.88822 (15)0.0471 (5)
H1130.62140.19780.92030.057*
C140.72269 (19)0.10561 (11)0.93131 (13)0.0436 (5)
C150.7427 (2)0.10627 (14)1.02213 (15)0.0560 (6)
H1150.71400.14361.05610.067*
C160.8050 (2)0.05180 (16)1.06122 (15)0.0603 (7)
H1160.82070.05121.12250.072*
C170.8441 (2)0.00174 (14)1.00967 (15)0.0538 (6)
H1170.88350.04051.03610.065*
C180.82615 (19)0.00041 (11)0.91858 (13)0.0422 (5)
C190.5278 (2)0.20385 (10)0.76894 (18)0.0521 (6)
H1190.55280.21600.70910.062*
H2190.52850.24610.80460.062*
C200.3952 (2)0.17269 (12)0.76642 (18)0.0541 (6)
H1200.36810.16410.82680.065*
H2200.33500.20560.73890.065*
C210.4462 (2)0.01261 (14)0.81960 (18)0.0598 (7)
H1210.46920.04310.86910.072*
H2210.41290.03070.84350.072*
C220.3441 (2)0.04713 (13)0.7611 (2)0.0662 (7)
H1220.31310.01390.71660.079*
H2220.27170.06020.79720.079*
C230.4955 (3)0.07487 (14)0.58063 (18)0.0662 (7)
H1230.48770.02490.58990.079*
H2230.49140.08360.51700.079*
C240.3855 (3)0.11161 (14)0.62390 (18)0.0636 (7)
H1240.38520.16030.60570.076*
H2240.30490.09080.60290.076*
C300.8760 (2)0.05699 (11)0.86279 (16)0.0499 (5)
H1300.80510.08450.83990.075*
H2300.93270.08610.89820.075*
H3300.92250.03760.81410.075*
C310.9747 (2)0.01544 (12)0.62110 (18)0.0582 (6)
H1310.94380.05340.58450.087*
H2311.05030.00450.59550.087*
H3310.99600.03250.67980.087*
C320.9929 (2)0.15047 (13)0.81536 (17)0.0577 (6)
H1320.93260.16510.85920.087*
H2321.07610.17040.82910.087*
H3320.99920.10040.81560.087*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.03466 (15)0.02659 (12)0.02938 (13)0.00129 (10)0.00209 (10)0.00048 (10)
Cl10.0572 (3)0.0406 (3)0.0532 (3)0.0049 (2)0.0148 (2)0.0020 (2)
Cl20.0643 (4)0.0516 (3)0.0649 (4)0.0024 (3)0.0037 (3)0.0078 (3)
N10.0549 (11)0.0448 (10)0.0465 (10)0.0096 (9)0.0104 (9)0.0092 (8)
N20.0477 (10)0.0335 (8)0.0453 (9)0.0075 (7)0.0070 (8)0.0025 (7)
N30.0325 (8)0.0424 (8)0.0368 (8)0.0069 (7)0.0069 (7)0.0019 (7)
N40.0353 (9)0.0337 (8)0.0547 (11)0.0004 (7)0.0075 (7)0.0030 (7)
N50.0312 (8)0.0514 (10)0.0486 (10)0.0022 (7)0.0013 (7)0.0183 (8)
N60.0465 (10)0.0352 (8)0.0380 (9)0.0063 (7)0.0057 (7)0.0072 (7)
N70.0835 (16)0.0423 (10)0.0603 (13)0.0106 (10)0.0103 (11)0.0073 (9)
O10.140 (2)0.1003 (16)0.0660 (13)0.0443 (15)0.0380 (14)0.0243 (12)
O20.0932 (15)0.0544 (11)0.1048 (16)0.0095 (10)0.0497 (13)0.0040 (10)
O30.0825 (15)0.0957 (17)0.0984 (17)0.0077 (12)0.0141 (13)0.0197 (13)
O70.164 (3)0.0642 (13)0.0837 (15)0.0315 (14)0.0053 (15)0.0203 (11)
O50.288 (5)0.264 (5)0.0569 (16)0.157 (4)0.048 (2)0.038 (2)
O60.135 (3)0.143 (2)0.131 (2)0.077 (2)0.0395 (19)0.055 (2)
O40.0836 (15)0.0538 (11)0.144 (2)0.0174 (11)0.0178 (14)0.0014 (12)
O80.117 (2)0.144 (2)0.0778 (16)0.0430 (17)0.0278 (14)0.0222 (15)
C10.0407 (12)0.0442 (12)0.0658 (14)0.0121 (9)0.0084 (10)0.0173 (10)
C20.0486 (12)0.0378 (10)0.0483 (11)0.0077 (9)0.0117 (9)0.0080 (9)
C30.0688 (17)0.0383 (11)0.0729 (16)0.0138 (11)0.0131 (13)0.0023 (11)
C40.087 (2)0.0451 (13)0.0631 (16)0.0009 (13)0.0070 (14)0.0122 (11)
C50.0758 (17)0.0456 (12)0.0467 (13)0.0029 (12)0.0027 (12)0.0007 (10)
C60.0545 (13)0.0418 (11)0.0373 (10)0.0002 (9)0.0032 (9)0.0050 (8)
C70.0731 (16)0.0490 (12)0.0369 (11)0.0155 (11)0.0015 (11)0.0001 (9)
C80.0632 (14)0.0388 (10)0.0430 (11)0.0121 (10)0.0136 (10)0.0013 (9)
C90.091 (2)0.0506 (14)0.0564 (15)0.0141 (14)0.0255 (14)0.0087 (11)
C100.085 (2)0.0506 (14)0.087 (2)0.0013 (14)0.0379 (17)0.0085 (14)
C110.0598 (16)0.0516 (14)0.090 (2)0.0049 (12)0.0213 (15)0.0035 (14)
C120.0468 (12)0.0386 (10)0.0617 (14)0.0040 (9)0.0100 (10)0.0070 (10)
C130.0417 (11)0.0474 (12)0.0529 (13)0.0037 (9)0.0139 (10)0.0162 (10)
C140.0351 (10)0.0561 (12)0.0401 (11)0.0088 (9)0.0097 (8)0.0111 (9)
C150.0424 (12)0.0843 (18)0.0418 (12)0.0138 (12)0.0118 (10)0.0161 (12)
C160.0397 (12)0.105 (2)0.0361 (11)0.0146 (13)0.0052 (9)0.0001 (12)
C170.0402 (12)0.0775 (16)0.0436 (12)0.0097 (11)0.0009 (9)0.0113 (11)
C180.0320 (10)0.0535 (12)0.0410 (11)0.0092 (9)0.0002 (8)0.0058 (9)
C190.0484 (13)0.0309 (10)0.0772 (16)0.0060 (9)0.0067 (11)0.0004 (10)
C200.0437 (12)0.0488 (12)0.0701 (16)0.0072 (10)0.0077 (11)0.0015 (11)
C210.0399 (12)0.0629 (14)0.0774 (17)0.0032 (11)0.0191 (11)0.0293 (13)
C220.0362 (12)0.0501 (13)0.112 (2)0.0063 (10)0.0034 (13)0.0229 (14)
C230.0696 (17)0.0670 (16)0.0605 (15)0.0020 (13)0.0268 (13)0.0174 (12)
C240.0619 (16)0.0591 (15)0.0685 (17)0.0091 (12)0.0233 (13)0.0061 (12)
C300.0490 (13)0.0471 (12)0.0531 (13)0.0037 (10)0.0080 (10)0.0088 (10)
C310.0592 (15)0.0422 (12)0.0746 (16)0.0005 (10)0.0284 (12)0.0020 (11)
C320.0459 (13)0.0614 (15)0.0657 (15)0.0083 (11)0.0039 (11)0.0015 (12)
Geometric parameters (Å, º) top
Fe1—N52.0710 (17)C9—C101.382 (4)
Fe1—N42.0755 (17)C9—H190.9400
Fe1—N12.0916 (18)C10—C111.378 (4)
Fe1—N32.2215 (16)C10—H1100.9400
Fe1—N22.2372 (18)C11—C121.387 (4)
Fe1—N62.2491 (18)C11—H1110.9400
Cl1—O11.414 (2)C12—C321.485 (3)
Cl1—O41.4154 (19)C13—C141.440 (3)
Cl1—O21.4255 (19)C13—H1130.9400
Cl1—O31.432 (2)C14—C151.388 (3)
Cl2—O51.323 (3)C15—C161.365 (4)
Cl2—O61.396 (3)C15—H1150.9400
Cl2—O71.403 (2)C16—C171.366 (4)
Cl2—O81.419 (2)C16—H1160.9400
N1—C71.267 (3)C17—C181.390 (3)
N1—C231.478 (3)C17—H1170.9400
N2—C121.344 (3)C18—C301.497 (3)
N2—C81.362 (3)C19—C201.513 (3)
N3—C181.344 (3)C19—H1190.9800
N3—C141.365 (3)C19—H2190.9800
N4—C131.266 (3)C20—H1200.9800
N4—C191.466 (3)C20—H2200.9800
N5—C11.258 (3)C21—C221.525 (3)
N5—C211.467 (3)C21—H1210.9800
N6—C61.345 (3)C21—H2210.9800
N6—C21.362 (3)C22—H1220.9800
N7—C241.417 (3)C22—H2220.9800
N7—C201.452 (3)C23—C241.516 (4)
N7—C221.452 (3)C23—H1230.9800
C1—C21.461 (3)C23—H2230.9800
C1—H110.9400C24—H1240.9800
C2—C31.381 (3)C24—H2240.9800
C3—C41.373 (4)C30—H1300.9700
C3—H130.9400C30—H2300.9700
C4—C51.351 (4)C30—H3300.9700
C4—H140.9400C31—H1310.9700
C5—C61.399 (3)C31—H2310.9700
C5—H150.9400C31—H3310.9700
C6—C311.497 (3)C32—H1320.9700
C7—C81.457 (4)C32—H2320.9700
C7—H170.9400C32—H3320.9700
C8—C91.377 (3)
N5—Fe1—N497.49 (7)C10—C11—C12120.5 (3)
N5—Fe1—N195.31 (7)C10—C11—H111119.8
N4—Fe1—N194.82 (7)C12—C11—H111119.8
N5—Fe1—N385.11 (6)N2—C12—C11121.6 (2)
N4—Fe1—N377.19 (7)N2—C12—C32119.3 (2)
N1—Fe1—N3171.97 (6)C11—C12—C32119.0 (2)
N5—Fe1—N2171.91 (7)N4—C13—C14119.92 (19)
N4—Fe1—N286.28 (6)N4—C13—H113120.0
N1—Fe1—N277.19 (7)C14—C13—H113120.0
N3—Fe1—N2102.75 (6)N3—C14—C15122.9 (2)
N5—Fe1—N676.72 (7)N3—C14—C13116.39 (18)
N4—Fe1—N6174.18 (6)C15—C14—C13120.7 (2)
N1—Fe1—N686.35 (6)C16—C15—C14118.8 (2)
N3—Fe1—N6101.52 (6)C16—C15—H115120.6
N2—Fe1—N699.54 (6)C14—C15—H115120.6
O1—Cl1—O4110.46 (17)C15—C16—C17118.8 (2)
O1—Cl1—O2110.69 (13)C15—C16—H116120.6
O4—Cl1—O2111.50 (13)C17—C16—H116120.6
O1—Cl1—O3106.79 (16)C16—C17—C18120.8 (2)
O4—Cl1—O3107.95 (14)C16—C17—H117119.6
O2—Cl1—O3109.28 (14)C18—C17—H117119.6
O5—Cl2—O6112.1 (3)N3—C18—C17121.3 (2)
O5—Cl2—O7107.58 (18)N3—C18—C30118.73 (18)
O6—Cl2—O7110.9 (2)C17—C18—C30120.0 (2)
O5—Cl2—O8109.1 (3)N4—C19—C20109.25 (18)
O6—Cl2—O8104.11 (17)N4—C19—H119109.8
O7—Cl2—O8113.02 (17)C20—C19—H119109.8
C7—N1—C23118.3 (2)N4—C19—H219109.8
C7—N1—Fe1116.43 (16)C20—C19—H219109.8
C23—N1—Fe1125.20 (18)H119—C19—H219108.3
C12—N2—C8117.67 (19)N7—C20—C19111.2 (2)
C12—N2—Fe1132.53 (15)N7—C20—H120109.4
C8—N2—Fe1109.78 (15)C19—C20—H120109.4
C18—N3—C14117.36 (18)N7—C20—H220109.4
C18—N3—Fe1132.43 (14)C19—C20—H220109.4
C14—N3—Fe1109.82 (14)H120—C20—H220108.0
C13—N4—C19117.97 (18)N5—C21—C22109.6 (2)
C13—N4—Fe1116.42 (15)N5—C21—H121109.8
C19—N4—Fe1125.57 (15)C22—C21—H121109.8
C1—N5—C21118.3 (2)N5—C21—H221109.8
C1—N5—Fe1117.55 (15)C22—C21—H221109.8
C21—N5—Fe1124.10 (16)H121—C21—H221108.2
C6—N6—C2117.05 (18)N7—C22—C21112.1 (2)
C6—N6—Fe1133.07 (14)N7—C22—H122109.2
C2—N6—Fe1109.76 (14)C21—C22—H122109.2
C24—N7—C20118.3 (2)N7—C22—H222109.2
C24—N7—C22119.1 (2)C21—C22—H222109.2
C20—N7—C22117.7 (2)H122—C22—H222107.9
N5—C1—C2119.82 (19)N1—C23—C24111.2 (2)
N5—C1—H11120.1N1—C23—H123109.4
C2—C1—H11120.1C24—C23—H123109.4
N6—C2—C3123.1 (2)N1—C23—H223109.4
N6—C2—C1115.72 (19)C24—C23—H223109.4
C3—C2—C1121.2 (2)H123—C23—H223108.0
C4—C3—C2118.9 (2)N7—C24—C23113.1 (2)
C4—C3—H13120.5N7—C24—H124109.0
C2—C3—H13120.5C23—C24—H124109.0
C5—C4—C3118.7 (2)N7—C24—H224109.0
C5—C4—H14120.6C23—C24—H224109.0
C3—C4—H14120.6H124—C24—H224107.8
C4—C5—C6120.9 (2)C18—C30—H130109.5
C4—C5—H15119.6C18—C30—H230109.5
C6—C5—H15119.6H130—C30—H230109.5
N6—C6—C5121.3 (2)C18—C30—H330109.5
N6—C6—C31118.57 (19)H130—C30—H330109.5
C5—C6—C31120.1 (2)H230—C30—H330109.5
N1—C7—C8119.9 (2)C6—C31—H131109.5
N1—C7—H17120.1C6—C31—H231109.5
C8—C7—H17120.1H131—C31—H231109.5
N2—C8—C9122.9 (2)C6—C31—H331109.5
N2—C8—C7116.7 (2)H131—C31—H331109.5
C9—C8—C7120.4 (2)H231—C31—H331109.5
C8—C9—C10119.1 (3)C12—C32—H132109.5
C8—C9—H19120.5C12—C32—H232109.5
C10—C9—H19120.5H132—C32—H232109.5
C11—C10—C9118.2 (3)C12—C32—H332109.5
C11—C10—H110120.9H132—C32—H332109.5
C9—C10—H110120.9H232—C32—H332109.5
(1_270) top
Crystal data top
C27H33Cl2FeN7O8Z = 4
Mr = 710.35F(000) = 1472
