Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806053712/bi2108sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806053712/bi2108Isup2.hkl |
CCDC reference: 608578
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.007 Å
- Disorder in main residue
- R factor = 0.060
- wR factor = 0.167
- Data-to-parameter ratio = 12.2
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for O1'
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for O2'
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for C28'
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
PLAT242_ALERT_2_A Check Low Ueq as Compared to Neighbors for S1
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
PLAT242_ALERT_2_A Check Low Ueq as Compared to Neighbors for O2
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
PLAT242_ALERT_2_A Check Low Ueq as Compared to Neighbors for O3
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
Alert level B PLAT220_ALERT_2_B Large Non-Solvent O Ueq(max)/Ueq(min) ... 4.41 Ratio PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.21 Ratio
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) . 300 Ang. PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.52 Ratio PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.32 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C12
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for S1'
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C23'
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C24'
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N4
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C22
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C22'
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C24
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C25
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C27
Author Response: The atom is part of a disordered methylbenzylsulfonate anion. |
PLAT245_ALERT_2_C U(iso) H24A Smaller than U(eq) C24' by ... 0.01 AngSq PLAT301_ALERT_3_C Main Residue Disorder ......................... 5.00 Perc. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O1 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C7 PLAT412_ALERT_2_C Short Intra XH3 .. XHn H4B .. H21A .. 1.87 Ang.
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C56 H66 Mn1 N12 O8 S2 Atom count from _chemical_formula_moiety:C322 H328 Mn1 N12 O120 S40 PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
