In the title complex, triaqua{μ-2,6-bis[2-(dimethylamino)ethyliminomethyl]-4-methylphenolato}-μ-bromo-bromodinickel(II) bromide monohydrate acetonitrile disolvate, [Ni2Br2(C17H27N4O)(H2O)3]Br·H2O·2C2H3N, the NiII atoms are octahedrally coordinated and the donor groups are different (N2O3Br and N2O2Br2), with an intermetallic separation of 3.2346 (9) Å.
Supporting information
CCDC reference: 236051
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean
(C-C) = 0.007 Å
- R factor = 0.041
- wR factor = 0.087
- Data-to-parameter ratio = 16.3
checkCIF/PLATON results
No syntax errors found
Alert level C
RINTA01_ALERT_3_C The value of Rint is greater than 0.10
Rint given 0.102
PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.10
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... C21
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 8
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
6 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
3 ALERT type 3 Indicator that the structure quality may be low
3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1997); cell refinement: SMART (Bruker, 1997); data reduction: SHELXTL (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Crystal data top
[Ni2Br2(C17H27N4O)(H2O)3]Br·H2O·2C2H3N | F(000) = 1640 |
Mr = 814.75 | Dx = 1.739 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 10.5662 (13) Å | Cell parameters from 4188 reflections |
b = 11.8911 (15) Å | θ = 4.5–55.9° |
c = 25.158 (3) Å | µ = 5.1 mm−1 |
β = 100.039 (2)° | T = 150 K |
V = 3112.5 (7) Å3 | Block, green |
Z = 4 | 0.25 × 0.18 × 0.1 mm |
Data collection top
CCD area detector diffractometer | 3844 reflections with I > 2σ(I) |
ω scans | Rint = 0.102 |
Absorption correction: multi-scan SADABS | θmax = 25°, θmin = 1.6° |
Tmin = 0.344, Tmax = 0.600 | h = −12→12 |
14837 measured reflections | k = −13→14 |
5468 independent reflections | l = −14→29 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.041 | w = 1/[σ2(Fo2) + (0.0396P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.088 | (Δ/σ)max = 0.004 |
S = 0.87 | Δρmax = 0.79 e Å−3 |
5468 reflections | Δρmin = −0.68 e Å−3 |
336 parameters | |
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. Hydrogen atoms for the solvent water molecules were calculated by
