A nickel(II) coordination polymer,
catena-poly[[aquatripyridinenickel(II)]-μ-isophthalato], [Ni(C
8H
4O
4)(C
5H
5N)
3(H
2O)]
n, obtained by reaction of
m-bda, pyridine and Ni(NO
3)
2·6H
2O under hydrothermal conditions, where
m-bda is isophthalic acid, was characterized by single-crystal X-ray diffraction. The Ni
II atom is six-coordinate and lies at the centre of a distorted octahedron, coordinated by two carboxylate O atoms from two
m-bda ligands, three N atoms from three pyridine molecules and one water molecule. The carboxylate groups of
m-bda link the Ni
II atoms, forming an extended one-dimensional zigzag chain. The chains are then knitted together, forming a two-dimensional supramolecular arrangement,
via C—H
O hydrogen bonds between the H atoms of pyridine rings and the coordinated carboxylate O atoms of
m-bda.
Supporting information
CCDC reference: 298561
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- R factor = 0.038
- wR factor = 0.071
- Data-to-parameter ratio = 18.2
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.87 Ratio
| Author Response: There are two H atoms bond to the water O5W atom. Both of the H atoms
have hydrogen-bond interaction, which
results in the large Ueq Ratio (Ueq(H5B)/Ueq(H5A))
|
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 78.00 A 3
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; 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.
catena-poly[[aquatripyridinenickel(II)]-µ-isophthalato]
top
Crystal data top
[Ni(C8H4O4)(C5H5N)3(H2O)] | F(000) = 992 |
Mr = 478.14 | Dx = 1.385 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 9.0723 (5) Å | Cell parameters from 13853 reflections |
b = 15.1897 (8) Å | θ = 1.8–28.2° |
c = 16.6524 (9) Å | µ = 0.88 mm−1 |
β = 91.886 (1)° | T = 293 K |
V = 2293.5 (2) Å3 | Block, blue |
Z = 4 | 0.35 × 0.29 × 0.23 mm |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 5392 independent reflections |
Radiation source: fine-focus sealed tube | 2787 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.042 |
Detector resolution: 10.0 pixels mm-1 | θmax = 28.3°, θmin = 1.8° |
ω scans | h = −12→11 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −19→20 |
Tmin = 0.751, Tmax = 0.814 | l = −22→15 |
14005 measured reflections | |
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)] = 0.038 | Hydrogen site location: geom and difmap |
wR(F2) = 0.071 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0201P)2] where P = (Fo2 + 2Fc2)/3 |
