The title complex, [Ni(C7H3NO4)(C12H8N2)(H2O)]·H2O, has been prepared hydrothermally. The asymmetric unit contains three water molecules and three nearly identical molecules of the mononuclear nickel(II) complex. A mer-O3N3 donor set defines a distorted octahedron around the metal atom. The crystal structure contains two independent networks of hydrogen bonds.
Supporting information
CCDC reference: 226214
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean
(C-C) = 0.004 Å
- R factor = 0.034
- wR factor = 0.081
- Data-to-parameter ratio = 15.4
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.95
Alert level C
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.80
PLAT230_ALERT_2_C Hirshfeld Test Diff for O11 - C106 .. 5.28 su
PLAT230_ALERT_2_C Hirshfeld Test Diff for O21 - C206 .. 5.09 su
PLAT230_ALERT_2_C Hirshfeld Test Diff for C203 - C204 .. 5.07 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - O11 .. 5.36 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni2 - O21 .. 7.00 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni2 - N22 .. 5.82 su
PLAT245_ALERT_2_C U(iso) H2W Smaller than U(eq) O1W by ... 0.02 AngSq
PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C201 - C206 ... 1.53 Ang.
Alert level G
ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be
replaced by the scaled T values. Since the ratio of scaled T's
is identical to the ratio of reported T values, the scaling
does not imply a change to the absorption corrections used in
the study.
Ratio of Tmax expected/reported 0.801
Tmax scaled 0.799 Tmin scaled 0.796
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
9 ALERT level C = Check and explain
2 ALERT level G = General alerts; check
1 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
2 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: Please provide missing details; cell refinement: Please provide missing details; data reduction: Please provide missing details; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Aqua(pyridine-2,6-dicarboxylato-
κ3N,
O,
O')(1,10-phenanthroline-
κ2N,
N')nickel(II)] monohydrate
top
Crystal data top
[Ni(C7H3NO4)(C12H8N2)]·H2O | F(000) = 2712 |
Mr = 440.03 | Dx = 1.623 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 33411 reflections |
a = 10.686 (5) Å | θ = 1.3–28.3° |
b = 27.285 (13) Å | µ = 1.12 mm−1 |
c = 19.169 (9) Å | T = 293 K |
β = 104.777 (9)° | Prism, blue |
V = 5404 (4) Å3 | 0.2 × 0.2 × 0.2 mm |
Z = 12 | |
Data collection top
Siemens SMART CCD area-detector diffractometer | 9027 reflections with I > 2σ(I) |
CCD; rotation images; thin–slice scans | Rint = 0.033 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | θmax = 28.3°, θmin = 1.3° |
Tmin = 0.994, Tmax = 0.998 | h = −10→14 |
33411 measured reflections | k = −36→35 |
12839 independent reflections | l = −25→25 |
Refinement top
Refinement on F2 | H atoms treated by a mixture of independent and constrained refinement |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0417P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.034 | (Δ/σ)max = 0.001 |
wR(F2) = 0.081 | Δρmax = 0.41 e Å−3 |
S = 0.94 | Δρmin = −0.45 e Å−3 |
12839 reflections | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
833 parameters | Extinction coefficient: 0.00031 (5) |
0 restraints | |
Special details top
Experimental. Selected FT–IR data (KBr, ν, cm-1): 3401 (w), 1626 (s), 1583
(s), 1519 (w), 1426 (m), 1279 (m), 847 (m),
727 (m). |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ni1 | 1.03620 (3) | 0.167210 (9) | 0.649506 (13) | 0.03279 (7) | |
O11 | 1.23959 (14) | 0.16211 (5) | 0.68082 (7) | 0.0412 (4) | |
O12 | 1.40041 (16) | 0.10664 (7) | 0.70707 (10) | 0.0628 (5) | |
O13 | 0.84360 (14) | 0.13938 (5) | 0.61718 (7) | 0.0383 (3) | |
O14 | 0.73110 (16) | 0.07025 (6) | 0.61857 (10) | 0.0579 (5) | |
O15 | 1.0445 (2) | 0.17367 (6) | 0.54387 (9) | 0.0418 (4) | |
N11 | 1.06282 (17) | 0.09531 (6) | 0.66092 (8) | 0.0345 (4) | |
N12 | 1.00720 (17) | 0.24210 (6) | 0.65028 (9) | 0.0377 (4) | |
N13 | 1.02258 (17) | 0.17749 (6) | 0.75570 (9) | 0.0370 (4) | |
C101 | 1.1829 (2) | 0.07874 (8) | 0.68512 (11) | 0.0393 (5) | |
C102 | 1.2046 (3) | 0.02952 (9) | 0.70319 (13) | 0.0536 (6) | |
H102 | 1.2881 | 0.0177 | 0.7216 | 0.064* | |
C103 | 1.0994 (3) | −0.00112 (9) | 0.69317 (15) | 0.0626 (7) | |
H103 | 1.1122 | −0.0342 | 0.7045 | 0.075* | |
C104 | 0.9751 (3) | 0.01646 (8) | 0.66657 (13) | 0.0528 (6) | |
H104 | 0.904 | −0.0044 | 0.659 | 0.063* | |
C105 | 0.9597 (2) | 0.06598 (8) | 0.65155 (11) | 0.0377 (5) | |
C106 | 1.2847 (2) | 0.11849 (9) | 0.69175 (11) | 0.0427 (5) | |
C107 | 0.8332 (2) | 0.09338 (8) | 0.62692 (11) | 0.0386 (5) | |
C108 | 0.9938 (2) | 0.27362 (8) | 0.59608 (13) | 0.0503 (6) | |
H108 | 0.9923 | 0.2614 | 0.5506 | 0.06* | |
C109 | 0.9820 (3) | 0.32405 (9) | 0.60398 (17) | 0.0646 (8) | |
H109 | 0.9713 | 0.3447 | 0.5643 | 0.078* | |
C110 | 0.9861 (3) | 0.34263 (9) | 0.67018 (18) | 0.0664 (8) | |
H110 | 0.9802 | 0.3763 | 0.6765 | 0.08* | |
C111 | 0.9991 (2) | 0.31086 (9) | 0.72879 (15) | 0.0536 (6) | |