6 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 21 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 22 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: SMART-NT (Bruker, 1998); cell refinement: SAINT-NT (Bruker, 1998; data reduction: SAINT-NT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-NT (Bruker, 1998; software used to prepare material for publication: SHELXTL-NT.
[Mn(C21H24N6)2](C7H7O3S)2·2H2O | Z = 1 |
Mr = 1154.27 | F(000) = 607 |
Triclinic, P1 | Dx = 1.380 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.481 (3) Å | Cell parameters from 1774 reflections |
b = 11.635 (3) Å | θ = 2.2–22.0° |
c = 13.170 (3) Å | µ = 0.38 mm−1 |
α = 64.764 (4)° | T = 293 K |
β = 88.190 (5)° | Block, colourless |
γ = 63.025 (4)° | 0.30 × 0.20 × 0.18 mm |
V = 1389.4 (6) Å3 |
Bruker SMART 1000 CCD diffractometer | 4878 independent reflections |
Radiation source: fine-focus sealed tube | 2988 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
φ and ω scans | θmax = 25.0°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→12 |
Tmin = 0.890, Tmax = 0.932 | k = −13→12 |
7123 measured reflections | l = −15→8 |
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)] = 0.060 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.167 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0717P)2 + 0.9438P] where P = (Fo2 + 2Fc2)/3 |
4878 reflections | (Δ/σ)max = 0.004 |
399 parameters | Δρmax = 0.70 e Å−3 |
87 restraints | Δρmin = −0.47 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Mn1 | 0.0000 | 0.0000 | 0.5000 | 0.0367 (3) | |
N1 | 0.0658 (3) | 0.0837 (3) | 0.6064 (3) | 0.0441 (8) | |
N2 | 0.1547 (3) | 0.1100 (3) | 0.7366 (3) | 0.0408 (8) | |
N3 | 0.7507 (3) | −0.0745 (4) | 0.7583 (3) | 0.0469 (9) | |
N4 | 0.8702 (3) | −0.0598 (3) | 0.6230 (3) | 0.0451 (8) | |
N5 | 0.3172 (3) | 0.5451 (3) | 0.7156 (3) | 0.0440 (8) | |
N6 | 0.1761 (3) | 0.7714 (3) | 0.5897 (3) | 0.0436 (8) | |
C1 | 0.1298 (4) | 0.0207 (4) | 0.7128 (3) | 0.0427 (10) | |
H1A | 0.1550 | −0.0749 | 0.7655 | 0.051* | |
C2 | 0.0485 (5) | 0.2231 (5) | 0.5604 (4) | 0.0551 (12) | |
H2A | 0.0051 | 0.2954 | 0.4859 | 0.066* | |
C3 | 0.1035 (5) | 0.2396 (5) | 0.6389 (4) | 0.0555 (12) | |
H3A | 0.1060 | 0.3226 | 0.6284 | 0.067* | |
C4 | 0.2144 (4) | 0.0778 (4) | 0.8493 (3) | 0.0423 (10) | |