5392 reflections | (Δ/σ)max = 0.001 |
297 parameters | Δρmax = 0.29 e Å−3 |
0 restraints | Δρmin = −0.39 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 | −0.1103 (3) | 0.28392 (15) | 0.07613 (14) | 0.0542 (7) | |
H1 | −0.0219 | 0.2911 | 0.0501 | 0.065* | |
C2 | −0.2400 (3) | 0.29249 (16) | 0.03144 (15) | 0.0607 (7) | |
H2 | −0.2386 | 0.3057 | −0.0231 | 0.073* | |
C3 | −0.3715 (3) | 0.28119 (14) | 0.06883 (16) | 0.0604 (7) | |
H3 | −0.4609 | 0.2857 | 0.0401 | 0.072* | |
C4 | −0.3675 (3) | 0.26319 (15) | 0.14910 (16) | 0.0601 (7) | |
H4 | −0.4545 | 0.2555 | 0.1762 | 0.072* | |
C5 | −0.2340 (3) | 0.25659 (14) | 0.18927 (14) | 0.0567 (6) | |
H5 | −0.2333 | 0.2449 | 0.2441 | 0.068* | |
C6 | 0.3616 (3) | 0.29492 (16) | 0.32772 (14) | 0.0539 (7) | |
H6 | 0.3152 | 0.3495 | 0.3266 | 0.065* | |
C7 | 0.4910 (3) | 0.28624 (18) | 0.37249 (14) | 0.0606 (7) | |
H7 | 0.5302 | 0.3338 | 0.4011 | 0.073* | |
C8 | 0.5613 (3) | 0.20643 (19) | 0.37424 (15) | 0.0638 (7) | |
H8 | 0.6484 | 0.1985 | 0.4044 | 0.077* | |
C9 | 0.5001 (3) | 0.13842 (17) | 0.33039 (14) | 0.0609 (7) | |
H9 | 0.5460 | 0.0837 | 0.3297 | 0.073* | |
C10 | 0.3699 (3) | 0.15199 (16) | 0.28735 (13) | 0.0535 (7) | |
H10 | 0.3294 | 0.1052 | 0.2581 | 0.064* | |
C11 | −0.0073 (3) | 0.13249 (15) | 0.35274 (14) | 0.0530 (6) | |
H11 | 0.0316 | 0.1785 | 0.3836 | 0.064* | |
C12 | −0.0809 (3) | 0.06672 (17) | 0.39078 (16) | 0.0760 (9) | |
H12 | −0.0932 | 0.0684 | 0.4460 | 0.091* | |
C13 | −0.1363 (3) | −0.00209 (18) | 0.3452 (2) | 0.0880 (10) | |
H13 | −0.1877 | −0.0476 | 0.3691 | 0.106* | |
C14 | −0.1149 (3) | −0.00271 (16) | 0.26429 (18) | 0.0768 (9) | |
H14 | −0.1496 | −0.0490 | 0.2324 | 0.092* | |
C15 | −0.0411 (3) | 0.06655 (15) | 0.23119 (15) | 0.0578 (7) | |
H15 | −0.0272 | 0.0661 | 0.1761 | 0.069* | |
C16 | 0.2371 (2) | 0.19310 (15) | 0.06644 (12) | 0.0401 (5) | |
C17 | 0.2821 (2) | 0.11976 (14) | 0.01114 (12) | 0.0377 (5) | |
C18 | 0.2480 (3) | 0.03284 (15) | 0.02536 (14) | 0.0568 (7) | |
H18 | 0.1959 | 0.0180 | 0.0706 | 0.068* | |
C19 | 0.2902 (3) | −0.03237 (15) | −0.02684 (15) | 0.0685 (8) | |
H19 | 0.2669 | −0.0908 | −0.0165 | 0.082* | |
C20 | 0.3673 (3) | −0.01087 (15) | −0.09455 (14) | 0.0575 (7) | |
H20 | 0.3959 | −0.0550 | −0.1294 | 0.069* | |
C21 | 0.4019 (2) | 0.07581 (13) | −0.11053 (12) | 0.0397 (6) | |
C22 | 0.3590 (2) | 0.13961 (14) | −0.05730 (11) | 0.0382 (5) | |
H22 | 0.3825 | 0.1981 | −0.0676 | 0.046* | |