C112 | 1.0081 (2) | 0.26053 (8) | 0.71570 (12) | 0.0387 (5) | |
C113 | 1.0158 (2) | 0.22569 (9) | 0.77254 (11) | 0.0395 (5) | |
C114 | 1.0142 (2) | 0.24229 (11) | 0.84148 (12) | 0.0544 (7) | |
C115 | 1.0167 (3) | 0.20584 (13) | 0.89364 (13) | 0.0691 (9) | |
H115 | 1.0159 | 0.2149 | 0.9403 | 0.083* | |
C116 | 1.0203 (3) | 0.15796 (13) | 0.87697 (13) | 0.0650 (8) | |
H116 | 1.0203 | 0.1341 | 0.9116 | 0.078* | |
C117 | 1.0241 (2) | 0.14450 (10) | 0.80661 (12) | 0.0507 (6) | |
H117 | 1.0278 | 0.1114 | 0.7956 | 0.061* | |
C118 | 1.0035 (3) | 0.32628 (12) | 0.80080 (19) | 0.0768 (9) | |
H118 | 1.002 | 0.3596 | 0.8109 | 0.092* | |
C119 | 1.0100 (3) | 0.29353 (13) | 0.85428 (17) | 0.0774 (10) | |
H119 | 1.0117 | 0.3047 | 0.9004 | 0.093* | |
H15A | 0.983 (3) | 0.1641 (9) | 0.5168 (14) | 0.058 (9)* | |
H15B | 1.101 (3) | 0.1586 (10) | 0.5365 (15) | 0.070 (11)* | |
Ni2 | 0.65024 (3) | 0.160592 (9) | 0.409016 (13) | 0.03425 (8) | |
O21 | 0.44688 (16) | 0.15619 (6) | 0.38268 (8) | 0.0483 (4) | |
O22 | 0.2868 (2) | 0.10129 (9) | 0.36884 (13) | 0.0920 (7) | |
O23 | 0.84408 (14) | 0.13440 (5) | 0.44625 (7) | 0.0395 (3) | |
O24 | 0.95513 (19) | 0.06430 (6) | 0.47262 (11) | 0.0710 (6) | |
O25 | 0.6520 (2) | 0.18108 (7) | 0.51374 (9) | 0.0455 (4) | |
N21 | 0.62406 (19) | 0.08999 (6) | 0.42150 (9) | 0.0401 (4) | |
N22 | 0.67169 (18) | 0.23290 (6) | 0.38328 (10) | 0.0407 (4) | |
N23 | 0.65743 (17) | 0.15335 (6) | 0.30163 (9) | 0.0367 (4) | |
C201 | 0.5038 (2) | 0.07286 (9) | 0.40506 (13) | 0.0495 (6) | |
C202 | 0.4830 (3) | 0.02288 (11) | 0.40883 (16) | 0.0730 (9) | |
H202 | 0.3995 | 0.0102 | 0.3976 | 0.088* | |
C203 | 0.5899 (4) | −0.00781 (10) | 0.42974 (18) | 0.0821 (10) | |
H203 | 0.5777 | −0.0414 | 0.4324 | 0.098* | |
C204 | 0.7131 (3) | 0.01080 (9) | 0.44649 (15) | 0.0625 (7) | |
H204 | 0.7848 | −0.0096 | 0.4611 | 0.075* | |
C205 | 0.7273 (2) | 0.06075 (8) | 0.44100 (12) | 0.0428 (5) | |
C206 | 0.4019 (3) | 0.11309 (11) | 0.38373 (13) | 0.0556 (7) | |
C207 | 0.8542 (2) | 0.08770 (8) | 0.45470 (12) | 0.0438 (5) | |
C208 | 0.6796 (2) | 0.27244 (9) | 0.42464 (15) | 0.0549 (6) | |
H208 | 0.684 | 0.2684 | 0.4734 | 0.066* | |
C209 | 0.6815 (3) | 0.32025 (10) | 0.3973 (2) | 0.0736 (9) | |
H209 | 0.6867 | 0.3472 | 0.4276 | 0.088* | |
C210 | 0.6759 (3) | 0.32660 (10) | 0.3267 (2) | 0.0757 (9) | |
H210 | 0.6755 | 0.3581 | 0.308 | 0.091* | |
C211 | 0.6706 (2) | 0.28625 (9) | 0.28196 (16) | 0.0573 (7) | |
C212 | 0.6681 (2) | 0.23965 (8) | 0.31266 (12) | 0.0414 (5) | |
C213 | 0.6625 (2) | 0.19706 (8) | 0.26944 (11) | 0.0383 (5) | |
C214 | 0.6626 (2) | 0.20107 (11) | 0.19587 (13) | 0.0536 (7) | |
C215 | 0.6606 (2) | 0.15789 (12) | 0.15739 (13) | 0.0642 (8) | |
H215 | 0.6603 | 0.159 | 0.1089 | 0.077* | |
C216 | 0.6592 (3) | 0.11394 (12) | 0.19052 (13) | 0.0634 (8) | |
H216 | 0.6604 | 0.0849 | 0.1654 | 0.076* | |
C217 | 0.6558 (2) | 0.11302 (9) | 0.26251 (12) | 0.0492 (6) | |
H217 | 0.6522 | 0.0828 | 0.2843 | 0.059* | |
C218 | 0.6691 (3) | 0.28916 (12) | 0.20692 (18) | 0.0762 (10) | |
H218 | 0.6705 | 0.3198 | 0.1858 | 0.091* | |
C219 | 0.6658 (3) | 0.24927 (13) | 0.16701 (16) | 0.0757 (9) | |
H219 | 0.6655 | 0.2527 | 0.1187 | 0.091* | |
H25A | 0.594 (3) | 0.1694 (9) | 0.5269 (14) | 0.053 (9)* | |
H25B | 0.711 (3) | 0.1706 (9) | 0.5421 (14) | 0.052 (9)* | |
Ni3 | 0.28367 (2) | 0.075170 (9) | 0.020223 (13) | 0.02929 (7) | |
O31 | 0.47127 (13) | 0.04514 (5) | 0.05463 (7) | 0.0358 (3) | |
O32 | 0.58666 (14) | −0.00801 (6) | 0.13465 (8) | 0.0448 (4) | |
O33 | 0.07790 (13) | 0.08008 (5) | 0.01419 (7) | 0.0355 (3) | |
O34 | −0.07418 (14) | 0.04604 (5) | 0.06005 (9) | 0.0486 (4) | |
O35 | 0.22798 (17) | 0.03268 (6) | −0.07157 (8) | 0.0383 (4) | |
N31 | 0.25857 (16) | 0.02392 (5) | 0.08882 (8) | 0.0299 (4) | |
N32 | 0.32508 (16) | 0.13301 (6) | −0.03966 (8) | 0.0306 (4) | |
N33 | 0.31338 (16) | 0.13164 (6) | 0.09764 (8) | 0.0316 (4) | |
C301 | 0.3632 (2) | −0.00004 (7) | 0.12640 (10) | 0.0325 (4) | |
C302 | 0.3556 (2) | −0.03099 (8) | 0.18209 (12) | 0.0447 (6) | |
H302 | 0.4283 | −0.0474 | 0.2089 | 0.054* | |
C303 | 0.2370 (3) | −0.03673 (9) | 0.19663 (14) | 0.0577 (7) | |
H303 | 0.2296 | −0.0571 | 0.2343 | 0.069* | |
C304 | 0.1284 (2) | −0.01275 (8) | 0.15617 (13) | 0.0509 (6) | |
H304 | 0.0478 | −0.0174 | 0.1653 | 0.061* | |
C305 | 0.1431 (2) | 0.01817 (7) | 0.10182 (11) | 0.0333 (5) | |
C306 | 0.4849 (2) | 0.01273 (7) | 0.10356 (11) | 0.0342 (5) | |
C307 | 0.0392 (2) | 0.05050 (7) | 0.05436 (11) | 0.0337 (5) | |
C308 | 0.3389 (2) | 0.13297 (8) | −0.10641 (11) | 0.0390 (5) | |
H308 | 0.3381 | 0.1031 | −0.1299 | 0.047* | |
C309 | 0.3545 (2) | 0.17579 (8) | −0.14306 (11) | 0.0437 (5) | |
H309 | 0.365 | 0.1741 | −0.1897 | 0.052* | |
C310 | 0.3544 (2) | 0.22007 (8) | −0.11018 (11) | 0.0415 (5) | |
H310 | 0.3613 | 0.2489 | −0.1349 | 0.05* | |
C311 | 0.3440 (2) | 0.22194 (7) | −0.03890 (11) | 0.0351 (5) | |
C312 | 0.33036 (18) | 0.17711 (7) | −0.00555 (10) | 0.0295 (4) | |
C313 | 0.32348 (18) | 0.17649 (7) | 0.06761 (10) | 0.0296 (4) | |