difference Fourier and the H atoms for acetonitrile solvent molecules were
calculated using SHELXTL defaults and refined in riding mode. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ni1 | 0.81815 (6) | 0.43356 (5) | 0.14829 (2) | 0.01980 (15) | |
Ni2 | 1.07830 (6) | 0.57845 (5) | 0.15104 (2) | 0.02007 (16) | |
N1 | 0.7472 (4) | 0.3633 (3) | 0.20799 (15) | 0.0203 (9) | |
N2 | 0.6588 (4) | 0.3550 (3) | 0.09806 (15) | 0.0246 (10) | |
N3 | 1.2025 (4) | 0.6669 (3) | 0.10632 (15) | 0.0264 (10) | |
N4 | 1.1978 (4) | 0.6352 (3) | 0.21460 (15) | 0.0210 (9) | |
O1 | 0.9667 (3) | 0.5039 (2) | 0.20028 (11) | 0.0203 (7) | |
Br1 | 0.68349 (5) | 0.62015 (4) | 0.158445 (19) | 0.02665 (14) | |
Br2 | 0.40820 (5) | 0.41207 (4) | 0.26204 (2) | 0.02823 (14) | |
Br3 | 0.92346 (5) | 0.50352 (4) | 0.071415 (18) | 0.02464 (13) | |
C1 | 0.9834 (5) | 0.5060 (4) | 0.25366 (17) | 0.0200 (11) | |
C2 | 1.0874 (5) | 0.5646 (4) | 0.28553 (18) | 0.0201 (11) | |
C3 | 1.1014 (5) | 0.5627 (4) | 0.34183 (18) | 0.0252 (12) | |
H3A | 1.1719 | 0.6021 | 0.3621 | 0.030* | |
C4 | 1.0187 (5) | 0.5069 (4) | 0.36972 (18) | 0.0265 (12) | |
C5 | 0.9178 (5) | 0.4516 (4) | 0.33876 (18) | 0.0243 (12) | |
H5A | 0.8589 | 0.4128 | 0.3567 | 0.029* | |
C6 | 0.8968 (5) | 0.4489 (4) | 0.28251 (18) | 0.0204 (11) | |
C7 | 0.7861 (5) | 0.3812 (4) | 0.25804 (18) | 0.0203 (11) | |
H7A | 0.7380 | 0.3468 | 0.2822 | 0.024* | |
C8 | 0.6403 (5) | 0.2865 (4) | 0.18958 (18) | 0.0255 (12) | |
H8A | 0.5827 | 0.2826 | 0.2166 | 0.031* | |
H8B | 0.6732 | 0.2100 | 0.1845 | 0.031* | |
C9 | 0.5680 (5) | 0.3315 (4) | 0.13649 (19) | 0.0272 (12) | |
H9A | 0.5030 | 0.2758 | 0.1203 | 0.033* | |
H9B | 0.5226 | 0.4016 | 0.1431 | 0.033* | |
C10 | 1.2670 (5) | 0.7499 (4) | 0.14618 (18) | 0.0275 (12) | |
H10A | 1.2072 | 0.8124 | 0.1498 | 0.033* | |
H10B | 1.3429 | 0.7816 | 0.1333 | 0.033* | |
C11 | 1.3087 (5) | 0.6947 (4) | 0.20040 (19) | 0.0256 (12) | |
H11A | 1.3796 | 0.6411 | 0.1986 | 0.031* | |
H11B | 1.3398 | 0.7522 | 0.2280 | 0.031* | |
C12 | 1.1860 (5) | 0.6243 (4) | 0.26417 (18) | 0.0225 (11) | |
H12A | 1.2499 | 0.6599 | 0.2899 | 0.027* | |
C13 | 0.6992 (5) | 0.2486 (4) | 0.07548 (19) | 0.0328 (13) | |
H13A | 0.6249 | 0.2133 | 0.0529 | 0.049* | |
H13B | 0.7343 | 0.1977 | 0.1050 | 0.049* | |