C23 | 0.4862 (2) | 0.10101 (15) | −0.18384 (13) | 0.0445 (6) | |
H5A | 0.115 (3) | 0.3905 (15) | 0.1643 (15) | 0.063 (10)* | |
H5B | 0.211 (4) | 0.350 (2) | 0.123 (2) | 0.178 (18)* | |
N1 | −0.1041 (2) | 0.26605 (11) | 0.15418 (11) | 0.0485 (5) | |
N2 | 0.01153 (19) | 0.13409 (11) | 0.27380 (11) | 0.0433 (5) | |
N3 | 0.2992 (2) | 0.22878 (12) | 0.28557 (11) | 0.0463 (5) | |
Ni1 | 0.09974 (3) | 0.247460 (19) | 0.219975 (15) | 0.04269 (10) | |
O1 | 0.17270 (16) | 0.16992 (9) | 0.12911 (8) | 0.0477 (4) | |
O2 | 0.26464 (17) | 0.27053 (9) | 0.04662 (9) | 0.0534 (4) | |
O3 | 0.52068 (16) | 0.18125 (9) | −0.18790 (8) | 0.0493 (4) | |
O4 | 0.5149 (2) | 0.04519 (10) | −0.23416 (11) | 0.0884 (7) | |
O5W | 0.1940 (3) | 0.36099 (13) | 0.17545 (12) | 0.0671 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0531 (17) | 0.0724 (17) | 0.0376 (15) | 0.0047 (13) | 0.0090 (12) | 0.0022 (13) |
C2 | 0.0583 (19) | 0.0849 (18) | 0.0388 (15) | 0.0125 (15) | 0.0015 (14) | −0.0018 (14) |
C3 | 0.0508 (18) | 0.0684 (17) | 0.0613 (18) | 0.0000 (13) | −0.0073 (14) | −0.0084 (14) |
C4 | 0.0490 (17) | 0.0680 (18) | 0.0641 (18) | −0.0028 (14) | 0.0121 (13) | 0.0060 (15) |
C5 | 0.0591 (17) | 0.0661 (16) | 0.0456 (14) | 0.0027 (15) | 0.0137 (12) | 0.0133 (14) |
C6 | 0.0579 (18) | 0.0552 (15) | 0.0491 (16) | −0.0088 (13) | 0.0103 (13) | −0.0090 (13) |
C7 | 0.0551 (19) | 0.0796 (19) | 0.0470 (17) | −0.0148 (16) | −0.0014 (14) | −0.0147 (14) |
C8 | 0.0512 (18) | 0.091 (2) | 0.0489 (17) | 0.0000 (17) | 0.0015 (13) | −0.0049 (16) |
C9 | 0.0528 (18) | 0.0722 (18) | 0.0578 (18) | 0.0020 (15) | 0.0027 (14) | −0.0082 (15) |
C10 | 0.0498 (18) | 0.0637 (17) | 0.0473 (16) | −0.0088 (14) | 0.0045 (13) | −0.0104 (14) |
C11 | 0.0658 (18) | 0.0524 (15) | 0.0410 (15) | 0.0009 (13) | 0.0035 (12) | 0.0075 (13) |
C12 | 0.111 (3) | 0.0617 (17) | 0.0571 (19) | 0.0019 (17) | 0.0236 (18) | 0.0186 (16) |
C13 | 0.110 (3) | 0.0586 (19) | 0.097 (3) | −0.0126 (18) | 0.028 (2) | 0.0238 (19) |
C14 | 0.093 (2) | 0.0579 (18) | 0.080 (2) | −0.0242 (16) | 0.0025 (18) | −0.0017 (16) |
C15 | 0.0621 (19) | 0.0596 (16) | 0.0519 (17) | −0.0099 (14) | 0.0060 (13) | −0.0039 (14) |
C16 | 0.0305 (13) | 0.0582 (16) | 0.0316 (13) | 0.0014 (11) | 0.0006 (10) | −0.0026 (12) |
C17 | 0.0333 (13) | 0.0465 (13) | 0.0333 (13) | −0.0017 (11) | 0.0035 (10) | −0.0004 (11) |
C18 | 0.0687 (19) | 0.0576 (15) | 0.0454 (15) | −0.0088 (13) | 0.0224 (13) | 0.0021 (13) |
