Investigation of the structure and phase transitions of the polymeric inorganic–organic hybrids: [M(Im)₄V₂O₆]_∞; M = Mn, Co, Ni, Im = imidazole

The polymeric isomorphous hybrid inorganic–organic vanadium oxide compounds [M(Im)₄V₂O₆]_∞, M = Mn, Co, Ni, Im = imidazole, were investigated at various temperatures between 100 and 295 K by single-crystal X-ray diffraction. The crystals all contain two-dimensional polymeric sheets packed perpendicular to c* and are 1:1 disordered in the space group P4₂/n (Z = 8) at 295 K. The disordered phase is reversibly transformed to an I4₁/a ordered phase (Z = 32) below 281 K for the Mn compound and below 175 K for the Co compound. Within a localized region of the I4₁/a phase eight imidazoles are in close proximity and seven of these are hydrogen bonded to framework O atoms. The hydrogen-bond connectivity of six of these ligands is unchanged by the phase transition that allows an inversion of the local geometry using an inversion operator that is a symmetry element of P4₂/n, but not I4₁/a. The Mn structure has a well defined phase transition but the Co structure shows a large hysteresis and it was necessary to include stacking faults in the modelling of the Co structure at low temperatures. The Ni structure was shown to be partially twinned, but ordered in the space group P2/n (Z = 8) at 100 K, with two different localized regions each containing four pairs of inversion-related imidazoles, hydrogen bonding to framework O atoms involving eight imidazoles in one region and six imidazoles in the other. Models for the phase transition mechanisms are considered.

Computing details

Data collection: Collect (Nonius BV, 1997-2000) for Mn_100K. Cell refinement: HKL SCALEPACK (Otwinowski & Minor 1997) for Mn_100K. Data reduction: DENZO and Scalepak (Otwinowski & Minor, 1997) for Mn_100K. Program(s) used to solve structure: SIR97 (Altomare, et al., 1999) for Mn_100K. Program(s) used to refine structure: RAELS06 (Rae, 2006) for Mn_100K. Molecular graphics: ORTEP (Burnett & Johnson, 1996) and Diamond V.3e (Brandenburg & Putz, 2006) for Mn_100K. Software used to prepare material for publication: RAELS06 (Rae, 2006) for Mn_100K.

catena-tetrakis(imidazole)-tetrakis(µ₂-oxo)-dioxo-manganese(ii)-di-vanadium (Mn_100K)

Crystal data

[Mn(C3H4N2)4V2O6]	Dx = 1.777 Mg m^−3
Mr = 525.13	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I41/a	Cell parameters from 65033 reflections
Hall symbol: -I 4ad	θ = 2.6–30.0°
a = 23.0354 (3) Å	µ = 1.61 mm^−1
c = 29.6005 (3) Å	T = 100 K
V = 15706.9 (3) Å^3	Hexagonal, orange-yellow
Z = 32	0.16 × 0.14 × 0.09 mm
F(000) = 8416.0

Data collection

Enraf-Nonius KappaCCD diffractometer	11464 independent reflections
Radiation source: fine-focus sealed tube	8019 reflections with I > 3σ(I)
Graphite monochromator	Rint = 0.058
φ scan plus ω scans with κ offsets	θmax = 30.0°, θmin = 2.6°
Absorption correction: multi-scan from symmetry-related measurements Sortav (Blessing 1995)	h = −31→32
Tmin = 0.684, Tmax = 0.767	k = −32→32
106159 measured reflections	l = −30→41

Refinement

Refinement on F	2 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.032	w = 1/[σ(F)^2 + (0.0004F)^2]
wR(F^2) = 0.046	(Δ/σ)max = 0.2
S = 1.47	Δρmax = 1.22 e Å^−3
8019 reflections	Δρmin = −0.98 e Å^−3
317 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mn1	0.74976 (1)	0.49552 (1)	0.45239 (1)	0.0105 (1)
Mn2	1.00000	0.25000	0.48952 (1)	0.0103 (1)
Mn3	0.50000	0.75000	0.48437 (1)	0.0104 (1)
V1	0.91179 (1)	0.51383 (1)	0.44988 (1)	0.0104 (1)
V2	0.98615 (1)	0.41145 (1)	0.49604 (1)	0.0105 (1)
V3	0.58420 (1)	0.48318 (1)	0.44659 (1)	0.0097 (1)
V4	0.51523 (1)	0.59016 (1)	0.49447 (1)	0.0100 (1)
O1	0.84265 (6)	0.50075 (6)	0.46053 (5)	0.0173 (3)
O2	0.94324 (6)	0.55721 (6)	0.49399 (4)	0.0159 (3)
O3	0.91703 (6)	0.54609 (6)	0.40076 (5)	0.0214 (3)
O4	0.99463 (6)	0.34219 (6)	0.48446 (5)	0.0167 (3)
O5	0.95193 (6)	0.44582 (6)	0.44783 (4)	0.0155 (3)
O6	0.94443 (6)	0.41840 (6)	0.54051 (5)	0.0194 (3)
O7	0.65431 (6)	0.49087 (6)	0.45420 (5)	0.0184 (3)
O8	0.55494 (6)	0.43992 (6)	0.49165 (4)	0.0149 (3)
O9	0.57402 (6)	0.45383 (6)	0.39635 (4)	0.0201 (3)
O10	0.50722 (6)	0.65821 (6)	0.47931 (5)	0.0172 (3)
O11	0.54778 (6)	0.55278 (6)	0.44683 (4)	0.0156 (3)
O12	0.55690 (6)	0.58685 (6)	0.53904 (4)	0.0191 (3)
N11	0.76200 (6)	0.43004 (5)	0.39626 (4)	0.0157 (4)
N12	0.74085 (6)	0.36262 (5)	0.34601 (4)	0.0201 (4)
C11	0.72271 (5)	0.39205 (6)	0.38272 (4)	0.0175 (4)
C12	0.79489 (6)	0.38262 (6)	0.33515 (4)	0.0202 (5)
C13	0.80755 (5)	0.42414 (6)	0.36628 (5)	0.0177 (4)
N21A	0.74371 (5)	0.41635 (5)	0.49720 (4)	0.0176 (4)	0.524 (9)
N22A	0.7096 (2)	0.33279 (7)	0.52206 (8)	0.0337 (6)	0.524 (9)
C21A	0.69777 (9)	0.38213 (10)	0.49943 (7)	0.0222 (4)	0.524 (9)
C22A	0.7664 (2)	0.33514 (11)	0.53522 (7)	0.0541 (6)	0.524 (9)
C23A	0.78705 (10)	0.38675 (13)	0.51976 (6)	0.0466 (5)	0.524 (9)
N21B	0.74371 (5)	0.41635 (5)	0.49720 (4)	0.0176 (4)	0.476
N22B	0.7753 (2)	0.34040 (12)	0.53532 (7)	0.0578 (7)	0.476
C21B	0.78875 (10)	0.39268 (13)	0.51782 (6)	0.0456 (5)	0.476
C22B	0.7184 (2)	0.32956 (7)	0.52551 (9)	0.0360 (6)	0.476
C23B	0.69929 (11)	0.37657 (11)	0.50203 (7)	0.0229 (4)	0.476
N31	0.92398 (5)	0.24790 (5)	0.44109 (4)	0.0146 (4)
N32	0.86053 (6)	0.22813 (6)	0.38748 (4)	0.0220 (4)
C31	0.91146 (6)	0.21348 (5)	0.40674 (4)	0.0175 (4)
C32	0.83883 (5)	0.27460 (6)	0.41061 (5)	0.0230 (5)
C33	0.87820 (6)	0.28648 (6)	0.44357 (5)	0.0184 (4)
N41	0.93337 (5)	0.24332 (6)	0.54494 (4)	0.0164 (3)
N42	0.87615 (6)	0.26758 (6)	0.60160 (4)	0.0217 (3)
C41	0.92001 (6)	0.28427 (5)	0.57442 (5)	0.0201 (3)
C42	0.86021 (6)	0.21281 (6)	0.58905 (5)	0.0243 (4)
C43	0.89569 (7)	0.19822 (5)	0.55413 (5)	0.0234 (3)
N51	0.74082 (6)	0.56070 (6)	0.39564 (4)	0.0155 (4)
N52	0.76173 (6)	0.61641 (6)	0.33729 (4)	0.0261 (4)
C51	0.78296 (5)	0.58366 (7)	0.37119 (5)	0.0262 (4)
C52	0.70257 (6)	0.61459 (7)	0.33991 (5)	0.0224 (5)
C53	0.69009 (5)	0.58018 (7)	0.37595 (5)	0.0227 (4)
N61	0.74517 (6)	0.56789 (5)	0.50157 (4)	0.0169 (4)
N62	0.73000 (7)	0.62031 (6)	0.56278 (4)	0.0250 (5)
C61	0.72668 (7)	0.56723 (6)	0.54383 (5)	0.0243 (5)
C62	0.75183 (8)	0.65743 (5)	0.53107 (5)	0.0332 (6)
C63	0.76104 (8)	0.62476 (6)	0.49348 (5)	0.0334 (7)
N71	0.57519 (5)	0.75269 (6)	0.43552 (4)	0.0149 (4)
N72	0.63613 (6)	0.77861 (6)	0.38173 (4)	0.0216 (4)
C71	0.58585 (6)	0.79056 (5)	0.40304 (4)	0.0180 (4)
C72	0.65936 (6)	0.73032 (7)	0.40148 (5)	0.0239 (5)
C73	0.62153 (6)	0.71467 (6)	0.43458 (5)	0.0205 (4)
N81	0.56574 (5)	0.75928 (6)	0.53993 (4)	0.0159 (4)
N82	0.63099 (5)	0.74168 (6)	0.59269 (4)	0.0192 (4)
C81	0.60626 (6)	0.72298 (5)	0.55409 (4)	0.0189 (4)
C82	0.60507 (6)	0.79291 (6)	0.60419 (4)	0.0195 (4)
C83	0.56495 (6)	0.80341 (5)	0.57150 (5)	0.0189 (4)
H1N12	0.72185	0.33604	0.33196	0.023
H1C11	0.68704	0.38635	0.39675	0.018
H1C12	0.81822	0.37037	0.31135	0.023
H1C13	0.84184	0.44543	0.36724	0.019
H1N22A	0.68579	0.30486	0.52727	0.042	0.524
H1C21A	0.66178	0.39099	0.48697	0.034	0.524
H1C22A	0.78678	0.30718	0.55142	0.085	0.524
H1C23A	0.82478	0.40015	0.52379	0.075	0.524
H1N22B	0.79834	0.31792	0.55001	0.090	0.476
H1C21B	0.82515	0.40994	0.51998	0.071	0.476
H1C22B	0.69705	0.29677	0.53329	0.045	0.476
H1C23B	0.66184	0.38125	0.49086	0.034	0.476
H1N32	0.84457	0.21126	0.36473	0.026
H1C31	0.93484	0.18300	0.39707	0.019
H1C32	0.80424	0.29412	0.40499	0.028
H1C33	0.87480	0.31620	0.46467	0.020
H1N42	0.86095	0.28777	0.62298	0.026
H1C41	0.93852	0.32007	0.57619	0.027
H1C42	0.83107	0.19014	0.60177	0.032
H1C43	0.89471	0.16306	0.53871	0.033
H1N52	0.78180	0.63509	0.31757	0.037
H1C51	0.82230	0.57794	0.37668	0.043
H1C52	0.67623	0.63309	0.32094	0.030
H1C53	0.65287	0.57110	0.38587	0.038
H1N62	0.72015	0.62920	0.58993	0.032
H1C61	0.71311	0.53430	0.55861	0.042
H1C62	0.75894	0.69692	0.53448	0.050
H1C63	0.77585	0.63867	0.46633	0.057
H1N72	0.65093	0.79789	0.35968	0.026
H1C71	0.56170	0.82155	0.39580	0.021
H1C72	0.69394	0.71193	0.39386	0.031
H1C73	0.62617	0.68302	0.45375	0.025
H1N82	0.65817	0.72446	0.60742	0.022
H1C81	0.61643	0.68885	0.53929	0.024
H1C82	0.61320	0.81590	0.62923	0.023
H1C83	0.54057	0.83556	0.57054	0.024

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mn1	0.0099 (1)	0.0118 (2)	0.0097 (2)	−0.0009 (1)	0.0007 (1)	−0.0003 (1)
Mn2	0.0112 (2)	0.0095 (2)	0.0101 (2)	0.0007 (2)	0.0000 (1)	0.0000 (1)
Mn3	0.0118 (2)	0.0096 (2)	0.0096 (2)	0.0011 (2)	0.0000 (1)	0.0000 (1)
V1	0.0094 (2)	0.0102 (2)	0.0117 (2)	0.0000 (1)	−0.0007 (1)	−0.0007 (1)
V2	0.0105 (2)	0.0088 (2)	0.0122 (2)	0.0001 (1)	0.0002 (1)	−0.0016 (1)
V3	0.0096 (2)	0.0102 (2)	0.0094 (2)	−0.0001 (1)	0.0017 (1)	−0.0002 (1)
V4	0.0111 (2)	0.0090 (2)	0.0099 (2)	0.0006 (1)	0.0009 (1)	0.0011 (1)
O1	0.0113 (7)	0.0196 (8)	0.0209 (8)	−0.0018 (6)	−0.0004 (6)	−0.0043 (6)
O2	0.0134 (7)	0.0157 (7)	0.0185 (7)	−0.0017 (6)	−0.0005 (5)	−0.0050 (5)
O3	0.0231 (8)	0.0215 (8)	0.0196 (8)	−0.0025 (6)	−0.0029 (6)	0.0057 (6)
O4	0.0170 (7)	0.0108 (7)	0.0222 (8)	0.0012 (6)	−0.0028 (6)	−0.0023 (6)
O5	0.0177 (7)	0.0145 (7)	0.0144 (7)	0.0027 (6)	−0.0021 (5)	−0.0023 (5)
O6	0.0212 (8)	0.0185 (8)	0.0185 (7)	0.0022 (6)	0.0067 (6)	−0.0003 (6)
O7	0.0120 (7)	0.0186 (8)	0.0245 (8)	−0.0004 (6)	0.0014 (6)	0.0041 (6)
O8	0.0140 (7)	0.0173 (7)	0.0135 (7)	−0.0010 (6)	0.0024 (5)	0.0026 (5)
O9	0.0264 (8)	0.0203 (8)	0.0135 (7)	−0.0070 (6)	0.0040 (6)	−0.0039 (6)
O10	0.0213 (8)	0.0117 (7)	0.0186 (7)	0.0025 (6)	0.0034 (6)	0.0031 (5)
O11	0.0194 (8)	0.0142 (7)	0.0133 (7)	0.0042 (6)	0.0033 (5)	0.0017 (5)
O12	0.0199 (8)	0.0214 (8)	0.0160 (7)	0.0010 (6)	−0.0044 (6)	0.0003 (6)
N11	0.0154 (6)	0.0162 (5)	0.0154 (5)	−0.0013 (4)	0.0004 (4)	−0.0019 (4)
N12	0.0250 (7)	0.0178 (5)	0.0175 (5)	−0.0003 (5)	−0.0021 (5)	−0.0038 (4)
C11	0.0189 (5)	0.0166 (5)	0.0171 (5)	−0.0023 (4)	−0.0013 (4)	−0.0026 (4)
C12	0.0242 (7)	0.0200 (6)	0.0164 (5)	0.0026 (5)	0.0008 (4)	−0.0032 (4)
C13	0.0179 (6)	0.0191 (6)	0.0160 (5)	0.0008 (4)	0.0019 (4)	−0.0021 (4)
N21A	0.0208 (6)	0.0209 (6)	0.0111 (6)	0.0004 (5)	0.0000 (5)	0.0031 (4)
N22A	0.0374 (10)	0.0261 (6)	0.0376 (9)	−0.0015 (6)	0.0055 (7)	0.0143 (5)
C21A	0.0260 (6)	0.0219 (6)	0.0187 (7)	−0.0033 (5)	0.0016 (5)	0.0043 (5)
C22A	0.0369 (10)	0.0486 (8)	0.0770 (12)	0.0023 (7)	−0.0014 (9)	0.0457 (8)
C23A	0.0283 (7)	0.0495 (8)	0.0619 (10)	−0.0031 (6)	−0.0108 (7)	0.0403 (8)
N21B	0.0208 (6)	0.0209 (6)	0.0111 (6)	0.0004 (5)	0.0000 (5)	0.0031 (4)
N22B	0.0361 (10)	0.0537 (8)	0.0836 (12)	0.0014 (8)	−0.0044 (9)	0.0515 (9)
C21B	0.0277 (7)	0.0492 (8)	0.0598 (10)	−0.0038 (6)	−0.0116 (7)	0.0392 (8)
C22B	0.0379 (11)	0.0279 (6)	0.0423 (9)	−0.0001 (5)	0.0059 (7)	0.0177 (6)
C23B	0.0270 (6)	0.0220 (6)	0.0198 (7)	−0.0031 (5)	0.0020 (5)	0.0048 (5)
N31	0.0160 (5)	0.0132 (6)	0.0145 (5)	0.0008 (4)	0.0000 (4)	−0.0009 (4)
N32	0.0224 (6)	0.0255 (7)	0.0181 (5)	−0.0073 (5)	−0.0048 (4)	0.0048 (4)
C31	0.0209 (5)	0.0176 (6)	0.0140 (5)	−0.0038 (4)	−0.0012 (4)	−0.0008 (4)
C32	0.0180 (5)	0.0255 (8)	0.0255 (7)	−0.0014 (4)	−0.0047 (4)	0.0075 (5)
C33	0.0159 (5)	0.0174 (6)	0.0219 (6)	0.0028 (4)	−0.0011 (4)	0.0023 (4)
N41	0.0172 (6)	0.0170 (6)	0.0151 (5)	−0.0008 (4)	0.0015 (4)	−0.0007 (4)
N42	0.0226 (6)	0.0238 (7)	0.0187 (5)	0.0007 (5)	0.0059 (5)	−0.0007 (4)
C41	0.0229 (6)	0.0193 (6)	0.0181 (6)	−0.0006 (5)	0.0054 (5)	−0.0023 (4)
C42	0.0239 (6)	0.0271 (7)	0.0219 (6)	−0.0051 (5)	0.0079 (5)	−0.0018 (5)
C43	0.0253 (7)	0.0227 (6)	0.0223 (6)	−0.0071 (5)	0.0083 (5)	−0.0036 (5)
N51	0.0164 (6)	0.0156 (6)	0.0143 (5)	−0.0019 (5)	0.0010 (4)	−0.0003 (4)
N52	0.0268 (6)	0.0287 (7)	0.0226 (6)	−0.0038 (6)	0.0012 (5)	0.0102 (5)
C51	0.0199 (5)	0.0331 (7)	0.0257 (6)	−0.0049 (5)	0.0014 (5)	0.0134 (6)
C52	0.0263 (6)	0.0222 (7)	0.0188 (6)	0.0005 (6)	−0.0010 (5)	0.0043 (5)
C53	0.0193 (5)	0.0271 (7)	0.0217 (6)	0.0016 (6)	0.0004 (5)	0.0075 (5)
N61	0.0166 (7)	0.0172 (5)	0.0169 (5)	−0.0026 (5)	0.0020 (5)	−0.0018 (4)
N62	0.0270 (8)	0.0259 (6)	0.0220 (5)	0.0013 (5)	0.0009 (5)	−0.0084 (5)
C61	0.0292 (9)	0.0245 (5)	0.0193 (6)	−0.0055 (5)	0.0078 (5)	−0.0057 (4)
C62	0.0552 (12)	0.0194 (5)	0.0250 (7)	−0.0022 (5)	−0.0005 (7)	−0.0062 (5)
C63	0.0601 (12)	0.0174 (6)	0.0228 (6)	−0.0096 (5)	0.0065 (6)	−0.0034 (4)
N71	0.0164 (5)	0.0154 (6)	0.0129 (5)	0.0013 (4)	0.0001 (4)	0.0005 (4)
N72	0.0227 (6)	0.0261 (7)	0.0160 (5)	−0.0059 (5)	0.0045 (4)	−0.0036 (4)
C71	0.0217 (5)	0.0189 (6)	0.0134 (6)	−0.0021 (4)	0.0019 (4)	0.0011 (4)
C72	0.0193 (5)	0.0298 (8)	0.0227 (7)	0.0007 (4)	0.0054 (5)	−0.0046 (5)
C73	0.0179 (5)	0.0227 (7)	0.0209 (6)	0.0052 (5)	0.0029 (4)	0.0000 (4)
N81	0.0170 (5)	0.0163 (6)	0.0144 (5)	0.0020 (4)	−0.0012 (4)	−0.0003 (4)
N82	0.0183 (6)	0.0234 (7)	0.0161 (5)	0.0013 (4)	−0.0028 (4)	0.0013 (4)
C81	0.0185 (6)	0.0214 (6)	0.0166 (5)	0.0048 (5)	−0.0029 (4)	−0.0008 (4)
C82	0.0223 (7)	0.0204 (7)	0.0157 (5)	−0.0011 (5)	−0.0037 (5)	0.0001 (4)
C83	0.0233 (7)	0.0172 (6)	0.0164 (5)	0.0017 (4)	−0.0041 (5)	−0.0018 (4)

Geometric parameters (Å, º)

Mn1—O1	2.157 (1)	N42—C42	1.366 (1)
Mn1—O7	2.202 (1)	C42—C43	1.360 (1)
Mn1—N11	2.262 (1)	N51—C51	1.321 (1)
Mn1—N21A	2.260 (1)	N51—C53	1.381 (1)
Mn1—N21B	2.260 (1)	N52—C51	1.347 (1)
Mn1—N51	2.262 (1)	N52—C52	1.366 (1)
Mn1—N61	2.216 (1)	C52—C53	1.360 (1)
Mn2—O4	2.132 (1)	N61—C61	1.321 (1)
Mn2—O4^i	2.132 (1)	N61—C63	1.381 (1)
Mn2—N31	2.264 (1)	N62—C61	1.347 (1)
Mn2—N31^i	2.264 (1)	N62—C62	1.366 (1)
Mn2—N41	2.252 (1)	C62—C63	1.360 (1)
Mn2—N41^i	2.252 (1)	N71—C71	1.321 (1)
Mn3—O10	2.126 (1)	N71—C73	1.381 (1)
Mn3—O10^ii	2.126 (1)	N72—C71	1.347 (1)
Mn3—N71	2.257 (1)	N72—C72	1.366 (1)
Mn3—N71^ii	2.257 (1)	C72—C73	1.360 (1)
Mn3—N81	2.246 (1)	N81—C81	1.321 (1)
Mn3—N81^ii	2.246 (1)	N81—C83	1.381 (1)
V1—O1	1.651 (1)	N82—C81	1.347 (1)
V1—O2	1.797 (1)	N82—C82	1.366 (1)
V1—O3	1.637 (1)	C82—C83	1.360 (1)
V1—O5	1.820 (1)	N12—H1N12	0.860
V2—O2^iii	1.804 (1)	C11—H1C11	0.930
V2—O4	1.644 (1)	C12—H1C12	0.930
V2—O5	1.812 (1)	C13—H1C13	0.930
V2—O6	1.638 (1)	N22A—H1N22A	0.860
V3—O7	1.640 (1)	C21A—H1C21A	0.930
V3—O8	1.796 (1)	C22A—H1C22A	0.930
V3—O9	1.650 (1)	C23A—H1C23A	0.930
V3—O11	1.810 (1)	N22B—H1N22B	0.860
V4—O8^iv	1.806 (1)	C21B—H1C21B	0.930
V4—O10	1.641 (1)	C22B—H1C22B	0.930
V4—O11	1.814 (1)	C23B—H1C23B	0.930
V4—O12	1.633 (1)	N32—H1N32	0.860
N11—C11	1.321 (1)	C31—H1C31	0.930
N11—C13	1.381 (1)	C32—H1C32	0.930
N12—C11	1.347 (1)	C33—H1C33	0.930
N12—C12	1.366 (1)	N42—H1N42	0.860
C12—C13	1.360 (1)	C41—H1C41	0.930
N21A—C21A	1.321 (1)	C42—H1C42	0.930
N21A—C23A	1.381 (1)	C43—H1C43	0.930
N22A—C21A	1.347 (1)	N52—H1N52	0.860
N22A—C22A	1.366 (1)	C51—H1C51	0.930
C22A—C23A	1.360 (1)	C52—H1C52	0.930
N21B—C21B	1.321 (1)	C53—H1C53	0.930
N21B—C23B	1.381 (1)	N62—H1N62	0.860
N22B—C21B	1.347 (1)	C61—H1C61	0.930
N22B—C22B	1.366 (1)	C62—H1C62	0.930
C22B—C23B	1.360 (1)	C63—H1C63	0.930
N31—C31	1.321 (1)	N72—H1N72	0.860
N31—C33	1.381 (1)	C71—H1C71	0.930
N32—C31	1.347 (1)	C72—H1C72	0.930
N32—C32	1.366 (1)	C73—H1C73	0.930
C32—C33	1.360 (1)	N82—H1N82	0.860
N41—C41	1.321 (1)	C81—H1C81	0.930
N41—C43	1.381 (1)	C82—H1C82	0.930
N42—C41	1.347 (1)	C83—H1C83	0.930
Mn1···V2	5.922	C11···C21A	3.510 (2)
Mn1···V4	5.957	C11···C61^vi	3.402 (2)
V2···V2^iii	4.136 (1)	C11···C82^x	3.565 (2)
V4···V4^iv	4.225 (1)	C11···C23B	3.590 (2)
O2···C52^v	3.375 (2)	C12···C21A^vi	3.393 (2)
O3···C22A^vi	3.488 (3)	C12···C32	3.494 (2)
O3···N42^vi	2.791 (2)	C12···C23B^vi	3.418 (2)
O3···C51	3.325 (2)	N22A···C72^x	3.469 (2)
O3···N22B^vi	3.455 (3)	C31···C71^vii	3.507 (2)
O5···N72^vii	2.764 (2)	C31···C73^xi	3.556 (2)
O5···C72^vii	3.432 (2)	N62···C53^v	3.280 (2)
O6···C41	3.297 (2)	C61···C52^v	3.487 (2)
O6···N52^v	2.782 (2)	C61···C53^v	3.409 (2)
O8···C12^v	3.314 (2)	C52···C72	3.379 (2)
O9···N62^vi	2.851 (2)	C72···C22B^xii	3.427 (2)
O9···N82^vi	2.762 (2)	C73···C81	3.560 (2)
O11···N32^viii	2.890 (2)	N82···C82^ix	3.399 (2)
O12···N12^v	2.774 (2)	N82···C83^ix	3.369 (2)
O12···C81	3.365 (2)	C81···C82^ix	3.568 (2)
O12···C82^ix	3.447 (2)	C82···C83^ix	3.525 (2)
N12···C61^vi	3.329 (2)
O1—Mn1—O7	172.2 (1)	N32—C32—C33	105.9 (1)
O1—Mn1—N11	89.7	N31—C33—C32	110.0 (1)
O1—Mn1—N21A	92.3	Mn2—N41—C41	126.2 (1)
O1—Mn1—N51	97.8 (1)	Mn2—N41—C43	128.6 (1)
O1—Mn1—N61	86.1 (1)	C41—N41—C43	105.1 (1)
O1—Mn1—N21B	92.3	C41—N42—C42	107.6 (1)
O7—Mn1—N11	96.3 (1)	N41—C41—N42	111.4 (1)
O7—Mn1—N21A	83.4	N42—C42—C43	105.9 (1)
O7—Mn1—N51	87.7	N41—C43—C42	110.0 (1)
O7—Mn1—N61	88.5 (1)	Mn1—N51—C51	127.3 (1)
O7—Mn1—N21B	83.4	Mn1—N51—C53	127.3 (1)
N11—Mn1—N21A	84.3	C51—N51—C53	105.1 (1)
N11—Mn1—N51	84.8 (1)	C51—N52—C52	107.6 (1)
N11—Mn1—N61	172.0 (1)	N51—C51—N52	111.4 (1)
N11—Mn1—N21B	84.3	N52—C52—C53	105.9 (1)
N21A—Mn1—N51	165.0	N51—C53—C52	110.0 (1)
N21A—Mn1—N61	102.6 (1)	Mn1—N61—C61	129.0 (1)
N21A—Mn1—N21B	0.0 (1)	Mn1—N61—C63	126.0 (1)
N51—Mn1—N61	89.1 (1)	C61—N61—C63	105.1 (1)
N51—Mn1—N21B	165.0	C61—N62—C62	107.6 (1)
N61—Mn1—N21B	102.6 (1)	N61—C61—N62	111.4 (1)
O4—Mn2—O4^i	171.9 (1)	N62—C62—C63	105.9 (1)
O4—Mn2—N31	86.1	N61—C63—C62	110.0 (1)
O4—Mn2—N31^i	88.8	Mn3—N71—C71	128.8 (1)
O4—Mn2—N41	94.6 (1)	Mn3—N71—C73	126.1 (1)
O4—Mn2—N41^i	91.3	C71—N71—C73	105.1 (1)
O4^i—Mn2—N31	88.8	C71—N72—C72	107.6 (1)
O4^i—Mn2—N31^i	86.1	N71—C71—N72	111.4 (1)
O4^i—Mn2—N41	91.3	N72—C72—C73	105.9 (1)
O4^i—Mn2—N41^i	94.6 (1)	N71—C73—C72	110.0 (1)
N31—Mn2—N31^i	101.4 (1)	Mn3—N81—C81	130.4 (1)
N31—Mn2—N41	86.1	Mn3—N81—C83	123.8 (1)
N31—Mn2—N41^i	171.9	C81—N81—C83	105.1 (1)
N31^i—Mn2—N41	171.9	C81—N82—C82	107.6 (1)
N31^i—Mn2—N41^i	86.1	N81—C81—N82	111.4 (1)
N41—Mn2—N41^i	86.5 (1)	N82—C82—C83	105.9 (1)
O10—Mn3—O10^ii	171.9 (1)	N81—C83—C82	110.0 (1)
O10—Mn3—N71	85.5	C11—N12—H1N12	126.2
O10—Mn3—N71^ii	89.3	C12—N12—H1N12	126.2
O10—Mn3—N81	95.4 (1)	N11—C11—H1C11	124.3
O10—Mn3—N81^ii	90.6	N12—C11—H1C11	124.3
O10^ii—Mn3—N71	89.3	N12—C12—H1C12	127.1
O10^ii—Mn3—N71^ii	85.5	C13—C12—H1C12	127.1
O10^ii—Mn3—N81	90.6	N11—C13—H1C13	125.0
O10^ii—Mn3—N81^ii	95.4 (1)	C12—C13—H1C13	125.0
N71—Mn3—N71^ii	100.3 (1)	C21A—N22A—H1N22A	126.2
N71—Mn3—N81	87.1	C22A—N22A—H1N22A	126.2
N71—Mn3—N81^ii	171.6	N21A—C21A—H1C21A	124.3
N71^ii—Mn3—N81	171.6	N22A—C21A—H1C21A	124.3
N71^ii—Mn3—N81^ii	87.1	N22A—C22A—H1C22A	127.1
N81—Mn3—N81^ii	85.8 (1)	C23A—C22A—H1C22A	127.1
O1—V1—O2	110.6 (1)	N21A—C23A—H1C23A	125.0
O1—V1—O3	108.9 (1)	C22A—C23A—H1C23A	125.0
O1—V1—O5	109.8 (1)	C21B—N22B—H1N22B	126.2
O2—V1—O3	111.3 (1)	C22B—N22B—H1N22B	126.2
O2—V1—O5	107.3 (1)	N21B—C21B—H1C21B	124.3
O3—V1—O5	108.9 (1)	N22B—C21B—H1C21B	124.3
O2^iii—V2—O4	108.4 (1)	N22B—C22B—H1C22B	127.1
O2^iii—V2—O5	110.3 (1)	C23B—C22B—H1C22B	127.1
O2^iii—V2—O6	111.0 (1)	N21B—C23B—H1C23B	125.0
O4—V2—O5	108.1 (1)	C22B—C23B—H1C23B	125.0
O4—V2—O6	109.4 (1)	C31—N32—H1N32	126.2
O5—V2—O6	109.6 (1)	C32—N32—H1N32	126.2
O7—V3—O8	109.1 (1)	N31—C31—H1C31	124.3
O7—V3—O9	107.9 (1)	N32—C31—H1C31	124.3
O7—V3—O11	111.1 (1)	N32—C32—H1C32	127.1
O8—V3—O9	112.9 (1)	C33—C32—H1C32	127.1
O8—V3—O11	108.3 (1)	N31—C33—H1C33	125.0
O9—V3—O11	107.5 (1)	C32—C33—H1C33	125.0
O8^iv—V4—O10	109.2 (1)	C41—N42—H1N42	126.2
O8^iv—V4—O11	111.4 (1)	C42—N42—H1N42	126.2
O8^iv—V4—O12	108.9 (1)	N41—C41—H1C41	124.3
O10—V4—O11	106.7 (1)	N42—C41—H1C41	124.3
O10—V4—O12	109.4 (1)	N42—C42—H1C42	127.1
O11—V4—O12	111.3 (1)	C43—C42—H1C42	127.1
Mn1—O1—V1	161.0 (1)	N41—C43—H1C43	125.0
V1—O2—V2^iii	134.8 (1)	C42—C43—H1C43	125.0
Mn2—O4—V2	163.5 (1)	C51—N52—H1N52	126.2
V1—O5—V2	124.8 (1)	C52—N52—H1N52	126.2
Mn1—O7—V3	170.1 (1)	N51—C51—H1C51	124.3
V3—O8—V4^iv	135.9 (1)	N52—C51—H1C51	124.3
Mn3—O10—V4	160.0 (1)	N52—C52—H1C52	127.1
V3—O11—V4	128.0 (1)	C53—C52—H1C52	127.1
Mn1—N11—C11	125.4 (1)	N51—C53—H1C53	125.0
Mn1—N11—C13	129.2 (1)	C52—C53—H1C53	125.0
C11—N11—C13	105.1 (1)	C61—N62—H1N62	126.2
C11—N12—C12	107.6 (1)	C62—N62—H1N62	126.2
N11—C11—N12	111.4 (1)	N61—C61—H1C61	124.3
N12—C12—C13	105.9 (1)	N62—C61—H1C61	124.3
N11—C13—C12	110.0 (1)	N62—C62—H1C62	127.1
Mn1—N21A—C21A	124.1 (1)	C63—C62—H1C62	127.1
Mn1—N21A—C23A	129.6 (1)	N61—C63—H1C63	125.0
C21A—N21A—C23A	105.1 (1)	C62—C63—H1C63	125.0
C21A—N22A—C22A	107.6 (1)	C71—N72—H1N72	126.2
N21A—C21A—N22A	111.4 (1)	C72—N72—H1N72	126.2
N22A—C22A—C23A	105.9 (1)	N71—C71—H1C71	124.3
N21A—C23A—C22A	110.0 (1)	N72—C71—H1C71	124.3
Mn1—N21B—C21B	123.8 (1)	N72—C72—H1C72	127.1
Mn1—N21B—C23B	129.9 (1)	C73—C72—H1C72	127.1
C21B—N21B—C23B	105.1 (1)	N71—C73—H1C73	125.0
C21B—N22B—C22B	107.6 (1)	C72—C73—H1C73	125.0
N21B—C21B—N22B	111.4 (1)	C81—N82—H1N82	126.2
N22B—C22B—C23B	105.9 (1)	C82—N82—H1N82	126.2
N21B—C23B—C22B	110.0 (1)	N81—C81—H1C81	124.3
Mn2—N31—C31	132.0 (1)	N82—C81—H1C81	124.3
Mn2—N31—C33	122.9 (1)	N82—C82—H1C82	127.1
C31—N31—C33	105.1 (1)	C83—C82—H1C82	127.1
C31—N32—C32	107.6 (1)	N81—C83—H1C83	125.0
N31—C31—N32	111.4 (1)	C82—C83—H1C83	125.0

Symmetry codes: (i) −x+2, −y+1/2, z; (ii) −x+1, −y+3/2, z; (iii) −x+2, −y+1, −z+1; (iv) −x+1, −y+1, −z+1; (v) y+1/4, −x+5/4, z+1/4; (vi) −y+5/4, x−1/4, z−1/4; (vii) −y+7/4, x−1/4, −z+3/4; (viii) −y+3/4, x−1/4, −z+3/4; (ix) y−1/4, −x+5/4, −z+5/4; (x) x, y−1/2, −z+1; (xi) y+1/4, −x+3/4, −z+3/4; (xii) x, y+1/2, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N12—H1N12···O12^vi	0.86	1.97	2.774 (2)	155
N32—H1N32···O11^xi	0.86	2.07	2.890 (2)	159
N42—H1N42···O3^v	0.86	2.00	2.791 (2)	153
N52—H1N52···O6^vi	0.86	1.96	2.782 (2)	161
N62—H1N62···O9^v	0.86	2.02	2.851 (2)	161
N72—H1N72···O5^xiii	0.86	1.99	2.764 (2)	149
N82—H1N82···O9^v	0.86	1.92	2.762 (2)	166
C51—H1C51···O3	0.93	2.41	3.325 (2)	168

Symmetry codes: (v) y+1/4, −x+5/4, z+1/4; (vi) −y+5/4, x−1/4, z−1/4; (xi) y+1/4, −x+3/4, −z+3/4; (xiii) y+1/4, −x+7/4, −z+3/4.

catena-tetrakis(imidazole)-tetrakis(µ₂-oxo)-dioxo-manganese(ii)-di-vanadium (Mn_200K)

Crystal data

[Mn(C3H4N2)4V2O6]	Dx = 1.772 Mg m^−3
Mr = 525.13	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I41/a	Cell parameters from 55984 reflections
Hall symbol: -I 4ad	θ = 2.6–30.0°
a = 23.0473 (3) Å	µ = 1.61 mm^−1
c = 29.6521 (3) Å	T = 200 K
V = 15750.5 (3) Å^3	Hexagonal, orange-yellow
Z = 32	0.19 × 0.14 × 0.09 mm
F(000) = 8416.0

Data collection

Enraf-Nonius KappaCCD diffractometer	11499 independent reflections
Radiation source: fine-focus sealed tube	7205 reflections with I > 3σ(I)
Graphite monochromator	Rint = 0.061
φ scan plus ω scans with κ offsets	θmax = 30.0°, θmin = 2.7°
Absorption correction: multi-scan from symmetry-related measurements Sortav (Blessing 1995)	h = −32→29
Tmin = 0.708, Tmax = 0.768	k = −30→32
96520 measured reflections	l = −41→41

