Acta Crystallographica Section E
Acta Crystallographica
Section E CRYSTALLOGRAPHIC COMMUNICATIONS

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Bis[tris(2,2′-bipyridyl-κ²N,N′)iron(II)] cyclo-tetravanadate decahydrate

M.-H. Huang, L.-H. Bi and S.-J. Dong

The hydrothermal reactions of metavanadate and divalent iron salts in the presence of nitrogen-donor chelating ligands yield the complex [Fe(C₁₀H₈N₂)₃]₂[V₄O₁₂]·10H₂O, which consists of one centrosymmetric eight-membered ring [V₄O₁₂]⁴⁻ anion cluster, formed by four VO₄ tetrahedra sharing vertices, two discrete octahedral [Fe(C₁₀H₈N₂)₃]²⁺ cations, formed by three 2,2′-bipyridyl ligands coordinated to Fe^II, and ten water molecules of solvation. The anion and coordination cations are isolated and form anion and cation layers, respectively. In the anion layers, these anions and water molecules of solvation are linked to each other, in a two-dimensional motif, through hydrogen-bonding interactions.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803029532/om6193sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536803029532/om6193Isup2.hkl Contains datablock I

CCDC reference: 234791

checkCIF report

Key indicators

Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.010 Å
H-atom completeness 71%
Disorder in solvent or counterion
R factor = 0.074
wR factor = 0.211
Data-to-parameter ratio = 15.1

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        OW1

Author Response: Because the H-atoms are not located.

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        OW2

Author Response: Because the H-atoms are not located.

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        OW3

Author Response: Because the H-atoms are not located.

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        OW4

Author Response: Because the H-atoms are not located.

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        OW5

Author Response: Because the H-atoms are not located.


Alert level B
PLAT241_ALERT_2_B Check High   U(eq) as Compared to Neighbors ....         O4
PLAT242_ALERT_2_B Check Low    U(eq) as Compared to Neighbors ....         V1
PLAT242_ALERT_2_B Check Low    U(eq) as Compared to Neighbors ....         V2
PLAT430_ALERT_2_B Short Inter D...A Contact  OW1    ..  O2       =       2.70 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  OW1    ..  O2       =       2.70 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  OW2    ..  OW5      =       2.78 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  OW2    ..  OW2      =       2.82 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  OW3    ..  O6       =       2.72 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  OW4    ..  OW6      =       2.69 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  OW4    ..  OW4      =       2.81 Ang.

Alert level C
CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.99 <> 1.01
           From the CIF: _cell_formula_units_Z                    4
           From the CIF: _chemical_formula_weight          1624.72
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   60.00  720.66
           H         1.01   48.00   48.38
           N        14.01   12.00  168.08
           O        16.00   22.00  351.98
           V        50.94    4.00  203.77
           Fe       55.85    2.00  111.69
           Calculated formula weight             1604.57
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT043_ALERT_1_C Check Reported Molecular Weight ................    1624.72
PLAT044_ALERT_1_C Calculated and Reported Dx Differ ..............          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       0.50 Ratio
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor ....       2.29
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................       8.00 Perc.
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         10
PLAT430_ALERT_2_C Short Inter D...A Contact  OW4    ..  O5       =       2.89 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          6

Alert level G
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C60 H68 Fe2 N12 O22 V4
            Atom count from the _atom_site data:  C60 H48 Fe2 N12 O22 V4
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    4
           From the CIF: _chemical_formula_sum  C60 H68 Fe2 N12 O22 V4
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C        240.00    240.00    0.00
           H        272.00    192.00   80.00
           Fe         8.00      8.00    0.00
           N         48.00     48.00    0.00
           O         88.00     88.00    0.00
           V         16.00     16.00    0.00

   5 ALERT level A = In general: serious problem
  10 ALERT level B = Potentially serious problem
  13 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  19 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: XSCANS (Siemens, 1994); cell refinement: XSCANS; data reduction: SHELXTL (Siemens, 1994); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Bis[tris(2,2'-bipyridyl-κ²N,N')iron(II)] cyclo-tetravanadate decahydrate top

Crystal data top

[Fe(C₁₀H₈N₂)₃]₂[V₄O₁₂]·10H₂O	F(000) = 3328
M_r = 1624.72	D_x = 1.597 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 21.619 (3) Å	Cell parameters from 28 reflections
b = 13.656 (3) Å	θ = 5.2–11.2°
c = 23.517 (4) Å	µ = 1.03 mm⁻¹
β = 103.296 (14)°	T = 293 K
V = 6757 (2) Å³	Block, black–red
Z = 4	0.48 × 0.32 × 0.18 mm

