Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806051701/cv2154sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806051701/cv2154Isup2.hkl |
CCDC reference: 633665
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.056
- wR factor = 0.122
- Data-to-parameter ratio = 16.1
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 1 N2 -NI1 -O1 -C1 90.20 0.70 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 8 N4 -NI1 -N1 -C15 -165.60 0.70 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 13 N4 -NI1 -N1 -C26 23.50 0.90 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 16 O1 -NI1 -N2 -C24 159.90 0.60 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 21 O1 -NI1 -N2 -C25 -22.60 0.80 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 30 O7 -NI1 -N3 -C27 -174.50 0.80 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 35 O7 -NI1 -N3 -C38 7.10 1.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 39 N1 -NI1 -N4 -C36 -105.90 0.80 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 44 N1 -NI1 -N4 -C37 73.40 0.90 1.555 1.555 1.555 1.555 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 H2 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 H2 O
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 12 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Ni(C14H8O6S)(C12H8N2)2(H2O)]·2H2O | Z = 2 |
Mr = 777.43 | F(000) = 804 |
Triclinic, P1 | Dx = 1.520 Mg m−3 |
a = 8.8457 (10) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 12.4789 (14) Å | Cell parameters from 3276 reflections |
c = 16.673 (2) Å | θ = 2.4–27.5° |
α = 105.894 (4)° | µ = 0.70 mm−1 |
β = 105.091 (4)° | T = 293 K |
γ = 91.836 (5)° | Prism, green |
V = 1698.4 (3) Å3 | 0.35 × 0.25 × 0.10 mm |
Mercury CCD diffractometer | 7689 independent reflections |
Radiation source: fine-focus sealed tube | 5663 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
Detector resolution: 14.6306 pixels mm-1 | θmax = 27.5°, θmin = 2.4° |
φ? ω? scans | h = −11→10 |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2000) | k = −16→16 |
Tmin = 0.792, Tmax = 0.934 | l = −21→21 |
13188 measured reflections |
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)] = 0.056 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.122 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0418P)2 + 0.8893P] where P = (Fo2 + 2Fc2)/3 |
7689 reflections | (Δ/σ)max < 0.001 |
478 parameters | Δρmax = 0.49 e Å−3 |
2 restraints | Δρmin = −0.34 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 | ||
Ni1 | 0.29581 (5) | 0.26435 (3) | 0.22952 (2) | 0.03447 (12) | |
S1 | −0.25633 (9) | −0.12158 (6) | 0.43467 (5) | 0.03760 (19) | |
O1 | 0.1371 (3) | 0.18269 (16) | 0.26739 (14) | 0.0420 (5) | |
O2 | 0.0149 (3) | 0.31978 (19) | 0.33203 (19) | 0.0691 (8) | |