Monoclinic, P21/cDx = 1.523 Mg m3
a = 10.5290 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 19.3683 (7) ŵ = 0.72 mm1
c = 15.1933 (6) ÅT = 270 K
β = 91.541 (3)°Polyhedron, dark red
V = 3097.2 (2) Å30.34 × 0.29 × 0.10 mm
Data collection top
KM4_CCD_Sapphire3
diffractometer
10242 independent reflections
Radiation source: fine-focus sealed tube5733 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
Detector resolution: 16.0328 pixels mm-1θmax = 32.9°, θmin = 2.9°
θ–scanh = 1515
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 2921
Tmin = 0.903, Tmax = 0.933l = 2222
29143 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.135H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.0745P)2]
where P = (Fo2 + 2Fc2)/3
10242 reflections(Δ/σ)max = 0.001
409 parametersΔρmax = 0.84 e Å3
0 restraintsΔρmin = 0.82 e Å3
Crystal data top
C27H33Cl2FeN7O8V = 3097.2 (2) Å3
Mr = 710.35Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.5290 (4) ŵ = 0.72 mm1
b = 19.3683 (7) ÅT = 270 K
c = 15.1933 (6) Å0.34 × 0.29 × 0.10 mm
β = 91.541 (3)°
Data collection top
KM4_CCD_Sapphire3
diffractometer
10242 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
5733 reflections with I > 2σ(I)
Tmin = 0.903, Tmax = 0.933Rint = 0.021
29143 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0450 restraints
wR(F2) = 0.135H-atom parameters constrained
S = 1.00Δρmax = 0.84 e Å3
10242 reflectionsΔρmin = 0.82 e Å3
409 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.69950 (3)0.070931 (13)0.740592 (17)0.03341 (9)
Cl11.36079 (6)0.31813 (3)0.53917 (4)0.05571 (16)
Cl21.22320 (7)0.14734 (3)0.69511 (5)0.06625 (18)
N10.62382 (19)0.10042 (9)0.61542 (12)0.0497 (4)
N20.84273 (17)0.14882 (8)0.69133 (12)0.0437 (4)
N30.76614 (15)0.05322 (9)0.88087 (11)0.0402 (4)
N40.61898 (16)0.15360 (8)0.80949 (12)0.0445 (4)
N50.56046 (16)0.00365 (9)0.76629 (12)0.0457 (4)
N60.77067 (17)0.02642 (8)0.67293 (10)0.0409 (4)
N70.3998 (2)0.10755 (10)0.71596 (15)0.0619 (5)
O11.3275 (3)0.30662 (13)0.62753 (15)0.1104 (9)
O21.4372 (2)0.26344 (10)0.50793 (15)0.0921 (7)
O31.2437 (2)0.32010 (13)0.48888 (18)0.1036 (8)
O71.1687 (3)0.20537 (11)0.65464 (16)0.1102 (9)
O51.2958 (5)0.1176 (3)0.6376 (2)0.220 (2)
O61.1305 (3)0.10200 (17)0.7251 (2)0.1472 (13)
O41.4207 (2)0.38282 (10)0.53017 (19)0.1007 (8)
O81.2956 (3)0.16359 (17)0.77201 (17)0.1263 (11)
C10.5755 (2)0.06323 (11)0.73482 (17)0.0521 (6)
H110.51740.09800.74670.062*
C20.6835 (2)0.07781 (10)0.67987 (15)0.0469 (5)
C30.6959 (3)0.14103 (12)0.63885 (19)0.0631 (7)
H130.63370.17480.64420.076*
C40.8018 (3)0.15317 (13)0.58980 (18)0.0687 (7)
H140.81200.19510.56090.082*
C50.8900 (3)0.10338 (12)0.58454 (16)0.0585 (6)
H150.96260.11140.55260.070*
C60.8746 (2)0.03978 (11)0.62603 (14)0.0467 (5)
C70.6874 (3)0.14380 (12)0.57263 (15)0.0554 (6)
H170.65860.15810.51720.067*
C80.8060 (2)0.17158 (11)0.60998 (15)0.0503 (5)
C90.8763 (3)0.21797 (13)0.56257 (18)0.0691 (8)
H190.84920.23160.50640.083*
C100.9882 (3)0.24398 (14)0.6001 (2)0.0782 (9)
H1101.03760.27530.56970.094*
C111.0238 (3)0.22238 (13)0.6826 (2)0.0701 (8)
H1111.09810.23940.70900.084*
C120.9499 (2)0.17508 (11)0.72773 (17)0.0515 (5)
C130.6486 (2)0.15832 (12)0.89051 (16)0.0516 (5)
H1130.62250.19640.92260.062*
C140.7230 (2)0.10466 (12)0.93325 (14)0.0481 (5)
C150.7430 (2)0.10498 (15)1.02363 (15)0.0605 (7)
H1150.71430.14171.05720.073*
C160.8049 (2)0.05112 (17)1.06279 (16)0.0667 (8)
H1160.82030.05061.12330.080*
C170.8442 (2)0.00227 (15)1.01129 (15)0.0587 (6)
H1170.88320.04051.03740.070*
C180.82650 (19)0.00002 (12)0.92034 (13)0.0456 (5)
C190.5283 (2)0.20370 (11)0.77184 (18)0.0565 (6)
H1190.55390.21720.71350.068*
H2190.52640.24470.80840.068*
C200.3981 (2)0.17103 (12)0.76675 (19)0.0595 (6)
H1200.37020.16120.82580.071*
H2200.33820.20310.73960.071*
C210.4462 (2)0.01037 (13)0.81643 (18)0.0610 (6)
H1210.46750.03980.86630.073*
H2210.41190.03260.83850.073*
C220.3476 (2)0.04588 (14)0.7569 (2)0.0705 (8)
H1220.31880.01400.71130.085*
H2220.27490.05860.79110.085*
C230.5000 (3)0.07715 (14)0.57806 (18)0.0689 (7)
H1230.49220.02760.58560.083*
H2230.49580.08710.51550.083*
C240.3916 (3)0.11302 (14)0.62271 (19)0.0677 (7)
H1240.39130.16140.60640.081*
H2240.31190.09300.60180.081*
C300.8757 (2)0.05668 (12)0.86431 (16)0.0548 (6)
H1300.80590.08350.84110.082*
H2300.93110.08580.89910.082*
H3300.92190.03730.81660.082*
C310.9748 (3)0.01464 (12)0.62108 (19)0.0642 (7)
H1310.94360.05240.58570.096*
H2311.04910.00450.59510.096*
H3310.99600.03100.67930.096*
C320.9933 (2)0.15104 (14)0.81607 (18)0.0635 (7)
H1320.93540.16710.85930.095*
H2321.07660.16900.82930.095*
H3320.99590.10150.81680.095*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.03795 (15)0.02948 (13)0.03288 (14)0.00161 (11)0.00248 (10)0.00045 (10)
Cl10.0629 (4)0.0442 (3)0.0609 (3)0.0055 (2)0.0171 (3)0.0012 (2)
Cl20.0704 (4)0.0568 (4)0.0712 (4)0.0010 (3)0.0038 (3)0.0087 (3)
N10.0580 (12)0.0456 (10)0.0451 (10)0.0063 (9)0.0088 (9)0.0051 (8)
N20.0484 (10)0.0344 (8)0.0489 (10)0.0047 (7)0.0092 (8)0.0012 (7)
N30.0364 (9)0.0473 (9)0.0372 (9)0.0080 (7)0.0066 (7)0.0008 (7)
N40.0389 (9)0.0366 (8)0.0582 (11)0.0011 (7)0.0078 (8)0.0040 (8)
N50.0357 (9)0.0500 (10)0.0513 (10)0.0035 (8)0.0009 (7)0.0145 (8)
N60.0485 (10)0.0341 (8)0.0398 (9)0.0036 (7)0.0040 (7)0.0045 (7)
N70.0685 (14)0.0468 (11)0.0698 (14)0.0068 (10)0.0079 (11)0.0096 (10)
O10.146 (2)0.1116 (18)0.0754 (15)0.0468 (17)0.0415 (15)0.0237 (13)
O20.1021 (17)0.0577 (11)0.1193 (18)0.0097 (11)0.0564 (14)0.0053 (11)
O30.0946 (17)0.1055 (18)0.1095 (19)0.0096 (14)0.0178 (14)0.0206 (14)
O70.166 (3)0.0689 (14)0.0950 (17)0.0333 (15)0.0075 (16)0.0213 (12)
O50.326 (6)0.268 (5)0.0685 (18)0.172 (5)0.062 (3)0.047 (2)
O60.148 (3)0.154 (3)0.137 (3)0.083 (2)0.043 (2)0.057 (2)
O40.0904 (16)0.0551 (12)0.158 (2)0.0176 (11)0.0225 (15)0.0011 (13)
O80.130 (2)0.159 (3)0.0877 (18)0.0465 (19)0.0345 (16)0.0254 (17)
C10.0437 (12)0.0426 (12)0.0693 (15)0.0118 (9)0.0076 (11)0.0132 (10)
C20.0513 (12)0.0391 (10)0.0497 (12)0.0054 (9)0.0110 (10)0.0051 (9)
C30.0731 (17)0.0376 (11)0.0778 (17)0.0109 (11)0.0116 (14)0.0058 (11)
C40.091 (2)0.0470 (13)0.0681 (17)0.0020 (13)0.0032 (15)0.0165 (12)
C50.0777 (18)0.0467 (13)0.0513 (14)0.0070 (12)0.0058 (12)0.0041 (10)
C60.0575 (14)0.0411 (11)0.0417 (11)0.0023 (10)0.0052 (10)0.0030 (9)
C70.0764 (17)0.0518 (13)0.0381 (11)0.0128 (12)0.0012 (11)0.0036 (10)
C80.0659 (15)0.0391 (11)0.0466 (12)0.0091 (10)0.0161 (10)0.0035 (9)
C90.097 (2)0.0507 (14)0.0615 (16)0.0105 (14)0.0305 (15)0.0107 (12)
C100.089 (2)0.0529 (15)0.095 (2)0.0066 (15)0.0415 (18)0.0104 (15)
C110.0617 (16)0.0532 (14)0.097 (2)0.0088 (12)0.0244 (15)0.0034 (14)
C120.0462 (12)0.0400 (11)0.0690 (15)0.0018 (9)0.0127 (11)0.0064 (10)
C130.0464 (12)0.0536 (13)0.0555 (14)0.0030 (10)0.0142 (10)0.0175 (10)
C140.0397 (11)0.0620 (14)0.0431 (11)0.0096 (10)0.0105 (9)0.0114 (10)
C150.0456 (13)0.094 (2)0.0430 (12)0.0137 (13)0.0107 (10)0.0159 (13)
C160.0431 (13)0.120 (2)0.0370 (12)0.0158 (14)0.0049 (10)0.0019 (14)
C170.0436 (13)0.0867 (18)0.0458 (12)0.0110 (12)0.0019 (10)0.0145 (12)
C180.0353 (11)0.0579 (13)0.0435 (11)0.0103 (9)0.0003 (8)0.0068 (10)
C190.0541 (14)0.0357 (11)0.0801 (17)0.0082 (10)0.0076 (12)0.0027 (11)
C200.0459 (13)0.0516 (13)0.0811 (18)0.0096 (11)0.0072 (12)0.0020 (12)
C210.0441 (13)0.0597 (14)0.0799 (17)0.0011 (11)0.0189 (12)0.0240 (13)
C220.0405 (13)0.0544 (14)0.116 (2)0.0056 (11)0.0010 (13)0.0214 (15)
C230.0806 (19)0.0657 (16)0.0586 (15)0.0017 (14)0.0296 (14)0.0093 (12)
C240.0617 (16)0.0624 (16)0.0775 (19)0.0042 (13)0.0250 (14)0.0104 (13)
C300.0557 (14)0.0519 (13)0.0563 (14)0.0044 (10)0.0097 (11)0.0092 (10)
C310.0655 (16)0.0456 (13)0.0830 (18)0.0006 (11)0.0318 (13)0.0028 (12)
C320.0512 (14)0.0668 (16)0.0721 (17)0.0109 (12)0.0040 (12)0.0012 (13)
Geometric parameters (Å, º) top
Fe1—N52.1006 (17)C9—C101.390 (4)
Fe1—N42.1038 (17)C9—H190.9300
Fe1—N12.1205 (18)C10—C111.364 (4)
Fe1—N32.2521 (17)C10—H1100.9300
Fe1—N22.2740 (17)C11—C121.394 (3)
Fe1—N62.2836 (17)C11—H1110.9300
Cl1—O41.411 (2)C12—C321.481 (4)
Cl1—O11.414 (2)C13—C141.445 (3)
Cl1—O21.4193 (19)C13—H1130.9300
Cl1—O31.434 (3)C14—C151.384 (3)
Cl2—O51.310 (3)C15—C161.359 (4)
Cl2—O71.397 (2)C15—H1150.9300
Cl2—O61.398 (3)C16—C171.367 (4)
Cl2—O81.413 (2)C16—H1160.9300
N1—C71.265 (3)C17—C181.390 (3)
N1—C231.478 (3)C17—H1170.9300
N2—C121.343 (3)C18—C301.490 (3)
N2—C81.359 (3)C19—C201.509 (3)
N3—C181.344 (3)C19—H1190.9700
N3—C141.361 (3)C19—H2190.9700
N4—C131.265 (3)C20—H1200.9700
N4—C191.467 (3)C20—H2200.9700
N5—C11.261 (3)C21—C221.522 (4)
N5—C211.467 (3)C21—H1210.9700
N6—C61.347 (3)C21—H2210.9700
N6—C21.360 (3)C22—H1220.9700
N7—C241.421 (3)C22—H2220.9700
N7—C201.452 (3)C23—C241.513 (4)
N7—C221.460 (3)C23—H1230.9700
C1—C21.457 (3)C23—H2230.9700
C1—H110.9300C24—H1240.9700
C2—C31.382 (3)C24—H2240.9700
C3—C41.378 (4)C30—H1300.9600
C3—H130.9300C30—H2300.9600
C4—C51.342 (4)C30—H3300.9600
C4—H140.9300C31—H1310.9600