C314 | 0.3287 (2) | 0.22053 (7) | 0.10574 (11) | 0.0359 (5) | |
C315 | 0.3258 (2) | 0.21756 (8) | 0.17860 (12) | 0.0444 (6) | |
H315 | 0.3289 | 0.2459 | 0.2058 | 0.053* | |
C316 | 0.3185 (2) | 0.17295 (9) | 0.20898 (11) | 0.0450 (6) | |
H316 | 0.3179 | 0.1705 | 0.2573 | 0.054* | |
C317 | 0.3118 (2) | 0.13080 (8) | 0.16651 (11) | 0.0398 (5) | |
H317 | 0.3059 | 0.1006 | 0.1878 | 0.048* | |
C318 | 0.3449 (2) | 0.26614 (8) | 0.00045 (12) | 0.0445 (6) | |
H318 | 0.3505 | 0.296 | −0.022 | 0.053* | |
C319 | 0.3378 (2) | 0.26572 (8) | 0.06927 (13) | 0.0453 (6) | |
H319 | 0.3388 | 0.2952 | 0.0937 | 0.054* | |
H35A | 0.180 (3) | 0.0120 (9) | −0.0688 (14) | 0.061 (9)* | |
H35B | 0.291 (3) | 0.0210 (9) | −0.0909 (14) | 0.067 (9)* | |
O1W | 0.1956 (3) | 0.10761 (11) | 0.49860 (19) | 0.0912 (8) | |
H1W | 0.211 (4) | 0.1074 (15) | 0.459 (2) | 0.120 (18)* | |
H2W | 0.139 (3) | 0.0894 (11) | 0.4873 (17) | 0.070 (12)* | |
O2W | 0.5080 (3) | 0.12559 (8) | 0.58117 (17) | 0.0807 (7) | |
H3W | 0.427 (3) | 0.1234 (11) | 0.5561 (16) | 0.079 (11)* | |
H4W | 0.496 (5) | 0.1286 (19) | 0.631 (3) | 0.22 (3)* | |
O3W | 0.6773 (3) | 0.09247 (9) | 0.00863 (14) | 0.0763 (7) | |
H5W | 0.616 (4) | 0.0753 (14) | 0.015 (2) | 0.124 (16)* | |
H6W | 0.744 (3) | 0.0780 (13) | 0.0159 (19) | 0.105 (15)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.03610 (16) | 0.03462 (14) | 0.02687 (13) | −0.00081 (12) | 0.00662 (12) | 0.00304 (10) |
O11 | 0.0404 (9) | 0.0460 (9) | 0.0359 (8) | −0.0046 (7) | 0.0076 (7) | 0.0033 (7) |
O12 | 0.0333 (10) | 0.0792 (13) | 0.0733 (12) | 0.0061 (9) | 0.0088 (9) | 0.0021 (10) |
O13 | 0.0353 (9) | 0.0394 (8) | 0.0381 (8) | 0.0005 (6) | 0.0054 (7) | 0.0047 (6) |
O14 | 0.0405 (10) | 0.0544 (10) | 0.0774 (12) | −0.0088 (8) | 0.0124 (9) | 0.0112 (9) |
O15 | 0.0411 (11) | 0.0533 (10) | 0.0301 (8) | −0.0056 (9) | 0.0073 (8) | −0.0007 (7) |
N11 | 0.0340 (10) | 0.0378 (9) | 0.0315 (9) | 0.0008 (8) | 0.0081 (8) | 0.0037 (7) |
N12 | 0.0385 (11) | 0.0387 (10) | 0.0359 (9) | −0.0011 (8) | 0.0092 (8) | 0.0034 (8) |
N13 | 0.0331 (10) | 0.0481 (11) | 0.0293 (9) | 0.0014 (8) | 0.0070 (8) | 0.0051 (8) |
C101 | 0.0390 (13) | 0.0472 (13) | 0.0324 (10) | 0.0044 (10) | 0.0106 (10) | 0.0010 (9) |
C102 | 0.0492 (16) | 0.0474 (14) | 0.0631 (16) | 0.0163 (12) | 0.0125 (13) | 0.0102 (12) |
C103 | 0.0670 (19) | 0.0392 (14) | 0.0819 (19) | 0.0126 (13) | 0.0195 (16) | 0.0135 (13) |
C104 | 0.0563 (17) | 0.0402 (13) | 0.0612 (15) | −0.0026 (12) | 0.0140 (13) | 0.0054 (11) |
C105 | 0.0408 (13) | 0.0391 (12) | 0.0333 (11) | −0.0016 (10) | 0.0097 (10) | 0.0021 (9) |
C106 | 0.0369 (14) | 0.0591 (15) | 0.0310 (11) | 0.0000 (11) | 0.0069 (10) | −0.0012 (10) |
C107 | 0.0394 (13) | 0.0437 (12) | 0.0327 (11) | −0.0026 (10) | 0.0092 (10) | 0.0028 (9) |
C108 | 0.0559 (16) | 0.0444 (13) | 0.0501 (14) | 0.0000 (12) | 0.0123 (12) | 0.0121 (11) |
C109 | 0.0608 (18) | 0.0450 (15) | 0.089 (2) | 0.0025 (13) | 0.0206 (17) | 0.0231 (14) |
C110 | 0.0541 (18) | 0.0381 (14) | 0.110 (2) | 0.0018 (12) | 0.0265 (17) | −0.0018 (15) |
C111 | 0.0373 (14) | 0.0474 (14) | 0.0773 (18) | −0.0017 (11) | 0.0172 (13) | −0.0155 (13) |
C112 | 0.0280 (12) | 0.0442 (12) | 0.0440 (12) | −0.0004 (9) | 0.0092 (10) | −0.0062 (10) |
C113 | 0.0250 (11) | 0.0600 (14) | 0.0327 (11) | −0.0008 (10) | 0.0058 (9) | −0.0064 (10) |
C114 | 0.0345 (14) | 0.089 (2) | 0.0404 (13) | −0.0019 (13) | 0.0104 (11) | −0.0198 (13) |
C115 | 0.0472 (17) | 0.133 (3) | 0.0285 (12) | 0.0009 (17) | 0.0122 (12) | −0.0106 (16) |
C116 | 0.0449 (16) | 0.116 (3) | 0.0344 (13) | 0.0040 (16) | 0.0104 (12) | 0.0210 (15) |
C117 | 0.0439 (15) | 0.0704 (16) | 0.0373 (12) | 0.0020 (12) | 0.0095 (11) | 0.0161 (11) |
C118 | 0.064 (2) | 0.073 (2) | 0.095 (2) | −0.0008 (16) | 0.0235 (19) | −0.0433 (19) |
C119 | 0.064 (2) | 0.108 (3) | 0.0627 (18) | −0.0011 (18) | 0.0206 (17) | −0.0449 (19) |
Ni2 | 0.04047 (17) | 0.03110 (14) | 0.02927 (13) | 0.00154 (12) | 0.00535 (12) | −0.00032 (10) |
O21 | 0.0462 (10) | 0.0574 (10) | 0.0396 (8) | 0.0063 (8) | 0.0079 (8) | −0.0020 (7) |
O22 | 0.0439 (13) | 0.1166 (18) | 0.1158 (18) | −0.0122 (12) | 0.0210 (13) | 0.0039 (15) |
O23 | 0.0418 (9) | 0.0369 (8) | 0.0368 (8) | 0.0007 (7) | 0.0043 (7) | 0.0009 (6) |
O24 | 0.0559 (12) | 0.0530 (11) | 0.0987 (15) | 0.0170 (9) | 0.0098 (11) | 0.0025 (10) |
O25 | 0.0448 (11) | 0.0578 (11) | 0.0313 (8) | 0.0114 (9) | 0.0051 (9) | −0.0004 (8) |
N21 | 0.0470 (12) | 0.0381 (10) | 0.0376 (10) | −0.0040 (9) | 0.0149 (9) | 0.0018 (8) |
N22 | 0.0411 (11) | 0.0348 (10) | 0.0436 (10) | 0.0017 (8) | 0.0060 (9) | −0.0028 (8) |
N23 | 0.0340 (10) | 0.0414 (10) | 0.0330 (9) | −0.0021 (8) | 0.0052 (8) | −0.0016 (8) |
C201 | 0.0516 (16) | 0.0531 (14) | 0.0469 (13) | −0.0132 (12) | 0.0180 (12) | −0.0006 (11) |
C202 | 0.077 (2) | 0.0639 (19) | 0.084 (2) | −0.0338 (17) | 0.0317 (18) | −0.0078 (16) |
C203 | 0.112 (3) | 0.0374 (15) | 0.103 (2) | −0.0172 (18) | 0.038 (2) | −0.0010 (15) |
C204 | 0.082 (2) | 0.0376 (13) | 0.0720 (18) | −0.0003 (14) | 0.0279 (16) | 0.0042 (12) |