O3 | −0.9014 (3) | −0.44655 (17) | 0.15404 (14) | 0.0456 (5) | |
O4 | −1.0106 (3) | −0.2960 (2) | 0.20935 (16) | 0.0552 (6) | |
O5 | −0.1548 (3) | −0.20901 (18) | 0.43217 (16) | 0.0517 (6) | |
O6 | −0.2873 (3) | −0.06434 (19) | 0.51491 (14) | 0.0502 (6) | |
O7 | 0.2017 (3) | 0.41669 (16) | 0.26634 (13) | 0.0451 (5) | |
H7A | 0.1650 | 0.4536 | 0.2311 | 0.054* | |
H7B | 0.1257 | 0.3967 | 0.2835 | 0.054* | |
O8 | −1.3178 (4) | −0.3031 (3) | 0.0894 (2) | 0.0902 (10) | |
H8B | −1.3002 | −0.3612 | 0.0538 | 0.108* | |
H8A | −1.2415 | −0.2833 | 0.1355 | 0.108* | |
O9 | −1.1926 (3) | −0.5004 (2) | 0.00396 (19) | 0.0785 (8) | |
H9A | −1.1753 | −0.5163 | −0.0456 | 0.094* | |
H9B | −1.1052 | −0.4822 | 0.0433 | 0.094* | |
N1 | 0.4555 (3) | 0.3136 (2) | 0.35388 (15) | 0.0387 (6) | |
N2 | 0.4791 (3) | 0.34821 (19) | 0.20564 (16) | 0.0379 (6) | |
N3 | 0.3744 (3) | 0.10997 (19) | 0.18140 (15) | 0.0354 (6) | |
N4 | 0.1579 (3) | 0.22000 (19) | 0.10079 (15) | 0.0354 (6) | |
C1 | 0.0435 (4) | 0.2202 (2) | 0.31045 (19) | 0.0380 (7) | |
C2 | −0.0392 (3) | 0.1361 (2) | 0.33908 (18) | 0.0313 (6) | |
C3 | −0.0172 (4) | 0.0235 (2) | 0.31225 (19) | 0.0365 (7) | |
H3 | 0.0462 | 0.0007 | 0.2755 | 0.044* | |
C4 | −0.0880 (3) | −0.0548 (2) | 0.33929 (19) | 0.0364 (7) | |
H4 | −0.0748 | −0.1302 | 0.3198 | 0.044* | |
C5 | −0.1785 (3) | −0.0203 (2) | 0.39545 (18) | 0.0328 (6) | |
C6 | −0.2020 (4) | 0.0914 (2) | 0.4236 (2) | 0.0388 (7) | |
H6 | −0.2628 | 0.1141 | 0.4619 | 0.047* | |
C7 | −0.1341 (4) | 0.1689 (2) | 0.3942 (2) | 0.0385 (7) | |
H7 | −0.1521 | 0.2437 | 0.4115 | 0.046* | |
C8 | −0.4407 (3) | −0.1801 (2) | 0.35907 (19) | 0.0343 (6) | |
C9 | −0.5743 (4) | −0.1358 (3) | 0.3732 (2) | 0.0447 (8) | |
H9 | −0.5669 | −0.0704 | 0.4179 | 0.054* | |
C10 | −0.7201 (4) | −0.1885 (3) | 0.3206 (2) | 0.0436 (8) | |
H10 | −0.8107 | −0.1576 | 0.3296 | 0.052* | |
C11 | −0.7333 (4) | −0.2872 (2) | 0.25427 (19) | 0.0358 (7) | |
C12 | −0.5965 (4) | −0.3286 (3) | 0.2401 (2) | 0.0445 (8) | |
H12 | −0.6034 | −0.3937 | 0.1951 | 0.053* | |
C13 | −0.4498 (4) | −0.2756 (3) | 0.2912 (2) | 0.0465 (8) | |
H13 | −0.3587 | −0.3036 | 0.2801 | 0.056* | |
C14 | −0.8950 (4) | −0.3467 (2) | 0.20213 (19) | 0.0370 (7) | |
C15 | 0.4431 (4) | 0.2953 (3) | 0.4267 (2) | 0.0492 (8) | |
H15 | 0.3608 | 0.2449 | 0.4239 | 0.059* | |
C16 | 0.5500 (5) | 0.3493 (3) | 0.5078 (2) | 0.0624 (11) | |
H16 | 0.5384 | 0.3341 | 0.5576 | 0.075* | |
C17 | 0.6704 (5) | 0.4238 (3) | 0.5133 (2) | 0.0616 (11) | |
H17 | 0.7405 | 0.4609 | 0.5669 | 0.074* | |
C18 | 0.6882 (4) | 0.4445 (3) | 0.4378 (2) | 0.0480 (8) | |
C19 | 0.8128 (4) | 0.5199 (3) | 0.4363 (3) | 0.0601 (11) | |
H19 | 0.8834 | 0.5618 | 0.4884 | 0.072* | |
C20 | 0.8292 (4) | 0.5311 (3) | 0.3607 (3) | 0.0584 (10) | |
H20 | 0.9124 | 0.5793 | 0.3617 | 0.070* | |