C5—C61.395 (3)C31—H2310.9600
C5—H150.9300C31—H3310.9600
C6—C311.495 (3)C32—H1320.9600
C7—C81.460 (4)C32—H2320.9600
C7—H170.9300C32—H3320.9600
C8—C91.379 (3)
N5—Fe1—N497.97 (7)C10—C11—C12120.7 (3)
N5—Fe1—N196.02 (7)C10—C11—H111119.7
N4—Fe1—N195.43 (7)C12—C11—H111119.7
N5—Fe1—N385.43 (6)N2—C12—C11121.3 (3)
N4—Fe1—N376.38 (7)N2—C12—C32119.3 (2)
N1—Fe1—N3171.80 (6)C11—C12—C32119.4 (2)
N5—Fe1—N2171.49 (7)N4—C13—C14120.13 (19)
N4—Fe1—N286.48 (6)N4—C13—H113119.9
N1—Fe1—N276.27 (7)C14—C13—H113119.9
N3—Fe1—N2102.71 (6)N3—C14—C15122.6 (2)
N5—Fe1—N675.80 (7)N3—C14—C13116.69 (19)
N4—Fe1—N6173.66 (6)C15—C14—C13120.6 (2)
N1—Fe1—N686.48 (6)C16—C15—C14119.3 (2)
N3—Fe1—N6101.69 (6)C16—C15—H115120.3
N2—Fe1—N699.85 (6)C14—C15—H115120.3
O4—Cl1—O1110.78 (18)C15—C16—C17118.6 (2)
O4—Cl1—O2111.79 (13)C15—C16—H116120.7
O1—Cl1—O2110.91 (13)C17—C16—H116120.7
O4—Cl1—O3107.77 (15)C16—C17—C18120.7 (2)
O1—Cl1—O3106.19 (17)C16—C17—H117119.6
O2—Cl1—O3109.19 (15)C18—C17—H117119.6
O5—Cl2—O7107.46 (19)N3—C18—C17121.1 (2)
O5—Cl2—O6111.5 (3)N3—C18—C30118.54 (18)
O7—Cl2—O6111.5 (2)C17—C18—C30120.3 (2)
O5—Cl2—O8109.8 (3)N4—C19—C20108.87 (18)
O7—Cl2—O8113.00 (18)N4—C19—H119109.9
O6—Cl2—O8103.63 (17)C20—C19—H119109.9
C7—N1—C23118.6 (2)N4—C19—H219109.9
C7—N1—Fe1116.63 (16)C20—C19—H219109.9
C23—N1—Fe1124.66 (17)H119—C19—H219108.3
C12—N2—C8117.84 (19)N7—C20—C19111.0 (2)
C12—N2—Fe1132.30 (15)N7—C20—H120109.4
C8—N2—Fe1109.85 (15)C19—C20—H120109.4
C18—N3—C14117.52 (18)N7—C20—H220109.4
C18—N3—Fe1132.11 (14)C19—C20—H220109.4
C14—N3—Fe1109.97 (14)H120—C20—H220108.0
C13—N4—C19118.21 (19)N5—C21—C22109.3 (2)
C13—N4—Fe1116.55 (15)N5—C21—H121109.8
C19—N4—Fe1125.19 (15)C22—C21—H121109.8
C1—N5—C21118.6 (2)N5—C21—H221109.8
C1—N5—Fe1117.63 (15)C22—C21—H221109.8
C21—N5—Fe1123.70 (15)H121—C21—H221108.3
C6—N6—C2117.37 (18)N7—C22—C21111.4 (2)
C6—N6—Fe1132.68 (14)N7—C22—H122109.4
C2—N6—Fe1109.84 (14)C21—C22—H122109.4
C24—N7—C20117.7 (2)N7—C22—H222109.4
C24—N7—C22118.1 (2)C21—C22—H222109.4
C20—N7—C22117.2 (2)H122—C22—H222108.0
N5—C1—C2120.18 (19)N1—C23—C24110.9 (2)
N5—C1—H11119.9N1—C23—H123109.5
C2—C1—H11119.9C24—C23—H123109.5
N6—C2—C3122.8 (2)N1—C23—H223109.5
N6—C2—C1116.20 (19)C24—C23—H223109.5
C3—C2—C1121.0 (2)H123—C23—H223108.1
C4—C3—C2118.8 (2)N7—C24—C23112.7 (2)
C4—C3—H13120.6N7—C24—H124109.0
C2—C3—H13120.6C23—C24—H124109.0
C5—C4—C3118.7 (2)N7—C24—H224109.0
C5—C4—H14120.6C23—C24—H224109.0
C3—C4—H14120.6H124—C24—H224107.8
C4—C5—C6121.2 (2)C18—C30—H130109.5
C4—C5—H15119.4C18—C30—H230109.5
C6—C5—H15119.4H130—C30—H230109.5
N6—C6—C5121.0 (2)C18—C30—H330109.5
N6—C6—C31118.41 (19)H130—C30—H330109.5
C5—C6—C31120.6 (2)H230—C30—H330109.5
N1—C7—C8120.3 (2)C6—C31—H131109.5
N1—C7—H17119.9C6—C31—H231109.5
C8—C7—H17119.9H131—C31—H231109.5
N2—C8—C9122.9 (3)C6—C31—H331109.5
N2—C8—C7116.97 (19)H131—C31—H331109.5
C9—C8—C7120.1 (2)H231—C31—H331109.5
C8—C9—C10118.9 (3)C12—C32—H132109.5
C8—C9—H19120.6C12—C32—H232109.5
C10—C9—H19120.6H132—C32—H232109.5
C11—C10—C9118.3 (3)C12—C32—H332109.5
C11—C10—H110120.8H132—C32—H332109.5
C9—C10—H110120.8H232—C32—H332109.5
(1_290) top
Crystal data top
C27H33Cl2FeN7O8Z = 4
Mr = 710.35F(000) = 1472
Monoclinic, P21/cDx = 1.513 Mg m3
a = 10.5677 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 19.4022 (7) ŵ = 0.72 mm1
c = 15.2137 (6) ÅT = 290 K
β = 91.564 (4)°Polyhedron, dark red
V = 3118.2 (2) Å30.34 × 0.29 × 0.10 mm
Data collection top
KM4_CCD_Sapphire3
diffractometer
10248 independent reflections
Radiation source: fine-focus sealed tube5381 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.022
Detector resolution: 16.0328 pixels mm-1θmax = 32.8°, θmin = 3.1°
θ–scanh = 1515
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 2921
Tmin = 0.909, Tmax = 0.933l = 2222
29041 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.142H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0755P)2]
where P = (Fo2 + 2Fc2)/3
10248 reflections(Δ/σ)max = 0.001
409 parametersΔρmax = 0.82 e Å3
0 restraintsΔρmin = 0.83 e Å3
Crystal data top
C27H33Cl2FeN7O8V = 3118.2 (2) Å3
Mr = 710.35Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.5677 (5) ŵ = 0.72 mm1
b = 19.4022 (7) ÅT = 290 K
c = 15.2137 (6) Å0.34 × 0.29 × 0.10 mm
β = 91.564 (4)°
Data collection top
KM4_CCD_Sapphire3
diffractometer
10248 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
5381 reflections with I > 2σ(I)
Tmin = 0.909, Tmax = 0.933Rint = 0.022
29041 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0470 restraints
wR(F2) = 0.142H-atom parameters constrained
S = 1.01Δρmax = 0.82 e Å3
10248 reflectionsΔρmin = 0.83 e Å3
409 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.69982 (3)0.070940 (13)0.740744 (18)0.03666 (9)
Cl11.36097 (6)0.31814 (3)0.53935 (4)0.06154 (17)
Cl21.22336 (7)0.14742 (4)0.69402 (5)0.0733 (2)
N10.62583 (19)0.10103 (10)0.61486 (12)0.0523 (5)
N20.84387 (17)0.14950 (9)0.69197 (12)0.0459 (4)
N30.76602 (16)0.05300 (9)0.88181 (11)0.0436 (4)
N40.61913 (17)0.15356 (9)0.81064 (13)0.0480 (4)
N50.56104 (17)0.00439 (10)0.76547 (12)0.0474 (4)
N60.77136 (17)0.02689 (8)0.67265 (11)0.0431 (4)
N70.4034 (2)0.10731 (10)0.71545 (16)0.0642 (6)
O11.3263 (3)0.30648 (15)0.62684 (17)0.1254 (10)
O21.4373 (2)0.26394 (11)0.50813 (17)0.1027 (8)
O31.2442 (3)0.32000 (14)0.4890 (2)0.1164 (9)
O71.1685 (3)0.20498 (12)0.65362 (18)0.1192 (10)
O51.2935 (6)0.1176 (3)0.6371 (2)0.239 (3)
O61.1324 (4)0.10214 (19)0.7249 (2)0.1626 (15)
O41.4190 (2)0.38268 (10)0.5301 (2)0.1115 (9)
O81.2946 (3)0.16403 (19)0.77127 (19)0.1402 (12)
C10.5765 (2)0.06351 (12)0.73419 (18)0.0549 (6)
H110.51860.09820.74590.066*
C20.6847 (2)0.07824 (11)0.67961 (16)0.0494 (5)
C30.6969 (3)0.14117 (12)0.6385 (2)0.0674 (7)
H130.63500.17490.64370.081*
C40.8025 (3)0.15319 (14)0.5897 (2)0.0736 (8)
H140.81270.19500.56090.088*
C50.8902 (3)0.10378 (13)0.58436 (17)0.0632 (7)
H150.96260.11180.55250.076*
C60.8746 (2)0.03995 (11)0.62617 (14)0.0498 (5)
C70.6896 (3)0.14450 (13)0.57283 (15)0.0591 (6)
H170.66130.15890.51740.071*
C80.8075 (3)0.17231 (11)0.61064 (16)0.0535 (6)
C90.8777 (3)0.21848 (14)0.5636 (2)0.0732 (8)
H190.85100.23220.50760.088*
C100.9896 (3)0.24429 (15)0.6017 (2)0.0826 (10)
H1101.03910.27560.57150.099*
C111.0248 (3)0.22266 (14)0.6838 (2)0.0748 (8)
H1111.09880.23950.71040.090*
C120.9506 (2)0.17537 (12)0.72830 (18)0.0550 (6)
C130.6484 (2)0.15781 (13)0.89137 (17)0.0565 (6)
H1130.62210.19570.92360.068*
C140.7226 (2)0.10427 (13)0.93428 (15)0.0524 (6)
C150.7423 (2)0.10445 (16)1.02431 (16)0.0660 (7)
H1150.71320.14091.05790.079*
C160.8045 (3)0.05103 (19)1.06338 (17)0.0730 (9)
H1160.82000.05061.12380.088*
C170.8440 (2)0.00225 (16)1.01184 (16)0.0639 (7)
H1170.88300.04031.03790.077*
C180.8264 (2)0.00002 (12)0.92113 (14)0.0492 (5)
C190.5286 (2)0.20351 (12)0.7731 (2)0.0614 (7)
H1190.55490.21770.71520.074*
H2190.52560.24410.81030.074*
C200.3994 (2)0.17020 (13)0.7665 (2)0.0658 (7)
H1200.37060.15990.82510.079*
H2200.33960.20200.73900.079*
C210.4464 (2)0.00958 (14)0.81530 (19)0.0644 (7)
H1210.46710.03880.86540.077*
H2210.41160.03330.83680.077*
C220.3497 (3)0.04549 (15)0.7548 (2)0.0759 (9)
H1220.32210.01400.70860.091*
H2220.27620.05810.78810.091*
C230.5019 (3)0.07814 (15)0.57714 (19)0.0715 (8)
H1230.49390.02860.58400.086*
H2230.49760.08860.51480.086*
C240.3947 (3)0.11359 (15)0.6222 (2)0.0724 (8)
H1240.39460.16210.60660.087*
H2240.31510.09390.60120.087*
C300.8757 (3)0.05631 (13)0.86515 (18)0.0606 (6)
H1300.80600.08190.83980.091*
H2300.92810.08650.90040.091*
H3300.92470.03690.81910.091*
C310.9743 (3)0.01432 (13)0.6215 (2)0.0696 (8)
H1310.94380.05160.58520.104*
H2311.04900.00490.59660.104*
H3310.99410.03120.67950.104*
C320.9930 (3)0.15134 (15)0.81642 (19)0.0696 (7)
H1320.93510.16740.85950.104*
H2321.07600.16910.82990.104*
H3320.99530.10190.81720.104*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.04113 (17)0.03248 (14)0.03646 (15)0.00195 (12)0.00256 (11)0.00062 (11)
Cl10.0688 (4)0.0484 (3)0.0683 (4)0.0062 (3)0.0192 (3)0.0006 (3)
Cl20.0772 (5)0.0620 (4)0.0804 (5)0.0002 (3)0.0048 (4)0.0101 (3)
N10.0623 (13)0.0479 (10)0.0462 (11)0.0034 (9)0.0078 (9)0.0018 (9)
N20.0493 (11)0.0368 (9)0.0521 (11)0.0029 (8)0.0111 (8)0.0001 (8)
N30.0400 (10)0.0511 (10)0.0398 (9)0.0082 (8)0.0066 (7)0.0006 (8)
N40.0431 (10)0.0409 (9)0.0602 (12)0.0002 (8)0.0081 (9)0.0053 (8)
N50.0375 (10)0.0494 (10)0.0554 (11)0.0037 (8)0.0009 (8)0.0128 (8)
N60.0519 (11)0.0355 (8)0.0416 (9)0.0027 (7)0.0023 (8)0.0032 (7)
N70.0654 (14)0.0508 (12)0.0759 (15)0.0067 (10)0.0072 (11)0.0095 (10)
O10.166 (3)0.127 (2)0.0851 (17)0.056 (2)0.0498 (17)0.0286 (15)
O20.1137 (19)0.0639 (13)0.134 (2)0.0125 (12)0.0654 (16)0.0083 (12)
O30.105 (2)0.120 (2)0.123 (2)0.0113 (16)0.0209 (17)0.0253 (16)
O70.176 (3)0.0754 (15)0.1055 (19)0.0365 (17)0.0107 (18)0.0220 (13)
O50.363 (7)0.281 (5)0.077 (2)0.190 (5)0.079 (3)0.057 (3)
O60.167 (3)0.166 (3)0.152 (3)0.090 (3)0.044 (2)0.060 (2)
