Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807012780/bg2040sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807012780/bg2040Isup2.hkl |
CCDC reference: 642907
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- H-atom completeness 94%
- R factor = 0.032
- wR factor = 0.082
- Data-to-parameter ratio = 14.1
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O6W
Alert level C STRVA01_ALERT_4_C Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.508 From the CIF: _refine_ls_abs_structure_Flack_su 0.012 PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.51 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S2 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.35 PLAT420_ALERT_2_C D-H Without Acceptor N3 - H3A ... ? PLAT430_ALERT_2_C Short Inter D...A Contact O1 .. O6W .. 2.90 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10
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:C22 H32 N4 Ni1 O12 S2 Atom count from the _atom_site data: C22 H30 N4 Ni1 O12 S2 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 2 From the CIF: _chemical_formula_sum C22 H32 N4 Ni O12 S2 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 44.00 44.00 0.00 H 64.00 60.00 4.00 N 8.00 8.00 0.00 Ni 2.00 2.00 0.00 O 24.00 24.00 0.00 S 4.00 4.00 0.00 REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 26.08 From the CIF: _reflns_number_total 5316 Count of symmetry unique reflns 3023 Completeness (_total/calc) 175.85% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 2293 Fraction of Friedel pairs measured 0.759 Are heavy atom types Z>Si present yes PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 11 ALERT level C = Check and explain 6 ALERT level G = General alerts; check 7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 8 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97.
[Ni(C10H8N2)(H2O)4](C6H6NO3S)2·2H2O | F(000) = 696 |
Mr = 667.35 | Dx = 1.562 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2yb | Cell parameters from 3996 reflections |
a = 11.288 (2) Å | θ = 2.9–26.0° |
b = 8.0129 (16) Å | µ = 0.90 mm−1 |
c = 15.702 (3) Å | T = 293 K |
β = 92.77 (3)° | Block, green |
V = 1418.6 (5) Å3 | 0.33 × 0.29 × 0.12 mm |
Z = 2 |
Bruker SMART APEX II CCD diffractometer | 5316 independent reflections |
