Poly[di-μ2-aqua-hexa­quabis(μ4-benzene-1,3,5-tricarboxyl­ato)trinickel(II)]

Liu, Y.-Y.; Ma, J.-F.; Ma, J.-C.

doi:10.1107/S1600536806032053

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Poly[di-μ₂-aqua-hexaquabis(μ₄-benzene-1,3,5-tricarboxylato)trinickel(II)]

Y.-Y. Liu, J.-F. Ma and J.-C. Ma

The solvothermal reaction of nickel^II acetate with H₃BTC (benzene-1,3,5-tricarboxylic acid) in water gave the title complex, [Ni₃(C₉H₃O₆)₂(H₂O)₈]_n. Single-crystal X-ray analysis shows that the structure contains four crystallographically unique Ni atoms. Two of these each lie at a center of symmetry and each is coordinated by two water molecules and four O atoms from four carboxylate groups. The other two are each coordinated by four water molecules and two O atoms from two carboxylate groups. The different types of chemically unique Ni atoms are connected by μ₂-H₂O and carboxylate groups of BTC ligands to form two two-dimensional networks. The hydrogen-bonding interactions between the layers further connected these two-dimensional layers into a three-dimensional frame work in a parallel fashion.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806032053/at2082sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806032053/at2082Isup2.hkl Contains datablock I

CCDC reference: 620537

checkCIF report

Key indicators

Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.003 Å
R factor = 0.027
wR factor = 0.085
Data-to-parameter ratio = 11.9

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving .   ?
PLAT420_ALERT_2_B D-H Without Acceptor       O6W    -   H6A    ...          ?

Alert level C
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.35 Ratio
PLAT731_ALERT_1_C Bond    Calc     0.90(4), Rep   0.896(17) ......       2.35 su-Ra
              O4W  -H4A     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(4), Rep   0.848(18) ......       2.22 su-Ra
              O6W  -H6B     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.90(4), Rep   0.896(17) ......       2.35 su-Ra
              O4W  -H4A     1.555   1.555
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.11 Ratio

Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K

   0 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
   5 ALERT level C = Check and explain
   2 ALERT level G = General alerts; check

   5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 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
   0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; 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.

Poly[di-µ₂-aqua-hexaquabis(µ₄-benzene-1,3,5-tricarboxylato)trinickel(II)] top

Crystal data top

[Ni₃(C₉H₃O₆)₂(H₂O)₈]	Z = 2
M_r = 734.49	F(000) = 748
Triclinic, P1	D_x = 2.173 Mg m⁻³
Hall symbol: -P 1	Melting point: not measured K
a = 10.040 (5) Å	Mo Kα radiation, λ = 0.71069 Å
b = 10.092 (5) Å	Cell parameters from 4601 reflections
c = 13.165 (5) Å	θ = 1.7–28.3°
α = 75.719 (5)°	µ = 2.60 mm⁻¹
β = 68.643 (5)°	T = 293 K
γ = 65.409 (5)°	Block, green
V = 1122.5 (9) Å³	0.38 × 0.28 × 0.16 mm

Data collection top

Bruker APEX CCD area-detector diffractometer	5008 independent reflections
Radiation source: fine-focus sealed tube	4047 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.013
ω scans	θ_max = 28.3°, θ_min = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −12→13
T_min = 0.42, T_max = 0.65	k = −11→12
6913 measured reflections	l = −17→11