H13C | 0.7652 | 0.2645 | 0.0535 | 0.049* | |
C14 | 0.5935 (5) | 0.4243 (5) | 0.05395 (18) | 0.0332 (13) | |
H14A | 0.5218 | 0.3820 | 0.0333 | 0.050* | |
H14B | 0.6541 | 0.4451 | 0.0302 | 0.050* | |
H14C | 0.5606 | 0.4925 | 0.0687 | 0.050* | |
C15 | 1.1333 (5) | 0.7290 (4) | 0.05864 (19) | 0.0333 (13) | |
H15A | 1.1957 | 0.7664 | 0.0400 | 0.050* | |
H15B | 1.0766 | 0.7853 | 0.0706 | 0.050* | |
H15C | 1.0819 | 0.6760 | 0.0339 | 0.050* | |
C16 | 1.2985 (5) | 0.5928 (4) | 0.0880 (2) | 0.0347 (14) | |
H16A | 1.3524 | 0.6372 | 0.0678 | 0.052* | |
H16B | 1.2543 | 0.5339 | 0.0645 | 0.052* | |
H16C | 1.3524 | 0.5582 | 0.1193 | 0.052* | |
C17 | 1.0411 (6) | 0.5036 (4) | 0.43073 (18) | 0.0343 (13) | |
H17A | 0.9728 | 0.4597 | 0.4427 | 0.052* | |
H17B | 1.0405 | 0.5803 | 0.4448 | 0.052* | |
H17C | 1.1245 | 0.4685 | 0.4442 | 0.052* | |
N5 | 0.2358 (5) | 0.2975 (4) | 0.06533 (19) | 0.0457 (13) | |
C18 | 0.2516 (5) | 0.2751 (4) | 0.0233 (2) | 0.0331 (13) | |
C19 | 0.2753 (6) | 0.2474 (5) | −0.03043 (19) | 0.0415 (15) | |
H19A | 0.2929 | 0.3165 | −0.0491 | 0.062* | |
H19B | 0.1994 | 0.2102 | −0.0509 | 0.062* | |
H19C | 0.3495 | 0.1969 | −0.0275 | 0.062* | |
N6 | 0.8338 (7) | 0.0137 (5) | 0.0290 (3) | 0.0721 (18) | |
C21 | 0.9275 (7) | 0.0317 (5) | 0.0569 (3) | 0.0446 (16) | |
C20 | 1.0464 (6) | 0.0526 (5) | 0.0928 (2) | 0.0497 (17) | |
H20A | 1.0549 | 0.1334 | 0.1005 | 0.074* | |
H20B | 1.1183 | 0.0275 | 0.0759 | 0.074* | |
H20C | 1.0472 | 0.0113 | 0.1266 | 0.074* | |
O1W | 0.8943 (3) | 0.1239 (3) | 0.21606 (14) | 0.0350 (9) | |
H1WA | 0.9438 | 0.0710 | 0.2295 | 0.042* | |
H1WB | 0.8755 | 0.1293 | 0.2475 | 0.042* | |
O2W | 0.9432 (3) | 0.2916 (3) | 0.14973 (12) | 0.0250 (8) | |
H2WA | 1.0184 | 0.3177 | 0.1599 | 0.030* | |
H2WB | 0.9200 | 0.2395 | 0.1691 | 0.030* | |
O3W | 1.1767 (3) | 0.4181 (3) | 0.15724 (12) | 0.0253 (8) | |
H3WA | 1.1940 | 0.3825 | 0.1301 | 0.030* | |
H3WB | 1.2367 | 0.4166 | 0.1845 | 0.030* | |
O4W | 0.9652 (3) | 0.7244 (2) | 0.15005 (12) | 0.0237 (8) | |
H4WA | 0.9985 | 0.7733 | 0.1729 | 0.028* | |
H4WB | 0.8919 | 0.6972 | 0.1521 | 0.028* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0218 (4) | 0.0167 (3) | 0.0219 (3) | −0.0015 (3) | 0.0064 (3) | −0.0012 (2) |