Radiation source: fine-focus sealed tube | 5031 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.015 |
ω scans | θmax = 26.1°, θmin = 1.3° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −13→10 |
Tmin = 0.756, Tmax = 0.900 | k = −9→9 |
7701 measured reflections | l = −19→17 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.032 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.082 | w = 1/[σ2(Fo2) + (0.0427P)2 + 0.51P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max = 0.002 |
5316 reflections | Δρmax = 0.20 e Å−3 |
377 parameters | Δρmin = −0.32 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 2293 Friedel pairs? |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.508 (12) |
Experimental. The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures' each set had a different φ angle for the crystal and each exposure covered 0.3° in ω. The crystal-to-detector distance was 4.97 cm. Coverage of the unique set was over 95% complete to at least 28° in θ. Crystal decay was monitored by repeating the initial 50 frames at the end of data collection and analyzing the duplicate reflections. Decay was found to be less than 1% and no decay correction was therefore applied. IR (KBr pellets, µ /cm-1): 569, 637, 698, 819, 1003, 1028, 1122, 1160, 1203, 1221, 1299, 1417, 1504, 1540, 1597, 1612, 1634, 3367. |
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 | ||
Ni1 | 0.48777 (3) | 0.46905 (5) | 0.77301 (2) | 0.03077 (9) | |
O1W | 0.49613 (18) | 0.7153 (3) | 0.73796 (16) | 0.0482 (6) | |
H1WA | 0.5407 | 0.7778 | 0.7643 | 0.058* | |
H1WB | 0.4408 | 0.7620 | 0.7153 | 0.058* | |
O2W | 0.50551 (18) | 0.5349 (3) | 0.90043 (13) | 0.0479 (6) | |
H2WA | 0.5580 | 0.5985 | 0.9173 | 0.058* | |
H2WB | 0.4509 | 0.5345 | 0.9333 | 0.058* | |
O3W | 0.48271 (18) | 0.3930 (3) | 0.64724 (14) | 0.0425 (5) | |
H3WA | 0.4747 | 0.4458 | 0.5984 | 0.051* | |
H3WB | 0.4365 | 0.3148 | 0.6364 | 0.051* | |
O4W | 0.47752 (18) | 0.2193 (3) | 0.81013 (16) | 0.0475 (6) | |
H4WA | 0.5260 | 0.1471 | 0.8250 | 0.057* | |
H4WB | 0.4261 | 0.1733 | 0.7780 | 0.057* | |
N1 | −0.32691 (17) | 0.4633 (4) | 0.76999 (14) | 0.0334 (5) | |
N2 | 0.30230 (16) | 0.4711 (4) | 0.76875 (14) | 0.0329 (5) | |
C1 | −0.2710 (2) | 0.5293 (4) | 0.70475 (19) | 0.0402 (8) | |