C21 | 0.7220 (4) | 0.4706 (2) | 0.2796 (2) | 0.0479 (8) | |
C22 | 0.7336 (5) | 0.4774 (3) | 0.1985 (3) | 0.0607 (10) | |
H22 | 0.8180 | 0.5210 | 0.1954 | 0.073* | |
C23 | 0.6215 (5) | 0.4203 (3) | 0.1246 (3) | 0.0609 (10) | |
H23 | 0.6297 | 0.4229 | 0.0707 | 0.073* | |
C24 | 0.4946 (4) | 0.3579 (3) | 0.1309 (2) | 0.0492 (8) | |
H24 | 0.4167 | 0.3210 | 0.0802 | 0.059* | |
C25 | 0.5929 (4) | 0.4023 (2) | 0.2793 (2) | 0.0380 (7) | |
C26 | 0.5779 (4) | 0.3863 (2) | 0.35916 (19) | 0.0379 (7) | |
C27 | 0.4784 (4) | 0.0548 (3) | 0.2223 (2) | 0.0486 (8) | |
H27 | 0.5238 | 0.0855 | 0.2817 | 0.058* | |
C28 | 0.5231 (4) | −0.0468 (3) | 0.1806 (2) | 0.0545 (9) | |
H28 | 0.5964 | −0.0827 | 0.2119 | 0.065* | |
C29 | 0.4585 (4) | −0.0929 (3) | 0.0935 (2) | 0.0529 (9) | |
H29 | 0.4883 | −0.1603 | 0.0649 | 0.064* | |
C30 | 0.3471 (4) | −0.0387 (2) | 0.0472 (2) | 0.0412 (7) | |
C31 | 0.2681 (4) | −0.0809 (3) | −0.0430 (2) | 0.0510 (9) | |
H31 | 0.2936 | −0.1479 | −0.0750 | 0.061* | |
C32 | 0.1580 (4) | −0.0272 (3) | −0.0835 (2) | 0.0510 (9) | |
H32 | 0.1086 | −0.0579 | −0.1425 | 0.061* | |
C33 | 0.1154 (4) | 0.0768 (2) | −0.03714 (19) | 0.0410 (7) | |
C34 | −0.0012 (4) | 0.1363 (3) | −0.0752 (2) | 0.0488 (8) | |
H34 | −0.0555 | 0.1091 | −0.1338 | 0.059* | |
C35 | −0.0337 (4) | 0.2338 (3) | −0.0253 (2) | 0.0479 (8) | |
H35 | −0.1101 | 0.2740 | −0.0497 | 0.057* | |
C36 | 0.0481 (4) | 0.2732 (3) | 0.0625 (2) | 0.0429 (7) | |
H36 | 0.0243 | 0.3400 | 0.0957 | 0.051* | |
C37 | 0.1909 (3) | 0.1223 (2) | 0.05146 (18) | 0.0330 (6) | |
C38 | 0.3084 (4) | 0.0635 (2) | 0.09479 (19) | 0.0349 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0406 (2) | 0.0309 (2) | 0.0278 (2) | −0.00624 (16) | 0.00455 (16) | 0.00766 (15) |
S1 | 0.0365 (4) | 0.0375 (4) | 0.0377 (4) | −0.0014 (3) | 0.0067 (3) | 0.0133 (3) |
O1 | 0.0500 (14) | 0.0340 (11) | 0.0440 (13) | −0.0039 (10) | 0.0210 (11) | 0.0082 (9) |
O2 | 0.100 (2) | 0.0377 (13) | 0.097 (2) | 0.0213 (14) | 0.0628 (19) | 0.0305 (13) |
O3 | 0.0487 (14) | 0.0373 (11) | 0.0437 (13) | −0.0037 (10) | 0.0094 (11) | 0.0045 (10) |
O4 | 0.0392 (14) | 0.0531 (14) | 0.0610 (16) | 0.0046 (12) | 0.0066 (12) | 0.0037 (12) |
O5 | 0.0448 (14) | 0.0427 (12) | 0.0665 (16) | 0.0088 (11) | 0.0040 (12) | 0.0246 (11) |
O6 | 0.0549 (15) | 0.0576 (14) | 0.0338 (12) | −0.0085 (12) | 0.0095 (11) | 0.0108 (10) |
O7 | 0.0585 (15) | 0.0350 (11) | 0.0416 (13) | −0.0008 (10) | 0.0123 (11) | 0.0132 (9) |
O8 | 0.074 (2) | 0.093 (2) | 0.099 (3) | 0.0248 (18) | 0.0105 (18) | 0.0325 (19) |
O9 | 0.076 (2) | 0.098 (2) | 0.0632 (19) | 0.0006 (17) | 0.0277 (16) | 0.0182 (16) |
N1 | 0.0490 (16) | 0.0356 (13) | 0.0282 (13) | 0.0018 (12) | 0.0065 (12) | 0.0083 (10) |
N2 | 0.0423 (15) | 0.0326 (12) | 0.0361 (14) | −0.0062 (11) | 0.0083 (12) | 0.0097 (10) |