Data collection top

Siemens P4 diffractometer	4004 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.030
Graphite monochromator	θ_max = 26.0°, θ_min = 1.8°
ω scans	h = −1→26
Absorption correction: ψ scan (SHELXTL; Siemens, 1994)	k = −1→16
T_min = 0.622, T_max = 0.830	l = −29→28
7943 measured reflections	3 standard reflections every 197 reflections
6634 independent reflections	intensity decay: none

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.074	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.211	H-atom parameters constrained
S = 1.07	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
6634 reflections	(Δ/σ)_max < 0.001
439 parameters	Δρ_max = 1.55 e Å⁻³
1 restraint	Δρ_min = −1.37 e Å⁻³

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Fe	0.17144 (4)	0.98323 (6)	0.27258 (3)	0.0317 (2)
V1	0.03685 (5)	0.45290 (8)	0.41920 (4)	0.0424 (3)
V2	0.05750 (6)	0.65404 (9)	0.49935 (5)	0.0547 (4)
O1	−0.0281 (2)	0.4029 (4)	0.4448 (2)	0.0661 (14)
O2	0.0232 (3)	0.4332 (5)	0.3489 (2)	0.0857 (13)
O3	0.1043 (2)	0.4024 (4)	0.4501 (2)	0.0700 (15)
O4	0.0395 (3)	0.5821 (4)	0.4335 (2)	0.0849 (13)
O5	0.0189 (3)	0.7593 (4)	0.4863 (2)	0.0849 (13)
O6	0.1337 (3)	0.6697 (5)	0.5217 (2)	0.0857 (13)
N1	0.2319 (2)	0.9328 (3)	0.22723 (19)	0.0358 (11)
N2	0.2503 (2)	1.0420 (3)	0.3192 (2)	0.0365 (11)
N3	0.0998 (2)	0.9093 (3)	0.22477 (19)	0.0349 (10)
N4	0.1798 (2)	0.8625 (3)	0.32018 (19)	0.0346 (11)
N5	0.1181 (2)	1.0503 (3)	0.31795 (19)	0.0351 (10)
N6	0.1520 (2)	1.1033 (3)	0.22506 (19)	0.0386 (11)
C1	0.2175 (3)	0.8798 (5)	0.1785 (3)	0.0504 (16)
H1	0.1764	0.8554	0.1665	0.050*
C2	0.2608 (4)	0.8592 (6)	0.1447 (3)	0.0605 (19)
H2	0.2496	0.8202	0.1115	0.061*
C3	0.3203 (3)	0.8983 (5)	0.1619 (3)	0.0599 (19)
H3	0.3497	0.8892	0.1390	0.060*
C4	0.3370 (3)	0.9511 (5)	0.2129 (3)	0.0522 (16)
H4	0.3779	0.9760	0.2256	0.052*
C5	0.2917 (3)	0.9664 (4)	0.2449 (3)	0.0384 (13)
C6	0.3034 (3)	1.0216 (4)	0.2995 (3)	0.0419 (14)
C7	0.3630 (3)	1.0494 (5)	0.3315 (3)	0.0525 (17)
H7	0.3989	1.0338	0.3179	0.053*
C8	0.3695 (3)	1.0989 (5)	0.3824 (3)	0.0601 (19)
H8	0.4096	1.1163	0.4042	0.060*
C9	0.3167 (3)	1.1227 (5)	0.4010 (3)	0.0555 (18)
H9	0.3198	1.1589	0.4350	0.056*
C10	0.2581 (3)	1.0926 (5)	0.3689 (3)	0.0486 (15)
H10	0.2222	1.1083	0.3825	0.049*
C11	0.0627 (3)	0.9355 (5)	0.1717 (3)	0.0467 (15)
H11	0.0651	0.9995	0.1589	0.047*
C12	0.0225 (3)	0.8721 (5)	0.1368 (3)	0.0469 (15)
H12	−0.0015	0.8926	0.1007	0.047*
C13	0.0177 (3)	0.7776 (6)	0.1554 (3)	0.0553 (18)