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)] = 0.027	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.085	H atoms treated by a mixture of independent and constrained refinement
S = 1.09	w = 1/[σ²(F_o²) + (0.0477P)² + 0.3629P] where P = (F_o² + 2F_c²)/3
5008 reflections	(Δ/σ)_max = 0.001
421 parameters	Δρ_max = 0.44 e Å⁻³
16 restraints	Δρ_min = −0.57 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	U_iso*/U_eq
Ni1	0.0000	0.0000	0.0000	0.01262 (10)
Ni2	−0.5000	1.0000	−0.5000	0.01334 (10)
Ni3	−0.12592 (3)	0.23573 (3)	−0.22699 (2)	0.01497 (9)
Ni4	−0.34778 (3)	0.76820 (3)	−0.27960 (2)	0.01604 (9)
C1	−0.7044 (2)	0.2851 (2)	−0.09744 (18)	0.0148 (4)
H1	−0.6662	0.1833	−0.0850	0.018*
C2	−0.8471 (2)	0.3585 (2)	−0.11582 (18)	0.0135 (4)
C3	−0.9057 (2)	0.5105 (2)	−0.12997 (18)	0.0147 (4)
H3	−0.9995	0.5598	−0.1445	0.018*
C4	−0.8252 (2)	0.5903 (2)	−0.12266 (17)	0.0134 (4)
C5	−0.6809 (2)	0.5164 (2)	−0.10742 (18)	0.0149 (4)
H5	−0.6259	0.5690	−0.1037	0.018*
C6	−0.6188 (2)	0.3642 (2)	−0.09768 (18)	0.0149 (4)
C7	−0.4562 (2)	0.2809 (3)	−0.0960 (2)	0.0185 (5)
C8	−0.8964 (2)	0.7545 (2)	−0.13081 (19)	0.0159 (4)
C9	−0.9339 (2)	0.2700 (2)	−0.12070 (18)	0.0149 (4)
C10	0.3471 (2)	0.4112 (2)	−0.37873 (17)	0.0136 (4)
C11	0.4242 (2)	0.4911 (2)	−0.36759 (18)	0.0145 (4)
H11	0.5167	0.4424	−0.3512	0.017*
C12	0.3637 (2)	0.6440 (2)	−0.38081 (18)	0.0138 (4)
C13	0.2233 (2)	0.7161 (2)	−0.40248 (18)	0.0145 (4)
H13	0.1841	0.8180	−0.4138	0.017*
C14	0.1412 (2)	0.6367 (2)	−0.40726 (18)	0.0144 (4)
C15	0.2041 (2)	0.4846 (2)	−0.39715 (18)	0.0151 (4)
H15	0.1508	0.4315	−0.4027	0.018*
C16	0.4221 (2)	0.2475 (2)	−0.37572 (18)	0.0146 (4)
C17	0.4461 (2)	0.7333 (2)	−0.37048 (18)	0.0146 (4)
C18	−0.0188 (2)	0.7203 (2)	−0.41480 (19)	0.0164 (4)
O1	−1.00803 (19)	0.81491 (18)	−0.16946 (16)	0.0269 (4)
O2	−0.84308 (17)	0.82391 (17)	−0.09739 (15)	0.0215 (4)
O3	−0.42371 (18)	0.15599 (19)	−0.04360 (16)	0.0305 (4)
O4	−0.35895 (17)	0.34167 (17)	−0.15288 (14)	0.0217 (4)
O5	−0.88404 (17)	0.13550 (17)	−0.08873 (14)	0.0209 (4)
O6	−1.04856 (17)	0.33730 (17)	−0.15678 (14)	0.0199 (3)
O7	−0.04891 (17)	0.84302 (18)	−0.46889 (14)	0.0229 (4)
O8	−0.11833 (17)	0.66093 (17)	−0.35751 (16)	0.0250 (4)
O9	0.56637 (17)	0.66533 (17)	−0.34118 (14)	0.0192 (3)