Refinement

Refinement on F	2 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.033	w = 1/[σ(F)^2 + (0.0004F)^2]
wR(F^2) = 0.046	(Δ/σ)max = 0.2
S = 1.45	Δρmax = 0.76 e Å^−3
7205 reflections	Δρmin = −0.70 e Å^−3
317 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mn1	0.74975 (1)	0.49579 (1)	0.45189 (1)	0.0159 (1)
Mn2	1.00000	0.25000	0.48963 (1)	0.0155 (1)
Mn3	0.50000	0.75000	0.48468 (1)	0.0150 (1)
V1	0.91217 (2)	0.51361 (2)	0.44968 (1)	0.0152 (1)
V2	0.98624 (2)	0.41129 (2)	0.49605 (1)	0.0154 (1)
V3	0.58396 (2)	0.48376 (2)	0.44629 (1)	0.0144 (1)
V4	0.51508 (2)	0.59006 (2)	0.49476 (1)	0.0147 (1)
O1	0.84297 (7)	0.50112 (7)	0.45997 (5)	0.0267 (4)
O2	0.94355 (7)	0.55702 (7)	0.49357 (5)	0.0238 (4)
O3	0.91793 (7)	0.54534 (7)	0.40067 (5)	0.0325 (4)
O4	0.99516 (7)	0.34221 (6)	0.48436 (5)	0.0256 (4)
O5	0.95188 (7)	0.44552 (6)	0.44803 (5)	0.0232 (4)
O6	0.94432 (7)	0.41791 (7)	0.54021 (5)	0.0303 (4)
O7	0.65398 (7)	0.49130 (7)	0.45375 (5)	0.0272 (4)
O8	0.55479 (6)	0.44022 (7)	0.49101 (5)	0.0226 (4)
O9	0.57374 (7)	0.45493 (7)	0.39610 (5)	0.0313 (4)
O10	0.50678 (7)	0.65805 (7)	0.48008 (5)	0.0260 (4)
O11	0.54741 (7)	0.55323 (6)	0.44705 (5)	0.0236 (4)
O12	0.55719 (7)	0.58647 (7)	0.53887 (5)	0.0296 (4)
N11	0.76207 (7)	0.43027 (6)	0.39577 (4)	0.0239 (5)
N12	0.74147 (7)	0.36315 (7)	0.34561 (5)	0.0330 (6)
C11	0.72305 (6)	0.39256 (7)	0.38208 (5)	0.0281 (5)
C12	0.79522 (8)	0.38287 (8)	0.33515 (5)	0.0333 (6)
C13	0.80773 (6)	0.42421 (7)	0.36615 (5)	0.0287 (5)
N21A	0.74401 (6)	0.41688 (6)	0.49663 (5)	0.0266 (4)	0.515 (9)
N22A	0.7100 (2)	0.33362 (9)	0.52125 (10)	0.0522 (8)	0.515 (9)
C21A	0.69840 (11)	0.38267 (13)	0.49839 (8)	0.0353 (6)	0.515 (9)
C22A	0.7660 (3)	0.33623 (13)	0.53501 (9)	0.0742 (9)	0.515 (9)
C23A	0.78679 (13)	0.38760 (15)	0.51976 (8)	0.0620 (7)	0.515 (9)
N21B	0.74401 (6)	0.41688 (6)	0.49663 (5)	0.0266 (4)	0.485
N22B	0.7763 (3)	0.34224 (14)	0.53531 (9)	0.0789 (9)	0.485
C21B	0.78901 (12)	0.39444 (15)	0.51758 (8)	0.0605 (7)	0.485
C22B	0.7202 (3)	0.33028 (8)	0.52531 (11)	0.0553 (8)	0.485
C23B	0.70048 (13)	0.37638 (13)	0.50148 (9)	0.0366 (6)	0.485
N31	0.92382 (6)	0.24808 (6)	0.44113 (5)	0.0226 (5)
N32	0.86069 (7)	0.22815 (7)	0.38778 (5)	0.0344 (6)
C31	0.91148 (7)	0.21367 (7)	0.40708 (5)	0.0272 (5)
C32	0.83904 (7)	0.27434 (8)	0.41054 (6)	0.0363 (6)
C33	0.87808 (7)	0.28646 (7)	0.44337 (5)	0.0290 (5)
N41	0.93327 (6)	0.24350 (7)	0.54508 (5)	0.0237 (4)
N42	0.87590 (7)	0.26757 (7)	0.60124 (5)	0.0341 (4)
C41	0.92011 (7)	0.28404 (6)	0.57455 (5)	0.0308 (4)
C42	0.85960 (7)	0.21354 (8)	0.58837 (6)	0.0388 (6)
C43	0.89507 (8)	0.19889 (7)	0.55375 (6)	0.0368 (5)
N51	0.74140 (7)	0.56111 (6)	0.39533 (4)	0.0230 (5)
N52	0.76229 (8)	0.61711 (7)	0.33757 (5)	0.0387 (5)
C51	0.78339 (6)	0.58430 (8)	0.37131 (6)	0.0375 (6)
C52	0.70359 (8)	0.61504 (8)	0.33988 (6)	0.0363 (6)
C53	0.69092 (6)	0.58049 (8)	0.37551 (6)	0.0354 (6)
N61	0.74521 (7)	0.56805 (6)	0.50111 (5)	0.0260 (6)
N62	0.73071 (8)	0.62045 (8)	0.56200 (5)	0.0404 (6)
C61	0.72670 (8)	0.56758 (7)	0.54305 (5)	0.0396 (7)
C62	0.75299 (11)	0.65704 (7)	0.53067 (7)	0.0561 (9)
C63	0.76185 (10)	0.62456 (8)	0.49322 (6)	0.0568 (10)
N71	0.57506 (6)	0.75227 (6)	0.43558 (5)	0.0223 (5)
N72	0.63581 (7)	0.77836 (7)	0.38217 (5)	0.0347 (5)
C71	0.58562 (7)	0.79012 (7)	0.40343 (5)	0.0285 (5)
C72	0.65893 (7)	0.73040 (8)	0.40158 (6)	0.0361 (6)
C73	0.62135 (7)	0.71448 (7)	0.43447 (5)	0.0300 (6)
N81	0.56606 (6)	0.75909 (7)	0.54014 (4)	0.0245 (5)
N82	0.63103 (6)	0.74124 (7)	0.59259 (5)	0.0301 (5)
C81	0.60617 (7)	0.72274 (6)	0.55415 (5)	0.0299 (5)
C82	0.60567 (8)	0.79222 (7)	0.60404 (5)	0.0301 (5)
C83	0.56567 (7)	0.80304 (7)	0.57163 (5)	0.0296 (5)
H1N12	0.72255	0.33663	0.33147	0.038
H1C11	0.68724	0.38693	0.39587	0.031
H1C12	0.81872	0.37054	0.31153	0.039
H1C13	0.84206	0.44537	0.36727	0.032
H1N22A	0.68614	0.30564	0.52625	0.067
H1C21A	0.66266	0.39130	0.48546	0.050	0.515
H1C22A	0.78609	0.30843	0.55154	0.113	0.515
H1C23A	0.82438	0.40110	0.52424	0.096	0.515
H1N22B	0.79966	0.32039	0.55030	0.119	0.485
H1C21B	0.82503	0.41240	0.51986	0.090	0.485
H1C22B	0.69949	0.29718	0.53319	0.070	0.485
H1C23B	0.66307	0.38014	0.49007	0.051	0.485
H1N32	0.84482	0.21117	0.36509	0.040	0.515
H1C31	0.93490	0.18319	0.39754	0.029
H1C32	0.80445	0.29375	0.40478	0.045
H1C33	0.87453	0.31627	0.46433	0.032
H1N42	0.86071	0.28769	0.62263	0.042
H1C41	0.93899	0.31960	0.57667	0.044
H1C42	0.83010	0.19111	0.60076	0.053
H1C43	0.89382	0.16390	0.53816	0.054
H1N52	0.78242	0.63600	0.31805	0.054
H1C51	0.82269	0.57873	0.37694	0.061
H1C52	0.67736	0.63355	0.32088	0.049
H1C53	0.65366	0.57122	0.38517	0.058
H1N62	0.72092	0.62943	0.58910	0.054
H1C61	0.71261	0.53484	0.55776	0.073
H1C62	0.76064	0.69640	0.53418	0.088
H1C63	0.77694	0.63837	0.46618	0.101
H1N72	0.65057	0.79778	0.36022	0.042
H1C71	0.56144	0.82109	0.39629	0.034
H1C72	0.69353	0.71214	0.39390	0.046
H1C73	0.62610	0.68274	0.45348	0.037
H1N82	0.65812	0.72386	0.60726	0.035
H1C81	0.61610	0.68857	0.53936	0.039
H1C82	0.61402	0.81510	0.62905	0.036
H1C83	0.54153	0.83536	0.57076	0.038

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mn1	0.0149 (2)	0.0177 (2)	0.0152 (2)	−0.0018 (1)	0.0011 (1)	−0.0005 (1)
Mn2	0.0172 (3)	0.0134 (2)	0.0159 (2)	0.0009 (2)	0.0000 (1)	0.0000 (1)
Mn3	0.0172 (3)	0.0134 (2)	0.0143 (2)	0.0017 (2)	0.0000 (1)	0.0000 (1)
V1	0.0138 (2)	0.0147 (2)	0.0171 (2)	−0.0001 (1)	−0.0013 (1)	−0.0004 (1)
V2	0.0158 (2)	0.0123 (2)	0.0180 (2)	0.0005 (1)	−0.0001 (1)	−0.0025 (1)
V3	0.0141 (2)	0.0148 (2)	0.0142 (2)	−0.0003 (1)	0.0030 (1)	−0.0005 (1)
V4	0.0168 (2)	0.0127 (2)	0.0146 (2)	0.0007 (1)	0.0012 (1)	0.0018 (1)
O1	0.0163 (9)	0.0310 (10)	0.0328 (9)	−0.0031 (7)	−0.0003 (7)	−0.0064 (7)
O2	0.0197 (9)	0.0241 (9)	0.0276 (8)	−0.0033 (7)	−0.0018 (7)	−0.0077 (7)
O3	0.0351 (11)	0.0349 (11)	0.0277 (9)	−0.0050 (8)	−0.0043 (7)	0.0116 (7)
O4	0.0274 (9)	0.0133 (8)	0.0360 (9)	0.0023 (7)	−0.0049 (7)	−0.0032 (7)
O5	0.0285 (10)	0.0199 (9)	0.0210 (8)	0.0062 (7)	−0.0034 (6)	−0.0032 (6)
O6	0.0327 (10)	0.0299 (10)	0.0281 (9)	0.0033 (8)	0.0112 (7)	−0.0002 (7)
O7	0.0154 (9)	0.0283 (10)	0.0381 (10)	−0.0009 (7)	0.0030 (7)	0.0075 (7)
O8	0.0213 (9)	0.0254 (9)	0.0212 (8)	−0.0028 (7)	0.0038 (6)	0.0051 (7)
O9	0.0414 (11)	0.0321 (10)	0.0203 (8)	−0.0109 (8)	0.0065 (7)	−0.0075 (7)
O10	0.0325 (10)	0.0168 (9)	0.0287 (9)	0.0043 (7)	0.0073 (7)	0.0046 (7)
O11	0.0292 (10)	0.0208 (9)	0.0207 (8)	0.0087 (7)	0.0059 (6)	0.0027 (6)
O12	0.0319 (10)	0.0325 (10)	0.0243 (8)	0.0022 (8)	−0.0093 (7)	−0.0011 (7)
N11	0.0242 (8)	0.0260 (7)	0.0215 (6)	−0.0030 (6)	0.0001 (5)	−0.0032 (5)
N12	0.0412 (9)	0.0309 (7)	0.0269 (7)	−0.0020 (6)	−0.0034 (6)	−0.0084 (6)
C11	0.0304 (7)	0.0281 (8)	0.0259 (7)	−0.0053 (6)	−0.0023 (6)	−0.0060 (6)
C12	0.0408 (9)	0.0342 (9)	0.0249 (6)	0.0022 (7)	0.0022 (6)	−0.0072 (6)
C13	0.0296 (8)	0.0322 (9)	0.0241 (7)	−0.0006 (6)	0.0039 (6)	−0.0049 (6)
N21A	0.0307 (8)	0.0300 (8)	0.0192 (7)	0.0006 (6)	0.0017 (6)	0.0050 (5)
N22A	0.0610 (15)	0.0393 (8)	0.0564 (11)	−0.0060 (8)	0.0065 (10)	0.0219 (7)
C21A	0.0392 (9)	0.0336 (8)	0.0331 (9)	−0.0060 (7)	0.0047 (7)	0.0087 (6)
C22A	0.0639 (15)	0.0622 (10)	0.0965 (15)	0.0004 (10)	−0.0069 (13)	0.0547 (10)
C23A	0.0461 (10)	0.0621 (11)	0.0779 (13)	−0.0036 (8)	−0.0161 (10)	0.0467 (10)
N21B	0.0307 (8)	0.0300 (8)	0.0192 (7)	0.0006 (6)	0.0017 (6)	0.0050 (5)
N22B	0.0626 (15)	0.0687 (11)	0.1053 (16)	−0.0003 (10)	−0.0119 (13)	0.0619 (12)
C21B	0.0443 (10)	0.0619 (11)	0.0754 (13)	−0.0043 (8)	−0.0170 (9)	0.0454 (10)
C22B	0.0629 (15)	0.0413 (8)	0.0615 (12)	−0.0038 (8)	0.0059 (10)	0.0262 (7)
C23B	0.0415 (9)	0.0337 (8)	0.0345 (9)	−0.0059 (7)	0.0050 (7)	0.0096 (6)
N31	0.0241 (6)	0.0217 (8)	0.0221 (6)	0.0029 (5)	−0.0010 (5)	−0.0024 (5)
N32	0.0345 (8)	0.0411 (10)	0.0276 (7)	−0.0110 (6)	−0.0087 (6)	0.0076 (6)
C31	0.0322 (7)	0.0285 (7)	0.0210 (6)	−0.0049 (5)	−0.0029 (5)	−0.0019 (5)
C32	0.0271 (7)	0.0418 (11)	0.0398 (9)	−0.0010 (6)	−0.0086 (6)	0.0119 (7)
C33	0.0238 (7)	0.0289 (8)	0.0343 (7)	0.0063 (6)	−0.0028 (5)	0.0029 (5)
N41	0.0247 (7)	0.0236 (8)	0.0228 (6)	−0.0022 (6)	0.0024 (5)	−0.0025 (5)
N42	0.0358 (8)	0.0370 (9)	0.0295 (7)	0.0030 (7)	0.0110 (6)	−0.0008 (6)
C41	0.0358 (8)	0.0290 (8)	0.0277 (7)	−0.0015 (6)	0.0093 (6)	−0.0058 (6)
C42	0.0369 (8)	0.0415 (10)	0.0381 (8)	−0.0068 (7)	0.0152 (7)	−0.0013 (7)
C43	0.0386 (9)	0.0332 (8)	0.0385 (8)	−0.0122 (7)	0.0153 (7)	−0.0064 (6)
N51	0.0245 (8)	0.0233 (8)	0.0213 (6)	−0.0030 (6)	0.0019 (5)	0.0005 (5)
N52	0.0433 (9)	0.0402 (9)	0.0326 (7)	−0.0041 (8)	0.0040 (7)	0.0143 (6)
C51	0.0308 (6)	0.0452 (10)	0.0366 (8)	−0.0066 (7)	0.0039 (6)	0.0181 (7)
C52	0.0424 (8)	0.0365 (9)	0.0299 (7)	0.0015 (8)	−0.0016 (7)	0.0097 (6)
C53	0.0296 (7)	0.0425 (10)	0.0342 (8)	0.0019 (7)	−0.0003 (6)	0.0138 (7)
N61	0.0260 (10)	0.0278 (7)	0.0241 (7)	−0.0054 (6)	0.0042 (6)	−0.0046 (5)
N62	0.0441 (12)	0.0442 (9)	0.0329 (7)	0.0041 (8)	−0.0002 (7)	−0.0166 (6)
C61	0.0491 (13)	0.0416 (8)	0.0280 (7)	−0.0092 (7)	0.0141 (7)	−0.0116 (5)
C62	0.0951 (19)	0.0324 (7)	0.0407 (10)	−0.0051 (8)	−0.0010 (10)	−0.0137 (6)
C63	0.1053 (19)	0.0286 (8)	0.0366 (8)	−0.0196 (7)	0.0134 (9)	−0.0084 (6)
N71	0.0242 (7)	0.0225 (8)	0.0201 (6)	0.0009 (5)	0.0015 (5)	0.0012 (5)
N72	0.0337 (7)	0.0462 (10)	0.0243 (6)	−0.0116 (6)	0.0077 (6)	−0.0045 (6)
C71	0.0325 (7)	0.0316 (9)	0.0214 (7)	−0.0049 (5)	0.0042 (5)	0.0041 (6)
C72	0.0272 (7)	0.0478 (11)	0.0333 (9)	−0.0021 (6)	0.0079 (6)	−0.0108 (7)
C73	0.0255 (7)	0.0329 (9)	0.0316 (8)	0.0057 (6)	0.0045 (6)	−0.0027 (6)
N81	0.0267 (7)	0.0253 (8)	0.0215 (6)	0.0044 (6)	−0.0031 (5)	−0.0012 (5)
N82	0.0296 (7)	0.0357 (9)	0.0251 (6)	0.0026 (6)	−0.0064 (6)	0.0018 (6)
C81	0.0300 (8)	0.0332 (8)	0.0264 (6)	0.0090 (6)	−0.0068 (6)	−0.0023 (6)
C82	0.0352 (9)	0.0318 (9)	0.0235 (6)	−0.0011 (7)	−0.0069 (6)	−0.0002 (6)
C83	0.0368 (9)	0.0272 (8)	0.0248 (6)	0.0040 (6)	−0.0078 (6)	−0.0038 (6)

Geometric parameters (Å, º)

Mn1—O1	2.165 (2)	N42—C42	1.356 (1)
Mn1—O7	2.210 (2)	C42—C43	1.355 (1)
Mn1—N11	2.265 (1)	N51—C51	1.315 (1)
Mn1—N21A	2.255 (1)	N51—C53	1.378 (1)
Mn1—N21B	2.255 (1)	N52—C51	1.345 (1)
Mn1—N51	2.262 (1)	N52—C52	1.356 (1)
Mn1—N61	2.217 (1)	C52—C53	1.355 (1)
Mn2—O4	2.134 (1)	N61—C61	1.315 (1)
Mn2—O4^i	2.134 (1)	N61—C63	1.378 (1)
Mn2—N31	2.270 (1)	N62—C61	1.345 (1)
Mn2—N31^i	2.270 (1)	N62—C62	1.356 (1)
Mn2—N41	2.256 (1)	C62—C63	1.355 (1)
Mn2—N41^i	2.256 (1)	N71—C71	1.315 (1)
Mn3—O10	2.129 (2)	N71—C73	1.378 (1)
Mn3—O10^ii	2.129 (2)	N72—C71	1.345 (1)
Mn3—N71	2.262 (1)	N72—C72	1.356 (1)
Mn3—N71^ii	2.262 (1)	C72—C73	1.355 (1)
Mn3—N81	2.251 (1)	N81—C81	1.315 (1)
Mn3—N81^ii	2.251 (1)	N81—C83	1.378 (1)
V1—O1	1.649 (2)	N82—C81	1.345 (1)
V1—O2	1.794 (1)	N82—C82	1.356 (1)
V1—O3	1.632 (2)	C82—C83	1.355 (1)
V1—O5	1.817 (2)	N12—H1N12	0.860
V2—O2^iii	1.802 (2)	C11—H1C11	0.930
V2—O4	1.642 (1)	C12—H1C12	0.930
V2—O5	1.810 (1)	C13—H1C13	0.930
V2—O6	1.635 (2)	N22A—H1N22A	0.860
V3—O7	1.638 (2)	C21A—H1C21A	0.930
V3—O8	1.794 (1)	C22A—H1C22A	0.930
V3—O9	1.647 (2)	C23A—H1C23A	0.930
V3—O11	1.809 (2)	N22B—H1N22B	0.860
V4—O8^iv	1.805 (2)	C21B—H1C21B	0.930
V4—O10	1.638 (2)	C22B—H1C22B	0.930
V4—O11	1.810 (1)	C23B—H1C23B	0.930
V4—O12	1.631 (2)	N32—H1N32	0.860
N11—C11	1.315 (1)	C31—H1C31	0.930
N11—C13	1.378 (1)	C32—H1C32	0.930
N12—C11	1.345 (1)	C33—H1C33	0.930
N12—C12	1.356 (1)	N42—H1N42	0.860
C12—C13	1.355 (1)	C41—H1C41	0.930
N21A—C21A	1.315 (1)	C42—H1C42	0.930
N21A—C23A	1.378 (1)	C43—H1C43	0.930
N22A—C21A	1.345 (1)	N52—H1N52	0.860
N22A—C22A	1.356 (1)	C51—H1C51	0.930
C22A—C23A	1.355 (1)	C52—H1C52	0.930
N21B—C21B	1.315 (1)	C53—H1C53	0.930
N21B—C23B	1.378 (1)	N62—H1N62	0.860
N22B—C21B	1.345 (1)	C61—H1C61	0.930
N22B—C22B	1.356 (1)	C62—H1C62	0.930
C22B—C23B	1.355 (1)	C63—H1C63	0.930
N31—C31	1.315 (1)	N72—H1N72	0.860
N31—C33	1.378 (1)	C71—H1C71	0.930
N32—C31	1.345 (1)	C72—H1C72	0.930
N32—C32	1.356 (1)	C73—H1C73	0.930
C32—C33	1.355 (1)	N82—H1N82	0.860
N41—C41	1.315 (1)	C81—H1C81	0.930
N41—C43	1.378 (1)	C82—H1C82	0.930
N42—C41	1.345 (1)	C83—H1C83	0.930
Mn1···V2	5.934	C11···C21A	3.503 (3)
Mn1···V4	5.965	C11···C23B	3.598 (3)
V2···V2^iii	4.145 (1)	C11···C61^vi	3.407 (2)
V4···V4^iv	4.221 (1)	C11···C82^x	3.583 (2)
O2···C52^v	3.390 (2)	C12···C21A^vi	3.415 (3)
O3···C22A^vi	3.497 (3)	C12···C23B^vi	3.442 (3)
O3···N22B^vi	3.456 (3)	C12···C32	3.503 (2)
O3···N42^vi	2.794 (2)	N22A···C72^x	3.504 (2)
O3···C51	3.344 (2)	C31···C71^vii	3.516 (2)
O5···N72^vii	2.785 (2)	C31···C73^xi	3.564 (2)
O5···C72^vii	3.445 (2)	N62···C53^v	3.292 (3)
O6···C41	3.296 (2)	C61···C52^v	3.512 (3)
O6···N52^v	2.780 (2)	C61···C53^v	3.426 (3)
O8···C12^v	3.338 (2)	C52···C72	3.388 (3)
O9···N62^vi	2.868 (2)	C72···C22B^xii	3.463 (2)
O9···N82^vi	2.768 (2)	C73···C81	3.571 (2)
O11···N32^viii	2.903 (2)	N82···C82^ix	3.418 (2)
O12···N12^v	2.779 (2)	N82···C83^ix	3.380 (2)
O12···C81	3.368 (2)	C81···C82^ix	3.585 (2)
O12···C82^ix	3.461 (2)	C82···C83^ix	3.537 (3)
N12···C61^vi	3.336 (2)
O1—Mn1—O7	172.2 (1)	N32—C32—C33	106.0 (1)
O1—Mn1—N11	89.7 (1)	N31—C33—C32	109.9 (1)
O1—Mn1—N21A	92.2 (1)	Mn2—N41—C41	126.5 (1)
O1—Mn1—N21B	92.2 (1)	Mn2—N41—C43	128.4 (1)
O1—Mn1—N51	97.4 (1)	C41—N41—C43	105.0 (1)
O1—Mn1—N61	86.1 (1)	C41—N42—C42	107.7 (1)
O7—Mn1—N11	96.4 (1)	N41—C41—N42	111.4 (1)
O7—Mn1—N21A	83.6 (1)	N42—C42—C43	106.0 (1)
O7—Mn1—N21B	83.6 (1)	N41—C43—C42	109.9 (1)
O7—Mn1—N51	88.0 (1)	Mn1—N51—C51	127.5 (1)
O7—Mn1—N61	88.4 (1)	Mn1—N51—C53	127.1 (1)
N11—Mn1—N21A	84.4 (1)	C51—N51—C53	105.0 (1)
N11—Mn1—N21B	84.4 (1)	C51—N52—C52	107.7 (1)
N11—Mn1—N51	84.8 (1)	N51—C51—N52	111.4 (1)
N11—Mn1—N61	172.1 (1)	N52—C52—C53	106.0 (1)
N21A—Mn1—N51	165.5 (1)	N51—C53—C52	109.9 (1)
N21A—Mn1—N61	102.5 (1)	Mn1—N61—C61	129.2 (1)
N21A—Mn1—N21B	0.0 (1)	Mn1—N61—C63	125.8 (1)
N51—Mn1—N61	89.1 (1)	C61—N61—C63	105.0 (1)
N51—Mn1—N21B	165.5 (1)	C61—N62—C62	107.7 (1)
N61—Mn1—N21B	102.5 (1)	N61—C61—N62	111.4 (1)
O4—Mn2—O4^i	171.6 (1)	N62—C62—C63	106.0 (1)
O4—Mn2—N31	86.1 (1)	N61—C63—C62	109.9 (1)
O4—Mn2—N31^i	88.5 (1)	Mn3—N71—C71	128.6 (1)
O4—Mn2—N41	94.8 (1)	Mn3—N71—C73	126.4 (1)
O4—Mn2—N41^i	91.3 (1)	C71—N71—C73	105.0 (1)
O4^i—Mn2—N31	88.5 (1)	C71—N72—C72	107.7 (1)
O4^i—Mn2—N31^i	86.1 (1)	N71—C71—N72	111.4 (1)
O4^i—Mn2—N41	91.3 (1)	N72—C72—C73	106.0 (1)
O4^i—Mn2—N41^i	94.8 (1)	N71—C73—C72	109.9 (1)
N31—Mn2—N31^i	101.4 (1)	Mn3—N81—C81	130.3 (1)
N31—Mn2—N41	86.2 (1)	Mn3—N81—C83	124.0 (1)
N31—Mn2—N41^i	172.0 (1)	C81—N81—C83	105.0 (1)
N31^i—Mn2—N41	172.0 (1)	C81—N82—C82	107.7 (1)
N31^i—Mn2—N41^i	86.2 (1)	N81—C81—N82	111.4 (1)
N41—Mn2—N41^i	86.4 (1)	N82—C82—C83	106.0 (1)
O10—Mn3—O10^ii	172.6 (1)	N81—C83—C82	109.9 (1)
O10—Mn3—N71	85.7 (1)	C11—N12—H1N12	126.2
O10—Mn3—N71^ii	89.5 (1)	C12—N12—H1N12	126.2
O10—Mn3—N81	95.2 (1)	N11—C11—H1C11	124.3
O10—Mn3—N81^ii	90.2 (1)	N12—C11—H1C11	124.3
O10^ii—Mn3—N71	89.5 (1)	N12—C12—H1C12	127.0
O10^ii—Mn3—N71^ii	85.7 (1)	C13—C12—H1C12	127.0
O10^ii—Mn3—N81	90.2 (1)	N11—C13—H1C13	125.0
O10^ii—Mn3—N81^ii	95.2 (1)	C12—C13—H1C13	125.0
N71—Mn3—N71^ii	99.8 (1)	C21A—N22A—H1N22A	126.2
N71—Mn3—N81	87.2 (1)	C22A—N22A—H1N22A	126.2
N71—Mn3—N81^ii	171.8 (1)	N21A—C21A—H1C21A	124.3
N71^ii—Mn3—N81	171.8 (1)	N22A—C21A—H1C21A	124.3
N71^ii—Mn3—N81^ii	87.2 (1)	N22A—C22A—H1C22A	127.0
N81—Mn3—N81^ii	86.1 (1)	C23A—C22A—H1C22A	127.0
O1—V1—O2	110.7 (1)	N21A—C23A—H1C23A	125.0
O1—V1—O3	108.8 (1)	C22A—C23A—H1C23A	125.0
O1—V1—O5	109.9 (1)	C21B—N22B—H1N22B	126.2
O2—V1—O3	111.3 (1)	C22B—N22B—H1N22B	126.2
O2—V1—O5	107.3 (1)	N21B—C21B—H1C21B	124.3
O3—V1—O5	108.8 (1)	N22B—C21B—H1C21B	124.3
O2^iii—V2—O4	108.5 (1)	N22B—C22B—H1C22B	127.0
O2^iii—V2—O5	110.5 (1)	C23B—C22B—H1C22B	127.0
O2^iii—V2—O6	110.9 (1)	N21B—C23B—H1C23B	125.0
O4—V2—O5	108.1 (1)	C22B—C23B—H1C23B	125.0
O4—V2—O6	109.5 (1)	C31—N32—H1N32	126.2
O5—V2—O6	109.3 (1)	C32—N32—H1N32	126.2
O7—V3—O8	109.2 (1)	N31—C31—H1C31	124.3
O7—V3—O9	107.8 (1)	N32—C31—H1C31	124.3
O7—V3—O11	111.3 (1)	N32—C32—H1C32	127.0
O8—V3—O9	112.9 (1)	C33—C32—H1C32	127.0
O8—V3—O11	108.1 (1)	N31—C33—H1C33	125.0
O9—V3—O11	107.6 (1)	C32—C33—H1C33	125.0
O8^iv—V4—O10	109.1 (1)	C41—N42—H1N42	126.2
O8^iv—V4—O11	111.6 (1)	C42—N42—H1N42	126.2
O8^iv—V4—O12	108.9 (1)	N41—C41—H1C41	124.3
O10—V4—O11	106.8 (1)	N42—C41—H1C41	124.3
O10—V4—O12	109.3 (1)	N42—C42—H1C42	127.0
O11—V4—O12	111.0 (1)	C43—C42—H1C42	127.0
Mn1—O1—V1	161.6 (1)	N41—C43—H1C43	125.0
V1—O2—V2^iii	135.4 (1)	C42—C43—H1C43	125.0
Mn2—O4—V2	163.1 (1)	C51—N52—H1N52	126.2
V1—O5—V2	125.1 (1)	C52—N52—H1N52	126.2
Mn1—O7—V3	170.2 (1)	N51—C51—H1C51	124.3
V3—O8—V4^iv	136.3 (1)	N52—C51—H1C51	124.3
Mn3—O10—V4	160.7 (1)	N52—C52—H1C52	127.0
V3—O11—V4	128.1 (1)	C53—C52—H1C52	127.0
Mn1—N11—C11	125.6 (1)	N51—C53—H1C53	125.0
Mn1—N11—C13	129.2 (1)	C52—C53—H1C53	125.0
C11—N11—C13	105.0 (1)	C61—N62—H1N62	126.2
C11—N12—C12	107.7 (1)	C62—N62—H1N62	126.2
N11—C11—N12	111.4 (1)	N61—C61—H1C61	124.3
N12—C12—C13	106.0 (1)	N62—C61—H1C61	124.3
N11—C13—C12	109.9 (1)	N62—C62—H1C62	127.0
Mn1—N21A—C21A	123.6 (2)	C63—C62—H1C62	127.0
Mn1—N21A—C23A	130.2 (2)	N61—C63—H1C63	125.0
C21A—N21A—C23A	105.0 (1)	C62—C63—H1C63	125.0
C21A—N22A—C22A	107.7 (1)	C71—N72—H1N72	126.2
N21A—C21A—N22A	111.4 (1)	C72—N72—H1N72	126.2
N22A—C22A—C23A	106.0 (1)	N71—C71—H1C71	124.3
N21A—C23A—C22A	109.9 (1)	N72—C71—H1C71	124.3
Mn1—N21B—C21B	123.3 (2)	N72—C72—H1C72	127.0
Mn1—N21B—C23B	130.6 (2)	C73—C72—H1C72	127.0
C21B—N21B—C23B	105.0 (1)	N71—C73—H1C73	125.0
C21B—N22B—C22B	107.7 (1)	C72—C73—H1C73	125.0
N21B—C21B—N22B	111.4 (1)	C81—N82—H1N82	126.2
N22B—C22B—C23B	106.0 (1)	C82—N82—H1N82	126.2
N21B—C23B—C22B	109.9 (1)	N81—C81—H1C81	124.3
Mn2—N31—C31	131.7 (1)	N82—C81—H1C81	124.3
Mn2—N31—C33	123.3 (1)	N82—C82—H1C82	127.0
C31—N31—C33	105.0 (1)	C83—C82—H1C82	127.0
C31—N32—C32	107.7 (1)	N81—C83—H1C83	125.0
N31—C31—N32	111.4 (1)	C82—C83—H1C83	125.0

Symmetry codes: (i) −x+2, −y+1/2, z; (ii) −x+1, −y+3/2, z; (iii) −x+2, −y+1, −z+1; (iv) −x+1, −y+1, −z+1; (v) y+1/4, −x+5/4, z+1/4; (vi) −y+5/4, x−1/4, z−1/4; (vii) −y+7/4, x−1/4, −z+3/4; (viii) −y+3/4, x−1/4, −z+3/4; (ix) y−1/4, −x+5/4, −z+5/4; (x) x, y−1/2, −z+1; (xi) y+1/4, −x+3/4, −z+3/4; (xii) x, y+1/2, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N12—H1N12···O12^vi	0.86	1.98	2.779 (2)	155
N32—H1N32···O11^xi	0.86	2.09	2.903 (2)	158
N42—H1N42···O3^v	0.86	2.00	2.794 (2)	153
N52—H1N52···O6^vi	0.86	1.95	2.780 (2)	162
N62—H1N62···O9^v	0.86	2.04	2.868 (2)	162
N72—H1N72···O5^xiii	0.86	2.01	2.785 (2)	149
N82—H1N82···O9^v	0.86	1.92	2.768 (2)	168
C51—H1C51···O3	0.93	2.43	3.344 (2)	167

Symmetry codes: (v) y+1/4, −x+5/4, z+1/4; (vi) −y+5/4, x−1/4, z−1/4; (xi) y+1/4, −x+3/4, −z+3/4; (xiii) y+1/4, −x+7/4, −z+3/4.

catena-tetrakis(imidazole)-tetrakis(µ₂-oxo)-dioxo-manganese(ii)-di-vanadium (Mn_279K)

Crystal data

[Mn(C3H4N2)4V2O6]	Dx = 1.767 Mg m^−3
Mr = 525.13	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I41/a	Cell parameters from 62920 reflections
Hall symbol: -I 4ad	θ = 2.6–30.0°
a = 23.0645 (3) Å	µ = 1.61 mm^−1
c = 29.6897 (3) Å	T = 279 K
V = 15794.1 (3) Å^3	Hexagonal, orange-yellow
Z = 32	0.16 × 0.14 × 0.09 mm
F(000) = 8416.0

Data collection

Enraf-Nonius KappaCCD diffractometer	11539 independent reflections
Radiation source: fine-focus sealed tube	6608 reflections with I > 3σ(I)
Graphite monochromator	Rint = 0.059
φ scan plus ω scans with κ offsets	θmax = 30.0°, θmin = 2.6°
Absorption correction: multi-scan from symmetry-related measurements Sortav (Blessing 1995)	h = −32→30
Tmin = 0.707, Tmax = 0.765	k = −32→32
109552 measured reflections	l = −41→41

Refinement

Refinement on F	2 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.035	w = 1/[σ(F)^2 + (0.0004F)^2]
wR(F^2) = 0.050	(Δ/σ)max = 0.2
S = 1.56	Δρmax = 1.08 e Å^−3
6608 reflections	Δρmin = −0.70 e Å^−3
317 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mn1	0.74985 (2)	0.49629 (2)	0.45160 (1)	0.0212 (1)
Mn2	1.00000	0.25000	0.48963 (2)	0.0204 (1)
Mn3	0.50000	0.75000	0.48515 (2)	0.0198 (1)
V1	0.91264 (2)	0.51347 (2)	0.44945 (1)	0.0198 (1)
V2	0.98625 (2)	0.41112 (2)	0.49609 (1)	0.0199 (1)
V3	0.58389 (2)	0.48421 (2)	0.44632 (1)	0.0187 (1)
V4	0.51489 (2)	0.58994 (2)	0.49500 (1)	0.0192 (1)
O1	0.84353 (7)	0.50156 (8)	0.45945 (6)	0.0350 (5)
O2	0.94384 (7)	0.55691 (8)	0.49321 (6)	0.0311 (4)
O3	0.91898 (9)	0.54472 (9)	0.40052 (6)	0.0432 (5)
O4	0.99535 (8)	0.34231 (7)	0.48427 (6)	0.0338 (4)
O5	0.95209 (8)	0.44533 (7)	0.44817 (5)	0.0298 (4)
O6	0.94448 (8)	0.41747 (8)	0.54010 (6)	0.0398 (5)
O7	0.65359 (8)	0.49202 (8)	0.45375 (6)	0.0370 (5)
O8	0.55473 (7)	0.44044 (8)	0.49080 (5)	0.0294 (4)
O9	0.57378 (9)	0.45571 (8)	0.39623 (6)	0.0417 (5)
O10	0.50663 (8)	0.65793 (7)	0.48062 (6)	0.0333 (4)
O11	0.54707 (8)	0.55332 (7)	0.44721 (5)	0.0302 (4)
O12	0.55692 (8)	0.58593 (8)	0.53880 (6)	0.0396 (5)
N11	0.76188 (8)	0.43075 (7)	0.39550 (5)	0.0312 (6)
N12	0.74156 (9)	0.36386 (8)	0.34542 (6)	0.0455 (7)
C11	0.72290 (8)	0.39347 (9)	0.38146 (6)	0.0397 (7)
C12	0.79525 (9)	0.38278 (9)	0.33554 (6)	0.0448 (7)
C13	0.80760 (8)	0.42401 (9)	0.36650 (7)	0.0394 (7)
N21A	0.74433 (7)	0.41757 (7)	0.49627 (6)	0.0366 (6)	0.439 (12)
N22A	0.7105 (3)	0.33464 (11)	0.52111 (13)	0.0725 (11)	0.439 (12)
C21A	0.69900 (15)	0.38326 (16)	0.49804 (11)	0.0509 (8)	0.439 (12)
C22A	0.7659 (4)	0.33744 (17)	0.53501 (11)	0.0992 (11)	0.439 (12)
C23A	0.78662 (17)	0.3886 (2)	0.51962 (9)	0.0841 (9)	0.439 (12)
N21B	0.74433 (7)	0.41757 (7)	0.49627 (6)	0.0366 (6)	0.561
N22B	0.7757 (3)	0.34315 (17)	0.53530 (11)	0.1053 (12)	0.561
C21B	0.78875 (14)	0.39498 (18)	0.51759 (9)	0.0825 (9)	0.561
C22B	0.7201 (3)	0.33145 (10)	0.52502 (13)	0.0755 (11)	0.561
C23B	0.70094 (15)	0.37744 (15)	0.50096 (11)	0.0523 (8)	0.561
N31	0.92382 (7)	0.24796 (7)	0.44121 (5)	0.0297 (5)
N32	0.86112 (9)	0.22776 (9)	0.38792 (6)	0.0470 (7)
C31	0.91164 (8)	0.21354 (8)	0.40732 (6)	0.0370 (6)
C32	0.83939 (8)	0.27362 (10)	0.41026 (7)	0.0501 (6)
C33	0.87819 (9)	0.28592 (8)	0.44308 (7)	0.0398 (6)
N41	0.93336 (7)	0.24365 (8)	0.54508 (5)	0.0316 (5)
N42	0.87585 (8)	0.26760 (9)	0.60090 (6)	0.0465 (5)
C41	0.92011 (9)	0.28393 (8)	0.57454 (6)	0.0418 (5)
C42	0.85951 (9)	0.21413 (10)	0.58798 (8)	0.0538 (7)
C43	0.89509 (10)	0.19954 (8)	0.55356 (7)	0.0508 (5)
N51	0.74160 (8)	0.56160 (7)	0.39517 (5)	0.0308 (6)
N52	0.76263 (9)	0.61793 (9)	0.33794 (6)	0.0524 (7)
C51	0.78348 (7)	0.58506 (10)	0.37145 (7)	0.0507 (7)
C52	0.70440 (10)	0.61577 (10)	0.33994 (7)	0.0491 (8)
C53	0.69164 (7)	0.58099 (10)	0.37527 (7)	0.0478 (8)
N61	0.74542 (9)	0.56833 (8)	0.50066 (6)	0.0351 (7)
N62	0.73109 (10)	0.62069 (10)	0.56132 (6)	0.0570 (9)
C61	0.72658 (11)	0.56814 (9)	0.54236 (7)	0.0574 (10)
C62	0.75395 (14)	0.65680 (8)	0.53048 (9)	0.0783 (13)
C63	0.76271 (13)	0.62433 (9)	0.49314 (7)	0.0807 (14)
N71	0.57508 (7)	0.75233 (7)	0.43585 (5)	0.0295 (6)
N72	0.63575 (8)	0.77816 (9)	0.38261 (6)	0.0454 (6)
C71	0.58569 (8)	0.78984 (8)	0.40366 (6)	0.0379 (6)
C72	0.65884 (8)	0.73078 (10)	0.40203 (7)	0.0479 (8)
C73	0.62129 (9)	0.71501 (8)	0.43483 (7)	0.0407 (7)
N81	0.56625 (8)	0.75859 (8)	0.54031 (5)	0.0335 (6)
N82	0.63096 (8)	0.74057 (9)	0.59261 (6)	0.0440 (7)
C81	0.60568 (9)	0.72195 (8)	0.55462 (6)	0.0452 (7)
C82	0.60683 (10)	0.79177 (9)	0.60355 (6)	0.0466 (7)
C83	0.56696 (9)	0.80271 (8)	0.57122 (7)	0.0473 (8)
H1N12	0.72261	0.33750	0.33117	0.056
H1C11	0.68682	0.38824	0.39484	0.049
H1C12	0.81900	0.37011	0.31221	0.055
H1C13	0.84211	0.44477	0.36789	0.049
H1N22A	0.68668	0.30668	0.52612	0.094	0.439
H1C21A	0.66336	0.39164	0.48493	0.075	0.439
H1C22A	0.78593	0.30985	0.55175	0.151	0.439
H1C23A	0.82412	0.40221	0.52422	0.132	0.439
H1N22B	0.79868	0.32130	0.55051	0.159	0.561
H1C21B	0.82481	0.41273	0.52010	0.126	0.561
H1C22B	0.69912	0.29851	0.53284	0.098	0.561
H1C23B	0.66372	0.38127	0.48929	0.077	0.561
H1N32	0.84542	0.21064	0.36527	0.056
H1C31	0.93512	0.18308	0.39792	0.042
H1C32	0.80480	0.29291	0.40436	0.064
H1C33	0.87443	0.31581	0.46390	0.046
H1N42	0.86062	0.28769	0.62224	0.059
H1C41	0.93906	0.31940	0.57684	0.061
H1C42	0.82986	0.19178	0.60020	0.074
H1C43	0.89376	0.16463	0.53792	0.076
H1N52	0.78285	0.63699	0.31862	0.073
H1C51	0.82274	0.57956	0.37718	0.083
H1C52	0.67828	0.63436	0.32094	0.067
H1C53	0.65434	0.57160	0.38469	0.078
H1N62	0.72115	0.62970	0.58834	0.079
H1C61	0.71194	0.53561	0.55695	0.111
H1C62	0.76206	0.69603	0.53409	0.126
H1C63	0.77822	0.63804	0.46626	0.149
H1N72	0.65048	0.79749	0.36064	0.055
H1C71	0.56148	0.82069	0.39636	0.047
H1C72	0.69349	0.71261	0.39447	0.062
H1C73	0.62613	0.68341	0.45392	0.052
H1N82	0.65779	0.72295	0.60735	0.055
H1C81	0.61493	0.68738	0.54020	0.069
H1C82	0.61572	0.81490	0.62826	0.062
H1C83	0.54345	0.83543	0.57012	0.071