H1 | −0.3167 | 0.5793 | 0.6610 | 0.048* | |
C2 | −0.1501 (2) | 0.5274 (4) | 0.69853 (18) | 0.0375 (7) | |
H2 | −0.1160 | 0.5749 | 0.6515 | 0.045* | |
C3 | −0.0787 (2) | 0.4537 (4) | 0.76318 (16) | 0.0279 (6) | |
C4 | −0.1376 (2) | 0.3840 (4) | 0.8302 (2) | 0.0378 (7) | |
H4 | −0.0945 | 0.3320 | 0.8747 | 0.045* | |
C5 | −0.2588 (2) | 0.3912 (4) | 0.8312 (2) | 0.0368 (7) | |
H5 | −0.2955 | 0.3433 | 0.8770 | 0.044* | |
C6 | 0.2439 (2) | 0.3972 (4) | 0.83002 (19) | 0.0356 (7) | |
H6 | 0.2876 | 0.3500 | 0.8756 | 0.043* | |
C7 | 0.1218 (2) | 0.3870 (4) | 0.82929 (18) | 0.0326 (6) | |
H7 | 0.0855 | 0.3324 | 0.8733 | 0.039* | |
C8 | 0.05302 (19) | 0.4577 (4) | 0.76331 (16) | 0.0271 (5) | |
C9 | 0.1143 (2) | 0.5346 (4) | 0.6995 (2) | 0.0381 (7) | |
H9 | 0.0728 | 0.5839 | 0.6535 | 0.046* | |
C10 | 0.2366 (2) | 0.5382 (4) | 0.70432 (19) | 0.0387 (7) | |
H10 | 0.2753 | 0.5899 | 0.6605 | 0.046* | |
S1 | 0.69124 (7) | 0.92635 (9) | 0.91342 (5) | 0.0420 (2) | |
O1 | 0.6482 (2) | 0.9289 (4) | 0.82489 (17) | 0.0693 (9) | |
O2 | 0.6740 (2) | 0.7648 (3) | 0.95262 (17) | 0.0550 (7) | |
O3 | 0.6418 (2) | 1.0619 (4) | 0.9610 (2) | 0.0774 (9) | |
N3 | 1.2148 (2) | 0.9914 (5) | 0.9260 (2) | 0.0677 (9) | |
H3A | 1.2550 | 0.9387 | 0.8895 | 0.081* | |
H3B | 1.2507 | 1.0491 | 0.9656 | 0.081* | |
C11 | 0.8456 (2) | 0.9574 (4) | 0.91396 (16) | 0.0327 (6) | |
C12 | 0.9114 (3) | 0.8781 (4) | 0.8536 (2) | 0.0398 (7) | |
H12 | 0.8730 | 0.8160 | 0.8105 | 0.048* | |
C13 | 1.0334 (3) | 0.8906 (4) | 0.8572 (2) | 0.0445 (7) | |
H13 | 1.0766 | 0.8363 | 0.8165 | 0.053* | |
C14 | 1.0931 (3) | 0.9837 (5) | 0.92110 (18) | 0.0415 (7) | |
C15 | 1.0256 (3) | 1.0677 (4) | 0.98021 (19) | 0.0429 (8) | |
H15 | 1.0631 | 1.1334 | 1.0222 | 0.051* | |
C16 | 0.9027 (3) | 1.0532 (4) | 0.97626 (18) | 0.0380 (7) | |
H16 | 0.8586 | 1.1086 | 1.0160 | 0.046* | |
S2 | 0.29256 (7) | 1.00821 (10) | 0.63346 (6) | 0.0456 (2) | |
O4 | 0.3593 (2) | 0.8742 (4) | 0.5987 (2) | 0.0818 (10) | |
O5 | 0.3094 (2) | 1.0145 (5) | 0.72543 (16) | 0.0788 (10) | |
O6 | 0.3190 (3) | 1.1667 (4) | 0.5944 (2) | 0.0736 (9) | |
N4 | −0.2151 (3) | 0.8899 (5) | 0.5451 (2) | 0.0812 (12) | |
H4A | −0.2363 | 0.8273 | 0.5026 | 0.097* | |
H4B | −0.2680 | 0.9361 | 0.5750 | 0.097* | |
C17 | 0.1422 (2) | 0.9663 (5) | 0.60810 (17) | 0.0370 (6) | |
