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In the dinuclear and centrosymmetric title complex, μ-fumarato-bis[aquabis(1,10-phenanthroline)nickel(II)] fumarate hexadecahydrate, [Ni2(C4H2O4)(C12H8N2)4(H2O)2](C4H2O4)·16H2O or [Ni2(phen)4L(H2O)2]L·16H2O, where phen = 1,10-phenanthroline and L2− = fumarate, the nickel(II) cation is six-coordinated by two O atoms, one from a water molecule and the other from one end of a bridging L2− anion, and four N atoms from two bidentate phen ligands. Each of the two independent L2− anions is located about an inversion centre. Interestingly, one L2− anion is bridging and the other acts as a counter-ion. The [Ni2(phen)4L(H2O)2]2+ cations, water molecules and L2− anions are connected through complex hydrogen-bonding interactions to form a three-dimensional structure.
Supporting information
CCDC reference: 225670
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.008 Å
- R factor = 0.057
- wR factor = 0.143
- Data-to-parameter ratio = 13.6
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.99
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 9
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3
H2 O
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 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
2 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: XSCANS (Siemens, 1994); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990); software used to prepare material for publication: SHELXL97.
Crystal data top
[Ni2(C12H8N2)4(C4H2O4)(H2O)2]C4H2O4·16H2O | Z = 1 |
Mr = 1390.60 | F(000) = 728 |
Triclinic, P1 | Dx = 1.402 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.736 (4) Å | Cell parameters from 22 reflections |
b = 10.903 (3) Å | θ = 4.7–9.3° |
c = 14.802 (5) Å | µ = 0.66 mm−1 |
α = 86.68 (3)° | T = 293 K |
β = 86.27 (3)° | Block, green |
γ = 72.46 (3)° | 0.44 × 0.35 × 0.32 mm |
V = 1647.3 (10) Å3 | |
Data collection top
Siemens P4 diffractometer | 3577 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.022 |
Graphite monochromator | θmax = 26.0°, θmin = 2.0° |
ω scan | h = −1→13 |
Absorption correction: ψ scan (North et al., 1968) | k = −13→13 |
Tmin = 0.734, Tmax = 0.810 | l = −18→18 |
7676 measured reflections | 3 standard reflections every 97 reflections |
6365 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)] = 0.057 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.143 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.88 | w = 1/[σ2(Fo2) + (0.0653P)2] where P = (Fo2 + 2Fc2)/3 |