H13	−0.0089	0.7331	0.1317	0.055*
C14	0.0524 (3)	0.7497 (5)	0.2091 (3)	0.0497 (16)
H14	0.0487	0.6867	0.2229	0.050*
C15	0.0936 (3)	0.8172 (4)	0.2428 (2)	0.0372 (13)
C16	0.1361 (3)	0.7917 (4)	0.2986 (2)	0.0384 (13)
C17	0.1326 (3)	0.7061 (5)	0.3285 (3)	0.0521 (16)
H17	0.1033	0.6579	0.3126	0.052*
C18	0.1731 (4)	0.6930 (5)	0.3820 (3)	0.0607 (19)
H18	0.1704	0.6365	0.4033	0.061*
C19	0.2170 (3)	0.7617 (5)	0.4040 (3)	0.0583 (18)
H19	0.2450	0.7523	0.4400	0.058*
C20	0.2199 (3)	0.8472 (5)	0.3721 (3)	0.0498 (16)
H20	0.2502	0.8944	0.3872	0.050*
C21	0.1033 (3)	1.0187 (5)	0.3678 (3)	0.0466 (15)
H21	0.1161	0.9562	0.3813	0.047*
C22	0.0707 (3)	1.0745 (5)	0.3990 (3)	0.0540 (17)
H22	0.0613	1.0501	0.4330	0.054*
C23	0.0517 (3)	1.1666 (6)	0.3798 (3)	0.0591 (19)
H23	0.0295	1.2055	0.4008	0.059*
C24	0.0653 (3)	1.2006 (5)	0.3306 (3)	0.0552 (17)
H24	0.0529	1.2633	0.3174	0.055*
C25	0.0984 (3)	1.1408 (4)	0.2992 (3)	0.0376 (13)
C26	0.1159 (3)	1.1700 (4)	0.2447 (2)	0.0377 (13)
C27	0.0952 (3)	1.2559 (5)	0.2144 (3)	0.0531 (17)
H27	0.0708	1.3012	0.2292	0.053*
C28	0.1117 (4)	1.2725 (5)	0.1618 (3)	0.063 (2)
H28	0.0977	1.3286	0.1402	0.063*
C29	0.1480 (3)	1.2071 (5)	0.1422 (3)	0.0528 (17)
H29	0.1601	1.2179	0.1073	0.053*
C30	0.1674 (3)	1.1233 (5)	0.1743 (3)	0.0488 (16)
H30	0.1924	1.0785	0.1599	0.049*
OW1	0.0000	0.5410 (5)	0.2500	0.0624 (18)
OW2	0.1874 (3)	0.2310 (5)	0.4682 (3)	0.099 (2)
OW3	0.2147 (4)	0.5325 (6)	0.4971 (3)	0.127 (3)
OW4	0.0536 (4)	0.9523 (6)	0.5337 (4)	0.132 (3)
OW5	0.1135 (5)	0.1647 (8)	0.5429 (4)	0.172 (4)
OW6	0.1540 (7)	0.8919 (13)	0.4932 (7)	0.133 (5)*	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe	0.0299 (4)	0.0341 (4)	0.0317 (4)	−0.0001 (3)	0.0082 (3)	0.0042 (3)
V1	0.0473 (6)	0.0531 (7)	0.0274 (5)	0.0037 (5)	0.0099 (4)	−0.0040 (4)
V2	0.0772 (9)	0.0534 (7)	0.0342 (6)	−0.0136 (6)	0.0146 (5)	−0.0091 (5)
O1	0.072 (3)	0.080 (4)	0.052 (3)	−0.029 (3)	0.027 (2)	−0.017 (3)
O2	0.093 (3)	0.119 (3)	0.046 (2)	−0.029 (3)	0.0180 (19)	−0.032 (2)
O3	0.055 (3)	0.090 (4)	0.062 (3)	0.020 (3)	0.008 (2)	0.008 (3)
O4	0.145 (4)	0.060 (2)	0.0478 (19)	0.004 (2)	0.018 (2)	−0.0013 (17)
O5	0.145 (4)	0.060 (2)	0.0478 (19)	0.004 (2)	0.018 (2)	−0.0013 (17)
O6	0.093 (3)	0.119 (3)	0.046 (2)	−0.029 (3)	0.0180 (19)	−0.032 (2)
N1	0.038 (3)	0.036 (3)	0.036 (2)	0.001 (2)	0.014 (2)	0.002 (2)
N2	0.037 (2)	0.036 (3)	0.036 (2)	0.000 (2)	0.007 (2)	0.002 (2)
N3	0.030 (2)	0.039 (3)	0.035 (2)	0.001 (2)	0.0049 (19)	−0.002 (2)