Ni2 | 0.0213 (4) | 0.0168 (3) | 0.0233 (3) | −0.0006 (3) | 0.0070 (3) | −0.0005 (2) |
N1 | 0.023 (2) | 0.012 (2) | 0.027 (2) | −0.0014 (18) | 0.0090 (18) | 0.0015 (16) |
N2 | 0.025 (3) | 0.024 (2) | 0.025 (2) | 0.000 (2) | 0.0076 (19) | −0.0046 (17) |
N3 | 0.027 (3) | 0.024 (2) | 0.030 (2) | −0.004 (2) | 0.010 (2) | −0.0013 (18) |
N4 | 0.019 (2) | 0.014 (2) | 0.030 (2) | 0.0000 (18) | 0.0048 (18) | 0.0001 (16) |
O1 | 0.022 (2) | 0.0182 (17) | 0.0220 (17) | −0.0030 (14) | 0.0070 (14) | −0.0001 (13) |
Br1 | 0.0264 (3) | 0.0205 (3) | 0.0343 (3) | 0.0011 (2) | 0.0088 (2) | −0.0015 (2) |
Br2 | 0.0293 (3) | 0.0199 (3) | 0.0354 (3) | 0.0011 (2) | 0.0057 (2) | 0.0046 (2) |
Br3 | 0.0291 (3) | 0.0235 (3) | 0.0224 (2) | −0.0031 (2) | 0.0075 (2) | −0.0009 (2) |
C1 | 0.023 (3) | 0.013 (2) | 0.024 (2) | 0.005 (2) | 0.005 (2) | −0.0007 (19) |
C2 | 0.019 (3) | 0.018 (3) | 0.023 (2) | 0.005 (2) | 0.003 (2) | −0.002 (2) |
C3 | 0.025 (3) | 0.020 (3) | 0.029 (3) | 0.005 (2) | 0.001 (2) | −0.009 (2) |
C4 | 0.032 (3) | 0.022 (3) | 0.026 (3) | 0.005 (2) | 0.007 (2) | −0.004 (2) |
C5 | 0.028 (3) | 0.022 (3) | 0.025 (3) | 0.006 (2) | 0.010 (2) | 0.003 (2) |
C6 | 0.020 (3) | 0.016 (3) | 0.026 (3) | 0.000 (2) | 0.007 (2) | −0.0019 (19) |
C7 | 0.022 (3) | 0.017 (2) | 0.024 (3) | 0.004 (2) | 0.009 (2) | 0.006 (2) |
C8 | 0.024 (3) | 0.022 (3) | 0.032 (3) | −0.006 (2) | 0.009 (2) | 0.002 (2) |
C9 | 0.027 (3) | 0.022 (3) | 0.034 (3) | −0.006 (2) | 0.007 (2) | −0.001 (2) |
C10 | 0.029 (3) | 0.024 (3) | 0.032 (3) | −0.007 (2) | 0.015 (2) | 0.000 (2) |
C11 | 0.020 (3) | 0.025 (3) | 0.032 (3) | −0.007 (2) | 0.005 (2) | −0.002 (2) |
C12 | 0.021 (3) | 0.017 (3) | 0.028 (3) | 0.002 (2) | −0.001 (2) | −0.004 (2) |
C13 | 0.036 (3) | 0.027 (3) | 0.036 (3) | −0.006 (3) | 0.008 (3) | −0.012 (2) |
C14 | 0.036 (4) | 0.039 (3) | 0.023 (3) | −0.006 (3) | −0.001 (2) | 0.002 (2) |
C15 | 0.040 (4) | 0.029 (3) | 0.034 (3) | −0.006 (3) | 0.014 (3) | 0.005 (2) |
C16 | 0.034 (4) | 0.029 (3) | 0.047 (3) | −0.003 (3) | 0.023 (3) | −0.005 (2) |
C17 | 0.044 (4) | 0.037 (3) | 0.022 (3) | 0.001 (3) | 0.003 (2) | −0.001 (2) |
N5 | 0.056 (4) | 0.042 (3) | 0.042 (3) | −0.001 (3) | 0.016 (3) | −0.009 (2) |
C18 | 0.035 (4) | 0.025 (3) | 0.037 (3) | 0.001 (3) | −0.001 (3) | 0.002 (2) |
C19 | 0.054 (4) | 0.041 (4) | 0.029 (3) | 0.004 (3) | 0.007 (3) | 0.001 (2) |