O40.0986 (18)0.0600 (13)0.177 (3)0.0198 (12)0.0260 (17)0.0017 (15)
O80.145 (3)0.176 (3)0.097 (2)0.047 (2)0.0388 (19)0.0293 (19)
C10.0470 (13)0.0446 (12)0.0726 (16)0.0115 (10)0.0078 (11)0.0118 (11)
C20.0525 (13)0.0411 (11)0.0542 (13)0.0049 (10)0.0096 (10)0.0031 (9)
C30.0784 (19)0.0388 (12)0.0844 (19)0.0093 (12)0.0108 (15)0.0089 (12)
C40.095 (2)0.0486 (14)0.0767 (19)0.0022 (14)0.0025 (17)0.0205 (13)
C50.0834 (19)0.0506 (14)0.0561 (15)0.0103 (13)0.0077 (13)0.0070 (11)
C60.0618 (15)0.0434 (12)0.0444 (12)0.0040 (10)0.0054 (10)0.0020 (9)
C70.0816 (19)0.0543 (14)0.0413 (12)0.0118 (13)0.0009 (12)0.0061 (11)
C80.0683 (16)0.0417 (11)0.0515 (13)0.0063 (11)0.0185 (11)0.0048 (10)
C90.099 (2)0.0548 (15)0.0677 (17)0.0097 (15)0.0321 (16)0.0131 (13)
C100.094 (2)0.0582 (17)0.098 (2)0.0094 (16)0.043 (2)0.0103 (16)
C110.0640 (18)0.0574 (16)0.104 (2)0.0123 (13)0.0260 (16)0.0044 (16)
C120.0489 (13)0.0432 (12)0.0735 (16)0.0010 (10)0.0146 (12)0.0076 (11)
C130.0505 (14)0.0591 (14)0.0606 (15)0.0041 (11)0.0157 (11)0.0201 (12)
C140.0418 (12)0.0693 (15)0.0467 (13)0.0090 (11)0.0106 (10)0.0123 (11)
C150.0509 (15)0.104 (2)0.0435 (13)0.0124 (15)0.0111 (11)0.0174 (14)
C160.0478 (15)0.132 (3)0.0391 (13)0.0158 (16)0.0053 (11)0.0002 (15)
C170.0481 (14)0.095 (2)0.0481 (14)0.0120 (13)0.0022 (11)0.0156 (14)
C180.0383 (12)0.0632 (14)0.0459 (12)0.0114 (10)0.0017 (9)0.0082 (10)
C190.0593 (16)0.0378 (11)0.0874 (19)0.0084 (11)0.0079 (13)0.0037 (12)
C200.0515 (15)0.0555 (14)0.091 (2)0.0105 (12)0.0073 (13)0.0031 (13)
C210.0495 (14)0.0594 (15)0.0852 (19)0.0007 (12)0.0186 (13)0.0225 (13)
C220.0425 (14)0.0601 (16)0.125 (3)0.0047 (12)0.0024 (15)0.0209 (16)
C230.088 (2)0.0669 (17)0.0582 (16)0.0055 (15)0.0300 (15)0.0048 (13)
C240.0650 (18)0.0665 (17)0.084 (2)0.0037 (14)0.0251 (15)0.0130 (15)
C300.0615 (16)0.0570 (14)0.0626 (15)0.0047 (12)0.0121 (12)0.0115 (12)
C310.0721 (18)0.0483 (14)0.090 (2)0.0004 (12)0.0362 (15)0.0033 (13)
C320.0556 (16)0.0740 (18)0.0791 (19)0.0121 (13)0.0044 (14)0.0014 (15)
Geometric parameters (Å, º) top
Fe1—N52.1117 (18)C9—C101.396 (5)
Fe1—N42.1159 (18)C9—H190.9300
Fe1—N12.1303 (19)C10—C111.361 (5)
Fe1—N32.2659 (18)C10—H1100.9300
Fe1—N22.2919 (18)C11—C121.395 (4)
Fe1—N62.3001 (17)C11—H1110.9300
Cl1—O41.403 (2)C12—C321.477 (4)
Cl1—O11.408 (2)C13—C141.446 (4)
Cl1—O21.415 (2)C13—H1130.9300
Cl1—O31.435 (3)C14—C151.380 (3)
Cl2—O51.292 (4)C15—C161.356 (4)
Cl2—O61.393 (3)C15—H1150.9300
Cl2—O71.393 (2)C16—C171.369 (4)
Cl2—O81.416 (3)C16—H1160.9300
N1—C71.264 (3)C17—C181.388 (3)
N1—C231.483 (3)C17—H1170.9300
N2—C121.340 (3)C18—C301.488 (4)
N2—C81.360 (3)C19—C201.512 (4)
N3—C181.342 (3)C19—H1190.9700
N3—C141.363 (3)C19—H2190.9700
N4—C131.261 (3)C20—H1200.9700
N4—C191.466 (3)C20—H2200.9700
N5—C11.254 (3)C21—C221.525 (4)
N5—C211.472 (3)C21—H1210.9700
N6—C61.341 (3)C21—H2210.9700
N6—C21.359 (3)C22—H1220.9700
N7—C241.425 (4)C22—H2220.9700
N7—C201.448 (3)C23—C241.506 (4)
N7—C221.462 (3)C23—H1230.9700
C1—C21.460 (4)C23—H2230.9700
C1—H110.9300C24—H1240.9700
C2—C31.379 (3)C24—H2240.9700
C3—C41.377 (4)C30—H1300.9600
C3—H130.9300C30—H2300.9600
C4—C51.338 (4)C30—H3300.9600
C4—H140.9300C31—H1310.9600
C5—C61.404 (3)C31—H2310.9600
C5—H150.9300C31—H3310.9600
C6—C311.492 (3)C32—H1320.9600
C7—C81.461 (4)C32—H2320.9600
C7—H170.9300C32—H3320.9600
C8—C91.375 (3)
N5—Fe1—N498.25 (7)C10—C11—C12120.4 (3)
N5—Fe1—N196.32 (8)C10—C11—H111119.8
N4—Fe1—N195.81 (8)C12—C11—H111119.8
N5—Fe1—N385.58 (7)N2—C12—C11121.6 (3)
N4—Fe1—N376.03 (7)N2—C12—C32119.2 (2)
N1—Fe1—N3171.82 (7)C11—C12—C32119.2 (3)
N5—Fe1—N2171.37 (7)N4—C13—C14120.6 (2)
N4—Fe1—N286.51 (7)N4—C13—H113119.7
N1—Fe1—N275.96 (7)C14—C13—H113119.7
N3—Fe1—N2102.60 (7)N3—C14—C15122.6 (2)
N5—Fe1—N675.37 (7)N3—C14—C13116.5 (2)
N4—Fe1—N6173.46 (7)C15—C14—C13120.8 (2)
N1—Fe1—N686.46 (7)C16—C15—C14119.4 (3)
N3—Fe1—N6101.72 (6)C16—C15—H115120.3
N2—Fe1—N6100.00 (6)C14—C15—H115120.3
O4—Cl1—O1111.3 (2)C15—C16—C17118.5 (2)
O4—Cl1—O2112.02 (15)C15—C16—H116120.7
O1—Cl1—O2111.28 (15)C17—C16—H116120.7
O4—Cl1—O3107.19 (17)C16—C17—C18120.7 (3)
O1—Cl1—O3105.5 (2)C16—C17—H117119.6
O2—Cl1—O3109.23 (17)C18—C17—H117119.6
O5—Cl2—O6110.9 (3)N3—C18—C17121.1 (2)
O5—Cl2—O7107.6 (2)N3—C18—C30118.49 (19)
O6—Cl2—O7111.8 (2)C17—C18—C30120.4 (2)
O5—Cl2—O8110.9 (3)N4—C19—C20108.8 (2)
O6—Cl2—O8102.72 (19)N4—C19—H119109.9
O7—Cl2—O8112.9 (2)C20—C19—H119109.9
C7—N1—C23118.8 (2)N4—C19—H219109.9
C7—N1—Fe1116.73 (17)C20—C19—H219109.9
C23—N1—Fe1124.35 (17)H119—C19—H219108.3
C12—N2—C8117.9 (2)N7—C20—C19110.9 (2)
C12—N2—Fe1132.42 (16)N7—C20—H120109.5
C8—N2—Fe1109.72 (15)C19—C20—H120109.5
C18—N3—C14117.50 (19)N7—C20—H220109.5
C18—N3—Fe1132.11 (15)C19—C20—H220109.5
C14—N3—Fe1110.02 (15)H120—C20—H220108.1
C13—N4—C19118.4 (2)N5—C21—C22108.7 (2)
C13—N4—Fe1116.57 (16)N5—C21—H121109.9
C19—N4—Fe1124.93 (16)C22—C21—H121109.9
C1—N5—C21118.8 (2)N5—C21—H221109.9
C1—N5—Fe1117.85 (16)C22—C21—H221109.9
C21—N5—Fe1123.35 (16)H121—C21—H221108.3
C6—N6—C2117.54 (19)N7—C22—C21111.1 (2)
C6—N6—Fe1132.52 (14)N7—C22—H122109.4
C2—N6—Fe1109.84 (15)C21—C22—H122109.4
C24—N7—C20117.4 (2)N7—C22—H222109.4
C24—N7—C22117.6 (2)C21—C22—H222109.4
C20—N7—C22117.0 (3)H122—C22—H222108.0
N5—C1—C2120.5 (2)N1—C23—C24110.8 (2)
N5—C1—H11119.8N1—C23—H123109.5
C2—C1—H11119.8C24—C23—H123109.5
N6—C2—C3122.8 (2)N1—C23—H223109.5
N6—C2—C1116.15 (19)C24—C23—H223109.5
C3—C2—C1121.0 (2)H123—C23—H223108.1
C4—C3—C2118.8 (3)N7—C24—C23112.7 (2)
C4—C3—H13120.6N7—C24—H124109.1
C2—C3—H13120.6C23—C24—H124109.1
C5—C4—C3119.0 (2)N7—C24—H224109.1
C5—C4—H14120.5C23—C24—H224109.1
C3—C4—H14120.5H124—C24—H224107.8
C4—C5—C6121.0 (3)C18—C30—H130109.5
C4—C5—H15119.5C18—C30—H230109.5
C6—C5—H15119.5H130—C30—H230109.5
N6—C6—C5120.9 (2)C18—C30—H330109.5
N6—C6—C31118.5 (2)H130—C30—H330109.5
C5—C6—C31120.6 (2)H230—C30—H330109.5
N1—C7—C8120.5 (2)C6—C31—H131109.5
N1—C7—H17119.7C6—C31—H231109.5
C8—C7—H17119.7H131—C31—H231109.5
N2—C8—C9122.8 (3)C6—C31—H331109.5
N2—C8—C7117.1 (2)H131—C31—H331109.5
C9—C8—C7120.1 (3)H231—C31—H331109.5
C8—C9—C10118.8 (3)C12—C32—H132109.5
C8—C9—H19120.6C12—C32—H232109.5
C10—C9—H19120.6H132—C32—H232109.5
C11—C10—C9118.5 (3)C12—C32—H332109.5
C11—C10—H110120.7H132—C32—H332109.5
C9—C10—H110120.7H232—C32—H332109.5
(1_310) top
Crystal data top
C27H33Cl2FeN7O8Z = 4
Mr = 710.35F(000) = 1472
Monoclinic, P21/cDx = 1.504 Mg m3
a = 10.6005 (7) ÅMo Kα radiation, λ = 0.71073 Å
b = 19.4289 (11) ŵ = 0.71 mm1
c = 15.2382 (10) ÅT = 310 K
β = 91.595 (6)°Polyhedron, dark red
V = 3137.2 (3) Å30.48 × 0.32 × 0.12 mm
Data collection top
KM4_CCD_Sapphire3
diffractometer
9909 independent reflections
Radiation source: fine-focus sealed tube4883 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.022
Detector resolution: 16.0328 pixels mm-1θmax = 32.8°, θmin = 2.9°
θ–scanh = 1515
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 2920
Tmin = 0.873, Tmax = 0.920l = 2220
27567 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.049Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.152H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0815P)2]
where P = (Fo2 + 2Fc2)/3
9909 reflections(Δ/σ)max = 0.001
409 parametersΔρmax = 0.87 e Å3
0 restraintsΔρmin = 0.76 e Å3
Crystal data top
C27H33Cl2FeN7O8V = 3137.2 (3) Å3
Mr = 710.35Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.6005 (7) ŵ = 0.71 mm1
b = 19.4289 (11) ÅT = 310 K
c = 15.2382 (10) Å0.48 × 0.32 × 0.12 mm
β = 91.595 (6)°
Data collection top
KM4_CCD_Sapphire3
diffractometer
9909 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
4883 reflections with I > 2σ(I)
Tmin = 0.873, Tmax = 0.920Rint = 0.022
27567 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0490 restraints
wR(F2) = 0.152H-atom parameters constrained
S = 1.01Δρmax = 0.87 e Å3
9909 reflectionsΔρmin = 0.76 e Å3
409 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.69984 (3)0.071036 (15)0.74088 (2)0.04021 (11)
Cl11.36110 (7)0.31812 (3)0.53943 (5)0.0673 (2)
Cl21.22357 (8)0.14727 (4)0.69278 (6)0.0808 (2)
N10.6271 (2)0.10148 (11)0.61448 (14)0.0564 (5)
N20.84428 (19)0.14990 (9)0.69259 (13)0.0491 (5)
N30.76553 (18)0.05296 (10)0.88239 (12)0.0467 (5)
N40.61889 (19)0.15357 (10)0.81119 (14)0.0516 (5)
N50.56116 (18)0.00456 (10)0.76501 (14)0.0503 (5)
N60.77121 (19)0.02714 (9)0.67262 (12)0.0459 (4)
N70.4051 (2)0.10732 (11)0.71511 (17)0.0679 (6)
O11.3249 (4)0.30643 (17)0.6259 (2)0.1396 (13)
O21.4376 (3)0.26426 (12)0.50823 (19)0.1130 (10)
O31.2451 (3)0.31980 (17)0.4888 (2)0.1321 (11)
O71.1690 (4)0.20451 (14)0.6525 (2)0.1279 (11)
O51.2928 (7)0.1181 (3)0.6366 (2)0.260 (3)
O61.1336 (4)0.1022 (2)0.7246 (3)0.1757 (17)
O41.4174 (3)0.38257 (12)0.5295 (2)0.1232 (10)
O81.2935 (3)0.1636 (2)0.7699 (2)0.1545 (15)
C10.5766 (3)0.06363 (13)0.73359 (19)0.0585 (7)
H110.51880.09830.74490.070*
C20.6848 (3)0.07821 (12)0.67949 (17)0.0532 (6)
C30.6967 (3)0.14110 (13)0.6387 (2)0.0714 (8)
H130.63500.17480.64380.086*