H4A | 0.2476 | −0.0244 | 0.9016 | 0.051* | |
H4B | 0.1458 | 0.1340 | 0.8795 | 0.051* | |
C5 | 0.3282 (4) | 0.1122 (4) | 0.8443 (3) | 0.0368 (9) | |
C6 | 0.4580 (4) | 0.0063 (4) | 0.8528 (3) | 0.0363 (9) | |
C7 | 0.4800 (5) | −0.1384 (4) | 0.8655 (4) | 0.0520 (11) | |
H7A | 0.4282 | −0.1222 | 0.8003 | 0.078* | |
H7B | 0.4530 | −0.1853 | 0.9339 | 0.078* | |
H7C | 0.5729 | −0.1992 | 0.8705 | 0.078* | |
C8 | 0.5630 (4) | 0.0368 (4) | 0.8480 (3) | 0.0378 (9) | |
C9 | 0.7065 (4) | −0.0800 (4) | 0.8660 (3) | 0.0483 (11) | |
H9A | 0.7655 | −0.0689 | 0.9077 | 0.058* | |
H9B | 0.7143 | −0.1749 | 0.9129 | 0.058* | |
C10 | 0.8543 (4) | −0.0579 (4) | 0.7212 (3) | 0.0466 (10) | |
H10A | 0.9098 | −0.0460 | 0.7613 | 0.056* | |
C11 | 0.7678 (6) | −0.0782 (7) | 0.5954 (5) | 0.0828 (17) | |
H11A | 0.7517 | −0.0839 | 0.5294 | 0.099* | |
C12 | 0.6944 (6) | −0.0866 (7) | 0.6764 (5) | 0.092 (2) | |
H12A | 0.6195 | −0.0984 | 0.6768 | 0.110* | |
C13 | 0.5390 (4) | 0.1741 (4) | 0.8317 (3) | 0.0401 (9) | |
C14 | 0.6516 (5) | 0.2110 (5) | 0.8158 (4) | 0.0618 (13) | |
H14A | 0.6165 | 0.3125 | 0.7638 | 0.093* | |
H14B | 0.7167 | 0.1539 | 0.7851 | 0.093* | |
H14C | 0.6928 | 0.1899 | 0.8884 | 0.093* | |
C15 | 0.4111 (4) | 0.2757 (4) | 0.8288 (3) | 0.0389 (9) | |
C16 | 0.3882 (5) | 0.4162 (4) | 0.8276 (3) | 0.0483 (11) | |
H16A | 0.3370 | 0.4305 | 0.8853 | 0.058* | |
H16B | 0.4738 | 0.4066 | 0.8479 | 0.058* | |
C17 | 0.2156 (4) | 0.6738 (4) | 0.6983 (3) | 0.0454 (10) | |
H17A | 0.1773 | 0.6921 | 0.7568 | 0.055* | |
C18 | 0.2598 (4) | 0.6984 (4) | 0.5343 (4) | 0.0541 (12) | |
H18A | 0.2570 | 0.7390 | 0.4558 | 0.065* | |
C19 | 0.3450 (5) | 0.5610 (5) | 0.6100 (4) | 0.0552 (12) | |
H19A | 0.4105 | 0.4900 | 0.5940 | 0.066* | |
C20 | 0.3046 (4) | 0.2461 (4) | 0.8349 (3) | 0.0406 (9) | |
C21 | 0.1655 (4) | 0.3611 (5) | 0.8293 (4) | 0.0572 (12) | |
H21A | 0.1124 | 0.3154 | 0.8621 | 0.086* | |
H21B | 0.1242 | 0.4317 | 0.7509 | 0.086* | |
H21C | 0.1725 | 0.4083 | 0.8716 | 0.086* | |
S1 | 0.1668 (4) | 0.6824 (5) | 0.0014 (3) | 0.0636 (11) | 0.50 |
O1 | 0.1382 (9) | 0.6071 (9) | −0.0461 (7) | 0.080 (3) | 0.50 |
O2 | 0.2580 (7) | 0.7278 (7) | −0.0455 (6) | 0.071 (2) | 0.50 |
O3 | 0.0442 (6) | 0.7976 (9) | 0.0000 (7) | 0.095 (3) | 0.50 |
C22 | 0.2368 (10) | 0.5705 (11) | 0.1482 (6) | 0.046 (2)* | 0.50 |
C23 | 0.1726 (10) | 0.5962 (12) | 0.2306 (7) | 0.055 (3)* | 0.50 |