C18 | 0.0572 (3) | 1.0393 (4) | 0.65646 (19) | 0.0424 (7) | |
H18 | 0.0801 | 1.1050 | 0.7032 | 0.051* | |
C19 | −0.0617 (3) | 1.0148 (5) | 0.6354 (2) | 0.0490 (8) | |
H19 | −0.1186 | 1.0641 | 0.6681 | 0.059* | |
C20 | −0.0968 (3) | 0.9163 (4) | 0.5654 (2) | 0.0460 (8) | |
C21 | −0.0107 (3) | 0.8436 (5) | 0.5185 (2) | 0.0503 (8) | |
H21 | −0.0332 | 0.7769 | 0.4720 | 0.060* | |
C22 | 0.1075 (3) | 0.8677 (4) | 0.5390 (2) | 0.0459 (8) | |
H22 | 0.1644 | 0.8178 | 0.5065 | 0.055* | |
O5W | 0.4875 (7) | 0.6177 (7) | 0.5271 (3) | 0.127 (3) | |
H5WB | 0.454 (9) | 0.639 (13) | 0.498 (6) | 0.152* | |
H5WA | 0.534 (7) | 0.625 (11) | 0.496 (5) | 0.152* | |
O6W | 0.3478 (5) | 0.5964 (7) | 0.3384 (3) | 0.1508 (19) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.01413 (13) | 0.03661 (17) | 0.04146 (18) | −0.00051 (14) | 0.00022 (11) | 0.00519 (16) |
O1W | 0.0346 (12) | 0.0372 (13) | 0.0711 (15) | −0.0019 (10) | −0.0157 (11) | 0.0089 (12) |
O2W | 0.0297 (10) | 0.0695 (17) | 0.0450 (12) | −0.0164 (10) | 0.0060 (9) | −0.0042 (11) |
O3W | 0.0319 (11) | 0.0495 (13) | 0.0463 (12) | −0.0076 (10) | 0.0026 (9) | −0.0038 (10) |
O4W | 0.0300 (11) | 0.0402 (13) | 0.0711 (15) | 0.0024 (10) | −0.0092 (10) | 0.0129 (12) |
N1 | 0.0178 (9) | 0.0398 (13) | 0.0426 (11) | 0.0002 (13) | 0.0021 (8) | 0.0051 (14) |
N2 | 0.0175 (9) | 0.0399 (13) | 0.0412 (11) | −0.0006 (13) | 0.0013 (8) | 0.0014 (14) |
C1 | 0.0205 (13) | 0.056 (2) | 0.0430 (16) | −0.0007 (13) | −0.0046 (12) | 0.0158 (15) |
C2 | 0.0213 (13) | 0.0541 (19) | 0.0372 (14) | −0.0045 (12) | 0.0021 (11) | 0.0113 (13) |
C3 | 0.0171 (10) | 0.0289 (15) | 0.0375 (13) | −0.0024 (12) | 0.0008 (9) | −0.0038 (13) |
C4 | 0.0225 (13) | 0.0454 (18) | 0.0453 (17) | −0.0029 (12) | −0.0014 (12) | 0.0172 (14) |
C5 | 0.0218 (13) | 0.0464 (18) | 0.0422 (16) | −0.0002 (12) | 0.0020 (12) | 0.0125 (14) |
C6 | 0.0213 (13) | 0.0466 (17) | 0.0387 (15) | 0.0024 (12) | 0.0005 (11) | 0.0065 (13) |
C7 | 0.0197 (12) | 0.0444 (16) | 0.0338 (14) | 0.0006 (11) | 0.0033 (11) | 0.0046 (12) |
C8 | 0.0161 (10) | 0.0280 (13) | 0.0372 (12) | 0.0007 (12) | 0.0011 (9) | −0.0027 (13) |
C9 | 0.0201 (13) | 0.0479 (19) | 0.0459 (16) | 0.0007 (12) | −0.0016 (12) | 0.0139 (14) |
C10 | 0.0226 (13) | 0.0476 (18) | 0.0460 (16) | −0.0027 (12) | 0.0034 (12) | 0.0119 (14) |