C205 | 0.0560 (16) | 0.0347 (11) | 0.0396 (12) | 0.0026 (11) | 0.0157 (11) | 0.0019 (9) |
C206 | 0.0436 (16) | 0.0781 (19) | 0.0466 (14) | −0.0039 (14) | 0.0143 (13) | −0.0036 (13) |
C207 | 0.0490 (15) | 0.0421 (13) | 0.0394 (12) | 0.0044 (11) | 0.0094 (11) | −0.0011 (10) |
C208 | 0.0488 (16) | 0.0446 (14) | 0.0693 (17) | −0.0009 (12) | 0.0112 (13) | −0.0140 (12) |
C209 | 0.0578 (19) | 0.0382 (15) | 0.125 (3) | −0.0037 (13) | 0.024 (2) | −0.0197 (16) |
C210 | 0.0573 (19) | 0.0404 (15) | 0.131 (3) | 0.0009 (13) | 0.027 (2) | 0.0203 (18) |
C211 | 0.0390 (15) | 0.0468 (15) | 0.0849 (19) | 0.0037 (11) | 0.0139 (14) | 0.0249 (14) |
C212 | 0.0275 (12) | 0.0410 (12) | 0.0529 (13) | 0.0011 (9) | 0.0049 (10) | 0.0131 (10) |
C213 | 0.0254 (11) | 0.0525 (13) | 0.0350 (11) | 0.0003 (10) | 0.0040 (9) | 0.0084 (10) |
C214 | 0.0311 (13) | 0.088 (2) | 0.0408 (13) | 0.0008 (12) | 0.0069 (11) | 0.0172 (13) |
C215 | 0.0435 (16) | 0.116 (3) | 0.0322 (12) | −0.0104 (16) | 0.0076 (12) | −0.0078 (15) |
C216 | 0.0521 (17) | 0.096 (2) | 0.0428 (14) | −0.0147 (15) | 0.0139 (13) | −0.0273 (15) |
C217 | 0.0490 (15) | 0.0558 (15) | 0.0424 (13) | −0.0088 (12) | 0.0107 (12) | −0.0117 (11) |
C218 | 0.0572 (19) | 0.082 (2) | 0.090 (2) | 0.0027 (16) | 0.0185 (18) | 0.0533 (19) |
C219 | 0.0572 (19) | 0.110 (3) | 0.0609 (18) | 0.0023 (18) | 0.0174 (16) | 0.0450 (19) |
Ni3 | 0.02861 (14) | 0.02904 (13) | 0.03127 (13) | −0.00043 (11) | 0.00957 (11) | 0.00346 (10) |
O31 | 0.0302 (8) | 0.0394 (8) | 0.0394 (8) | 0.0007 (6) | 0.0121 (7) | 0.0074 (6) |
O32 | 0.0312 (9) | 0.0591 (10) | 0.0449 (8) | 0.0114 (7) | 0.0111 (7) | 0.0095 (7) |
O33 | 0.0294 (8) | 0.0358 (8) | 0.0415 (8) | 0.0021 (6) | 0.0091 (7) | 0.0073 (6) |
O34 | 0.0285 (9) | 0.0451 (9) | 0.0745 (11) | 0.0000 (7) | 0.0174 (8) | 0.0081 (8) |
O35 | 0.0357 (9) | 0.0371 (8) | 0.0456 (9) | −0.0074 (7) | 0.0169 (8) | −0.0069 (7) |
N31 | 0.0284 (9) | 0.0284 (8) | 0.0343 (8) | −0.0003 (7) | 0.0107 (8) | 0.0016 (7) |
N32 | 0.0291 (9) | 0.0324 (9) | 0.0300 (8) | −0.0028 (7) | 0.0067 (7) | 0.0006 (7) |
N33 | 0.0287 (9) | 0.0353 (9) | 0.0301 (8) | 0.0007 (7) | 0.0063 (7) | 0.0023 (7) |
C301 | 0.0318 (11) | 0.0307 (10) | 0.0355 (10) | 0.0033 (9) | 0.0097 (9) | 0.0014 (8) |
C302 | 0.0400 (14) | 0.0486 (13) | 0.0468 (13) | 0.0102 (11) | 0.0131 (11) | 0.0184 (10) |
C303 | 0.0572 (17) | 0.0613 (16) | 0.0620 (16) | 0.0087 (13) | 0.0286 (14) | 0.0336 (13) |
C304 | 0.0428 (14) | 0.0528 (14) | 0.0654 (15) | 0.0020 (11) | 0.0289 (13) | 0.0208 (12) |
C305 | 0.0305 (12) | 0.0310 (10) | 0.0411 (11) | −0.0009 (9) | 0.0142 (10) | 0.0020 (9) |
C306 | 0.0333 (12) | 0.0353 (11) | 0.0350 (11) | 0.0018 (9) | 0.0104 (10) | −0.0018 (9) |
C307 | 0.0299 (12) | 0.0308 (11) | 0.0413 (11) | −0.0002 (9) | 0.0104 (10) | −0.0036 (9) |
C308 | 0.0413 (13) | 0.0442 (12) | 0.0315 (11) | −0.0069 (10) | 0.0092 (10) | −0.0035 (9) |
C309 | 0.0477 (15) | 0.0521 (14) | 0.0318 (11) | −0.0116 (11) | 0.0111 (10) | 0.0045 (10) |
C310 | 0.0419 (14) | 0.0421 (12) | 0.0387 (12) | −0.0083 (10) | 0.0069 (10) | 0.0108 (10) |
C311 | 0.0296 (12) | 0.0344 (11) | 0.0394 (11) | −0.0022 (9) | 0.0051 (10) | 0.0051 (9) |
C312 | 0.0246 (11) | 0.0319 (10) | 0.0306 (10) | −0.0014 (8) | 0.0040 (9) | 0.0020 (8) |
C313 | 0.0227 (10) | 0.0332 (10) | 0.0307 (10) | 0.0005 (8) | 0.0031 (8) | 0.0019 (8) |
C314 | 0.0281 (11) | 0.0396 (11) | 0.0379 (11) | −0.0006 (9) | 0.0048 (9) | −0.0032 (9) |
C315 | 0.0424 (14) | 0.0497 (14) | 0.0399 (12) | 0.0007 (11) | 0.0084 (11) | −0.0126 (10) |
C316 | 0.0438 (14) | 0.0595 (15) | 0.0304 (11) | 0.0029 (11) | 0.0072 (10) | −0.0025 (10) |
C317 | 0.0405 (13) | 0.0458 (13) | 0.0333 (11) | 0.0012 (10) | 0.0099 (10) | 0.0057 (9) |
C318 | 0.0474 (15) | 0.0317 (11) | 0.0532 (14) | −0.0034 (10) | 0.0105 (12) | 0.0025 (10) |
C319 | 0.0462 (15) | 0.0319 (11) | 0.0572 (14) | −0.0029 (10) | 0.0119 (12) | −0.0062 (10) |
O1W | 0.0681 (18) | 0.0896 (19) | 0.123 (3) | 0.0040 (14) | 0.0372 (17) | −0.0155 (17) |
O2W | 0.0712 (17) | 0.0644 (13) | 0.114 (2) | −0.0071 (12) | 0.0378 (16) | 0.0012 (13) |
O3W | 0.0565 (15) | 0.0754 (15) | 0.1043 (17) | 0.0118 (13) | 0.0339 (14) | 0.0377 (13) |
Geometric parameters (Å, º) top
Ni1—N11 | 1.9863 (19) | C208—C209 | 1.408 (4) |
Ni1—O15 | 2.0568 (19) | C208—H208 | 0.93 |
Ni1—N12 | 2.067 (2) | C209—C210 | 1.350 (4) |
Ni1—N13 | 2.0964 (19) | C209—H209 | 0.93 |
Ni1—O11 | 2.1066 (18) | C210—C211 | 1.388 (4) |
Ni1—O13 | 2.1321 (17) | C210—H210 | 0.93 |
O11—C106 | 1.281 (3) | C211—C212 | 1.404 (3) |
O12—C106 | 1.239 (3) | C211—C218 | 1.437 (4) |
O13—C107 | 1.278 (2) | C212—C213 | 1.420 (3) |
O14—C107 | 1.235 (3) | C213—C214 | 1.415 (3) |
O15—H15A | 0.77 (3) | C214—C215 | 1.387 (4) |
O15—H15B | 0.77 (3) | C214—C219 | 1.431 (4) |
N11—C101 | 1.328 (3) | C215—C216 | 1.359 (4) |
N11—C105 | 1.337 (3) | C215—H215 | 0.93 |
N12—C108 | 1.328 (3) | C216—C217 | 1.390 (3) |
N12—C112 | 1.349 (3) | C216—H216 | 0.93 |
N13—C117 | 1.325 (3) | C217—H217 | 0.93 |
N13—C113 | 1.361 (3) | C218—C219 | 1.326 (4) |
C101—C102 | 1.391 (3) | C218—H218 | 0.93 |