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mn1	0.0197 (2)	0.0236 (2)	0.0203 (2)	−0.0022 (2)	0.0014 (1)	−0.0006 (1)
Mn2	0.0227 (3)	0.0172 (3)	0.0213 (3)	0.0013 (2)	0.0000 (1)	0.0000 (1)
Mn3	0.0224 (3)	0.0170 (3)	0.0198 (3)	0.0023 (2)	0.0000 (1)	0.0000 (1)
V1	0.0180 (2)	0.0190 (2)	0.0223 (2)	−0.0003 (2)	−0.0021 (2)	0.0001 (2)
V2	0.0202 (2)	0.0157 (2)	0.0236 (2)	0.0005 (2)	0.0000 (2)	−0.0033 (2)
V3	0.0179 (2)	0.0186 (2)	0.0197 (2)	−0.0007 (2)	0.0044 (2)	−0.0008 (2)
V4	0.0216 (2)	0.0158 (2)	0.0202 (2)	0.0010 (2)	0.0016 (2)	0.0027 (2)
O1	0.0208 (10)	0.0410 (12)	0.0432 (11)	−0.0045 (9)	−0.0021 (8)	−0.0084 (9)
O2	0.0261 (10)	0.0309 (11)	0.0362 (10)	−0.0034 (8)	−0.0025 (8)	−0.0105 (8)
O3	0.0484 (13)	0.0466 (13)	0.0346 (11)	−0.0071 (10)	−0.0062 (9)	0.0167 (9)
O4	0.0368 (11)	0.0168 (9)	0.0479 (12)	0.0026 (8)	−0.0069 (9)	−0.0040 (8)
O5	0.0372 (11)	0.0256 (10)	0.0267 (10)	0.0078 (8)	−0.0044 (8)	−0.0051 (7)
O6	0.0432 (13)	0.0401 (12)	0.0361 (11)	0.0037 (10)	0.0162 (9)	−0.0014 (9)
O7	0.0199 (10)	0.0384 (12)	0.0526 (13)	−0.0024 (9)	0.0044 (8)	0.0108 (9)
O8	0.0275 (10)	0.0318 (11)	0.0289 (10)	−0.0025 (8)	0.0048 (8)	0.0066 (8)
O9	0.0574 (14)	0.0427 (12)	0.0250 (10)	−0.0156 (10)	0.0096 (9)	−0.0111 (8)
O10	0.0407 (12)	0.0195 (10)	0.0397 (11)	0.0045 (8)	0.0096 (9)	0.0055 (8)
O11	0.0370 (11)	0.0269 (10)	0.0267 (10)	0.0104 (8)	0.0074 (8)	0.0037 (7)
O12	0.0427 (12)	0.0435 (12)	0.0325 (11)	0.0029 (10)	−0.0126 (9)	−0.0005 (9)
N11	0.0327 (9)	0.0333 (9)	0.0276 (8)	−0.0043 (7)	0.0005 (6)	−0.0037 (6)
N12	0.0570 (12)	0.0422 (9)	0.0372 (9)	−0.0035 (8)	−0.0038 (8)	−0.0130 (7)
C11	0.0426 (9)	0.0395 (10)	0.0370 (9)	−0.0094 (8)	−0.0011 (7)	−0.0108 (7)
C12	0.0558 (12)	0.0457 (11)	0.0328 (8)	0.0034 (9)	0.0032 (8)	−0.0100 (8)
C13	0.0406 (10)	0.0446 (11)	0.0332 (9)	−0.0018 (8)	0.0066 (8)	−0.0083 (8)
N21A	0.0415 (10)	0.0408 (10)	0.0274 (10)	0.0039 (8)	0.0021 (8)	0.0069 (7)
N22A	0.0880 (19)	0.0534 (10)	0.0761 (15)	−0.0060 (10)	0.0100 (14)	0.0289 (9)
C21A	0.0546 (11)	0.0476 (11)	0.0504 (13)	−0.0067 (9)	0.0061 (10)	0.0141 (9)
C22A	0.093 (2)	0.0818 (13)	0.1231 (19)	0.0050 (13)	−0.0089 (17)	0.0692 (14)
C23A	0.0652 (13)	0.0834 (14)	0.1038 (18)	−0.0010 (11)	−0.0233 (13)	0.0612 (14)
N21B	0.0415 (10)	0.0408 (10)	0.0274 (10)	0.0039 (8)	0.0021 (8)	0.0069 (7)
N22B	0.0909 (19)	0.0902 (15)	0.135 (2)	0.0042 (14)	−0.0158 (18)	0.0785 (15)
C21B	0.0627 (12)	0.0834 (15)	0.1015 (18)	−0.0021 (10)	−0.0248 (13)	0.0600 (14)
C22B	0.091 (2)	0.0552 (10)	0.0805 (16)	−0.0026 (10)	0.0094 (14)	0.0332 (10)
C23B	0.0579 (11)	0.0475 (11)	0.0515 (13)	−0.0065 (9)	0.0067 (10)	0.0148 (8)
N31	0.0332 (8)	0.0277 (10)	0.0281 (8)	0.0023 (7)	−0.0022 (6)	−0.0028 (6)
N32	0.0473 (9)	0.0581 (13)	0.0357 (9)	−0.0169 (8)	−0.0127 (7)	0.0100 (7)
C31	0.0450 (9)	0.0382 (10)	0.0278 (9)	−0.0082 (7)	−0.0056 (7)	−0.0031 (7)
C32	0.0375 (8)	0.0613 (15)	0.0514 (12)	−0.0016 (7)	−0.0124 (8)	0.0159 (9)
C33	0.0336 (9)	0.0412 (11)	0.0447 (10)	0.0087 (7)	−0.0052 (7)	0.0035 (7)
N41	0.0328 (9)	0.0319 (10)	0.0300 (8)	−0.0021 (7)	0.0041 (7)	−0.0026 (7)
N42	0.0494 (10)	0.0497 (11)	0.0404 (9)	0.0048 (8)	0.0172 (8)	−0.0003 (7)
C41	0.0491 (11)	0.0389 (9)	0.0374 (9)	−0.0013 (8)	0.0144 (8)	−0.0071 (7)
C42	0.0512 (11)	0.0576 (13)	0.0525 (12)	−0.0099 (10)	0.0234 (9)	−0.0025 (9)
C43	0.0535 (12)	0.0463 (10)	0.0526 (11)	−0.0174 (9)	0.0232 (9)	−0.0093 (8)
N51	0.0343 (10)	0.0309 (9)	0.0273 (8)	−0.0030 (8)	0.0034 (7)	0.0012 (7)
N52	0.0600 (11)	0.0543 (11)	0.0429 (9)	−0.0056 (10)	0.0054 (9)	0.0202 (8)
C51	0.0429 (8)	0.0609 (12)	0.0482 (10)	−0.0086 (9)	0.0056 (8)	0.0252 (9)
C52	0.0588 (11)	0.0490 (11)	0.0395 (10)	0.0026 (11)	−0.0017 (9)	0.0141 (8)
C53	0.0412 (8)	0.0570 (12)	0.0451 (10)	0.0036 (9)	0.0003 (8)	0.0194 (9)
N61	0.0365 (13)	0.0373 (9)	0.0314 (9)	−0.0051 (8)	0.0053 (8)	−0.0058 (7)
N62	0.0635 (16)	0.0617 (11)	0.0458 (9)	0.0048 (10)	0.0021 (9)	−0.0245 (9)
C61	0.0741 (18)	0.0588 (10)	0.0392 (9)	−0.0153 (10)	0.0230 (9)	−0.0180 (7)
C62	0.137 (3)	0.0437 (9)	0.0544 (13)	−0.0057 (10)	−0.0013 (14)	−0.0185 (9)
C63	0.155 (3)	0.0387 (10)	0.0484 (11)	−0.0269 (10)	0.0193 (12)	−0.0111 (8)
N71	0.0315 (8)	0.0301 (10)	0.0269 (8)	0.0015 (7)	0.0017 (6)	0.0019 (7)
N72	0.0449 (9)	0.0581 (12)	0.0332 (8)	−0.0149 (8)	0.0108 (7)	−0.0065 (7)
C71	0.0434 (9)	0.0410 (10)	0.0292 (9)	−0.0055 (7)	0.0063 (7)	0.0055 (7)
C72	0.0361 (8)	0.0623 (15)	0.0454 (11)	−0.0021 (7)	0.0110 (8)	−0.0129 (8)
C73	0.0339 (9)	0.0451 (11)	0.0431 (10)	0.0088 (8)	0.0067 (7)	−0.0015 (7)
N81	0.0380 (9)	0.0324 (10)	0.0301 (8)	0.0049 (7)	−0.0062 (7)	−0.0003 (6)
N82	0.0424 (10)	0.0543 (12)	0.0352 (9)	0.0052 (8)	−0.0109 (7)	0.0024 (7)
C81	0.0463 (10)	0.0505 (11)	0.0389 (9)	0.0173 (9)	−0.0139 (8)	−0.0053 (8)
C82	0.0566 (13)	0.0460 (12)	0.0373 (9)	−0.0009 (9)	−0.0167 (9)	−0.0018 (8)
C83	0.0634 (13)	0.0368 (10)	0.0418 (10)	0.0079 (8)	−0.0214 (9)	−0.0079 (7)

Geometric parameters (Å, º)

Mn1—O1	2.177 (2)	N42—C42	1.345 (2)
Mn1—O7	2.223 (2)	C42—C43	1.353 (2)
Mn1—N11	2.266 (1)	N51—C51	1.312 (1)
Mn1—N21A	2.252 (2)	N51—C53	1.370 (1)
Mn1—N21B	2.252 (2)	N52—C51	1.340 (1)
Mn1—N51	2.261 (1)	N52—C52	1.345 (2)
Mn1—N61	2.212 (1)	C52—C53	1.353 (2)
Mn2—O4	2.138 (2)	N61—C61	1.312 (1)
Mn2—O4^i	2.138 (2)	N61—C63	1.370 (1)
Mn2—N31	2.271 (1)	N62—C61	1.340 (1)
Mn2—N31^i	2.271 (1)	N62—C62	1.345 (2)
Mn2—N41	2.257 (1)	C62—C63	1.353 (2)
Mn2—N41^i	2.257 (1)	N71—C71	1.312 (1)
Mn3—O10	2.134 (2)	N71—C73	1.370 (1)
Mn3—O10^ii	2.133 (2)	N72—C71	1.340 (1)
Mn3—N71	2.276 (1)	N72—C72	1.345 (2)
Mn3—N71^ii	2.260 (1)	C72—C73	1.353 (2)
Mn3—N81	2.256 (1)	N81—C81	1.312 (1)
Mn3—N81^ii	2.242 (1)	N81—C83	1.370 (1)
V1—O1	1.645 (2)	N82—C81	1.340 (1)
V1—O2	1.792 (2)	N82—C82	1.345 (2)
V1—O3	1.628 (2)	C82—C83	1.353 (2)
V1—O5	1.816 (2)	N12—H1N12	0.860
V2—O2^iii	1.801 (2)	C11—H1C11	0.930
V2—O4	1.639 (2)	C12—H1C12	0.930
V2—O5	1.808 (2)	C13—H1C13	0.930
V2—O6	1.630 (2)	N22A—H1N22A	0.860
V3—O7	1.633 (2)	C21A—H1C21A	0.930
V3—O8	1.793 (2)	C22A—H1C22A	0.930
V3—O9	1.643 (2)	C23A—H1C23A	0.930
V3—O11	1.806 (2)	N22B—H1N22B	0.860
V4—O8^iv	1.802 (2)	C21B—H1C21B	0.930
V4—O10	1.636 (2)	C22B—H1C22B	0.930
V4—O11	1.810 (2)	C23B—H1C23B	0.930
V4—O12	1.625 (2)	N32—H1N32	0.860
N11—C11	1.312 (1)	C31—H1C31	0.930
N11—C13	1.370 (1)	C32—H1C32	0.930
N12—C11	1.340 (1)	C33—H1C33	0.930
N12—C12	1.345 (2)	N42—H1N42	0.860
C12—C13	1.353 (2)	C41—H1C41	0.930
N21A—C21A	1.312 (1)	C42—H1C42	0.930
N21A—C23A	1.370 (1)	C43—H1C43	0.930
N22A—C21A	1.340 (1)	N52—H1N52	0.860
N22A—C22A	1.345 (2)	C51—H1C51	0.930
C22A—C23A	1.353 (2)	C52—H1C52	0.930
N21B—C21B	1.312 (1)	C53—H1C53	0.930
N21B—C23B	1.370 (1)	N62—H1N62	0.860
N22B—C21B	1.340 (1)	C61—H1C61	0.930
N22B—C22B	1.345 (2)	C62—H1C62	0.930
C22B—C23B	1.353 (2)	C63—H1C63	0.930
N31—C31	1.312 (1)	N72—H1N72	0.860
N31—C33	1.370 (1)	C71—H1C71	0.930
N32—C31	1.340 (1)	C72—H1C72	0.930
N32—C32	1.345 (2)	C73—H1C73	0.930
C32—C33	1.353 (2)	N82—H1N82	0.860
N41—C41	1.312 (1)	C81—H1C81	0.930
N41—C43	1.370 (1)	C82—H1C82	0.930
N42—C41	1.340 (1)	C83—H1C83	0.930
O1—Mn1—O7	172.2 (1)	N32—C32—C33	105.9 (1)
O1—Mn1—N11	89.7 (1)	N31—C33—C32	110.2 (1)
O1—Mn1—N21A	92.2 (1)	Mn2—N41—C41	126.8 (1)
O1—Mn1—N21B	92.2 (1)	Mn2—N41—C43	128.4 (1)
O1—Mn1—N51	97.2 (1)	C41—N41—C43	104.7 (1)
O1—Mn1—N61	86.2 (1)	C41—N42—C42	107.7 (1)
O7—Mn1—N11	96.5 (1)	N41—C41—N42	111.6 (1)
O7—Mn1—N21A	83.7 (1)	N42—C42—C43	105.9 (1)
O7—Mn1—N21B	83.7 (1)	N41—C43—C42	110.2 (1)
O7—Mn1—N51	88.1 (1)	Mn1—N51—C51	127.6 (1)
O7—Mn1—N61	88.2 (1)	Mn1—N51—C53	127.4 (1)
N11—Mn1—N21A	84.4 (1)	C51—N51—C53	104.7 (1)
N11—Mn1—N21B	84.4 (1)	C51—N52—C52	107.7 (1)
N11—Mn1—N51	84.8 (1)	N51—C51—N52	111.6 (1)
N11—Mn1—N61	172.2 (1)	N52—C52—C53	105.9 (1)
N21A—Mn1—N51	165.6 (1)	N51—C53—C52	110.2 (1)
N21A—Mn1—N61	102.4 (1)	Mn1—N61—C61	129.4 (1)
N21A—Mn1—N21B	0.0 (1)	Mn1—N61—C63	126.0 (1)
N51—Mn1—N61	89.1 (1)	C61—N61—C63	104.7 (1)
N51—Mn1—N21B	165.6 (1)	C61—N62—C62	107.7 (1)
N61—Mn1—N21B	102.4 (1)	N61—C61—N62	111.6 (1)
O4—Mn2—O4^i	171.5 (1)	N62—C62—C63	105.9 (1)
O4—Mn2—N31	86.3 (1)	N61—C63—C62	110.2 (1)
O4—Mn2—N31^i	88.3 (1)	Mn3—N71—C71	128.8 (1)
O4—Mn2—N41	94.9 (1)	Mn3—N71—C73	126.5 (1)
O4—Mn2—N41^i	91.4 (1)	C71—N71—C73	104.7 (1)
O4^i—Mn2—N31	88.3 (1)	C71—N72—C72	107.7 (1)
O4^i—Mn2—N31^i	86.3 (1)	N71—C71—N72	111.6 (1)
O4^i—Mn2—N41	91.4 (1)	N72—C72—C73	105.9 (1)
O4^i—Mn2—N41^i	94.9 (1)	N71—C73—C72	110.2 (1)
N31—Mn2—N31^i	101.4 (1)	Mn3—N81—C81	130.6 (1)
N31—Mn2—N41	86.2 (1)	Mn3—N81—C83	124.0 (1)
N31—Mn2—N41^i	171.9 (1)	C81—N81—C83	104.7 (1)
N31^i—Mn2—N41	171.9 (1)	C81—N82—C82	107.7 (1)
N31^i—Mn2—N41^i	86.2 (1)	N81—C81—N82	111.6 (1)
N41—Mn2—N41^i	86.3 (1)	N82—C82—C83	105.9 (1)
O10—Mn3—O10^ii	172.8 (1)	N81—C83—C82	110.2 (1)
O10—Mn3—N71	85.7 (1)	C11—N12—H1N12	126.1
O10—Mn3—N71^ii	89.6 (1)	C12—N12—H1N12	126.1
O10—Mn3—N81	94.7 (1)	N11—C11—H1C11	124.2
O10—Mn3—N81^ii	90.6 (1)	N12—C11—H1C11	124.2
O10^ii—Mn3—N71	89.3 (1)	N12—C12—H1C12	127.1
O10^ii—Mn3—N71^ii	86.1 (1)	C13—C12—H1C12	127.1
O10^ii—Mn3—N81	90.2 (1)	N11—C13—H1C13	124.9
O10^ii—Mn3—N81^ii	95.1 (1)	C12—C13—H1C13	124.9
N71—Mn3—N71^ii	99.6 (1)	C21A—N22A—H1N22A	126.1
N71—Mn3—N81	86.7 (1)	C22A—N22A—H1N22A	126.1
N71—Mn3—N81^ii	172.0 (1)	N21A—C21A—H1C21A	124.2
N71^ii—Mn3—N81	172.6 (1)	N22A—C21A—H1C21A	124.2
N71^ii—Mn3—N81^ii	87.4 (1)	N22A—C22A—H1C22A	127.1
N81—Mn3—N81^ii	86.5 (1)	C23A—C22A—H1C22A	127.1
O1—V1—O2	110.6 (1)	N21A—C23A—H1C23A	124.9
O1—V1—O3	108.8 (1)	C22A—C23A—H1C23A	124.9
O1—V1—O5	110.2 (1)	C21B—N22B—H1N22B	126.1
O2—V1—O3	111.3 (1)	C22B—N22B—H1N22B	126.1
O2—V1—O5	107.3 (1)	N21B—C21B—H1C21B	124.2
O3—V1—O5	108.6 (1)	N22B—C21B—H1C21B	124.2
O2^iii—V2—O4	108.6 (1)	N22B—C22B—H1C22B	127.1
O2^iii—V2—O5	110.5 (1)	C23B—C22B—H1C22B	127.1
O2^iii—V2—O6	110.5 (1)	N21B—C23B—H1C23B	124.9
O4—V2—O5	108.1 (1)	C22B—C23B—H1C23B	124.9
O4—V2—O6	109.5 (1)	C31—N32—H1N32	126.1
O5—V2—O6	109.5 (1)	C32—N32—H1N32	126.1
O7—V3—O8	109.4 (1)	N31—C31—H1C31	124.2
O7—V3—O9	107.8 (1)	N32—C31—H1C31	124.2
O7—V3—O11	111.3 (1)	N32—C32—H1C32	127.1
O8—V3—O9	112.8 (1)	C33—C32—H1C32	127.1
O8—V3—O11	108.1 (1)	N31—C33—H1C33	124.9
O9—V3—O11	107.4 (1)	C32—C33—H1C33	124.9
O8^iv—V4—O10	109.3 (1)	C41—N42—H1N42	126.1
O8^iv—V4—O11	111.6 (1)	C42—N42—H1N42	126.1
O8^iv—V4—O12	108.8 (1)	N41—C41—H1C41	124.2
O10—V4—O11	106.9 (1)	N42—C41—H1C41	124.2
O10—V4—O12	109.4 (1)	N42—C42—H1C42	127.1
O11—V4—O12	110.9 (1)	C43—C42—H1C42	127.1
Mn1—O1—V1	162.2 (1)	N41—C43—H1C43	124.9
V1—O2—V2^iii	135.7 (1)	C42—C43—H1C43	124.9
Mn2—O4—V2	162.7 (1)	C51—N52—H1N52	126.1
V1—O5—V2	125.4 (1)	C52—N52—H1N52	126.1
Mn1—O7—V3	169.8 (1)	N51—C51—H1C51	124.2
V3—O8—V4^iv	136.5 (1)	N52—C51—H1C51	124.2
Mn3—O10—V4	161.1 (1)	N52—C52—H1C52	127.1
V3—O11—V4	128.0 (1)	C53—C52—H1C52	127.1
Mn1—N11—C11	125.9 (1)	N51—C53—H1C53	124.9
Mn1—N11—C13	129.2 (1)	C52—C53—H1C53	124.9
C11—N11—C13	104.7 (1)	C61—N62—H1N62	126.1
C11—N12—C12	107.7 (1)	C62—N62—H1N62	126.1
N11—C11—N12	111.6 (1)	N61—C61—H1C61	124.2
N12—C12—C13	105.9 (1)	N62—C61—H1C61	124.2
N11—C13—C12	110.2 (1)	N62—C62—H1C62	127.1
Mn1—N21A—C21A	123.7 (2)	C63—C62—H1C62	127.1
Mn1—N21A—C23A	130.6 (2)	N61—C63—H1C63	124.9
C21A—N21A—C23A	104.7 (1)	C62—C63—H1C63	124.9
C21A—N22A—C22A	107.7 (1)	C71—N72—H1N72	126.1
N21A—C21A—N22A	111.6 (1)	C72—N72—H1N72	126.1
N22A—C22A—C23A	105.9 (1)	N71—C71—H1C71	124.2
N21A—C23A—C22A	110.2 (1)	N72—C71—H1C71	124.2
Mn1—N21B—C21B	124.1 (2)	N72—C72—H1C72	127.1
Mn1—N21B—C23B	130.2 (2)	C73—C72—H1C72	127.1
C21B—N21B—C23B	104.7 (1)	N71—C73—H1C73	124.9
C21B—N22B—C22B	107.7 (1)	C72—C73—H1C73	124.9
N21B—C21B—N22B	111.6 (1)	C81—N82—H1N82	126.1
N22B—C22B—C23B	105.9 (1)	C82—N82—H1N82	126.1
N21B—C23B—C22B	110.2 (1)	N81—C81—H1C81	124.2
Mn2—N31—C31	131.6 (1)	N82—C81—H1C81	124.2
Mn2—N31—C33	123.7 (1)	N82—C82—H1C82	127.1
C31—N31—C33	104.7 (1)	C83—C82—H1C82	127.1
C31—N32—C32	107.7 (1)	N81—C83—H1C83	124.9
N31—C31—N32	111.6 (1)	C82—C83—H1C83	124.9

Symmetry codes: (i) −x+2, −y+1/2, z; (ii) −x+1, −y+3/2, z; (iii) −x+2, −y+1, −z+1; (iv) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N12—H1N12···O12^v	0.86	1.98	2.783 (2)	156
N32—H1N32···O11^vi	0.86	2.10	2.914 (2)	158
N42—H1N42···O3^vii	0.86	2.00	2.795 (2)	153
N52—H1N52···O6^v	0.86	1.95	2.781 (2)	163
N62—H1N62···O9^vii	0.86	2.06	2.888 (2)	162
N72—H1N72···O5^viii	0.86	2.03	2.801 (2)	149
N82—H1N82···O9^vii	0.86	1.93	2.777 (2)	169
C51—H1C51···O3	0.93	2.46	3.373 (3)	167

Symmetry codes: (v) −y+5/4, x−1/4, z−1/4; (vi) y+1/4, −x+3/4, −z+3/4; (vii) y+1/4, −x+5/4, z+1/4; (viii) y+1/4, −x+7/4, −z+3/4.

catena-tetrakis(imidazole)-tetrakis(µ₂-oxo)-dioxo-manganese(ii)-di-vanadium (Mn_283K)

Crystal data

[Mn(C3H4N2)4V2O6]	Dx = 1.765 Mg m^−3
Mr = 525.13	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P42/n	Cell parameters from 32397 reflections
Hall symbol: -P 4bc	θ = 2.6–30.0°
a = 16.3271 (2) Å	µ = 1.61 mm^−1
c = 14.8304 (2) Å	T = 283 K
V = 3953.40 (9) Å^3	Hexagonal, orange-yellow
Z = 8	0.16 × 0.14 × 0.09 mm
F(000) = 2004.0

Data collection

Enraf-Nonius KappaCCD diffractometer	5769 independent reflections
Radiation source: fine-focus sealed tube	4293 reflections with I > 3σ(I)
Graphite monochromator	Rint = 0.055
φ scan plus ω scans with κ offsets	θmax = 30.0°, θmin = 2.8°
Absorption correction: multi-scan multi-scan from symmetry-related measurements Sortav (Blessing 1995)	h = −22→21
Tmin = 0.678, Tmax = 0.765	k = −22→22
55800 measured reflections	l = −19→20

Refinement

Refinement on F	6 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.048	w = 1/[σ(F)^2 + (0.0004F)^2]
wR(F^2) = 0.075	(Δ/σ)max = 0.2
S = 2.59	Δρmax = 2.14 e Å^−3
4293 reflections	Δρmin = −1.24 e Å^−3
174 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mn1	0.25000	0.75000	0.90361 (4)	0.0244 (2)
N11A	0.1956 (3)	0.6791 (3)	0.7871 (2)	0.0325 (9)	0.500
C11A	0.1301 (4)	0.6969 (4)	0.7408 (4)	0.053 (3)	0.500
N12A	0.1176 (4)	0.6439 (4)	0.6728 (3)	0.051 (3)	0.500
C12A	0.1773 (5)	0.5898 (4)	0.6752 (4)	0.054 (3)	0.500
C13A	0.2259 (4)	0.6108 (4)	0.7454 (4)	0.058 (4)	0.500
N11B	0.1944 (3)	0.6711 (2)	0.7941 (2)	0.0319 (11)	0.500
C11B	0.1196 (3)	0.6743 (4)	0.7634 (3)	0.0413 (18)	0.500
N12B	0.1085 (4)	0.6237 (4)	0.6928 (3)	0.045 (2)	0.500
C12B	0.1785 (5)	0.5866 (4)	0.6773 (4)	0.050 (3)	0.500
C13B	0.2322 (4)	0.6153 (4)	0.7394 (4)	0.049 (3)	0.500
N21A	0.1677 (3)	0.6741 (3)	0.9889 (3)	0.0468 (10)	0.500
C21A	0.0891 (3)	0.6821 (3)	1.0017 (4)	0.066 (2)	0.500
N22A	0.0576 (3)	0.6188 (4)	1.0484 (5)	0.096 (3)	0.500
C22A	0.1180 (5)	0.5682 (3)	1.0665 (5)	0.107 (3)	0.500
C23A	0.1864 (3)	0.6015 (4)	1.0301 (4)	0.077 (3)	0.500
N21B	0.1824 (2)	0.6740 (2)	1.0029 (2)	0.0362 (11)	0.500
C21B	0.1999 (3)	0.6582 (3)	1.0868 (3)	0.061 (2)	0.500
N22B	0.1456 (3)	0.6063 (3)	1.1243 (3)	0.055 (2)	0.500
C22B	0.0911 (4)	0.5880 (4)	1.0622 (4)	0.107 (5)	0.500
C23B	0.1130 (3)	0.6294 (5)	0.9869 (3)	0.120 (6)	0.500
Mn2	0.25000	0.25000	0.97498 (4)	0.0231 (2)
N31	0.17179 (11)	0.32283 (11)	0.87740 (12)	0.0341 (6)
C31	0.12498 (15)	0.29900 (18)	0.81123 (16)	0.0424 (9)
N32	0.08730 (14)	0.36243 (19)	0.77075 (16)	0.0501 (11)
C32	0.11064 (18)	0.42958 (19)	0.8123 (2)	0.0558 (14)
C33	0.16285 (17)	0.40610 (17)	0.87835 (19)	0.0484 (11)
N41	0.17685 (13)	0.30939 (12)	1.08618 (14)	0.0361 (6)
C41	0.1988 (2)	0.3709 (2)	1.1367 (2)	0.105 (3)
N42	0.1398 (2)	0.39200 (17)	1.19570 (19)	0.0649 (14)
C42	0.0776 (2)	0.3423 (3)	1.1828 (3)	0.132 (3)
C43	0.0996 (2)	0.2909 (3)	1.1154 (3)	0.195 (5)
V1	0.42902 (3)	0.60039 (3)	0.89632 (3)	0.0215 (1)
V2	0.39636 (3)	0.42493 (3)	0.99105 (3)	0.0213 (1)
O1	0.34949 (14)	0.66006 (14)	0.91380 (18)	0.0412 (6)
O2	0.50275 (13)	0.61374 (13)	0.98456 (14)	0.0310 (5)
O3	0.46725 (16)	0.62282 (18)	0.79747 (16)	0.0495 (7)
O4	0.33648 (14)	0.34798 (13)	0.96511 (17)	0.0365 (6)
O5	0.39859 (14)	0.49396 (13)	0.89580 (14)	0.0321 (5)
O6	0.36020 (15)	0.47166 (15)	1.07940 (16)	0.0431 (6)
H1C11A	0.09595	0.74111	0.75340	0.096	0.500
H1N12A	0.07795	0.64505	0.63470	0.073	0.500
H1C12A	0.18464	0.54580	0.63624	0.080	0.500
H1C13A	0.27300	0.58292	0.76281	0.105	0.500
H1C11B	0.07884	0.70747	0.78752	0.060	0.500
H1N12B	0.06366	0.61691	0.66324	0.055	0.500
H1C12B	0.18913	0.54823	0.63255	0.069	0.500
H1C13B	0.28671	0.59941	0.74407	0.074	0.500
H1C21A	0.05845	0.72621	0.98092	0.075	0.500
H1N22A	0.00717	0.61265	1.06368	0.123	0.500
H1C22A	0.11448	0.51913	1.09804	0.147	0.500
H1C23A	0.23846	0.57848	1.03282	0.095	0.500
H1C21B	0.24461	0.68018	1.11728	0.146	0.500
H1N22B	0.14643	0.58844	1.17880	0.079	0.500
H1C22B	0.04629	0.55342	1.06882	0.194	0.500
H1C23B	0.08507	0.62770	0.93228	0.247	0.500
H1C31	0.11839	0.24462	0.79402	0.053
H1N32	0.05403	0.35954	0.72590	0.060
H1C32	0.09446	0.48283	0.79893	0.073
H1C33	0.18880	0.44139	0.91845	0.063
H1C41	0.24919	0.39716	1.13243	0.325
H1N42	0.14238	0.43089	1.23470	0.132
H1C42	0.02817	0.34237	1.21395	0.276
H1C43	0.06694	0.24917	1.09229	0.481

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mn1	0.0240 (3)	0.0276 (4)	0.0216 (3)	0.0048 (3)	0.0000 (1)	0.0000 (1)
N11A	0.0384 (18)	0.0361 (15)	0.0232 (9)	0.0046 (9)	−0.0062 (10)	0.0051 (11)
C11A	0.055 (4)	0.061 (4)	0.044 (5)	0.015 (3)	−0.026 (3)	−0.009 (3)
N12A	0.060 (4)	0.062 (4)	0.034 (4)	−0.003 (3)	−0.018 (3)	−0.002 (3)
C12A	0.066 (6)	0.059 (5)	0.039 (4)	0.000 (3)	−0.011 (3)	−0.013 (4)
C13A	0.066 (5)	0.058 (5)	0.052 (6)	0.020 (4)	−0.022 (3)	−0.022 (4)
N11B	0.0360 (16)	0.037 (2)	0.0231 (12)	0.0044 (9)	−0.0045 (13)	0.0042 (11)
C11B	0.040 (2)	0.052 (4)	0.032 (2)	0.0046 (16)	−0.011 (2)	−0.002 (2)
N12B	0.048 (3)	0.058 (3)	0.027 (2)	−0.007 (2)	−0.007 (2)	0.000 (2)
C12B	0.051 (6)	0.065 (8)	0.036 (4)	−0.009 (3)	0.002 (5)	−0.015 (5)
C13B	0.044 (6)	0.060 (9)	0.045 (4)	0.004 (2)	−0.003 (5)	−0.019 (5)
N21A	0.0553 (14)	0.047 (2)	0.038 (2)	−0.0034 (12)	0.0071 (11)	0.0101 (10)
C21A	0.0580 (17)	0.070 (4)	0.069 (4)	−0.0133 (19)	0.025 (3)	−0.004 (3)
N22A	0.101 (3)	0.095 (5)	0.095 (5)	−0.039 (3)	0.048 (4)	0.002 (3)
C22A	0.138 (5)	0.086 (5)	0.098 (6)	−0.034 (4)	0.036 (5)	0.038 (4)
C23A	0.099 (3)	0.062 (4)	0.072 (5)	−0.008 (3)	0.010 (4)	0.039 (3)
N21B	0.0447 (17)	0.0371 (16)	0.0270 (15)	0.0034 (12)	−0.0007 (10)	0.0087 (11)
C21B	0.059 (3)	0.087 (4)	0.0359 (19)	−0.008 (3)	−0.0068 (15)	0.033 (2)
N22B	0.070 (4)	0.053 (3)	0.043 (3)	0.008 (3)	0.014 (2)	0.022 (2)
C22B	0.138 (6)	0.136 (7)	0.049 (4)	−0.086 (6)	0.004 (3)	0.021 (5)
C23B	0.132 (5)	0.187 (8)	0.045 (3)	−0.113 (6)	−0.019 (3)	0.036 (4)
Mn2	0.0245 (3)	0.0198 (3)	0.0250 (3)	−0.0027 (2)	0.0000 (1)	0.0000 (1)
N31	0.0345 (9)	0.0351 (9)	0.0327 (8)	−0.0019 (6)	−0.0016 (6)	0.0029 (6)
C31	0.0384 (13)	0.0544 (11)	0.0343 (11)	−0.0021 (9)	−0.0066 (9)	0.0040 (8)
N32	0.0380 (12)	0.0728 (16)	0.0395 (12)	0.0053 (11)	−0.0011 (9)	0.0170 (10)
C32	0.0534 (16)	0.0569 (12)	0.0570 (16)	0.0116 (12)	−0.0017 (12)	0.0208 (11)
C33	0.0552 (16)	0.0362 (9)	0.0539 (15)	0.0048 (9)	−0.0071 (12)	0.0084 (8)
N41	0.0438 (9)	0.0309 (9)	0.0336 (9)	−0.0014 (7)	0.0035 (7)	−0.0044 (7)
C41	0.1084 (19)	0.094 (3)	0.114 (3)	−0.0553 (18)	0.065 (2)	−0.079 (3)
N42	0.103 (2)	0.0377 (15)	0.0544 (13)	−0.0024 (13)	0.0341 (16)	−0.0113 (12)
C42	0.089 (2)	0.170 (5)	0.140 (3)	−0.038 (2)	0.065 (3)	−0.104 (3)
C43	0.103 (2)	0.255 (6)	0.228 (5)	−0.108 (3)	0.113 (3)	−0.198 (5)
V1	0.0203 (3)	0.0203 (3)	0.0240 (3)	0.0004 (2)	−0.0037 (2)	0.0030 (2)
V2	0.0212 (3)	0.0187 (3)	0.0240 (3)	−0.0024 (2)	−0.0030 (2)	−0.0023 (2)
O1	0.0342 (13)	0.0367 (13)	0.0527 (16)	0.0144 (11)	−0.0152 (11)	−0.0064 (11)
O2	0.0257 (11)	0.0330 (12)	0.0342 (12)	0.0024 (9)	−0.0100 (9)	−0.0045 (10)
O3	0.0414 (15)	0.0702 (19)	0.0367 (15)	−0.0084 (14)	0.0010 (11)	0.0205 (13)
O4	0.0330 (13)	0.0264 (12)	0.0500 (15)	−0.0101 (10)	−0.0087 (11)	−0.0001 (10)
O5	0.0411 (13)	0.0245 (11)	0.0308 (12)	−0.0056 (10)	−0.0080 (10)	0.0001 (9)
O6	0.0486 (16)	0.0413 (14)	0.0395 (14)	−0.0008 (11)	0.0118 (12)	−0.0127 (11)

Geometric parameters (Å, º)