N6 | 0.065 (5) | 0.059 (4) | 0.087 (5) | 0.004 (4) | −0.003 (4) | −0.012 (3) |
C21 | 0.048 (5) | 0.037 (4) | 0.048 (4) | 0.004 (3) | 0.007 (3) | −0.005 (3) |
C20 | 0.062 (5) | 0.043 (4) | 0.044 (4) | 0.001 (3) | 0.010 (3) | −0.008 (3) |
O1W | 0.038 (2) | 0.027 (2) | 0.040 (2) | 0.0096 (18) | 0.0104 (18) | 0.0104 (16) |
O2W | 0.026 (2) | 0.0182 (18) | 0.0331 (19) | −0.0003 (15) | 0.0113 (16) | −0.0008 (14) |
O3W | 0.024 (2) | 0.0252 (18) | 0.0266 (18) | 0.0031 (16) | 0.0059 (15) | −0.0036 (14) |
O4W | 0.024 (2) | 0.0186 (17) | 0.0295 (18) | −0.0050 (15) | 0.0067 (15) | −0.0049 (14) |
Geometric parameters (Å, º) top
Ni1—N1 | 1.977 (3) | C9—H9B | 0.9900 |
Ni1—O1 | 2.039 (3) | C10—C11 | 1.509 (6) |
Ni1—N2 | 2.136 (4) | C10—H10A | 0.9900 |
Ni1—O2W | 2.140 (3) | C10—H10B | 0.9900 |
Ni1—Br3 | 2.5339 (7) | C11—H11A | 0.9900 |
Ni1—Br1 | 2.6720 (8) | C11—H11B | 0.9900 |
Ni1—Ni2 | 3.2346 (9) | C12—H12A | 0.9500 |
Ni2—N4 | 1.976 (4) | C13—H13A | 0.9800 |
Ni2—O1 | 2.055 (3) | C13—H13B | 0.9800 |
Ni2—O4W | 2.105 (3) | C13—H13C | 0.9800 |
Ni2—N3 | 2.147 (4) | C14—H14A | 0.9800 |
Ni2—O3W | 2.164 (3) | C14—H14B | 0.9800 |
Ni2—Br3 | 2.5181 (8) | C14—H14C | 0.9800 |
N1—C7 | 1.272 (5) | C15—H15A | 0.9800 |
N1—C8 | 1.463 (6) | C15—H15B | 0.9800 |
N2—C14 | 1.457 (6) | C15—H15C | 0.9800 |
N2—C13 | 1.479 (6) | C16—H16A | 0.9800 |
N2—C9 | 1.502 (5) | C16—H16B | 0.9800 |
N3—C16 | 1.477 (6) | C16—H16C | 0.9800 |
N3—C10 | 1.485 (6) | C17—H17A | 0.9800 |
N3—C15 | 1.488 (6) | C17—H17B | 0.9800 |
N4—C12 | 1.281 (5) | C17—H17C | 0.9800 |
N4—C11 | 1.466 (6) | N5—C18 | 1.131 (6) |
O1—C1 | 1.324 (5) | C18—C19 | 1.454 (7) |
C1—C2 | 1.424 (7) | C19—H19A | 0.9800 |
C1—C6 | 1.434 (6) | C19—H19B | 0.9800 |
C2—C3 | 1.398 (6) | C19—H19C | 0.9800 |
C2—C12 | 1.440 (6) | N6—C21 | 1.129 (8) |
C3—C4 | 1.382 (7) | C21—C20 | 1.436 (9) |
C3—H3A | 0.9500 | C20—H20A | 0.9800 |
C4—C5 | 1.374 (7) | C20—H20B | 0.9800 |
C4—C17 | 1.512 (6) | C20—H20C | 0.9800 |
C5—C6 | 1.394 (6) | O1W—H1WA | 0.8499 |
C5—H5A | 0.9500 | O1W—H1WB | 0.8501 |
C6—C7 | 1.464 (7) | O2W—H2WA | 0.8500 |
C7—H7A | 0.9500 | O2W—H2WB | 0.8500 |
C8—C9 | 1.516 (7) | O3W—H3WA | 0.8499 |
C8—H8A | 0.9900 | O3W—H3WB | 0.8499 |
C8—H8B | 0.9900 | O4W—H4WA | 0.8500 |