6365 reflections | (Δ/σ)max < 0.001 |
469 parameters | Δρmax = 0.63 e Å−3 |
33 restraints | Δρmin = −0.49 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 | Uiso*/Ueq | |
C1 | 0.0557 (5) | 0.0474 (5) | 0.1107 (3) | 0.0446 (12) | |
C2 | 0.0331 (5) | −0.0263 (5) | 0.0352 (3) | 0.0463 (12) | |
H2 | 0.0683 | −0.1154 | 0.0384 | 0.056* | |
C3 | 0.9680 (6) | 0.4876 (5) | 0.3742 (4) | 0.0533 (13) | |
C4 | 0.9521 (5) | 0.5176 (5) | 0.4725 (4) | 0.0569 (14) | |
H4 | 0.8696 | 0.5636 | 0.4956 | 0.068* | |
C101 | 0.0994 (5) | −0.1304 (5) | 0.3551 (3) | 0.0506 (13) | |
H101 | 0.0731 | −0.1414 | 0.2982 | 0.061* | |
C102 | 0.0633 (6) | −0.1998 (5) | 0.4303 (4) | 0.0658 (17) | |
H102 | 0.0138 | −0.2552 | 0.4234 | 0.079* | |
C103 | 0.1028 (6) | −0.1838 (6) | 0.5134 (4) | 0.077 (2) | |
H103 | 0.0814 | −0.2299 | 0.5638 | 0.092* | |
C104 | 0.1745 (6) | −0.0993 (5) | 0.5233 (3) | 0.0591 (15) | |
C105 | 0.2185 (7) | −0.0734 (7) | 0.6079 (4) | 0.082 (2) | |
H105 | 0.2001 | −0.1175 | 0.6603 | 0.098* | |
C106 | 0.2846 (7) | 0.0114 (7) | 0.6143 (4) | 0.088 (2) | |
H106 | 0.3103 | 0.0257 | 0.6705 | 0.105* | |
C107 | 0.3164 (6) | 0.0811 (6) | 0.5350 (3) | 0.0642 (16) | |
C108 | 0.3850 (7) | 0.1707 (7) | 0.5354 (4) | 0.083 (2) | |
H108 | 0.4132 | 0.1893 | 0.5896 | 0.100* | |
C109 | 0.4107 (6) | 0.2310 (6) | 0.4572 (5) | 0.0795 (19) | |
H109 | 0.4552 | 0.2921 | 0.4577 | 0.095* | |
C110 | 0.3703 (5) | 0.2012 (5) | 0.3755 (4) | 0.0576 (14) | |
H110 | 0.3907 | 0.2416 | 0.3220 | 0.069* | |
C111 | 0.2764 (5) | 0.0567 (5) | 0.4505 (3) | 0.0454 (12) | |
C112 | 0.2054 (5) | −0.0337 (4) | 0.4442 (3) | 0.0420 (11) | |
C201 | 0.4507 (5) | −0.1939 (5) | 0.2532 (3) | 0.0507 (13) | |
H201 | 0.3979 | −0.2280 | 0.2931 | 0.061* | |
C202 | 0.5744 (6) | −0.2738 (5) | 0.2259 (4) | 0.0633 (15) | |
H202 | 0.6025 | −0.3593 | 0.2469 | 0.076* | |
C203 | 0.6526 (6) | −0.2250 (6) | 0.1685 (4) | 0.0691 (17) | |
H203 | 0.7356 | −0.2768 | 0.1507 | 0.083* | |
C204 | 0.6084 (5) | −0.0950 (5) | 0.1353 (3) | 0.0560 (14) | |
C205 | 0.6819 (6) | −0.0385 (7) | 0.0732 (4) | 0.0759 (18) | |
H205 | 0.7658 | −0.0863 | 0.0540 | 0.091* | |
C206 | 0.6319 (6) | 0.0856 (7) | 0.0406 (4) | 0.0782 (19) | |
H206 | 0.6815 | 0.1200 | −0.0016 | 0.094* | |
C207 | 0.5049 (5) | 0.1632 (5) | 0.0704 (3) | 0.0541 (13) | |
C208 | 0.4465 (7) | 0.2905 (6) | 0.0385 (4) | 0.0695 (17) | |
H208 | 0.4928 | 0.3307 | −0.0021 | 0.083* | |
C209 | 0.3223 (6) | 0.3546 (6) | 0.0672 (3) | 0.0656 (16) | |