Mn1—N11A	2.262 (2)	N32—C32	1.314 (4)
Mn1—N11A^i	2.262 (2)	C32—C33	1.354 (3)
Mn1—N11B	2.263 (2)	N41—C41	1.303 (3)
Mn1—N11B^i	2.263 (2)	N41—C43	1.368 (3)
Mn1—N21A	2.223 (2)	C41—N42	1.346 (3)
Mn1—N21A^i	2.223 (2)	N42—C42	1.314 (4)
Mn1—N21B	2.219 (2)	C42—C43	1.354 (3)
Mn1—N21B^i	2.219 (2)	V1—O1	1.644 (2)
Mn1—O1	2.195 (2)	V1—O2	1.791 (2)
Mn1—O1^i	2.195 (2)	V1—O3	1.635 (2)
N11A—C11A	1.303 (3)	V1—O5	1.807 (2)
N11A—C13A	1.368 (3)	V2—O2^iii	1.801 (2)
C11A—N12A	1.346 (3)	V2—O4	1.638 (2)
N12A—C12A	1.314 (4)	V2—O5	1.807 (2)
C12A—C13A	1.354 (3)	V2—O6	1.627 (2)
N11B—C11B	1.303 (3)	C11A—H1C11A	0.930
N11B—C13B	1.368 (3)	N12A—H1N12A	0.860
C11B—N12B	1.346 (3)	C12A—H1C12A	0.930
N12B—C12B	1.314 (4)	C13A—H1C13A	0.930
C12B—C13B	1.354 (3)	C11B—H1C11B	0.930
N21A—C21A	1.303 (3)	N12B—H1N12B	0.860
N21A—C23A	1.368 (3)	C12B—H1C12B	0.930
C21A—N22A	1.346 (3)	C13B—H1C13B	0.930
N22A—C22A	1.314 (4)	C21A—H1C21A	0.930
C22A—C23A	1.354 (3)	N22A—H1N22A	0.860
N21B—C21B	1.303 (3)	C22A—H1C22A	0.930
N21B—C23B	1.368 (3)	C23A—H1C23A	0.930
C21B—N22B	1.346 (3)	C21B—H1C21B	0.930
N22B—C22B	1.314 (4)	N22B—H1N22B	0.860
C22B—C23B	1.354 (3)	C22B—H1C22B	0.930
Mn2—N31	2.267 (2)	C23B—H1C23B	0.930
Mn2—N31^ii	2.267 (2)	C31—H1C31	0.930
Mn2—N41	2.255 (2)	N32—H1N32	0.860
Mn2—N41^ii	2.255 (2)	C32—H1C32	0.930
Mn2—O4	2.139 (2)	C33—H1C33	0.930
Mn2—O4^ii	2.139 (2)	C41—H1C41	0.930
N31—C31	1.303 (3)	N42—H1N42	0.860
N31—C33	1.368 (3)	C42—H1C42	0.930
C31—N32	1.346 (3)	C43—H1C43	0.930
N11A—Mn1—N11A^i	80.3 (2)	N41—Mn2—O4	94.5 (1)
N11A—Mn1—N11B	4.3 (2)	N41—Mn2—O4^ii	91.3 (1)
N11A—Mn1—N11B^i	84.3 (1)	N41^ii—Mn2—O4	91.3 (1)
N11A—Mn1—N21A	84.9 (2)	N41^ii—Mn2—O4^ii	94.5 (1)
N11A—Mn1—N21A^i	163.2 (2)	O4—Mn2—O4^ii	172.2 (1)
N11A—Mn1—N21B	91.5 (2)	Mn2—N31—C31	130.9 (2)
N11A—Mn1—N21B^i	171.3 (2)	Mn2—N31—C33	125.1 (2)
N11A—Mn1—O1	90.1 (1)	C31—N31—C33	104.0 (2)
N11A—Mn1—O1^i	96.0 (1)	N31—C31—N32	112.0 (2)
N11A^i—Mn1—N11B	84.3 (1)	C31—N32—C32	107.5 (2)
N11A^i—Mn1—N11B^i	4.3 (2)	N32—C32—C33	106.6 (2)
N11A^i—Mn1—N21A	163.2 (2)	N31—C33—C32	109.9 (2)
N11A^i—Mn1—N21A^i	84.9 (2)	Mn2—N41—C41	127.3 (2)
N11A^i—Mn1—N21B	171.3 (2)	Mn2—N41—C43	128.7 (2)
N11A^i—Mn1—N21B^i	91.5 (2)	C41—N41—C43	104.0 (2)
N11A^i—Mn1—O1	96.0 (1)	N41—C41—N42	112.0 (2)
N11A^i—Mn1—O1^i	90.1 (1)	C41—N42—C42	107.5 (2)
N11B—Mn1—N11B^i	88.3 (2)	N42—C42—C43	106.6 (2)
N11B—Mn1—N21A	81.3 (2)	N41—C43—C42	109.9 (2)
N11B—Mn1—N21A^i	165.5 (2)	O1—V1—O2	110.1 (1)
N11B—Mn1—N21B	87.6 (2)	O1—V1—O3	108.1 (1)
N11B—Mn1—N21B^i	173.7 (2)	O1—V1—O5	110.7 (1)
N11B—Mn1—O1	88.0 (1)	O2—V1—O3	111.8 (1)
N11B—Mn1—O1^i	97.6 (1)	O2—V1—O5	107.8 (1)
N11B^i—Mn1—N21A	165.5 (2)	O3—V1—O5	108.5 (1)
N11B^i—Mn1—N21A^i	81.3 (2)	O2^iii—V2—O4	108.9 (1)
N11B^i—Mn1—N21B	173.7 (2)	O2^iii—V2—O5	110.9 (1)
N11B^i—Mn1—N21B^i	87.6 (2)	O2^iii—V2—O6	109.5 (1)
N11B^i—Mn1—O1	97.6 (1)	O4—V2—O5	107.9 (1)
N11B^i—Mn1—O1^i	88.0 (1)	O4—V2—O6	109.4 (1)
N21A—Mn1—N21A^i	110.6 (2)	O5—V2—O6	110.1 (1)
N21A—Mn1—N21B	8.2 (2)	Mn1—O1—V1	166.0 (2)
N21A—Mn1—N21B^i	103.6 (1)	V1—O2—V2^iii	135.9 (1)
N21A—Mn1—O1	92.0 (1)	Mn2—O4—V2	162.1 (2)
N21A—Mn1—O1^i	83.5 (1)	V1—O5—V2	127.0 (1)
N21A^i—Mn1—N21B	103.6 (1)	N11A—C11A—H1C11A	124.0
N21A^i—Mn1—N21B^i	8.2 (2)	N12A—C11A—H1C11A	124.0
N21A^i—Mn1—O1	83.5 (1)	C11A—N12A—H1N12A	126.3
N21A^i—Mn1—O1^i	92.0 (1)	C12A—N12A—H1N12A	126.3
N21B—Mn1—N21B^i	96.9 (2)	N12A—C12A—H1C12A	126.7
N21B—Mn1—O1	87.0 (1)	C13A—C12A—H1C12A	126.7
N21B—Mn1—O1^i	87.7 (1)	N11A—C13A—H1C13A	125.0
N21B^i—Mn1—O1	87.7 (1)	C12A—C13A—H1C13A	125.0
N21B^i—Mn1—O1^i	87.0 (1)	N11B—C11B—H1C11B	124.0
O1—Mn1—O1^i	172.1 (1)	N12B—C11B—H1C11B	124.0
Mn1—N11A—C11A	127.6 (2)	C11B—N12B—H1N12B	126.3
Mn1—N11A—C13A	128.3 (2)	C12B—N12B—H1N12B	126.3
C11A—N11A—C13A	104.0 (2)	N12B—C12B—H1C12B	126.7
N11A—C11A—N12A	112.0 (2)	C13B—C12B—H1C12B	126.7
C11A—N12A—C12A	107.5 (2)	N11B—C13B—H1C13B	125.0
N12A—C12A—C13A	106.6 (2)	C12B—C13B—H1C13B	125.0
N11A—C13A—C12A	109.9 (2)	N21A—C21A—H1C21A	124.0
Mn1—N11B—C11B	127.1 (2)	N22A—C21A—H1C21A	124.0
Mn1—N11B—C13B	128.6 (2)	C21A—N22A—H1N22A	126.3
C11B—N11B—C13B	104.0 (2)	C22A—N22A—H1N22A	126.3
N11B—C11B—N12B	112.0 (2)	N22A—C22A—H1C22A	126.7
C11B—N12B—C12B	107.5 (2)	C23A—C22A—H1C22A	126.7
N12B—C12B—C13B	106.6 (2)	N21A—C23A—H1C23A	125.0
N11B—C13B—C12B	109.9 (2)	C22A—C23A—H1C23A	125.0
Mn1—N21A—C21A	128.4 (3)	N21B—C21B—H1C21B	124.0
Mn1—N21A—C23A	127.0 (3)	N22B—C21B—H1C21B	124.0
C21A—N21A—C23A	104.0 (2)	C21B—N22B—H1N22B	126.3
N21A—C21A—N22A	112.0 (2)	C22B—N22B—H1N22B	126.3
C21A—N22A—C22A	107.5 (2)	N22B—C22B—H1C22B	126.7
N22A—C22A—C23A	106.6 (2)	C23B—C22B—H1C22B	126.7
N21A—C23A—C22A	109.9 (2)	N21B—C23B—H1C23B	125.0
Mn1—N21B—C21B	129.5 (3)	C22B—C23B—H1C23B	125.0
Mn1—N21B—C23B	126.5 (3)	N31—C31—H1C31	124.0
C21B—N21B—C23B	104.0 (2)	N32—C31—H1C31	124.0
N21B—C21B—N22B	112.0 (2)	C31—N32—H1N32	126.3
C21B—N22B—C22B	107.5 (2)	C32—N32—H1N32	126.3
N22B—C22B—C23B	106.6 (2)	N32—C32—H1C32	126.7
N21B—C23B—C22B	109.9 (2)	C33—C32—H1C32	126.7
N31—Mn2—N31^ii	100.7 (1)	N31—C33—H1C33	125.0
N31—Mn2—N41	86.7 (1)	C32—C33—H1C33	125.0
N31—Mn2—N41^ii	172.2 (1)	N41—C41—H1C41	124.0
N31—Mn2—O4	86.3 (1)	N42—C41—H1C41	124.0
N31—Mn2—O4^ii	88.7 (1)	C41—N42—H1N42	126.3
N31^ii—Mn2—N41	172.2 (1)	C42—N42—H1N42	126.3
N31^ii—Mn2—N41^ii	86.7 (1)	N42—C42—H1C42	126.7
N31^ii—Mn2—O4	88.7 (1)	C43—C42—H1C42	126.7
N31^ii—Mn2—O4^ii	86.3 (1)	N41—C43—H1C43	125.0
N41—Mn2—N41^ii	86.0 (1)	C42—C43—H1C43	125.0

Symmetry codes: (i) −x+1/2, −y+3/2, z; (ii) −x+1/2, −y+1/2, z; (iii) −x+1, −y+1, −z+2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N12A—H1N12A···O6^iv	0.86	1.92	2.758 (5)	164
N12B—H1N12B···O6^iv	0.86	1.99	2.808 (5)	160
N22B—H1N22B···O3^v	0.86	2.02	2.860 (4)	166
N32—H1N32···O5^vi	0.86	2.07	2.865 (3)	154
N42—H1N42···O3^v	0.86	1.93	2.763 (3)	162

Symmetry codes: (iv) y−1/2, −x+1, z−1/2; (v) y−1/2, −x+1, z+1/2; (vi) −y+1/2, x, −z+3/2.

catena-tetrakis(imidazole)-tetrakis(µ₂-oxo)-dioxo-manganese(ii)-di-vanadium (Mn_295K)

Crystal data

[Mn(C3H4N2)4V2O6]	Dx = 1.760 Mg m^−3
Mr = 525.13	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P42/n	Cell parameters from 31642 reflections
Hall symbol: -P 4bc	θ = 2.6–30.0°
a = 16.3615 (2) Å	µ = 1.61 mm^−1
c = 14.8030 (2) Å	T = 295 K
V = 3962.74 (9) Å^3	Hexagonal, orange-yellow
Z = 8	0.16 × 0.14 × 0.09 mm
F(000) = 2004.0

Data collection

Enraf-Nonius KappaCCD diffractometer	5784 independent reflections
Radiation source: fine-focus sealed tube	4271 reflections with I > 3σ(I)
Graphite monochromator	Rint = 0.059
φ scan plus ω scans with κ offsets	θmax = 30.0°, θmin = 2.8°
Absorption correction: multi-scan multi-scan from symmetry-related measurements Sortav (Blessing 1995)	h = −23→16
Tmin = 0.672, Tmax = 0.765	k = −23→16
54609 measured reflections	l = −20→19

Refinement

Refinement on F	6 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.040	w = 1/[σ(F)^2 + (0.0004F)^2]
wR(F^2) = 0.060	(Δ/σ)max = 0.2
S = 2.06	Δρmax = 1.11 e Å^−3
4271 reflections	Δρmin = −0.80 e Å^−3
174 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mn1	0.25000	0.75000	0.90425 (3)	0.0243 (1)
N11A	0.19443 (18)	0.67788 (17)	0.78972 (15)	0.0358 (7)	0.500
C11A	0.1310 (3)	0.6981 (3)	0.7409 (3)	0.063 (3)	0.500
N12A	0.1164 (3)	0.6429 (4)	0.6757 (3)	0.066 (3)	0.500
C12A	0.1725 (4)	0.5847 (3)	0.6825 (3)	0.072 (3)	0.500
C13A	0.2208 (3)	0.6061 (3)	0.7530 (3)	0.072 (3)	0.500
N11B	0.19529 (16)	0.67384 (15)	0.79238 (14)	0.0321 (8)	0.500
C11B	0.1210 (2)	0.6792 (3)	0.7604 (2)	0.046 (2)	0.500
N12B	0.1096 (3)	0.6284 (3)	0.6902 (3)	0.051 (2)	0.500
C12B	0.1791 (3)	0.5887 (3)	0.6761 (3)	0.050 (3)	0.500
C13B	0.2322 (3)	0.6166 (3)	0.7392 (2)	0.047 (3)	0.500
N21A	0.17083 (17)	0.67301 (16)	0.99151 (19)	0.0459 (8)	0.500
C21A	0.0930 (2)	0.6816 (2)	1.0089 (3)	0.072 (2)	0.500
N22A	0.0631 (2)	0.6170 (3)	1.0543 (3)	0.100 (2)	0.500
C22A	0.1239 (3)	0.5647 (2)	1.0668 (3)	0.101 (3)	0.500
C23A	0.1906 (3)	0.5991 (2)	1.0281 (3)	0.074 (2)	0.500
N21B	0.18251 (16)	0.67280 (15)	1.00232 (15)	0.0360 (9)	0.500
C21B	0.1973 (2)	0.6607 (2)	1.08807 (18)	0.070 (2)	0.500
N22B	0.1453 (2)	0.6060 (2)	1.1240 (2)	0.0587 (16)	0.500
C22B	0.0949 (3)	0.5819 (3)	1.0591 (3)	0.118 (5)	0.500
C23B	0.1177 (2)	0.6230 (3)	0.9838 (2)	0.137 (5)	0.500
Mn2	0.25000	0.25000	0.97547 (3)	0.0236 (1)
N31	0.17104 (7)	0.32174 (8)	0.87752 (8)	0.0348 (4)
C31	0.12503 (11)	0.29778 (14)	0.81035 (12)	0.0432 (7)
N32	0.08691 (10)	0.36115 (14)	0.77080 (12)	0.0512 (9)
C32	0.10905 (13)	0.42863 (14)	0.81394 (15)	0.0580 (11)
C33	0.16108 (13)	0.40451 (13)	0.87998 (14)	0.0502 (9)
N41	0.17741 (9)	0.30935 (8)	1.08670 (9)	0.0379 (4)
C41	0.20325 (14)	0.36486 (13)	1.14344 (15)	0.0689 (13)
N42	0.14278 (15)	0.39108 (12)	1.19766 (13)	0.0652 (10)
C42	0.07530 (15)	0.35107 (17)	1.17519 (18)	0.0924 (15)
C43	0.09647 (14)	0.30047 (17)	1.10661 (18)	0.1035 (19)
V1	0.42906 (2)	0.60069 (2)	0.89720 (3)	0.0214 (1)
V2	0.39651 (2)	0.42493 (2)	0.99101 (3)	0.0221 (1)
O1	0.35000 (11)	0.66031 (11)	0.91484 (14)	0.0405 (5)
O2	0.50269 (10)	0.61384 (11)	0.98573 (11)	0.0318 (4)
O3	0.46749 (12)	0.62361 (14)	0.79872 (12)	0.0494 (5)
O4	0.33641 (11)	0.34803 (10)	0.96530 (13)	0.0364 (4)
O5	0.39854 (11)	0.49417 (11)	0.89618 (11)	0.0345 (4)
O6	0.36119 (12)	0.47124 (12)	1.07987 (13)	0.0453 (5)
H1C11A	0.09989	0.74497	0.75010	0.115	0.500
H1N12A	0.07769	0.64489	0.63648	0.096	0.500
H1C12A	0.17758	0.53848	0.64634	0.111	0.500
H1C13A	0.26552	0.57620	0.77336	0.132	0.500
H1C11B	0.08102	0.71385	0.78342	0.068	0.500
H1N12B	0.06520	0.62272	0.65975	0.067	0.500
H1C12B	0.18932	0.54962	0.63192	0.067	0.500
H1C13B	0.28608	0.59930	0.74534	0.070	0.500
H1C21A	0.06205	0.72679	0.99189	0.093	0.500
H1N22A	0.01348	0.61078	1.07205	0.133	0.500
H1C22A	0.12134	0.51450	1.09620	0.139	0.500
H1C23A	0.24242	0.57566	1.02665	0.095	0.500
H1C21B	0.23870	0.68664	1.12021	0.182	0.500
H1N22B	0.14475	0.58966	1.17917	0.091	0.500
H1C22B	0.05252	0.54430	1.06421	0.220	0.500
H1C23B	0.09286	0.61806	0.92753	0.294	0.500
H1C31	0.11937	0.24365	0.79221	0.054
H1N32	0.05402	0.35841	0.72558	0.061
H1C32	0.09228	0.48174	0.80141	0.077
H1C33	0.18634	0.43933	0.92105	0.066
H1C41	0.25678	0.38384	1.14598	0.149
H1N42	0.14710	0.42733	1.23945	0.098
H1C42	0.02387	0.35661	1.20123	0.156
H1C43	0.06096	0.26485	1.07733	0.209

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mn1	0.0233 (3)	0.0273 (3)	0.0222 (3)	0.0029 (2)	0.0000 (1)	0.0000 (1)
N11A	0.0373 (15)	0.0403 (11)	0.0298 (9)	0.0026 (8)	−0.0078 (8)	0.0004 (9)
C11A	0.057 (3)	0.077 (4)	0.056 (5)	0.016 (3)	−0.033 (3)	−0.018 (2)
N12A	0.067 (4)	0.084 (4)	0.048 (3)	−0.006 (3)	−0.025 (2)	−0.015 (3)
C12A	0.092 (6)	0.070 (4)	0.057 (5)	0.000 (3)	−0.024 (3)	−0.025 (3)
C13A	0.090 (6)	0.060 (4)	0.069 (7)	0.025 (4)	−0.036 (3)	−0.031 (3)
N11B	0.0306 (10)	0.0379 (13)	0.0278 (10)	0.0036 (7)	−0.0046 (8)	0.0011 (7)
C11B	0.036 (2)	0.059 (5)	0.043 (3)	0.0067 (13)	−0.015 (3)	−0.010 (2)
N12B	0.046 (2)	0.068 (3)	0.0395 (18)	−0.005 (2)	−0.0122 (19)	−0.0097 (18)
C12B	0.048 (4)	0.065 (6)	0.040 (4)	−0.010 (2)	0.001 (4)	−0.017 (3)
C13B	0.039 (4)	0.057 (7)	0.046 (4)	0.0028 (16)	−0.002 (4)	−0.019 (3)
N21A	0.0497 (11)	0.0444 (13)	0.0437 (15)	−0.0022 (11)	0.0094 (9)	0.0087 (10)
C21A	0.0570 (14)	0.067 (3)	0.093 (4)	−0.0080 (19)	0.036 (2)	0.005 (3)
N22A	0.098 (3)	0.087 (3)	0.116 (4)	−0.030 (3)	0.058 (3)	0.009 (3)
C22A	0.127 (4)	0.077 (3)	0.102 (5)	−0.026 (3)	0.039 (4)	0.035 (3)
C23A	0.088 (3)	0.058 (3)	0.076 (4)	−0.0045 (18)	0.011 (3)	0.036 (2)
N21B	0.0385 (13)	0.0377 (13)	0.0318 (12)	0.0027 (10)	0.0002 (7)	0.0075 (9)
C21B	0.071 (3)	0.100 (4)	0.0385 (15)	−0.027 (3)	−0.0093 (12)	0.0317 (16)
N22B	0.068 (3)	0.059 (3)	0.049 (2)	0.003 (2)	0.0137 (17)	0.0235 (19)
C22B	0.153 (6)	0.143 (5)	0.059 (3)	−0.100 (5)	0.007 (3)	0.022 (4)
C23B	0.159 (5)	0.201 (6)	0.052 (3)	−0.139 (6)	−0.020 (3)	0.036 (3)
Mn2	0.0252 (3)	0.0210 (3)	0.0245 (3)	−0.0031 (2)	0.0000 (1)	0.0000 (1)
N31	0.0345 (7)	0.0368 (7)	0.0332 (6)	−0.0011 (5)	−0.0024 (5)	0.0018 (4)
C31	0.0385 (10)	0.0553 (8)	0.0358 (8)	−0.0026 (7)	−0.0080 (7)	0.0037 (6)
N32	0.0392 (10)	0.0735 (12)	0.0408 (9)	0.0060 (9)	−0.0031 (7)	0.0153 (8)
C32	0.0594 (14)	0.0588 (9)	0.0558 (12)	0.0157 (10)	−0.0045 (10)	0.0168 (9)
C33	0.0600 (13)	0.0383 (7)	0.0522 (11)	0.0079 (7)	−0.0091 (9)	0.0056 (6)
N41	0.0450 (7)	0.0319 (7)	0.0367 (6)	−0.0029 (5)	0.0057 (5)	−0.0059 (5)
C41	0.0731 (10)	0.0690 (16)	0.0646 (11)	−0.0194 (10)	0.0209 (9)	−0.0409 (13)
N42	0.0943 (15)	0.0460 (12)	0.0553 (10)	−0.0026 (11)	0.0290 (11)	−0.0167 (9)
C42	0.0756 (12)	0.108 (3)	0.0946 (18)	−0.0037 (13)	0.0392 (15)	−0.0480 (16)
C43	0.0562 (9)	0.139 (3)	0.116 (2)	−0.0274 (10)	0.0388 (12)	−0.081 (2)
V1	0.0197 (2)	0.0207 (2)	0.0238 (2)	0.0006 (1)	−0.0023 (1)	0.0027 (1)
V2	0.0211 (2)	0.0191 (2)	0.0260 (2)	−0.0023 (1)	−0.0032 (1)	−0.0023 (1)
O1	0.0312 (10)	0.0373 (11)	0.0530 (12)	0.0124 (8)	−0.0094 (8)	−0.0060 (9)
O2	0.0264 (9)	0.0339 (10)	0.0351 (9)	0.0026 (7)	−0.0093 (7)	−0.0048 (8)
O3	0.0427 (12)	0.0695 (15)	0.0359 (11)	−0.0055 (11)	0.0044 (9)	0.0203 (10)
O4	0.0330 (10)	0.0272 (9)	0.0491 (11)	−0.0095 (8)	−0.0080 (8)	−0.0007 (8)
O5	0.0445 (11)	0.0253 (9)	0.0337 (10)	−0.0067 (8)	−0.0103 (8)	0.0012 (7)
O6	0.0498 (13)	0.0433 (12)	0.0429 (11)	−0.0003 (9)	0.0127 (9)	−0.0143 (9)

Geometric parameters (Å, º)

Mn1—N11A	2.257 (1)	N32—C32	1.326 (3)
Mn1—N11A^i	2.257 (1)	C32—C33	1.355 (3)
Mn1—N11B	2.257 (1)	N41—C41	1.307 (2)
Mn1—N11B^i	2.257 (1)	N41—C43	1.364 (2)
Mn1—N21A	2.221 (2)	C41—N42	1.344 (2)
Mn1—N21A^i	2.221 (2)	N42—C42	1.326 (3)
Mn1—N21B	2.219 (2)	C42—C43	1.355 (3)
Mn1—N21B^i	2.219 (2)	V1—O1	1.641 (2)
Mn1—O1	2.203 (2)	V1—O2	1.793 (2)
Mn1—O1^i	2.203 (2)	V1—O3	1.631 (2)
N11A—C11A	1.307 (2)	V1—O5	1.813 (2)
N11A—C13A	1.364 (2)	V2—O2^iii	1.800 (2)
C11A—N12A	1.344 (2)	V2—O4	1.642 (2)
N12A—C12A	1.326 (3)	V2—O5	1.804 (2)
C12A—C13A	1.355 (3)	V2—O6	1.624 (2)
N11B—C11B	1.307 (2)	C11A—H1C11A	0.930
N11B—C13B	1.364 (2)	N12A—H1N12A	0.860
C11B—N12B	1.344 (2)	C12A—H1C12A	0.930
N12B—C12B	1.326 (3)	C13A—H1C13A	0.930
C12B—C13B	1.355 (3)	C11B—H1C11B	0.930
N21A—C21A	1.307 (2)	N12B—H1N12B	0.860
N21A—C23A	1.364 (2)	C12B—H1C12B	0.930
C21A—N22A	1.344 (2)	C13B—H1C13B	0.930
N22A—C22A	1.326 (3)	C21A—H1C21A	0.930
C22A—C23A	1.355 (3)	N22A—H1N22A	0.860
N21B—C21B	1.307 (2)	C22A—H1C22A	0.930
N21B—C23B	1.364 (2)	C23A—H1C23A	0.930
C21B—N22B	1.344 (2)	C21B—H1C21B	0.930
N22B—C22B	1.326 (3)	N22B—H1N22B	0.860
C22B—C23B	1.355 (3)	C22B—H1C22B	0.930
Mn2—N31	2.269 (1)	C23B—H1C23B	0.930
Mn2—N31^ii	2.269 (1)	C31—H1C31	0.930
Mn2—N41	2.250 (1)	N32—H1N32	0.860
Mn2—N41^ii	2.250 (1)	C32—H1C32	0.930
Mn2—O4	2.143 (2)	C33—H1C33	0.930
Mn2—O4^ii	2.143 (2)	C41—H1C41	0.930
N31—C31	1.307 (2)	N42—H1N42	0.860
N31—C33	1.364 (2)	C42—H1C42	0.930
C31—N32	1.344 (2)	C43—H1C43	0.930
N11A—Mn1—N11A^i	82.6 (2)	N41—Mn2—O4	94.4 (1)
N11A—Mn1—N11B	2.0 (1)	N41—Mn2—O4^ii	91.5 (1)
N11A—Mn1—N11B^i	84.1 (1)	N41^ii—Mn2—O4	91.5 (1)
N11A—Mn1—N21A	84.6 (1)	N41^ii—Mn2—O4^ii	94.4 (1)
N11A—Mn1—N21A^i	165.5 (1)	O4—Mn2—O4^ii	171.9 (1)
N11A—Mn1—N21B	89.6 (1)	Mn2—N31—C31	131.2 (1)
N11A—Mn1—N21B^i	171.8 (1)	Mn2—N31—C33	124.4 (1)
N11A—Mn1—O1	90.2 (1)	C31—N31—C33	104.4 (1)
N11A—Mn1—O1^i	95.9 (1)	N31—C31—N32	111.5 (2)
N11A^i—Mn1—N11B	84.1 (1)	C31—N32—C32	107.8 (1)
N11A^i—Mn1—N11B^i	2.0 (1)	N32—C32—C33	106.1 (2)
N11A^i—Mn1—N21A	165.5 (1)	N31—C33—C32	110.2 (2)
N11A^i—Mn1—N21A^i	84.6 (1)	Mn2—N41—C41	126.8 (1)
N11A^i—Mn1—N21B	171.8 (1)	Mn2—N41—C43	128.6 (1)
N11A^i—Mn1—N21B^i	89.6 (1)	C41—N41—C43	104.4 (1)
N11A^i—Mn1—O1	95.9 (1)	N41—C41—N42	111.5 (2)
N11A^i—Mn1—O1^i	90.2 (1)	C41—N42—C42	107.8 (1)
N11B—Mn1—N11B^i	85.6 (1)	N42—C42—C43	106.1 (2)
N11B—Mn1—N21A	83.2 (1)	N41—C43—C42	110.2 (2)
N11B—Mn1—N21A^i	166.1 (1)	O1—V1—O2	110.0 (1)
N11B—Mn1—N21B	88.2 (1)	O1—V1—O3	108.0 (1)
N11B—Mn1—N21B^i	172.6 (1)	O1—V1—O5	110.8 (1)
N11B—Mn1—O1	88.8 (1)	O2—V1—O3	111.5 (1)
N11B—Mn1—O1^i	97.2 (1)	O2—V1—O5	107.9 (1)
N11B^i—Mn1—N21A	166.1 (1)	O3—V1—O5	108.6 (1)
N11B^i—Mn1—N21A^i	83.2 (1)	O2^iii—V2—O4	108.8 (1)
N11B^i—Mn1—N21B	172.6 (1)	O2^iii—V2—O5	110.7 (1)
N11B^i—Mn1—N21B^i	88.2 (1)	O2^iii—V2—O6	109.6 (1)
N11B^i—Mn1—O1	97.2 (1)	O4—V2—O5	108.2 (1)
N11B^i—Mn1—O1^i	88.8 (1)	O4—V2—O6	109.4 (1)
N21A—Mn1—N21A^i	108.9 (2)	O5—V2—O6	110.1 (1)
N21A—Mn1—N21B	6.4 (1)	Mn1—O1—V1	165.9 (1)
N21A—Mn1—N21B^i	103.5 (1)	V1—O2—V2^iii	135.5 (1)
N21A—Mn1—O1	90.8 (1)	Mn2—O4—V2	162.2 (1)
N21A—Mn1—O1^i	84.5 (1)	V1—O5—V2	127.0 (1)
N21A^i—Mn1—N21B	103.5 (1)	N11A—C11A—H1C11A	124.2
N21A^i—Mn1—N21B^i	6.4 (1)	N12A—C11A—H1C11A	124.2
N21A^i—Mn1—O1	84.5 (1)	C11A—N12A—H1N12A	126.1
N21A^i—Mn1—O1^i	90.8 (1)	C12A—N12A—H1N12A	126.1
N21B—Mn1—N21B^i	98.3 (1)	N12A—C12A—H1C12A	127.0
N21B—Mn1—O1	86.8 (1)	C13A—C12A—H1C12A	127.0
N21B—Mn1—O1^i	87.9 (1)	N11A—C13A—H1C13A	124.9
N21B^i—Mn1—O1	87.9 (1)	C12A—C13A—H1C13A	124.9
N21B^i—Mn1—O1^i	86.8 (1)	N11B—C11B—H1C11B	124.2
O1—Mn1—O1^i	171.8 (1)	N12B—C11B—H1C11B	124.2
Mn1—N11A—C11A	127.0 (2)	C11B—N12B—H1N12B	126.1
Mn1—N11A—C13A	128.5 (2)	C12B—N12B—H1N12B	126.1
C11A—N11A—C13A	104.4 (1)	N12B—C12B—H1C12B	127.0
N11A—C11A—N12A	111.5 (2)	C13B—C12B—H1C12B	127.0
C11A—N12A—C12A	107.8 (1)	N11B—C13B—H1C13B	124.9
N12A—C12A—C13A	106.1 (2)	C12B—C13B—H1C13B	124.9
N11B—C13A—C12A	110.2 (2)	N21A—C21A—H1C21A	124.2
Mn1—N11B—C11B	126.7 (2)	N22A—C21A—H1C21A	124.2
Mn1—N11B—C13B	128.8 (2)	C21A—N22A—H1N22A	126.1
C11B—N11B—C13B	104.4 (1)	C22A—N22A—H1N22A	126.1
N11B—C11B—N12B	111.5 (2)	N22A—C22A—H1C22A	127.0
C11B—N12B—C12B	107.8 (1)	C23A—C22A—H1C22A	127.0
N12B—C12B—C13B	106.1 (2)	N21A—C23A—H1C23A	124.9
N11B—C13B—C12B	110.2 (2)	C22A—C23A—H1C23A	124.9
Mn1—N21A—C21A	128.4 (2)	N21B—C21B—H1C21B	124.2
Mn1—N21A—C23A	126.5 (2)	N22B—C21B—H1C21B	124.2
C21A—N21A—C23A	104.4 (1)	C21B—N22B—H1N22B	126.1
N21A—C21A—N22A	111.5 (2)	C22B—N22B—H1N22B	126.1
C21A—N22A—C22A	107.8 (1)	N22B—C22B—H1C22B	127.0
N22A—C22A—C23A	106.1 (2)	C23B—C22B—H1C22B	127.0
N21A—C23A—C22A	110.2 (2)	N21B—C23B—H1C23B	124.9
Mn1—N21B—C21B	129.0 (2)	C22B—C23B—H1C23B	124.9
Mn1—N21B—C23B	126.5 (2)	N31—C31—H1C31	124.2
C21B—N21B—C23B	104.4 (1)	N32—C31—H1C31	124.2
N21B—C21B—N22B	111.5 (2)	C31—N32—H1N32	126.1
C21B—N22B—C22B	107.8 (1)	C32—N32—H1N32	126.1
N22B—C22B—C23B	106.1 (2)	N32—C32—H1C32	127.0
N21B—C23B—C22B	110.2 (2)	C33—C32—H1C32	127.0
N31—Mn2—N31^ii	100.6 (1)	N31—C33—H1C33	124.9
N31—Mn2—N41	86.8	C32—C33—H1C33	124.9
N31—Mn2—N41^ii	172.4 (1)	N41—C41—H1C41	124.2
N31—Mn2—O4	86.8 (1)	N42—C41—H1C41	124.2
N31—Mn2—O4^ii	88.1 (1)	C41—N42—H1N42	126.1
N31^ii—Mn2—N41	172.4 (1)	C42—N42—H1N42	126.1
N31^ii—Mn2—N41^ii	86.8	N42—C42—H1C42	127.0
N31^ii—Mn2—O4	88.1 (1)	C43—C42—H1C42	127.0
N31^ii—Mn2—O4^ii	86.8 (1)	N41—C43—H1C43	124.9
N41—Mn2—N41^ii	86.0 (1)	C42—C43—H1C43	124.9

Symmetry codes: (i) −x+1/2, −y+3/2, z; (ii) −x+1/2, −y+1/2, z; (iii) −x+1, −y+1, −z+2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N12A—H1N12A···O6^iv	0.86	1.94	2.768 (4)	163
N12B—H1N12B···O6^iv	0.86	1.96	2.797 (4)	165
N22B—H1N22B···O3^v	0.86	2.03	2.875 (3)	167
N32—H1N32···O5^vi	0.86	2.07	2.871 (2)	154
N42—H1N42···O3^v	0.86	1.97	2.773 (3)	155

Symmetry codes: (iv) y−1/2, −x+1, z−1/2; (v) y−1/2, −x+1, z+1/2; (vi) −y+1/2, x, −z+3/2.

catena-tetrakis(imidazole)-tetrakis(µ₂-oxo)-dioxo-cobalt(ii)-di-vanadium (Co_100K)

Crystal data

[Co(C3H4N2)4V2O6]	Dx = 1.839 Mg m^−3
Mr = 529.13	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I41/a	Cell parameters from 104113 reflections
Hall symbol: -I 4ad	θ = 2.6–30.0°
a = 22.8606 (3) Å	µ = 1.86 mm^−1
c = 29.2658 (3) Å	T = 100 K
V = 15294.5 (3) Å^3	Hexagonal, orange-red
Z = 32	0.25 × 0.19 × 0.18 mm
F(000) = 8480

Data collection

Enraf-Nonius KappaCCD diffractometer	11163 independent reflections
Radiation source: fine-focus sealed tube	7414 reflections with I > 3σ(I)
Graphite monochromator	Rint = 0.059
φ scan plus ω scans with κ offsets	θmax = 30.0°, θmin = 2.8°
Absorption correction: multi-scan from symmetry-related measurements Sortav (Blessing 1995)	h = −32→32
Tmin = 0.636, Tmax = 0.720	k = −32→30
127079 measured reflections	l = −41→41

Refinement

Refinement on F	2 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.035	w = 1/[σ(F)^2 + (0.0004F)^2]
wR(F^2) = 0.056	(Δ/σ)max = 0.2
S = 1.85	Δρmax = 1.20 e Å^−3
7414 reflections	Δρmin = −1.13 e Å^−3
318 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Co1	0.74949 (2)	0.49602 (2)	0.45166 (1)	0.0102 (1)
Co2	1.00000	0.25000	0.49042 (2)	0.0106 (1)
Co3	0.50000	0.75000	0.48544 (2)	0.0110 (1)
V1	0.91181 (2)	0.51338 (2)	0.44903 (1)	0.0105 (1)
V2	0.98617 (2)	0.41039 (2)	0.49665 (1)	0.0110 (1)
V3	0.58555 (2)	0.48370 (2)	0.44683 (1)	0.0103 (1)
V4	0.51517 (2)	0.59049 (2)	0.49474 (1)	0.0107 (1)
O1	0.84136 (8)	0.50231 (8)	0.45764 (6)	0.0156 (4)
O2	0.94290 (8)	0.55621 (8)	0.49446 (6)	0.0162 (4)
O3	0.92030 (9)	0.54539 (9)	0.39927 (6)	0.0206 (4)
O4	0.99597 (8)	0.34052 (8)	0.48600 (6)	0.0156 (4)
O5	0.94981 (8)	0.44309 (8)	0.44806 (6)	0.0154 (4)
O6	0.94524 (9)	0.41759 (8)	0.54239 (6)	0.0200 (4)
O7	0.65608 (8)	0.49077 (8)	0.45435 (6)	0.0164 (4)
O8	0.55580 (8)	0.44074 (8)	0.49276 (6)	0.0143 (4)
O9	0.57528 (9)	0.45364 (9)	0.39610 (6)	0.0201 (4)
O10	0.50714 (8)	0.65974 (8)	0.48120 (6)	0.0163 (4)
O11	0.54951 (8)	0.55456 (8)	0.44641 (6)	0.0159 (4)
O12	0.55599 (9)	0.58570 (9)	0.54054 (6)	0.0198 (4)
N11	0.76000 (8)	0.43207 (7)	0.39877 (5)	0.0142 (5)
N12	0.73958 (8)	0.36235 (7)	0.34938 (6)	0.0192 (5)
C11	0.72063 (7)	0.39370 (8)	0.38545 (6)	0.0169 (5)
C12	0.79456 (8)	0.38180 (9)	0.33887 (6)	0.0205 (6)
C13	0.80671 (7)	0.42466 (8)	0.36942 (6)	0.0186 (6)
N21A	0.74754 (7)	0.42255 (7)	0.49681 (6)	0.0163 (5)	0.425 (15)
N22A	0.7170 (4)	0.33881 (11)	0.52532 (12)	0.0371 (8)	0.425 (15)
C21A	0.70230 (16)	0.38764 (17)	0.50225 (10)	0.0247 (6)	0.425 (15)
C22A	0.7754 (4)	0.34257 (17)	0.53533 (10)	0.0600 (8)	0.425 (15)
C23A	0.79371 (17)	0.3942 (2)	0.51766 (9)	0.0519 (7)	0.425 (15)
N31	0.92818 (7)	0.24773 (8)	0.44269 (5)	0.0142 (5)
N32	0.86425 (8)	0.22401 (8)	0.38956 (6)	0.0209 (6)
C31	0.91610 (8)	0.21140 (8)	0.40911 (6)	0.0171 (5)
C32	0.84160 (7)	0.27141 (9)	0.41198 (7)	0.0219 (5)
C33	0.88123 (8)	0.28565 (8)	0.44457 (6)	0.0180 (5)
N41	0.93556 (7)	0.24385 (8)	0.54275 (5)	0.0144 (5)
N42	0.87839 (8)	0.26671 (8)	0.60060 (5)	0.0195 (5)
C41	0.92348 (8)	0.28345 (7)	0.57399 (6)	0.0159 (4)
C42	0.86037 (9)	0.21299 (9)	0.58551 (7)	0.0249 (6)
C43	0.89579 (9)	0.19933 (8)	0.54995 (7)	0.0220 (4)
N51	0.74246 (8)	0.55914 (8)	0.39799 (5)	0.0143 (5)
N52	0.76430 (8)	0.61675 (9)	0.34017 (6)	0.0253 (6)
C51	0.78508 (7)	0.58189 (10)	0.37355 (7)	0.0263 (7)
C52	0.70458 (8)	0.61639 (9)	0.34336 (7)	0.0238 (7)
C53	0.69160 (7)	0.58084 (10)	0.37901 (7)	0.0252 (8)
N61	0.74492 (8)	0.56395 (7)	0.50028 (5)	0.0142 (5)
N62	0.72920 (9)	0.61504 (9)	0.56286 (5)	0.0254 (6)
C61	0.72614 (10)	0.56211 (8)	0.54277 (6)	0.0259 (7)
C62	0.75132 (12)	0.65330 (7)	0.53133 (8)	0.0344 (9)
C63	0.76084 (11)	0.62146 (9)	0.49298 (6)	0.0357 (9)
N71	0.57041 (7)	0.75341 (8)	0.43699 (6)	0.0152 (4)
N72	0.63057 (8)	0.78289 (8)	0.38294 (6)	0.0204 (5)
C71	0.57974 (8)	0.79270 (8)	0.40495 (6)	0.0171 (5)
C72	0.65546 (8)	0.73424 (9)	0.40203 (7)	0.0239 (5)
C73	0.61813 (8)	0.71646 (8)	0.43522 (7)	0.0209 (5)
N81	0.56351 (8)	0.75740 (8)	0.53842 (5)	0.0168 (5)
N82	0.62983 (8)	0.73908 (9)	0.59106 (6)	0.0233 (6)
C81	0.60384 (9)	0.72043 (8)	0.55240 (6)	0.0231 (5)
C82	0.60463 (9)	0.79131 (9)	0.60266 (6)	0.0242 (5)
C83	0.56392 (9)	0.80218 (8)	0.57009 (7)	0.0236 (5)
N21B	0.74754 (7)	0.42255 (7)	0.49681 (6)	0.0163 (5)	0.575
N22B	0.7813 (3)	0.34662 (16)	0.53484 (10)	0.0629 (8)	0.575
C21B	0.79397 (13)	0.39879 (18)	0.51583 (9)	0.0502 (7)	0.575
C22B	0.7231 (3)	0.33621 (10)	0.52759 (11)	0.0386 (8)	0.575
C23B	0.70274 (14)	0.38314 (15)	0.50419 (10)	0.0255 (6)	0.575
H1N12	0.72061	0.33514	0.33553	0.023
H1C11	0.68428	0.38882	0.39921	0.020
H1C12	0.81867	0.36836	0.31552	0.025
H1C13	0.84136	0.44592	0.37047	0.023
H1N22A	0.69400	0.31049	0.53243	0.050	0.425
H1C21A	0.66486	0.39567	0.49151	0.044	0.425
H1C22A	0.79784	0.31527	0.55105	0.098	0.425
H1C23A	0.83176	0.40844	0.51933	0.090	0.425
H1N22B	0.80539	0.32403	0.54893	0.102	0.575
H1C21B	0.83090	0.41586	0.51610	0.085	0.575
H1C22B	0.70186	0.30360	0.53683	0.052	0.575
H1C23B	0.66430	0.38808	0.49453	0.045	0.575
H1N32	0.84832	0.20566	0.36713	0.025
H1C31	0.94031	0.18086	0.40001	0.019
H1C32	0.80624	0.29004	0.40606	0.027
H1C33	0.87738	0.31641	0.46515	0.020
H1N42	0.86364	0.28619	0.62294	0.022
H1C41	0.94354	0.31858	0.57729	0.019
H1C42	0.83002	0.19047	0.59726	0.033
H1C43	0.89364	0.16506	0.53292	0.029
H1N52	0.78479	0.63574	0.32049	0.037
H1C51	0.82460	0.57479	0.37868	0.048
H1C52	0.67828	0.63643	0.32485	0.035
H1C53	0.65401	0.57233	0.38918	0.046
H1N62	0.71911	0.62327	0.59043	0.037
H1C61	0.71248	0.52848	0.55711	0.053
H1C62	0.75838	0.69302	0.53538	0.057
H1C63	0.77586	0.63617	0.46577	0.069
H1N72	0.64476	0.80341	0.36095	0.023
H1C71	0.55443	0.82340	0.39832	0.019
H1C72	0.69077	0.71693	0.39390	0.031
H1C73	0.62382	0.68416	0.45402	0.026
H1N82	0.65722	0.72142	0.60574	0.029
H1C81	0.61322	0.68577	0.53746	0.034
H1C82	0.61361	0.81458	0.62776	0.032
H1C83	0.53983	0.83494	0.56919	0.035