N3 | 0.0361 (14) | 0.0367 (13) | 0.0314 (13) | −0.0039 (11) | 0.0046 (11) | 0.0122 (10) |
N4 | 0.0403 (15) | 0.0324 (12) | 0.0304 (13) | −0.0020 (11) | 0.0051 (11) | 0.0094 (10) |
C1 | 0.0477 (19) | 0.0330 (15) | 0.0315 (16) | 0.0000 (14) | 0.0082 (14) | 0.0099 (12) |
C2 | 0.0310 (15) | 0.0305 (14) | 0.0298 (15) | 0.0005 (12) | 0.0044 (12) | 0.0088 (11) |
C3 | 0.0397 (17) | 0.0336 (15) | 0.0383 (17) | 0.0067 (13) | 0.0163 (14) | 0.0085 (12) |
C4 | 0.0339 (16) | 0.0319 (14) | 0.0407 (17) | 0.0042 (13) | 0.0098 (14) | 0.0069 (12) |
C5 | 0.0269 (15) | 0.0332 (14) | 0.0355 (16) | −0.0010 (12) | 0.0039 (12) | 0.0105 (12) |
C6 | 0.0408 (18) | 0.0359 (15) | 0.0408 (17) | 0.0057 (14) | 0.0172 (15) | 0.0073 (13) |
C7 | 0.0416 (18) | 0.0284 (14) | 0.0446 (18) | 0.0071 (13) | 0.0130 (15) | 0.0079 (13) |
C8 | 0.0322 (16) | 0.0310 (14) | 0.0398 (17) | 0.0000 (12) | 0.0090 (13) | 0.0117 (12) |
C9 | 0.0439 (19) | 0.0343 (16) | 0.0468 (19) | 0.0033 (14) | 0.0103 (16) | −0.0007 (13) |
C10 | 0.0350 (18) | 0.0410 (17) | 0.0488 (19) | 0.0066 (14) | 0.0110 (15) | 0.0040 (14) |
C11 | 0.0363 (17) | 0.0323 (14) | 0.0373 (16) | −0.0004 (13) | 0.0092 (14) | 0.0095 (12) |
C12 | 0.045 (2) | 0.0354 (16) | 0.0466 (19) | 0.0025 (15) | 0.0169 (16) | −0.0015 (14) |
C13 | 0.0390 (19) | 0.0399 (17) | 0.058 (2) | 0.0029 (15) | 0.0191 (17) | 0.0044 (15) |
C14 | 0.0428 (18) | 0.0361 (15) | 0.0331 (16) | −0.0006 (14) | 0.0105 (14) | 0.0123 (13) |
C15 | 0.064 (2) | 0.0484 (19) | 0.0363 (18) | 0.0082 (17) | 0.0128 (17) | 0.0155 (15) |
C16 | 0.090 (3) | 0.063 (2) | 0.0310 (18) | 0.025 (2) | 0.0085 (19) | 0.0147 (17) |
C17 | 0.072 (3) | 0.052 (2) | 0.038 (2) | 0.019 (2) | −0.0097 (18) | −0.0011 (16) |
C18 | 0.046 (2) | 0.0341 (16) | 0.047 (2) | 0.0119 (15) | −0.0030 (16) | −0.0005 (14) |
C19 | 0.041 (2) | 0.0381 (18) | 0.072 (3) | 0.0036 (16) | −0.0137 (19) | −0.0041 (17) |
C20 | 0.036 (2) | 0.0347 (17) | 0.092 (3) | −0.0014 (15) | 0.009 (2) | 0.0060 (18) |
C21 | 0.0361 (18) | 0.0296 (15) | 0.075 (3) | 0.0033 (14) | 0.0141 (18) | 0.0113 (15) |
C22 | 0.051 (2) | 0.049 (2) | 0.095 (3) | 0.0008 (18) | 0.036 (2) | 0.027 (2) |
C23 | 0.068 (3) | 0.060 (2) | 0.068 (3) | −0.001 (2) | 0.035 (2) | 0.026 (2) |
C24 | 0.058 (2) | 0.0482 (19) | 0.0444 (19) | −0.0039 (17) | 0.0159 (17) | 0.0172 (15) |
C25 | 0.0378 (17) | 0.0268 (14) | 0.0463 (18) | 0.0018 (13) | 0.0086 (14) | 0.0089 (13) |
C26 | 0.0393 (18) | 0.0295 (14) | 0.0369 (17) | 0.0038 (13) | 0.0019 (14) | 0.0050 (12) |
C27 | 0.045 (2) | 0.052 (2) | 0.0427 (19) | 0.0028 (16) | −0.0008 (16) | 0.0175 (16) |
C28 | 0.052 (2) | 0.054 (2) | 0.057 (2) | 0.0142 (18) | 0.0073 (18) | 0.0222 (18) |
C29 | 0.055 (2) | 0.0418 (18) | 0.061 (2) | 0.0088 (17) | 0.0188 (19) | 0.0104 (16) |
C30 | 0.0438 (19) | 0.0342 (15) | 0.0438 (18) | −0.0015 (14) | 0.0136 (15) | 0.0077 (13) |