O10	0.38693 (17)	0.87011 (17)	−0.39059 (14)	0.0200 (3)
O11	0.36478 (17)	0.18017 (17)	−0.40757 (14)	0.0193 (3)
O12	0.54126 (18)	0.18654 (18)	−0.34567 (15)	0.0243 (4)
O1W	0.0974 (2)	0.1182 (2)	−0.31043 (17)	0.0283 (4)
H1A	0.184 (3)	0.135 (3)	−0.347 (2)	0.042*
H1B	0.134 (3)	0.041 (3)	−0.272 (2)	0.042*
O2W	−0.1779 (2)	0.1367 (2)	−0.32182 (15)	0.0255 (4)
H2A	−0.114 (3)	0.125 (3)	−0.3801 (17)	0.038*
H2B	−0.262 (3)	0.177 (3)	−0.343 (3)	0.038*
O3W	−0.1384 (2)	0.40550 (19)	−0.35140 (15)	0.0235 (4)
H3A	−0.230 (2)	0.448 (3)	−0.363 (2)	0.035*
H3B	−0.126 (3)	0.473 (3)	−0.331 (3)	0.035*
O4W	−0.3321 (2)	0.5979 (2)	−0.15424 (15)	0.0274 (4)
H4A	−0.361 (4)	0.529 (3)	−0.163 (3)	0.041*
H4B	−0.243 (2)	0.551 (3)	−0.144 (3)	0.041*
O5W	−0.5614 (2)	0.8860 (2)	−0.18510 (16)	0.0325 (4)
H5A	−0.658 (2)	0.888 (4)	−0.173 (3)	0.049*
H5B	−0.575 (4)	0.883 (4)	−0.1152 (16)	0.049*
O6W	−0.2813 (2)	0.8676 (2)	−0.19621 (19)	0.0382 (5)
H6A	−0.327 (4)	0.952 (2)	−0.183 (3)	0.057*
H6B	−0.205 (3)	0.820 (4)	−0.172 (3)	0.057*
O7W	−0.13031 (17)	0.06607 (17)	−0.10456 (13)	0.0150 (3)
H7A	−0.228 (2)	0.084 (3)	−0.082 (2)	0.022*
H7B	−0.109 (3)	−0.024 (2)	−0.115 (2)	0.022*
O8W	−0.34808 (17)	0.93427 (17)	−0.40872 (14)	0.0166 (3)
H8A	−0.373 (3)	1.025 (2)	−0.393 (2)	0.025*
H8B	−0.250 (2)	0.917 (3)	−0.438 (2)	0.025*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.01258 (18)	0.0082 (2)	0.0192 (2)	−0.00326 (14)	−0.00809 (15)	−0.00076 (15)
Ni2	0.01264 (18)	0.0083 (2)	0.0211 (2)	−0.00285 (15)	−0.00839 (15)	−0.00160 (15)
Ni3	0.01459 (14)	0.01145 (16)	0.02125 (17)	−0.00442 (11)	−0.00908 (12)	−0.00061 (12)
Ni4	0.01594 (15)	0.01207 (16)	0.02310 (18)	−0.00463 (11)	−0.01029 (12)	−0.00090 (12)
C1	0.0143 (9)	0.0109 (10)	0.0184 (11)	−0.0040 (8)	−0.0052 (8)	−0.0010 (8)
C2	0.0133 (9)	0.0132 (11)	0.0154 (10)	−0.0057 (8)	−0.0051 (8)	−0.0010 (8)
C3	0.0127 (9)	0.0134 (11)	0.0192 (11)	−0.0038 (8)	−0.0065 (8)	−0.0029 (9)
C4	0.0136 (9)	0.0100 (10)	0.0154 (11)	−0.0026 (8)	−0.0046 (8)	−0.0019 (8)
C5	0.0141 (9)	0.0147 (11)	0.0185 (11)	−0.0063 (8)	−0.0055 (8)	−0.0030 (8)
C6	0.0126 (9)	0.0150 (11)	0.0177 (11)	−0.0038 (8)	−0.0071 (8)	−0.0010 (9)
C7	0.0157 (10)	0.0163 (12)	0.0260 (13)	−0.0052 (9)	−0.0098 (9)	−0.0024 (9)
C8	0.0167 (10)	0.0107 (11)	0.0197 (11)	−0.0031 (8)	−0.0060 (9)	−0.0030 (8)