C40.8024 (4)0.15296 (15)0.5899 (2)0.0805 (9)
H140.81270.19470.56110.097*
C50.8898 (3)0.10362 (14)0.58455 (19)0.0685 (8)
H150.96190.11160.55260.082*
C60.8745 (3)0.04007 (12)0.62630 (16)0.0532 (6)
C70.6904 (3)0.14493 (14)0.57301 (17)0.0630 (7)
H170.66210.15950.51780.076*
C80.8082 (3)0.17272 (12)0.61109 (17)0.0575 (7)
C90.8782 (4)0.21890 (15)0.5642 (2)0.0787 (9)
H190.85180.23280.50820.094*
C100.9907 (4)0.24457 (17)0.6030 (3)0.0886 (11)
H1101.04030.27590.57330.106*
C111.0250 (3)0.22258 (16)0.6847 (3)0.0808 (9)
H1111.09900.23910.71140.097*
C120.9509 (3)0.17562 (13)0.7289 (2)0.0589 (7)
C130.6478 (3)0.15747 (14)0.89178 (19)0.0612 (7)
H1130.62100.19500.92420.073*
C140.7223 (2)0.10394 (14)0.93436 (16)0.0569 (6)
C150.7412 (3)0.10438 (19)1.02430 (18)0.0710 (8)
H1150.71140.14061.05770.085*
C160.8038 (3)0.0512 (2)1.06333 (19)0.0797 (10)
H1160.81940.05091.12370.096*
C170.8436 (3)0.00192 (18)1.01252 (18)0.0687 (8)
H1170.88280.03981.03870.082*
C180.8260 (2)0.00025 (14)0.92146 (16)0.0539 (6)
C190.5288 (3)0.20321 (13)0.7742 (2)0.0658 (7)
H1190.55530.21790.71670.079*
H2190.52520.24340.81180.079*
C200.4003 (3)0.16998 (15)0.7665 (2)0.0708 (8)
H1200.37080.15940.82470.085*
H2200.34100.20180.73890.085*
C210.4463 (3)0.00938 (15)0.8145 (2)0.0684 (8)
H1210.46660.03840.86470.082*
H2210.41120.03340.83560.082*
C220.3507 (3)0.04552 (16)0.7536 (3)0.0799 (10)
H1220.32380.01430.70710.096*
H2220.27700.05810.78640.096*
C230.5036 (3)0.07866 (16)0.5766 (2)0.0752 (9)
H1230.49560.02920.58320.090*
H2230.49920.08930.51440.090*
C240.3965 (3)0.11393 (16)0.6219 (2)0.0779 (9)
H1240.39650.16240.60660.093*
H2240.31720.09430.60070.093*
C300.8755 (3)0.05570 (14)0.8659 (2)0.0657 (7)
H1300.80650.08270.84260.099*
H2300.93100.08450.90060.099*
H3300.92110.03610.81840.099*
C310.9736 (3)0.01404 (14)0.6217 (2)0.0746 (9)
H1310.94500.05010.58300.112*
H2311.04960.00570.59990.112*
H3310.99010.03260.67930.112*
C320.9925 (3)0.15176 (17)0.8166 (2)0.0749 (8)
H1320.93520.16830.85950.112*
H2321.07570.16910.83000.112*
H3320.99390.10240.81750.112*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.04445 (19)0.03613 (16)0.04014 (18)0.00209 (13)0.00299 (13)0.00053 (13)
Cl10.0746 (5)0.0533 (4)0.0750 (5)0.0070 (3)0.0211 (4)0.0002 (3)
Cl20.0832 (6)0.0677 (5)0.0910 (6)0.0006 (4)0.0062 (5)0.0116 (4)
N10.0681 (14)0.0504 (12)0.0501 (12)0.0021 (11)0.0073 (11)0.0008 (10)
N20.0513 (12)0.0383 (10)0.0582 (12)0.0021 (8)0.0119 (10)0.0004 (9)
N30.0429 (11)0.0561 (11)0.0414 (10)0.0088 (9)0.0055 (8)0.0002 (9)
N40.0474 (11)0.0448 (10)0.0627 (13)0.0004 (9)0.0069 (10)0.0053 (9)
N50.0409 (11)0.0506 (11)0.0595 (12)0.0033 (9)0.0008 (9)0.0126 (9)
N60.0565 (12)0.0370 (9)0.0440 (10)0.0018 (8)0.0014 (9)0.0020 (8)
N70.0650 (15)0.0558 (13)0.0826 (17)0.0055 (11)0.0064 (13)0.0107 (12)
O10.186 (3)0.139 (2)0.097 (2)0.063 (2)0.059 (2)0.0338 (17)
O20.126 (2)0.0706 (15)0.146 (2)0.0151 (14)0.0732 (19)0.0095 (14)
O30.116 (2)0.142 (3)0.137 (3)0.0131 (19)0.024 (2)0.032 (2)
O70.183 (3)0.0816 (17)0.118 (2)0.0396 (19)0.014 (2)0.0234 (16)
O50.401 (8)0.300 (6)0.084 (2)0.213 (6)0.088 (3)0.059 (3)
O60.185 (4)0.177 (3)0.163 (3)0.095 (3)0.042 (3)0.063 (3)
O40.107 (2)0.0652 (15)0.199 (3)0.0198 (14)0.030 (2)0.0027 (17)
O80.157 (3)0.197 (4)0.107 (2)0.051 (3)0.045 (2)0.032 (2)
C10.0519 (15)0.0468 (14)0.0763 (18)0.0119 (11)0.0081 (13)0.0115 (12)
C20.0581 (15)0.0439 (13)0.0571 (14)0.0044 (11)0.0100 (12)0.0016 (11)
C30.082 (2)0.0409 (13)0.090 (2)0.0081 (13)0.0101 (17)0.0106 (13)
C40.104 (3)0.0524 (16)0.085 (2)0.0023 (17)0.003 (2)0.0230 (15)
C50.089 (2)0.0554 (16)0.0620 (17)0.0147 (15)0.0101 (16)0.0080 (13)
C60.0663 (17)0.0464 (13)0.0471 (14)0.0040 (12)0.0051 (12)0.0004 (10)
C70.085 (2)0.0583 (15)0.0455 (14)0.0103 (14)0.0012 (14)0.0073 (12)
C80.0743 (18)0.0460 (13)0.0534 (15)0.0076 (12)0.0201 (13)0.0067 (11)
C90.107 (3)0.0581 (17)0.0727 (19)0.0069 (18)0.0363 (19)0.0139 (15)
C100.098 (3)0.0612 (18)0.109 (3)0.0125 (18)0.046 (2)0.0111 (18)
C110.070 (2)0.0627 (18)0.112 (3)0.0138 (15)0.0297 (19)0.0057 (18)
C120.0504 (14)0.0461 (13)0.0812 (19)0.0015 (11)0.0179 (13)0.0069 (12)
C130.0544 (15)0.0641 (16)0.0658 (17)0.0043 (13)0.0162 (13)0.0207 (13)
C140.0466 (14)0.0757 (17)0.0488 (14)0.0102 (13)0.0112 (11)0.0128 (13)
C150.0539 (16)0.113 (3)0.0469 (15)0.0119 (17)0.0118 (13)0.0176 (16)
C160.0542 (17)0.144 (3)0.0415 (15)0.0172 (19)0.0065 (13)0.0002 (18)
C170.0518 (16)0.101 (2)0.0530 (16)0.0108 (15)0.0031 (13)0.0162 (16)
C180.0416 (13)0.0717 (17)0.0481 (13)0.0116 (12)0.0018 (11)0.0087 (12)
C190.0620 (17)0.0425 (13)0.093 (2)0.0089 (12)0.0090 (15)0.0032 (13)
C200.0539 (16)0.0611 (17)0.098 (2)0.0122 (13)0.0081 (16)0.0048 (15)
C210.0539 (16)0.0614 (16)0.091 (2)0.0023 (13)0.0193 (15)0.0202 (15)
C220.0469 (16)0.0650 (18)0.128 (3)0.0042 (14)0.0032 (17)0.0214 (18)
C230.093 (2)0.0718 (19)0.0592 (17)0.0075 (17)0.0292 (16)0.0018 (14)
C240.070 (2)0.0685 (19)0.093 (2)0.0009 (15)0.0285 (18)0.0152 (17)
C300.0673 (18)0.0628 (16)0.0663 (17)0.0048 (13)0.0122 (14)0.0127 (13)
C310.078 (2)0.0532 (16)0.095 (2)0.0022 (14)0.0381 (17)0.0025 (15)
C320.0587 (18)0.080 (2)0.085 (2)0.0114 (15)0.0048 (16)0.0011 (17)
Geometric parameters (Å, º) top
Fe1—N52.1174 (19)C9—C101.407 (5)
Fe1—N42.123 (2)C9—H190.9300
Fe1—N12.138 (2)C10—C111.357 (5)
Fe1—N32.2747 (19)C10—H1100.9300
Fe1—N22.3014 (19)C11—C121.391 (4)
Fe1—N62.3101 (19)C11—H1110.9300
Cl1—O41.397 (2)C12—C321.470 (4)
Cl1—O11.401 (3)C13—C141.449 (4)
Cl1—O21.414 (2)C13—H1130.9300
Cl1—O31.434 (3)C14—C151.379 (4)
Cl2—O51.276 (4)C15—C161.357 (5)
Cl2—O71.389 (3)C15—H1150.9300
Cl2—O61.392 (3)C16—C171.364 (5)
Cl2—O81.408 (3)C16—H1160.9300
N1—C71.259 (3)C17—C181.396 (4)
N1—C231.484 (4)C17—H1170.9300
N2—C121.341 (3)C18—C301.483 (4)
N2—C81.363 (3)C19—C201.509 (4)
N3—C181.339 (3)C19—H1190.9700
N3—C141.356 (3)C19—H2190.9700
N4—C131.260 (3)C20—H1200.9700
N4—C191.459 (3)C20—H2200.9700
N5—C11.256 (3)C21—C221.526 (4)
N5—C211.475 (3)C21—H1210.9700
N6—C61.342 (3)C21—H2210.9700
N6—C21.357 (3)C22—H1220.9700
N7—C241.427 (4)C22—H2220.9700
N7—C201.450 (4)C23—C241.509 (5)
N7—C221.462 (4)C23—H1230.9700
C1—C21.458 (4)C23—H2230.9700
C1—H110.9300C24—H1240.9700
C2—C31.379 (4)C24—H2240.9700
C3—C41.382 (5)C30—H1300.9600
C3—H130.9300C30—H2300.9600
C4—C51.337 (4)C30—H3300.9600
C4—H140.9300C31—H1310.9600
C5—C61.401 (4)C31—H2310.9600
C5—H150.9300C31—H3310.9600
C6—C311.490 (4)C32—H1320.9600
C7—C81.465 (4)C32—H2320.9600
C7—H170.9300C32—H3320.9600
C8—C91.377 (4)
N5—Fe1—N498.28 (8)C10—C11—C12120.7 (3)
N5—Fe1—N196.54 (8)C10—C11—H111119.6
N4—Fe1—N196.03 (8)C12—C11—H111119.6
N5—Fe1—N385.64 (7)N2—C12—C11121.7 (3)
N4—Fe1—N375.85 (8)N2—C12—C32119.1 (2)
N1—Fe1—N3171.84 (7)C11—C12—C32119.2 (3)
N5—Fe1—N2171.36 (8)N4—C13—C14120.5 (2)
N4—Fe1—N286.58 (7)N4—C13—H113119.7
N1—Fe1—N275.76 (8)C14—C13—H113119.7
N3—Fe1—N2102.54 (7)N3—C14—C15122.9 (3)
N5—Fe1—N675.12 (8)N3—C14—C13116.9 (2)
N4—Fe1—N6173.22 (7)C15—C14—C13120.2 (3)
N1—Fe1—N686.39 (7)C16—C15—C14119.1 (3)
N3—Fe1—N6101.77 (7)C16—C15—H115120.4
N2—Fe1—N6100.17 (7)C14—C15—H115120.4
O4—Cl1—O1112.1 (2)C15—C16—C17118.9 (3)
O4—Cl1—O2112.10 (16)C15—C16—H116120.6
O1—Cl1—O2111.76 (17)C17—C16—H116120.6
O4—Cl1—O3106.5 (2)C16—C17—C18120.4 (3)
O1—Cl1—O3104.8 (2)C16—C17—H117119.8
O2—Cl1—O3109.1 (2)C18—C17—H117119.8
O5—Cl2—O7107.4 (2)N3—C18—C17121.0 (3)
O5—Cl2—O6111.5 (4)N3—C18—C30118.6 (2)
O7—Cl2—O6112.2 (3)C17—C18—C30120.4 (3)
O5—Cl2—O8111.1 (4)N4—C19—C20109.1 (2)
O7—Cl2—O8113.1 (2)N4—C19—H119109.9
O6—Cl2—O8101.6 (2)C20—C19—H119109.9
C7—N1—C23118.8 (2)N4—C19—H219109.9
C7—N1—Fe1117.02 (19)C20—C19—H219109.9
C23—N1—Fe1124.02 (19)H119—C19—H219108.3
C12—N2—C8117.8 (2)N7—C20—C19110.8 (2)
C12—N2—Fe1132.56 (18)N7—C20—H120109.5
C8—N2—Fe1109.59 (17)C19—C20—H120109.5
C18—N3—C14117.7 (2)N7—C20—H220109.5
C18—N3—Fe1132.05 (16)C19—C20—H220109.5
C14—N3—Fe1109.96 (16)H120—C20—H220108.1
C13—N4—C19118.4 (2)N5—C21—C22108.5 (2)
C13—N4—Fe1116.54 (18)N5—C21—H121110.0
C19—N4—Fe1125.01 (18)C22—C21—H121110.0
C1—N5—C21118.7 (2)N5—C21—H221110.0
C1—N5—Fe1117.96 (18)C22—C21—H221110.0
C21—N5—Fe1123.26 (17)H121—C21—H221108.4
C6—N6—C2117.8 (2)N7—C22—C21111.0 (2)
C6—N6—Fe1132.33 (16)N7—C22—H122109.4
C2—N6—Fe1109.80 (16)C21—C22—H122109.4
C24—N7—C20117.4 (2)N7—C22—H222109.4
C24—N7—C22117.2 (3)C21—C22—H222109.4
C20—N7—C22116.9 (3)H122—C22—H222108.0
N5—C1—C2120.4 (2)N1—C23—C24110.7 (2)
N5—C1—H11119.8N1—C23—H123109.5
C2—C1—H11119.8C24—C23—H123109.5
N6—C2—C3122.9 (3)N1—C23—H223109.5
N6—C2—C1116.4 (2)C24—C23—H223109.5
C3—C2—C1120.7 (3)H123—C23—H223108.1
C2—C3—C4118.5 (3)N7—C24—C23112.7 (2)
C2—C3—H13120.8N7—C24—H124109.0
C4—C3—H13120.8C23—C24—H124109.0
C5—C4—C3119.1 (3)N7—C24—H224109.0
C5—C4—H14120.4C23—C24—H224109.0
C3—C4—H14120.4H124—C24—H224107.8
C4—C5—C6121.0 (3)C18—C30—H130109.5
C4—C5—H15119.5C18—C30—H230109.5
C6—C5—H15119.5H130—C30—H230109.5
N6—C6—C5120.7 (2)C18—C30—H330109.5
N6—C6—C31118.6 (2)H130—C30—H330109.5
C5—C6—C31120.7 (3)H230—C30—H330109.5