C31 | 0.064 (2) | 0.0419 (18) | 0.0426 (19) | 0.0023 (17) | 0.0188 (18) | 0.0019 (15) |
C32 | 0.067 (2) | 0.0476 (19) | 0.0289 (17) | −0.0036 (18) | 0.0071 (16) | 0.0027 (14) |
C33 | 0.049 (2) | 0.0377 (16) | 0.0322 (16) | −0.0075 (14) | 0.0084 (14) | 0.0074 (13) |
C34 | 0.055 (2) | 0.0514 (19) | 0.0327 (17) | −0.0063 (17) | 0.0004 (16) | 0.0138 (15) |
C35 | 0.052 (2) | 0.0494 (19) | 0.0394 (18) | 0.0023 (16) | 0.0007 (16) | 0.0197 (15) |
C36 | 0.048 (2) | 0.0358 (16) | 0.0416 (18) | 0.0030 (15) | 0.0047 (15) | 0.0131 (13) |
C37 | 0.0369 (17) | 0.0295 (14) | 0.0294 (15) | −0.0074 (12) | 0.0055 (13) | 0.0081 (11) |
C38 | 0.0373 (17) | 0.0313 (14) | 0.0340 (16) | −0.0065 (13) | 0.0079 (13) | 0.0092 (12) |
Ni1—O1 | 2.032 (2) | C11—C12 | 1.382 (4) |
Ni1—N2 | 2.083 (2) | C11—C14 | 1.511 (4) |
Ni1—N4 | 2.084 (2) | C12—C13 | 1.381 (4) |
Ni1—N3 | 2.090 (2) | C12—H12 | 0.9300 |
Ni1—N1 | 2.096 (2) | C13—H13 | 0.9300 |
Ni1—O7 | 2.101 (2) | C15—C16 | 1.404 (5) |
S1—O6 | 1.434 (2) | C15—H15 | 0.9300 |
S1—O5 | 1.434 (2) | C16—C17 | 1.359 (6) |
S1—C5 | 1.769 (3) | C16—H16 | 0.9300 |
S1—C8 | 1.769 (3) | C17—C18 | 1.398 (5) |
O1—C1 | 1.253 (3) | C17—H17 | 0.9300 |
O2—C1 | 1.250 (3) | C18—C26 | 1.402 (4) |
O3—C14 | 1.274 (3) | C18—C19 | 1.435 (5) |
O4—C14 | 1.234 (4) | C19—C20 | 1.349 (5) |
O7—H7A | 0.8501 | C19—H19 | 0.9300 |
O7—H7B | 0.8500 | C20—C21 | 1.424 (5) |
O8—H8B | 0.8500 | C20—H20 | 0.9300 |
O8—H8A | 0.8501 | C21—C25 | 1.402 (4) |
O9—H9A | 0.8500 | C21—C22 | 1.407 (5) |
O9—H9B | 0.8500 | C22—C23 | 1.358 (5) |
N1—C15 | 1.325 (4) | C22—H22 | 0.9300 |
N1—C26 | 1.359 (4) | C23—C24 | 1.388 (5) |
N2—C24 | 1.325 (4) | C23—H23 | 0.9300 |
N2—C25 | 1.355 (4) | C24—H24 | 0.9300 |
N3—C27 | 1.325 (4) | C25—C26 | 1.437 (4) |
N3—C38 | 1.358 (4) | C27—C28 | 1.393 (5) |
N4—C36 | 1.319 (4) | C27—H27 | 0.9300 |
N4—C37 | 1.359 (4) | C28—C29 | 1.362 (5) |
C1—C2 | 1.507 (4) | C28—H28 | 0.9300 |
C2—C3 | 1.389 (4) | C29—C30 | 1.400 (5) |
C2—C7 | 1.392 (4) | C29—H29 | 0.9300 |
C3—C4 | 1.378 (4) | C30—C38 | 1.410 (4) |
C3—H3 | 0.9300 | C30—C31 | 1.422 (4) |
C4—C5 | 1.376 (4) | C31—C32 | 1.342 (5) |
C4—H4 | 0.9300 | C31—H31 | 0.9300 |
C5—C6 | 1.385 (4) | C32—C33 | 1.434 (4) |
C6—C7 | 1.383 (4) | C32—H32 | 0.9300 |
C6—H6 | 0.9300 | C33—C37 | 1.398 (4) |
C7—H7 | 0.9300 | C33—C34 | 1.408 (5) |
C8—C9 | 1.369 (4) | C34—C35 | 1.359 (5) |
C8—C13 | 1.384 (4) | C34—H34 | 0.9300 |
C9—C10 | 1.381 (4) | C35—C36 | 1.393 (4) |
C9—H9 | 0.9300 | C35—H35 | 0.9300 |
C10—C11 | 1.389 (4) | C36—H36 | 0.9300 |
C10—H10 | 0.9300 | C37—C38 | 1.445 (4) |
O1—Ni1—N2 | 172.65 (10) | C8—C13—H13 | 120.6 |
O1—Ni1—N4 | 93.11 (9) | O4—C14—O3 | 124.8 (3) |
N2—Ni1—N4 | 93.95 (9) | O4—C14—C11 | 118.2 (3) |
O1—Ni1—N3 | 88.40 (9) | O3—C14—C11 | 117.0 (3) |
N2—Ni1—N3 | 90.82 (9) | N1—C15—C16 | 122.3 (3) |