C9	0.0142 (9)	0.0126 (11)	0.0192 (11)	−0.0055 (8)	−0.0055 (8)	−0.0021 (9)
C10	0.0146 (9)	0.0106 (10)	0.0159 (11)	−0.0036 (8)	−0.0055 (8)	−0.0020 (8)
C11	0.0131 (9)	0.0131 (11)	0.0179 (11)	−0.0030 (8)	−0.0072 (8)	−0.0019 (8)
C12	0.0146 (9)	0.0123 (11)	0.0178 (11)	−0.0069 (8)	−0.0064 (8)	−0.0015 (8)
C13	0.0142 (10)	0.0102 (10)	0.0190 (11)	−0.0026 (8)	−0.0068 (8)	−0.0018 (8)
C14	0.0120 (9)	0.0142 (11)	0.0171 (11)	−0.0043 (8)	−0.0044 (8)	−0.0026 (8)
C15	0.0138 (9)	0.0156 (11)	0.0184 (11)	−0.0060 (8)	−0.0058 (8)	−0.0029 (9)
C16	0.0137 (9)	0.0113 (11)	0.0182 (11)	−0.0032 (8)	−0.0050 (8)	−0.0021 (8)
C17	0.0136 (9)	0.0141 (11)	0.0173 (11)	−0.0052 (8)	−0.0053 (8)	−0.0021 (8)
C18	0.0134 (9)	0.0140 (11)	0.0231 (12)	−0.0029 (8)	−0.0078 (9)	−0.0044 (9)
O1	0.0270 (9)	0.0151 (9)	0.0450 (11)	0.0010 (7)	−0.0244 (8)	−0.0085 (8)
O2	0.0166 (7)	0.0136 (8)	0.0382 (10)	−0.0024 (6)	−0.0118 (7)	−0.0093 (7)
O3	0.0190 (8)	0.0200 (10)	0.0480 (12)	−0.0062 (7)	−0.0158 (8)	0.0111 (8)
O4	0.0126 (7)	0.0136 (8)	0.0356 (10)	−0.0039 (6)	−0.0071 (7)	0.0012 (7)
O5	0.0191 (8)	0.0119 (8)	0.0354 (10)	−0.0072 (6)	−0.0135 (7)	0.0025 (7)
O6	0.0193 (8)	0.0137 (8)	0.0322 (10)	−0.0048 (6)	−0.0155 (7)	−0.0017 (7)
O7	0.0161 (8)	0.0168 (9)	0.0314 (10)	−0.0039 (7)	−0.0091 (7)	0.0040 (7)
O8	0.0135 (7)	0.0130 (8)	0.0469 (11)	−0.0045 (6)	−0.0106 (7)	0.0014 (7)
O9	0.0187 (8)	0.0129 (8)	0.0312 (9)	−0.0047 (6)	−0.0147 (7)	−0.0017 (7)
O10	0.0185 (7)	0.0102 (8)	0.0341 (10)	−0.0064 (6)	−0.0112 (7)	0.0003 (7)
O11	0.0163 (7)	0.0121 (8)	0.0323 (10)	−0.0026 (6)	−0.0101 (7)	−0.0073 (7)
O12	0.0218 (8)	0.0137 (8)	0.0427 (11)	−0.0005 (7)	−0.0198 (8)	−0.0073 (7)
O1W	0.0211 (9)	0.0244 (10)	0.0363 (11)	−0.0057 (8)	−0.0069 (8)	−0.0050 (8)
O2W	0.0269 (9)	0.0301 (10)	0.0254 (10)	−0.0119 (8)	−0.0107 (7)	−0.0055 (8)
O3W	0.0313 (9)	0.0160 (9)	0.0259 (9)	−0.0098 (7)	−0.0122 (8)	0.0009 (7)
O4W	0.0382 (10)	0.0180 (9)	0.0287 (10)	−0.0099 (8)	−0.0157 (8)	0.0014 (7)
O5W	0.0246 (9)	0.0355 (11)	0.0331 (11)	−0.0071 (8)	−0.0031 (8)	−0.0117 (9)
O6W	0.0413 (12)	0.0284 (11)	0.0597 (15)	−0.0076 (9)	−0.0320 (11)	−0.0131 (10)
O7W	0.0148 (7)	0.0095 (8)	0.0225 (9)	−0.0030 (6)	−0.0100 (6)	−0.0005 (6)
O8W	0.0146 (7)	0.0105 (8)	0.0262 (9)	−0.0023 (6)	−0.0106 (7)	−0.0017 (6)