H23A | 0.0893 | 0.6782 | 0.2093 | 0.066* | 0.50 |
C24 | 0.2280 (10) | 0.5040 (13) | 0.3447 (7) | 0.059 (3)* | 0.50 |
H24A | 0.1829 | 0.5264 | 0.3992 | 0.071* | 0.50 |
C25 | 0.3489 (12) | 0.3791 (14) | 0.3799 (10) | 0.060 (4)* | 0.50 |
C26 | 0.4200 (11) | 0.3581 (12) | 0.2962 (8) | 0.063 (3)* | 0.50 |
H26A | 0.5059 | 0.2798 | 0.3181 | 0.075* | 0.50 |
C27 | 0.3655 (10) | 0.4513 (10) | 0.1813 (7) | 0.044 (2)* | 0.50 |
H27A | 0.4137 | 0.4351 | 0.1262 | 0.052* | 0.50 |
C28 | 0.4065 (16) | 0.2743 (19) | 0.5080 (11) | 0.098 (7)* | 0.50 |
H28A | 0.4926 | 0.1955 | 0.5174 | 0.148* | 0.50 |
H28B | 0.3479 | 0.2365 | 0.5407 | 0.148* | 0.50 |
H28C | 0.4151 | 0.3253 | 0.5459 | 0.148* | 0.50 |
O11 | 0.0746 (9) | 0.3892 (9) | 0.0925 (8) | 0.121 (3) | 0.50 |
H111 | 0.1052 | 0.4310 | 0.0375 | 0.182* | 0.50 |
H112 | 0.0080 | 0.3905 | 0.0645 | 0.182* | 0.50 |
S1' | 0.2369 (7) | 0.6208 (6) | 0.0231 (4) | 0.129 (3) | 0.50 |
O1' | 0.1178 (14) | 0.7539 (14) | 0.0021 (18) | 0.310 (15) | 0.50 |
O2' | 0.3364 (14) | 0.6464 (17) | −0.0284 (12) | 0.223 (8) | 0.50 |
O3' | 0.2025 (10) | 0.5372 (10) | −0.0114 (8) | 0.092 (3) | 0.50 |
C22' | 0.2915 (11) | 0.5135 (12) | 0.1719 (7) | 0.051 (3)* | 0.50 |
C23' | 0.2071 (12) | 0.5380 (15) | 0.2454 (8) | 0.089 (5)* | 0.50 |
H23B | 0.1197 | 0.6138 | 0.2162 | 0.107* | 0.50 |
C24' | 0.2507 (12) | 0.4516 (15) | 0.3622 (9) | 0.086 (5)* | 0.50 |
H24B | 0.1924 | 0.4692 | 0.4111 | 0.103* | 0.50 |
C25' | 0.3790 (14) | 0.3402 (17) | 0.4066 (10) | 0.084 (6)* | 0.50 |
C26' | 0.4646 (12) | 0.3126 (13) | 0.3347 (10) | 0.076 (4)* | 0.50 |
H26B | 0.5511 | 0.2348 | 0.3646 | 0.092* | 0.50 |
C27' | 0.4228 (11) | 0.3993 (11) | 0.2194 (8) | 0.054 (3)* | 0.50 |
H27B | 0.4825 | 0.3824 | 0.1713 | 0.065* | 0.50 |
C28' | 0.428 (2) | 0.240 (2) | 0.5356 (12) | 0.146 (11)* | 0.50 |
H28D | 0.5191 | 0.1657 | 0.5501 | 0.219* | 0.50 |
H28E | 0.3735 | 0.1952 | 0.5636 | 0.219* | 0.50 |
H28F | 0.4236 | 0.2954 | 0.5739 | 0.219* | 0.50 |
O12 | 0.0408 (9) | 0.9912 (11) | 0.0824 (9) | 0.127 (3) | 0.50 |
H121 | 0.0216 | 1.0720 | 0.0247 | 0.191* | 0.50 |
H122 | 0.0069 | 0.9493 | 0.0644 | 0.191* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0448 (6) | 0.0387 (5) | 0.0333 (5) | −0.0230 (4) | 0.0097 (4) | −0.0193 (4) |
N1 | 0.056 (2) | 0.047 (2) | 0.042 (2) | −0.0313 (18) | 0.0110 (17) | −0.0240 (17) |