N4—Ni1—N3 | 79.99 (9) | N1—C15—H15 | 118.9 |
O1—Ni1—N1 | 93.08 (9) | C16—C15—H15 | 118.9 |
N2—Ni1—N1 | 79.81 (10) | C17—C16—C15 | 119.8 (3) |
N4—Ni1—N1 | 173.57 (10) | C17—C16—H16 | 120.1 |
N3—Ni1—N1 | 98.44 (9) | C15—C16—H16 | 120.1 |
O1—Ni1—O7 | 91.59 (8) | C16—C17—C18 | 119.6 (3) |
N2—Ni1—O7 | 89.87 (9) | C16—C17—H17 | 120.2 |
N4—Ni1—O7 | 94.64 (9) | C18—C17—H17 | 120.2 |
N3—Ni1—O7 | 174.62 (9) | C17—C18—C26 | 117.2 (3) |
N1—Ni1—O7 | 86.92 (9) | C17—C18—C19 | 124.0 (3) |
O6—S1—O5 | 119.73 (15) | C26—C18—C19 | 118.8 (3) |
O6—S1—C5 | 108.08 (13) | C20—C19—C18 | 121.1 (3) |
O5—S1—C5 | 107.59 (14) | C20—C19—H19 | 119.4 |
O6—S1—C8 | 106.91 (14) | C18—C19—H19 | 119.4 |
O5—S1—C8 | 107.40 (14) | C19—C20—C21 | 121.4 (3) |
C5—S1—C8 | 106.42 (13) | C19—C20—H20 | 119.3 |
C1—O1—Ni1 | 130.42 (19) | C21—C20—H20 | 119.3 |
Ni1—O7—H7A | 122.9 | C25—C21—C22 | 117.0 (3) |
Ni1—O7—H7B | 101.6 | C25—C21—C20 | 118.7 (3) |
H7A—O7—H7B | 107.1 | C22—C21—C20 | 124.3 (3) |
H8B—O8—H8A | 110.3 | C23—C22—C21 | 120.0 (3) |
H9A—O9—H9B | 109.2 | C23—C22—H22 | 120.0 |
C15—N1—C26 | 117.9 (3) | C21—C22—H22 | 120.0 |
C15—N1—Ni1 | 129.6 (2) | C22—C23—C24 | 119.0 (3) |
C26—N1—Ni1 | 111.85 (19) | C22—C23—H23 | 120.5 |
C24—N2—C25 | 118.1 (3) | C24—C23—H23 | 120.5 |
C24—N2—Ni1 | 129.2 (2) | N2—C24—C23 | 123.2 (3) |
C25—N2—Ni1 | 112.66 (19) | N2—C24—H24 | 118.4 |
C27—N3—C38 | 117.6 (3) | C23—C24—H24 | 118.4 |
C27—N3—Ni1 | 129.7 (2) | N2—C25—C21 | 122.6 (3) |
C38—N3—Ni1 | 112.73 (19) | N2—C25—C26 | 117.2 (3) |
C36—N4—C37 | 117.8 (3) | C21—C25—C26 | 120.2 (3) |
C36—N4—Ni1 | 129.3 (2) | N1—C26—C18 | 123.2 (3) |
C37—N4—Ni1 | 112.90 (19) | N1—C26—C25 | 117.3 (3) |
O2—C1—O1 | 126.0 (3) | C18—C26—C25 | 119.5 (3) |
O2—C1—C2 | 118.1 (3) | N3—C27—C28 | 123.2 (3) |
O1—C1—C2 | 115.9 (3) | N3—C27—H27 | 118.4 |
C3—C2—C7 | 118.8 (3) | C28—C27—H27 | 118.4 |
C3—C2—C1 | 119.7 (3) | C29—C28—C27 | 119.3 (3) |
C7—C2—C1 | 121.5 (3) | C29—C28—H28 | 120.3 |
C4—C3—C2 | 121.0 (3) | C27—C28—H28 | 120.3 |
C4—C3—H3 | 119.5 | C28—C29—C30 | 119.9 (3) |
C2—C3—H3 | 119.5 | C28—C29—H29 | 120.1 |
C5—C4—C3 | 119.4 (3) | C30—C29—H29 | 120.1 |
C5—C4—H4 | 120.3 | C29—C30—C38 | 116.9 (3) |
C3—C4—H4 | 120.3 | C29—C30—C31 | 124.7 (3) |
C4—C5—C6 | 120.9 (3) | C38—C30—C31 | 118.4 (3) |
C4—C5—S1 | 118.1 (2) | C32—C31—C30 | 122.1 (3) |
C6—C5—S1 | 120.9 (2) | C32—C31—H31 | 118.9 |
C7—C6—C5 | 119.2 (3) | C30—C31—H31 | 118.9 |
C7—C6—H6 | 120.4 | C31—C32—C33 | 121.0 (3) |
C5—C6—H6 | 120.4 | C31—C32—H32 | 119.5 |
C6—C7—C2 | 120.6 (3) | C33—C32—H32 | 119.5 |
C6—C7—H7 | 119.7 | C37—C33—C34 | 117.1 (3) |
C2—C7—H7 | 119.7 | C37—C33—C32 | 119.0 (3) |
C9—C8—C13 | 120.7 (3) | C34—C33—C32 | 123.9 (3) |
C9—C8—S1 | 119.1 (2) | C35—C34—C33 | 119.3 (3) |
C13—C8—S1 | 119.9 (2) | C35—C34—H34 | 120.3 |