C101—C106 | 1.518 (3) | C219—H219 | 0.93 |
C102—C103 | 1.374 (4) | Ni3—N31 | 1.9840 (17) |
C102—H102 | 0.93 | Ni3—O35 | 2.0640 (17) |
C103—C104 | 1.382 (3) | Ni3—N32 | 2.0647 (17) |
C103—H103 | 0.93 | Ni3—N33 | 2.1065 (17) |
C104—C105 | 1.383 (3) | Ni3—O31 | 2.1097 (16) |
C104—H104 | 0.93 | Ni3—O33 | 2.1763 (17) |
C105—C107 | 1.511 (3) | O31—C306 | 1.270 (2) |
C108—C109 | 1.393 (3) | O32—C306 | 1.236 (2) |
C108—H108 | 0.93 | O33—C307 | 1.256 (2) |
C109—C110 | 1.357 (4) | O34—C307 | 1.249 (2) |
C109—H109 | 0.93 | O35—H35A | 0.77 (3) |
C110—C111 | 1.398 (4) | O35—H35B | 0.91 (3) |
C110—H110 | 0.93 | N31—C305 | 1.329 (3) |
C111—C112 | 1.404 (3) | N31—C301 | 1.336 (2) |
C111—C118 | 1.432 (4) | N32—C308 | 1.325 (3) |
C112—C113 | 1.432 (3) | N32—C312 | 1.364 (2) |
C113—C114 | 1.401 (3) | N33—C317 | 1.325 (3) |
C114—C115 | 1.406 (4) | N33—C313 | 1.368 (2) |
C114—C119 | 1.422 (4) | C301—C302 | 1.380 (3) |
C115—C116 | 1.348 (4) | C301—C306 | 1.515 (3) |
C115—H115 | 0.93 | C302—C303 | 1.374 (3) |
C116—C117 | 1.408 (3) | C302—H302 | 0.93 |
C116—H116 | 0.93 | C303—C304 | 1.385 (3) |
C117—H117 | 0.93 | C303—H303 | 0.93 |
C118—C119 | 1.348 (4) | C304—C305 | 1.381 (3) |
C118—H118 | 0.93 | C304—H304 | 0.93 |
C119—H119 | 0.93 | C305—C307 | 1.525 (3) |
Ni2—N21 | 1.9699 (19) | C308—C309 | 1.395 (3) |
Ni2—N22 | 2.0605 (19) | C308—H308 | 0.93 |
Ni2—O25 | 2.0794 (19) | C309—C310 | 1.363 (3) |
Ni2—N23 | 2.0889 (19) | C309—H309 | 0.93 |
Ni2—O21 | 2.1052 (19) | C310—C311 | 1.400 (3) |
Ni2—O23 | 2.1347 (17) | C310—H310 | 0.93 |
O21—C206 | 1.273 (3) | C311—C312 | 1.405 (3) |
O22—C206 | 1.232 (3) | C311—C318 | 1.421 (3) |
O23—C207 | 1.285 (3) | C312—C313 | 1.423 (3) |
O24—C207 | 1.225 (3) | C313—C314 | 1.400 (3) |
O25—H25A | 0.80 (3) | C314—C315 | 1.407 (3) |
O25—H25B | 0.77 (3) | C314—C319 | 1.433 (3) |
N21—C201 | 1.328 (3) | C315—C316 | 1.360 (3) |
N21—C205 | 1.335 (3) | C315—H315 | 0.93 |
N22—C208 | 1.329 (3) | C316—C317 | 1.400 (3) |
N22—C212 | 1.357 (3) | C316—H316 | 0.93 |
N23—C217 | 1.329 (3) | C317—H317 | 0.93 |
N23—C213 | 1.350 (3) | C318—C319 | 1.340 (3) |
C201—C202 | 1.386 (4) | C318—H318 | 0.93 |
C201—C206 | 1.526 (4) | C319—H319 | 0.93 |
C202—C203 | 1.390 (4) | O1W—H1W | 0.82 (4) |
C202—H202 | 0.93 | O1W—H2W | 0.77 (3) |
C203—C204 | 1.370 (4) | O2W—H3W | 0.88 (3) |
C203—H203 | 0.93 | O2W—H4W | 1.00 (5) |
C204—C205 | 1.378 (3) | O3W—H5W | 0.84 (4) |
C204—H204 | 0.93 | O3W—H6W | 0.80 (3) |
C205—C207 | 1.506 (3) | | |
| | | |
N11—Ni1—O15 | 98.75 (7) | O22—C206—C201 | 118.4 (3) |
N11—Ni1—N12 | 173.17 (7) | O21—C206—C201 | 115.0 (2) |
O15—Ni1—N12 | 88.08 (7) | O24—C207—O23 | 126.3 (2) |
N11—Ni1—N13 | 93.94 (7) | O24—C207—C205 | 118.9 (2) |
O15—Ni1—N13 | 167.31 (7) | O23—C207—C205 | 114.8 (2) |
N12—Ni1—N13 | 79.23 (7) | N22—C208—C209 | 122.3 (3) |
N11—Ni1—O11 | 78.17 (6) | N22—C208—H208 | 118.8 |
O15—Ni1—O11 | 89.19 (7) | C209—C208—H208 | 118.8 |
N12—Ni1—O11 | 102.06 (6) | C210—C209—C208 | 119.4 (3) |
N13—Ni1—O11 | 93.11 (6) | C210—C209—H209 | 120.3 |
N11—Ni1—O13 | 77.34 (7) | C208—C209—H209 | 120.3 |
O15—Ni1—O13 | 91.44 (7) | C209—C210—C211 | 120.1 (3) |
N12—Ni1—O13 | 102.63 (7) | C209—C210—H210 | 119.9 |
N13—Ni1—O13 | 91.66 (6) | C211—C210—H210 | 119.9 |
O11—Ni1—O13 | 155.31 (6) | C210—C211—C212 | 117.5 (3) |
C106—O11—Ni1 | 115.21 (14) | C210—C211—C218 | 124.3 (3) |
C107—O13—Ni1 | 114.89 (13) | C212—C211—C218 | 118.3 (3) |
Ni1—O15—H15A | 113 (2) | N22—C212—C211 | 122.9 (2) |
Ni1—O15—H15B | 111 (2) | N22—C212—C213 | 117.21 (18) |
H15A—O15—H15B | 105 (3) | C211—C212—C213 | 119.9 (2) |
C101—N11—C105 | 122.25 (19) | N23—C213—C214 | 122.3 (2) |
C101—N11—Ni1 | 118.24 (14) | N23—C213—C212 | 117.19 (19) |
C105—N11—Ni1 | 119.11 (15) | C214—C213—C212 | 120.5 (2) |
C108—N12—C112 | 117.4 (2) | C215—C214—C213 | 117.4 (2) |
C108—N12—Ni1 | 128.38 (16) | C215—C214—C219 | 125.0 (3) |
C112—N12—Ni1 | 114.18 (14) | C213—C214—C219 | 117.6 (3) |
C117—N13—C113 | 118.26 (19) | C216—C215—C214 | 120.1 (2) |
C117—N13—Ni1 | 129.32 (17) | C216—C215—H215 | 120 |
C113—N13—Ni1 | 112.38 (13) | C214—C215—H215 | 120 |
N11—C101—C102 | 120.0 (2) | C215—C216—C217 | 119.1 (3) |
N11—C101—C106 | 113.20 (19) | C215—C216—H216 | 120.5 |
C102—C101—C106 | 126.8 (2) | C217—C216—H216 | 120.5 |
C103—C102—C101 | 118.3 (2) | N23—C217—C216 | 123.0 (2) |
C103—C102—H102 | 120.8 | N23—C217—H217 | 118.5 |
C101—C102—H102 | 120.8 | C216—C217—H217 | 118.5 |
C102—C103—C104 | 121.0 (2) | C219—C218—C211 | 121.6 (3) |
C102—C103—H103 | 119.5 | C219—C218—H218 | 119.2 |
C104—C103—H103 | 119.5 | C211—C218—H218 | 119.2 |
C103—C104—C105 | 117.9 (2) | C218—C219—C214 | 122.1 (3) |
C103—C104—H104 | 121 | C218—C219—H219 | 118.9 |
C105—C104—H104 | 121 | C214—C219—H219 | 118.9 |
N11—C105—C104 | 120.4 (2) | N31—Ni3—O35 | 96.36 (7) |
N11—C105—C107 | 112.77 (18) | N31—Ni3—N32 | 172.55 (6) |
C104—C105—C107 | 126.7 (2) | O35—Ni3—N32 | 90.65 (7) |
O12—C106—O11 | 126.3 (2) | N31—Ni3—N33 | 94.03 (7) |
O12—C106—C101 | 118.9 (2) | O35—Ni3—N33 | 166.02 (6) |
O11—C106—C101 | 114.7 (2) | N32—Ni3—N33 | 79.48 (7) |
O14—C107—O13 | 126.2 (2) | N31—Ni3—O31 | 78.31 (6) |