N2 | 0.055 (2) | 0.0446 (19) | 0.0346 (18) | −0.0327 (18) | 0.0076 (15) | −0.0188 (16) |
N3 | 0.052 (2) | 0.057 (2) | 0.044 (2) | −0.0316 (19) | 0.0177 (17) | −0.0282 (17) |
N4 | 0.049 (2) | 0.052 (2) | 0.043 (2) | −0.0284 (18) | 0.0165 (16) | −0.0250 (17) |
N5 | 0.058 (2) | 0.0337 (18) | 0.0382 (19) | −0.0228 (18) | 0.0052 (16) | −0.0144 (15) |
N6 | 0.048 (2) | 0.0404 (19) | 0.041 (2) | −0.0212 (17) | 0.0065 (16) | −0.0180 (17) |
C1 | 0.052 (3) | 0.042 (2) | 0.043 (2) | −0.028 (2) | 0.010 (2) | −0.0206 (19) |
C2 | 0.072 (3) | 0.049 (3) | 0.044 (3) | −0.032 (2) | 0.001 (2) | −0.018 (2) |
C3 | 0.077 (3) | 0.044 (3) | 0.051 (3) | −0.033 (2) | 0.004 (2) | −0.021 (2) |
C4 | 0.054 (3) | 0.051 (2) | 0.039 (2) | −0.033 (2) | 0.0159 (19) | −0.0263 (19) |
C5 | 0.048 (3) | 0.042 (2) | 0.029 (2) | −0.028 (2) | 0.0089 (17) | −0.0175 (17) |
C6 | 0.053 (3) | 0.036 (2) | 0.030 (2) | −0.028 (2) | 0.0110 (17) | −0.0163 (17) |
C7 | 0.067 (3) | 0.047 (2) | 0.061 (3) | −0.036 (2) | 0.024 (2) | −0.031 (2) |
C8 | 0.049 (3) | 0.043 (2) | 0.027 (2) | −0.026 (2) | 0.0108 (17) | −0.0168 (17) |
C9 | 0.058 (3) | 0.051 (2) | 0.036 (2) | −0.029 (2) | 0.014 (2) | −0.019 (2) |
C10 | 0.051 (3) | 0.059 (3) | 0.042 (2) | −0.034 (2) | 0.014 (2) | −0.026 (2) |
C11 | 0.095 (4) | 0.146 (5) | 0.076 (4) | −0.085 (4) | 0.048 (3) | −0.082 (4) |
C12 | 0.099 (4) | 0.180 (7) | 0.096 (4) | −0.110 (5) | 0.062 (4) | −0.103 (5) |
C13 | 0.055 (3) | 0.045 (2) | 0.035 (2) | −0.035 (2) | 0.0116 (18) | −0.0198 (18) |
C14 | 0.070 (3) | 0.066 (3) | 0.069 (3) | −0.046 (3) | 0.020 (3) | −0.034 (3) |
C15 | 0.056 (3) | 0.039 (2) | 0.033 (2) | −0.030 (2) | 0.0087 (18) | −0.0175 (17) |
C16 | 0.069 (3) | 0.036 (2) | 0.038 (2) | −0.027 (2) | −0.002 (2) | −0.0142 (18) |
C17 | 0.060 (3) | 0.039 (2) | 0.043 (2) | −0.025 (2) | 0.011 (2) | −0.022 (2) |
C18 | 0.060 (3) | 0.047 (3) | 0.040 (2) | −0.017 (2) | 0.011 (2) | −0.018 (2) |
C19 | 0.060 (3) | 0.043 (3) | 0.051 (3) | −0.016 (2) | 0.016 (2) | −0.023 (2) |
C20 | 0.051 (3) | 0.040 (2) | 0.033 (2) | −0.023 (2) | 0.0074 (18) | −0.0181 (18) |
C21 | 0.058 (3) | 0.053 (3) | 0.066 (3) | −0.025 (2) | 0.009 (2) | −0.034 (2) |
S1 | 0.079 (3) | 0.093 (3) | 0.0514 (19) | −0.061 (2) | 0.0253 (18) | −0.0412 (19) |
O1 | 0.112 (7) | 0.095 (6) | 0.057 (5) | −0.068 (5) | 0.008 (4) | −0.034 (4) |
O2 | 0.073 (5) | 0.060 (4) | 0.069 (4) | −0.055 (4) | 0.011 (3) | 0.002 (3) |