C8—C9—C10 | 119.7 (3) | C33—C34—H34 | 120.3 |
C8—C9—H9 | 120.2 | C34—C35—C36 | 119.7 (3) |
C10—C9—H9 | 120.2 | C34—C35—H35 | 120.2 |
C9—C10—C11 | 120.9 (3) | C36—C35—H35 | 120.2 |
C9—C10—H10 | 119.6 | N4—C36—C35 | 123.0 (3) |
C11—C10—H10 | 119.6 | N4—C36—H36 | 118.5 |
C12—C11—C10 | 118.2 (3) | C35—C36—H36 | 118.5 |
C12—C11—C14 | 122.5 (3) | N4—C37—C33 | 123.2 (3) |
C10—C11—C14 | 119.3 (3) | N4—C37—C38 | 117.1 (3) |
C11—C12—C13 | 121.5 (3) | C33—C37—C38 | 119.7 (3) |
C11—C12—H12 | 119.2 | N3—C38—C30 | 123.1 (3) |
C13—C12—H12 | 119.2 | N3—C38—C37 | 117.1 (3) |
C12—C13—C8 | 118.9 (3) | C30—C38—C37 | 119.8 (3) |
C12—C13—H13 | 120.6 | ||
N2—Ni1—O1—C1 | 90.2 (7) | C9—C8—C13—C12 | −2.9 (5) |
N4—Ni1—O1—C1 | −105.9 (3) | S1—C8—C13—C12 | 171.2 (3) |
N3—Ni1—O1—C1 | 174.2 (3) | C12—C11—C14—O4 | −168.8 (3) |
N1—Ni1—O1—C1 | 75.8 (3) | C10—C11—C14—O4 | 12.7 (4) |
O7—Ni1—O1—C1 | −11.2 (3) | C12—C11—C14—O3 | 11.6 (4) |
O1—Ni1—N1—C15 | −1.3 (3) | C10—C11—C14—O3 | −166.8 (3) |
N2—Ni1—N1—C15 | −179.4 (3) | C26—N1—C15—C16 | 0.9 (5) |
N4—Ni1—N1—C15 | −165.6 (7) | Ni1—N1—C15—C16 | −169.5 (2) |
N3—Ni1—N1—C15 | −90.1 (3) | N1—C15—C16—C17 | 0.5 (5) |
O7—Ni1—N1—C15 | 90.2 (3) | C15—C16—C17—C18 | −1.1 (5) |
O1—Ni1—N1—C26 | −172.2 (2) | C16—C17—C18—C26 | 0.3 (5) |
N2—Ni1—N1—C26 | 9.69 (19) | C16—C17—C18—C19 | −178.8 (3) |
N4—Ni1—N1—C26 | 23.5 (9) | C17—C18—C19—C20 | 175.9 (3) |
N3—Ni1—N1—C26 | 99.0 (2) | C26—C18—C19—C20 | −3.2 (5) |
O7—Ni1—N1—C26 | −80.7 (2) | C18—C19—C20—C21 | 1.4 (5) |
O1—Ni1—N2—C24 | 159.9 (6) | C19—C20—C21—C25 | 3.0 (5) |
N4—Ni1—N2—C24 | −4.0 (3) | C19—C20—C21—C22 | −179.2 (3) |
N3—Ni1—N2—C24 | 76.0 (3) | C25—C21—C22—C23 | 0.8 (5) |
N1—Ni1—N2—C24 | 174.5 (3) | C20—C21—C22—C23 | −177.1 (3) |
O7—Ni1—N2—C24 | −98.6 (3) | C21—C22—C23—C24 | 1.5 (6) |
O1—Ni1—N2—C25 | −22.6 (8) | C25—N2—C24—C23 | 0.1 (5) |
N4—Ni1—N2—C25 | 173.5 (2) | Ni1—N2—C24—C23 | 177.5 (3) |
N3—Ni1—N2—C25 | −106.4 (2) | C22—C23—C24—N2 | −2.1 (6) |
N1—Ni1—N2—C25 | −8.00 (19) | C24—N2—C25—C21 | 2.4 (4) |
O7—Ni1—N2—C25 | 78.9 (2) | Ni1—N2—C25—C21 | −175.4 (2) |
O1—Ni1—N3—C27 | −84.5 (3) | C24—N2—C25—C26 | −177.0 (3) |
N2—Ni1—N3—C27 | 88.1 (3) | Ni1—N2—C25—C26 | 5.2 (3) |
N4—Ni1—N3—C27 | −178.0 (3) | C22—C21—C25—N2 | −2.8 (4) |
N1—Ni1—N3—C27 | 8.3 (3) | C20—C21—C25—N2 | 175.2 (3) |
O7—Ni1—N3—C27 | −174.5 (8) | C22—C21—C25—C26 | 176.5 (3) |
O1—Ni1—N3—C38 | 97.0 (2) | C20—C21—C25—C26 | −5.5 (4) |
N2—Ni1—N3—C38 | −90.3 (2) | C15—N1—C26—C18 | −1.8 (4) |
N4—Ni1—N3—C38 | 3.58 (19) | Ni1—N1—C26—C18 | 170.3 (2) |
N1—Ni1—N3—C38 | −170.10 (19) | C15—N1—C26—C25 | 177.9 (3) |
O7—Ni1—N3—C38 | 7.1 (10) | Ni1—N1—C26—C25 | −10.1 (3) |
O1—Ni1—N4—C36 | 89.8 (3) | C17—C18—C26—N1 | 1.2 (4) |
N2—Ni1—N4—C36 | −92.3 (3) | C19—C18—C26—N1 | −179.7 (3) |
N3—Ni1—N4—C36 | 177.6 (3) | C17—C18—C26—C25 | −178.5 (3) |