O14—C107—C105 | 118.5 (2) | O35—Ni3—O31 | 95.32 (6) |
O13—C107—C105 | 115.30 (19) | N32—Ni3—O31 | 98.59 (6) |
N12—C108—C109 | 123.3 (2) | N33—Ni3—O31 | 95.93 (6) |
N12—C108—H108 | 118.4 | N31—Ni3—O33 | 76.88 (6) |
C109—C108—H108 | 118.4 | O35—Ni3—O33 | 85.50 (6) |
C110—C109—C108 | 119.2 (3) | N32—Ni3—O33 | 106.28 (6) |
C110—C109—H109 | 120.4 | N33—Ni3—O33 | 87.77 (6) |
C108—C109—H109 | 120.4 | O31—Ni3—O33 | 155.11 (5) |
C109—C110—C111 | 119.5 (2) | C306—O31—Ni3 | 114.96 (13) |
C109—C110—H110 | 120.2 | C307—O33—Ni3 | 114.48 (12) |
C111—C110—H110 | 120.2 | Ni3—O35—H35A | 114 (2) |
C110—C111—C112 | 117.4 (2) | Ni3—O35—H35B | 117.6 (16) |
C110—C111—C118 | 124.4 (3) | H35A—O35—H35B | 110 (2) |
C112—C111—C118 | 118.2 (3) | C305—N31—C301 | 122.03 (17) |
N12—C112—C111 | 123.1 (2) | C305—N31—Ni3 | 119.77 (13) |
N12—C112—C113 | 116.44 (19) | C301—N31—Ni3 | 117.78 (13) |
C111—C112—C113 | 120.4 (2) | C308—N32—C312 | 117.56 (17) |
N13—C113—C114 | 123.4 (2) | C308—N32—Ni3 | 128.96 (14) |
N13—C113—C112 | 117.21 (18) | C312—N32—Ni3 | 113.34 (13) |
C114—C113—C112 | 119.4 (2) | C317—N33—C313 | 117.22 (17) |
C113—C114—C115 | 116.1 (2) | C317—N33—Ni3 | 130.65 (14) |
C113—C114—C119 | 119.3 (3) | C313—N33—Ni3 | 111.81 (13) |
C115—C114—C119 | 124.7 (3) | N31—C301—C302 | 120.68 (19) |
C116—C115—C114 | 120.9 (2) | N31—C301—C306 | 113.18 (17) |
C116—C115—H115 | 119.5 | C302—C301—C306 | 126.07 (19) |
C114—C115—H115 | 119.5 | C303—C302—C301 | 117.8 (2) |
C115—C116—C117 | 119.3 (2) | C303—C302—H302 | 121.1 |
C115—C116—H116 | 120.3 | C301—C302—H302 | 121.1 |
C117—C116—H116 | 120.3 | C302—C303—C304 | 121.2 (2) |
N13—C117—C116 | 122.0 (3) | C302—C303—H303 | 119.4 |
N13—C117—H117 | 119 | C304—C303—H303 | 119.4 |
C116—C117—H117 | 119 | C305—C304—C303 | 118.0 (2) |
C119—C118—C111 | 121.4 (3) | C305—C304—H304 | 121 |
C119—C118—H118 | 119.3 | C303—C304—H304 | 121 |
C111—C118—H118 | 119.3 | N31—C305—C304 | 120.27 (19) |
C118—C119—C114 | 121.2 (3) | N31—C305—C307 | 112.95 (17) |
C118—C119—H119 | 119.4 | C304—C305—C307 | 126.70 (19) |
C114—C119—H119 | 119.4 | O32—C306—O31 | 126.6 (2) |
N21—Ni2—N22 | 173.36 (7) | O32—C306—C301 | 118.03 (18) |
N21—Ni2—O25 | 96.44 (7) | O31—C306—C301 | 115.38 (18) |
N22—Ni2—O25 | 89.98 (8) | O34—C307—O33 | 126.47 (19) |
N21—Ni2—N23 | 93.97 (7) | O34—C307—C305 | 117.82 (18) |
N22—Ni2—N23 | 79.65 (7) | O33—C307—C305 | 115.68 (18) |
O25—Ni2—N23 | 169.53 (7) | N32—C308—C309 | 122.9 (2) |
N21—Ni2—O21 | 78.66 (7) | N32—C308—H308 | 118.6 |
N22—Ni2—O21 | 99.69 (7) | C309—C308—H308 | 118.6 |
O25—Ni2—O21 | 90.08 (8) | C310—C309—C308 | 119.7 (2) |
N23—Ni2—O21 | 93.06 (6) | C310—C309—H309 | 120.2 |
N21—Ni2—O23 | 77.75 (7) | C308—C309—H309 | 120.2 |
N22—Ni2—O23 | 104.06 (7) | C309—C310—C311 | 119.55 (19) |
O25—Ni2—O23 | 89.90 (7) | C309—C310—H310 | 120.2 |
N23—Ni2—O23 | 91.22 (6) | C311—C310—H310 | 120.2 |
O21—Ni2—O23 | 156.26 (6) | C310—C311—C312 | 117.12 (18) |
C206—O21—Ni2 | 114.81 (16) | C310—C311—C318 | 123.88 (19) |
C207—O23—Ni2 | 114.67 (14) | C312—C311—C318 | 118.99 (19) |
Ni2—O25—H25A | 112.6 (19) | N32—C312—C311 | 123.12 (18) |
Ni2—O25—H25B | 112.7 (19) | N32—C312—C313 | 117.12 (16) |
H25A—O25—H25B | 101 (3) | C311—C312—C313 | 119.76 (18) |
C201—N21—C205 | 122.5 (2) | N33—C313—C314 | 123.01 (18) |
C201—N21—Ni2 | 118.31 (16) | N33—C313—C312 | 117.06 (17) |
C205—N21—Ni2 | 119.05 (16) | C314—C313—C312 | 119.93 (17) |
C208—N22—C212 | 117.8 (2) | C313—C314—C315 | 117.42 (19) |
C208—N22—Ni2 | 128.96 (17) | C313—C314—C319 | 118.85 (19) |
C212—N22—Ni2 | 113.10 (14) | C315—C314—C319 | 123.7 (2) |
C217—N23—C213 | 118.02 (19) | C316—C315—C314 | 119.7 (2) |
C217—N23—Ni2 | 129.48 (15) | C316—C315—H315 | 120.2 |
C213—N23—Ni2 | 112.49 (14) | C314—C315—H315 | 120.2 |
N21—C201—C202 | 119.4 (3) | C315—C316—C317 | 119.1 (2) |
N21—C201—C206 | 113.0 (2) | C315—C316—H316 | 120.5 |
C202—C201—C206 | 127.5 (3) | C317—C316—H316 | 120.5 |
C201—C202—C203 | 118.5 (3) | N33—C317—C316 | 123.6 (2) |
C201—C202—H202 | 120.8 | N33—C317—H317 | 118.2 |
C203—C202—H202 | 120.8 | C316—C317—H317 | 118.2 |
C204—C203—C202 | 120.9 (3) | C319—C318—C311 | 121.4 (2) |
C204—C203—H203 | 119.5 | C319—C318—H318 | 119.3 |
C202—C203—H203 | 119.5 | C311—C318—H318 | 119.3 |
C203—C204—C205 | 117.8 (3) | C318—C319—C314 | 121.0 (2) |
C203—C204—H204 | 121.1 | C318—C319—H319 | 119.5 |
C205—C204—H204 | 121.1 | C314—C319—H319 | 119.5 |
N21—C205—C204 | 120.9 (2) | H1W—O1W—H2W | 94 (4) |
N21—C205—C207 | 113.59 (19) | H3W—O2W—H4W | 100 (3) |
C204—C205—C207 | 125.5 (2) | H5W—O3W—H6W | 113 (3) |
O22—C206—O21 | 126.6 (3) | | |
| | | |
N11—Ni1—O11—C106 | 0.36 (14) | Ni2—O21—C206—C201 | 1.0 (3) |
O15—Ni1—O11—C106 | −98.75 (15) | N21—C201—C206—O22 | −178.5 (2) |
N12—Ni1—O11—C106 | 173.38 (14) | C202—C201—C206—O22 | 1.2 (4) |
N13—Ni1—O11—C106 | 93.74 (15) | N21—C201—C206—O21 | 2.1 (3) |
O13—Ni1—O11—C106 | −7.1 (2) | C202—C201—C206—O21 | −178.1 (2) |
N11—Ni1—O13—C107 | 7.00 (14) | Ni2—O23—C207—O24 | 176.8 (2) |
O15—Ni1—O13—C107 | 105.65 (15) | Ni2—O23—C207—C205 | −3.5 (2) |