H209 | 0.2822 | 0.4379 | 0.0451 | 0.079* | |
C210 | 0.2558 (5) | 0.2941 (5) | 0.1303 (3) | 0.0544 (13) | |
H210 | 0.1714 | 0.3398 | 0.1501 | 0.065* | |
C211 | 0.4286 (5) | 0.1093 (5) | 0.1334 (3) | 0.0428 (11) | |
C212 | 0.4832 (5) | −0.0226 (5) | 0.1662 (3) | 0.0417 (11) | |
N1 | 0.1686 (4) | −0.0508 (3) | 0.3618 (2) | 0.0402 (9) | |
N2 | 0.3043 (4) | 0.1178 (4) | 0.3719 (2) | 0.0431 (10) | |
N3 | 0.4055 (4) | −0.0715 (4) | 0.2246 (2) | 0.0401 (9) | |
N4 | 0.3067 (4) | 0.1736 (4) | 0.1641 (2) | 0.0416 (9) | |
O1 | 0.1446 (3) | −0.0129 (3) | 0.16211 (19) | 0.0450 (8) | |
O2 | −0.0097 (4) | 0.1634 (4) | 0.1174 (3) | 0.0855 (14) | |
O3 | 1.0781 (4) | 0.4334 (4) | 0.3386 (3) | 0.0684 (11) | |
O4 | 0.8644 (4) | 0.5190 (4) | 0.3323 (3) | 0.0810 (13) | |
OW1 | 0.0543 (3) | 0.2098 (3) | 0.2789 (2) | 0.0441 (8) | |
OW2 | 0.3940 (4) | −0.3808 (4) | 0.4223 (3) | 0.0706 (11) | |
OW3 | 0.3520 (4) | 0.5473 (5) | 0.6029 (3) | 0.0770 (12) | |
OW4 | 0.2876 (5) | 0.5299 (4) | 0.2810 (3) | 0.0742 (12) | |
OW5 | 0.9106 (5) | 0.4839 (5) | 0.1472 (4) | 0.0956 (15) | |
OW6 | 0.7294 (5) | 0.3541 (6) | 0.0993 (4) | 0.1202 (19) | |
OW7 | 0.4464 (5) | 0.6379 (5) | 0.7500 (3) | 0.1004 (16) | |
OW8 | 0.2373 (8) | 0.7051 (5) | 0.1336 (4) | 0.140 (3) | |
OW9 | 1.0125 (9) | 0.6600 (6) | 0.0530 (4) | 0.156 (3) | |
Ni | 0.22718 (6) | 0.06337 (6) | 0.25907 (4) | 0.03582 (19) | |
H11 | 0.065 (5) | 0.270 (3) | 0.302 (3) | 0.043* | |
H12 | 0.033 (4) | 0.211 (4) | 0.2288 (17) | 0.043* | |
H21 | 0.363 (4) | −0.403 (4) | 0.468 (2) | 0.043* | |
H22 | 0.464 (3) | −0.432 (4) | 0.410 (3) | 0.043* | |
H31 | 0.288 (3) | 0.530 (5) | 0.622 (3) | 0.043* | |
H32 | 0.362 (4) | 0.592 (4) | 0.643 (2) | 0.043* | |
H41 | 0.290 (5) | 0.561 (4) | 0.330 (2) | 0.043* | |
H42 | 0.220 (3) | 0.512 (5) | 0.301 (3) | 0.043* | |
H51 | 0.845 (3) | 0.471 (4) | 0.131 (3) | 0.043* | |
H52 | 0.889 (4) | 0.535 (3) | 0.1849 (17) | 0.043* | |
H61 | 0.735 (4) | 0.352 (3) | 0.0320 (12) | 0.043* | |
H62 | 0.791 (3) | 0.288 (2) | 0.1068 (15) | 0.043* | |
H71 | 0.499 (3) | 0.578 (3) | 0.761 (2) | 0.043* | |
H72 | 0.419 (4) | 0.653 (4) | 0.8138 (14) | 0.043* | |
H81 | 0.237 (4) | 0.670 (3) | 0.176 (2) | 0.043* | |
H82 | 0.216 (5) | 0.7794 (19) | 0.132 (3) | 0.043* | |
H91 | 1.001 (4) | 0.668 (3) | 0.1042 (15) | 0.043* | |
H92 | 1.007 (5) | 0.589 (2) | 0.0506 (19) | 0.043* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.044 (3) | 0.044 (3) | 0.043 (3) | −0.008 (2) | −0.006 (2) | −0.004 (2) |