C19 | 0.098 (2) | 0.0445 (14) | 0.0645 (18) | −0.0176 (14) | 0.0303 (16) | −0.0039 (14) |
C20 | 0.0753 (19) | 0.0474 (14) | 0.0511 (16) | −0.0067 (13) | 0.0208 (13) | −0.0095 (13) |
C21 | 0.0406 (15) | 0.0426 (13) | 0.0364 (13) | −0.0032 (11) | 0.0067 (11) | −0.0067 (11) |
C22 | 0.0355 (14) | 0.0444 (13) | 0.0349 (12) | −0.0001 (10) | 0.0027 (10) | 0.0011 (11) |
C23 | 0.0479 (16) | 0.0469 (14) | 0.0392 (15) | −0.0026 (12) | 0.0101 (12) | −0.0070 (13) |
N1 | 0.0520 (13) | 0.0564 (13) | 0.0378 (11) | 0.0039 (10) | 0.0116 (9) | 0.0035 (10) |
N2 | 0.0452 (13) | 0.0483 (12) | 0.0366 (12) | −0.0034 (9) | 0.0049 (9) | −0.0010 (10) |
N3 | 0.0461 (12) | 0.0521 (13) | 0.0412 (12) | −0.0054 (10) | 0.0088 (9) | −0.0065 (10) |
Ni1 | 0.04917 (18) | 0.04774 (17) | 0.03189 (15) | −0.00513 (16) | 0.01236 (12) | −0.00088 (16) |
O1 | 0.0577 (11) | 0.0531 (9) | 0.0333 (9) | −0.0062 (8) | 0.0158 (8) | −0.0024 (8) |
O2 | 0.0672 (12) | 0.0472 (10) | 0.0473 (10) | 0.0008 (8) | 0.0242 (8) | 0.0002 (8) |
O3 | 0.0687 (12) | 0.0436 (9) | 0.0369 (9) | 0.0021 (8) | 0.0220 (8) | −0.0018 (8) |
O4 | 0.1388 (19) | 0.0555 (11) | 0.0751 (14) | −0.0217 (11) | 0.0655 (13) | −0.0240 (10) |
O5W | 0.0863 (17) | 0.0588 (12) | 0.0579 (13) | −0.0081 (12) | 0.0292 (12) | 0.0020 (11) |
Geometric parameters (Å, º) top
C1—N1 | 1.327 (3) | C14—C15 | 1.372 (3) |
C1—C2 | 1.378 (3) | C14—H14 | 0.9300 |
C1—H1 | 0.9300 | C15—N2 | 1.327 (2) |
C2—C3 | 1.374 (3) | C15—H15 | 0.9300 |
C2—H2 | 0.9300 | C16—O2 | 1.249 (2) |
C3—C4 | 1.364 (3) | C16—O1 | 1.263 (2) |
C3—H3 | 0.9300 | C16—C17 | 1.510 (3) |
C4—C5 | 1.367 (3) | C17—C18 | 1.378 (3) |
C4—H4 | 0.9300 | C17—C22 | 1.389 (2) |
C5—N1 | 1.340 (3) | C18—C19 | 1.380 (3) |
C5—H5 | 0.9300 | C18—H18 | 0.9300 |
C6—N3 | 1.341 (3) | C19—C20 | 1.385 (3) |
C6—C7 | 1.376 (3) | C19—H19 | 0.9300 |
C6—H6 | 0.9300 | C20—C21 | 1.381 (3) |
C7—C8 | 1.370 (3) | C20—H20 | 0.9300 |
C7—H7 | 0.9300 | C21—C22 | 1.378 (2) |
C8—C9 | 1.372 (3) | C21—C23 | 1.511 (3) |
C8—H8 | 0.9300 | C22—H22 | 0.9300 |
C9—C10 | 1.377 (3) | C23—O4 | 1.226 (2) |
C9—H9 | 0.9300 | C23—O3 | 1.261 (2) |
C10—N3 | 1.331 (3) | N1—Ni1 | 2.1372 (19) |
C10—H10 | 0.9300 | N2—Ni1 | 2.1110 (17) |
C11—N2 | 1.331 (2) | N3—Ni1 | 2.102 (2) |
C11—C12 | 1.368 (3) | Ni1—O3i | 2.0280 (13) |
C11—H11 | 0.9300 | Ni1—O1 | 2.0446 (13) |
C12—C13 | 1.377 (3) | Ni1—O5W | 2.0727 (17) |
C12—H12 | 0.9300 | O3—Ni1ii | 2.0280 (13) |
C13—C14 | 1.367 (4) | O5W—H5A | 0.86 (2) |
C13—H13 | 0.9300 | O5W—H5B | 0.90 (4) |