N12—Ni1—O13—C107 | −165.99 (14) | N21—C205—C207—O24 | −179.7 (2) |
N13—Ni1—O13—C107 | −86.66 (14) | C204—C205—C207—O24 | −0.3 (4) |
O11—Ni1—O13—C107 | 14.5 (2) | N21—C205—C207—O23 | 0.6 (3) |
O15—Ni1—N11—C101 | 91.36 (16) | C204—C205—C207—O23 | 179.9 (2) |
N13—Ni1—N11—C101 | −88.31 (15) | C212—N22—C208—C209 | 1.3 (4) |
O11—Ni1—N11—C101 | 4.04 (14) | Ni2—N22—C208—C209 | −173.63 (19) |
O13—Ni1—N11—C101 | −179.13 (16) | N22—C208—C209—C210 | −0.3 (4) |
O15—Ni1—N11—C105 | −95.72 (16) | C208—C209—C210—C211 | −1.2 (5) |
N13—Ni1—N11—C105 | 84.60 (15) | C209—C210—C211—C212 | 1.6 (4) |
O11—Ni1—N11—C105 | 176.96 (16) | C209—C210—C211—C218 | −177.7 (3) |
O13—Ni1—N11—C105 | −6.21 (14) | C208—N22—C212—C211 | −0.8 (3) |
O15—Ni1—N12—C108 | 3.7 (2) | Ni2—N22—C212—C211 | 174.92 (18) |
N13—Ni1—N12—C108 | −176.6 (2) | C208—N22—C212—C213 | 178.6 (2) |
O11—Ni1—N12—C108 | 92.5 (2) | Ni2—N22—C212—C213 | −5.6 (2) |
O13—Ni1—N12—C108 | −87.3 (2) | C210—C211—C212—N22 | −0.6 (4) |
O15—Ni1—N12—C112 | −173.10 (16) | C218—C211—C212—N22 | 178.7 (2) |
N13—Ni1—N12—C112 | 6.57 (15) | C210—C211—C212—C213 | 179.9 (2) |
O11—Ni1—N12—C112 | −84.34 (15) | C218—C211—C212—C213 | −0.8 (3) |
O13—Ni1—N12—C112 | 95.86 (15) | C217—N23—C213—C214 | 1.7 (3) |
N11—Ni1—N13—C117 | −3.7 (2) | Ni2—N23—C213—C214 | −177.35 (17) |
O15—Ni1—N13—C117 | 177.8 (3) | C217—N23—C213—C212 | −178.2 (2) |
N12—Ni1—N13—C117 | 176.3 (2) | Ni2—N23—C213—C212 | 2.8 (2) |
O11—Ni1—N13—C117 | −82.0 (2) | N22—C212—C213—N23 | 1.9 (3) |
O13—Ni1—N13—C117 | 73.7 (2) | C211—C212—C213—N23 | −178.6 (2) |
N11—Ni1—N13—C113 | 173.88 (14) | N22—C212—C213—C214 | −178.0 (2) |
O15—Ni1—N13—C113 | −4.7 (4) | C211—C212—C213—C214 | 1.5 (3) |
N12—Ni1—N13—C113 | −6.16 (14) | N23—C213—C214—C215 | −1.6 (3) |
O11—Ni1—N13—C113 | 95.53 (14) | C212—C213—C214—C215 | 178.2 (2) |
O13—Ni1—N13—C113 | −108.70 (14) | N23—C213—C214—C219 | 178.9 (2) |
C105—N11—C101—C102 | −1.4 (3) | C212—C213—C214—C219 | −1.3 (3) |
Ni1—N11—C101—C102 | 171.26 (16) | C213—C214—C215—C216 | −0.2 (4) |
C105—N11—C101—C106 | −179.83 (18) | C219—C214—C215—C216 | 179.2 (3) |
Ni1—N11—C101—C106 | −7.2 (2) | C214—C215—C216—C217 | 1.9 (4) |
N11—C101—C102—C103 | 2.0 (3) | C213—N23—C217—C216 | 0.1 (3) |
C106—C101—C102—C103 | −179.9 (2) | Ni2—N23—C217—C216 | 178.95 (18) |
C101—C102—C103—C104 | −0.7 (4) | C215—C216—C217—N23 | −1.9 (4) |
C102—C103—C104—C105 | −1.1 (4) | C210—C211—C218—C219 | 179.1 (3) |
C101—N11—C105—C104 | −0.5 (3) | C212—C211—C218—C219 | −0.2 (4) |
Ni1—N11—C105—C104 | −173.09 (16) | C211—C218—C219—C214 | 0.4 (5) |
C101—N11—C105—C107 | 177.32 (17) | C215—C214—C219—C218 | −179.1 (3) |
Ni1—N11—C105—C107 | 4.7 (2) | C213—C214—C219—C218 | 0.3 (4) |
C103—C104—C105—N11 | 1.7 (3) | N31—Ni3—O31—C306 | −4.36 (13) |
C103—C104—C105—C107 | −175.7 (2) | O35—Ni3—O31—C306 | −99.77 (14) |
Ni1—O11—C106—O12 | 176.34 (18) | N32—Ni3—O31—C306 | 168.76 (14) |
Ni1—O11—C106—C101 | −4.0 (2) | N33—Ni3—O31—C306 | 88.54 (14) |
N11—C101—C106—O12 | −173.08 (19) | O33—Ni3—O31—C306 | −9.0 (2) |
C102—C101—C106—O12 | 8.6 (3) | N31—Ni3—O33—C307 | 0.36 (13) |
N11—C101—C106—O11 | 7.3 (3) | O35—Ni3—O33—C307 | 97.97 (14) |
C102—C101—C106—O11 | −171.0 (2) | N32—Ni3—O33—C307 | −172.66 (13) |
Ni1—O13—C107—O14 | 172.85 (18) | N33—Ni3—O33—C307 | −94.30 (14) |
Ni1—O13—C107—C105 | −6.6 (2) | O31—Ni3—O33—C307 | 5.0 (2) |
N11—C105—C107—O14 | −177.85 (19) | O35—Ni3—N31—C305 | −87.28 (15) |
C104—C105—C107—O14 | −0.2 (3) | N33—Ni3—N31—C305 | 83.35 (15) |
N11—C105—C107—O13 | 1.7 (3) | O31—Ni3—N31—C305 | 178.58 (16) |
C104—C105—C107—O13 | 179.3 (2) | O33—Ni3—N31—C305 | −3.42 (14) |
C112—N12—C108—C109 | 0.5 (4) | O35—Ni3—N31—C301 | 100.02 (14) |
Ni1—N12—C108—C109 | −176.22 (19) | N33—Ni3—N31—C301 | −89.36 (14) |
N12—C108—C109—C110 | 1.1 (4) | O31—Ni3—N31—C301 | 5.87 (13) |
C108—C109—C110—C111 | −1.5 (4) | O33—Ni3—N31—C301 | −176.12 (15) |
C109—C110—C111—C112 | 0.4 (4) | O35—Ni3—N32—C308 | −14.69 (18) |
C109—C110—C111—C118 | −179.5 (3) | N33—Ni3—N32—C308 | 175.28 (19) |
C108—N12—C112—C111 | −1.7 (3) | O31—Ni3—N32—C308 | 80.79 (18) |
Ni1—N12—C112—C111 | 175.49 (17) | O33—Ni3—N32—C308 | −100.19 (18) |
C108—N12—C112—C113 | 176.8 (2) | O35—Ni3—N32—C312 | 160.90 (14) |
Ni1—N12—C112—C113 | −6.0 (2) | N33—Ni3—N32—C312 | −9.13 (13) |
C110—C111—C112—N12 | 1.3 (3) | O31—Ni3—N32—C312 | −103.62 (13) |
C118—C111—C112—N12 | −178.8 (2) | O33—Ni3—N32—C312 | 75.39 (14) |
C110—C111—C112—C113 | −177.2 (2) | N31—Ni3—N33—C317 | −1.20 (19) |
C118—C111—C112—C113 | 2.7 (3) | O35—Ni3—N33—C317 | 136.7 (3) |
C117—N13—C113—C114 | 1.9 (3) | N32—Ni3—N33—C317 | −177.5 (2) |
Ni1—N13—C113—C114 | −175.92 (17) | O31—Ni3—N33—C317 | −79.85 (19) |
C117—N13—C113—C112 | −177.1 (2) | O33—Ni3—N33—C317 | 75.47 (19) |
Ni1—N13—C113—C112 | 5.0 (2) | N31—Ni3—N33—C313 | −174.37 (13) |
N12—C112—C113—N13 | 0.5 (3) | O35—Ni3—N33—C313 | −36.4 (4) |
C111—C112—C113—N13 | 179.13 (19) | N32—Ni3—N33—C313 | 9.32 (13) |
N12—C112—C113—C114 | −178.6 (2) | O31—Ni3—N33—C313 | 106.99 (13) |
C111—C112—C113—C114 | 0.0 (3) | O33—Ni3—N33—C313 | −97.69 (13) |