Geometric parameters (Å, º) top

Ni1—O5ⁱ	2.0338 (17)	C9—O6	1.265 (3)
Ni1—O5ⁱⁱ	2.034 (2)	C10—C11	1.391 (3)
Ni1—O7W	2.046 (2)	C10—C15	1.396 (3)
Ni1—O7Wⁱⁱⁱ	2.0455 (17)	C10—C16	1.501 (3)
Ni1—O2^iv	2.1464 (17)	C11—C12	1.394 (3)
Ni1—O2^v	2.146 (2)	C11—H11	0.9300
Ni2—O10^vi	2.049 (2)	C12—C13	1.391 (3)
Ni2—O10^vii	2.0488 (17)	C12—C17	1.509 (3)
Ni2—O8W	2.076 (2)	C13—C14	1.392 (3)
Ni2—O8W^viii	2.0761 (17)	C13—H13	0.9300
Ni2—O11^ix	2.113 (2)	C14—C15	1.388 (3)
Ni2—O11^x	2.1128 (17)	C14—C18	1.500 (3)
Ni3—O6ⁱⁱ	2.040 (2)	C15—H15	0.9300
Ni3—O7W	2.045 (2)	C16—O12	1.256 (3)
Ni3—O3W	2.054 (2)	C16—O11	1.269 (3)
Ni3—O1W	2.068 (2)	C17—O10	1.258 (3)
Ni3—O4	2.083 (2)	C17—O9	1.264 (3)
Ni3—O2W	2.087 (2)	C18—O7	1.242 (3)
Ni4—O9^vi	2.036 (2)	C18—O8	1.286 (3)
Ni4—O5W	2.056 (2)	O2—Ni1^ix	2.1464 (17)
Ni4—O4W	2.066 (2)	O5—Ni1^vi	2.0338 (17)
Ni4—O8	2.069 (2)	O6—Ni3^vi	2.0400 (16)
Ni4—O6W	2.072 (2)	O9—Ni4ⁱⁱ	2.0363 (16)
Ni4—O8W	2.072 (2)	O10—Ni2ⁱⁱ	2.0488 (17)
C1—C2	1.393 (3)	O11—Ni2^v	2.1128 (17)
C1—C6	1.394 (3)	O1W—H1A	0.888 (17)
C1—H1	0.9300	O1W—H1B	0.841 (18)
C2—C3	1.387 (3)	O2W—H2A	0.797 (17)
C2—C9	1.509 (3)	O2W—H2B	0.885 (17)
C3—C4	1.395 (3)	O3W—H3A	0.889 (17)
C3—H3	0.9300	O3W—H3B	0.860 (17)
C4—C5	1.391 (3)	O4W—H4A	0.896 (17)
C4—C8	1.500 (3)	O4W—H4B	0.861 (17)
C5—C6	1.389 (3)	O5W—H5A	0.917 (18)
C5—H5	0.9300	O5W—H5B	0.876 (17)
C6—C7	1.499 (3)	O6W—H6A	0.809 (18)
C7—O3	1.251 (3)	O6W—H6B	0.848 (18)
C7—O4	1.277 (3)	O7W—H7A	0.865 (16)
C8—O1	1.257 (3)	O7W—H7B	0.881 (17)
C8—O2	1.267 (3)	O8W—H8A	0.899 (17)
C9—O5	1.255 (3)	O8W—H8B	0.872 (16)