N1—C7—C8120.5 (2)C6—C31—H131109.5
N1—C7—H17119.7C6—C31—H231109.5
C8—C7—H17119.7H131—C31—H231109.5
N2—C8—C9122.9 (3)C6—C31—H331109.5
N2—C8—C7117.1 (2)H131—C31—H331109.5
C9—C8—C7120.0 (3)H231—C31—H331109.5
C8—C9—C10118.4 (3)C12—C32—H132109.5
C8—C9—H19120.8C12—C32—H232109.5
C10—C9—H19120.8H132—C32—H232109.5
C11—C10—C9118.5 (3)C12—C32—H332109.5
C11—C10—H110120.8H132—C32—H332109.5
C9—C10—H110120.8H232—C32—H332109.5
(1_330) top
Crystal data top
C27H33Cl2FeN7O8Z = 4
Mr = 710.35F(000) = 1472
Monoclinic, P21/cDx = 1.496 Mg m3
a = 10.6286 (7) ÅMo Kα radiation, λ = 0.71073 Å
b = 19.4535 (11) ŵ = 0.71 mm1
c = 15.2589 (10) ÅT = 330 K
β = 91.626 (6)°Polyhedron, dark red
V = 3153.7 (3) Å30.48 × 0.32 × 0.12 mm
Data collection top
KM4_CCD_Sapphire3
diffractometer
9826 independent reflections
Radiation source: fine-focus sealed tube4778 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
Detector resolution: 16.0328 pixels mm-1θmax = 32.8°, θmin = 2.9°
θ–scanh = 1515
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 2920
Tmin = 0.864, Tmax = 0.913l = 2220
27325 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.051Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.162H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.0875P)2]
where P = (Fo2 + 2Fc2)/3
9826 reflections(Δ/σ)max = 0.001
409 parametersΔρmax = 0.90 e Å3
0 restraintsΔρmin = 0.76 e Å3
Crystal data top
C27H33Cl2FeN7O8V = 3153.7 (3) Å3
Mr = 710.35Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.6286 (7) ŵ = 0.71 mm1
b = 19.4535 (11) ÅT = 330 K
c = 15.2589 (10) Å0.48 × 0.32 × 0.12 mm
β = 91.626 (6)°
Data collection top
KM4_CCD_Sapphire3
diffractometer
9826 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
4778 reflections with I > 2σ(I)
Tmin = 0.864, Tmax = 0.913Rint = 0.021
27325 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0510 restraints
wR(F2) = 0.162H-atom parameters constrained
S = 1.00Δρmax = 0.90 e Å3
9826 reflectionsΔρmin = 0.76 e Å3
409 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.69961 (3)0.071182 (16)0.74103 (2)0.04317 (12)
Cl11.36123 (8)0.31808 (4)0.53953 (6)0.0727 (2)
Cl21.22389 (9)0.14705 (5)0.69166 (7)0.0881 (3)
N10.6277 (2)0.10185 (11)0.61455 (14)0.0591 (6)
N20.8444 (2)0.15038 (10)0.69306 (14)0.0519 (5)
N30.76502 (19)0.05309 (11)0.88287 (13)0.0505 (5)
N40.6188 (2)0.15368 (10)0.81151 (15)0.0550 (5)
N50.56106 (19)0.00453 (11)0.76475 (14)0.0531 (5)
N60.7704 (2)0.02719 (10)0.67259 (12)0.0485 (5)
N70.4063 (2)0.10733 (12)0.71469 (18)0.0719 (7)
O11.3230 (4)0.30619 (19)0.6249 (2)0.1543 (15)
O21.4371 (3)0.26463 (13)0.5082 (2)0.1246 (11)
O31.2454 (4)0.31955 (19)0.4888 (3)0.1489 (13)
O71.1692 (4)0.20407 (15)0.6517 (2)0.1378 (12)
O51.2917 (7)0.1184 (3)0.6363 (3)0.286 (4)
O61.1357 (5)0.1021 (2)0.7244 (3)0.193 (2)
O41.4157 (3)0.38241 (13)0.5291 (3)0.1349 (12)
O81.2930 (4)0.1628 (3)0.7690 (2)0.1693 (17)
C10.5770 (3)0.06345 (13)0.7336 (2)0.0619 (7)
H110.51950.09810.74490.074*
C20.6849 (3)0.07807 (12)0.67972 (18)0.0564 (6)
C30.6967 (3)0.14090 (14)0.6391 (2)0.0762 (9)
H130.63540.17460.64460.091*
C40.8015 (4)0.15254 (16)0.5900 (2)0.0853 (10)
H140.81120.19410.56090.102*
C50.8891 (3)0.10347 (15)0.5846 (2)0.0731 (8)
H150.96100.11160.55290.088*
C60.8737 (3)0.03979 (13)0.62637 (17)0.0575 (6)
C70.6913 (3)0.14531 (15)0.57336 (18)0.0672 (8)
H170.66350.15990.51810.081*
C80.8086 (3)0.17310 (13)0.61167 (19)0.0616 (7)
C90.8786 (4)0.21912 (16)0.5654 (2)0.0852 (11)
H190.85230.23320.50950.102*
C100.9908 (4)0.24458 (19)0.6039 (3)0.0957 (12)
H1101.04030.27580.57430.115*
C111.0249 (3)0.22251 (17)0.6852 (3)0.0865 (10)
H1111.09890.23870.71180.104*
C120.9504 (3)0.17575 (13)0.7293 (2)0.0621 (7)
C130.6472 (3)0.15746 (15)0.8918 (2)0.0660 (8)
H1130.62030.19490.92420.079*
C140.7216 (3)0.10390 (16)0.93479 (17)0.0612 (7)
C150.7401 (3)0.1045 (2)1.02413 (19)0.0762 (9)
H1150.71000.14071.05740.091*
C160.8032 (3)0.0515 (2)1.0635 (2)0.0867 (11)
H1160.81890.05141.12380.104*
C170.8430 (3)0.0015 (2)1.01281 (19)0.0747 (9)
H1170.88200.03931.03900.090*
C180.8256 (2)0.00069 (15)0.92189 (17)0.0577 (7)
C190.5284 (3)0.20312 (14)0.7749 (2)0.0706 (8)
H1190.55520.21840.71790.085*
H2190.52410.24290.81300.085*
C200.4010 (3)0.16989 (16)0.7663 (3)0.0769 (9)
H1200.37080.15920.82410.092*
H2200.34210.20170.73840.092*
C210.4466 (3)0.00957 (16)0.8141 (2)0.0729 (8)
H1210.46680.03860.86420.088*
H2210.41130.03310.83520.088*
C220.3516 (3)0.04575 (17)0.7524 (3)0.0865 (11)
H1220.32560.01460.70580.104*
H2220.27770.05820.78470.104*
C230.5045 (4)0.07919 (17)0.5764 (2)0.0799 (10)
H1230.49650.02980.58250.096*
H2230.50010.09020.51440.096*
C240.3979 (3)0.11412 (17)0.6219 (2)0.0828 (10)
H1240.39770.16260.60680.099*
H2240.31880.09460.60060.099*
C300.8753 (3)0.05520 (15)0.8660 (2)0.0713 (8)
H1300.80640.08140.84140.107*
H2300.92890.08470.90100.107*
H3300.92260.03550.81960.107*
C310.9724 (3)0.01409 (15)0.6219 (2)0.0799 (9)
H1310.94530.04930.58160.120*
H2311.04910.00600.60230.120*
H3310.98650.03380.67900.120*
C320.9918 (3)0.15204 (18)0.8169 (2)0.0809 (9)
H1320.93380.16790.85950.121*
H2321.07410.17000.83070.121*
H3320.99460.10270.81760.121*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0478 (2)0.03863 (17)0.04322 (19)0.00242 (14)0.00286 (14)0.00061 (13)
Cl10.0804 (5)0.0570 (4)0.0819 (5)0.0076 (3)0.0228 (4)0.0002 (3)
Cl20.0903 (6)0.0721 (5)0.1012 (7)0.0012 (4)0.0077 (5)0.0133 (5)
N10.0710 (15)0.0530 (12)0.0526 (13)0.0015 (11)0.0076 (11)0.0000 (10)
N20.0546 (13)0.0414 (10)0.0603 (13)0.0013 (9)0.0129 (10)0.0009 (9)
N30.0463 (11)0.0607 (12)0.0446 (11)0.0093 (9)0.0051 (9)0.0007 (9)
N40.0512 (12)0.0479 (11)0.0663 (14)0.0003 (9)0.0067 (10)0.0061 (10)
N50.0443 (11)0.0520 (12)0.0630 (13)0.0038 (9)0.0010 (10)0.0111 (10)
N60.0604 (13)0.0391 (10)0.0459 (11)0.0011 (9)0.0011 (10)0.0014 (8)
N70.0669 (16)0.0596 (14)0.0886 (19)0.0055 (12)0.0062 (14)0.0114 (13)
O10.205 (4)0.152 (3)0.110 (2)0.073 (3)0.070 (2)0.041 (2)
O20.139 (2)0.0762 (16)0.163 (3)0.0177 (16)0.081 (2)0.0111 (16)
O30.129 (3)0.161 (3)0.156 (3)0.015 (2)0.026 (2)0.041 (2)
O70.193 (3)0.0905 (19)0.128 (2)0.043 (2)0.019 (2)0.0230 (18)
O50.444 (9)0.326 (7)0.093 (2)0.239 (7)0.102 (4)0.069 (3)
O60.210 (4)0.188 (4)0.177 (4)0.100 (4)0.041 (3)0.064 (3)
O40.119 (2)0.0703 (17)0.218 (4)0.0211 (16)0.035 (2)0.0040 (19)
O80.171 (4)0.218 (4)0.116 (3)0.051 (3)0.051 (3)0.036 (3)
C10.0558 (16)0.0488 (15)0.0806 (19)0.0134 (12)0.0089 (14)0.0109 (13)
C20.0631 (16)0.0450 (13)0.0603 (15)0.0042 (12)0.0110 (13)0.0010 (11)
C30.088 (2)0.0440 (14)0.096 (2)0.0087 (14)0.0103 (19)0.0130 (15)
C40.109 (3)0.0564 (18)0.090 (2)0.0036 (18)0.004 (2)0.0258 (17)
C50.095 (2)0.0576 (17)0.0675 (19)0.0159 (17)0.0118 (17)0.0092 (14)
C60.0728 (18)0.0482 (14)0.0516 (15)0.0065 (13)0.0053 (13)0.0005 (11)
C70.092 (2)0.0624 (16)0.0470 (14)0.0097 (16)0.0017 (15)0.0088 (13)
C80.0794 (19)0.0471 (14)0.0595 (16)0.0059 (13)0.0219 (15)0.0056 (12)
C90.113 (3)0.0632 (18)0.081 (2)0.0067 (19)0.039 (2)0.0165 (16)
C100.106 (3)0.068 (2)0.115 (3)0.015 (2)0.048 (3)0.012 (2)
C110.073 (2)0.068 (2)0.120 (3)0.0160 (16)0.031 (2)0.007 (2)
C120.0546 (15)0.0480 (14)0.085 (2)0.0024 (12)0.0189 (14)0.0070 (13)
C130.0594 (17)0.0685 (18)0.0709 (19)0.0043 (14)0.0164 (15)0.0244 (15)
C140.0490 (15)0.0834 (19)0.0518 (15)0.0110 (14)0.0128 (12)0.0136 (14)
C150.0575 (17)0.124 (3)0.0479 (16)0.0121 (18)0.0106 (14)0.0188 (17)
C160.0584 (19)0.158 (4)0.0440 (16)0.021 (2)0.0064 (14)0.002 (2)
C170.0565 (17)0.112 (3)0.0555 (17)0.0132 (17)0.0039 (14)0.0173 (18)
C180.0456 (14)0.0745 (18)0.0527 (14)0.0133 (13)0.0027 (11)0.0105 (13)
C190.0658 (18)0.0464 (14)0.100 (2)0.0103 (13)0.0088 (16)0.0039 (15)
C200.0598 (18)0.0641 (18)0.107 (3)0.0137 (15)0.0087 (17)0.0053 (17)
C210.0582 (17)0.0647 (17)0.097 (2)0.0043 (14)0.0217 (16)0.0192 (16)
C220.0502 (17)0.069 (2)0.140 (3)0.0061 (15)0.0032 (18)0.022 (2)
C230.101 (3)0.075 (2)0.0618 (18)0.0094 (18)0.0324 (18)0.0011 (15)
C240.073 (2)0.073 (2)0.101 (3)0.0026 (17)0.0307 (19)0.0151 (18)
C300.073 (2)0.0676 (18)0.0725 (19)0.0057 (15)0.0145 (16)0.0136 (15)
C310.083 (2)0.0560 (17)0.103 (2)0.0025 (15)0.0422 (19)0.0033 (16)
C320.0623 (19)0.087 (2)0.094 (2)0.0129 (16)0.0040 (17)0.0008 (19)
Geometric parameters (Å, º) top
Fe1—N52.121 (2)C9—C101.404 (6)
Fe1—N42.127 (2)C9—H190.9300
Fe1—N12.140 (2)C10—C111.352 (6)
Fe1—N32.282 (2)C10—H1100.9300
Fe1—N22.311 (2)C11—C121.392 (4)
Fe1—N62.3160 (19)C11—H1110.9300
Cl1—O41.390 (3)C12—C321.469 (5)
Cl1—O11.395 (3)C13—C141.453 (4)
Cl1—O21.408 (3)C13—H1130.9300
Cl1—O31.435 (4)C14—C151.372 (4)
Cl2—O51.256 (4)C15—C161.360 (5)
Cl2—O61.386 (4)C15—H1150.9300
Cl2—O71.386 (3)C16—C171.363 (5)
Cl2—O81.406 (3)C16—H1160.9300
N1—C71.261 (4)C17—C181.395 (4)
N1—C231.485 (4)C17—H1170.9300
N2—C121.336 (4)C18—C301.488 (4)
N2—C81.362 (4)C19—C201.503 (4)
N3—C181.337 (3)C19—H1190.9700
N3—C141.356 (3)C19—H2190.9700
N4—C131.256 (4)C20—H1200.9700
N4—C191.459 (4)C20—H2200.9700
N5—C11.254 (3)C21—C221.531 (4)