S1 | 0.0327 (4) | 0.0405 (5) | 0.0524 (4) | −0.0021 (3) | −0.0004 (3) | 0.0077 (3) |
O1 | 0.0419 (13) | 0.097 (3) | 0.0667 (15) | −0.0140 (14) | −0.0209 (12) | 0.0272 (16) |
O2 | 0.0438 (13) | 0.0483 (15) | 0.0718 (16) | −0.0153 (11) | −0.0105 (12) | 0.0179 (13) |
O3 | 0.0562 (17) | 0.0587 (18) | 0.121 (3) | 0.0006 (14) | 0.0434 (17) | −0.0123 (18) |
N3 | 0.0382 (15) | 0.079 (2) | 0.086 (2) | −0.0096 (17) | 0.0008 (14) | −0.003 (2) |
C11 | 0.0345 (13) | 0.0284 (14) | 0.0350 (12) | −0.0029 (14) | −0.0001 (10) | 0.0044 (13) |
C12 | 0.0441 (17) | 0.0389 (17) | 0.0363 (16) | −0.0046 (14) | 0.0012 (13) | −0.0059 (13) |
C13 | 0.0455 (18) | 0.0442 (18) | 0.0447 (17) | −0.0003 (14) | 0.0100 (14) | −0.0022 (14) |
C14 | 0.0363 (14) | 0.0415 (17) | 0.0465 (15) | −0.0072 (15) | −0.0010 (12) | 0.0143 (16) |
C15 | 0.0498 (19) | 0.0419 (18) | 0.0359 (16) | −0.0136 (15) | −0.0089 (14) | 0.0012 (14) |
C16 | 0.0474 (18) | 0.0337 (16) | 0.0334 (15) | −0.0042 (13) | 0.0064 (13) | −0.0007 (13) |
S2 | 0.0357 (4) | 0.0420 (5) | 0.0581 (5) | −0.0031 (3) | −0.0083 (3) | 0.0112 (4) |
O4 | 0.0469 (16) | 0.072 (2) | 0.126 (3) | 0.0091 (15) | 0.0023 (17) | −0.015 (2) |
O5 | 0.0525 (15) | 0.124 (3) | 0.0582 (15) | −0.0261 (17) | −0.0193 (12) | 0.0247 (18) |
O6 | 0.0592 (17) | 0.0559 (17) | 0.102 (2) | −0.0244 (14) | −0.0327 (16) | 0.0348 (16) |
N4 | 0.0442 (18) | 0.107 (3) | 0.091 (3) | −0.0072 (19) | −0.0164 (18) | −0.036 (2) |
C17 | 0.0369 (14) | 0.0317 (14) | 0.0419 (14) | −0.0005 (16) | −0.0042 (11) | 0.0053 (16) |
C18 | 0.0451 (18) | 0.0415 (17) | 0.0398 (16) | −0.0051 (14) | −0.0048 (14) | −0.0063 (14) |
C19 | 0.0426 (17) | 0.059 (2) | 0.0454 (17) | −0.0021 (15) | 0.0034 (13) | −0.0073 (16) |
C20 | 0.0424 (17) | 0.0444 (19) | 0.0502 (18) | −0.0089 (14) | −0.0091 (14) | 0.0016 (15) |
C21 | 0.053 (2) | 0.0497 (19) | 0.047 (2) | −0.0042 (16) | −0.0097 (16) | −0.0124 (15) |
C22 | 0.050 (2) | 0.0413 (18) | 0.0459 (18) | 0.0041 (15) | −0.0021 (15) | −0.0064 (15) |
O5W | 0.196 (6) | 0.101 (3) | 0.090 (3) | 0.053 (4) | 0.081 (4) | 0.039 (2) |
O6W | 0.160 (5) | 0.155 (5) | 0.141 (4) | −0.044 (4) | 0.038 (3) | −0.007 (3) |
Ni1—O1W | 2.052 (2) | S1—O3 | 1.446 (3) |
Ni1—O3W | 2.065 (2) | S1—O2 | 1.450 (3) |
Ni1—O2W | 2.070 (2) | S1—O1 | 1.450 (3) |
Ni1—O4W | 2.089 (2) | S1—C11 | 1.759 (3) |