C2 | 0.046 (3) | 0.049 (3) | 0.042 (3) | −0.010 (2) | −0.011 (2) | −0.003 (2) |
C3 | 0.059 (4) | 0.045 (3) | 0.060 (3) | −0.024 (3) | 0.006 (3) | −0.003 (3) |
C4 | 0.058 (4) | 0.046 (3) | 0.069 (4) | −0.021 (3) | 0.007 (3) | −0.005 (3) |
C101 | 0.052 (3) | 0.044 (3) | 0.056 (3) | −0.016 (3) | 0.002 (3) | 0.001 (2) |
C102 | 0.058 (4) | 0.047 (3) | 0.089 (4) | −0.017 (3) | 0.023 (3) | 0.012 (3) |
C103 | 0.078 (5) | 0.058 (4) | 0.071 (4) | 0.004 (3) | 0.035 (4) | 0.023 (3) |
C104 | 0.059 (4) | 0.052 (3) | 0.048 (3) | 0.005 (3) | 0.013 (3) | 0.010 (2) |
C105 | 0.090 (5) | 0.090 (5) | 0.033 (3) | 0.018 (4) | 0.003 (3) | 0.018 (3) |
C106 | 0.099 (6) | 0.111 (6) | 0.035 (3) | −0.002 (5) | −0.018 (3) | 0.000 (3) |
C107 | 0.062 (4) | 0.076 (4) | 0.041 (3) | 0.005 (3) | −0.015 (3) | −0.012 (3) |
C108 | 0.085 (5) | 0.097 (5) | 0.064 (4) | −0.010 (4) | −0.039 (4) | −0.029 (4) |
C109 | 0.077 (5) | 0.083 (5) | 0.088 (5) | −0.030 (4) | −0.027 (4) | −0.028 (4) |
C110 | 0.063 (4) | 0.062 (3) | 0.057 (3) | −0.030 (3) | −0.009 (3) | −0.011 (3) |
C111 | 0.041 (3) | 0.048 (3) | 0.039 (3) | 0.001 (2) | −0.007 (2) | −0.003 (2) |
C112 | 0.040 (3) | 0.042 (3) | 0.033 (2) | 0.003 (2) | 0.002 (2) | 0.005 (2) |
C201 | 0.059 (3) | 0.051 (3) | 0.040 (3) | −0.013 (3) | −0.006 (2) | 0.000 (2) |
C202 | 0.072 (4) | 0.051 (3) | 0.056 (3) | −0.002 (3) | −0.006 (3) | 0.000 (3) |
C203 | 0.056 (4) | 0.070 (4) | 0.068 (4) | 0.003 (3) | 0.004 (3) | −0.015 (3) |
C204 | 0.043 (3) | 0.068 (4) | 0.053 (3) | −0.012 (3) | 0.009 (3) | −0.010 (3) |
C205 | 0.057 (4) | 0.086 (5) | 0.077 (4) | −0.015 (4) | 0.020 (3) | −0.008 (4) |
C206 | 0.067 (4) | 0.103 (5) | 0.069 (4) | −0.037 (4) | 0.025 (3) | −0.004 (4) |
C207 | 0.057 (4) | 0.068 (4) | 0.040 (3) | −0.026 (3) | 0.005 (2) | 0.005 (3) |
C208 | 0.085 (5) | 0.081 (4) | 0.049 (3) | −0.039 (4) | 0.007 (3) | 0.009 (3) |
C209 | 0.086 (5) | 0.058 (4) | 0.049 (3) | −0.022 (3) | 0.001 (3) | 0.019 (3) |
C210 | 0.055 (3) | 0.057 (3) | 0.047 (3) | −0.011 (3) | −0.005 (3) | 0.008 (2) |
C211 | 0.044 (3) | 0.053 (3) | 0.033 (2) | −0.017 (2) | −0.001 (2) | −0.002 (2) |
C212 | 0.043 (3) | 0.053 (3) | 0.030 (2) | −0.015 (2) | −0.005 (2) | 0.001 (2) |
N1 | 0.043 (2) | 0.042 (2) | 0.037 (2) | −0.014 (2) | 0.0013 (18) | 0.0017 (17) |
N2 | 0.051 (3) | 0.043 (2) | 0.037 (2) | −0.014 (2) | −0.0071 (18) | −0.0023 (17) |
N3 | 0.042 (2) | 0.048 (2) | 0.0321 (19) | −0.016 (2) | −0.0053 (17) | −0.0028 (17) |
N4 | 0.041 (2) | 0.043 (2) | 0.039 (2) | −0.010 (2) | −0.0012 (18) | 0.0014 (17) |