O5ⁱ—Ni1—O5ⁱⁱ	180.00 (8)	C5—C6—C7	121.81 (18)
O5ⁱ—Ni1—O7W	88.51 (7)	C1—C6—C7	118.1 (2)
O5ⁱⁱ—Ni1—O7W	91.49 (7)	O3—C7—O4	124.6 (2)
O5ⁱ—Ni1—O7Wⁱⁱⁱ	91.49 (7)	O3—C7—C6	118.69 (19)
O5ⁱⁱ—Ni1—O7Wⁱⁱⁱ	88.51 (7)	O4—C7—C6	116.6 (2)
O7W—Ni1—O7Wⁱⁱⁱ	180.00 (7)	O1—C8—O2	123.9 (2)
O5ⁱ—Ni1—O2^iv	92.59 (7)	O1—C8—C4	117.23 (19)
O5ⁱⁱ—Ni1—O2^iv	87.41 (7)	O2—C8—C4	118.86 (19)
O7W—Ni1—O2^iv	91.79 (7)	O5—C9—O6	126.32 (19)
O7Wⁱⁱⁱ—Ni1—O2^iv	88.21 (7)	O5—C9—C2	116.25 (19)
O5ⁱ—Ni1—O2^v	87.41 (7)	O6—C9—C2	117.43 (19)
O5ⁱⁱ—Ni1—O2^v	92.59 (7)	C11—C10—C15	119.6 (2)
O7W—Ni1—O2^v	88.21 (7)	C11—C10—C16	119.37 (19)
O7Wⁱⁱⁱ—Ni1—O2^v	91.79 (7)	C15—C10—C16	120.95 (18)
O2^iv—Ni1—O2^v	180.00 (9)	C10—C11—C12	120.41 (19)
O10^vi—Ni2—O10^vii	180.000 (1)	C10—C11—H11	119.8
O10^vi—Ni2—O8W	89.60 (7)	C12—C11—H11	119.8
O10^vii—Ni2—O8W	90.39 (7)	C13—C12—C11	119.44 (18)
O10^vi—Ni2—O8W^viii	90.40 (7)	C13—C12—C17	119.12 (19)
O10^vii—Ni2—O8W^viii	89.61 (7)	C11—C12—C17	121.43 (19)
O8W—Ni2—O8W^viii	180.000 (1)	C12—C13—C14	120.4 (2)
O10^vi—Ni2—O11^ix	92.26 (7)	C12—C13—H13	119.8
O10^vii—Ni2—O11^ix	87.74 (7)	C14—C13—H13	119.8
O8W—Ni2—O11^ix	88.23 (6)	C15—C14—C13	119.80 (19)
O8W^viii—Ni2—O11^ix	91.77 (6)	C15—C14—C18	122.23 (18)
O10^vi—Ni2—O11^x	87.74 (7)	C13—C14—C18	117.81 (19)
O10^vii—Ni2—O11^x	92.26 (7)	C14—C15—C10	120.15 (19)
O8W—Ni2—O11^x	91.77 (6)	C14—C15—H15	119.9
O8W^viii—Ni2—O11^x	88.23 (6)	C10—C15—H15	119.9
O11^ix—Ni2—O11^x	180.0	O12—C16—O11	124.2 (2)
O6ⁱⁱ—Ni3—O7W	95.69 (7)	O12—C16—C10	117.70 (18)
O6ⁱⁱ—Ni3—O3W	88.42 (8)	O11—C16—C10	118.03 (19)
O7W—Ni3—O3W	174.96 (6)	O10—C17—O9	125.66 (19)
O6ⁱⁱ—Ni3—O1W	90.27 (8)	O10—C17—C12	116.53 (19)
O7W—Ni3—O1W	91.20 (7)	O9—C17—C12	117.8 (2)
O3W—Ni3—O1W	91.70 (8)	O7—C18—O8	124.5 (2)
O6ⁱⁱ—Ni3—O4	96.66 (7)	O7—C18—C14	119.47 (19)
O7W—Ni3—O4	88.43 (6)	O8—C18—C14	115.9 (2)
O3W—Ni3—O4	88.19 (7)	C8—O2—Ni1^ix	118.88 (14)
O1W—Ni3—O4	173.06 (7)	C7—O4—Ni3	126.64 (15)
O6ⁱⁱ—Ni3—O2W	170.81 (7)	C9—O5—Ni1^vi	129.92 (14)
O7W—Ni3—O2W	90.59 (8)	C9—O6—Ni3^vi	122.71 (14)
O3W—Ni3—O2W	85.68 (8)	C18—O8—Ni4	126.83 (15)
O1W—Ni3—O2W	82.87 (8)	C17—O9—Ni4ⁱⁱ	121.83 (14)
O4—Ni3—O2W	90.21 (7)	C17—O10—Ni2ⁱⁱ	124.83 (14)
O9^vi—Ni4—O5W	92.83 (8)	C16—O11—Ni2^v	122.86 (14)
O9^vi—Ni4—O4W	87.07 (8)	Ni3—O1W—H1A	138 (2)
O5W—Ni4—O4W	89.68 (8)	Ni3—O1W—H1B	111 (2)
O9^vi—Ni4—O8	97.04 (7)	H1A—O1W—H1B	98 (3)
O5W—Ni4—O8	169.79 (8)	Ni3—O2W—H2A	111 (2)
O4W—Ni4—O8	88.23 (8)	Ni3—O2W—H2B	123 (2)
O9^vi—Ni4—O6W	172.08 (8)	H2A—O2W—H2B	100 (3)
O5W—Ni4—O6W	81.41 (9)	Ni3—O3W—H3A	114 (2)
O4W—Ni4—O6W	87.47 (9)	Ni3—O3W—H3B	107 (2)
O8—Ni4—O6W	88.52 (8)	H3A—O3W—H3B	105 (3)
O9^vi—Ni4—O8W	94.41 (7)	Ni4—O4W—H4A	112 (2)
O5W—Ni4—O8W	93.66 (8)	Ni4—O4W—H4B	117 (2)
O4W—Ni4—O8W	176.27 (7)	H4A—O4W—H4B	105 (3)
O8—Ni4—O8W	88.19 (7)	Ni4—O5W—H5A	134 (2)
O6W—Ni4—O8W	91.38 (8)	Ni4—O5W—H5B	118 (2)
C2—C1—C6	120.1 (2)	H5A—O5W—H5B	93 (3)
C2—C1—H1	120.0	Ni4—O6W—H6A	123 (2)
C6—C1—H1	120.0	Ni4—O6W—H6B	121 (2)
C3—C2—C1	119.47 (19)	H6A—O6W—H6B	116 (3)
C3—C2—C9	121.54 (19)	Ni3—O7W—Ni1	123.07 (7)
C1—C2—C9	118.99 (19)	Ni3—O7W—H7A	98.7 (19)
C2—C3—C4	120.7 (2)	Ni1—O7W—H7A	123.2 (18)
C2—C3—H3	119.7	Ni3—O7W—H7B	124.4 (18)
C4—C3—H3	119.7	Ni1—O7W—H7B	93.3 (18)
C5—C4—C3	119.5 (2)	H7A—O7W—H7B	92 (2)
C5—C4—C8	121.14 (18)	Ni4—O8W—Ni2	121.78 (7)
C3—C4—C8	119.37 (19)	Ni4—O8W—H8A	117.8 (18)
C6—C5—C4	120.14 (19)	Ni2—O8W—H8A	94.4 (18)
C6—C5—H5	119.9	Ni4—O8W—H8B	101.0 (19)
C4—C5—H5	119.9	Ni2—O8W—H8B	123.7 (18)
C5—C6—C1	119.94 (19)	H8A—O8W—H8B	96 (2)