N4	0.037 (2)	0.032 (3)	0.035 (2)	0.004 (2)	0.010 (2)	0.0096 (19)
N5	0.031 (2)	0.037 (3)	0.037 (2)	−0.001 (2)	0.009 (2)	0.001 (2)
N6	0.038 (3)	0.042 (3)	0.034 (2)	−0.005 (2)	0.004 (2)	0.006 (2)
C1	0.055 (4)	0.051 (4)	0.051 (4)	−0.006 (3)	0.022 (3)	0.001 (3)
C2	0.066 (5)	0.068 (5)	0.056 (4)	−0.002 (4)	0.031 (4)	−0.010 (4)
C3	0.064 (5)	0.063 (5)	0.066 (4)	0.003 (4)	0.042 (4)	0.003 (4)
C4	0.044 (4)	0.053 (4)	0.065 (4)	0.001 (3)	0.022 (3)	0.011 (3)
C5	0.039 (3)	0.035 (3)	0.045 (3)	0.007 (3)	0.017 (3)	0.004 (3)
C6	0.036 (3)	0.039 (3)	0.051 (3)	0.000 (3)	0.011 (3)	0.014 (3)
C7	0.034 (3)	0.060 (4)	0.062 (4)	−0.006 (3)	0.007 (3)	−0.001 (3)
C8	0.040 (4)	0.065 (5)	0.068 (5)	−0.016 (3)	−0.003 (3)	−0.005 (4)
C9	0.061 (4)	0.053 (4)	0.046 (4)	−0.015 (4)	−0.001 (3)	−0.007 (3)
C10	0.050 (4)	0.048 (4)	0.048 (4)	−0.007 (3)	0.012 (3)	−0.001 (3)
C11	0.043 (3)	0.046 (4)	0.049 (4)	0.004 (3)	0.007 (3)	0.005 (3)
C12	0.037 (3)	0.057 (4)	0.041 (3)	−0.001 (3)	−0.001 (3)	−0.006 (3)
C13	0.043 (4)	0.071 (5)	0.049 (4)	−0.010 (3)	0.004 (3)	−0.020 (4)
C14	0.055 (4)	0.041 (4)	0.057 (4)	−0.011 (3)	0.021 (3)	−0.006 (3)
C15	0.036 (3)	0.038 (3)	0.042 (3)	−0.004 (3)	0.017 (2)	−0.003 (3)
C16	0.043 (3)	0.035 (3)	0.041 (3)	0.003 (3)	0.018 (3)	0.002 (3)
C17	0.060 (4)	0.037 (4)	0.059 (4)	−0.005 (3)	0.015 (3)	0.012 (3)
C18	0.075 (5)	0.049 (4)	0.065 (4)	0.009 (4)	0.031 (4)	0.026 (4)
C19	0.058 (4)	0.059 (4)	0.053 (4)	0.004 (4)	0.002 (3)	0.020 (3)
C20	0.043 (3)	0.066 (4)	0.038 (3)	0.003 (3)	0.005 (3)	0.010 (3)
C21	0.051 (4)	0.046 (4)	0.046 (3)	0.000 (3)	0.019 (3)	−0.003 (3)
C22	0.049 (4)	0.066 (5)	0.053 (4)	−0.007 (4)	0.025 (3)	−0.009 (3)
C23	0.052 (4)	0.064 (5)	0.068 (5)	0.002 (4)	0.027 (4)	−0.021 (4)
C24	0.045 (4)	0.051 (4)	0.069 (5)	0.010 (3)	0.013 (3)	−0.007 (3)
C25	0.031 (3)	0.033 (3)	0.045 (3)	−0.001 (2)	0.000 (2)	−0.006 (3)
C26	0.037 (3)	0.032 (3)	0.041 (3)	0.002 (3)	0.000 (2)	0.002 (2)
C27	0.051 (4)	0.038 (4)	0.064 (4)	0.005 (3)	0.000 (3)	0.006 (3)
C28	0.073 (5)	0.047 (4)	0.053 (4)	−0.006 (4)	−0.017 (4)	0.023 (3)
C29	0.057 (4)	0.052 (4)	0.045 (4)	−0.013 (3)	0.003 (3)	0.014 (3)
C30	0.052 (4)	0.049 (4)	0.049 (4)	−0.001 (3)	0.021 (3)	0.017 (3)
OW1	0.075 (5)	0.047 (4)	0.064 (4)	0.000	0.013 (4)	0.000
OW2	0.078 (4)	0.122 (5)	0.095 (4)	−0.012 (4)	0.019 (3)	−0.019 (4)
OW3	0.120 (6)	0.154 (7)	0.096 (5)	−0.016 (5)	−0.002 (4)	0.050 (5)
OW4	0.141 (7)	0.115 (6)	0.156 (7)	0.037 (5)	0.064 (6)	0.038 (5)
OW5	0.175 (9)	0.233 (11)	0.118 (7)	−0.038 (8)	0.055 (6)	−0.042 (7)