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0100 (2)	0.0106 (2)	0.0100 (2)	−0.0010 (1)	0.0009 (1)	−0.0003 (1)
Co2	0.0121 (3)	0.0099 (3)	0.0098 (2)	0.0012 (2)	0.0000 (1)	0.0000 (1)
Co3	0.0124 (3)	0.0108 (3)	0.0098 (2)	0.0019 (2)	0.0000 (1)	0.0000 (1)
V1	0.0091 (2)	0.0109 (2)	0.0117 (2)	−0.0004 (2)	−0.0002 (2)	−0.0004 (2)
V2	0.0101 (2)	0.0096 (2)	0.0133 (2)	0.0001 (2)	0.0001 (2)	−0.0024 (2)
V3	0.0100 (2)	0.0107 (2)	0.0102 (2)	−0.0003 (2)	0.0017 (2)	−0.0001 (2)
V4	0.0110 (2)	0.0103 (2)	0.0109 (2)	0.0008 (2)	0.0003 (2)	0.0017 (2)
O1	0.0110 (10)	0.0188 (11)	0.0171 (9)	−0.0028 (8)	0.0005 (7)	−0.0018 (8)
O2	0.0127 (10)	0.0177 (11)	0.0180 (9)	−0.0009 (8)	0.0001 (8)	−0.0037 (8)
O3	0.0211 (11)	0.0235 (11)	0.0172 (10)	−0.0037 (9)	−0.0001 (8)	0.0054 (8)
O4	0.0156 (10)	0.0109 (10)	0.0203 (10)	0.0017 (8)	−0.0034 (8)	−0.0028 (8)
O5	0.0166 (11)	0.0140 (10)	0.0157 (9)	0.0013 (8)	−0.0028 (7)	−0.0031 (8)
O6	0.0207 (11)	0.0174 (11)	0.0219 (10)	0.0014 (9)	0.0079 (9)	−0.0012 (8)
O7	0.0127 (10)	0.0139 (10)	0.0227 (10)	−0.0009 (8)	0.0022 (8)	0.0023 (8)
O8	0.0129 (10)	0.0167 (10)	0.0132 (9)	−0.0010 (8)	0.0030 (7)	0.0035 (7)
O9	0.0244 (12)	0.0216 (11)	0.0144 (9)	−0.0069 (9)	0.0050 (8)	−0.0026 (8)
O10	0.0170 (10)	0.0139 (10)	0.0180 (9)	0.0015 (8)	0.0030 (8)	0.0034 (8)
O11	0.0188 (11)	0.0143 (10)	0.0148 (9)	0.0040 (8)	0.0035 (8)	0.0018 (8)
O12	0.0226 (11)	0.0201 (11)	0.0168 (10)	0.0025 (9)	−0.0061 (8)	0.0011 (8)
N11	0.0138 (8)	0.0154 (7)	0.0135 (6)	−0.0004 (6)	−0.0010 (5)	0.0002 (6)
N12	0.0230 (10)	0.0178 (7)	0.0169 (7)	0.0004 (6)	−0.0033 (6)	−0.0027 (6)
C11	0.0183 (8)	0.0164 (8)	0.0161 (6)	−0.0026 (6)	−0.0016 (6)	−0.0013 (6)
C12	0.0209 (9)	0.0235 (10)	0.0171 (7)	0.0033 (8)	−0.0011 (7)	−0.0047 (7)
C13	0.0158 (8)	0.0232 (10)	0.0167 (7)	0.0005 (6)	0.0008 (6)	−0.0038 (7)
N21A	0.0203 (9)	0.0187 (8)	0.0098 (8)	0.0020 (6)	−0.0007 (6)	0.0004 (6)
N22A	0.0438 (13)	0.0267 (9)	0.0407 (12)	−0.0001 (8)	0.0064 (10)	0.0155 (8)
C21A	0.0263 (8)	0.0225 (9)	0.0252 (10)	−0.0019 (7)	0.0035 (8)	0.0060 (7)
C22A	0.0455 (13)	0.0520 (11)	0.0825 (17)	0.0047 (11)	−0.0058 (14)	0.0490 (13)
C23A	0.0317 (9)	0.0529 (12)	0.0709 (17)	−0.0021 (9)	−0.0170 (11)	0.0440 (13)
N21B	0.0203 (9)	0.0187 (8)	0.0098 (8)	0.0020 (6)	−0.0007 (6)	0.0004 (6)
N22B	0.0446 (13)	0.0560 (12)	0.0882 (18)	0.0040 (11)	−0.0086 (14)	0.0534 (13)
C21B	0.0307 (9)	0.0519 (12)	0.0681 (16)	−0.0026 (8)	−0.0173 (11)	0.0421 (12)
C22B	0.0450 (13)	0.0278 (9)	0.0430 (12)	0.0011 (8)	0.0063 (10)	0.0175 (8)
C23B	0.0277 (8)	0.0227 (9)	0.0261 (10)	−0.0020 (7)	0.0036 (8)	0.0065 (7)
N31	0.0158 (7)	0.0142 (9)	0.0126 (7)	0.0005 (6)	0.0009 (5)	0.0001 (6)
N32	0.0227 (8)	0.0221 (10)	0.0180 (7)	−0.0041 (7)	−0.0051 (6)	0.0026 (6)
C31	0.0213 (8)	0.0160 (8)	0.0139 (7)	−0.0018 (6)	−0.0019 (6)	−0.0002 (6)
C32	0.0181 (7)	0.0264 (11)	0.0213 (8)	0.0007 (6)	−0.0036 (6)	0.0034 (7)
C33	0.0162 (7)	0.0203 (9)	0.0175 (7)	0.0033 (6)	−0.0002 (6)	0.0008 (6)
N41	0.0145 (7)	0.0162 (8)	0.0125 (6)	−0.0004 (6)	0.0007 (6)	−0.0023 (5)
N42	0.0199 (8)	0.0229 (9)	0.0158 (7)	0.0024 (7)	0.0048 (6)	−0.0013 (6)
C41	0.0181 (8)	0.0168 (7)	0.0129 (6)	0.0022 (6)	0.0021 (6)	−0.0018 (6)
C42	0.0234 (8)	0.0296 (12)	0.0217 (9)	−0.0068 (8)	0.0092 (7)	−0.0050 (7)
C43	0.0224 (9)	0.0239 (9)	0.0195 (8)	−0.0079 (8)	0.0071 (7)	−0.0059 (6)
N51	0.0157 (9)	0.0130 (8)	0.0142 (7)	−0.0016 (6)	0.0003 (6)	0.0001 (6)
N52	0.0241 (9)	0.0278 (9)	0.0239 (8)	−0.0050 (8)	−0.0010 (7)	0.0120 (7)
C51	0.0184 (7)	0.0332 (10)	0.0272 (8)	−0.0049 (7)	−0.0001 (7)	0.0159 (8)
C52	0.0240 (9)	0.0245 (10)	0.0229 (8)	0.0004 (8)	−0.0014 (7)	0.0093 (7)
C53	0.0183 (7)	0.0308 (10)	0.0266 (8)	0.0028 (8)	0.0010 (7)	0.0137 (8)
N61	0.0130 (10)	0.0142 (7)	0.0154 (7)	−0.0034 (7)	0.0019 (6)	−0.0004 (6)
N62	0.0263 (12)	0.0266 (8)	0.0233 (7)	−0.0038 (8)	0.0045 (7)	−0.0101 (6)
C61	0.0351 (13)	0.0236 (7)	0.0188 (7)	−0.0100 (7)	0.0109 (7)	−0.0057 (6)
C62	0.0559 (17)	0.0186 (7)	0.0288 (9)	−0.0066 (8)	0.0054 (10)	−0.0083 (6)
C63	0.0670 (18)	0.0151 (8)	0.0250 (8)	−0.0135 (8)	0.0122 (9)	−0.0039 (6)
N71	0.0146 (7)	0.0164 (9)	0.0147 (7)	0.0025 (6)	0.0001 (6)	0.0018 (6)
N72	0.0203 (8)	0.0244 (10)	0.0166 (7)	−0.0046 (7)	0.0035 (6)	−0.0023 (6)
C71	0.0195 (7)	0.0174 (9)	0.0145 (7)	−0.0011 (6)	0.0014 (6)	0.0012 (6)
C72	0.0173 (7)	0.0321 (12)	0.0223 (8)	0.0029 (6)	0.0045 (6)	−0.0011 (7)
C73	0.0165 (7)	0.0254 (9)	0.0208 (7)	0.0071 (7)	0.0027 (6)	0.0026 (6)
N81	0.0184 (8)	0.0180 (9)	0.0139 (6)	0.0007 (7)	0.0003 (6)	0.0007 (6)
N82	0.0238 (8)	0.0273 (10)	0.0189 (7)	0.0020 (7)	−0.0049 (6)	0.0008 (7)
C81	0.0240 (9)	0.0254 (9)	0.0199 (7)	0.0065 (7)	−0.0052 (7)	−0.0022 (6)
C82	0.0284 (10)	0.0256 (10)	0.0186 (7)	0.0001 (8)	−0.0061 (7)	−0.0016 (7)
C83	0.0296 (10)	0.0215 (9)	0.0197 (7)	0.0034 (7)	−0.0068 (7)	−0.0039 (7)

Geometric parameters (Å, º)

Co1—O1	2.112 (2)	N42—C42	1.368 (2)
Co1—O7	2.140 (2)	C42—C43	1.355 (1)
Co1—N11	2.143 (1)	N51—C51	1.316 (1)
Co1—N21A	2.138 (2)	N51—C53	1.381 (1)
Co1—N21B	2.138 (2)	N52—C51	1.347 (1)
Co1—N51	2.139 (1)	N52—C52	1.368 (2)
Co1—N61	2.109 (1)	C52—C53	1.355 (1)
Co2—O4	2.075 (2)	N61—C61	1.316 (1)
Co2—O4^i	2.075 (2)	N61—C63	1.381 (1)
Co2—N31	2.156 (1)	N62—C61	1.347 (1)
Co2—N31^i	2.156 (1)	N62—C62	1.368 (2)
Co2—N41	2.130 (1)	C62—C63	1.355 (1)
Co2—N41^i	2.130 (1)	N71—C71	1.316 (1)
Co3—O10	2.074 (2)	N71—C73	1.381 (1)
Co3—O10^ii	2.074 (2)	N72—C71	1.347 (1)
Co3—N71	2.147 (1)	N72—C72	1.368 (2)
Co3—N71^ii	2.147 (1)	C72—C73	1.355 (1)
Co3—N81	2.131 (1)	N81—C81	1.316 (1)
Co3—N81^ii	2.131 (1)	N81—C83	1.381 (1)
V1—O1	1.650 (2)	N82—C81	1.347 (1)
V1—O2	1.798 (2)	N82—C82	1.368 (2)
V1—O3	1.641 (2)	C82—C83	1.355 (1)
V1—O5	1.827 (2)	N12—H1N12	0.860
V2—O2^iii	1.811 (2)	C11—H1C11	0.930
V2—O4	1.643 (2)	C12—H1C12	0.930
V2—O5	1.809 (2)	C13—H1C13	0.930
V2—O6	1.642 (2)	N22A—H1N22A	0.860
V3—O7	1.635 (2)	C21A—H1C21A	0.930
V3—O8	1.798 (2)	C22A—H1C22A	0.930
V3—O9	1.653 (2)	C23A—H1C23A	0.930
V3—O11	1.817 (2)	N22B—H1N22B	0.860
V4—O8^iv	1.810 (2)	C21B—H1C21B	0.930
V4—O10	1.642 (2)	C22B—H1C22B	0.930
V4—O11	1.814 (2)	C23B—H1C23B	0.930
V4—O12	1.637 (2)	N32—H1N32	0.860
N11—C11	1.316 (1)	C31—H1C31	0.930
N11—C13	1.381 (1)	C32—H1C32	0.930
N12—C11	1.347 (1)	C33—H1C33	0.930
N12—C12	1.368 (2)	N42—H1N42	0.860
C12—C13	1.355 (1)	C41—H1C41	0.930
N21A—C21A	1.316 (1)	C42—H1C42	0.930
N21A—C23A	1.381 (1)	C43—H1C43	0.930
N22A—C21A	1.347 (1)	N52—H1N52	0.860
N22A—C22A	1.368 (2)	C51—H1C51	0.930
C22A—C23A	1.355 (1)	C52—H1C52	0.930
N21B—C21B	1.316 (1)	C53—H1C53	0.930
N21B—C23B	1.381 (1)	N62—H1N62	0.860
N22B—C21B	1.347 (1)	C61—H1C61	0.930
N22B—C22B	1.368 (2)	C62—H1C62	0.930
C22B—C23B	1.355 (1)	C63—H1C63	0.930
N31—C31	1.316 (1)	N72—H1N72	0.860
N31—C33	1.381 (1)	C71—H1C71	0.930
N32—C31	1.347 (1)	C72—H1C72	0.930
N32—C32	1.368 (2)	C73—H1C73	0.930
C32—C33	1.355 (1)	N82—H1N82	0.860
N41—C41	1.316 (1)	C81—H1C81	0.930
N41—C43	1.381 (1)	C82—H1C82	0.930
N42—C41	1.347 (1)	C83—H1C83	0.930
O1—Co1—O7	173.1 (1)	N42—C42—C43	105.9 (1)
O1—Co1—N11	89.7 (1)	N41—C43—C42	109.9 (1)
O1—Co1—N21A	91.3 (1)	Co1—N51—C51	127.6 (1)
O1—Co1—N51	95.1 (1)	Co1—N51—C53	127.0 (1)
O1—Co1—N61	86.7 (1)	C51—N51—C53	105.2 (1)
O1—Co1—N21B	91.3 (1)	C51—N52—C52	107.4 (1)
O7—Co1—N11	95.7 (1)	N51—C51—N52	111.5 (1)
O7—Co1—N21A	85.0 (1)	N52—C52—C53	105.9 (1)
O7—Co1—N51	89.4 (1)	N51—C53—C52	109.9 (1)
O7—Co1—N61	88.1 (1)	Co1—N61—C61	129.1 (1)
O7—Co1—N21B	85.0 (1)	Co1—N61—C63	125.7 (1)
N11—Co1—N21A	85.0 (1)	C61—N61—C63	105.2 (1)
N11—Co1—N51	86.5 (1)	C61—N62—C62	107.4 (1)
N11—Co1—N61	174.5 (1)	N61—C61—N62	111.5 (1)
N11—Co1—N21B	85.0 (1)	N62—C62—C63	105.9 (1)
N21A—Co1—N51	169.3 (1)	N61—C63—C62	109.9 (1)
N21A—Co1—N61	99.2 (1)	Co3—N71—C71	128.1 (1)
N21A—Co1—N21B	0.0 (1)	Co3—N71—C73	126.5 (1)
N51—Co1—N61	89.7 (1)	C71—N71—C73	105.2 (1)
N51—Co1—N21B	169.3 (1)	C71—N72—C72	107.4 (1)
N61—Co1—N21B	99.2 (1)	N71—C71—N72	111.5 (1)
O4—Co2—O4^i	172.8 (1)	N72—C72—C73	105.9 (1)
O4—Co2—N31	87.1 (1)	N71—C73—C72	109.9 (1)
O4—Co2—N31^i	88.2 (1)	Co3—N81—C81	130.7 (1)
O4—Co2—N41	94.6 (1)	Co3—N81—C83	123.5 (1)
O4—Co2—N41^i	90.6 (1)	C81—N81—C83	105.2 (1)
O4^i—Co2—N31	88.2 (1)	C81—N82—C82	107.4 (1)
O4^i—Co2—N31^i	87.1 (1)	N81—C81—N82	111.5 (1)
O4^i—Co2—N41	90.6 (1)	N82—C82—C83	105.9 (1)
O4^i—Co2—N41^i	94.6 (1)	N81—C83—C82	109.9 (1)
N31—Co2—N31^i	99.2 (1)	Co1—N21B—C21B	124.7 (2)
N31—Co2—N41	86.4 (1)	Co1—N21B—C23B	128.7 (2)
N31—Co2—N41^i	173.8 (1)	C21B—N21B—C23B	105.2 (1)
N31^i—Co2—N41	173.8 (1)	C21B—N22B—C22B	107.4 (1)
N31^i—Co2—N41^i	86.4 (1)	N21B—C21B—N22B	111.5 (1)
N41—Co2—N41^i	88.0 (1)	N22B—C22B—C23B	105.9 (1)
O10—Co3—O10^ii	173.1 (1)	N21B—C23B—C22B	109.9 (1)
O10—Co3—N71	86.4 (1)	C11—N12—H1N12	126.3
O10—Co3—N71^ii	89.0 (1)	C12—N12—H1N12	126.3
O10—Co3—N81	94.0 (1)	N11—C11—H1C11	124.2
O10—Co3—N81^ii	91.0 (1)	N12—C11—H1C11	124.2
O10^ii—Co3—N71	89.0 (1)	N12—C12—H1C12	127.0
O10^ii—Co3—N71^ii	86.4 (1)	C13—C12—H1C12	127.0
O10^ii—Co3—N81	91.0 (1)	N11—C13—H1C13	125.0
O10^ii—Co3—N81^ii	94.0 (1)	C12—C13—H1C13	125.0
N71—Co3—N71^ii	97.3 (1)	C21A—N22A—H1N22A	126.3
N71—Co3—N81	88.1 (1)	C22A—N22A—H1N22A	126.3
N71—Co3—N81^ii	174.0 (1)	N21A—C21A—H1C21A	124.2
N71^ii—Co3—N81	174.0 (1)	N22A—C21A—H1C21A	124.2
N71^ii—Co3—N81^ii	88.1 (1)	N22A—C22A—H1C22A	127.0
N81—Co3—N81^ii	86.6 (1)	C23A—C22A—H1C22A	127.0
O1—V1—O2	110.9 (1)	N21A—C23A—H1C23A	125.0
O1—V1—O3	108.6 (1)	C22A—C23A—H1C23A	125.0
O1—V1—O5	109.4 (1)	C31—N32—H1N32	126.3
O2—V1—O3	111.5 (1)	C32—N32—H1N32	126.3
O2—V1—O5	107.6 (1)	N31—C31—H1C31	124.2
O3—V1—O5	108.8 (1)	N32—C31—H1C31	124.2
O2^iii—V2—O4	108.4 (1)	N32—C32—H1C32	127.0
O2^iii—V2—O5	110.5 (1)	C33—C32—H1C32	127.0
O2^iii—V2—O6	110.5 (1)	N31—C33—H1C33	125.0
O4—V2—O5	108.4 (1)	C32—C33—H1C33	125.0
O4—V2—O6	109.3 (1)	C41—N42—H1N42	126.3
O5—V2—O6	109.7 (1)	C42—N42—H1N42	126.3
O7—V3—O8	109.0 (1)	N41—C41—H1C41	124.2
O7—V3—O9	107.6 (1)	N42—C41—H1C41	124.2
O7—V3—O11	111.1 (1)	N42—C42—H1C42	127.0
O8—V3—O9	113.0 (1)	C43—C42—H1C42	127.0
O8—V3—O11	108.7 (1)	N41—C43—H1C43	125.0
O9—V3—O11	107.5 (1)	C42—C43—H1C43	125.0
O8^iv—V4—O10	109.2 (1)	C51—N52—H1N52	126.3
O8^iv—V4—O11	111.5 (1)	C52—N52—H1N52	126.3
O8^iv—V4—O12	108.6 (1)	N51—C51—H1C51	124.2
O10—V4—O11	107.3 (1)	N52—C51—H1C51	124.2
O10—V4—O12	109.0 (1)	N52—C52—H1C52	127.0
O11—V4—O12	111.2 (1)	C53—C52—H1C52	127.0
Co1—O1—V1	165.6 (1)	N51—C53—H1C53	125.0
V1—O2—V2^iii	133.6 (1)	C52—C53—H1C53	125.0
Co2—O4—V2	164.5 (1)	C61—N62—H1N62	126.3
V1—O5—V2	124.7 (1)	C62—N62—H1N62	126.3
Co1—O7—V3	169.8 (1)	N61—C61—H1C61	124.2
V3—O8—V4^iv	134.9 (1)	N62—C61—H1C61	124.2
Co3—O10—V4	162.5 (1)	N62—C62—H1C62	127.0
V3—O11—V4	126.5 (1)	C63—C62—H1C62	127.0
Co1—N11—C11	126.3 (1)	N61—C63—H1C63	125.0
Co1—N11—C13	128.3 (1)	C62—C63—H1C63	125.0
C11—N11—C13	105.2 (1)	C71—N72—H1N72	126.3
C11—N12—C12	107.4 (1)	C72—N72—H1N72	126.3
N11—C11—N12	111.5 (1)	N71—C71—H1C71	124.2
N12—C12—C13	105.9 (1)	N72—C71—H1C71	124.2
N11—C13—C12	109.9 (1)	N72—C72—H1C72	127.0
Co1—N21A—C21A	124.6 (2)	C73—C72—H1C72	127.0
Co1—N21A—C23A	128.8 (2)	N71—C73—H1C73	125.0
C21A—N21A—C23A	105.2 (1)	C72—C73—H1C73	125.0
C21A—N22A—C22A	107.4 (1)	C81—N82—H1N82	126.3
N21A—C21A—N22A	111.5 (1)	C82—N82—H1N82	126.3
N22A—C22A—C23A	105.9 (1)	N81—C81—H1C81	124.2
N21A—C23A—C22A	109.9 (1)	N82—C81—H1C81	124.2
Co2—N31—C31	131.2 (1)	N82—C82—H1C82	127.0
Co2—N31—C33	123.4 (1)	C83—C82—H1C82	127.0
C31—N31—C33	105.2 (1)	N81—C83—H1C83	125.0
C31—N32—C32	107.4 (1)	C82—C83—H1C83	125.0
N31—C31—N32	111.5 (1)	C21B—N22B—H1N22B	126.3
N32—C32—C33	105.9 (1)	C22B—N22B—H1N22B	126.3
N31—C33—C32	109.9 (1)	N21B—C21B—H1C21B	124.2
Co2—N41—C41	126.8 (1)	N22B—C21B—H1C21B	124.2
Co2—N41—C43	127.9 (1)	N22B—C22B—H1C22B	127.0
C41—N41—C43	105.2 (1)	C23B—C22B—H1C22B	127.0
C41—N42—C42	107.4 (1)	N21B—C23B—H1C23B	125.0
N41—C41—N42	111.5 (1)	C22B—C23B—H1C23B	125.0

Symmetry codes: (i) −x+2, −y+1/2, z; (ii) −x+1, −y+3/2, z; (iii) −x+2, −y+1, −z+1; (iv) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N12—H1N12···O12^v	0.86	1.96	2.754 (2)	154
N32—H1N32···O11^vi	0.86	2.12	2.912 (2)	154
N42—H1N42···O3^vii	0.86	2.00	2.775 (2)	149
N52—H1N52···O6^v	0.86	1.93	2.757 (2)	162
N62—H1N62···O9^vii	0.86	2.04	2.853 (2)	157
N72—H1N72···O5^viii	0.86	2.05	2.796 (2)	145
N82—H1N82···O9^vii	0.86	1.91	2.758 (2)	167
C51—H1C51···O3	0.93	2.37	3.289 (3)	171

Symmetry codes: (v) −y+5/4, x−1/4, z−1/4; (vi) y+1/4, −x+3/4, −z+3/4; (vii) y+1/4, −x+5/4, z+1/4; (viii) y+1/4, −x+7/4, −z+3/4.

catena-tetrakis(imidazole)-tetrakis(µ₂-oxo)-dioxo-cobalt(ii)-di-vanadium (Co_170K)

Crystal data

[Co(C3H4N2)4V2O6]	Dx = 1.835 Mg m^−3
Mr = 529.13	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I41/a	Cell parameters from 91573 reflections
Hall symbol: -I 4ad	θ = 2.6–30.0°
a = 22.8863 (3) Å	µ = 1.86 mm^−1
c = 29.2700 (3) Å	T = 170 K
V = 15331.1 (3) Å^3	Hexagonal, orange-red
Z = 32	0.25 × 0.19 × 0.18 mm
F(000) = 8480

Data collection

Enraf-Nonius KappaCCD diffractometer	11199 independent reflections
Radiation source: fine-focus sealed tube	6461 reflections with I > 3σ(I)
Graphite monochromator	Rint = 0.057
φ scan plus ω scans with κ offsets	θmax = 30.0°, θmin = 2.8°
Absorption correction: multi-scan from symmetry-related measurements Sortav (Blessing 1995)	h = −32→32
Tmin = 0.639, Tmax = 0.719	k = −32→30
107994 measured reflections	l = −41→41

Refinement

Refinement on F	2 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.040	w = 1/[σ(F)^2 + (0.0004F)^2]
wR(F^2) = 0.065	(Δ/σ)max = 0.2
S = 2.10	Δρmax = 2.40 e Å^−3
6461 reflections	Δρmin = −1.40 e Å^−3
318 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Co1	0.74950 (3)	0.49608 (3)	0.45142 (1)	0.0134 (1)
Co2	1.00000	0.25000	0.49050 (3)	0.0140 (2)
Co3	0.50000	0.75000	0.48585 (3)	0.0146 (2)
V1	0.91203 (3)	0.51325 (3)	0.44896 (2)	0.0141 (2)
V2	0.98624 (3)	0.41037 (3)	0.49660 (2)	0.0147 (2)
V3	0.58537 (3)	0.48403 (3)	0.44678 (2)	0.0135 (2)
V4	0.51495 (3)	0.59051 (3)	0.49498 (2)	0.0143 (2)
O1	0.84173 (12)	0.50246 (13)	0.45746 (9)	0.0210 (7)
O2	0.94310 (12)	0.55614 (13)	0.49422 (9)	0.0219 (7)
O3	0.92057 (14)	0.54520 (14)	0.39942 (9)	0.0276 (8)
O4	0.99645 (13)	0.34062 (12)	0.48590 (9)	0.0208 (7)
O5	0.95000 (13)	0.44320 (12)	0.44797 (9)	0.0214 (7)
O6	0.94536 (13)	0.41746 (13)	0.54231 (9)	0.0270 (8)
O7	0.65574 (13)	0.49097 (13)	0.45419 (9)	0.0225 (7)
O8	0.55588 (12)	0.44083 (13)	0.49255 (9)	0.0195 (7)
O9	0.57477 (14)	0.45427 (14)	0.39603 (9)	0.0283 (8)
O10	0.50695 (13)	0.65965 (12)	0.48173 (9)	0.0219 (7)
O11	0.54941 (13)	0.55483 (12)	0.44682 (9)	0.0215 (7)
O12	0.55571 (14)	0.58552 (13)	0.54061 (9)	0.0281 (8)
N11	0.76020 (12)	0.43240 (11)	0.39856 (8)	0.0208 (8)
N12	0.73945 (13)	0.36325 (11)	0.34922 (9)	0.0277 (9)
C11	0.72077 (11)	0.39462 (13)	0.38516 (9)	0.0248 (9)
C12	0.79425 (13)	0.38204 (14)	0.33891 (9)	0.0290 (10)
C13	0.80669 (11)	0.42464 (13)	0.36947 (10)	0.0266 (10)
N21A	0.74829 (10)	0.42319 (11)	0.49645 (9)	0.0221 (7)	0.389 (18)
N22A	0.7173 (5)	0.34017 (16)	0.52509 (17)	0.0526 (14)	0.389 (18)
C21A	0.7030 (2)	0.3889 (2)	0.50207 (15)	0.0368 (10)	0.389 (18)
C22A	0.7753 (5)	0.3434 (2)	0.53486 (14)	0.0706 (13)	0.389 (18)
C23A	0.7940 (3)	0.3946 (3)	0.51710 (13)	0.0594 (11)	0.389 (18)
N21B	0.74829 (10)	0.42319 (11)	0.49645 (9)	0.0221 (7)	0.611
N22B	0.7831 (4)	0.3481 (2)	0.53436 (14)	0.0742 (13)	0.611
C21B	0.79492 (17)	0.4000 (2)	0.51502 (13)	0.0578 (11)	0.611
C22B	0.7252 (4)	0.33730 (15)	0.52781 (16)	0.0538 (14)	0.611
C23B	0.70416 (19)	0.3838 (2)	0.50443 (14)	0.0379 (10)	0.611
N31	0.92821 (10)	0.24754 (12)	0.44265 (8)	0.0183 (8)
N32	0.86451 (12)	0.22381 (13)	0.38977 (8)	0.0271 (9)
C31	0.91620 (12)	0.21141 (11)	0.40924 (9)	0.0219 (7)
C32	0.84193 (11)	0.27081 (14)	0.41205 (11)	0.0295 (9)
C33	0.88145 (13)	0.28514 (12)	0.44457 (9)	0.0242 (8)
N41	0.93562 (10)	0.24392 (11)	0.54265 (7)	0.0167 (7)
N42	0.87858 (11)	0.26676 (12)	0.60022 (8)	0.0256 (8)
C41	0.92407 (11)	0.28295 (10)	0.57411 (9)	0.0187 (6)
C42	0.85977 (12)	0.21408 (13)	0.58456 (10)	0.0303 (8)
C43	0.89515 (13)	0.20033 (11)	0.54910 (9)	0.0239 (6)
N51	0.74300 (11)	0.55943 (11)	0.39775 (8)	0.0179 (8)
N52	0.76460 (13)	0.61734 (13)	0.34042 (9)	0.0314 (10)
C51	0.78531 (10)	0.58214 (14)	0.37339 (10)	0.0305 (10)
C52	0.70535 (13)	0.61723 (15)	0.34381 (10)	0.0346 (10)
C53	0.69242 (11)	0.58145 (15)	0.37921 (11)	0.0346 (11)
N61	0.74488 (13)	0.56431 (11)	0.49998 (8)	0.0191 (8)
N62	0.72954 (14)	0.61551 (13)	0.56223 (8)	0.0381 (10)
C61	0.72624 (15)	0.56275 (12)	0.54227 (9)	0.0371 (11)
C62	0.75166 (19)	0.65328 (11)	0.53081 (12)	0.0543 (16)
C63	0.76098 (19)	0.62138 (13)	0.49257 (10)	0.0547 (16)
N71	0.57053 (10)	0.75341 (12)	0.43729 (8)	0.0199 (8)
N72	0.63030 (13)	0.78269 (13)	0.38332 (8)	0.0282 (9)
C71	0.57968 (12)	0.79237 (12)	0.40529 (9)	0.0241 (8)
C72	0.65518 (12)	0.73455 (15)	0.40237 (11)	0.0318 (8)
C73	0.61808 (13)	0.71680 (12)	0.43559 (10)	0.0282 (9)
N81	0.56373 (12)	0.75723 (13)	0.53860 (8)	0.0261 (9)
N82	0.62940 (13)	0.73866 (15)	0.59127 (10)	0.0373 (10)
C81	0.60291 (15)	0.71982 (13)	0.55305 (10)	0.0450 (11)
C82	0.60578 (17)	0.79141 (15)	0.60203 (10)	0.0437 (12)
C83	0.56537 (16)	0.80252 (13)	0.56941 (12)	0.0506 (13)
H1N12	0.72029	0.33626	0.33531	0.033
H1C11	0.68437	0.39008	0.39883	0.030
H1C12	0.81828	0.36840	0.31561	0.036
H1C13	0.84150	0.44554	0.37061	0.034
H1N22A	0.69402	0.31214	0.53232	0.073	0.389
H1C21A	0.66565	0.39727	0.49144	0.061	0.389
H1C22A	0.79752	0.31589	0.55055	0.111	0.389
H1C23A	0.83219	0.40846	0.51863	0.100	0.389
H1N22B	0.80751	0.32586	0.54831	0.116	0.611
H1C21B	0.83168	0.41734	0.51484	0.095	0.611
H1C22B	0.70443	0.30464	0.53743	0.074	0.611
H1C23B	0.66557	0.38832	0.49515	0.063	0.611
H1N32	0.84863	0.20543	0.36735	0.032
H1C31	0.94044	0.18095	0.40013	0.025
H1C32	0.80656	0.28933	0.40614	0.037
H1C33	0.87755	0.31585	0.46514	0.028
H1N42	0.86405	0.28613	0.62268	0.029
H1C41	0.94477	0.31758	0.57790	0.019
H1C42	0.82890	0.19200	0.59590	0.040
H1C43	0.89246	0.16645	0.53170	0.027
H1N52	0.78505	0.63641	0.32079	0.045
H1C51	0.82478	0.57480	0.37831	0.055
H1C52	0.67907	0.63759	0.32554	0.052
H1C53	0.65489	0.57302	0.38946	0.061
H1N62	0.71952	0.62385	0.58978	0.056
H1C61	0.71244	0.52928	0.55669	0.078
H1C62	0.75890	0.69294	0.53479	0.092
H1C63	0.77604	0.63592	0.46533	0.107
H1N72	0.64437	0.80316	0.36127	0.033
H1C71	0.55430	0.82293	0.39862	0.030
H1C72	0.69050	0.71734	0.39424	0.041
H1C73	0.62389	0.68462	0.45445	0.037
H1N82	0.65633	0.72068	0.60618	0.053
H1C81	0.61134	0.68460	0.53864	0.089
H1C82	0.61543	0.81504	0.62675	0.069
H1C83	0.54216	0.83583	0.56805	0.097

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0134 (2)	0.0127 (3)	0.0141 (2)	−0.0015 (2)	0.0015 (2)	−0.0007 (2)
Co2	0.0165 (5)	0.0121 (4)	0.0134 (4)	0.0011 (3)	0.0000 (1)	0.0000 (1)
Co3	0.0158 (5)	0.0146 (5)	0.0134 (4)	0.0024 (3)	0.0000 (1)	0.0000 (1)
V1	0.0124 (4)	0.0139 (4)	0.0161 (3)	−0.0003 (3)	−0.0009 (3)	0.0002 (3)
V2	0.0136 (4)	0.0115 (4)	0.0190 (4)	−0.0001 (3)	−0.0001 (3)	−0.0029 (3)
V3	0.0125 (4)	0.0140 (4)	0.0139 (3)	−0.0011 (3)	0.0022 (3)	−0.0002 (3)
V4	0.0152 (4)	0.0134 (4)	0.0144 (3)	0.0016 (3)	0.0003 (3)	0.0026 (3)
O1	0.0124 (16)	0.0266 (17)	0.0240 (15)	−0.0043 (13)	−0.0006 (12)	−0.0025 (12)
O2	0.0173 (17)	0.0239 (18)	0.0244 (15)	−0.0014 (14)	0.0005 (13)	−0.0053 (13)
O3	0.0285 (19)	0.032 (2)	0.0226 (15)	−0.0063 (15)	0.0001 (13)	0.0090 (13)
O4	0.0214 (17)	0.0125 (16)	0.0284 (15)	0.0023 (13)	−0.0042 (13)	−0.0019 (12)
O5	0.0237 (19)	0.0189 (17)	0.0214 (15)	0.0031 (14)	−0.0050 (12)	−0.0048 (12)
O6	0.0261 (19)	0.0242 (18)	0.0307 (17)	0.0038 (15)	0.0124 (14)	−0.0014 (14)
O7	0.0175 (17)	0.0189 (16)	0.0309 (16)	−0.0007 (13)	0.0010 (12)	0.0037 (12)
O8	0.0182 (17)	0.0211 (17)	0.0192 (14)	−0.0027 (14)	0.0053 (12)	0.0047 (12)
O9	0.035 (2)	0.0308 (19)	0.0195 (15)	−0.0115 (15)	0.0079 (13)	−0.0072 (13)
O10	0.0218 (17)	0.0188 (17)	0.0250 (15)	0.0022 (13)	0.0052 (12)	0.0058 (12)
O11	0.0250 (19)	0.0189 (17)	0.0207 (15)	0.0075 (14)	0.0048 (12)	0.0033 (12)
O12	0.034 (2)	0.0258 (19)	0.0244 (16)	0.0036 (16)	−0.0083 (14)	0.0014 (13)
N11	0.0231 (14)	0.0201 (11)	0.0191 (10)	−0.0021 (9)	−0.0005 (9)	−0.0002 (9)
N12	0.0345 (15)	0.0241 (12)	0.0245 (11)	−0.0010 (10)	−0.0034 (10)	−0.0049 (9)
C11	0.0296 (12)	0.0220 (12)	0.0229 (10)	−0.0058 (10)	−0.0004 (9)	−0.0026 (9)
C12	0.0299 (14)	0.0331 (15)	0.0241 (11)	0.0041 (12)	−0.0025 (10)	−0.0080 (10)
C13	0.0242 (13)	0.0327 (15)	0.0230 (11)	−0.0003 (10)	0.0005 (9)	−0.0065 (10)
N21A	0.0270 (14)	0.0246 (13)	0.0148 (12)	0.0038 (10)	−0.0007 (10)	0.0024 (9)
N22A	0.059 (2)	0.0382 (14)	0.0605 (19)	−0.0010 (13)	0.0066 (18)	0.0262 (13)
C21A	0.0343 (13)	0.0328 (14)	0.0433 (18)	−0.0013 (12)	0.0060 (13)	0.0147 (12)
C22A	0.065 (2)	0.0577 (17)	0.090 (3)	0.0050 (16)	−0.012 (2)	0.0512 (18)
C23A	0.0441 (15)	0.0569 (19)	0.077 (2)	−0.0005 (13)	−0.0231 (17)	0.0440 (19)
N21B	0.0270 (14)	0.0246 (13)	0.0148 (12)	0.0038 (10)	−0.0007 (10)	0.0024 (9)
N22B	0.063 (2)	0.0623 (18)	0.097 (3)	0.0044 (17)	−0.017 (2)	0.056 (2)
C21B	0.0423 (15)	0.0562 (19)	0.075 (2)	−0.0011 (13)	−0.0236 (17)	0.0425 (18)
C22B	0.062 (2)	0.0389 (14)	0.061 (2)	0.0006 (13)	0.0056 (18)	0.0276 (13)
C23B	0.0365 (14)	0.0330 (14)	0.0443 (17)	−0.0014 (12)	0.0061 (13)	0.0154 (12)
N31	0.0203 (11)	0.0167 (14)	0.0180 (10)	−0.0004 (9)	0.0005 (8)	−0.0010 (9)
N32	0.0279 (12)	0.0293 (16)	0.0241 (11)	−0.0061 (11)	−0.0061 (9)	0.0015 (9)
C31	0.0274 (12)	0.0181 (14)	0.0201 (10)	−0.0035 (9)	−0.0033 (8)	−0.0010 (9)
C32	0.0227 (11)	0.0399 (19)	0.0258 (13)	0.0023 (10)	−0.0036 (9)	0.0012 (11)
C33	0.0216 (12)	0.0291 (14)	0.0219 (11)	0.0055 (10)	−0.0006 (8)	−0.0013 (9)
N41	0.0146 (10)	0.0202 (13)	0.0152 (9)	−0.0010 (8)	0.0006 (8)	−0.0032 (8)
N42	0.0242 (11)	0.0312 (14)	0.0213 (9)	0.0030 (10)	0.0082 (8)	−0.0019 (9)
C41	0.0196 (11)	0.0212 (11)	0.0152 (9)	0.0033 (8)	0.0022 (8)	−0.0022 (8)
C42	0.0246 (11)	0.0387 (15)	0.0276 (11)	−0.0074 (10)	0.0109 (9)	−0.0042 (10)
C43	0.0204 (11)	0.0292 (12)	0.0220 (10)	−0.0082 (10)	0.0052 (8)	−0.0047 (8)
N51	0.0176 (13)	0.0169 (12)	0.0192 (10)	−0.0015 (10)	0.0013 (9)	0.0014 (9)
N52	0.0358 (14)	0.0303 (14)	0.0282 (11)	−0.0057 (12)	0.0010 (11)	0.0123 (10)
C51	0.0233 (11)	0.0364 (15)	0.0319 (12)	−0.0067 (11)	0.0019 (10)	0.0163 (12)
C52	0.0355 (14)	0.0358 (16)	0.0327 (13)	0.0045 (15)	−0.0007 (12)	0.0160 (12)
C53	0.0231 (11)	0.0434 (17)	0.0372 (14)	0.0064 (13)	0.0017 (11)	0.0209 (13)
N61	0.0191 (16)	0.0186 (11)	0.0195 (10)	−0.0052 (10)	0.0035 (10)	−0.0011 (9)
N62	0.044 (2)	0.0387 (14)	0.0318 (11)	−0.0040 (13)	0.0067 (12)	−0.0167 (11)
C61	0.054 (2)	0.0331 (12)	0.0238 (11)	−0.0126 (12)	0.0162 (12)	−0.0085 (9)
C62	0.091 (3)	0.0271 (11)	0.0448 (16)	−0.0130 (13)	0.0128 (18)	−0.0162 (11)
C63	0.105 (3)	0.0207 (12)	0.0381 (13)	−0.0229 (13)	0.0234 (16)	−0.0081 (10)
N71	0.0200 (12)	0.0218 (15)	0.0179 (11)	0.0028 (9)	−0.0002 (9)	0.0018 (9)
N72	0.0278 (13)	0.0354 (17)	0.0213 (11)	−0.0061 (11)	0.0048 (10)	−0.0023 (9)
C71	0.0271 (12)	0.0258 (16)	0.0194 (11)	−0.0009 (10)	0.0026 (9)	0.0032 (10)
C72	0.0236 (12)	0.044 (2)	0.0283 (14)	0.0031 (10)	0.0059 (10)	−0.0025 (11)
C73	0.0230 (12)	0.0341 (16)	0.0275 (12)	0.0093 (11)	0.0041 (10)	0.0031 (10)
N81	0.0310 (15)	0.0273 (16)	0.0201 (11)	0.0006 (12)	−0.0026 (10)	0.0018 (10)
N82	0.0390 (16)	0.0457 (19)	0.0272 (13)	0.0065 (13)	−0.0101 (11)	−0.0012 (12)
C81	0.0499 (18)	0.0494 (17)	0.0356 (14)	0.0215 (15)	−0.0191 (13)	−0.0125 (12)
C82	0.057 (2)	0.0390 (19)	0.0351 (13)	0.0042 (15)	−0.0216 (15)	−0.0054 (13)
C83	0.072 (2)	0.0347 (16)	0.0452 (15)	0.0142 (13)	−0.0331 (16)	−0.0129 (12)

Geometric parameters (Å, º)