O1 | 0.047 (2) | 0.048 (2) | 0.0385 (17) | −0.0095 (17) | −0.0135 (15) | −0.0029 (14) |
O2 | 0.096 (3) | 0.061 (3) | 0.085 (3) | 0.015 (2) | −0.051 (3) | −0.029 (2) |
O3 | 0.058 (3) | 0.075 (3) | 0.076 (3) | −0.025 (2) | 0.006 (2) | −0.026 (2) |
O4 | 0.063 (3) | 0.105 (3) | 0.068 (3) | −0.017 (3) | −0.005 (2) | 0.005 (2) |
OW1 | 0.052 (2) | 0.046 (2) | 0.0341 (17) | −0.0131 (18) | −0.0010 (16) | −0.0094 (15) |
OW2 | 0.060 (3) | 0.084 (3) | 0.059 (2) | −0.010 (2) | −0.002 (2) | 0.006 (2) |
OW3 | 0.059 (3) | 0.108 (4) | 0.064 (3) | −0.026 (3) | −0.010 (2) | 0.008 (2) |
OW4 | 0.075 (3) | 0.085 (3) | 0.070 (3) | −0.033 (3) | −0.013 (3) | 0.004 (2) |
OW5 | 0.106 (4) | 0.085 (3) | 0.091 (3) | −0.021 (3) | −0.001 (3) | −0.010 (3) |
OW6 | 0.092 (4) | 0.135 (5) | 0.125 (4) | −0.022 (4) | −0.008 (4) | 0.004 (4) |
OW7 | 0.098 (4) | 0.107 (4) | 0.091 (3) | −0.022 (3) | −0.005 (3) | −0.009 (3) |
OW8 | 0.242 (7) | 0.060 (3) | 0.114 (4) | −0.031 (4) | −0.090 (5) | 0.026 (3) |
OW9 | 0.231 (8) | 0.148 (6) | 0.115 (5) | −0.100 (6) | 0.000 (5) | 0.005 (4) |
Ni | 0.0397 (4) | 0.0413 (3) | 0.0274 (3) | −0.0137 (3) | −0.0030 (2) | 0.0006 (2) |
Geometric parameters (Å, º) top
C1—O2 | 1.254 (5) | C204—C212 | 1.400 (6) |
C1—O1 | 1.257 (5) | C204—C205 | 1.407 (8) |
C1—C2 | 1.487 (6) | C205—C206 | 1.368 (8) |
C2—C2i | 1.305 (8) | C205—H205 | 0.9300 |
C2—H2 | 0.9300 | C206—C207 | 1.428 (8) |
C3—O3 | 1.248 (6) | C206—H206 | 0.9300 |
C3—O4 | 1.254 (6) | C207—C208 | 1.407 (7) |
C3—C4 | 1.498 (7) | C207—C211 | 1.419 (6) |
C4—C4ii | 1.305 (10) | C208—C209 | 1.358 (8) |
C4—H4 | 0.9300 | C208—H208 | 0.9300 |
C101—N1 | 1.312 (6) | C209—C210 | 1.394 (7) |
C101—C102 | 1.409 (7) | C209—H209 | 0.9300 |
C101—H101 | 0.9300 | C210—N4 | 1.343 (6) |
C102—C103 | 1.364 (8) | C210—H210 | 0.9300 |
C102—H102 | 0.9300 | C211—N4 | 1.348 (6) |
C103—C104 | 1.385 (9) | C211—C212 | 1.447 (6) |
C103—H103 | 0.9300 | C212—N3 | 1.360 (6) |
C104—C112 | 1.411 (6) | Ni—O1 | 2.070 (3) |
C104—C105 | 1.439 (8) | Ni—OW1 | 2.068 (4) |
C105—C106 | 1.335 (9) | Ni—N1 | 2.094 (4) |
C105—H105 | 0.9300 | Ni—N2 | 2.102 (4) |
C106—C107 | 1.440 (9) | Ni—N3 | 2.086 (4) |
C106—H106 | 0.9300 | Ni—N4 | 2.102 (4) |
C107—C108 | 1.389 (9) | OW1—H11 | 0.80 (2) |
C107—C111 | 1.414 (7) | OW1—H12 | 0.79 (2) |
C108—C109 | 1.352 (9) | OW2—H21 | 0.80 (2) |
C108—H108 | 0.9300 | OW2—H22 | 0.80 (2) |
C109—C110 | 1.398 (7) | OW3—H31 | 0.80 (2) |
C109—H109 | 0.9300 | OW3—H32 | 0.82 (4) |
C110—N2 | 1.315 (6) | OW4—H41 | 0.82 (2) |