Geometric parameters (Å, º) top

Fe—N5	1.968 (5)	C8—C9	1.354 (10)
Fe—N3	1.971 (4)	C8—H8	0.9300
Fe—N2	1.973 (5)	C9—C10	1.380 (8)
Fe—N4	1.978 (4)	C9—H9	0.9300
Fe—N6	1.975 (5)	C10—H10	0.9300
Fe—N1	1.990 (5)	C11—C12	1.359 (8)
V1—O3	1.626 (5)	C11—H11	0.9300
V1—O2	1.633 (5)	C12—C13	1.375 (10)
V1—O1	1.786 (5)	C12—H12	0.9300
V1—O4	1.794 (5)	C13—C14	1.365 (9)
V2—O6	1.625 (6)	C13—H13	0.9300
V2—O5	1.656 (6)	C14—C15	1.396 (8)
V2—O1ⁱ	1.765 (5)	C14—H14	0.9300
V2—O4	1.799 (5)	C15—C16	1.460 (8)
O1—V2ⁱ	1.765 (5)	C16—C17	1.375 (8)
N1—C1	1.330 (8)	C17—C18	1.370 (9)
N1—C5	1.345 (7)	C17—H17	0.9300
N2—C10	1.334 (7)	C18—C19	1.350 (10)
N2—C6	1.363 (7)	C18—H18	0.9300
N3—C15	1.344 (7)	C19—C20	1.396 (9)
N3—C11	1.366 (7)	C19—H19	0.9300
N4—C20	1.342 (7)	C20—H20	0.9300
N4—C16	1.365 (7)	C21—C22	1.362 (9)
N5—C21	1.355 (7)	C21—H21	0.9300
N5—C25	1.347 (7)	C22—C23	1.367 (10)
N6—C30	1.339 (7)	C22—H22	0.9300
N6—C26	1.347 (7)	C23—C24	1.341 (9)
C1—C2	1.390 (9)	C23—H23	0.9300
C1—H1	0.9300	C24—C25	1.402 (8)
C2—C3	1.366 (10)	C24—H24	0.9300
C2—H2	0.9300	C25—C26	1.473 (8)
C3—C4	1.376 (10)	C26—C27	1.392 (8)
C3—H3	0.9300	C27—C28	1.382 (9)
C4—C5	1.382 (8)	C27—H27	0.9300
C4—H4	0.9300	C28—C29	1.339 (10)
C5—C6	1.459 (9)	C28—H28	0.9300
C6—C7	1.388 (8)	C29—C30	1.381 (9)
C7—C8	1.353 (9)	C29—H29	0.9300
C7—H7	0.9300	C30—H30	0.9300