O3 | 0.063 (5) | 0.153 (7) | 0.073 (5) | −0.039 (4) | 0.020 (4) | −0.072 (5) |
O11 | 0.120 (6) | 0.095 (5) | 0.137 (7) | −0.046 (5) | 0.020 (5) | −0.051 (5) |
S1' | 0.185 (7) | 0.109 (4) | 0.115 (4) | −0.075 (4) | −0.018 (4) | −0.062 (3) |
O1' | 0.335 (18) | 0.296 (17) | 0.280 (17) | −0.110 (11) | 0.046 (10) | −0.166 (12) |
O2' | 0.226 (11) | 0.269 (12) | 0.207 (12) | −0.187 (10) | 0.034 (8) | −0.066 (8) |
O3' | 0.104 (7) | 0.118 (7) | 0.077 (6) | −0.057 (5) | 0.010 (5) | −0.061 (5) |
O12 | 0.100 (6) | 0.146 (7) | 0.142 (7) | −0.040 (5) | 0.010 (5) | −0.092 (6) |
Mn1—N6i | 2.270 (3) | C15—C16 | 1.526 (5) |
Mn1—N6ii | 2.270 (3) | C16—H16A | 0.970 |
Mn1—N4iii | 2.271 (3) | C16—H16B | 0.970 |
Mn1—N4iv | 2.271 (3) | C17—H17A | 0.930 |
Mn1—N1v | 2.319 (3) | C18—C19 | 1.338 (6) |
Mn1—N1 | 2.319 (3) | C18—H18A | 0.930 |
N1—C1 | 1.320 (5) | C19—H19A | 0.930 |
N1—C2 | 1.384 (5) | C20—C21 | 1.527 (6) |
N2—C1 | 1.347 (5) | C21—H21A | 0.960 |
N2—C3 | 1.365 (5) | C21—H21B | 0.960 |
N2—C4 | 1.472 (5) | C21—H21C | 0.960 |
N3—C10 | 1.336 (5) | S1—O2 | 1.393 (5) |
N3—C12 | 1.363 (6) | S1—O1 | 1.417 (6) |
N3—C9 | 1.476 (5) | S1—O3 | 1.431 (6) |
N4—C10 | 1.309 (5) | S1—C22 | 1.756 (8) |
N4—C11 | 1.371 (6) | C22—C23 | 1.355 (9) |
N4—Mn1vi | 2.271 (3) | C22—C27 | 1.400 (12) |
N5—C17 | 1.340 (5) | C23—C24 | 1.371 (10) |
N5—C19 | 1.370 (5) | C23—H23A | 0.930 |
N5—C16 | 1.474 (5) | C24—C25 | 1.375 (13) |
N6—C17 | 1.316 (5) | C24—H24A | 0.930 |
N6—C18 | 1.386 (5) | C25—C26 | 1.390 (9) |
N6—Mn1vii | 2.270 (3) | C25—C28 | 1.534 (14) |
C1—H1A | 0.930 | C26—C27 | 1.380 (12) |
C2—C3 | 1.351 (6) | C26—H26A | 0.930 |
C2—H2A | 0.930 | C27—H27A | 0.930 |
C3—H3A | 0.930 | C28—H28A | 0.960 |
C4—C5 | 1.522 (5) | C28—H28B | 0.960 |
C4—H4A | 0.970 | C28—H28C | 0.960 |
C4—H4B | 0.970 | O11—H111 | 0.850 |
C5—C20 | 1.404 (5) | O11—H112 | 0.850 |
C5—C6 | 1.407 (5) | S1'—O2' | 1.394 (7) |
C6—C8 | 1.395 (5) | S1'—O3' | 1.430 (6) |
C6—C7 | 1.517 (5) | S1'—O1' | 1.443 (7) |
C7—H7A | 0.960 | S1'—C22' | 1.752 (9) |
C7—H7B | 0.960 | C22'—C23' | 1.373 (10) |
C7—H7C | 0.960 | C22'—C27' | 1.402 (12) |
C8—C13 | 1.409 (5) | C23'—C24' | 1.378 (11) |
C8—C9 | 1.528 (5) | C23'—H23B | 0.930 |
C9—H9A | 0.970 | C24'—C25' | 1.367 (13) |
C9—H9B | 0.970 | C24'—H24B | 0.930 |
C10—H10A | 0.930 | C25'—C26' | 1.371 (9) |
C11—C12 | 1.337 (6) | C25'—C28' | 1.530 (14) |