C6—C1—C2—C3	−2.5 (3)	C13—C14—C18—O7	36.0 (3)
C6—C1—C2—C9	177.0 (2)	C15—C14—C18—O8	35.5 (3)
C1—C2—C3—C4	−2.0 (3)	C13—C14—C18—O8	−139.8 (2)
C9—C2—C3—C4	178.5 (2)	O1—C8—O2—Ni1^ix	43.0 (3)
C2—C3—C4—C5	3.8 (3)	C4—C8—O2—Ni1^ix	−135.87 (16)
C2—C3—C4—C8	−175.9 (2)	O3—C7—O4—Ni3	26.4 (3)
C3—C4—C5—C6	−1.1 (3)	C6—C7—O4—Ni3	−150.61 (15)
C8—C4—C5—C6	178.6 (2)	O6ⁱⁱ—Ni3—O4—C7	−125.21 (19)
C4—C5—C6—C1	−3.4 (3)	O7W—Ni3—O4—C7	−29.67 (19)
C4—C5—C6—C7	171.8 (2)	O3W—Ni3—O4—C7	146.6 (2)
C2—C1—C6—C5	5.2 (3)	O2W—Ni3—O4—C7	60.9 (2)
C2—C1—C6—C7	−170.2 (2)	O6—C9—O5—Ni1^vi	−39.5 (3)
C5—C6—C7—O3	150.2 (2)	C2—C9—O5—Ni1^vi	140.92 (16)
C1—C6—C7—O3	−34.5 (3)	O5—C9—O6—Ni3^vi	−25.0 (3)
C5—C6—C7—O4	−32.6 (3)	C2—C9—O6—Ni3^vi	154.59 (15)
C1—C6—C7—O4	142.7 (2)	O7—C18—O8—Ni4	−30.2 (3)
C5—C4—C8—O1	163.8 (2)	C14—C18—O8—Ni4	145.34 (16)
C3—C4—C8—O1	−16.5 (3)	O9^vi—Ni4—O8—C18	129.1 (2)
C5—C4—C8—O2	−17.2 (3)	O5W—Ni4—O8—C18	−65.8 (5)
C3—C4—C8—O2	162.5 (2)	O4W—Ni4—O8—C18	−144.1 (2)
C3—C2—C9—O5	−168.3 (2)	O6W—Ni4—O8—C18	−56.6 (2)
C1—C2—C9—O5	12.1 (3)	O8W—Ni4—O8—C18	34.9 (2)
C3—C2—C9—O6	12.0 (3)	O10—C17—O9—Ni4ⁱⁱ	17.8 (3)
C1—C2—C9—O6	−167.5 (2)	C12—C17—O9—Ni4ⁱⁱ	−161.11 (14)
C15—C10—C11—C12	−3.6 (3)	O9—C17—O10—Ni2ⁱⁱ	54.3 (3)
C16—C10—C11—C12	173.7 (2)	C12—C17—O10—Ni2ⁱⁱ	−126.75 (17)
C10—C11—C12—C13	1.7 (3)	O12—C16—O11—Ni2^v	−36.1 (3)
C10—C11—C12—C17	−179.3 (2)	C10—C16—O11—Ni2^v	141.14 (16)
C11—C12—C13—C14	2.2 (3)	O6ⁱⁱ—Ni3—O7W—Ni1	−23.16 (10)
C17—C12—C13—C14	−176.9 (2)	O1W—Ni3—O7W—Ni1	67.23 (10)
C12—C13—C14—C15	−4.0 (3)	O4—Ni3—O7W—Ni1	−119.70 (10)
C12—C13—C14—C18	171.4 (2)	O2W—Ni3—O7W—Ni1	150.11 (9)
C13—C14—C15—C10	2.0 (3)	O5ⁱ—Ni1—O7W—Ni3	172.01 (9)
C18—C14—C15—C10	−173.2 (2)	O5ⁱⁱ—Ni1—O7W—Ni3	−7.99 (9)
C11—C10—C15—C14	1.7 (3)	O2^iv—Ni1—O7W—Ni3	79.47 (10)
C16—C10—C15—C14	−175.5 (2)	O2^v—Ni1—O7W—Ni3	−100.53 (10)
C11—C10—C16—O12	11.2 (3)	O9^vi—Ni4—O8W—Ni2	26.92 (9)
C15—C10—C16—O12	−171.5 (2)	O5W—Ni4—O8W—Ni2	−66.20 (10)
C11—C10—C16—O11	−166.2 (2)	O8—Ni4—O8W—Ni2	123.84 (10)
C15—C10—C16—O11	11.1 (3)	O6W—Ni4—O8W—Ni2	−147.68 (10)
C13—C12—C17—O10	−5.2 (3)	O10^vi—Ni2—O8W—Ni4	8.34 (9)
C11—C12—C17—O10	175.7 (2)	O10^vii—Ni2—O8W—Ni4	−171.66 (9)
C13—C12—C17—O9	173.8 (2)	O11^ix—Ni2—O8W—Ni4	100.61 (10)
C11—C12—C17—O9	−5.3 (3)	O11^x—Ni2—O8W—Ni4	−79.39 (10)
C15—C14—C18—O7	−148.6 (2)