N5—Fe—N3	93.80 (19)	C7—C8—H8	120.6
N5—Fe—N2	92.76 (19)	C9—C8—H8	120.6
N3—Fe—N2	172.33 (19)	C8—C9—C10	119.3 (6)
N5—Fe—N4	94.00 (19)	C8—C9—H9	120.4
N3—Fe—N4	81.54 (19)	C10—C9—H9	120.4
N2—Fe—N4	94.03 (18)	N2—C10—C9	123.3 (6)
N5—Fe—N6	81.07 (19)	N2—C10—H10	118.4
N3—Fe—N6	93.76 (19)	C9—C10—H10	118.4
N2—Fe—N6	91.19 (19)	N3—C11—C12	122.9 (6)
N4—Fe—N6	172.99 (19)	N3—C11—H11	118.5
N5—Fe—N1	172.07 (19)	C12—C11—H11	118.5
N3—Fe—N1	92.51 (19)	C11—C12—C13	119.4 (6)
N2—Fe—N1	81.3 (2)	C11—C12—H12	120.3
N4—Fe—N1	91.68 (19)	C13—C12—H12	120.3
N6—Fe—N1	93.73 (19)	C14—C13—C12	119.3 (6)
O3—V1—O2	108.5 (3)	C14—C13—H13	120.3
O3—V1—O1	112.4 (3)	C12—C13—H13	120.3
O2—V1—O1	107.7 (3)	C13—C14—C15	119.0 (6)
O3—V1—O4	110.2 (3)	C13—C14—H14	120.5
O2—V1—O4	110.1 (3)	C15—C14—H14	120.5
O1—V1—O4	107.8 (3)	N3—C15—C14	122.4 (5)
O6—V2—O5	112.1 (3)	N3—C15—C16	114.8 (5)
O6—V2—O1ⁱ	109.2 (3)	C14—C15—C16	122.8 (5)
O5—V2—O1ⁱ	105.5 (3)	N4—C16—C17	121.7 (5)
O6—V2—O4	110.7 (3)	N4—C16—C15	113.8 (5)
O5—V2—O4	108.4 (3)	C17—C16—C15	124.4 (6)
O1ⁱ—V2—O4	110.8 (2)	C16—C17—C18	118.8 (6)
V2ⁱ—O1—V1	149.8 (3)	C16—C17—H17	120.6
V1—O4—V2	133.6 (3)	C18—C17—H17	120.6
C1—N1—C5	118.0 (5)	C19—C18—C17	120.3 (6)
C1—N1—Fe	126.7 (4)	C19—C18—H18	119.8
C5—N1—Fe	114.8 (4)	C17—C18—H18	119.8
C10—N2—C6	117.3 (5)	C18—C19—C20	119.4 (6)
C10—N2—Fe	128.0 (4)	C18—C19—H19	120.3
C6—N2—Fe	114.6 (4)	C20—C19—H19	120.3
C15—N3—C11	117.0 (5)	N4—C20—C19	121.3 (6)
C15—N3—Fe	114.9 (4)	N4—C20—H20	119.4
C11—N3—Fe	127.3 (4)	C19—C20—H20	119.4
C20—N4—C16	118.4 (5)	N5—C21—C22	122.8 (6)
C20—N4—Fe	126.9 (4)	N5—C21—H21	118.6
C16—N4—Fe	114.5 (3)	C22—C21—H21	118.6
C21—N5—C25	117.1 (5)	C21—C22—C23	119.4 (7)
C21—N5—Fe	127.2 (4)	C21—C22—H22	120.3
C25—N5—Fe	115.5 (4)	C23—C22—H22	120.3
C30—N6—C26	116.7 (5)	C24—C23—C22	119.6 (7)
C30—N6—Fe	127.5 (4)	C24—C23—H23	120.2
C26—N6—Fe	115.6 (4)	C22—C23—H23	120.2
N1—C1—C2	123.2 (6)	C23—C24—C25	119.6 (7)
N1—C1—H1	118.4	C23—C24—H24	120.2
C2—C1—H1	118.4	C25—C24—H24	120.2
C3—C2—C1	117.7 (7)	N5—C25—C24	121.5 (6)
C3—C2—H2	121.2	N5—C25—C26	114.0 (5)
C1—C2—H2	121.2	C24—C25—C26	124.4 (5)
C4—C3—C2	120.2 (6)	N6—C26—C27	122.5 (6)
C4—C3—H3	119.9	N6—C26—C25	113.6 (5)
C2—C3—H3	119.9	C27—C26—C25	123.9 (6)
C3—C4—C5	118.5 (6)	C28—C27—C26	118.6 (7)
C3—C4—H4	120.7	C28—C27—H27	120.7
C5—C4—H4	120.7	C26—C27—H27	120.7
N1—C5—C4	122.1 (6)	C29—C28—C27	119.3 (6)
N1—C5—C6	114.1 (5)	C29—C28—H28	120.4
C4—C5—C6	123.7 (6)	C27—C28—H28	120.4
N2—C6—C7	120.6 (6)	C28—C29—C30	119.6 (6)
N2—C6—C5	114.5 (5)	C28—C29—H29	120.2
C7—C6—C5	124.8 (6)	C30—C29—H29	120.2
C8—C7—C6	120.8 (6)	N6—C30—C29	123.3 (7)
C8—C7—H7	119.6	N6—C30—H30	118.4
C6—C7—H7	119.6	C29—C30—H30	118.4
C7—C8—C9	118.8 (6)

Symmetry code: (i) −x, −y+1, −z+1.

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