| | | |
N1—C1—C2 | 123.8 (2) | C18—C17—C16 | 122.34 (18) |
N1—C1—H1 | 118.1 | C22—C17—C16 | 119.58 (19) |
C2—C1—H1 | 118.1 | C17—C18—C19 | 120.7 (2) |
C3—C2—C1 | 118.8 (2) | C17—C18—H18 | 119.7 |
C3—C2—H2 | 120.6 | C19—C18—H18 | 119.7 |
C1—C2—H2 | 120.6 | C18—C19—C20 | 120.1 (2) |
C4—C3—C2 | 118.3 (2) | C18—C19—H19 | 120.0 |
C4—C3—H3 | 120.9 | C20—C19—H19 | 120.0 |
C2—C3—H3 | 120.9 | C21—C20—C19 | 120.4 (2) |
C3—C4—C5 | 119.3 (2) | C21—C20—H20 | 119.8 |
C3—C4—H4 | 120.4 | C19—C20—H20 | 119.8 |
C5—C4—H4 | 120.4 | C22—C21—C20 | 118.40 (19) |
N1—C5—C4 | 123.8 (2) | C22—C21—C23 | 120.17 (18) |
N1—C5—H5 | 118.1 | C20—C21—C23 | 121.42 (19) |
C4—C5—H5 | 118.1 | C21—C22—C17 | 122.35 (19) |
N3—C6—C7 | 123.4 (2) | C21—C22—H22 | 118.8 |
N3—C6—H6 | 118.3 | C17—C22—H22 | 118.8 |
C7—C6—H6 | 118.3 | O4—C23—O3 | 125.0 (2) |
C8—C7—C6 | 119.0 (2) | O4—C23—C21 | 120.1 (2) |
C8—C7—H7 | 120.5 | O3—C23—C21 | 114.92 (19) |
C6—C7—H7 | 120.5 | C1—N1—C5 | 116.1 (2) |
C7—C8—C9 | 118.4 (2) | C1—N1—Ni1 | 122.47 (15) |
C7—C8—H8 | 120.8 | C5—N1—Ni1 | 121.39 (16) |
C9—C8—H8 | 120.8 | C15—N2—C11 | 117.26 (19) |
C8—C9—C10 | 119.3 (2) | C15—N2—Ni1 | 122.57 (15) |
C8—C9—H9 | 120.3 | C11—N2—Ni1 | 119.79 (16) |
C10—C9—H9 | 120.3 | C10—N3—C6 | 116.7 (2) |
N3—C10—C9 | 123.2 (2) | C10—N3—Ni1 | 122.41 (16) |
N3—C10—H10 | 118.4 | C6—N3—Ni1 | 120.86 (16) |
C9—C10—H10 | 118.4 | O3i—Ni1—O1 | 176.88 (6) |
N2—C11—C12 | 123.4 (2) | O3i—Ni1—O5W | 89.24 (7) |
N2—C11—H11 | 118.3 | O1—Ni1—O5W | 93.85 (7) |
C12—C11—H11 | 118.3 | O3i—Ni1—N3 | 89.93 (7) |
C11—C12—C13 | 118.3 (3) | O1—Ni1—N3 | 90.73 (6) |
C11—C12—H12 | 120.9 | O5W—Ni1—N3 | 86.56 (8) |
C13—C12—H12 | 120.9 | O3i—Ni1—N2 | 88.05 (6) |
C14—C13—C12 | 119.2 (3) | O1—Ni1—N2 | 88.90 (6) |
C14—C13—H13 | 120.4 | O5W—Ni1—N2 | 175.67 (8) |
C12—C13—H13 | 120.4 | N3—Ni1—N2 | 90.06 (7) |
C13—C14—C15 | 118.5 (3) | O3i—Ni1—N1 | 89.74 (6) |
C13—C14—H14 | 120.7 | O1—Ni1—N1 | 89.57 (6) |
C15—C14—H14 | 120.7 | O5W—Ni1—N1 | 93.84 (8) |
N2—C15—C14 | 123.3 (2) | N3—Ni1—N1 | 179.48 (7) |
N2—C15—H15 | 118.3 | N2—Ni1—N1 | 89.52 (7) |
C14—C15—H15 | 118.3 | C16—O1—Ni1 | 128.38 (14) |
O2—C16—O1 | 125.7 (2) | C23—O3—Ni1ii | 130.64 (14) |
O2—C16—C17 | 118.22 (18) | Ni1—O5W—H5A | 99.1 (16) |
O1—C16—C17 | 116.12 (19) | Ni1—O5W—H5B | 106 (2) |
C18—C17—C22 | 118.08 (19) | H5A—O5W—H5B | 94 (3) |
| | | |
N1—C1—C2—C3 | −0.7 (4) | C12—C11—N2—Ni1 | 171.24 (19) |
C1—C2—C3—C4 | 0.9 (3) | C9—C10—N3—C6 | 0.7 (3) |