Ni1—N2 | 2.0914 (19) | N3—C14 | 1.373 (4) |
Ni1—N1i | 2.095 (2) | N3—H3A | 0.8600 |
O1W—H1WA | 0.8093 | N3—H3B | 0.8600 |
O1W—H1WB | 0.7968 | C11—C16 | 1.378 (4) |
O2W—H2WA | 0.8162 | C11—C12 | 1.386 (4) |
O2W—H2WB | 0.8221 | C12—C13 | 1.380 (4) |
O3W—H3WA | 0.8765 | C12—H12 | 0.9300 |
O3W—H3WB | 0.8272 | C13—C14 | 1.397 (5) |
O4W—H4WA | 0.8224 | C13—H13 | 0.9300 |
O4W—H4WB | 0.8352 | C14—C15 | 1.402 (5) |
N1—C5 | 1.333 (4) | C15—C16 | 1.391 (4) |
N1—C1 | 1.338 (4) | C15—H15 | 0.9300 |
N1—Ni1ii | 2.095 (2) | C16—H16 | 0.9300 |
N2—C6 | 1.331 (4) | S2—O4 | 1.435 (3) |
N2—C10 | 1.338 (4) | S2—O5 | 1.448 (3) |
C1—C2 | 1.373 (4) | S2—O6 | 1.448 (3) |
C1—H1 | 0.9300 | S2—C17 | 1.757 (3) |
C2—C3 | 1.396 (4) | N4—C20 | 1.375 (4) |
C2—H2 | 0.9300 | N4—H4A | 0.8600 |
C3—C4 | 1.389 (4) | N4—H4B | 0.8600 |
C3—C8 | 1.487 (3) | C17—C18 | 1.382 (4) |
C4—C5 | 1.370 (4) | C17—C22 | 1.383 (4) |
C4—H4 | 0.9300 | C18—C19 | 1.380 (4) |
C5—H5 | 0.9300 | C18—H18 | 0.9300 |
C6—C7 | 1.381 (4) | C19—C20 | 1.395 (4) |
C6—H6 | 0.9300 | C19—H19 | 0.9300 |
C7—C8 | 1.385 (4) | C20—C21 | 1.377 (5) |
C7—H7 | 0.9300 | C21—C22 | 1.371 (5) |
C8—C9 | 1.389 (4) | C21—H21 | 0.9300 |
C9—C10 | 1.379 (4) | C22—H22 | 0.9300 |
C9—H9 | 0.9300 | O5W—H5WB | 0.60 (9) |
C10—H10 | 0.9300 | O5W—H5WA | 0.74 (7) |
O1W—Ni1—O3W | 91.54 (10) | C8—C9—H9 | 119.9 |
O1W—Ni1—O2W | 90.61 (10) | N2—C10—C9 | 123.4 (3) |
O3W—Ni1—O2W | 175.40 (9) | N2—C10—H10 | 118.3 |
O1W—Ni1—O4W | 179.14 (11) | C9—C10—H10 | 118.3 |
O3W—Ni1—O4W | 89.12 (10) | O3—S1—O2 | 112.81 (18) |
O2W—Ni1—O4W | 88.77 (10) | O3—S1—O1 | 111.4 (2) |
O1W—Ni1—N2 | 92.45 (11) | O2—S1—O1 | 111.93 (18) |
O3W—Ni1—N2 | 89.45 (9) | O3—S1—C11 | 107.34 (16) |
O2W—Ni1—N2 | 94.52 (9) | O2—S1—C11 | 106.12 (16) |
O4W—Ni1—N2 | 87.00 (11) | O1—S1—C11 | 106.77 (14) |
O1W—Ni1—N1i | 87.49 (10) | C14—N3—H3A | 120.0 |
O3W—Ni1—N1i | 87.33 (9) | C14—N3—H3B | 120.0 |
O2W—Ni1—N1i | 88.70 (9) | H3A—N3—H3B | 120.0 |
O4W—Ni1—N1i | 93.10 (10) | C16—C11—C12 | 119.5 (3) |
N2—Ni1—N1i | 176.78 (10) | C16—C11—S1 | 120.7 (2) |
Ni1—O1W—H1WA | 119.5 | C12—C11—S1 | 119.7 (2) |
Ni1—O1W—H1WB | 121.8 | C13—C12—C11 | 120.4 (3) |
H1WA—O1W—H1WB | 113.0 | C13—C12—H12 | 119.8 |
Ni1—O2W—H2WA | 120.6 | C11—C12—H12 | 119.8 |
Ni1—O2W—H2WB | 124.4 | C12—C13—C14 | 120.9 (3) |