Co1—O1	2.123 (3)	N52—C52	1.360 (2)
Co1—O7	2.151 (3)	C52—C53	1.353 (2)
Co1—N11	2.140 (2)	N61—C61	1.310 (2)
Co1—N21A	2.126 (2)	N61—C63	1.374 (2)
Co1—N51	2.143 (2)	N62—C61	1.343 (2)
Co1—N61	2.114 (2)	N62—C62	1.360 (2)
Co1—N21B	2.126 (2)	C62—C63	1.353 (2)
Co2—O4	2.080 (3)	N71—C71	1.310 (2)
Co2—O4^i	2.080 (3)	N71—C73	1.374 (2)
Co2—N31	2.160 (2)	N72—C71	1.343 (2)
Co2—N31^i	2.160 (2)	N72—C72	1.360 (2)
Co2—N41	2.126 (2)	C72—C73	1.353 (2)
Co2—N41^i	2.126 (2)	N81—C81	1.310 (2)
Co3—O10	2.077 (3)	N81—C83	1.374 (2)
Co3—O10^ii	2.077 (3)	N82—C81	1.343 (2)
Co3—N71	2.152 (2)	N82—C82	1.360 (2)
Co3—N71^ii	2.152 (2)	C82—C83	1.353 (2)
Co3—N81	2.130 (2)	N21B—C21B	1.310 (2)
Co3—N81^ii	2.130 (2)	N21B—C23B	1.374 (2)
V1—O1	1.647 (3)	N22B—C21B	1.343 (2)
V1—O2	1.796 (3)	N22B—C22B	1.360 (2)
V1—O3	1.636 (3)	C22B—C23B	1.353 (2)
V1—O5	1.824 (3)	N12—H1N12	0.860
V2—O2^iii	1.810 (3)	C11—H1C11	0.930
V2—O4	1.643 (3)	C12—H1C12	0.930
V2—O5	1.811 (3)	C13—H1C13	0.930
V2—O6	1.641 (3)	N22A—H1N22A	0.860
V3—O7	1.633 (3)	C21A—H1C21A	0.930
V3—O8	1.797 (3)	C22A—H1C22A	0.930
V3—O9	1.652 (3)	C23A—H1C23A	0.930
V3—O11	1.817 (3)	N32—H1N32	0.860
V4—O8^iv	1.810 (3)	C31—H1C31	0.930
V4—O10	1.639 (3)	C32—H1C32	0.930
V4—O11	1.810 (3)	C33—H1C33	0.930
V4—O12	1.633 (3)	N42—H1N42	0.860
N11—C11	1.310 (2)	C41—H1C41	0.930
N11—C13	1.374 (2)	C42—H1C42	0.930
N12—C11	1.343 (2)	C43—H1C43	0.930
N12—C12	1.360 (2)	N52—H1N52	0.860
C12—C13	1.353 (2)	C51—H1C51	0.930
N21A—C21A	1.310 (2)	C52—H1C52	0.930
N21A—C23A	1.374 (2)	C53—H1C53	0.930
N22A—C21A	1.343 (2)	N62—H1N62	0.860
N22A—C22A	1.360 (2)	C61—H1C61	0.930
C22A—C23A	1.353 (2)	C62—H1C62	0.930
N31—C31	1.310 (2)	C63—H1C63	0.930
N31—C33	1.374 (2)	N72—H1N72	0.860
N32—C31	1.343 (2)	C71—H1C71	0.930
N32—C32	1.360 (2)	C72—H1C72	0.930
C32—C33	1.353 (2)	C73—H1C73	0.930
N41—C41	1.310 (2)	N82—H1N82	0.860
N41—C43	1.374 (2)	C81—H1C81	0.930
N42—C41	1.343 (2)	C82—H1C82	0.930
N42—C42	1.360 (2)	C83—H1C83	0.930
C42—C43	1.353 (2)	N22B—H1N22B	0.860
N51—C51	1.310 (2)	C21B—H1C21B	0.930
N51—C53	1.374 (2)	C22B—H1C22B	0.930
N52—C51	1.343 (2)	C23B—H1C23B	0.930
O1—Co1—O7	173.0 (1)	N42—C42—C43	106.0 (1)
O1—Co1—N11	89.6 (1)	N41—C43—C42	109.9 (1)
O1—Co1—N21A	90.9 (1)	Co1—N51—C51	128.0 (2)
O1—Co1—N51	94.8 (1)	Co1—N51—C53	126.6 (2)
O1—Co1—N61	86.7 (1)	C51—N51—C53	105.2 (1)
O1—Co1—N21B	90.9 (1)	C51—N52—C52	107.4 (1)
O7—Co1—N11	96.0 (1)	N51—C51—N52	111.6 (1)
O7—Co1—N21A	85.5 (1)	N52—C52—C53	106.0 (1)
O7—Co1—N51	89.7 (1)	N51—C53—C52	109.9 (1)
O7—Co1—N61	88.0 (1)	Co1—N61—C61	129.2 (2)
O7—Co1—N21B	85.5 (1)	Co1—N61—C63	125.6 (2)
N11—Co1—N21A	85.1 (1)	C61—N61—C63	105.2 (1)
N11—Co1—N51	86.5 (1)	C61—N62—C62	107.4 (1)
N11—Co1—N61	174.3 (1)	N61—C61—N62	111.6 (1)
N11—Co1—N21B	85.1 (1)	N62—C62—C63	106.0 (1)
N21A—Co1—N51	169.8 (1)	N61—C63—C62	109.9 (1)
N21A—Co1—N61	99.3 (1)	Co3—N71—C71	128.1 (2)
N21A—Co1—N21B	0.0 (2)	Co3—N71—C73	126.6 (2)
N51—Co1—N61	89.4 (1)	C71—N71—C73	105.2 (1)
N51—Co1—N21B	169.8 (1)	C71—N72—C72	107.4 (1)
N61—Co1—N21B	99.3 (1)	N71—C71—N72	111.6 (1)
O4—Co2—O4^i	172.6 (2)	N72—C72—C73	106.0 (1)
O4—Co2—N31	87.4 (1)	N71—C73—C72	109.9 (1)
O4—Co2—N31^i	87.8 (1)	Co3—N81—C81	130.7 (2)
O4—Co2—N41	94.9 (1)	Co3—N81—C83	123.6 (2)
O4—Co2—N41^i	90.5 (1)	C81—N81—C83	105.2 (1)
O4^i—Co2—N31	87.8 (1)	C81—N82—C82	107.4 (1)
O4^i—Co2—N31^i	87.4 (1)	N81—C81—N82	111.6 (1)
O4^i—Co2—N41	90.5 (1)	N82—C82—C83	106.0 (1)
O4^i—Co2—N41^i	94.9 (1)	N81—C83—C82	109.9 (1)
N31—Co2—N31^i	99.1 (1)	Co1—N21B—C21B	124.3 (3)
N31—Co2—N41	86.4 (1)	Co1—N21B—C23B	129.1 (3)
N31—Co2—N41^i	174.0 (1)	C21B—N21B—C23B	105.2 (1)
N31^i—Co2—N41	174.0 (1)	C21B—N22B—C22B	107.4 (1)
N31^i—Co2—N41^i	86.4 (1)	N21B—C21B—N22B	111.6 (1)
N41—Co2—N41^i	88.2 (1)	N22B—C22B—C23B	106.0 (1)
O10—Co3—O10^ii	173.3 (2)	N21B—C23B—C22B	109.9 (1)
O10—Co3—N71	86.6 (1)	C11—N12—H1N12	126.3
O10—Co3—N71^ii	89.0 (1)	C12—N12—H1N12	126.3
O10—Co3—N81	93.8 (1)	N11—C11—H1C11	124.2
O10—Co3—N81^ii	91.0 (1)	N12—C11—H1C11	124.2
O10^ii—Co3—N71	89.0 (1)	N12—C12—H1C12	127.0
O10^ii—Co3—N71^ii	86.6 (1)	C13—C12—H1C12	127.0
O10^ii—Co3—N81	91.0 (1)	N11—C13—H1C13	125.1
O10^ii—Co3—N81^ii	93.8 (1)	C12—C13—H1C13	125.1
N71—Co3—N71^ii	97.3 (1)	C21A—N22A—H1N22A	126.3
N71—Co3—N81	87.8 (1)	C22A—N22A—H1N22A	126.3
N71—Co3—N81^ii	174.2 (1)	N21A—C21A—H1C21A	124.2
N71^ii—Co3—N81	174.2 (1)	N22A—C21A—H1C21A	124.2
N71^ii—Co3—N81^ii	87.8 (1)	N22A—C22A—H1C22A	127.0
N81—Co3—N81^ii	87.1 (2)	C23A—C22A—H1C22A	127.0
O1—V1—O2	110.9 (1)	N21A—C23A—H1C23A	125.1
O1—V1—O3	108.5 (1)	C22A—C23A—H1C23A	125.1
O1—V1—O5	109.6 (1)	C31—N32—H1N32	126.3
O2—V1—O3	111.2 (1)	C32—N32—H1N32	126.3
O2—V1—O5	107.7 (1)	N31—C31—H1C31	124.2
O3—V1—O5	108.8 (1)	N32—C31—H1C31	124.2
O2^iii—V2—O4	108.2 (1)	N32—C32—H1C32	127.0
O2^iii—V2—O5	110.5 (1)	C33—C32—H1C32	127.0
O2^iii—V2—O6	110.3 (1)	N31—C33—H1C33	125.1
O4—V2—O5	108.6 (1)	C32—C33—H1C33	125.1
O4—V2—O6	109.4 (1)	C41—N42—H1N42	126.3
O5—V2—O6	109.8 (1)	C42—N42—H1N42	126.3
O7—V3—O8	109.0 (1)	N41—C41—H1C41	124.2
O7—V3—O9	107.7 (2)	N42—C41—H1C41	124.2
O7—V3—O11	111.1 (1)	N42—C42—H1C42	127.0
O8—V3—O9	112.9 (1)	C43—C42—H1C42	127.0
O8—V3—O11	108.7 (1)	N41—C43—H1C43	125.1
O9—V3—O11	107.6 (1)	C42—C43—H1C43	125.1
O8^iv—V4—O10	109.3 (1)	C51—N52—H1N52	126.3
O8^iv—V4—O11	111.6 (1)	C52—N52—H1N52	126.3
O8^iv—V4—O12	108.6 (1)	N51—C51—H1C51	124.2
O10—V4—O11	107.5 (1)	N52—C51—H1C51	124.2
O10—V4—O12	108.9 (2)	N52—C52—H1C52	127.0
O11—V4—O12	110.9 (1)	C53—C52—H1C52	127.0
Co1—O1—V1	165.7 (2)	N51—C53—H1C53	125.1
V1—O2—V2^iii	134.0 (2)	C52—C53—H1C53	125.1
Co2—O4—V2	164.1 (2)	C61—N62—H1N62	126.3
V1—O5—V2	124.8 (1)	C62—N62—H1N62	126.3
Co1—O7—V3	169.9 (2)	N61—C61—H1C61	124.2
V3—O8—V4^iv	134.8 (2)	N62—C61—H1C61	124.2
Co3—O10—V4	162.8 (2)	N62—C62—H1C62	127.0
V3—O11—V4	126.9 (1)	C63—C62—H1C62	127.0
Co1—N11—C11	126.0 (2)	N61—C63—H1C63	125.1
Co1—N11—C13	128.7 (2)	C62—C63—H1C63	125.1
C11—N11—C13	105.2 (1)	C71—N72—H1N72	126.3
C11—N12—C12	107.4 (1)	C72—N72—H1N72	126.3
N11—C11—N12	111.6 (1)	N71—C71—H1C71	124.2
N12—C12—C13	106.0 (1)	N72—C71—H1C71	124.2
N11—C13—C12	109.9 (1)	N72—C72—H1C72	127.0
Co1—N21A—C21A	123.9 (3)	C73—C72—H1C72	127.0
Co1—N21A—C23A	129.5 (3)	N71—C73—H1C73	125.1
C21A—N21A—C23A	105.2 (1)	C72—C73—H1C73	125.1
C21A—N22A—C22A	107.4 (1)	C81—N82—H1N82	126.3
N21A—C21A—N22A	111.6 (1)	C82—N82—H1N82	126.3
N22A—C22A—C23A	106.0 (1)	N81—C81—H1C81	124.2
N21A—C23A—C22A	109.9 (1)	N82—C81—H1C81	124.2
Co2—N31—C31	131.3 (2)	N82—C82—H1C82	127.0
Co2—N31—C33	123.3 (2)	C83—C82—H1C82	127.0
C31—N31—C33	105.2 (1)	N81—C83—H1C83	125.1
C31—N32—C32	107.4 (1)	C82—C83—H1C83	125.1
N31—C31—N32	111.6 (1)	C21B—N22B—H1N22B	126.3
N32—C32—C33	106.0 (1)	C22B—N22B—H1N22B	126.3
N31—C33—C32	109.9 (1)	N21B—C21B—H1C21B	124.2
Co2—N41—C41	126.9 (2)	N22B—C21B—H1C21B	124.2
Co2—N41—C43	127.8 (2)	N22B—C22B—H1C22B	127.0
C41—N41—C43	105.2 (1)	C23B—C22B—H1C22B	127.0
C41—N42—C42	107.4 (1)	N21B—C23B—H1C23B	125.1
N41—C41—N42	111.6 (1)	C22B—C23B—H1C23B	125.1

Symmetry codes: (i) −x+2, −y+1/2, z; (ii) −x+1, −y+3/2, z; (iii) −x+2, −y+1, −z+1; (iv) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N12—H1N12···O12^v	0.86	1.96	2.761 (4)	155
N32—H1N32···O11^vi	0.86	2.13	2.928 (3)	154
N42—H1N42···O3^vii	0.86	2.02	2.788 (3)	148
N52—H1N52···O6^v	0.86	1.92	2.755 (4)	163
N62—H1N62···O9^vii	0.86	2.05	2.867 (3)	158
N72—H1N72···O5^viii	0.86	2.06	2.809 (3)	145
N82—H1N82···O9^vii	0.86	1.91	2.759 (4)	169
C51—H1C51···O3	0.93	2.38	3.298 (4)	171

Symmetry codes: (v) −y+5/4, x−1/4, z−1/4; (vi) y+1/4, −x+3/4, −z+3/4; (vii) y+1/4, −x+5/4, z+1/4; (viii) y+1/4, −x+7/4, −z+3/4.

catena-tetrakis(imidazole)-tetrakis(µ₂-oxo)-dioxo-cobalt(ii)-di-vanadium (Co_180K)

Crystal data

[Co(C3H4N2)4V2O6]	Dx = 1.829 Mg m^−3
Mr = 529.13	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P42/n	Cell parameters from 44916 reflections
Hall symbol: -P 4bc	θ = 2.6–30.0°
a = 16.2544 (2) Å	µ = 1.86 mm^−1
c = 14.5532 (2) Å	T = 180 K
V = 3845.04 (9) Å^3	Hexagonal, orange-red
Z = 8	0.25 × 0.19 × 0.18 mm
F(000) = 2012

Data collection

Enraf-Nonius KappaCCD diffractometer	5608 independent reflections
Radiation source: fine-focus sealed tube	4475 reflections with I > 3σ(I)
Graphite monochromator	Rint = 0.046
φ scan plus ω scans with κ offsets	θmax = 30.0°, θmin = 2.8°
Absorption correction: multi-scan from symmetry-related measurements Sortav (Blessing 1995)	h = −32→30
Tmin = 0.658, Tmax = 0.721	k = −32→32
59858 measured reflections	l = −41→41

Refinement

Refinement on F	6 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.032	w = 1/[σ(F)^2 + (0.0004F)^2]
wR(F^2) = 0.050	(Δ/σ)max = 0.2
S = 1.81	Δρmax = 1.07 e Å^−3
4475 reflections	Δρmin = −0.53 e Å^−3
174 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Co1	0.25000	0.75000	0.90371 (2)	0.0159 (1)
N11A	0.19434 (12)	0.68041 (11)	0.79638 (11)	0.0241 (8)	0.500
C11A	0.13466 (18)	0.70424 (19)	0.74245 (19)	0.0395 (11)	0.500
N12A	0.1156 (2)	0.6461 (2)	0.6800 (2)	0.0449 (13)	0.500
C12A	0.1661 (3)	0.58136 (19)	0.6950 (2)	0.055 (3)	0.500
C13A	0.2144 (2)	0.60290 (16)	0.7667 (2)	0.052 (3)	0.500
N11B	0.19579 (11)	0.67922 (10)	0.79640 (10)	0.0196 (5)	0.500
C11B	0.12001 (14)	0.68429 (18)	0.76701 (16)	0.029 (3)	0.500
N12B	0.10620 (16)	0.6326 (2)	0.69625 (17)	0.031 (3)	0.500
C12B	0.1774 (2)	0.59219 (17)	0.67962 (16)	0.0282 (14)	0.500
C13B	0.23226 (16)	0.62119 (16)	0.74148 (16)	0.026 (3)	0.500
N21A	0.18066 (13)	0.67538 (12)	0.99332 (14)	0.0274 (5)	0.500
C21A	0.10541 (16)	0.68663 (18)	1.0223 (3)	0.0740 (9)	0.500
N22A	0.07640 (17)	0.6197 (2)	1.0663 (3)	0.0788 (11)	0.500
C22A	0.1368 (2)	0.56239 (16)	1.0653 (2)	0.0527 (13)	0.500
C23A	0.20071 (17)	0.59708 (16)	1.0203 (2)	0.0459 (10)	0.500
N21B	0.18606 (12)	0.67712 (12)	0.99977 (12)	0.0231 (6)	0.500
C21B	0.20390 (16)	0.66238 (19)	1.08575 (14)	0.072 (2)	0.500
N22B	0.15044 (19)	0.60882 (19)	1.12370 (16)	0.0459 (12)	0.500
C22B	0.0953 (2)	0.5883 (2)	1.0580 (2)	0.112 (4)	0.500
C23B	0.11760 (17)	0.6305 (2)	0.98193 (17)	0.145 (5)	0.500
Co2	0.25000	0.25000	0.97768 (2)	0.0164 (1)
N31	0.17519 (5)	0.31710 (6)	0.88110 (6)	0.0227 (3)
C31	0.12860 (8)	0.29094 (10)	0.81402 (9)	0.0267 (4)
N32	0.08779 (8)	0.35334 (10)	0.77343 (8)	0.0317 (6)
C32	0.10969 (10)	0.42335 (10)	0.81726 (11)	0.0378 (8)
C33	0.16347 (9)	0.40061 (10)	0.88342 (10)	0.0331 (6)
N41	0.17999 (6)	0.30758 (6)	1.08299 (6)	0.0245 (3)
C41	0.20687 (10)	0.35920 (9)	1.14492 (10)	0.0337 (6)
N42	0.14497 (10)	0.38900 (9)	1.19684 (9)	0.0384 (5)
C42	0.07453 (10)	0.35429 (11)	1.16614 (12)	0.0537 (7)
C43	0.09652 (10)	0.30427 (11)	1.09610 (11)	0.0515 (8)
V1	0.42756 (2)	0.60114 (2)	0.89699 (2)	0.0151 (1)
V2	0.39602 (2)	0.42367 (2)	0.99204 (2)	0.0156 (1)
O1	0.34863 (8)	0.66289 (9)	0.91299 (10)	0.0251 (3)
O2	0.50087 (8)	0.61429 (9)	0.98825 (9)	0.0222 (3)
O3	0.46795 (10)	0.62287 (10)	0.79651 (10)	0.0319 (4)
O4	0.33553 (8)	0.34524 (8)	0.96819 (10)	0.0235 (3)
O5	0.39410 (9)	0.49404 (9)	0.89552 (9)	0.0245 (3)
O6	0.36269 (9)	0.46951 (9)	1.08507 (10)	0.0304 (3)
H1C11A	0.10857	0.75503	0.74665	0.070	0.500
H1N12A	0.07826	0.64945	0.63827	0.062	0.500
H1C12A	0.16743	0.53206	0.66260	0.086	0.500
H1C13A	0.25527	0.56997	0.79221	0.092	0.500
H1C11B	0.08051	0.71923	0.79181	0.044	0.500
H1N12B	0.06058	0.62639	0.66710	0.043	0.500
H1C12B	0.18673	0.55253	0.63475	0.036	0.500
H1C13B	0.28675	0.60425	0.74610	0.039	0.500
H1C21A	0.07558	0.73483	1.01363	0.137	0.500
H1N22A	0.02843	0.61432	1.09050	0.128	0.500
H1C22A	0.13467	0.50983	1.09040	0.075	0.500
H1C23A	0.25096	0.57157	1.00922	0.090	0.500
H1C21B	0.24797	0.68589	1.11689	0.229	0.500
H1N22B	0.15124	0.59104	1.17935	0.089	0.500
H1C22B	0.05109	0.55237	1.06392	0.236	0.500
H1C23B	0.09046	0.62826	0.92572	0.350	0.500
H1C31	0.12415	0.23611	0.79647	0.033
H1N32	0.05409	0.34936	0.72809	0.037
H1C32	0.09147	0.47636	0.80449	0.050
H1C33	0.18881	0.43638	0.92450	0.043
H1C41	0.26185	0.37360	1.15227	0.056
H1N42	0.14944	0.42364	1.24123	0.049
H1C42	0.02170	0.36305	1.18864	0.082
H1C43	0.06033	0.27230	1.06183	0.086

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0154 (2)	0.0174 (2)	0.0148 (2)	0.0007 (1)	0.0000 (1)	0.0000 (1)
N11A	0.0248 (14)	0.0267 (11)	0.0207 (7)	0.0000 (7)	−0.0050 (17)	−0.0011 (11)
C11A	0.0260 (13)	0.060 (2)	0.0327 (12)	0.0127 (13)	−0.0142 (12)	−0.0176 (13)
N12A	0.034 (2)	0.068 (3)	0.0329 (13)	−0.0044 (17)	−0.011 (2)	−0.0174 (18)
C12A	0.091 (5)	0.038 (2)	0.0386 (19)	−0.0066 (19)	−0.027 (5)	−0.010 (3)
C13A	0.091 (5)	0.027 (2)	0.040 (2)	0.0115 (15)	−0.033 (4)	−0.010 (3)
N11B	0.0179 (8)	0.0225 (8)	0.0185 (10)	0.0026 (7)	−0.0029 (5)	0.0003 (4)
C11B	0.020 (4)	0.040 (5)	0.029 (9)	0.005 (5)	−0.008 (3)	−0.0095 (11)
N12B	0.026 (4)	0.042 (4)	0.028 (7)	−0.001 (4)	−0.008 (2)	−0.0083 (11)
C12B	0.030 (2)	0.032 (2)	0.023 (3)	−0.002 (2)	−0.0026 (13)	−0.0056 (10)
C13B	0.025 (3)	0.029 (4)	0.025 (7)	0.004 (4)	−0.003 (2)	−0.0072 (10)
N21A	0.0280 (7)	0.0268 (8)	0.0274 (9)	0.0006 (7)	0.0052 (7)	0.0055 (6)
C21A	0.0499 (15)	0.058 (2)	0.114 (4)	0.0150 (11)	0.052 (2)	0.039 (2)
N22A	0.0596 (18)	0.070 (3)	0.107 (3)	−0.0024 (15)	0.045 (2)	0.039 (2)
C22A	0.064 (2)	0.0423 (15)	0.051 (2)	−0.0128 (16)	0.014 (2)	0.0183 (17)
C23A	0.0477 (15)	0.0344 (10)	0.056 (2)	0.0031 (13)	0.0108 (18)	0.0236 (14)
N21B	0.0258 (10)	0.0231 (9)	0.0204 (7)	−0.0001 (7)	0.0018 (5)	0.0017 (6)
C21B	0.053 (2)	0.127 (3)	0.0372 (10)	−0.042 (2)	−0.0169 (10)	0.0465 (15)
N22B	0.046 (2)	0.052 (2)	0.0398 (14)	0.0016 (16)	0.0111 (13)	0.0237 (15)
C22B	0.157 (5)	0.148 (5)	0.034 (2)	−0.125 (4)	0.006 (2)	0.008 (3)
C23B	0.164 (4)	0.238 (6)	0.0343 (18)	−0.175 (5)	−0.0253 (18)	0.037 (3)
Co2	0.0172 (2)	0.0148 (2)	0.0172 (2)	−0.0014 (1)	0.0000 (1)	0.0000 (1)
N31	0.0220 (5)	0.0232 (5)	0.0229 (4)	−0.0001 (3)	−0.0012 (3)	0.0008 (3)
C31	0.0231 (7)	0.0333 (5)	0.0237 (5)	−0.0012 (5)	−0.0034 (5)	0.0017 (4)
N32	0.0245 (6)	0.0441 (7)	0.0264 (5)	0.0042 (6)	−0.0015 (5)	0.0075 (5)
C32	0.0408 (9)	0.0361 (6)	0.0365 (7)	0.0110 (6)	−0.0054 (6)	0.0078 (5)
C33	0.0403 (9)	0.0244 (5)	0.0347 (7)	0.0057 (5)	−0.0076 (6)	0.0024 (4)
N41	0.0257 (4)	0.0232 (5)	0.0248 (4)	−0.0009 (4)	0.0024 (3)	−0.0041 (3)
C41	0.0390 (5)	0.0306 (8)	0.0314 (6)	−0.0072 (5)	0.0080 (5)	−0.0127 (6)
N42	0.0509 (8)	0.0302 (8)	0.0339 (6)	0.0004 (6)	0.0136 (6)	−0.0093 (6)
C42	0.0387 (6)	0.0724 (14)	0.0499 (9)	0.0072 (7)	0.0127 (7)	−0.0258 (9)
C43	0.0267 (5)	0.0770 (14)	0.0507 (9)	−0.0024 (5)	0.0089 (5)	−0.0322 (9)
V1	0.0139 (2)	0.0151 (2)	0.0163 (2)	0.0009 (1)	−0.0010 (1)	0.0020 (1)
V2	0.0148 (2)	0.0135 (2)	0.0184 (2)	−0.0006 (1)	−0.0022 (1)	−0.0017 (1)
O1	0.0189 (7)	0.0232 (7)	0.0331 (8)	0.0048 (6)	−0.0046 (6)	−0.0019 (6)
O2	0.0175 (7)	0.0249 (8)	0.0241 (7)	0.0019 (6)	−0.0052 (5)	−0.0025 (6)
O3	0.0274 (8)	0.0452 (10)	0.0232 (7)	0.0005 (7)	0.0039 (6)	0.0106 (6)
O4	0.0220 (7)	0.0176 (7)	0.0310 (7)	−0.0029 (6)	−0.0061 (6)	0.0000 (6)
O5	0.0314 (8)	0.0172 (7)	0.0249 (7)	−0.0037 (6)	−0.0078 (6)	0.0012 (5)
O6	0.0330 (9)	0.0266 (8)	0.0317 (8)	−0.0010 (7)	0.0082 (7)	−0.0094 (6)

Geometric parameters (Å, º)

Co1—N11A	2.130 (1)	N32—C32	1.352 (2)
Co1—N11A^i	2.130 (1)	C32—C33	1.352 (2)
Co1—N11B	2.130 (1)	N41—C41	1.307 (1)
Co1—N11B^i	2.130 (1)	N41—C43	1.371 (2)
Co1—N21A	2.108 (1)	C41—N42	1.348 (2)
Co1—N21A^i	2.108 (1)	N42—C42	1.352 (2)
Co1—N21B	2.107 (1)	C42—C43	1.352 (2)
Co1—N21B^i	2.107 (1)	V1—O1	1.646 (1)
Co1—O1	2.143 (1)	V1—O2	1.797 (1)
Co1—O1^i	2.143 (1)	V1—O3	1.641 (1)
N11A—C11A	1.307 (1)	V1—O5	1.824 (1)
N11A—C13A	1.371 (2)	V2—O2^iii	1.809 (1)
C11A—N12A	1.348 (2)	V2—O4	1.647 (1)
N12A—C12A	1.352 (2)	V2—O5	1.812 (1)
C12A—C13A	1.352 (2)	V2—O6	1.638 (1)
N11B—C11B	1.307 (1)	C11A—H1C11A	0.930
N11B—C13B	1.371 (2)	N12A—H1N12A	0.860
C11B—N12B	1.348 (2)	C12A—H1C12A	0.930
N12B—C12B	1.352 (2)	C13A—H1C13A	0.930
C12B—C13B	1.352 (2)	C11B—H1C11B	0.930
N21A—C21A	1.307 (1)	N12B—H1N12B	0.860
N21A—C23A	1.371 (2)	C12B—H1C12B	0.930
C21A—N22A	1.348 (2)	C13B—H1C13B	0.930
N22A—C22A	1.352 (2)	C21A—H1C21A	0.930
C22A—C23A	1.352 (2)	N22A—H1N22A	0.860
N21B—C21B	1.307 (1)	C22A—H1C22A	0.930
N21B—C23B	1.371 (2)	C23A—H1C23A	0.930
C21B—N22B	1.348 (2)	C21B—H1C21B	0.930
N22B—C22B	1.352 (2)	N22B—H1N22B	0.860
C22B—C23B	1.352 (2)	C22B—H1C22B	0.930
Co2—N31	2.155 (1)	C23B—H1C23B	0.930
Co2—N31^ii	2.155 (1)	C31—H1C31	0.930
Co2—N41	2.126 (1)	N32—H1N32	0.860
Co2—N41^ii	2.126 (1)	C32—H1C32	0.930
Co2—O4	2.085 (1)	C33—H1C33	0.930
Co2—O4^ii	2.085 (1)	C41—H1C41	0.930
N31—C31	1.307 (1)	N42—H1N42	0.860
N31—C33	1.371 (2)	C42—H1C42	0.930
C31—N32	1.348 (2)	C43—H1C43	0.930
N11A—Co1—N11A^i	85.7 (1)	N41—Co2—O4	94.5
N11A—Co1—N11B	0.8 (1)	N41—Co2—O4^ii	91.0
N11A—Co1—N11B^i	85.7 (1)	N41^ii—Co2—O4	91.0
N11A—Co1—N21A	85.5 (1)	N41^ii—Co2—O4^ii	94.5
N11A—Co1—N21A^i	170.5 (1)	O4—Co2—O4^ii	172.4 (1)
N11A—Co1—N21B	88.8 (1)	Co2—N31—C31	130.5 (1)
N11A—Co1—N21B^i	174.1 (1)	Co2—N31—C33	124.3 (1)
N11A—Co1—O1	90.8 (1)	C31—N31—C33	105.1 (1)
N11A—Co1—O1^i	94.5 (1)	N31—C31—N32	111.6 (1)
N11A^i—Co1—N11B	85.7 (1)	C31—N32—C32	107.3 (1)
N11A^i—Co1—N11B^i	0.8 (1)	N32—C32—C33	106.0 (1)
N11A^i—Co1—N21A	170.5 (1)	N31—C33—C32	110.1 (1)
N11A^i—Co1—N21A^i	85.5 (1)	Co2—N41—C41	126.9 (1)
N11A^i—Co1—N21B	174.1 (1)	Co2—N41—C43	127.8 (1)
N11A^i—Co1—N21B^i	88.8 (1)	C41—N41—C43	105.1 (1)
N11A^i—Co1—O1	94.5 (1)	N41—C41—N42	111.6 (1)
N11A^i—Co1—O1^i	90.8 (1)	C41—N42—C42	107.3 (1)
N11B—Co1—N11B^i	85.7 (1)	N42—C42—C43	106.0 (1)
N11B—Co1—N21A	85.5 (1)	N41—C43—C42	110.1 (1)
N11B—Co1—N21A^i	170.2 (1)	O1—V1—O2	109.9 (1)
N11B—Co1—N21B	88.8 (1)	O1—V1—O3	107.9 (1)
N11B—Co1—N21B^i	173.8 (1)	O1—V1—O5	110.6 (1)
N11B—Co1—O1	89.9 (1)	O2—V1—O3	111.6 (1)
N11B—Co1—O1^i	95.4 (1)	O2—V1—O5	108.7 (1)
N11B^i—Co1—N21A	170.2 (1)	O3—V1—O5	108.3 (1)
N11B^i—Co1—N21A^i	85.5 (1)	O2^iii—V2—O4	108.8 (1)
N11B^i—Co1—N21B	173.8 (1)	O2^iii—V2—O5	110.7 (1)
N11B^i—Co1—N21B^i	88.8 (1)	O2^iii—V2—O6	109.3 (1)
N11B^i—Co1—O1	95.4 (1)	O4—V2—O5	108.4 (1)
N11B^i—Co1—O1^i	89.9 (1)	O4—V2—O6	109.2 (1)
N21A—Co1—N21A^i	103.5 (1)	O5—V2—O6	110.4 (1)
N21A—Co1—N21B	3.6 (1)	Co1—O1—V1	167.8 (1)
N21A—Co1—N21B^i	100.2 (1)	V1—O2—V2^iii	133.7 (1)
N21A—Co1—O1	88.9 (1)	Co2—O4—V2	163.5 (1)
N21A—Co1—O1^i	86.6 (1)	V1—O5—V2	126.0 (1)
N21A^i—Co1—N21B	100.2 (1)	N11A—C11A—H1C11A	124.2
N21A^i—Co1—N21B^i	3.6 (1)	N12A—C11A—H1C11A	124.2
N21A^i—Co1—O1	86.6 (1)	C11A—N12A—H1N12A	126.4
N21A^i—Co1—O1^i	88.9 (1)	C12A—N12A—H1N12A	126.4
N21B—Co1—N21B^i	96.8 (1)	N12A—C12A—H1C12A	127.0
N21B—Co1—O1	87.5 (1)	C13A—C12A—H1C12A	127.0
N21B—Co1—O1^i	87.7 (1)	N11A—C13A—H1C13A	125.0
N21B^i—Co1—O1	87.7 (1)	C12A—C13A—H1C13A	125.0
N21B^i—Co1—O1^i	87.5 (1)	N11B—C11B—H1C11B	124.2
O1—Co1—O1^i	172.8 (1)	N12B—C11B—H1C11B	124.2
Co1—N11A—C11A	126.8 (1)	C11B—N12B—H1N12B	126.4
Co1—N11A—C13A	128.1 (1)	C12B—N12B—H1N12B	126.4
C11A—N11A—C13A	105.1 (1)	N12B—C12B—H1C12B	127.0
N11A—C11A—N12A	111.6 (1)	C13B—C12B—H1C12B	127.0
C11A—N12A—C12A	107.3 (1)	N11B—C13B—H1C13B	125.0
N12A—C12A—C13A	106.0 (1)	C12B—C13B—H1C13B	125.0
N11A—C13A—C12A	110.1 (1)	N21A—C21A—H1C21A	124.2
Co1—N11B—C11B	126.6 (1)	N22A—C21A—H1C21A	124.2
Co1—N11B—C13B	128.3 (1)	C21A—N22A—H1N22A	126.4
C11B—N11B—C13B	105.1 (1)	C22A—N22A—H1N22A	126.4
N11B—C11B—N12B	111.6 (1)	N22A—C22A—H1C22A	127.0
C11B—N12B—C12B	107.3 (1)	C23A—C22A—H1C22A	127.0
N12B—C12B—C13B	106.0 (1)	N21A—C23A—H1C23A	125.0
N11B—C13B—C12B	110.1 (1)	C22A—C23A—H1C23A	125.0
Co1—N21A—C21A	128.3 (1)	N21B—C21B—H1C21B	124.2
Co1—N21A—C23A	125.7 (1)	N22B—C21B—H1C21B	124.2
C21A—N21A—C23A	105.1 (1)	C21B—N22B—H1N22B	126.4
N21A—C21A—N22A	111.6 (1)	C22B—N22B—H1N22B	126.4
C21A—N22A—C22A	107.3 (1)	N22B—C22B—H1C22B	127.0
N22A—C22A—C23A	106.0 (1)	C23B—C22B—H1C22B	127.0
N21A—C23A—C22A	110.1 (1)	N21B—C23B—H1C23B	125.0
Co1—N21B—C21B	129.0 (1)	C22B—C23B—H1C23B	125.0
Co1—N21B—C23B	125.8 (1)	N31—C31—H1C31	124.2
C21B—N21B—C23B	105.1 (1)	N32—C31—H1C31	124.2
N21B—C21B—N22B	111.6 (1)	C31—N32—H1N32	126.4
C21B—N22B—C22B	107.3 (1)	C32—N32—H1N32	126.4
N22B—C22B—C23B	106.0 (1)	N32—C32—H1C32	127.0
N21B—C23B—C22B	110.1 (1)	C33—C32—H1C32	127.0
N31—Co2—N31^ii	98.6	N31—C33—H1C33	125.0
N31—Co2—N41	86.9	C32—C33—H1C33	125.0
N31—Co2—N41^ii	174.3	N41—C41—H1C41	124.2
N31—Co2—O4	87.6	N42—C41—H1C41	124.2
N31—Co2—O4^ii	87.5	C41—N42—H1N42	126.4
N31^ii—Co2—N41	174.3	C42—N42—H1N42	126.4
N31^ii—Co2—N41^ii	86.9	N42—C42—H1C42	127.0
N31^ii—Co2—O4	87.5	C43—C42—H1C42	127.0
N31^ii—Co2—O4^ii	87.6	N41—C43—H1C43	125.0
N41—Co2—N41^ii	87.7 (1)	C42—C43—H1C43	125.0

Symmetry codes: (i) −x+1/2, −y+3/2, z; (ii) −x+1/2, −y+1/2, z; (iii) −x+1, −y+1, −z+2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N12A—H1N12A···O6^iv	0.86	1.94	2.751 (3)	157
N12B—H1N12B···O6^iv	0.86	1.91	2.750 (2)	165
N22B—H1N22B···O3^v	0.86	2.01	2.843 (2)	163
N32—H1N32···O5^vi	0.86	2.09	2.873 (2)	151
N42—H1N42···O3^v	0.86	1.98	2.764 (2)	150
C11A—H1C11A···N22B^iv	0.93	2.36	2.957 (4)	122
C21B—H1C21B···C11A^vii	0.93	2.15	2.763 (4)	122
C21B—H1C21B···N12A^vii	0.93	2.26	2.899 (5)	125
C21B—H1C21B···N12B^vii	0.93	2.60	3.238 (4)	126

Symmetry codes: (iv) y−1/2, −x+1, z−1/2; (v) y−1/2, −x+1, z+1/2; (vi) −y+1/2, x, −z+3/2; (vii) −y+1, x+1/2, z+1/2.

catena-tetrakis(imidazole)-tetrakis(µ₂-oxo)-dioxo-cobalt(ii)-di-vanadium (Co_295K)

Crystal data

[Co(C3H4N2)4V2O6]	Dx = 1.819 Mg m^−3
Mr = 529.13	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P42/n	Cell parameters from 39470 reflections
Hall symbol: -P 4bc	θ = 2.6–30.0°
a = 16.2666 (3) Å	µ = 1.86 mm^−1
c = 14.6057 (2) Å	T = 295 K
V = 3864.70 (11) Å^3	Hexagonal, orange-red
Z = 8	0.25 × 0.19 × 0.18 mm
F(000) = 2012

Data collection

Enraf-Nonius KappaCCD diffractometer	5657 independent reflections
Radiation source: fine-focus sealed tube	3905 reflections with I > 3σ(I)
Graphite monochromator	Rint = 0.059
φ scan plus ω scans with κ offsets	θmax = 30.0°, θmin = 2.8°
Absorption correction: multi-scan multi-scan from symmetry-related measurements Sortav (Blessing 1995)	h = −22→22
Tmin = 0.662, Tmax = 0.720	k = −22→22
57596 measured reflections	l = −20→20