N1—Ni1—N4—C36 | −105.9 (8) | C19—C18—C26—C25 | 0.7 (4) |
O7—Ni1—N4—C36 | −2.1 (3) | N2—C25—C26—N1 | 3.4 (4) |
O1—Ni1—N4—C37 | −90.94 (19) | C21—C25—C26—N1 | −176.0 (3) |
N2—Ni1—N4—C37 | 87.02 (19) | N2—C25—C26—C18 | −176.9 (3) |
N3—Ni1—N4—C37 | −3.12 (18) | C21—C25—C26—C18 | 3.7 (4) |
N1—Ni1—N4—C37 | 73.4 (9) | C38—N3—C27—C28 | 0.5 (5) |
O7—Ni1—N4—C37 | 177.21 (19) | Ni1—N3—C27—C28 | −177.8 (2) |
Ni1—O1—C1—O2 | 8.7 (5) | N3—C27—C28—C29 | 0.2 (5) |
Ni1—O1—C1—C2 | −170.40 (19) | C27—C28—C29—C30 | −0.7 (5) |
O2—C1—C2—C3 | 176.4 (3) | C28—C29—C30—C38 | 0.3 (5) |
O1—C1—C2—C3 | −4.4 (4) | C28—C29—C30—C31 | −177.7 (3) |
O2—C1—C2—C7 | −5.5 (5) | C29—C30—C31—C32 | 177.5 (3) |
O1—C1—C2—C7 | 173.7 (3) | C38—C30—C31—C32 | −0.5 (5) |
C7—C2—C3—C4 | 0.1 (4) | C30—C31—C32—C33 | 0.4 (5) |
C1—C2—C3—C4 | 178.3 (3) | C31—C32—C33—C37 | 0.2 (5) |
C2—C3—C4—C5 | −1.7 (5) | C31—C32—C33—C34 | −178.7 (3) |
C3—C4—C5—C6 | 1.4 (5) | C37—C33—C34—C35 | 0.6 (5) |
C3—C4—C5—S1 | −175.7 (2) | C32—C33—C34—C35 | 179.4 (3) |
O6—S1—C5—C4 | 156.6 (2) | C33—C34—C35—C36 | −0.3 (5) |
O5—S1—C5—C4 | 26.0 (3) | C37—N4—C36—C35 | −0.2 (5) |
C8—S1—C5—C4 | −88.9 (3) | Ni1—N4—C36—C35 | 179.0 (2) |
O6—S1—C5—C6 | −20.5 (3) | C34—C35—C36—N4 | 0.1 (5) |
O5—S1—C5—C6 | −151.1 (2) | C36—N4—C37—C33 | 0.5 (4) |
C8—S1—C5—C6 | 94.0 (3) | Ni1—N4—C37—C33 | −178.8 (2) |
C4—C5—C6—C7 | 0.4 (5) | C36—N4—C37—C38 | −178.4 (3) |
S1—C5—C6—C7 | 177.4 (2) | Ni1—N4—C37—C38 | 2.2 (3) |
C5—C6—C7—C2 | −2.0 (5) | C34—C33—C37—N4 | −0.7 (4) |
C3—C2—C7—C6 | 1.7 (5) | C32—C33—C37—N4 | −179.7 (3) |
C1—C2—C7—C6 | −176.4 (3) | C34—C33—C37—C38 | 178.2 (3) |
O6—S1—C8—C9 | 21.8 (3) | C32—C33—C37—C38 | −0.8 (4) |
O5—S1—C8—C9 | 151.5 (2) | C27—N3—C38—C30 | −0.9 (4) |
C5—S1—C8—C9 | −93.5 (3) | Ni1—N3—C38—C30 | 177.8 (2) |
O6—S1—C8—C13 | −152.4 (3) | C27—N3—C38—C37 | 177.8 (3) |
O5—S1—C8—C13 | −22.8 (3) | Ni1—N3—C38—C37 | −3.5 (3) |
C5—S1—C8—C13 | 92.2 (3) | C29—C30—C38—N3 | 0.4 (4) |
C13—C8—C9—C10 | 1.8 (5) | C31—C30—C38—N3 | 178.6 (3) |
S1—C8—C9—C10 | −172.4 (3) | C29—C30—C38—C37 | −178.2 (3) |
C8—C9—C10—C11 | 1.1 (5) | C31—C30—C38—C37 | 0.0 (4) |
C9—C10—C11—C12 | −2.7 (5) | N4—C37—C38—N3 | 0.9 (4) |
C9—C10—C11—C14 | 175.8 (3) | C33—C37—C38—N3 | −178.1 (3) |
C10—C11—C12—C13 | 1.5 (5) | N4—C37—C38—C30 | 179.6 (3) |
C14—C11—C12—C13 | −177.0 (3) | C33—C37—C38—C30 | 0.7 (4) |
C11—C12—C13—C8 | 1.3 (5) |
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7A···O3i | 0.85 | 2.02 | 2.865 (3) | 174 |
O7—H7B···O2 | 0.85 | 1.82 | 2.633 (3) | 159 |
O8—H8B···O9 | 0.85 | 2.08 | 2.897 (4) | 160 |
O8—H8A···O4 | 0.85 | 2.13 | 2.907 (4) | 152 |
O9—H9A···O3ii | 0.85 | 2.04 | 2.879 (3) | 171 |
O9—H9B···O3 | 0.85 | 2.15 | 2.993 (4) | 171 |
Symmetry codes: (i) x+1, y+1, z; (ii) −x−2, −y−1, −z. |
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