N5—C211.474 (4)C21—H1210.9700
N6—C61.344 (3)C21—H2210.9700
N6—C21.351 (3)C22—H1220.9700
N7—C241.423 (4)C22—H2220.9700
N7—C201.451 (4)C23—C241.507 (5)
N7—C221.457 (4)C23—H1230.9700
C1—C21.457 (4)C23—H2230.9700
C1—H110.9300C24—H1240.9700
C2—C31.378 (4)C24—H2240.9700
C3—C41.379 (5)C30—H1300.9600
C3—H130.9300C30—H2300.9600
C4—C51.337 (5)C30—H3300.9600
C4—H140.9300C31—H1310.9600
C5—C61.405 (4)C31—H2310.9600
C5—H150.9300C31—H3310.9600
C6—C311.486 (4)C32—H1320.9600
C7—C81.465 (4)C32—H2320.9600
C7—H170.9300C32—H3320.9600
C8—C91.373 (4)
N5—Fe1—N498.36 (8)C10—C11—C12120.6 (4)
N5—Fe1—N196.63 (9)C10—C11—H111119.7
N4—Fe1—N196.12 (9)C12—C11—H111119.7
N5—Fe1—N385.72 (8)N2—C12—C11121.7 (3)
N4—Fe1—N375.72 (8)N2—C12—C32119.2 (2)
N1—Fe1—N3171.77 (8)C11—C12—C32119.0 (3)
N5—Fe1—N2171.36 (8)N4—C13—C14120.7 (2)
N4—Fe1—N286.52 (8)N4—C13—H113119.6
N1—Fe1—N275.67 (9)C14—C13—H113119.6
N3—Fe1—N2102.45 (8)N3—C14—C15123.0 (3)
N5—Fe1—N674.89 (8)N3—C14—C13116.7 (2)
N4—Fe1—N6173.07 (8)C15—C14—C13120.2 (3)
N1—Fe1—N686.33 (8)C16—C15—C14119.1 (3)
N3—Fe1—N6101.89 (7)C16—C15—H115120.4
N2—Fe1—N6100.38 (7)C14—C15—H115120.4
O4—Cl1—O1113.0 (3)C15—C16—C17118.7 (3)
O4—Cl1—O2112.42 (18)C15—C16—H116120.7
O1—Cl1—O2112.33 (18)C17—C16—H116120.7
O4—Cl1—O3105.9 (2)C16—C17—C18120.5 (3)
O1—Cl1—O3103.8 (3)C16—C17—H117119.8
O2—Cl1—O3108.8 (2)C18—C17—H117119.8
O5—Cl2—O6111.7 (5)N3—C18—C17121.0 (3)
O5—Cl2—O7107.5 (3)N3—C18—C30118.5 (2)
O6—Cl2—O7112.6 (3)C17—C18—C30120.6 (3)
O5—Cl2—O8111.4 (4)N4—C19—C20109.4 (2)
O6—Cl2—O8100.2 (3)N4—C19—H119109.8
O7—Cl2—O8113.4 (3)C20—C19—H119109.8
C7—N1—C23118.9 (3)N4—C19—H219109.8
C7—N1—Fe1117.0 (2)C20—C19—H219109.8
C23—N1—Fe1124.0 (2)H119—C19—H219108.2
C12—N2—C8117.9 (2)N7—C20—C19111.1 (2)
C12—N2—Fe1132.59 (19)N7—C20—H120109.4
C8—N2—Fe1109.51 (18)C19—C20—H120109.4
C18—N3—C14117.6 (2)N7—C20—H220109.4
C18—N3—Fe1132.08 (18)C19—C20—H220109.4
C14—N3—Fe1110.01 (18)H120—C20—H220108.0
C13—N4—C19118.2 (2)N5—C21—C22108.1 (3)
C13—N4—Fe1116.63 (19)N5—C21—H121110.1
C19—N4—Fe1125.1 (2)C22—C21—H121110.1
C1—N5—C21119.1 (2)N5—C21—H221110.1
C1—N5—Fe1117.90 (19)C22—C21—H221110.1
C21—N5—Fe1123.02 (18)H121—C21—H221108.4
C6—N6—C2118.1 (2)N7—C22—C21111.0 (2)
C6—N6—Fe1131.92 (17)N7—C22—H122109.4
C2—N6—Fe1109.94 (17)C21—C22—H122109.4
C24—N7—C20117.4 (3)N7—C22—H222109.4
C24—N7—C22117.1 (3)C21—C22—H222109.4
C20—N7—C22116.9 (3)H122—C22—H222108.0
N5—C1—C2120.6 (2)N1—C23—C24110.6 (3)
N5—C1—H11119.7N1—C23—H123109.5
C2—C1—H11119.7C24—C23—H123109.5
N6—C2—C3122.9 (3)N1—C23—H223109.5
N6—C2—C1116.4 (2)C24—C23—H223109.5
C3—C2—C1120.7 (3)H123—C23—H223108.1
C2—C3—C4118.4 (3)N7—C24—C23113.0 (3)
C2—C3—H13120.8N7—C24—H124109.0
C4—C3—H13120.8C23—C24—H124109.0
C5—C4—C3119.4 (3)N7—C24—H224109.0
C5—C4—H14120.3C23—C24—H224109.0
C3—C4—H14120.3H124—C24—H224107.8
C4—C5—C6120.8 (3)C18—C30—H130109.5
C4—C5—H15119.6C18—C30—H230109.5
C6—C5—H15119.6H130—C30—H230109.5
N6—C6—C5120.4 (3)C18—C30—H330109.5
N6—C6—C31118.9 (2)H130—C30—H330109.5
C5—C6—C31120.7 (3)H230—C30—H330109.5
N1—C7—C8120.7 (3)C6—C31—H131109.5
N1—C7—H17119.6C6—C31—H231109.5
C8—C7—H17119.6H131—C31—H231109.5
N2—C8—C9122.7 (3)C6—C31—H331109.5
N2—C8—C7117.2 (2)H131—C31—H331109.5
C9—C8—C7120.2 (3)H231—C31—H331109.5
C8—C9—C10118.7 (3)C12—C32—H132109.5
C8—C9—H19120.6C12—C32—H232109.5
C10—C9—H19120.6H132—C32—H232109.5
C11—C10—C9118.3 (3)C12—C32—H332109.5
C11—C10—H110120.8H132—C32—H332109.5
C9—C10—H110120.8H232—C32—H332109.5
(1-Zn_80) top
Crystal data top
C27H33Cl2N7O8ZnZ = 4
Mr = 719.87F(000) = 1488
Monoclinic, P21/cDx = 1.590 Mg m3
a = 10.3736 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 19.1884 (5) ŵ = 1.06 mm1
c = 15.1122 (4) ÅT = 80 K
β = 91.885 (2)°Polyhedron, yellow
V = 3006.50 (14) Å30.32 × 0.26 × 0.12 mm
Data collection top
KM4_CCD_Sapphire3
diffractometer
10191 independent reflections
Radiation source: fine-focus sealed tube7979 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.022
Detector resolution: 16.0328 pixels mm-1θmax = 32.9°, θmin = 2.9°
θ–scanh = 1515
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 2728
Tmin = 0.854, Tmax = 0.885l = 1322
29446 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.075H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.048P)2]
where P = (Fo2 + 2Fc2)/3
10191 reflections(Δ/σ)max = 0.003
409 parametersΔρmax = 0.82 e Å3
0 restraintsΔρmin = 0.58 e Å3
Crystal data top
C27H33Cl2N7O8ZnV = 3006.50 (14) Å3
Mr = 719.87Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.3736 (3) ŵ = 1.06 mm1
b = 19.1884 (5) ÅT = 80 K
c = 15.1122 (4) Å0.32 × 0.26 × 0.12 mm
β = 91.885 (2)°
Data collection top
KM4_CCD_Sapphire3
diffractometer
10191 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
7979 reflections with I > 2σ(I)
Tmin = 0.854, Tmax = 0.885Rint = 0.022
29446 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0270 restraints
wR(F2) = 0.075H-atom parameters constrained
S = 1.00Δρmax = 0.82 e Å3
10191 reflectionsΔρmin = 0.58 e Å3
409 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Zn10.696736 (13)0.070108 (7)0.739268 (8)0.01181 (4)
Cl11.36342 (3)0.318031 (15)0.538044 (19)0.01667 (6)
Cl21.22191 (3)0.148394 (16)0.701286 (19)0.01827 (6)
N10.61580 (10)0.09994 (5)0.61280 (7)0.01575 (19)
N20.84350 (10)0.14809 (5)0.68757 (7)0.01448 (19)
N30.77184 (10)0.04992 (5)0.88201 (6)0.01396 (18)
N40.62053 (10)0.15342 (5)0.81132 (7)0.01457 (19)
N50.55877 (10)0.00634 (5)0.76543 (7)0.01439 (19)
N60.77469 (10)0.02906 (5)0.67052 (6)0.01338 (18)
N70.39497 (10)0.10727 (5)0.71925 (7)0.0176 (2)
O11.33870 (11)0.30448 (6)0.62971 (6)0.0290 (2)
O21.43859 (9)0.26123 (5)0.50304 (6)0.0245 (2)
O31.24223 (9)0.32243 (5)0.48854 (6)0.0235 (2)
O41.43240 (10)0.38247 (5)0.52972 (7)0.0284 (2)
O51.29961 (15)0.11346 (8)0.63813 (8)0.0593 (4)
O61.12294 (12)0.10253 (7)0.72786 (8)0.0468 (3)
O71.16808 (13)0.20952 (6)0.66083 (7)0.0382 (3)
O81.30168 (12)0.16560 (7)0.77759 (7)0.0392 (3)
C10.57528 (12)0.06684 (6)0.73350 (8)0.0161 (2)
H110.51610.10310.74560.019*
C20.68643 (12)0.08068 (6)0.67770 (8)0.0146 (2)
C30.69752 (13)0.14506 (6)0.63774 (9)0.0190 (2)
H130.63240.17940.64360.023*
C40.80600 (13)0.15857 (7)0.58870 (9)0.0205 (2)
H140.81640.20220.56000.025*
C50.89767 (13)0.10714 (6)0.58284 (8)0.0178 (2)
H150.97330.11540.55070.021*
C60.88016 (12)0.04256 (6)0.62405 (7)0.0147 (2)
C70.68116 (13)0.14306 (6)0.56890 (8)0.0177 (2)
H170.65070.15760.51180.021*
C80.80412 (12)0.17073 (6)0.60608 (8)0.0161 (2)
C90.87419 (14)0.21741 (7)0.55664 (9)0.0214 (3)
H190.84450.23090.49900.026*
C100.98841 (14)0.24389 (7)0.59296 (10)0.0243 (3)
H1101.03850.27600.56080.029*
C111.02774 (13)0.22264 (7)0.67659 (9)0.0225 (3)
H1111.10500.24070.70300.027*
C120.95388 (12)0.17428 (6)0.72289 (8)0.0171 (2)
C130.65479 (12)0.15772 (7)0.89249 (8)0.0176 (2)
H1130.63080.19730.92590.021*
C140.73112 (12)0.10204 (7)0.93506 (8)0.0165 (2)
C150.75138 (12)0.10281 (7)1.02606 (8)0.0201 (3)
H1150.72440.14131.06040.024*
C160.81197 (12)0.04604 (8)1.06571 (8)0.0215 (3)
H1160.82810.04491.12790.026*
C170.84847 (12)0.00875 (7)1.01337 (8)0.0200 (2)
H1170.88620.04911.03980.024*
C180.83010 (11)0.00524 (7)0.92082 (8)0.0158 (2)
C190.52833 (12)0.20458 (6)0.77552 (8)0.0172 (2)
H1190.55280.21910.71550.021*
H2190.52780.24640.81390.021*
C200.39480 (12)0.17071 (6)0.77171 (9)0.0181 (2)
H1200.36850.15970.83250.022*
H2200.33120.20390.74550.022*
C210.44390 (12)0.00665 (7)0.81718 (9)0.0181 (2)
H1210.46720.03540.86970.022*
H2210.40810.03810.83790.022*
C220.34316 (12)0.04479 (7)0.75855 (9)0.0205 (2)
H1220.31170.01300.71090.025*
H2220.26870.05750.79460.025*
C230.48993 (13)0.07726 (7)0.57661 (8)0.0200 (2)
H1230.48080.02630.58430.024*
H2230.48340.08770.51250.024*
C240.38216 (13)0.11494 (7)0.62425 (8)0.0204 (2)
H1240.38400.16510.60900.025*
H2240.29770.09600.60350.025*
C300.87688 (13)0.06304 (7)0.86433 (8)0.0182 (2)
H1300.80320.09050.84190.027*
H2300.93530.09310.89950.027*
H3300.92300.04360.81440.027*
C310.98181 (13)0.01259 (7)0.61868 (9)0.0202 (2)
H1310.94910.05120.58190.030*
H2311.05880.00710.59230.030*
H3311.00410.02980.67830.030*
C320.99838 (13)0.15021 (7)0.81299 (9)0.0208 (2)
H1320.94470.17160.85770.031*
H2321.08850.16390.82380.031*
H3320.99100.09940.81640.031*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.01317 (7)0.01042 (6)0.01192 (6)0.00038 (5)0.00165 (4)0.00019 (5)
Cl10.01899 (14)0.01253 (12)0.01873 (13)0.00094 (10)0.00417 (10)0.00044 (10)
Cl20.02181 (14)0.01775 (13)0.01518 (12)0.00181 (11)0.00037 (10)0.00187 (10)
N10.0188 (5)0.0137 (5)0.0147 (4)0.0021 (4)0.0001 (4)0.0014 (4)
N20.0165 (5)0.0105 (4)0.0167 (4)0.0018 (4)0.0048 (4)0.0001 (4)
N30.0121 (4)0.0171 (5)0.0128 (4)0.0023 (4)0.0016 (3)0.0001 (4)
N40.0136 (5)0.0124 (4)0.0179 (5)0.0006 (4)0.0037 (4)0.0012 (4)
N50.0132 (4)0.0140 (4)0.0160 (4)0.0007 (4)0.0009 (4)0.0030 (4)
N60.0160 (5)0.0112 (4)0.0130 (4)0.0002 (4)0.0004 (4)0.0007 (3)
N70.0190 (5)0.0130 (5)0.0206 (5)0.0015 (4)0.0008 (4)0.0026 (4)