Refinement

Refinement on F	6 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.033	w = 1/[σ(F)^2 + (0.0004F)^2]
wR(F^2) = 0.047	(Δ/σ)max = 0.2
S = 1.56	Δρmax = 0.72 e Å^−3
3905 reflections	Δρmin = −0.55 e Å^−3
174 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Co1	0.25000	0.75000	0.90202 (3)	0.0222 (1)
N11A	0.19377 (15)	0.68061 (14)	0.79551 (13)	0.0335 (16)	0.500
C11A	0.1362 (2)	0.7058 (2)	0.7402 (2)	0.0447 (17)	0.500
N12A	0.1150 (3)	0.6471 (3)	0.6797 (2)	0.058 (3)	0.500
C12A	0.1617 (3)	0.5809 (2)	0.6976 (3)	0.069 (4)	0.500
C13A	0.2102 (3)	0.60155 (18)	0.7689 (2)	0.057 (3)	0.500
N11B	0.19611 (13)	0.67881 (13)	0.79545 (12)	0.0287 (6)	0.500
C11B	0.12080 (17)	0.6844 (2)	0.76572 (19)	0.039 (4)	0.500
N12B	0.1070 (2)	0.6327 (3)	0.6954 (2)	0.045 (3)	0.500
C12B	0.1775 (3)	0.5920 (2)	0.67961 (19)	0.042 (3)	0.500
C13B	0.2323 (2)	0.62042 (19)	0.74120 (19)	0.036 (4)	0.500
N21A	0.18201 (15)	0.67578 (15)	0.99257 (16)	0.0369 (7)	0.500
C21A	0.1102 (2)	0.6898 (2)	1.0288 (3)	0.0968 (15)	0.500
N22A	0.0812 (2)	0.6231 (3)	1.0729 (3)	0.1036 (18)	0.500
C22A	0.1378 (3)	0.56344 (19)	1.0641 (3)	0.0627 (18)	0.500
C23A	0.1998 (2)	0.59591 (19)	1.0147 (3)	0.0524 (15)	0.500
N21B	0.18558 (16)	0.67723 (15)	0.99713 (15)	0.0317 (9)	0.500
C21B	0.2059 (2)	0.6553 (3)	1.07988 (18)	0.119 (4)	0.500
N22B	0.1497 (3)	0.6044 (3)	1.1169 (2)	0.077 (2)	0.500
C22B	0.0903 (3)	0.5935 (3)	1.0540 (3)	0.135 (6)	0.500
C23B	0.1124 (2)	0.6383 (3)	0.9804 (2)	0.182 (7)	0.500
Co2	0.25000	0.25000	0.97838 (3)	0.0224 (1)
N31	0.17479 (7)	0.31674 (7)	0.88151 (7)	0.0308 (4)
C31	0.12873 (10)	0.29046 (12)	0.81465 (11)	0.0384 (6)
N32	0.08763 (10)	0.35249 (12)	0.77426 (10)	0.0456 (8)
C32	0.10879 (12)	0.42206 (13)	0.81796 (13)	0.0529 (10)
C33	0.16241 (12)	0.40001 (12)	0.88392 (13)	0.0460 (8)
N41	0.17958 (8)	0.30733 (7)	1.08344 (8)	0.0331 (4)
C41	0.20595 (12)	0.35910 (11)	1.14484 (12)	0.0451 (7)
N42	0.14393 (13)	0.38866 (11)	1.19626 (11)	0.0538 (7)
C42	0.07427 (13)	0.35367 (14)	1.16577 (15)	0.0692 (9)
C43	0.09626 (12)	0.30365 (14)	1.09637 (14)	0.0633 (10)
V1	0.42797 (2)	0.60023 (2)	0.89587 (2)	0.0209 (1)
V2	0.39579 (2)	0.42372 (2)	0.99242 (2)	0.0217 (1)
O1	0.34924 (10)	0.66201 (10)	0.91133 (12)	0.0341 (4)
O2	0.50149 (10)	0.61383 (10)	0.98644 (11)	0.0309 (4)
O3	0.46807 (11)	0.62076 (13)	0.79581 (12)	0.0443 (5)
O4	0.33543 (10)	0.34556 (9)	0.96874 (12)	0.0327 (4)
O5	0.39450 (11)	0.49343 (10)	0.89594 (11)	0.0332 (4)
O6	0.36195 (11)	0.46996 (11)	1.08391 (12)	0.0427 (5)
H1C11A	0.11271	0.75789	0.74223	0.059	0.500
H1N12A	0.07840	0.65117	0.63743	0.073	0.500
H1C12A	0.16083	0.53076	0.66695	0.097	0.500
H1C13A	0.24893	0.56726	0.79592	0.080	0.500
H1C11B	0.08149	0.71968	0.79004	0.051	0.500
H1N12B	0.06150	0.62677	0.66606	0.058	0.500
H1C12B	0.18662	0.55217	0.63508	0.052	0.500
H1C13B	0.28654	0.60298	0.74611	0.047	0.500
H1C21A	0.08239	0.73960	1.02476	0.173	0.500
H1N22A	0.03501	0.61938	1.10132	0.166	0.500
H1C22A	0.13476	0.51034	1.08746	0.084	0.500
H1C23A	0.24753	0.56820	0.99810	0.098	0.500
H1C21B	0.25337	0.67258	1.10970	0.357	0.500
H1N22B	0.15139	0.58297	1.17064	0.153	0.500
H1C22B	0.04327	0.56143	1.06014	0.288	0.500
H1C23B	0.08252	0.64221	0.92632	0.457	0.500
H1C31	0.12475	0.23567	0.79702	0.049
H1N32	0.05410	0.34836	0.72897	0.055
H1C32	0.09015	0.47488	0.80522	0.071
H1C33	0.18728	0.43597	0.92495	0.062
H1C41	0.26080	0.37381	1.15224	0.069
H1N42	0.14812	0.42343	1.24038	0.069
H1C42	0.02142	0.36226	1.18811	0.102
H1C43	0.06023	0.27144	1.06234	0.100

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0211 (2)	0.0238 (2)	0.0218 (2)	0.0008 (2)	0.0000 (1)	0.0000 (1)
N11A	0.0338 (19)	0.037 (2)	0.0299 (7)	0.0000 (7)	−0.007 (3)	−0.002 (3)
C11A	0.030 (2)	0.068 (3)	0.0360 (12)	0.0088 (14)	−0.011 (3)	−0.013 (3)
N12A	0.049 (4)	0.083 (4)	0.0441 (14)	−0.007 (2)	−0.015 (5)	−0.019 (5)
C12A	0.106 (6)	0.052 (4)	0.0490 (19)	−0.013 (2)	−0.027 (7)	−0.012 (6)
C13A	0.096 (5)	0.034 (3)	0.0418 (17)	0.0026 (12)	−0.024 (5)	−0.006 (5)
N11B	0.0262 (9)	0.0328 (8)	0.0270 (8)	0.0020 (8)	−0.0033 (6)	−0.0004 (5)
C11B	0.027 (5)	0.055 (5)	0.035 (10)	0.001 (6)	−0.007 (5)	−0.009 (2)
N12B	0.037 (4)	0.061 (4)	0.037 (7)	−0.007 (4)	−0.008 (4)	−0.0104 (17)
C12B	0.047 (4)	0.045 (4)	0.035 (7)	−0.004 (4)	−0.005 (4)	−0.0092 (16)
C13B	0.039 (6)	0.038 (5)	0.034 (11)	0.005 (6)	−0.005 (6)	−0.0078 (18)
N21A	0.0372 (10)	0.0368 (11)	0.0368 (11)	0.0002 (8)	0.0067 (11)	0.0067 (9)
C21A	0.075 (2)	0.075 (3)	0.141 (4)	0.0207 (17)	0.073 (3)	0.046 (3)
N22A	0.084 (3)	0.091 (4)	0.136 (4)	0.000 (2)	0.063 (3)	0.049 (4)
C22A	0.079 (3)	0.055 (2)	0.055 (3)	−0.0199 (19)	0.010 (3)	0.018 (2)
C23A	0.061 (2)	0.0401 (13)	0.056 (2)	−0.0003 (14)	0.009 (2)	0.0190 (16)
N21B	0.0336 (13)	0.0319 (13)	0.0296 (9)	0.0005 (9)	0.0032 (7)	0.0025 (9)
C21B	0.067 (3)	0.218 (6)	0.0742 (18)	−0.060 (4)	−0.0281 (17)	0.097 (3)
N22B	0.065 (3)	0.095 (4)	0.070 (2)	−0.002 (3)	0.015 (2)	0.050 (3)
C22B	0.167 (6)	0.190 (7)	0.049 (3)	−0.140 (6)	0.002 (3)	0.019 (4)
C23B	0.165 (5)	0.322 (9)	0.058 (3)	−0.198 (6)	−0.043 (3)	0.073 (4)
Co2	0.0231 (2)	0.0207 (2)	0.0235 (2)	−0.0023 (2)	0.0000 (1)	0.0000 (1)
N31	0.0295 (6)	0.0317 (6)	0.0313 (5)	−0.0007 (5)	−0.0025 (4)	0.0008 (4)
C31	0.0336 (9)	0.0473 (7)	0.0342 (7)	−0.0023 (7)	−0.0079 (7)	0.0021 (6)
N32	0.0348 (9)	0.0643 (11)	0.0377 (7)	0.0061 (8)	−0.0041 (7)	0.0110 (7)
C32	0.0566 (13)	0.0522 (8)	0.0498 (11)	0.0170 (9)	−0.0067 (9)	0.0115 (8)
C33	0.0566 (12)	0.0337 (6)	0.0477 (10)	0.0088 (7)	−0.0106 (8)	0.0032 (5)
N41	0.0349 (6)	0.0303 (6)	0.0342 (5)	−0.0024 (5)	0.0029 (4)	−0.0062 (4)
C41	0.0533 (8)	0.0401 (11)	0.0418 (7)	−0.0087 (7)	0.0088 (6)	−0.0171 (8)
N42	0.0706 (11)	0.0428 (10)	0.0478 (8)	0.0004 (9)	0.0183 (8)	−0.0148 (8)
C42	0.0543 (8)	0.0859 (18)	0.0674 (12)	0.0077 (10)	0.0195 (10)	−0.0295 (11)
C43	0.0366 (6)	0.0877 (18)	0.0656 (12)	−0.0036 (7)	0.0122 (7)	−0.0349 (12)
V1	0.0192 (2)	0.0208 (2)	0.0226 (2)	0.0010 (2)	−0.0010 (1)	0.0026 (1)
V2	0.0204 (2)	0.0187 (2)	0.0261 (2)	−0.0015 (2)	−0.0033 (1)	−0.0023 (1)
O1	0.0256 (9)	0.0318 (10)	0.0450 (10)	0.0063 (8)	−0.0056 (7)	−0.0036 (8)
O2	0.0250 (9)	0.0339 (10)	0.0337 (9)	0.0013 (7)	−0.0075 (7)	−0.0030 (7)
O3	0.0390 (11)	0.0622 (13)	0.0319 (10)	0.0018 (10)	0.0078 (8)	0.0137 (9)
O4	0.0304 (10)	0.0233 (9)	0.0443 (10)	−0.0054 (7)	−0.0074 (8)	−0.0008 (7)
O5	0.0419 (11)	0.0240 (9)	0.0337 (9)	−0.0044 (8)	−0.0114 (8)	0.0018 (7)
O6	0.0481 (12)	0.0384 (11)	0.0415 (10)	0.0001 (9)	0.0103 (9)	−0.0127 (9)

Geometric parameters (Å, º)

Co1—N11A	2.129 (1)	N32—C32	1.344 (3)
Co1—N11A^i	2.129 (1)	C32—C33	1.348 (2)
Co1—N11B	2.129 (1)	N41—C41	1.303 (2)
Co1—N11B^i	2.129 (1)	N41—C43	1.370 (2)
Co1—N21A	2.105 (1)	C41—N42	1.346 (2)
Co1—N21A^i	2.105 (1)	N42—C42	1.344 (3)
Co1—N21B	2.104 (1)	C42—C43	1.348 (2)
Co1—N21B^i	2.104 (1)	V1—O1	1.643 (2)
Co1—O1	2.162 (2)	V1—O2	1.797 (2)
Co1—O1^i	2.162 (2)	V1—O3	1.635 (2)
N11A—C11A	1.303 (2)	V1—O5	1.821 (2)
N11A—C13A	1.370 (2)	V2—O2^iii	1.806 (2)
C11A—N12A	1.346 (2)	V2—O4	1.643 (2)
N12A—C12A	1.344 (3)	V2—O5	1.809 (2)
C12A—C13A	1.348 (2)	V2—O6	1.629 (2)
N11B—C11B	1.303 (2)	C11A—H1C11A	0.930
N11B—C13B	1.370 (2)	N12A—H1N12A	0.860
C11B—N12B	1.346 (2)	C12A—H1C12A	0.930
N12B—C12B	1.344 (3)	C13A—H1C13A	0.930
C12B—C13B	1.348 (2)	C11B—H1C11B	0.930
N21A—C21A	1.303 (2)	N12B—H1N12B	0.860
N21A—C23A	1.370 (2)	C12B—H1C12B	0.930
C21A—N22A	1.346 (2)	C13B—H1C13B	0.930
N22A—C22A	1.344 (3)	C21A—H1C21A	0.930
C22A—C23A	1.348 (2)	N22A—H1N22A	0.860
N21B—C21B	1.303 (2)	C22A—H1C22A	0.930
N21B—C23B	1.370 (2)	C23A—H1C23A	0.930
C21B—N22B	1.346 (2)	C21B—H1C21B	0.930
N22B—C22B	1.344 (3)	N22B—H1N22B	0.860
C22B—C23B	1.348 (2)	C22B—H1C22B	0.930
Co2—N31	2.163 (1)	C23B—H1C23B	0.930
Co2—N31^ii	2.163 (1)	C31—H1C31	0.930
Co2—N41	2.130 (1)	N32—H1N32	0.860
Co2—N41^ii	2.130 (1)	C32—H1C32	0.930
Co2—O4	2.090 (2)	C33—H1C33	0.930
Co2—O4^ii	2.090 (2)	C41—H1C41	0.930
N31—C31	1.303 (2)	N42—H1N42	0.860
N31—C33	1.370 (2)	C42—H1C42	0.930
C31—N32	1.346 (2)	C43—H1C43	0.930
Co1···V2	5.961	C12B···C21A^v	3.099 (6)
Co1···V2^i	5.961	C12B···C21B^iv	3.614 (5)
C11A···N22B^iv	3.007 (6)	C12B···C32	3.602 (4)
C11A···C13B^i	3.545 (5)	C12B···O2^iv	3.368 (3)
C11A···C21B^iv	2.764 (5)	C13B···C21A^v	3.355 (5)
C11A···O3^i	3.391 (4)	C13B···N22A^v	3.462 (6)
N12A···O6^iv	2.747 (3)	C13B···C21B^v	3.291 (5)
N12A···C21B^iv	2.876 (6)	C22A···O3^vii	3.434 (4)
C12A···C21A^v	3.484 (7)	N22B···O3^vii	2.906 (3)
C12A···C32	3.241 (5)	C31···C31^viii	3.495 (3)
C13A···C23A	3.595 (5)	C31···C31^ix	3.495 (3)
C13A···C23B	3.526 (5)	C31···C32^ix	3.629 (3)
C13A···C32	3.429 (4)	C31···C33^ix	3.601 (2)
C11B···C21B^iv	3.297 (5)	N32···O5^ix	2.896 (2)
C11B···C23B	3.227 (5)	C33···C43	3.639 (3)
C11B···C42^vi	3.384 (4)	C41···O6	3.238 (3)
N12B···O6^iv	2.761 (3)	N42···O3^vii	2.773 (2)
N12B···C21B^iv	3.219 (5)	V1···V1^iii	5.038 (1)
N11A—Co1—N11A^i	86.1 (1)	N41—Co2—O4	94.6 (1)
N11A—Co1—N11B	1.3 (1)	N41—Co2—O4^ii	90.9 (1)
N11A—Co1—N11B^i	86.0 (1)	N41^ii—Co2—O4	90.9 (1)
N11A—Co1—N21A	85.9 (1)	N41^ii—Co2—O4^ii	94.6 (1)
N11A—Co1—N21A^i	171.6 (1)	O4—Co2—O4^ii	172.3 (1)
N11A—Co1—N21B	88.3 (1)	Co2—N31—C31	130.6 (1)
N11A—Co1—N21B^i	174.1 (1)	Co2—N31—C33	124.2 (1)
N11A—Co1—O1	90.9 (1)	C31—N31—C33	105.0 (1)
N11A—Co1—O1^i	94.4 (1)	N31—C31—N32	111.6 (1)
N11A^i—Co1—N11B	86.0 (1)	C31—N32—C32	107.2 (1)
N11A^i—Co1—N11B^i	1.3 (1)	N32—C32—C33	106.3 (2)
N11A^i—Co1—N21A	171.6 (1)	N31—C33—C32	109.9 (2)
N11A^i—Co1—N21A^i	85.9 (1)	Co2—N41—C41	127.0 (1)
N11A^i—Co1—N21B	174.1 (1)	Co2—N41—C43	127.8 (1)
N11A^i—Co1—N21B^i	88.3 (1)	C41—N41—C43	105.0 (1)
N11A^i—Co1—O1	94.4 (1)	N41—C41—N42	111.6 (1)
N11A^i—Co1—O1^i	90.9 (1)	C41—N42—C42	107.2 (1)
N11B—Co1—N11B^i	86.0 (1)	N42—C42—C43	106.3 (2)
N11B—Co1—N21A	86.0 (1)	N41—C43—C42	109.9 (2)
N11B—Co1—N21A^i	171.0 (1)	O1—V1—O2	110.0 (1)
N11B—Co1—N21B	88.4 (1)	O1—V1—O3	108.0 (1)
N11B—Co1—N21B^i	173.5 (1)	O1—V1—O5	110.5 (1)
N11B—Co1—O1	89.6 (1)	O2—V1—O3	111.6 (1)
N11B—Co1—O1^i	95.7 (1)	O2—V1—O5	108.4 (1)
N11B^i—Co1—N21A	171.0 (1)	O3—V1—O5	108.3 (1)
N11B^i—Co1—N21A^i	86.0 (1)	O2^iii—V2—O4	109.1 (1)
N11B^i—Co1—N21B	173.5 (1)	O2^iii—V2—O5	110.9 (1)
N11B^i—Co1—N21B^i	88.4 (1)	O2^iii—V2—O6	109.2 (1)
N11B^i—Co1—O1	95.7 (1)	O4—V2—O5	108.3 (1)
N11B^i—Co1—O1^i	89.6 (1)	O4—V2—O6	109.1 (1)
N21A—Co1—N21A^i	102.1 (2)	O5—V2—O6	110.2 (1)
N21A—Co1—N21B	2.5 (1)	Co1—O1—V1	168.0 (1)
N21A—Co1—N21B^i	99.8 (1)	V1—O2—V2^iii	134.4 (1)
N21A—Co1—O1	88.5 (1)	Co2—O4—V2	163.5 (1)
N21A—Co1—O1^i	87.0 (1)	V1—O5—V2	126.5 (1)
N21A^i—Co1—N21B	99.8 (1)	N11A—C11A—H1C11A	124.2
N21A^i—Co1—N21B^i	2.5 (1)	N12A—C11A—H1C11A	124.2
N21A^i—Co1—O1	87.0 (1)	C11A—N12A—H1N12A	126.4
N21A^i—Co1—O1^i	88.5 (1)	C12A—N12A—H1N12A	126.4
N21B—Co1—N21B^i	97.4 (1)	N12A—C12A—H1C12A	126.8
N21B—Co1—O1	87.6 (1)	C13A—C12A—H1C12A	126.8
N21B—Co1—O1^i	87.7 (1)	N11A—C13A—H1C13A	125.1
N21B^i—Co1—O1	87.7 (1)	C12A—C13A—H1C13A	125.1
N21B^i—Co1—O1^i	87.6 (1)	N11B—C11B—H1C11B	124.2
O1—Co1—O1^i	172.8 (1)	N12B—C11B—H1C11B	124.2
Co1—N11A—C11A	126.5 (1)	C11B—N12B—H1N12B	126.4
Co1—N11A—C13A	128.4 (1)	C12B—N12B—H1N12B	126.4
C11A—N11A—C13A	105.0 (1)	N12B—C12B—H1C12B	126.8
N11A—C11A—N12A	111.6 (1)	C13B—C12B—H1C12B	126.8
C11A—N12A—C12A	107.2 (1)	N11B—C13B—H1C13B	125.1
N12A—C12A—C13A	106.3 (2)	C12B—C13B—H1C13B	125.1
N11A—C13A—C12A	109.9 (2)	N21A—C21A—H1C21A	124.2
Co1—N11B—C11B	126.4 (1)	N22A—C21A—H1C21A	124.2
Co1—N11B—C13B	128.6 (1)	C21A—N22A—H1N22A	126.4
C11B—N11B—C13B	105.0 (1)	C22A—N22A—H1N22A	126.4
N11B—C11B—N12B	111.6 (1)	N22A—C22A—H1C22A	126.8
C11B—N12B—C12B	107.2 (1)	C23A—C22A—H1C22A	126.8
N12B—C12B—C13B	106.3 (2)	N21A—C23A—H1C23A	125.1
N11B—C13B—C12B	109.9 (2)	C22A—C23A—H1C23A	125.1
Co1—N21A—C21A	128.8 (2)	N21B—C21B—H1C21B	124.2
Co1—N21A—C23A	125.5 (2)	N22B—C21B—H1C21B	124.2
C21A—N21A—C23A	105.0 (1)	C21B—N22B—H1N22B	126.4
N21A—C21A—N22A	111.6 (1)	C22B—N22B—H1N22B	126.4
C21A—N22A—C22A	107.2 (1)	N22B—C22B—H1C22B	126.8
N22A—C22A—C23A	106.3 (2)	C23B—C22B—H1C22B	126.8
N21A—C23A—C22A	109.9 (2)	N21B—C23B—H1C23B	125.1
Co1—N21B—C21B	129.8 (2)	C22B—C23B—H1C23B	125.1
Co1—N21B—C23B	125.1 (2)	N31—C31—H1C31	124.2
C21B—N21B—C23B	105.0 (1)	N32—C31—H1C31	124.2
N21B—C21B—N22B	111.6 (1)	C31—N32—H1N32	126.4
C21B—N22B—C22B	107.2 (1)	C32—N32—H1N32	126.4
N22B—C22B—C23B	106.3 (2)	N32—C32—H1C32	126.8
N21B—C23B—C22B	109.9 (2)	C33—C32—H1C32	126.8
N31—Co2—N31^ii	98.3 (1)	N31—C33—H1C33	125.1
N31—Co2—N41	87.0	C32—C33—H1C33	125.1
N31—Co2—N41^ii	174.5	N41—C41—H1C41	124.2
N31—Co2—O4	87.6 (1)	N42—C41—H1C41	124.2
N31—Co2—O4^ii	87.3 (1)	C41—N42—H1N42	126.4
N31^ii—Co2—N41	174.5	C42—N42—H1N42	126.4
N31^ii—Co2—N41^ii	87.0	N42—C42—H1C42	126.8
N31^ii—Co2—O4	87.3 (1)	C43—C42—H1C42	126.8
N31^ii—Co2—O4^ii	87.6 (1)	N41—C43—H1C43	125.1
N41—Co2—N41^ii	87.8 (1)	C42—C43—H1C43	125.1

Symmetry codes: (i) −x+1/2, −y+3/2, z; (ii) −x+1/2, −y+1/2, z; (iii) −x+1, −y+1, −z+2; (iv) y−1/2, −x+1, z−1/2; (v) −y+1, x+1/2, z−1/2; (vi) −x, −y+1, −z+2; (vii) y−1/2, −x+1, z+1/2; (viii) y, −x+1/2, −z+3/2; (ix) −y+1/2, x, −z+3/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N12A—H1N12A···O6^iv	0.86	1.94	2.747 (3)	155
N12B—H1N12B···O6^iv	0.86	1.92	2.761 (3)	165
N22B—H1N22B···O3^vii	0.86	2.07	2.906 (3)	164
N32—H1N32···O5^ix	0.86	2.12	2.896 (2)	150
N42—H1N42···O3^vii	0.86	1.99	2.773 (2)	150

Symmetry codes: (iv) y−1/2, −x+1, z−1/2; (vii) y−1/2, −x+1, z+1/2; (ix) −y+1/2, x, −z+3/2.

catena-tetrakis(imidazole)-tetrakis(µ₂-oxo)-dioxo-nickel(ii)-di-vanadium (Ni_100K)

Crystal data

[Ni(C3H4N2)4V2O6]	F(000) = 2128
Mr = 528.90	Dx = 1.855 Mg m^−3
Monoclinic, P2/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yac	Cell parameters from 69838 reflections
a = 16.1379 (3) Å	θ = 2.6–30.0°
b = 14.3657 (2) Å	µ = 2.00 mm^−1
c = 16.3422 (4) Å	T = 100 K
β = 90.1205 (9)°	Hexagonal, blue
V = 3788.64 (13) Å^3	0.40 × 0.21 × 0.18 mm
Z = 8

Data collection

Enraf-Nonius KappaCCD diffractometer	11073 independent reflections
Radiation source: fine-focus sealed tube	9089 reflections with I > 3σ(I)
Graphite monochromator	Rint = 0.055
φ scan plus ω scans with κ offsets	θmax = 30.1°, θmin = 2.8°
Absorption correction: multi-scan from symmetry-related measurements Sortav (Blessing 1995)	h = −22→22
Tmin = 0.619, Tmax = 0.712	k = −20→19
53813 measured reflections	l = −23→23

Refinement

Refinement on F	0 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.039	w = 1/[σ(F)^2 + (0.0004F)^2]
wR(F^2) = 0.053	(Δ/σ)max = 0.2
S = 1.67	Δρmax = 2.30 e Å^−3
9089 reflections	Δρmin = −2.32 e Å^−3
287 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.25000	0.90166 (3)	0.75000	0.0069 (1)
Ni2	0.25000	0.98779 (3)	0.25000	0.0066 (1)
Ni3	0.25000	0.40531 (3)	0.75000	0.0066 (1)
Ni4	0.75000	0.47054 (3)	0.75000	0.0069 (1)
V1	0.42482 (3)	0.89545 (3)	0.59941 (3)	0.0064 (1)
V2	0.39388 (3)	0.99993 (3)	0.42503 (3)	0.0066 (1)
V3	0.39569 (3)	0.39805 (3)	0.92821 (3)	0.0062 (1)
V4	0.57793 (3)	0.48757 (3)	0.89692 (3)	0.0069 (1)
O1	0.34753 (11)	0.90897 (13)	0.66440 (12)	0.0113 (4)
O2	0.50135 (11)	0.98625 (13)	0.61246 (12)	0.0107 (4)
O3	0.46567 (12)	0.79194 (13)	0.61348 (14)	0.0163 (4)
O4	0.33161 (11)	0.98094 (13)	0.34664 (12)	0.0110 (4)
O5	0.38636 (12)	0.90085 (12)	0.49402 (12)	0.0116 (4)
O6	0.36548 (12)	1.09651 (13)	0.47065 (13)	0.0140 (4)
O7	0.33536 (11)	0.41572 (13)	0.84841 (12)	0.0109 (4)
O8	0.38333 (12)	0.49179 (13)	1.00010 (12)	0.0113 (4)
O9	0.36916 (12)	0.29721 (13)	0.96864 (12)	0.0143 (4)
O10	0.65556 (11)	0.46087 (13)	0.83571 (12)	0.0103 (4)
O11	0.50368 (11)	0.39212 (13)	0.89621 (12)	0.0113 (4)
O12	0.53323 (12)	0.58179 (14)	0.86300 (13)	0.0152 (4)
N11	0.19238 (10)	0.79761 (11)	0.68415 (10)	0.0105 (4)
C11	0.14133 (11)	0.73467 (13)	0.71545 (10)	0.0148 (5)
N12	0.11172 (11)	0.67764 (11)	0.65649 (12)	0.0171 (7)
C12	0.14570 (14)	0.70578 (14)	0.58400 (11)	0.0191 (6)
C13	0.19528 (12)	0.77971 (14)	0.60167 (11)	0.0176 (4)
N21	0.18562 (11)	0.99728 (12)	0.68108 (12)	0.0117 (5)
C21	0.21508 (11)	1.07244 (14)	0.64403 (14)	0.0248 (14)
N22	0.15670 (14)	1.11190 (13)	0.59584 (13)	0.0248 (14)
C22	0.08653 (13)	1.05908 (16)	0.60261 (17)	0.0316 (11)
C23	0.10496 (12)	0.98867 (15)	0.65524 (17)	0.0326 (10)
N31	0.17545 (10)	0.89109 (11)	0.31202 (10)	0.0099 (4)
C31	0.12914 (11)	0.82255 (12)	0.28246 (10)	0.0112 (4)
N32	0.08513 (10)	0.78127 (11)	0.34264 (12)	0.0140 (3)
C32	0.10446 (12)	0.82588 (14)	0.41411 (10)	0.0149 (6)
C33	0.16013 (12)	0.89340 (12)	0.39462 (11)	0.0121 (7)
N41	0.17833 (10)	1.09014 (11)	0.30376 (11)	0.0102 (8)
C41	0.20224 (9)	1.15028 (13)	0.36070 (12)	0.0127 (6)
N42	0.13817 (11)	1.20408 (12)	0.38503 (11)	0.0154 (12)
C42	0.07004 (10)	1.17671 (14)	0.34130 (14)	0.017 (2)
C43	0.09540 (11)	1.10650 (13)	0.29142 (13)	0.0146 (18)
N51	0.32236 (10)	0.30056 (11)	0.69821 (10)	0.0101 (4)
C51	0.32133 (11)	0.27421 (13)	0.62041 (10)	0.0129 (5)
N52	0.37466 (11)	0.20319 (12)	0.60760 (10)	0.0141 (6)
C52	0.41146 (11)	0.18339 (12)	0.68102 (12)	0.0149 (7)
C53	0.37885 (12)	0.24372 (13)	0.73644 (10)	0.0141 (6)
N61	0.32363 (11)	0.49977 (13)	0.68989 (12)	0.0140 (4)
C61	0.40542 (12)	0.50658 (15)	0.69547 (13)	0.0202 (5)
N62	0.43556 (11)	0.56477 (17)	0.63777 (16)	0.0275 (9)
C62	0.36952 (14)	0.59655 (16)	0.59324 (14)	0.0336 (11)
C63	0.30087 (11)	0.55613 (16)	0.62581 (14)	0.0270 (7)
N71	0.68530 (10)	0.37428 (11)	0.67703 (10)	0.0103 (3)
C71	0.71254 (9)	0.30655 (13)	0.62890 (11)	0.0117 (4)
N72	0.64949 (11)	0.26781 (11)	0.58632 (11)	0.0146 (6)
C72	0.57854 (10)	0.31325 (14)	0.60854 (13)	0.0158 (5)
C73	0.60123 (10)	0.37869 (13)	0.66442 (12)	0.0129 (3)
N81	0.69230 (11)	0.57485 (11)	0.68242 (11)	0.0114 (2)
C81	0.64662 (12)	0.64330 (13)	0.71290 (10)	0.0142 (4)
N82	0.61354 (11)	0.69570 (11)	0.65243 (12)	0.0180 (4)
C82	0.63953 (13)	0.65864 (15)	0.57979 (11)	0.0209 (6)
C83	0.68800 (13)	0.58425 (14)	0.59890 (11)	0.0176 (6)
H1C11	0.12773	0.73037	0.77060	0.022
H1N12	0.07781	0.63211	0.66328	0.022
H1C12	0.13669	0.67955	0.53272	0.027
H1C13	0.22634	0.81298	0.56375	0.027
H1C21	0.26874	1.09498	0.65038	0.053
H1N22	0.16257	1.16106	0.56639	0.038
H1C22	0.03614	1.06930	0.57639	0.054
H1C23	0.06857	0.94192	0.67124	0.066
H1C31	0.12722	0.80522	0.22766	0.011
H1N32	0.05127	0.73547	0.33704	0.016
H1C32	0.08365	0.81266	0.46584	0.018
H1C33	0.18410	0.93473	0.43152	0.013
H1C41	0.25591	1.15482	0.38114	0.016
H1N42	0.13990	1.24745	0.42126	0.019
H1C42	0.01685	1.20126	0.34495	0.022
H1C43	0.06178	1.07454	0.25465	0.019
H1C51	0.28833	0.30103	0.58009	0.017
H1N52	0.38376	0.17558	0.56179	0.017
H1C52	0.45100	0.13768	0.69108	0.019
H1C53	0.39267	0.24610	0.79168	0.019
H1C61	0.43770	0.47548	0.73394	0.028
H1N62	0.48674	0.57913	0.63042	0.035
H1C62	0.37122	0.63770	0.54934	0.049
H1C63	0.24687	0.56526	0.60750	0.039
H1C71	0.76765	0.28820	0.62499	0.012
H1N72	0.65327	0.22294	0.55170	0.017
H1C72	0.52527	0.30169	0.58924	0.019
H1C73	0.56536	0.42002	0.69011	0.014
H1C81	0.63846	0.65381	0.76846	0.018
H1N82	0.58201	0.74345	0.65849	0.022
H1C82	0.62661	0.68008	0.52760	0.028
H1C83	0.71417	0.54572	0.56123	0.023

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0063 (2)	0.0076 (2)	0.0068 (2)	0.0000 (1)	0.0000 (2)	0.0000 (1)
Ni2	0.0063 (2)	0.0077 (2)	0.0059 (2)	0.0000 (1)	−0.0015 (2)	0.0000 (1)
Ni3	0.0065 (2)	0.0080 (2)	0.0054 (2)	0.0000 (1)	−0.0012 (2)	0.0000 (1)
Ni4	0.0063 (2)	0.0079 (2)	0.0066 (2)	0.0000 (1)	−0.0004 (2)	0.0000 (1)
V1	0.0057 (2)	0.0076 (2)	0.0058 (2)	−0.0002 (1)	0.0000 (2)	0.0012 (1)
V2	0.0060 (2)	0.0084 (2)	0.0052 (2)	−0.0011 (1)	−0.0018 (2)	−0.0003 (1)
V3	0.0059 (2)	0.0075 (2)	0.0050 (2)	−0.0008 (1)	−0.0012 (2)	−0.0002 (1)
V4	0.0055 (2)	0.0087 (2)	0.0066 (2)	0.0005 (1)	0.0002 (2)	−0.0010 (2)
O1	0.0085 (9)	0.0161 (10)	0.0092 (9)	−0.0001 (7)	0.0025 (7)	−0.0008 (7)
O2	0.0088 (9)	0.0120 (9)	0.0113 (10)	−0.0029 (7)	−0.0007 (7)	−0.0008 (7)
O3	0.0143 (9)	0.0115 (9)	0.0231 (12)	0.0025 (7)	0.0023 (8)	0.0038 (8)
O4	0.0094 (9)	0.0148 (9)	0.0088 (9)	−0.0012 (7)	−0.0017 (7)	0.0005 (7)
O5	0.0141 (9)	0.0115 (9)	0.0092 (10)	−0.0047 (7)	−0.0029 (7)	0.0008 (7)
O6	0.0141 (10)	0.0151 (10)	0.0129 (10)	0.0014 (7)	−0.0016 (8)	−0.0044 (8)
O7	0.0097 (9)	0.0141 (9)	0.0089 (9)	0.0022 (7)	−0.0020 (7)	−0.0014 (7)
O8	0.0123 (9)	0.0122 (9)	0.0094 (10)	−0.0008 (7)	−0.0017 (7)	−0.0027 (7)
O9	0.0186 (10)	0.0129 (9)	0.0114 (10)	−0.0049 (7)	−0.0014 (8)	0.0015 (7)
O10	0.0073 (8)	0.0145 (9)	0.0091 (9)	0.0008 (7)	0.0017 (7)	−0.0024 (7)
O11	0.0072 (8)	0.0122 (9)	0.0143 (10)	−0.0015 (7)	0.0002 (7)	−0.0041 (7)
O12	0.0125 (9)	0.0158 (9)	0.0174 (11)	0.0049 (7)	−0.0006 (8)	0.0039 (8)
N11	0.0082 (6)	0.0102 (5)	0.0132 (7)	0.0001 (2)	0.0017 (4)	−0.0004 (4)
C11	0.0115 (8)	0.0131 (6)	0.0199 (8)	−0.0040 (5)	0.0024 (5)	−0.0008 (6)
N12	0.0137 (10)	0.0117 (5)	0.0258 (11)	−0.0016 (6)	−0.0043 (6)	−0.0013 (8)
C12	0.0250 (12)	0.0125 (7)	0.0198 (10)	−0.0007 (7)	−0.0071 (6)	−0.0022 (8)
C13	0.0247 (11)	0.0146 (7)	0.0135 (8)	−0.0036 (6)	0.0000 (5)	−0.0020 (6)
N21	0.0104 (8)	0.0114 (6)	0.0133 (12)	0.0015 (9)	0.0016 (8)	0.0003 (3)
C21	0.0190 (12)	0.0210 (8)	0.0344 (12)	−0.0005 (16)	−0.0008 (16)	0.0158 (10)
N22	0.0302 (17)	0.0200 (7)	0.0240 (17)	0.007 (2)	−0.0023 (19)	0.0080 (9)
C22	0.0310 (17)	0.0200 (17)	0.044 (3)	0.0031 (15)	−0.0208 (15)	0.0060 (9)
C23	0.0178 (11)	0.0239 (19)	0.056 (3)	−0.0032 (9)	−0.0171 (9)	0.0162 (9)
N31	0.0099 (6)	0.0111 (6)	0.0087 (10)	−0.0003 (6)	−0.0001 (13)	0.0008 (18)
C31	0.0098 (12)	0.0112 (7)	0.0126 (15)	−0.0008 (4)	−0.001 (2)	0.001 (3)
N32	0.0120 (13)	0.0129 (9)	0.017 (2)	−0.0013 (8)	0.002 (3)	0.003 (4)
C32	0.0158 (9)	0.0147 (11)	0.0142 (16)	−0.0006 (18)	0.005 (2)	0.003 (3)
C33	0.0139 (6)	0.0132 (9)	0.0093 (10)	−0.0001 (17)	0.0020 (14)	0.002 (2)
N41	0.0099 (10)	0.0115 (9)	0.0090 (17)	0.0006 (8)	−0.0006 (13)	−0.0011 (6)
C41	0.0137 (18)	0.0138 (7)	0.0107 (13)	0.0023 (11)	−0.002 (3)	−0.0036 (5)
N42	0.016 (2)	0.0157 (8)	0.015 (3)	0.0032 (16)	0.000 (3)	−0.0049 (8)
C42	0.0123 (16)	0.016 (3)	0.023 (4)	0.0025 (16)	0.0014 (19)	−0.006 (2)
C43	0.0099 (9)	0.015 (3)	0.019 (4)	0.0016 (11)	−0.0010 (8)	−0.005 (2)
N51	0.0094 (6)	0.0098 (5)	0.0110 (6)	0.0003 (2)	−0.0011 (5)	−0.0005 (3)
C51	0.0136 (9)	0.0132 (7)	0.0119 (6)	0.0018 (5)	−0.0007 (6)	−0.0025 (5)
N52	0.0138 (11)	0.0125 (8)	0.0160 (7)	0.0008 (6)	0.0016 (8)	−0.0032 (7)
C52	0.0137 (11)	0.0126 (8)	0.0185 (9)	0.0034 (6)	0.0006 (8)	−0.0013 (8)
C53	0.0138 (9)	0.0137 (7)	0.0147 (7)	0.0048 (6)	−0.0020 (7)	−0.0006 (6)
N61	0.0126 (6)	0.0125 (10)	0.0171 (8)	−0.0012 (3)	0.0015 (8)	0.0029 (11)
C61	0.0132 (5)	0.0223 (10)	0.0250 (10)	−0.0061 (5)	0.0015 (15)	0.004 (2)
N62	0.0206 (9)	0.0252 (17)	0.0368 (14)	−0.0072 (7)	0.0090 (18)	0.009 (3)
C62	0.0275 (15)	0.031 (3)	0.0423 (17)	−0.0014 (12)	0.0109 (13)	0.022 (2)
C63	0.0203 (12)	0.028 (2)	0.0330 (16)	0.0015 (11)	0.0045 (7)	0.0201 (13)
N71	0.0098 (5)	0.0112 (4)	0.0100 (5)	−0.0011 (2)	−0.0006 (4)	−0.0003 (2)
C71	0.0138 (5)	0.0115 (5)	0.0098 (6)	−0.0023 (3)	0.0009 (5)	−0.0008 (4)
N72	0.0185 (7)	0.0139 (5)	0.0114 (6)	−0.0046 (5)	−0.0015 (5)	−0.0013 (5)
C72	0.0154 (5)	0.0157 (6)	0.0162 (8)	−0.0040 (5)	−0.0053 (6)	−0.0006 (6)
C73	0.0104 (5)	0.0134 (6)	0.0148 (7)	−0.0017 (3)	−0.0032 (4)	−0.0001 (4)
N81	0.0095 (5)	0.0126 (4)	0.0119 (5)	0.0013 (1)	0.0002 (4)	0.0022 (1)
C81	0.0124 (7)	0.0131 (5)	0.0170 (5)	0.0034 (4)	0.0007 (5)	0.0023 (3)
N82	0.0144 (7)	0.0169 (5)	0.0227 (8)	0.0048 (5)	0.0005 (6)	0.0070 (5)
C82	0.0195 (9)	0.0248 (8)	0.0185 (6)	0.0075 (7)	−0.0003 (6)	0.0095 (6)
C83	0.0183 (9)	0.0221 (7)	0.0125 (5)	0.0066 (6)	0.0002 (5)	0.0052 (4)

Geometric parameters (Å, º)