N13—C113—C114—C115 | −1.6 (3) | C305—N31—C301—C302 | −1.8 (3) |
C112—C113—C114—C115 | 177.5 (2) | Ni3—N31—C301—C302 | 170.74 (16) |
N13—C113—C114—C119 | 178.5 (2) | C305—N31—C301—C306 | −178.90 (17) |
C112—C113—C114—C119 | −2.4 (3) | Ni3—N31—C301—C306 | −6.4 (2) |
C113—C114—C115—C116 | −0.1 (4) | N31—C301—C302—C303 | 0.9 (3) |
C119—C114—C115—C116 | 179.8 (3) | C306—C301—C302—C303 | 177.6 (2) |
C114—C115—C116—C117 | 1.2 (4) | C301—C302—C303—C304 | 0.8 (4) |
C113—N13—C117—C116 | −0.7 (3) | C302—C303—C304—C305 | −1.6 (4) |
Ni1—N13—C117—C116 | 176.78 (17) | C301—N31—C305—C304 | 0.9 (3) |
C115—C116—C117—N13 | −0.9 (4) | Ni3—N31—C305—C304 | −171.46 (17) |
C110—C111—C118—C119 | 176.8 (3) | C301—N31—C305—C307 | 177.86 (16) |
C112—C111—C118—C119 | −3.1 (4) | Ni3—N31—C305—C307 | 5.5 (2) |
C111—C118—C119—C114 | 0.8 (5) | C303—C304—C305—N31 | 0.8 (3) |
C113—C114—C119—C118 | 2.0 (4) | C303—C304—C305—C307 | −175.7 (2) |
C115—C114—C119—C118 | −177.8 (3) | Ni3—O31—C306—O32 | −175.92 (17) |
N21—Ni2—O21—C206 | −2.51 (16) | Ni3—O31—C306—C301 | 2.3 (2) |
N22—Ni2—O21—C206 | 170.95 (16) | N31—C301—C306—O32 | −179.17 (17) |
O25—Ni2—O21—C206 | −99.07 (16) | C302—C301—C306—O32 | 3.9 (3) |
N23—Ni2—O21—C206 | 90.93 (16) | N31—C301—C306—O31 | 2.4 (3) |
O23—Ni2—O21—C206 | −9.1 (2) | C302—C301—C306—O31 | −174.5 (2) |
N21—Ni2—O23—C207 | 3.89 (14) | Ni3—O33—C307—O34 | −179.45 (17) |
N22—Ni2—O23—C207 | −169.55 (14) | Ni3—O33—C307—C305 | 2.3 (2) |
O25—Ni2—O23—C207 | 100.51 (15) | N31—C305—C307—O34 | 176.60 (18) |
N23—Ni2—O23—C207 | −89.91 (15) | C304—C305—C307—O34 | −6.7 (3) |
O21—Ni2—O23—C207 | 10.5 (2) | N31—C305—C307—O33 | −5.0 (3) |
O25—Ni2—N21—C201 | 92.64 (17) | C304—C305—C307—O33 | 171.7 (2) |
N23—Ni2—N21—C201 | −88.48 (17) | C312—N32—C308—C309 | −1.9 (3) |
O21—Ni2—N21—C201 | 3.85 (16) | Ni3—N32—C308—C309 | 173.55 (16) |
O23—Ni2—N21—C201 | −178.87 (17) | N32—C308—C309—C310 | −0.8 (3) |
O25—Ni2—N21—C205 | −92.14 (17) | C308—C309—C310—C311 | 2.6 (3) |
N23—Ni2—N21—C205 | 86.74 (16) | C309—C310—C311—C312 | −1.7 (3) |
O21—Ni2—N21—C205 | 179.07 (17) | C309—C310—C311—C318 | 179.0 (2) |
O23—Ni2—N21—C205 | −3.65 (15) | C308—N32—C312—C311 | 2.8 (3) |
O25—Ni2—N22—C208 | −0.9 (2) | Ni3—N32—C312—C311 | −173.32 (15) |
N23—Ni2—N22—C208 | −179.5 (2) | C308—N32—C312—C313 | −176.22 (18) |
O21—Ni2—N22—C208 | 89.1 (2) | Ni3—N32—C312—C313 | 7.6 (2) |
O23—Ni2—N22—C208 | −90.8 (2) | C310—C311—C312—N32 | −1.0 (3) |
O25—Ni2—N22—C212 | −176.11 (16) | C318—C311—C312—N32 | 178.25 (19) |
N23—Ni2—N22—C212 | 5.34 (15) | C310—C311—C312—C313 | 177.98 (19) |
O21—Ni2—N22—C212 | −86.04 (15) | C318—C311—C312—C313 | −2.7 (3) |
O23—Ni2—N22—C212 | 94.00 (15) | C317—N33—C313—C314 | −1.7 (3) |
N21—Ni2—N23—C217 | −5.1 (2) | Ni3—N33—C313—C314 | 172.52 (15) |
N22—Ni2—N23—C217 | 176.7 (2) | C317—N33—C313—C312 | 177.56 (18) |
O21—Ni2—N23—C217 | −84.0 (2) | Ni3—N33—C313—C312 | −8.3 (2) |
O23—Ni2—N23—C217 | 72.7 (2) | N32—C312—C313—N33 | 0.6 (3) |
N21—Ni2—N23—C213 | 173.78 (15) | C311—C312—C313—N33 | −178.47 (17) |
N22—Ni2—N23—C213 | −4.36 (14) | N32—C312—C313—C314 | 179.83 (17) |
O21—Ni2—N23—C213 | 94.94 (15) | C311—C312—C313—C314 | 0.8 (3) |
O23—Ni2—N23—C213 | −108.42 (14) | N33—C313—C314—C315 | 1.2 (3) |
C205—N21—C201—C202 | 0.7 (3) | C312—C313—C314—C315 | −177.94 (19) |
Ni2—N21—C201—C202 | 175.79 (19) | N33—C313—C314—C319 | −179.29 (19) |
C205—N21—C201—C206 | −179.47 (19) | C312—C313—C314—C319 | 1.5 (3) |
Ni2—N21—C201—C206 | −4.4 (3) | C313—C314—C315—C316 | 0.2 (3) |
N21—C201—C202—C203 | −0.1 (4) | C319—C314—C315—C316 | −179.3 (2) |
C206—C201—C202—C203 | −179.9 (3) | C314—C315—C316—C317 | −1.0 (3) |
C201—C202—C203—C204 | 0.2 (5) | C313—N33—C317—C316 | 0.7 (3) |
C202—C203—C204—C205 | −0.8 (4) | Ni3—N33—C317—C316 | −172.17 (16) |
C201—N21—C205—C204 | −1.4 (3) | C315—C316—C317—N33 | 0.6 (4) |
Ni2—N21—C205—C204 | −176.43 (18) | C310—C311—C318—C319 | −178.3 (2) |
C201—N21—C205—C207 | 177.97 (19) | C312—C311—C318—C319 | 2.5 (3) |
Ni2—N21—C205—C207 | 3.0 (2) | C311—C318—C319—C314 | −0.2 (4) |
C203—C204—C205—N21 | 1.4 (4) | C313—C314—C319—C318 | −1.9 (3) |
C203—C204—C205—C207 | −177.9 (2) | C315—C314—C319—C318 | 177.6 (2) |
Ni2—O21—C206—O22 | −178.3 (2) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O15—H15A···O23 | 0.77 (3) | 1.92 (3) | 2.682 (2) | 173 (3) |
O15—H15B···O1Wi | 0.77 (3) | 1.96 (3) | 2.707 (3) | 161 (3) |
O25—H25A···O2W | 0.80 (3) | 1.96 (3) | 2.710 (3) | 157 (3) |
O25—H25B···O13 | 0.77 (3) | 1.94 (3) | 2.711 (2) | 173 (3) |
O35—H35A···O34ii | 0.77 (3) | 1.98 (3) | 2.747 (2) | 173 (3) |
O35—H35B···O32iii | 0.91 (3) | 1.76 (3) | 2.657 (2) | 170 (2) |
O1W—H1W···O22 | 0.82 (4) | 2.09 (4) | 2.899 (4) | 168 (4) |
O1W—H2W···O24iv | 0.77 (3) | 2.03 (3) | 2.756 (4) | 157 (3) |
O2W—H3W···O1W | 0.88 (3) | 2.47 (3) | 3.346 (4) | 171 (3) |
O2W—H4W···O12iv | 1.00 (5) | 2.07 (6) | 2.971 (3) | 149 (4) |
O3W—H5W···O31 | 0.84 (4) | 2.06 (4) | 2.878 (3) | 165 (4) |
O3W—H6W···O34i | 0.80 (3) | 2.10 (4) | 2.880 (3) | 166 (4) |
Symmetry codes: (i) x+1, y, z; (ii) −x, −y, −z; (iii) −x+1, −y, −z; (iv) x−1, y, z. |