H2WA—O2W—H2WB | 110.7 | C12—C13—H13 | 119.5 |
Ni1—O3W—H3WA | 133.7 | C14—C13—H13 | 119.5 |
Ni1—O3W—H3WB | 114.1 | N3—C14—C13 | 120.7 (3) |
H3WA—O3W—H3WB | 98.5 | N3—C14—C15 | 121.1 (3) |
Ni1—O4W—H4WA | 135.0 | C13—C14—C15 | 118.2 (3) |
Ni1—O4W—H4WB | 107.5 | C16—C15—C14 | 120.3 (3) |
H4WA—O4W—H4WB | 107.1 | C16—C15—H15 | 119.9 |
C5—N1—C1 | 116.5 (2) | C14—C15—H15 | 119.9 |
C5—N1—Ni1ii | 122.31 (19) | C11—C16—C15 | 120.6 (3) |
C1—N1—Ni1ii | 121.14 (18) | C11—C16—H16 | 119.7 |
C6—N2—C10 | 116.7 (2) | C15—C16—H16 | 119.7 |
C6—N2—Ni1 | 120.21 (19) | O4—S2—O5 | 111.1 (2) |
C10—N2—Ni1 | 123.02 (19) | O4—S2—O6 | 111.9 (2) |
N1—C1—C2 | 123.9 (3) | O5—S2—O6 | 111.8 (2) |
N1—C1—H1 | 118.1 | O4—S2—C17 | 106.86 (17) |
C2—C1—H1 | 118.1 | O5—S2—C17 | 108.13 (15) |
C1—C2—C3 | 119.6 (3) | O6—S2—C17 | 106.73 (16) |
C1—C2—H2 | 120.2 | C20—N4—H4A | 120.0 |
C3—C2—H2 | 120.2 | C20—N4—H4B | 120.0 |
C4—C3—C2 | 116.1 (2) | H4A—N4—H4B | 120.0 |
C4—C3—C8 | 121.5 (2) | C18—C17—C22 | 119.6 (3) |
C2—C3—C8 | 122.3 (2) | C18—C17—S2 | 118.9 (2) |
C5—C4—C3 | 120.5 (3) | C22—C17—S2 | 121.4 (2) |
C5—C4—H4 | 119.8 | C19—C18—C17 | 120.1 (3) |
C3—C4—H4 | 119.8 | C19—C18—H18 | 120.0 |
N1—C5—C4 | 123.4 (3) | C17—C18—H18 | 120.0 |
N1—C5—H5 | 118.3 | C18—C19—C20 | 120.3 (3) |
C4—C5—H5 | 118.3 | C18—C19—H19 | 119.8 |
N2—C6—C7 | 123.3 (3) | C20—C19—H19 | 119.8 |
N2—C6—H6 | 118.3 | N4—C20—C21 | 120.9 (3) |
C7—C6—H6 | 118.3 | N4—C20—C19 | 120.4 (3) |
C6—C7—C8 | 120.3 (3) | C21—C20—C19 | 118.7 (3) |
C6—C7—H7 | 119.8 | C22—C21—C20 | 121.2 (3) |
C8—C7—H7 | 119.8 | C22—C21—H21 | 119.4 |
C7—C8—C9 | 116.1 (2) | C20—C21—H21 | 119.4 |
C7—C8—C3 | 121.1 (2) | C21—C22—C17 | 120.0 (3) |
C9—C8—C3 | 122.8 (2) | C21—C22—H22 | 120.0 |
C10—C9—C8 | 120.1 (3) | C17—C22—H22 | 120.0 |
C10—C9—H9 | 119.9 | H5WB—O5W—H5WA | 85 (9) |
O1W—Ni1—N2—C6 | −137.0 (3) | O3—S1—C11—C16 | 22.4 (3) |
O3W—Ni1—N2—C6 | 131.5 (3) | O2—S1—C11—C16 | −98.5 (3) |
O2W—Ni1—N2—C6 | −46.2 (3) | O1—S1—C11—C16 | 142.0 (3) |
O4W—Ni1—N2—C6 | 42.4 (3) | O3—S1—C11—C12 | −160.8 (3) |
O1W—Ni1—N2—C10 | 46.1 (3) | O2—S1—C11—C12 | 78.3 (3) |
O3W—Ni1—N2—C10 | −45.5 (3) | O1—S1—C11—C12 | −41.2 (3) |
O2W—Ni1—N2—C10 | 136.9 (3) | C16—C11—C12—C13 | 1.9 (5) |
O4W—Ni1—N2—C10 | −134.6 (3) | S1—C11—C12—C13 | −174.9 (3) |
C5—N1—C1—C2 | −0.6 (5) | C11—C12—C13—C14 | −0.3 (5) |