O10.0401 (6)0.0288 (5)0.0185 (5)0.0100 (5)0.0066 (4)0.0039 (4)
O20.0270 (5)0.0161 (4)0.0310 (5)0.0027 (4)0.0124 (4)0.0004 (4)
O30.0214 (5)0.0233 (5)0.0257 (5)0.0021 (4)0.0011 (4)0.0015 (4)
O40.0247 (5)0.0156 (5)0.0450 (6)0.0068 (4)0.0032 (4)0.0016 (4)
O50.0793 (10)0.0776 (11)0.0221 (6)0.0468 (8)0.0161 (6)0.0094 (6)
O60.0423 (7)0.0537 (8)0.0433 (7)0.0300 (6)0.0171 (6)0.0249 (6)
O70.0668 (8)0.0201 (5)0.0276 (5)0.0130 (5)0.0005 (5)0.0074 (4)
O80.0461 (7)0.0486 (7)0.0222 (5)0.0250 (6)0.0103 (5)0.0080 (5)
C10.0136 (5)0.0142 (5)0.0202 (5)0.0012 (4)0.0010 (4)0.0030 (4)
C20.0155 (5)0.0124 (5)0.0157 (5)0.0002 (4)0.0016 (4)0.0012 (4)
C30.0212 (6)0.0124 (5)0.0232 (6)0.0023 (5)0.0013 (5)0.0010 (4)
C40.0269 (7)0.0130 (5)0.0214 (6)0.0017 (5)0.0004 (5)0.0045 (4)
C50.0225 (6)0.0145 (5)0.0165 (5)0.0023 (5)0.0020 (5)0.0017 (4)
C60.0174 (5)0.0129 (5)0.0138 (5)0.0014 (4)0.0016 (4)0.0010 (4)
C70.0252 (6)0.0148 (5)0.0131 (5)0.0044 (5)0.0018 (4)0.0006 (4)
C80.0218 (6)0.0119 (5)0.0150 (5)0.0022 (4)0.0065 (4)0.0009 (4)
C90.0296 (7)0.0140 (5)0.0213 (6)0.0029 (5)0.0119 (5)0.0035 (5)
C100.0275 (7)0.0152 (6)0.0311 (7)0.0016 (5)0.0156 (6)0.0023 (5)
C110.0187 (6)0.0159 (6)0.0335 (7)0.0021 (5)0.0090 (5)0.0014 (5)
C120.0166 (6)0.0120 (5)0.0229 (6)0.0011 (4)0.0058 (5)0.0014 (4)
C130.0154 (5)0.0186 (6)0.0192 (5)0.0019 (5)0.0039 (4)0.0049 (4)
C140.0138 (5)0.0202 (6)0.0157 (5)0.0031 (4)0.0026 (4)0.0032 (4)
C150.0160 (6)0.0299 (7)0.0147 (5)0.0063 (5)0.0034 (4)0.0054 (5)
C160.0156 (6)0.0367 (8)0.0123 (5)0.0072 (5)0.0006 (4)0.0011 (5)
C170.0155 (6)0.0281 (7)0.0162 (5)0.0046 (5)0.0017 (4)0.0053 (5)
C180.0119 (5)0.0190 (6)0.0166 (5)0.0034 (4)0.0003 (4)0.0023 (4)
C190.0177 (6)0.0115 (5)0.0225 (6)0.0026 (4)0.0035 (5)0.0001 (4)
C200.0162 (6)0.0150 (5)0.0230 (6)0.0027 (4)0.0027 (5)0.0011 (5)
C210.0147 (5)0.0166 (5)0.0234 (6)0.0013 (5)0.0063 (4)0.0049 (5)
C220.0134 (5)0.0164 (6)0.0320 (7)0.0008 (5)0.0026 (5)0.0050 (5)
C230.0239 (6)0.0186 (6)0.0170 (5)0.0002 (5)0.0055 (5)0.0008 (4)
C240.0200 (6)0.0184 (6)0.0225 (6)0.0014 (5)0.0056 (5)0.0020 (5)
C300.0187 (6)0.0179 (6)0.0179 (5)0.0002 (5)0.0021 (4)0.0025 (4)
C310.0204 (6)0.0146 (5)0.0261 (6)0.0007 (5)0.0096 (5)0.0022 (5)
C320.0163 (6)0.0202 (6)0.0259 (6)0.0022 (5)0.0008 (5)0.0004 (5)
Geometric parameters (Å, º) top
Zn1—N52.0961 (10)C9—C101.386 (2)
Zn1—N42.1030 (10)C9—H190.9500
Zn1—N12.1400 (10)C10—C111.377 (2)
Zn1—N22.2904 (10)C10—H1100.9500
Zn1—N32.3021 (10)C11—C121.4045 (18)
Zn1—N62.3258 (10)C11—H1110.9500
Cl1—O41.4362 (10)C12—C321.4964 (18)
Cl1—O11.4408 (10)C13—C141.4660 (18)
Cl1—O31.4441 (10)C13—H1130.9500
Cl1—O21.4503 (9)C14—C151.3844 (17)
Cl2—O61.4201 (11)C15—C161.384 (2)
Cl2—O71.4278 (11)C15—H1150.9500
Cl2—O51.4354 (12)C16—C171.3764 (19)
Cl2—O81.4355 (11)C16—H1160.9500
N1—C71.2705 (16)C17—C181.4070 (16)
N1—C231.4651 (17)C17—H1170.9500
N2—C121.3448 (16)C18—C301.4904 (17)
N2—C81.3561 (16)C19—C201.5295 (17)
N3—C181.3440 (16)C19—H1190.9900
N3—C141.3577 (16)C19—H2190.9900
N4—C131.2685 (16)C20—H1200.9900
N4—C191.4619 (15)C20—H2200.9900
N5—C11.2709 (15)C21—C221.5334 (18)
N5—C211.4680 (15)C21—H1210.9900
N6—C61.3446 (15)C21—H2210.9900
N6—C21.3556 (15)C22—H1220.9900
N7—C241.4449 (16)C22—H2220.9900
N7—C221.4491 (16)C23—C241.5309 (19)
N7—C201.4528 (16)C23—H1230.9900
C1—C21.4747 (17)C23—H2230.9900
C1—H110.9500C24—H1240.9900
C2—C31.3816 (17)C24—H2240.9900
C3—C41.3921 (19)C30—H1300.9800
C3—H130.9500C30—H2300.9800
C4—C51.3753 (18)C30—H3300.9800
C4—H140.9500C31—H1310.9800
C5—C61.4014 (17)C31—H2310.9800
C5—H150.9500C31—H3310.9800
C6—C311.4980 (17)C32—H1320.9800
C7—C81.4756 (18)C32—H2320.9800
C7—H170.9500C32—H3320.9800
C8—C91.3872 (17)
N5—Zn1—N499.42 (4)C10—C11—C12120.19 (13)
N5—Zn1—N196.05 (4)C10—C11—H111119.9
N4—Zn1—N196.66 (4)C12—C11—H111119.9
N5—Zn1—N2170.83 (4)N2—C12—C11121.37 (12)
N4—Zn1—N286.87 (4)N2—C12—C32118.62 (11)
N1—Zn1—N276.48 (4)C11—C12—C32120.01 (12)
N5—Zn1—N385.28 (4)N4—C13—C14120.47 (11)
N4—Zn1—N376.36 (4)N4—C13—H113119.8
N1—Zn1—N3173.01 (4)C14—C13—H113119.8
N2—Zn1—N3102.78 (4)N3—C14—C15123.67 (12)
N5—Zn1—N676.19 (4)N3—C14—C13116.85 (10)
N4—Zn1—N6174.46 (4)C15—C14—C13119.36 (11)
N1—Zn1—N687.24 (4)C16—C15—C14118.27 (12)
N2—Zn1—N697.90 (3)C16—C15—H115120.9
N3—Zn1—N699.73 (4)C14—C15—H115120.9
O4—Cl1—O1110.15 (7)C17—C16—C15118.82 (11)
O4—Cl1—O3109.39 (6)C17—C16—H116120.6
O1—Cl1—O3109.22 (6)C15—C16—H116120.6
O4—Cl1—O2109.86 (6)C16—C17—C18120.26 (12)
O1—Cl1—O2109.27 (6)C16—C17—H117119.9
O3—Cl1—O2108.92 (6)C18—C17—H117119.9
O6—Cl2—O7110.73 (8)N3—C18—C17121.04 (12)
O6—Cl2—O5109.00 (10)N3—C18—C30119.10 (10)
O7—Cl2—O5108.61 (7)C17—C18—C30119.85 (11)
O6—Cl2—O8108.56 (7)N4—C19—C20108.01 (10)
O7—Cl2—O8111.23 (8)N4—C19—H119110.1
O5—Cl2—O8108.66 (9)C20—C19—H119110.1
C7—N1—C23118.87 (11)N4—C19—H219110.1
C7—N1—Zn1116.12 (9)C20—C19—H219110.1
C23—N1—Zn1124.93 (8)H119—C19—H219108.4
C12—N2—C8117.89 (10)N7—C20—C19111.06 (10)
C12—N2—Zn1132.51 (8)N7—C20—H120109.4
C8—N2—Zn1109.59 (8)C19—C20—H120109.4
C18—N3—C14117.81 (10)N7—C20—H220109.4
C18—N3—Zn1132.44 (8)C19—C20—H220109.4
C14—N3—Zn1109.10 (8)H120—C20—H220108.0
C13—N4—C19118.24 (10)N5—C21—C22108.84 (10)
C13—N4—Zn1116.87 (9)N5—C21—H121109.9
C19—N4—Zn1124.85 (8)C22—C21—H121109.9
C1—N5—C21118.64 (10)N5—C21—H221109.9
C1—N5—Zn1117.79 (8)C22—C21—H221109.9
C21—N5—Zn1123.56 (8)H121—C21—H221108.3
C6—N6—C2117.67 (10)N7—C22—C21112.13 (10)
C6—N6—Zn1133.77 (8)N7—C22—H122109.2
C2—N6—Zn1108.44 (7)C21—C22—H122109.2
C24—N7—C22117.93 (10)N7—C22—H222109.2
C24—N7—C20117.07 (10)C21—C22—H222109.2
C22—N7—C20117.54 (11)H122—C22—H222107.9
N5—C1—C2119.95 (11)N1—C23—C24109.86 (10)
N5—C1—H11120.0N1—C23—H123109.7
C2—C1—H11120.0C24—C23—H123109.7
N6—C2—C3123.52 (11)N1—C23—H223109.7
N6—C2—C1117.20 (10)C24—C23—H223109.7
C3—C2—C1119.26 (11)H123—C23—H223108.2
C2—C3—C4118.66 (12)N7—C24—C23111.99 (10)
C2—C3—H13120.7N7—C24—H124109.2
C4—C3—H13120.7C23—C24—H124109.2
C5—C4—C3118.26 (12)N7—C24—H224109.2
C5—C4—H14120.9C23—C24—H224109.2
C3—C4—H14120.9H124—C24—H224107.9
C4—C5—C6120.39 (12)C18—C30—H130109.5
C4—C5—H15119.8C18—C30—H230109.5
C6—C5—H15119.8H130—C30—H230109.5
N6—C6—C5121.48 (11)C18—C30—H330109.5
N6—C6—C31118.58 (10)H130—C30—H330109.5
C5—C6—C31119.92 (11)H230—C30—H330109.5
N1—C7—C8120.33 (11)C6—C31—H131109.5
N1—C7—H17119.8C6—C31—H231109.5
C8—C7—H17119.8H131—C31—H231109.5
N2—C8—C9123.25 (12)C6—C31—H331109.5
N2—C8—C7117.47 (10)H131—C31—H331109.5
C9—C8—C7119.27 (11)H231—C31—H331109.5
C10—C9—C8118.67 (13)C12—C32—H132109.5
C10—C9—H19120.7C12—C32—H232109.5
C8—C9—H19120.7H132—C32—H232109.5
C11—C10—C9118.59 (12)C12—C32—H332109.5
C11—C10—H110120.7H132—C32—H332109.5
C9—C10—H110120.7H232—C32—H332109.5
(1-Zn_130) top
Crystal data top
C27H33Cl2N7O8ZnZ = 4
Mr = 719.87F(000) = 1488
Monoclinic, P21/cDx = 1.579 Mg m3
a = 10.4189 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 19.2284 (5) ŵ = 1.05 mm1
c = 15.1216 (4) ÅT = 130 K
β = 91.726 (2)°Polyhedron, yellow
V = 3028.07 (14) Å30.32 × 0.26 × 0.12 mm
Data collection top
KM4_CCD_Sapphire3
diffractometer
10213 independent reflections
Radiation source: fine-focus sealed tube7555 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
Detector resolution: 16.0328 pixels mm-1θmax = 32.9°, θmin = 2.9°
θ–scanh = 1515
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
k = 2728
Tmin = 0.838, Tmax = 0.880l = 1222
29476 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.029Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.079H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.047P)2]
where P = (Fo2 + 2Fc2)/3
10213 reflections(Δ/σ)max = 0.003
409 parametersΔρmax = 0.72 e Å3
0 restraintsΔρmin = 0.58 e Å3
Crystal data top
C27H33Cl2N7O8ZnV = 3028.07 (14) Å3
Mr = 719.87Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.4189 (3) ŵ = 1.05 mm1
b = 19.2284 (5) ÅT = 130 K
c = 15.1216 (4) Å0.32 × 0.26 × 0.12 mm
β = 91.726 (2)°
Data collection top
KM4_CCD_Sapphire3
diffractometer
10213 independent reflections
Absorption correction: multi-scan
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
7555 reflections with I > 2σ(I)
Tmin = 0.838, Tmax = 0.880Rint = 0.023
29476 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0290 restraints
wR(F2) = 0.079H-atom parameters constrained
S = 1.00Δρmax = 0.72 e Å3
10213 reflectionsΔρmin = 0.58 e Å3
409 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Zn10.696547 (14)0.070396 (7)0.739563 (9)0.01699 (4)
Cl11.36244 (3)0.318225 (17)0.53835 (2)0.02520 (7)
Cl21.22258 (3)0.148792 (18)0.70021 (2)0.02725 (8)
N10.61826 (11)0.10036 (6)0.61307 (7)0.0224 (2)
N20.84429 (11)0.14844 (5)0.68854 (7)0.0204 (2)
N30.77071 (10)0.05050 (6)0.88232 (7)0.0200 (2)
N40.61993 (11)0.15344 (6)0.81141 (7)0.0211 (2)
N50.55943 (10)0.00617 (6)0.76509 (7)0.0203 (2)
N60.77493 (10)0.02875 (5)0.67074 (7)0.0187 (2)
N70.39687 (11)0.10701 (6)0.71846 (8)0.0254 (2)
O11.33655 (13)0.30491 (7)0.62950 (7)0.0441 (3)
O21.43823 (11)0.26185 (6)0.50404 (8)0.0379 (3)