C110—H110 | 0.9300 | OW4—H42 | 0.84 (2) |
C111—N2 | 1.368 (6) | OW5—H51 | 0.81 (4) |
C111—C112 | 1.425 (7) | OW5—H52 | 0.786 (19) |
C112—N1 | 1.346 (5) | OW6—H61 | 0.996 (16) |
C201—N3 | 1.329 (6) | OW6—H62 | 0.824 (19) |
C201—C202 | 1.400 (7) | OW7—H71 | 0.744 (19) |
C201—H201 | 0.9300 | OW7—H72 | 0.979 (16) |
C202—C203 | 1.355 (8) | OW8—H81 | 0.716 (19) |
C202—H202 | 0.9300 | OW8—H82 | 0.772 (19) |
C203—C204 | 1.422 (8) | OW9—H91 | 0.765 (19) |
C203—H203 | 0.9300 | OW9—H92 | 0.797 (15) |
| | | |
O2—C1—O1 | 124.9 (4) | C204—C205—H205 | 119.5 |
O2—C1—C2 | 119.4 (4) | C205—C206—C207 | 121.1 (5) |
O1—C1—C2 | 115.7 (4) | C205—C206—H206 | 119.4 |
C2i—C2—C1 | 124.0 (6) | C207—C206—H206 | 119.4 |
C2i—C2—H2 | 118.0 | C208—C207—C211 | 116.7 (5) |
C1—C2—H2 | 118.0 | C208—C207—C206 | 124.1 (5) |
O3—C3—O4 | 123.7 (5) | C211—C207—C206 | 119.2 (5) |
O3—C3—C4 | 120.8 (5) | C209—C208—C207 | 120.0 (5) |
O4—C3—C4 | 115.5 (5) | C209—C208—H208 | 120.0 |
C4ii—C4—C3 | 123.4 (7) | C207—C208—H208 | 120.0 |
C4ii—C4—H4 | 118.3 | C208—C209—C210 | 119.1 (5) |
C3—C4—H4 | 118.3 | C208—C209—H209 | 120.4 |
N1—C101—C102 | 122.8 (5) | C210—C209—H209 | 120.4 |
N1—C101—H101 | 118.6 | N4—C210—C209 | 123.7 (5) |
C102—C101—H101 | 118.6 | N4—C210—H210 | 118.2 |
C103—C102—C101 | 118.4 (6) | C209—C210—H210 | 118.2 |
C103—C102—H102 | 120.8 | N4—C211—C207 | 123.7 (5) |
C101—C102—H102 | 120.8 | N4—C211—C212 | 117.7 (4) |
C102—C103—C104 | 120.5 (5) | C207—C211—C212 | 118.6 (5) |
C102—C103—H103 | 119.8 | N3—C212—C204 | 123.1 (4) |
C104—C103—H103 | 119.8 | N3—C212—C211 | 116.7 (4) |
C103—C104—C112 | 117.1 (5) | C204—C212—C211 | 120.2 (4) |
C103—C104—C105 | 124.9 (6) | C101—N1—C112 | 118.6 (4) |
C112—C104—C105 | 118.0 (6) | C101—N1—Ni | 128.2 (3) |
C106—C105—C104 | 122.6 (6) | C112—N1—Ni | 113.1 (3) |
C106—C105—H105 | 118.7 | C110—N2—C111 | 118.8 (4) |
C104—C105—H105 | 118.7 | C110—N2—Ni | 129.0 (3) |
C105—C106—C107 | 120.7 (6) | C111—N2—Ni | 112.2 (3) |
C105—C106—H106 | 119.6 | C201—N3—C212 | 118.2 (4) |
C107—C106—H106 | 119.6 | C201—N3—Ni | 128.6 (3) |
C108—C107—C111 | 117.3 (5) | C212—N3—Ni | 113.2 (3) |
C108—C107—C106 | 124.5 (6) | C210—N4—C211 | 116.8 (4) |
C111—C107—C106 | 118.2 (6) | C210—N4—Ni | 130.6 (3) |
C109—C108—C107 | 120.2 (5) | C211—N4—Ni | 112.6 (3) |
C109—C108—H108 | 119.9 | C1—O1—Ni | 127.1 (3) |
C107—C108—H108 | 119.9 | Ni—OW1—H11 | 112 (3) |
C108—C109—C110 | 119.8 (6) | Ni—OW1—H12 | 94 (3) |
C108—C109—H109 | 120.1 | H11—OW1—H12 | 124 (5) |
C110—C109—H109 | 120.1 | H21—OW2—H22 | 110 (5) |