Ni1—O1	2.111 (2)	N41—C43	1.373 (1)
Ni1—O1^i	2.111 (2)	C41—N42	1.351 (1)
Ni1—N11	2.062 (1)	N42—C42	1.368 (1)
Ni1—N11^i	2.062 (1)	C42—C43	1.360 (1)
Ni1—N21	2.057 (1)	N51—C51	1.327 (1)
Ni1—N21^i	2.057 (1)	N51—C53	1.373 (1)
Ni2—O4	2.057 (2)	C51—N52	1.351 (1)
Ni2—O4^ii	2.057 (2)	N52—C52	1.368 (1)
Ni2—N31	2.100 (1)	C52—C53	1.360 (1)
Ni2—N31^ii	2.100 (1)	N61—C61	1.327 (1)
Ni2—N41	2.068 (1)	N61—C63	1.373 (1)
Ni2—N41^ii	2.068 (1)	C61—N62	1.351 (1)
Ni3—O7	2.121 (2)	N62—C62	1.368 (1)
Ni3—O7^i	2.121 (2)	C62—C63	1.360 (1)
Ni3—N51	2.085 (1)	N71—C71	1.327 (1)
Ni3—N51^i	2.085 (1)	N71—C73	1.373 (1)
Ni3—N61	2.055 (2)	C71—N72	1.351 (1)
Ni3—N61^i	2.055 (2)	N72—C72	1.368 (1)
Ni4—O10	2.077 (2)	C72—C73	1.360 (1)
Ni4—O10^iii	2.077 (2)	N81—C81	1.327 (1)
Ni4—N71	2.102 (1)	N81—C83	1.373 (1)
Ni4—N71^iii	2.102 (1)	C81—N82	1.351 (1)
Ni4—N81	2.080 (1)	N82—C82	1.368 (1)
Ni4—N81^iii	2.080 (1)	C82—C83	1.360 (1)
V1—O1	1.651 (2)	C11—H1C11	0.930
V1—O2	1.809 (2)	N12—H1N12	0.860
V1—O3	1.643 (2)	C12—H1C12	0.930
V1—O5	1.831 (2)	C13—H1C13	0.930
V2—O2^iv	1.810 (2)	C21—H1C21	0.930
V2—O4	1.649 (2)	N22—H1N22	0.860
V2—O5	1.820 (2)	C22—H1C22	0.930
V2—O6	1.641 (2)	C23—H1C23	0.930
V3—O7	1.646 (2)	C31—H1C31	0.930
V3—O8	1.798 (2)	N32—H1N32	0.860
V3—O9	1.649 (2)	C32—H1C32	0.930
V3—O11	1.823 (2)	C33—H1C33	0.930
V4—O8^v	1.818 (2)	C41—H1C41	0.930
V4—O10	1.650 (2)	N42—H1N42	0.860
V4—O11	1.821 (2)	C42—H1C42	0.930
V4—O12	1.630 (2)	C43—H1C43	0.930
N11—C11	1.327 (1)	C51—H1C51	0.930
N11—C13	1.373 (1)	N52—H1N52	0.860
C11—N12	1.351 (1)	C52—H1C52	0.930
N12—C12	1.368 (1)	C53—H1C53	0.930
C12—C13	1.360 (1)	C61—H1C61	0.930
N21—C21	1.327 (1)	N62—H1N62	0.860
N21—C23	1.373 (1)	C62—H1C62	0.930
C21—N22	1.351 (1)	C63—H1C63	0.930
N22—C22	1.368 (1)	C71—H1C71	0.930
C22—C23	1.360 (1)	N72—H1N72	0.860
N31—C31	1.327 (1)	C72—H1C72	0.930
N31—C33	1.373 (1)	C73—H1C73	0.930
C31—N32	1.351 (1)	C81—H1C81	0.930
N32—C32	1.368 (1)	N82—H1N82	0.860
C32—C33	1.360 (1)	C82—H1C82	0.930
N41—C41	1.327 (1)	C83—H1C83	0.930
O3···C62	3.224 (3)	C21···C52^vii	3.597 (3)
O3···N82	2.829 (2)	C21···C53^x	3.490 (3)
O5···N72^vi	2.815 (2)	N22···C53^x	3.382 (3)
O6···C41	3.278 (2)	C22···C32^xi	3.508 (3)
O6···N52^vii	2.716 (2)	C31···C71^vi	3.471 (2)
O9···N22^viii	2.893 (2)	C31···C71^xii	3.400 (2)
O9···N42^viii	2.743 (2)	C31···C72^xii	3.541 (3)
O11···N32^ix	2.950 (2)	C31···C73^xii	3.504 (3)
O12···N12^i	2.732 (2)	C32···C71^vi	3.584 (2)
O12···C81	3.188 (3)	C33···C71^vi	3.553 (2)
C12···C32	3.335 (3)	C42···C81^xiii	3.554 (3)
C12···C63	3.369 (3)	C51···C82^vi	3.470 (2)
C13···C23	3.451 (3)	C52···C72	3.488 (3)
C13···C32	3.459 (3)	C73···C83	3.440 (3)
C21···N52^vii	3.243 (3)	C81···C81^iii	3.548 (4)
C21···C51^vii	3.390 (3)
O1—Ni1—O1^i	174.3 (1)	Ni2—N31—C31	129.7 (1)
O1—Ni1—N11	91.5 (1)	Ni2—N31—C33	124.3 (1)
O1—Ni1—N11^i	92.6 (1)	C31—N31—C33	105.9 (1)
O1—Ni1—N21	88.9 (1)	N31—C31—N32	110.9 (1)
O1—Ni1—N21^i	87.3 (1)	C31—N32—C32	107.3 (1)
O1^i—Ni1—N11	92.6 (1)	N32—C32—C33	106.5 (1)
O1^i—Ni1—N11^i	91.5 (1)	N31—C33—C32	109.5 (1)
O1^i—Ni1—N21	87.3 (1)	Ni2—N41—C41	126.8 (1)
O1^i—Ni1—N21^i	88.9 (1)	Ni2—N41—C43	127.2 (1)
N11—Ni1—N11^i	87.1 (1)	C41—N41—C43	105.9 (1)
N11—Ni1—N21	88.4 (1)	N41—C41—N42	110.9 (1)
N11—Ni1—N21^i	175.3 (1)	C41—N42—C42	107.3 (1)
N11^i—Ni1—N21	175.3 (1)	N42—C42—C43	106.5 (1)
N11^i—Ni1—N21^i	88.4 (1)	N41—C43—C42	109.5 (1)
N21—Ni1—N21^i	96.2 (1)	Ni3—N51—C51	126.1 (1)
O4—Ni2—O4^ii	174.5 (1)	Ni3—N51—C53	128.0 (1)
O4—Ni2—N31	88.0 (1)	C51—N51—C53	105.9 (1)
O4—Ni2—N31^ii	88.4 (1)	N51—C51—N52	110.9 (1)
O4—Ni2—N41	93.8 (1)	C51—N52—C52	107.3 (1)
O4—Ni2—N41^ii	90.1 (1)	N52—C52—C53	106.5 (1)
O4^ii—Ni2—N31	88.4 (1)	N51—C53—C52	109.5 (1)
O4^ii—Ni2—N31^ii	88.0 (1)	Ni3—N61—C61	126.3 (1)
O4^ii—Ni2—N41	90.1 (1)	Ni3—N61—C63	126.9 (1)
O4^ii—Ni2—N41^ii	93.8 (1)	C61—N61—C63	105.9 (1)
N31—Ni2—N31^ii	97.2 (1)	N61—C61—N62	110.9 (1)
N31—Ni2—N41	86.8 (1)	C61—N62—C62	107.3 (1)
N31—Ni2—N41^ii	175.6 (1)	N62—C62—C63	106.5 (1)
N31^ii—Ni2—N41	175.6 (1)	N61—C63—C62	109.5 (1)
N31^ii—Ni2—N41^ii	86.8 (1)	Ni4—N71—C71	130.8 (1)
N41—Ni2—N41^ii	89.4 (1)	Ni4—N71—C73	123.0 (1)
O7—Ni3—O7^i	171.9 (1)	C71—N71—C73	105.9 (1)
O7—Ni3—N51	89.7 (1)	N71—C71—N72	110.9 (1)
O7—Ni3—N51^i	96.1 (1)	C71—N72—C72	107.3 (1)
O7—Ni3—N61	86.6 (1)	N72—C72—C73	106.5 (1)
O7—Ni3—N61^i	88.1 (1)	N71—C73—C72	109.5 (1)
O7^i—Ni3—N51	96.1 (1)	Ni4—N81—C81	125.7 (1)
O7^i—Ni3—N51^i	89.7 (1)	Ni4—N81—C83	128.3 (1)
O7^i—Ni3—N61	88.1 (1)	C81—N81—C83	105.9 (1)
O7^i—Ni3—N61^i	86.6 (1)	N81—C81—N82	110.9 (1)
N51—Ni3—N51^i	87.6 (1)	C81—N82—C82	107.3 (1)
N51—Ni3—N61	87.6 (1)	N82—C82—C83	106.5 (1)
N51—Ni3—N61^i	174.5 (1)	N81—C83—C82	109.5 (1)
N51^i—Ni3—N61	174.5 (1)	N11—C11—H1C11	124.5
N51^i—Ni3—N61^i	87.6 (1)	N12—C11—H1C11	124.5
N61—Ni3—N61^i	97.4 (1)	C11—N12—H1N12	126.4
O10—Ni4—O10^iii	172.3 (1)	C12—N12—H1N12	126.4
O10—Ni4—N71	88.5 (1)	N12—C12—H1C12	126.8
O10—Ni4—N71^iii	86.4 (1)	C13—C12—H1C12	126.8
O10—Ni4—N81	94.5 (1)	N11—C13—H1C13	125.3
O10—Ni4—N81^iii	91.1 (1)	C12—C13—H1C13	125.3
O10^iii—Ni4—N71	86.4 (1)	N21—C21—H1C21	124.5
O10^iii—Ni4—N71^iii	88.5 (1)	N22—C21—H1C21	124.5
O10^iii—Ni4—N81	91.1 (1)	C21—N22—H1N22	126.4
O10^iii—Ni4—N81^iii	94.5 (1)	C22—N22—H1N22	126.4
N71—Ni4—N71^iii	97.7 (1)	N22—C22—H1C22	126.8
N71—Ni4—N81	87.2 (1)	C23—C22—H1C22	126.8
N71—Ni4—N81^iii	175.0 (1)	N21—C23—H1C23	125.3
N71^iii—Ni4—N81	175.0 (1)	C22—C23—H1C23	125.3
N71^iii—Ni4—N81^iii	87.2 (1)	N31—C31—H1C31	124.5
N81—Ni4—N81^iii	87.8 (1)	N32—C31—H1C31	124.5
O1—V1—O2	110.8 (1)	C31—N32—H1N32	126.4
O1—V1—O3	108.7 (1)	C32—N32—H1N32	126.4
O1—V1—O5	110.2 (1)	N32—C32—H1C32	126.8
O2—V1—O3	111.3 (1)	C33—C32—H1C32	126.8
O2—V1—O5	108.1 (1)	N31—C33—H1C33	125.3
O3—V1—O5	107.8 (1)	C32—C33—H1C33	125.3
O2^iv—V2—O4	108.9 (1)	N41—C41—H1C41	124.5
O2^iv—V2—O5	111.0 (1)	N42—C41—H1C41	124.5
O2^iv—V2—O6	108.8 (1)	C41—N42—H1N42	126.4
O4—V2—O5	108.1 (1)	C42—N42—H1N42	126.4
O4—V2—O6	108.8 (1)	N42—C42—H1C42	126.8
O5—V2—O6	111.2 (1)	C43—C42—H1C42	126.8
O7—V3—O8	109.6 (1)	N41—C43—H1C43	125.3
O7—V3—O9	107.4 (1)	C42—C43—H1C43	125.3
O7—V3—O11	110.1 (1)	N51—C51—H1C51	124.5
O8—V3—O9	111.5 (1)	N52—C51—H1C51	124.5
O8—V3—O11	109.3 (1)	C51—N52—H1N52	126.4
O9—V3—O11	108.8 (1)	C52—N52—H1N52	126.4
O8^v—V4—O10	109.8 (1)	N52—C52—H1C52	126.8
O8^v—V4—O11	110.7 (1)	C53—C52—H1C52	126.8
O8^v—V4—O12	109.3 (1)	N51—C53—H1C53	125.3
O10—V4—O11	108.8 (1)	C52—C53—H1C53	125.3
O10—V4—O12	108.8 (1)	N61—C61—H1C61	124.5
O11—V4—O12	109.4 (1)	N62—C61—H1C61	124.5
Ni1—O1—V1	170.3 (1)	C61—N62—H1N62	126.4
V1—O2—V2^iv	132.6 (1)	C62—N62—H1N62	126.4
Ni2—O4—V2	167.6 (1)	N62—C62—H1C62	126.8
V1—O5—V2	126.4 (1)	C63—C62—H1C62	126.8
Ni3—O7—V3	166.5 (1)	N61—C63—H1C63	125.3
V3—O8—V4^v	133.5 (1)	C62—C63—H1C63	125.3
Ni4—O10—V4	162.3 (1)	N71—C71—H1C71	124.5
V3—O11—V4	126.3 (1)	N72—C71—H1C71	124.5
Ni1—N11—C11	124.9 (1)	C71—N72—H1N72	126.4
Ni1—N11—C13	129.2 (1)	C72—N72—H1N72	126.4
C11—N11—C13	105.9 (1)	N72—C72—H1C72	126.8
N11—C11—N12	110.9 (1)	C73—C72—H1C72	126.8
C11—N12—C12	107.3 (1)	N71—C73—H1C73	125.3
N12—C12—C13	106.5 (1)	C72—C73—H1C73	125.3
N11—C13—C12	109.5 (1)	N81—C81—H1C81	124.5
Ni1—N21—C21	127.8 (1)	N82—C81—H1C81	124.5
Ni1—N21—C23	125.9 (1)	C81—N82—H1N82	126.4
C21—N21—C23	105.9 (1)	C82—N82—H1N82	126.4
N21—C21—N22	110.9 (1)	N82—C82—H1C82	126.8
C21—N22—C22	107.3 (1)	C83—C82—H1C82	126.8
N22—C22—C23	106.5 (1)	N81—C83—H1C83	125.3
N21—C23—C22	109.5 (1)	C82—C83—H1C83	125.3

Symmetry codes: (i) −x+1/2, y, −z+3/2; (ii) −x+1/2, y, −z+1/2; (iii) −x+3/2, y, −z+3/2; (iv) −x+1, −y+2, −z+1; (v) −x+1, −y+1, −z+2; (vi) −x+1, −y+1, −z+1; (vii) x, y+1, z; (viii) −x+1/2, y−1, −z+3/2; (ix) x+1/2, −y+1, z+1/2; (x) −x+1/2, y+1, −z+3/2; (xi) −x, −y+2, −z+1; (xii) x−1/2, −y+1, z−1/2; (xiii) x−1/2, −y+2, z−1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N12—H1N12···O12^i	0.86	1.98	2.732 (2)	146
N22—H1N22···O9^x	0.86	2.10	2.893 (2)	153
N32—H1N32···O11^xii	0.86	2.21	2.950 (2)	144
N42—H1N42···O9^x	0.86	1.94	2.743 (2)	155
N52—H1N52···O6^xiv	0.86	1.90	2.716 (2)	159
N72—H1N72···O5^vi	0.86	2.03	2.815 (2)	151
N82—H1N82···O3	0.86	2.13	2.829 (2)	138

Symmetry codes: (i) −x+1/2, y, −z+3/2; (vi) −x+1, −y+1, −z+1; (x) −x+1/2, y+1, −z+3/2; (xii) x−1/2, −y+1, z−1/2; (xiv) x, y−1, z.

catena-tetrakis(imidazole)-tetrakis(µ₂-oxo)-dioxo-nickel(ii)-di-vanadium (Ni_295K)

Crystal data

[Ni(C3H4N2)4V2O6]	Dx = 1.839 Mg m^−3
Mr = 528.90	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P42/n	Cell parameters from 30541 reflections
Hall symbol: -P 4bc	θ = 2.6–30.0°
a = 16.1988 (2) Å	µ = 2.00 mm^−1
c = 14.5589 (2) Å	T = 295 K
V = 3820.27 (8) Å^3	Hexagonal, blue
Z = 8	0.40 × 0.21 × 0.18 mm
F(000) = 2128

Data collection

Enraf-Nonius KappaCCD diffractometer	5581 independent reflections
Radiation source: fine-focus sealed tube	4334 reflections with I > 3σ(I)
Graphite monochromator	Rint = 0.047
φ scan plus ω scans with κ offsets	θmax = 30.0°, θmin = 2.8°
Absorption correction: multi-scan multi-scan from symmetry-related measurements Sortav (Blessing 1995)	h = −22→22
Tmin = 0.630, Tmax = 0.703	k = −22→22
48877 measured reflections	l = −20→19

Refinement

Refinement on F	6 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.031	w = 1/[σ(F)^2 + (0.0004F)^2]
wR(F^2) = 0.048	(Δ/σ)max = 0.2
S = 1.70	Δρmax = 0.81 e Å^−3
4334 reflections	Δρmin = −0.65 e Å^−3
174 parameters

Special details

Refinement. Refinement of the low temperature phase (100, 200, and 279 K) used origin choice 2 of the International Tables for X-ray Crystallography, Vol. A (Hahn, 1995), and 317 variables to describe 64 non hydrogen atom positions and 36 hydrogen atom positions. The second of eight imidazoles in the asymmetric unit was found to be disordered. All hydrogen atoms were reinserted in geometrically sensible positions after each refinement cycle and given atom displacement parameters defined by the 12 variable TL rigid body model (Rae, 1975) that described the anisotropic atom displacement parameters of the corresponding imidazole (or disordered imidazole). The centres of action for the librations were located on the associated Mn atom. A common set of refinable local orthonormal coordinates were used to impose equal planar geometry on every imidazole, their origins and orientations being independently determined. The 2-fold rotation related components of the disordered imidazole were constrained to be coplanar with the coordinating N atoms coincident. The metal atoms and oxygen atoms were refined as isolated anisotropic atoms. Atoms Mn2 and Mn3 lie on 2-fold axes.

Refinement of the high temperature phase (283 and 295 K) used origin choice 2 (Hahn, 1995) and 174 variables to describe 40 non hydrogen atom positions and 24 hydrogen atom positions. The first and second of the four imidazoles in the asymmetric unit were described as 1:1 disordered. All other atoms were modelled as being ordered. All hydrogen atoms were reinserted in geometrically sensible positions after each refinement cycle and given atom displacement parameters defined by the rigid body models for the atoms to which they were attached. The two disordered imidazoles are attached to the Mn1 atom and their atoms were modelled to have a common T rigid model parametrization plus individual librations about the relevant Mn1—N bonds. The other two imidazoles were attached to Mn2 and were also modelled to have a common T rigid model parametrization plus individual librations about the relevant Mn2—N bonds. A common set of refinable local orthonormal coordinates were used to impose equal planar geometry on every imidazole, their origins and orientations being independently determined. Restraints were used to match the Mn1—N bond distances of each component of a disordered imidazole. Restraints were also used to initially restrain second nearest neighbour Mn1—C distances but these restraints were reduced to minimal importance in the final refinement cycle. The metal atoms and oxygen atoms were refined as isolated anisotropic atoms. Atoms M1n and Mn2 lie on 2-fold axes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
NI1	0.25000	0.75000	0.90121 (2)	0.0192 (1)
N11A	0.19285 (12)	0.68178 (12)	0.79791 (11)	0.0283 (12)	0.500
C11A	0.13640 (18)	0.70816 (19)	0.74138 (19)	0.0409 (13)	0.500
N12A	0.1136 (2)	0.6495 (2)	0.68159 (18)	0.051 (2)	0.500
C12A	0.1585 (3)	0.58110 (19)	0.7013 (2)	0.058 (3)	0.500
C13A	0.2071 (2)	0.60170 (15)	0.7731 (2)	0.050 (3)	0.500
N11B	0.19677 (11)	0.67986 (11)	0.79688 (10)	0.0246 (5)	0.500
C11B	0.12088 (14)	0.68469 (19)	0.76783 (16)	0.033 (4)	0.500
N12B	0.10658 (17)	0.6325 (2)	0.69812 (17)	0.039 (3)	0.500
C12B	0.1781 (2)	0.59171 (17)	0.68159 (16)	0.037 (3)	0.500
C13B	0.23326 (17)	0.62135 (16)	0.74283 (16)	0.032 (4)	0.500
N21A	0.18526 (14)	0.67757 (13)	0.99320 (14)	0.0324 (5)	0.500
C21A	0.1170 (2)	0.69406 (19)	1.0367 (3)	0.1061 (15)	0.500
N22A	0.0875 (2)	0.6277 (2)	1.0809 (3)	0.1046 (17)	0.500
C22A	0.1406 (2)	0.56466 (17)	1.0645 (3)	0.0561 (15)	0.500
C23A	0.2006 (2)	0.59607 (17)	1.0104 (2)	0.0536 (13)	0.500
N21B	0.18725 (14)	0.67914 (13)	0.99634 (13)	0.0272 (7)	0.500
C21B	0.21046 (18)	0.6516 (2)	1.07631 (16)	0.115 (4)	0.500
N22B	0.1531 (2)	0.6025 (2)	1.1142 (2)	0.077 (2)	0.500
C22B	0.0891 (2)	0.5985 (3)	1.0544 (3)	0.108 (4)	0.500
C23B	0.11076 (17)	0.6460 (3)	0.9821 (2)	0.146 (6)	0.500
NI2	0.25000	0.25000	0.97882 (2)	0.0199 (1)
N31	0.17680 (6)	0.31489 (6)	0.88240 (6)	0.0274 (3)
C31	0.13007 (9)	0.28754 (11)	0.81628 (10)	0.0344 (5)
N32	0.08772 (8)	0.34865 (11)	0.77581 (9)	0.0409 (6)
C32	0.10884 (11)	0.41973 (11)	0.81899 (12)	0.0467 (8)
C33	0.16376 (10)	0.39821 (11)	0.88454 (11)	0.0404 (7)
N41	0.18087 (7)	0.30695 (6)	1.08148 (7)	0.0297 (3)
C41	0.20768 (11)	0.35782 (10)	1.14400 (11)	0.0398 (6)
N42	0.14592 (11)	0.38791 (10)	1.19536 (10)	0.0489 (6)
C42	0.07498 (11)	0.35398 (12)	1.16349 (13)	0.0636 (8)
C43	0.09723 (11)	0.30419 (12)	1.09333 (13)	0.0567 (9)
V1	0.42742 (2)	0.60059 (2)	0.89546 (2)	0.0186 (1)
V2	0.39579 (2)	0.42361 (2)	0.99282 (2)	0.0194 (1)
O1	0.34854 (9)	0.66330 (9)	0.90977 (10)	0.0296 (3)
O2	0.50080 (9)	0.61401 (9)	0.98684 (10)	0.0281 (3)
O3	0.46867 (10)	0.62039 (12)	0.79512 (10)	0.0407 (4)
O4	0.33526 (9)	0.34477 (8)	0.97026 (10)	0.0293 (3)
O5	0.39318 (10)	0.49350 (9)	0.89570 (10)	0.0308 (4)
O6	0.36243 (10)	0.47021 (10)	1.08501 (11)	0.0389 (4)
H1C11A	0.11456	0.76125	0.74236	0.060	0.500
H1N12A	0.07733	0.65431	0.63880	0.066	0.500
H1C12A	0.15628	0.53038	0.67145	0.084	0.500
H1C13A	0.24475	0.56658	0.80139	0.077	0.500
H1C11B	0.08141	0.72003	0.79245	0.044	0.500
H1N12B	0.06067	0.62619	0.66931	0.049	0.500
H1C12B	0.18731	0.55151	0.63715	0.047	0.500
H1C13B	0.28797	0.60444	0.74752	0.043	0.500
H1C21A	0.09169	0.74561	1.03703	0.210	0.500
H1N22A	0.04332	0.62553	1.11352	0.180	0.500
H1C22A	0.13649	0.51079	1.08617	0.082	0.500
H1C23A	0.24560	0.56661	0.98819	0.123	0.500
H1C21B	0.26069	0.66435	1.10379	0.331	0.500
H1N22B	0.15640	0.57818	1.16657	0.154	0.500
H1C22B	0.04022	0.56914	1.06176	0.232	0.500
H1C23B	0.07843	0.65475	0.93018	0.377	0.500
H1C31	0.12650	0.23233	0.79920	0.044
H1N32	0.05358	0.34369	0.73091	0.049
H1C32	0.08946	0.47252	0.80610	0.063
H1C33	0.18897	0.43469	0.92512	0.054
H1C41	0.26294	0.37160	1.15204	0.059
H1N42	0.15046	0.42227	1.24011	0.062
H1C42	0.02185	0.36312	1.18546	0.094
H1C43	0.06101	0.27271	1.05827	0.088

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
NI1	0.0183 (2)	0.0211 (2)	0.0183 (2)	0.0008 (1)	0.0000 (1)	0.0000 (1)
N11A	0.0283 (15)	0.0328 (19)	0.0240 (7)	−0.0005 (5)	−0.005 (2)	−0.001 (2)
C11A	0.0300 (18)	0.060 (2)	0.0329 (11)	0.0095 (12)	−0.013 (2)	−0.012 (2)
N12A	0.042 (3)	0.073 (4)	0.0366 (14)	−0.0060 (16)	−0.013 (4)	−0.016 (4)
C12A	0.089 (4)	0.047 (4)	0.0395 (19)	−0.0150 (16)	−0.020 (5)	−0.009 (5)
C13A	0.085 (4)	0.031 (3)	0.0367 (17)	0.0008 (9)	−0.022 (4)	−0.005 (4)
N11B	0.0230 (8)	0.0288 (7)	0.0221 (7)	0.0021 (6)	−0.0030 (5)	0.0000 (5)
C11B	0.024 (5)	0.047 (5)	0.030 (10)	0.001 (5)	−0.007 (3)	−0.0063 (17)
N12B	0.034 (3)	0.051 (4)	0.030 (6)	−0.006 (3)	−0.008 (2)	−0.0073 (15)
C12B	0.043 (4)	0.040 (4)	0.030 (7)	−0.002 (4)	−0.005 (3)	−0.0083 (14)
C13B	0.034 (5)	0.035 (6)	0.029 (11)	0.006 (6)	−0.005 (4)	−0.0080 (17)
N21A	0.0334 (9)	0.0330 (9)	0.0307 (8)	0.0006 (6)	0.0063 (9)	0.0063 (7)
C21A	0.098 (3)	0.070 (2)	0.151 (4)	0.0310 (19)	0.097 (3)	0.051 (3)
N22A	0.091 (3)	0.086 (3)	0.137 (4)	0.010 (2)	0.075 (3)	0.054 (3)
C22A	0.071 (3)	0.0497 (17)	0.048 (2)	−0.0176 (15)	0.009 (2)	0.0173 (18)
C23A	0.063 (2)	0.0366 (11)	0.061 (2)	0.0039 (11)	0.020 (2)	0.0209 (14)
N21B	0.0301 (10)	0.0283 (10)	0.0233 (7)	−0.0003 (7)	0.0025 (6)	0.0015 (8)
C21B	0.060 (2)	0.209 (6)	0.0781 (18)	−0.049 (3)	−0.0255 (16)	0.104 (3)
N22B	0.069 (3)	0.095 (3)	0.065 (2)	−0.008 (2)	0.0136 (18)	0.050 (2)
C22B	0.127 (4)	0.160 (6)	0.039 (2)	−0.110 (5)	−0.001 (2)	0.017 (3)
C23B	0.109 (3)	0.272 (8)	0.057 (2)	−0.142 (5)	−0.038 (2)	0.076 (4)
NI2	0.0203 (2)	0.0186 (2)	0.0208 (2)	−0.0019 (1)	0.0000 (1)	0.0000 (1)
N31	0.0268 (5)	0.0280 (5)	0.0272 (4)	−0.0007 (4)	−0.0022 (3)	0.0008 (3)
C31	0.0313 (7)	0.0421 (6)	0.0298 (6)	−0.0008 (5)	−0.0074 (6)	0.0007 (4)
N32	0.0327 (7)	0.0573 (8)	0.0328 (6)	0.0062 (7)	−0.0045 (5)	0.0087 (6)
C32	0.0496 (10)	0.0461 (6)	0.0444 (9)	0.0140 (7)	−0.0063 (7)	0.0107 (6)
C33	0.0488 (10)	0.0296 (5)	0.0427 (8)	0.0065 (5)	−0.0093 (7)	0.0036 (4)
N41	0.0317 (5)	0.0273 (5)	0.0301 (4)	−0.0021 (4)	0.0030 (3)	−0.0058 (4)
C41	0.0486 (6)	0.0349 (9)	0.0361 (6)	−0.0082 (6)	0.0083 (5)	−0.0146 (7)
N42	0.0649 (9)	0.0388 (9)	0.0431 (7)	−0.0005 (7)	0.0177 (7)	−0.0140 (6)
C42	0.0497 (7)	0.0795 (15)	0.0617 (10)	0.0075 (8)	0.0183 (8)	−0.0278 (10)
C43	0.0329 (5)	0.0795 (15)	0.0579 (10)	−0.0018 (6)	0.0105 (6)	−0.0309 (10)
V1	0.0173 (2)	0.0194 (2)	0.0190 (2)	0.0016 (1)	−0.0005 (1)	0.0023 (1)
V2	0.0187 (2)	0.0169 (2)	0.0227 (2)	−0.0013 (1)	−0.0030 (1)	−0.0023 (1)
O1	0.0220 (7)	0.0289 (8)	0.0378 (8)	0.0062 (6)	−0.0032 (6)	−0.0013 (6)
O2	0.0216 (7)	0.0315 (8)	0.0312 (8)	0.0005 (6)	−0.0064 (6)	−0.0020 (6)
O3	0.0358 (9)	0.0577 (11)	0.0285 (9)	0.0032 (8)	0.0072 (7)	0.0123 (7)
O4	0.0282 (8)	0.0216 (7)	0.0382 (9)	−0.0062 (6)	−0.0059 (6)	−0.0004 (6)
O5	0.0391 (9)	0.0221 (7)	0.0311 (8)	−0.0046 (6)	−0.0097 (6)	0.0018 (6)
O6	0.0452 (10)	0.0334 (9)	0.0380 (9)	0.0005 (7)	0.0084 (7)	−0.0125 (7)

Geometric parameters (Å, º)

NI1—N11A	2.083 (1)	N32—C32	1.356 (2)
NI1—N11A^i	2.083 (1)	C32—C33	1.351 (2)
NI1—N11B	2.084 (1)	N41—C41	1.302 (1)
NI1—N11B^i	2.084 (1)	N41—C43	1.366 (2)
NI1—N21A	2.066 (1)	C41—N42	1.341 (2)
NI1—N21A^i	2.066 (1)	N42—C42	1.356 (2)
NI1—N21B	2.066 (1)	C42—C43	1.351 (2)
NI1—N21B^i	2.066 (1)	V1—O1	1.646 (1)
NI1—O1	2.130 (1)	V1—O2	1.797 (1)
NI1—O1^i	2.130 (1)	V1—O3	1.638 (1)
N11A—C11A	1.302 (1)	V1—O5	1.821 (1)
N11A—C13A	1.366 (2)	V2—O2^iii	1.807 (1)
C11A—N12A	1.341 (2)	V2—O4	1.643 (1)
N12A—C12A	1.356 (2)	V2—O5	1.812 (1)
C12A—C13A	1.351 (2)	V2—O6	1.632 (2)
N11B—C11B	1.302 (1)	C11A—H1C11A	0.930
N11B—C13B	1.366 (2)	N12A—H1N12A	0.860
C11B—N12B	1.341 (2)	C12A—H1C12A	0.930
N12B—C12B	1.356 (2)	C13A—H1C13A	0.930
C12B—C13B	1.351 (2)	C11B—H1C11B	0.930
N21A—C21A	1.302 (1)	N12B—H1N12B	0.860
N21A—C23A	1.366 (2)	C12B—H1C12B	0.930
C21A—N22A	1.341 (2)	C13B—H1C13B	0.930
N22A—C22A	1.356 (2)	C21A—H1C21A	0.930
C22A—C23A	1.351 (2)	N22A—H1N22A	0.860
N21B—C21B	1.302 (1)	C22A—H1C22A	0.930
N21B—C23B	1.366 (2)	C23A—H1C23A	0.930
C21B—N22B	1.341 (2)	C21B—H1C21B	0.930
N22B—C22B	1.356 (2)	N22B—H1N22B	0.860
C22B—C23B	1.351 (2)	C22B—H1C22B	0.930
NI2—N31	2.117 (1)	C23B—H1C23B	0.930
NI2—N31^ii	2.117 (1)	C31—H1C31	0.930
NI2—N41	2.083 (1)	N32—H1N32	0.860
NI2—N41^ii	2.083 (1)	C32—H1C32	0.930
NI2—O4	2.069 (1)	C33—H1C33	0.930
NI2—O4^ii	2.069 (1)	C41—H1C41	0.930
N31—C31	1.302 (1)	N42—H1N42	0.860
N31—C33	1.366 (2)	C42—H1C42	0.930
C31—N32	1.341 (2)	C43—H1C43	0.930
NI1···V2	5.942	C12B···C21A^v	2.984 (5)
NI1···V2^i	5.942	C12B···C21B^iv	3.578 (4)
C11A···N22B^iv	2.963 (5)	C12B···C32	3.609 (4)
C11A···C13B^i	3.476 (4)	C12B···O2^iv	3.371 (2)
C11A···C21B^iv	2.752 (4)	C13B···C21A^v	3.225 (5)
C11A···O3^i	3.350 (3)	C13B···N22A^v	3.306 (5)
N12A···O6^iv	2.722 (3)	C13B···C21B^v	3.383 (4)
N12A···C21B^iv	2.806 (5)	C22A···O3^vii	3.416 (4)
C12A···C21A^v	3.433 (6)	N22B···O3^vii	2.924 (2)
C12A···C32	3.228 (4)	C31···C31^viii	3.466 (2)
C13A···C23A	3.459 (5)	C31···C31^ix	3.466 (2)
C13A···C23B	3.494 (5)	C31···C32^ix	3.593 (2)
C13A···C32	3.416 (4)	C31···C33^ix	3.575 (2)
C11B···C21B^iv	3.303 (4)	N32···O5^ix	2.913 (2)
C11B···C23B	3.185 (4)	C33···C43	3.567 (3)
C11B···C42^vi	3.385 (3)	C41···O6	3.215 (2)
N12B···O6^iv	2.757 (3)	N42···O3^vii	2.771 (2)
N12B···C21B^iv	3.185 (4)	V1···V1^iii	5.041 (1)
N11A—NI1—N11A^i	87.6 (1)	N41—NI2—O4	94.2 (1)
N11A—NI1—N11B	2.0 (1)	N41—NI2—O4^ii	90.7
N11A—NI1—N11B^i	87.0 (1)	N41^ii—NI2—O4	90.7
N11A—NI1—N21A	86.6 (1)	N41^ii—NI2—O4^ii	94.2 (1)
N11A—NI1—N21A^i	174.0 (1)	O4—NI2—O4^ii	173.1 (1)
N11A—NI1—N21B	88.3 (1)	NI2—N31—C31	130.3 (1)
N11A—NI1—N21B^i	175.7 (1)	NI2—N31—C33	124.2 (1)
N11A—NI1—O1	91.5 (1)	C31—N31—C33	105.3 (1)
N11A—NI1—O1^i	93.4 (1)	N31—C31—N32	111.8 (1)
N11A^i—NI1—N11B	87.0 (1)	C31—N32—C32	107.1 (1)
N11A^i—NI1—N11B^i	2.0 (1)	N32—C32—C33	105.9 (1)
N11A^i—NI1—N21A	174.0 (1)	N31—C33—C32	109.9 (1)
N11A^i—NI1—N21A^i	86.6 (1)	NI2—N41—C41	127.0 (1)
N11A^i—NI1—N21B	175.7 (1)	NI2—N41—C43	127.5 (1)
N11A^i—NI1—N21B^i	88.3 (1)	C41—N41—C43	105.3 (1)
N11A^i—NI1—O1	93.4 (1)	N41—C41—N42	111.8 (1)
N11A^i—NI1—O1^i	91.5 (1)	C41—N42—C42	107.1 (1)
N11B—NI1—N11B^i	86.4 (1)	N42—C42—C43	105.9 (1)
N11B—NI1—N21A	87.3 (1)	N41—C43—C42	109.9 (1)
N11B—NI1—N21A^i	172.8 (1)	O1—V1—O2	110.2 (1)
N11B—NI1—N21B	89.0 (1)	O1—V1—O3	108.0 (1)
N11B—NI1—N21B^i	174.4 (1)	O1—V1—O5	110.6 (1)
N11B—NI1—O1	89.6 (1)	O2—V1—O3	111.5 (1)
N11B—NI1—O1^i	95.3 (1)	O2—V1—O5	108.4 (1)
N11B^i—NI1—N21A	172.8 (1)	O3—V1—O5	108.2 (1)
N11B^i—NI1—N21A^i	87.3 (1)	O2^iii—V2—O4	108.9 (1)
N11B^i—NI1—N21B	174.4 (1)	O2^iii—V2—O5	111.1 (1)
N11B^i—NI1—N21B^i	89.0 (1)	O2^iii—V2—O6	109.2 (1)
N11B^i—NI1—O1	95.3 (1)	O4—V2—O5	108.4 (1)
N11B^i—NI1—O1^i	89.6 (1)	O4—V2—O6	109.0 (1)
N21A—NI1—N21A^i	99.2 (1)	O5—V2—O6	110.2 (1)
N21A—NI1—N21B	1.7 (1)	NI1—O1—V1	169.0 (1)
N21A—NI1—N21B^i	97.5 (1)	V1—O2—V2^iii	133.9 (1)
N21A—NI1—O1	88.2 (1)	NI2—O4—V2	164.4 (1)
N21A—NI1—O1^i	87.5 (1)	V1—O5—V2	126.1 (1)
N21A^i—NI1—N21B	97.5 (1)	N11A—C11A—H1C11A	124.1
N21A^i—NI1—N21B^i	1.7 (1)	N12A—C11A—H1C11A	124.1
N21A^i—NI1—O1	87.5 (1)	C11A—N12A—H1N12A	126.4
N21A^i—NI1—O1^i	88.2 (1)	C12A—N12A—H1N12A	126.4
N21B—NI1—N21B^i	95.8 (1)	N12A—C12A—H1C12A	127.0
N21B—NI1—O1	87.9 (1)	C13A—C12A—H1C12A	127.0
N21B—NI1—O1^i	87.6 (1)	N11A—C13A—H1C13A	125.0
N21B^i—NI1—O1	87.6 (1)	C12A—C13A—H1C13A	125.0
N21B^i—NI1—O1^i	87.9 (1)	N11B—C11B—H1C11B	124.1
O1—NI1—O1^i	173.3 (1)	N12B—C11B—H1C11B	124.1
NI1—N11A—C11A	126.5 (1)	C11B—N12B—H1N12B	126.4
NI1—N11A—C13A	128.3 (1)	C12B—N12B—H1N12B	126.4
C11A—N11A—C13A	105.3 (1)	N12B—C12B—H1C12B	127.0
N11A—C11A—N12A	111.8 (1)	C13B—C12B—H1C12B	127.0
C11A—N12A—C12A	107.1 (1)	N11B—C13B—H1C13B	125.0
N12A—C12A—C13A	105.9 (1)	C12B—C13B—H1C13B	125.0
N11A—C13A—C12A	109.9 (1)	N21A—C21A—H1C21A	124.1
NI1—N11B—C11B	126.5 (1)	N22A—C21A—H1C21A	124.1
NI1—N11B—C13B	128.2 (1)	C21A—N22A—H1N22A	126.4
C11B—N11B—C13B	105.3 (1)	C22A—N22A—H1N22A	126.4
N11B—C11B—N12B	111.8 (1)	N22A—C22A—H1C22A	127.0
C11B—N12B—C12B	107.1 (1)	C23A—C22A—H1C22A	127.0
N12B—C12B—C13B	105.9 (1)	N21A—C23A—H1C23A	125.0
N11B—C13B—C12B	109.9 (1)	C22A—C23A—H1C23A	125.0
NI1—N21A—C21A	129.0 (2)	N21B—C21B—H1C21B	124.1
NI1—N21A—C23A	125.1 (1)	N22B—C21B—H1C21B	124.1
C21A—N21A—C23A	105.3 (1)	C21B—N22B—H1N22B	126.4
N21A—C21A—N22A	111.8 (1)	C22B—N22B—H1N22B	126.4
C21A—N22A—C22A	107.1 (1)	N22B—C22B—H1C22B	127.0
N22A—C22A—C23A	105.9 (1)	C23B—C22B—H1C22B	127.0
N21A—C23A—C22A	109.9 (1)	N21B—C23B—H1C23B	125.0
NI1—N21B—C21B	130.4 (2)	C22B—C23B—H1C23B	125.0
NI1—N21B—C23B	124.2 (2)	N31—C31—H1C31	124.1
C21B—N21B—C23B	105.3 (1)	N32—C31—H1C31	124.1
N21B—C21B—N22B	111.8 (1)	C31—N32—H1N32	126.4
C21B—N22B—C22B	107.1 (1)	C32—N32—H1N32	126.4
N22B—C22B—C23B	105.9 (1)	N32—C32—H1C32	127.0
N21B—C23B—C22B	109.9 (1)	C33—C32—H1C32	127.0
N31—NI2—N31^ii	96.9 (1)	N31—C33—H1C33	125.0
N31—NI2—N41	87.4	C32—C33—H1C33	125.0
N31—NI2—N41^ii	175.4	N41—C41—H1C41	124.1
N31—NI2—O4	88.0	N42—C41—H1C41	124.1
N31—NI2—O4^ii	87.4	C41—N42—H1N42	126.4
N31^ii—NI2—N41	175.4	C42—N42—H1N42	126.4
N31^ii—NI2—N41^ii	87.4	N42—C42—H1C42	127.0
N31^ii—NI2—O4	87.4	C43—C42—H1C42	127.0
N31^ii—NI2—O4^ii	88.0	N41—C43—H1C43	125.0
N41—NI2—N41^ii	88.3 (1)	C42—C43—H1C43	125.0

Symmetry codes: (i) −x+1/2, −y+3/2, z; (ii) −x+1/2, −y+1/2, z; (iii) −x+1, −y+1, −z+2; (iv) y−1/2, −x+1, z−1/2; (v) −y+1, x+1/2, z−1/2; (vi) −x, −y+1, −z+2; (vii) y−1/2, −x+1, z+1/2; (viii) y, −x+1/2, −z+3/2; (ix) −y+1/2, x, −z+3/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N12A—H1N12A···O6^iv	0.86	1.92	2.722 (3)	154
N12B—H1N12B···O6^iv	0.86	1.92	2.757 (3)	164
N22B—H1N22B···O3^vii	0.86	2.10	2.924 (2)	160
N32—H1N32···O5^ix	0.86	2.15	2.913 (2)	148
N42—H1N42···O3^vii	0.86	2.00	2.771 (2)	149

Symmetry codes: (iv) y−1/2, −x+1, z−1/2; (vii) y−1/2, −x+1, z+1/2; (ix) −y+1/2, x, −z+3/2.