Symmetry codes: (i) −x−1, −y, −z; (ii) x+1, y, z; (iii) −x, −y, −z; (iv) −x−1, −y+1, −z; (v) x+1, y−1, z; (vi) x−1, y, z; (vii) −x, −y+2, −z−1; (viii) −x−1, −y+2, −z−1; (ix) x−1, y+1, z; (x) −x, −y+1, −z−1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O2W—H2A···O7^x	0.80 (2)	2.12 (2)	2.891 (3)	163 (3)
O5W—H5B···O3^iv	0.88 (2)	2.03 (2)	2.892 (3)	170 (3)
O1W—H1A···O11	0.89 (2)	1.90 (2)	2.781 (3)	172 (3)
O3W—H3B···O8	0.86 (2)	1.87 (2)	2.648 (3)	150 (3)
O4W—H4A···O4	0.90 (2)	1.86 (2)	2.705 (3)	157 (3)
O5W—H5A···O2	0.92 (2)	2.05 (2)	2.909 (3)	156 (3)
O7W—H7A···O3	0.87 (2)	1.71 (2)	2.561 (3)	168 (3)
O8W—H8B···O7	0.87 (2)	1.76 (2)	2.612 (3)	165 (3)

Symmetry codes: (iv) −x−1, −y+1, −z; (x) −x, −y+1, −z−1.

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