N2—C110—C109 | 122.1 (5) | H31—OW3—H32 | 101 (5) |
N2—C110—H110 | 118.9 | H41—OW4—H42 | 89 (5) |
C109—C110—H110 | 118.9 | H51—OW5—H52 | 107 (3) |
N2—C111—C107 | 121.7 (5) | H61—OW6—H62 | 95 (2) |
N2—C111—C112 | 117.5 (4) | H71—OW7—H72 | 93 (2) |
C107—C111—C112 | 120.8 (5) | H81—OW8—H82 | 120 (4) |
N1—C112—C104 | 122.7 (5) | H91—OW9—H92 | 99 (2) |
N1—C112—C111 | 117.7 (4) | O1—Ni—Ow1 | 90.76 (13) |
C104—C112—C111 | 119.6 (5) | O1—Ni—N1 | 91.27 (14) |
N3—C201—C202 | 122.8 (5) | O1—Ni—N2 | 170.68 (14) |
N3—C201—H201 | 118.6 | O1—Ni—N3 | 87.76 (13) |
C202—C201—H201 | 118.6 | O1—Ni—N4 | 94.03 (14) |
C203—C202—C201 | 119.1 (5) | OW1—Ni—N1 | 90.74 (14) |
C203—C202—H202 | 120.4 | OW1—Ni—N2 | 90.70 (14) |
C201—C202—H202 | 120.4 | OW1—Ni—N3 | 172.94 (14) |
C202—C203—C204 | 120.3 (5) | OW1—Ni—N4 | 93.49 (14) |
C202—C203—H203 | 119.9 | N1—Ni—N2 | 79.51 (15) |
C204—C203—H203 | 119.9 | N1—Ni—N3 | 96.19 (15) |
C212—C204—C205 | 119.8 (5) | N1—Ni—N4 | 173.17 (15) |
C212—C204—C203 | 116.5 (5) | N2—Ni—N3 | 91.88 (15) |
C205—C204—C203 | 123.7 (5) | N2—Ni—N4 | 95.07 (15) |
C206—C205—C204 | 121.0 (6) | N3—Ni—N4 | 79.74 (15) |
C206—C205—H205 | 119.5 | | |
Symmetry codes: (i) −x, −y, −z; (ii) −x+2, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW1—H12···O2 | 0.79 (2) | 1.88 (2) | 2.648 (5) | 163 (5) |
OW1—H11···O3iii | 0.80 (2) | 1.94 (2) | 2.727 (5) | 170 (5) |
OW2—H22···OW3iv | 0.80 (2) | 2.00 (2) | 2.799 (6) | 170 (5) |
OW2—H21···OW3v | 0.80 (2) | 2.04 (3) | 2.789 (6) | 157 (5) |
OW3—H31···O4vi | 0.80 (2) | 1.94 (2) | 2.735 (6) | 178 (5) |
OW3—H32···OW7 | 0.82 (4) | 2.04 (2) | 2.808 (7) | 157 (4) |
OW4—H42···O3iii | 0.84 (2) | 2.00 (2) | 2.823 (6) | 168 (5) |
OW4—H41···OW2vii | 0.82 (2) | 2.06 (3) | 2.800 (6) | 150 (5) |
OW5—H52···O4 | 0.79 (2) | 2.18 (3) | 2.780 (7) | 133 (3) |
OW5—H51···OW6 | 0.81 (4) | 2.12 (2) | 2.871 (8) | 154 (4) |
OW6—H62···O2viii | 0.82 (2) | 2.17 (2) | 2.960 (7) | 159 (4) |
OW7—H71···OW4vi | 0.74 (2) | 2.30 (3) | 2.914 (7) | 141 (5) |
OW7—H72···OW6vi | 0.98 (2) | 2.00 (3) | 2.815 (8) | 139 (4) |
OW8—H82···O1vii | 0.77 (2) | 2.22 (2) | 2.978 (6) | 167 (4) |
OW8—H81···OW4 | 0.72 (2) | 2.09 (2) | 2.784 (6) | 163 (4) |
OW9—H92···OW5 | 0.80 (2) | 2.18 (2) | 2.755 (8) | 129 (2) |
OW9—H91···OW8viii | 0.77 (2) | 2.75 (4) | 2.941 (10) | 97 (3) |
Symmetry codes: (iii) x−1, y, z; (iv) −x+1, −y, −z+1; (v) x, y−1, z; (vi) −x+1, −y+1, −z+1; (vii) x, y+1, z; (viii) x+1, y, z. |
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