C11—H11A | 0.930 | C26'—C27' | 1.362 (12) |
C12—H12A | 0.930 | C26'—H26B | 0.930 |
C13—C15 | 1.395 (5) | C27'—H27B | 0.930 |
C13—C14 | 1.520 (6) | C28'—H28D | 0.960 |
C14—H14A | 0.960 | C28'—H28E | 0.960 |
C14—H14B | 0.960 | C28'—H28F | 0.960 |
C14—H14C | 0.960 | O12—H121 | 0.850 |
C15—C20 | 1.404 (5) | O12—H122 | 0.850 |
N6i—Mn1—N6ii | 180.0 | C13—C15—C16 | 119.7 (4) |
N6i—Mn1—N4iii | 92.55 (12) | C20—C15—C16 | 119.3 (4) |
N6ii—Mn1—N4iii | 87.45 (12) | N5—C16—C15 | 113.1 (3) |
N6i—Mn1—N4iv | 87.45 (12) | N5—C16—H16A | 109.0 |
N6ii—Mn1—N4iv | 92.55 (12) | C15—C16—H16A | 109.0 |
N4iii—Mn1—N4iv | 180.0 | N5—C16—H16B | 109.0 |
N6i—Mn1—N1v | 85.55 (12) | C15—C16—H16B | 109.0 |
N6ii—Mn1—N1v | 94.45 (12) | H16A—C16—H16B | 107.8 |
N4iii—Mn1—N1v | 87.82 (12) | N6—C17—N5 | 112.6 (4) |
N4iv—Mn1—N1v | 92.18 (12) | N6—C17—H17A | 123.7 |
N6i—Mn1—N1 | 94.45 (12) | N5—C17—H17A | 123.7 |
N6ii—Mn1—N1 | 85.55 (12) | C19—C18—N6 | 110.2 (4) |
N4iii—Mn1—N1 | 92.18 (12) | C19—C18—H18A | 124.9 |
N4iv—Mn1—N1 | 87.82 (12) | N6—C18—H18A | 124.9 |
N1v—Mn1—N1 | 179.999 (1) | C18—C19—N5 | 106.6 (4) |
C1—N1—C2 | 104.0 (3) | C18—C19—H19A | 126.7 |
C1—N1—Mn1 | 133.0 (3) | N5—C19—H19A | 126.7 |
C2—N1—Mn1 | 122.9 (3) | C15—C20—C5 | 119.2 (4) |
C1—N2—C3 | 106.6 (3) | C15—C20—C21 | 119.3 (3) |
C1—N2—C4 | 126.3 (3) | C5—C20—C21 | 121.5 (4) |
C3—N2—C4 | 126.8 (3) | C20—C21—H21A | 109.5 |
C10—N3—C12 | 105.7 (3) | C20—C21—H21B | 109.5 |
C10—N3—C9 | 127.4 (4) | H21A—C21—H21B | 109.5 |
C12—N3—C9 | 127.0 (4) | C20—C21—H21C | 109.5 |
C10—N4—C11 | 103.6 (3) | H21A—C21—H21C | 109.5 |
C10—N4—Mn1vi | 131.1 (3) | H21B—C21—H21C | 109.5 |
C11—N4—Mn1vi | 124.1 (3) | O2—S1—O1 | 115.2 (5) |
C17—N5—C19 | 106.4 (3) | O2—S1—O3 | 113.2 (5) |
C17—N5—C16 | 125.9 (3) | O1—S1—O3 | 109.1 (5) |
C19—N5—C16 | 127.6 (3) | O2—S1—C22 | 105.2 (4) |
C17—N6—C18 | 104.1 (3) | O1—S1—C22 | 110.4 (5) |
C17—N6—Mn1vii | 130.8 (3) | O3—S1—C22 | 103.0 (5) |
C18—N6—Mn1vii | 124.7 (3) | C23—C22—C27 | 118.8 (8) |
N1—C1—N2 | 112.6 (3) | C23—C22—S1 | 122.7 (8) |
N1—C1—H1A | 123.7 | C27—C22—S1 | 118.5 (5) |
N2—C1—H1A | 123.7 | C22—C23—C24 | 121.4 (10) |
C3—C2—N1 | 110.4 (4) | C22—C23—H23A | 119.3 |
C3—C2—H2A | 124.8 | C24—C23—H23A | 119.3 |
N1—C2—H2A | 124.8 | C25—C24—C23 | 121.2 (8) |
C2—C3—N2 | 106.3 (4) | C25—C24—H24A | 119.4 |
C2—C3—H3A | 126.8 | C23—C24—H24A | 119.4 |
N2—C3—H3A | 126.8 | C24—C25—C26 | 117.5 (11) |