C9—H9A | 0.9900 | O4W—H4WB | 0.8499 |
| | | |
N1—Ni1—O1 | 92.14 (14) | N1—C7—H7A | 116.4 |
N1—Ni1—N2 | 84.28 (15) | C6—C7—H7A | 116.4 |
O1—Ni1—N2 | 176.42 (13) | N1—C8—C9 | 107.5 (4) |
N1—Ni1—O2W | 88.18 (13) | N1—C8—H8A | 110.2 |
O1—Ni1—O2W | 84.78 (12) | C9—C8—H8A | 110.2 |
N2—Ni1—O2W | 94.89 (14) | N1—C8—H8B | 110.2 |
N1—Ni1—Br3 | 173.56 (11) | C9—C8—H8B | 110.2 |
O1—Ni1—Br3 | 87.92 (8) | H8A—C8—H8B | 108.5 |
N2—Ni1—Br3 | 95.61 (10) | N2—C9—C8 | 110.6 (4) |
O2W—Ni1—Br3 | 85.41 (8) | N2—C9—H9A | 109.5 |
N1—Ni1—Br1 | 89.98 (11) | C8—C9—H9A | 109.5 |
O1—Ni1—Br1 | 87.77 (9) | N2—C9—H9B | 109.5 |
N2—Ni1—Br1 | 92.41 (11) | C8—C9—H9B | 109.5 |
O2W—Ni1—Br1 | 172.26 (9) | H9A—C9—H9B | 108.1 |
Br3—Ni1—Br1 | 96.45 (2) | N3—C10—C11 | 110.4 (4) |
N1—Ni1—Ni2 | 129.96 (12) | N3—C10—H10A | 109.6 |
O1—Ni1—Ni2 | 37.97 (8) | C11—C10—H10A | 109.6 |
N2—Ni1—Ni2 | 145.58 (10) | N3—C10—H10B | 109.6 |
O2W—Ni1—Ni2 | 84.27 (9) | C11—C10—H10B | 109.6 |
Br3—Ni1—Ni2 | 49.974 (19) | H10A—C10—H10B | 108.1 |
Br1—Ni1—Ni2 | 91.17 (2) | N4—C11—C10 | 108.1 (4) |
N4—Ni2—O1 | 90.72 (14) | N4—C11—H11A | 110.1 |
N4—Ni2—O4W | 90.51 (14) | C10—C11—H11A | 110.1 |
O1—Ni2—O4W | 88.77 (12) | N4—C11—H11B | 110.1 |
N4—Ni2—N3 | 83.91 (15) | C10—C11—H11B | 110.1 |
O1—Ni2—N3 | 174.27 (14) | H11A—C11—H11B | 108.4 |
O4W—Ni2—N3 | 89.28 (14) | N4—C12—C2 | 127.8 (5) |
N4—Ni2—O3W | 90.66 (14) | N4—C12—H12A | 116.1 |
O1—Ni2—O3W | 84.01 (12) | C2—C12—H12A | 116.1 |
O4W—Ni2—O3W | 172.71 (11) | N2—C13—H13A | 109.5 |
N3—Ni2—O3W | 98.01 (14) | N2—C13—H13B | 109.5 |
N4—Ni2—Br3 | 178.72 (11) | H13A—C13—H13B | 109.5 |
O1—Ni2—Br3 | 88.01 (9) | N2—C13—H13C | 109.5 |
O4W—Ni2—Br3 | 89.64 (9) | H13A—C13—H13C | 109.5 |
N3—Ni2—Br3 | 97.37 (11) | H13B—C13—H13C | 109.5 |
O3W—Ni2—Br3 | 89.03 (9) | N2—C14—H14A | 109.5 |
N4—Ni2—Ni1 | 128.33 (11) | N2—C14—H14B | 109.5 |
O1—Ni2—Ni1 | 37.63 (9) | H14A—C14—H14B | 109.5 |
O4W—Ni2—Ni1 | 87.74 (9) | N2—C14—H14C | 109.5 |
N3—Ni2—Ni1 | 147.63 (12) | H14A—C14—H14C | 109.5 |
O3W—Ni2—Ni1 | 85.88 (9) | H14B—C14—H14C | 109.5 |
Br3—Ni2—Ni1 | 50.403 (18) | N3—C15—H15A | 109.5 |
C7—N1—C8 | 121.1 (4) | N3—C15—H15B | 109.5 |
C7—N1—Ni1 | 125.5 (3) | H15A—C15—H15B | 109.5 |
C8—N1—Ni1 | 113.4 (3) | N3—C15—H15C | 109.5 |
C14—N2—C13 | 108.8 (4) | H15A—C15—H15C | 109.5 |