Ni1ii—N1—C1—C2 | −179.1 (3) | C12—C13—C14—N3 | 177.9 (3) |
N1—C1—C2—C3 | −0.2 (5) | C12—C13—C14—C15 | −1.7 (5) |
C1—C2—C3—C4 | 0.9 (5) | N3—C14—C15—C16 | −177.5 (3) |
C1—C2—C3—C8 | −175.7 (3) | C13—C14—C15—C16 | 2.1 (5) |
C2—C3—C4—C5 | −0.8 (5) | C12—C11—C16—C15 | −1.5 (5) |
C8—C3—C4—C5 | 175.8 (3) | S1—C11—C16—C15 | 175.3 (2) |
C1—N1—C5—C4 | 0.7 (5) | C14—C15—C16—C11 | −0.6 (5) |
Ni1ii—N1—C5—C4 | 179.2 (3) | O4—S2—C17—C18 | 158.0 (3) |
C3—C4—C5—N1 | 0.0 (5) | O5—S2—C17—C18 | 38.4 (3) |
C10—N2—C6—C7 | 0.3 (5) | O6—S2—C17—C18 | −82.1 (3) |
Ni1—N2—C6—C7 | −176.9 (2) | O4—S2—C17—C22 | −24.6 (4) |
N2—C6—C7—C8 | −1.0 (5) | O5—S2—C17—C22 | −144.2 (3) |
C6—C7—C8—C9 | 0.9 (5) | O6—S2—C17—C22 | 95.3 (3) |
C6—C7—C8—C3 | −177.6 (3) | C22—C17—C18—C19 | −0.5 (5) |
C4—C3—C8—C7 | 2.1 (4) | S2—C17—C18—C19 | 177.0 (3) |
C2—C3—C8—C7 | 178.5 (3) | C17—C18—C19—C20 | 0.0 (5) |
C4—C3—C8—C9 | −176.3 (4) | C18—C19—C20—N4 | 179.1 (4) |
C2—C3—C8—C9 | 0.1 (4) | C18—C19—C20—C21 | 0.5 (5) |
C7—C8—C9—C10 | −0.2 (5) | N4—C20—C21—C22 | −179.2 (4) |
C3—C8—C9—C10 | 178.2 (3) | C19—C20—C21—C22 | −0.6 (6) |
C6—N2—C10—C9 | 0.5 (5) | C20—C21—C22—C17 | 0.1 (6) |
Ni1—N2—C10—C9 | 177.5 (3) | C18—C17—C22—C21 | 0.4 (5) |
C8—C9—C10—N2 | −0.5 (5) | S2—C17—C22—C21 | −177.0 (3) |
Symmetry codes: (i) x+1, y, z; (ii) x−1, y, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O5W—H5WA···O6iii | 0.74 (7) | 2.25 (8) | 2.996 (7) | 175 (9) |
N4—H4B···O6Wiv | 0.86 | 2.10 | 2.930 (6) | 161 |
N4—H4A···O6v | 0.86 | 2.17 | 3.021 (4) | 170 |
N3—H3B···O2vi | 0.86 | 2.29 | 3.127 (5) | 164 |
O4W—H4WB···O5vii | 0.84 | 1.98 | 2.797 (4) | 164 |
O4W—H4WA···O3vii | 0.82 | 2.54 | 3.197 (4) | 137 |
O4W—H4WA···O1vii | 0.82 | 2.23 | 3.023 (4) | 163 |
O3W—H3WB···O6vii | 0.83 | 1.88 | 2.691 (3) | 168 |
O3W—H3WA···O5W | 0.88 | 1.78 | 2.610 (5) | 156 |
O2W—H2WB···O3viii | 0.82 | 2.02 | 2.809 (4) | 162 |
O2W—H2WA···O2 | 0.82 | 1.93 | 2.744 (3) | 175 |
O1W—H1WB···O5 | 0.80 | 2.52 | 3.192 (4) | 143 |
O1W—H1WB···O4 | 0.80 | 2.20 | 2.910 (4) | 148 |
O1W—H1WA···O1 | 0.81 | 1.93 | 2.741 (4) | 179 |
Symmetry codes: (iii) −x+1, y−1/2, −z+1; (iv) −x, y+1/2, −z+1; (v) −x, y−1/2, −z+1; (vi) −x+2, y+1/2, −z+2; (vii) x, y−1, z; (viii) −x+1, y−1/2, −z+2. |
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