N2—C4—C5 | 113.0 (3) | C24—C25—C28 | 120.4 (8) |
N2—C4—H4A | 109.0 | C26—C25—C28 | 121.9 (11) |
C5—C4—H4A | 109.0 | C27—C26—C25 | 121.2 (11) |
N2—C4—H4B | 109.0 | C27—C26—H26A | 119.4 |
C5—C4—H4B | 109.0 | C25—C26—H26A | 119.4 |
H4A—C4—H4B | 107.8 | C26—C27—C22 | 119.4 (7) |
C20—C5—C6 | 120.4 (3) | C26—C27—H27A | 120.3 |
C20—C5—C4 | 120.4 (4) | C22—C27—H27A | 120.3 |
C6—C5—C4 | 119.1 (3) | C25—C28—H28A | 109.5 |
C8—C6—C5 | 119.6 (3) | C25—C28—H28B | 109.5 |
C8—C6—C7 | 121.5 (4) | H28A—C28—H28B | 109.5 |
C5—C6—C7 | 118.9 (3) | C25—C28—H28C | 109.5 |
C6—C7—H7A | 109.5 | H28A—C28—H28C | 109.5 |
C6—C7—H7B | 109.5 | H28B—C28—H28C | 109.5 |
H7A—C7—H7B | 109.5 | H111—O11—H112 | 108.4 |
C6—C7—H7C | 109.5 | O2'—S1'—O3' | 112.8 (7) |
H7A—C7—H7C | 109.5 | O2'—S1'—O1' | 112.2 (7) |
H7B—C7—H7C | 109.5 | O3'—S1'—O1' | 109.2 (7) |
C6—C8—C13 | 120.4 (4) | O2'—S1'—C22' | 111.1 (7) |
C6—C8—C9 | 120.7 (3) | O3'—S1'—C22' | 103.4 (6) |
C13—C8—C9 | 118.8 (4) | O1'—S1'—C22' | 107.7 (9) |
N3—C9—C8 | 113.7 (3) | C23'—C22'—C27' | 117.9 (9) |
N3—C9—H9A | 108.8 | C23'—C22'—S1' | 121.2 (9) |
C8—C9—H9A | 108.8 | C27'—C22'—S1' | 120.9 (7) |
N3—C9—H9B | 108.8 | C22'—C23'—C24' | 120.6 (11) |
C8—C9—H9B | 108.8 | C22'—C23'—H23B | 119.7 |
H9A—C9—H9B | 107.7 | C24'—C23'—H23B | 119.7 |
N4—C10—N3 | 113.4 (4) | C25'—C24'—C23' | 120.4 (10) |
N4—C10—H10A | 123.3 | C25'—C24'—H24B | 119.8 |
N3—C10—H10A | 123.3 | C23'—C24'—H24B | 119.8 |
C12—C11—N4 | 110.6 (4) | C24'—C25'—C26' | 120.0 (12) |
C12—C11—H11A | 124.7 | C24'—C25'—C28' | 121.3 (9) |
N4—C11—H11A | 124.7 | C26'—C25'—C28' | 118.6 (12) |
C11—C12—N3 | 106.7 (5) | C27'—C26'—C25' | 119.9 (12) |
C11—C12—H12A | 126.7 | C27'—C26'—H26B | 120.1 |
N3—C12—H12A | 126.7 | C25'—C26'—H26B | 120.1 |
C15—C13—C8 | 119.4 (3) | C26'—C27'—C22' | 121.1 (8) |
C15—C13—C14 | 120.6 (3) | C26'—C27'—H27B | 119.4 |
C8—C13—C14 | 120.0 (4) | C22'—C27'—H27B | 119.4 |
C13—C14—H14A | 109.5 | C25'—C28'—H28D | 109.5 |
C13—C14—H14B | 109.5 | C25'—C28'—H28E | 109.5 |
H14A—C14—H14B | 109.5 | H28D—C28'—H28E | 109.5 |
C13—C14—H14C | 109.5 | C25'—C28'—H28F | 109.5 |
H14A—C14—H14C | 109.5 | H28D—C28'—H28F | 109.5 |
H14B—C14—H14C | 109.5 | H28E—C28'—H28F | 109.5 |
C13—C15—C20 | 120.8 (3) | H121—O12—H122 | 109.1 |
Symmetry codes: (i) x, y−1, z; (ii) −x, −y+1, −z+1; (iii) x−1, y, z; (iv) −x+1, −y, −z+1; (v) −x, −y, −z+1; (vi) x+1, y, z; (vii) x, y+1, z. |