C14—N2—C9 | 108.9 (4) | H15B—C15—H15C | 109.5 |
C13—N2—C9 | 110.4 (4) | N3—C16—H16A | 109.5 |
C14—N2—Ni1 | 115.0 (3) | N3—C16—H16B | 109.5 |
C13—N2—Ni1 | 110.5 (3) | H16A—C16—H16B | 109.5 |
C9—N2—Ni1 | 103.1 (3) | N3—C16—H16C | 109.5 |
C16—N3—C10 | 110.4 (4) | H16A—C16—H16C | 109.5 |
C16—N3—C15 | 108.2 (4) | H16B—C16—H16C | 109.5 |
C10—N3—C15 | 108.5 (4) | C4—C17—H17A | 109.5 |
C16—N3—Ni2 | 112.8 (3) | C4—C17—H17B | 109.5 |
C10—N3—Ni2 | 102.8 (3) | H17A—C17—H17B | 109.5 |
C15—N3—Ni2 | 113.9 (3) | C4—C17—H17C | 109.5 |
C12—N4—C11 | 120.3 (4) | H17A—C17—H17C | 109.5 |
C12—N4—Ni2 | 126.6 (3) | H17B—C17—H17C | 109.5 |
C11—N4—Ni2 | 113.1 (3) | N5—C18—C19 | 178.5 (6) |
C1—O1—Ni1 | 127.6 (3) | C18—C19—H19A | 109.5 |
C1—O1—Ni2 | 127.9 (3) | C18—C19—H19B | 109.5 |
Ni1—O1—Ni2 | 104.40 (13) | H19A—C19—H19B | 109.5 |
Ni2—Br3—Ni1 | 79.62 (2) | C18—C19—H19C | 109.5 |
O1—C1—C2 | 122.3 (4) | H19A—C19—H19C | 109.5 |
O1—C1—C6 | 121.4 (4) | H19B—C19—H19C | 109.5 |
C2—C1—C6 | 116.4 (4) | N6—C21—C20 | 178.9 (8) |
C3—C2—C1 | 119.8 (4) | C21—C20—H20A | 109.5 |
C3—C2—C12 | 115.5 (4) | C21—C20—H20B | 109.5 |
C1—C2—C12 | 124.6 (4) | H20A—C20—H20B | 109.5 |
C4—C3—C2 | 123.9 (5) | C21—C20—H20C | 109.5 |
C4—C3—H3A | 118.1 | H20A—C20—H20C | 109.5 |
C2—C3—H3A | 118.1 | H20B—C20—H20C | 109.5 |
C5—C4—C3 | 116.0 (4) | H1WA—O1W—H1WB | 85.0 |
C5—C4—C17 | 122.1 (4) | Ni1—O2W—H2WA | 105.0 |
C3—C4—C17 | 121.8 (5) | Ni1—O2W—H2WB | 110.2 |
C4—C5—C6 | 123.8 (4) | H2WA—O2W—H2WB | 116.2 |
C4—C5—H5A | 118.1 | Ni2—O3W—H3WA | 123.3 |
C6—C5—H5A | 118.1 | Ni2—O3W—H3WB | 111.0 |
C5—C6—C1 | 120.0 (4) | H3WA—O3W—H3WB | 113.8 |
C5—C6—C7 | 114.4 (4) | Ni2—O4W—H4WA | 112.9 |
C1—C6—C7 | 125.5 (4) | Ni2—O4W—H4WB | 101.9 |
N1—C7—C6 | 127.2 (4) | H4WA—O4W—H4WB | 119.7 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···Br2i | 0.85 | 2.44 | 3.256 (3) | 162 |
O1W—H1WB···Br1i | 0.85 | 2.55 | 3.398 (3) | 173 |
O2W—H2WA···O3W | 0.85 | 2.07 | 2.868 (4) | 157 |
O2W—H2WB···O1W | 0.85 | 1.86 | 2.707 (4) | 172 |
O3W—H3WA···N5ii | 0.85 | 2.03 | 2.880 (5) | 180 |
O3W—H3WB···Br2ii | 0.85 | 2.42 | 3.270 (3) | 180 |
O4W—H4WA···Br2iii | 0.85 | 2.41 | 3.260 (3) | 180 |
O4W—H4WB···Br1 | 0.85 | 2.42 | 3.266 (3) | 180 |
Symmetry codes: (i) −x+3/2, y−1/2, −z+1/2; (ii) x+1, y, z; (iii) −x+3/2, y+1/2, −z+1/2. |