C2—C3—C4—C5 | −0.3 (3) | C9—C10—N3—Ni1 | −179.56 (16) |
C3—C4—C5—N1 | −0.6 (4) | C7—C6—N3—C10 | −1.1 (3) |
N3—C6—C7—C8 | 0.4 (4) | C7—C6—N3—Ni1 | 179.19 (17) |
C6—C7—C8—C9 | 0.6 (3) | C10—N3—Ni1—O3i | 138.67 (17) |
C7—C8—C9—C10 | −1.0 (3) | C6—N3—Ni1—O3i | −41.64 (16) |
C8—C9—C10—N3 | 0.3 (4) | C10—N3—Ni1—O1 | −38.28 (17) |
N2—C11—C12—C13 | 1.1 (4) | C6—N3—Ni1—O1 | 141.42 (15) |
C11—C12—C13—C14 | 0.6 (4) | C10—N3—Ni1—O5W | −132.09 (18) |
C12—C13—C14—C15 | −1.3 (5) | C6—N3—Ni1—O5W | 47.60 (16) |
C13—C14—C15—N2 | 0.4 (4) | C10—N3—Ni1—N2 | 50.62 (17) |
O2—C16—C17—C18 | −175.8 (2) | C6—N3—Ni1—N2 | −129.68 (16) |
O1—C16—C17—C18 | 3.6 (3) | C15—N2—Ni1—O3i | 146.89 (17) |
O2—C16—C17—C22 | 3.4 (3) | C11—N2—Ni1—O3i | −25.89 (16) |
O1—C16—C17—C22 | −177.3 (2) | C15—N2—Ni1—O1 | −32.45 (17) |
C22—C17—C18—C19 | 0.4 (4) | C11—N2—Ni1—O1 | 154.77 (17) |
C16—C17—C18—C19 | 179.6 (2) | C15—N2—Ni1—N3 | −123.18 (17) |
C17—C18—C19—C20 | −0.2 (4) | C11—N2—Ni1—N3 | 64.04 (17) |
C18—C19—C20—C21 | −0.3 (4) | C15—N2—Ni1—N1 | 57.13 (17) |
C19—C20—C21—C22 | 0.6 (4) | C11—N2—Ni1—N1 | −115.65 (17) |
C19—C20—C21—C23 | 179.9 (2) | C1—N1—Ni1—O3i | 138.26 (17) |
C20—C21—C22—C17 | −0.3 (3) | C5—N1—Ni1—O3i | −44.56 (17) |
C23—C21—C22—C17 | −179.6 (2) | C1—N1—Ni1—O1 | −44.79 (17) |
C18—C17—C22—C21 | −0.2 (3) | C5—N1—Ni1—O1 | 132.39 (17) |
C16—C17—C22—C21 | −179.33 (19) | C1—N1—Ni1—O5W | 49.04 (18) |
C22—C21—C23—O4 | −174.7 (2) | C5—N1—Ni1—O5W | −133.78 (17) |
C20—C21—C23—O4 | 6.0 (4) | C1—N1—Ni1—N2 | −133.69 (17) |
C22—C21—C23—O3 | 4.7 (3) | C5—N1—Ni1—N2 | 43.49 (17) |
C20—C21—C23—O3 | −174.6 (2) | O2—C16—O1—Ni1 | −2.5 (3) |
C2—C1—N1—C5 | −0.2 (3) | C17—C16—O1—Ni1 | 178.19 (13) |
C2—C1—N1—Ni1 | 177.10 (18) | O5W—Ni1—O1—C16 | −6.73 (19) |
C4—C5—N1—C1 | 0.9 (3) | N3—Ni1—O1—C16 | −93.34 (18) |
C4—C5—N1—Ni1 | −176.46 (18) | N2—Ni1—O1—C16 | 176.61 (18) |
C14—C15—N2—C11 | 1.2 (3) | N1—Ni1—O1—C16 | 87.09 (18) |
C14—C15—N2—Ni1 | −171.8 (2) | O4—C23—O3—Ni1ii | 11.4 (4) |
C12—C11—N2—C15 | −1.9 (3) | C21—C23—O3—Ni1ii | −167.96 (14) |
Symmetry codes: (i) x−1/2, −y+1/2, z+1/2; (ii) x+1/2, −y+1/2, z−1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5W—H5B···O2 | 0.94 (4) | 1.81 (4) | 2.647 (3) | 146 (4) |
O5W—H5A···O4i | 0.87 (3) | 2.18 (3) | 2.664 (3) | 115 (2) |
C3—H3···O2iii | 0.93 | 2.51 | 3.315 (4) | 145 |
C8—H8···O2iv | 0.93 | 2.60 | 3.378 (3) | 141 |
Symmetry codes: (i) x−1/2, −y+1/2, z+1/2; (iii) x−1, y, z; (iv) x+1/2, −y+1/2, z+1/2. |