Bis(trimethyl­ene­diammonium) hexa­aqua­copper(II) deca­vanadate heptahydrate

The title compound, (C₃H₁₂N₂)₂[Cu(H₂O)₆][V₁₀O₂₈]·7H₂O, contains [V₁₀O₂₈]⁶⁻ polyanions, [Cu(H₂O)₆]²⁺ cations, H₃NCH₂CH₂CH₂NH₃²⁺ cations and non-coordinated water mol­ecules. A variety of O—H...O and N—H...O hydrogen bonds generate a three-dimensional network. The asymmetric unit contains two half-anions; each anion is centrosymmetric.

Key indicators

• Single-crystal X-ray study
• T = 253 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.028
• wR factor = 0.079
• Data-to-parameter ratio = 13.8

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT223_ALERT_4_C Large Solvent/Anion  H     Ueq(max)/Ueq(min) ...       3.79 Ratio
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  V2     -   O8_a    ..       5.71 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  V8     -   O28     ..       6.47 su
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.32
PLAT480_ALERT_4_C Long H...A H-Bond Reported H1C    ..  O13     ..       2.64 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........         25
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.19 Ratio
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          9
              H2 O

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

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   5 ALERT type 4 Improvement, methodology, query or suggestion

---

Computing details

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

Bis(trimethylenediammonium) hexaaquacopper(II) decavanadate hepatahydrate

Crystal data

(C3H12N2)2[Cu(H2O)6][V10O28]·7H2O	Z = 2
Mr = 1407.44	F(000) = 1402
Triclinic, P1	Dx = 2.294 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.351 (2) Å	Cell parameters from 5958 reflections
b = 11.125 (2) Å	θ = 2.1–28.2°
c = 18.536 (4) Å	µ = 2.82 mm^−1
α = 92.62 (3)°	T = 253 K
β = 103.14 (3)°	Block, green
γ = 100.17 (3)°	0.20 × 0.15 × 0.12 mm
V = 2037.7 (8) Å^3

Data collection

Bruker SMART CCD diffractometer	9825 independent reflections
Radiation source: fine-focus sealed tube	8442 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.018
φ and ω scans	θmax = 28.2°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −13→13
Tmin = 0.605, Tmax = 0.710	k = −14→14
24545 measured reflections	l = −24→24

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.028	Hydrogen site location: difmap and geom
wR(F^2) = 0.079	H atoms treated by a mixture of independent and constrained refinement
S = 1.01	w = 1/[σ^2(Fo^2) + (0.0587P)^2 + 0.0005P] where P = (Fo^2 + 2Fc^2)/3
9825 reflections	(Δ/σ)max = 0.002
713 parameters	Δρmax = 0.53 e Å^−3
105 restraints	Δρmin = −1.81 e Å^−3

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

	x	y	z	Uiso*/Ueq
Cu1	0.507057 (16)	0.507364 (15)	0.247932 (9)	0.01860 (8)
V1	0.73850 (3)	0.24931 (2)	0.447561 (15)	0.02029 (9)
V2	0.84080 (3)	0.32942 (2)	0.615366 (15)	0.01924 (9)
V3	0.94694 (2)	0.45715 (2)	0.410571 (13)	0.01532 (8)
V4	1.25437 (3)	0.48242 (2)	0.491942 (14)	0.01709 (9)
V5	1.04346 (3)	0.27136 (2)	0.524555 (15)	0.01798 (9)
V6	0.25128 (3)	0.75881 (2)	0.056468 (15)	0.01931 (9)
V7	−0.05545 (2)	0.46338 (2)	−0.089997 (13)	0.01396 (8)
V8	0.14378 (3)	0.68730 (2)	−0.112879 (15)	0.01895 (9)
V9	0.25503 (2)	0.49755 (2)	−0.011289 (14)	0.01600 (9)
V10	0.05585 (3)	0.27266 (2)	0.016254 (15)	0.01691 (9)
O1	0.62421 (13)	0.14580 (12)	0.39618 (7)	0.0325 (3)
OW1	0.39773 (14)	0.64337 (14)	0.24572 (8)	0.0362 (3)
HW1	0.3227 (13)	0.6423 (18)	0.2171 (10)	0.037 (6)*
HW1A	0.421 (2)	0.7120 (13)	0.2683 (13)	0.086 (10)*
O2	0.81543 (13)	0.28375 (12)	0.69246 (7)	0.0300 (3)
OW2	0.63070 (15)	0.37673 (14)	0.24849 (8)	0.0394 (4)
HW2A	0.661 (3)	0.356 (3)	0.2130 (12)	0.110 (12)*
HW2	0.6900 (17)	0.3720 (19)	0.2873 (8)	0.037 (6)*
O3	1.15152 (12)	0.18229 (11)	0.52983 (7)	0.0263 (3)
OW3	0.55378 (13)	0.55677 (13)	0.14865 (7)	0.0302 (3)
HW3A	0.4990 (17)	0.5904 (17)	0.1178 (10)	0.032 (6)*
HW3	0.589 (3)	0.513 (2)	0.1234 (14)	0.081 (10)*
O4	1.35946 (12)	0.39046 (11)	0.49829 (7)	0.0249 (3)
OW4	0.68183 (12)	0.63821 (12)	0.30521 (7)	0.0261 (3)
HW4A	0.7215 (19)	0.6160 (16)	0.3458 (7)	0.035 (6)*
HW4	0.668 (2)	0.7082 (11)	0.3126 (11)	0.048 (7)*
O5	0.90959 (10)	0.40995 (10)	0.51519 (6)	0.0162 (2)
OW5	0.45833 (13)	0.45664 (13)	0.34598 (7)	0.0268 (3)
HW5A	0.5095 (19)	0.4261 (19)	0.3801 (10)	0.040 (6)*
HW5	0.418 (3)	0.500 (2)	0.3689 (14)	0.077 (10)*
O6	0.81606 (11)	0.33990 (10)	0.37050 (6)	0.0208 (2)
OW6	0.33499 (12)	0.37704 (12)	0.19219 (7)	0.0247 (3)
HW6A	0.2880 (18)	0.3919 (17)	0.1516 (7)	0.029 (5)*
HW6	0.348 (3)	0.3064 (12)	0.1847 (14)	0.062 (8)*
O7	1.16692 (10)	0.42672 (10)	0.57352 (6)	0.0164 (2)
OW7	0.54041 (14)	0.80520 (13)	−0.02948 (9)	0.0394 (3)
H7A	0.4630 (11)	0.783 (2)	−0.0283 (14)	0.062 (8)*
H7	0.576 (2)	0.7474 (17)	−0.0233 (17)	0.085 (11)*
O8	1.00037 (11)	0.52455 (10)	0.34045 (6)	0.0201 (2)
OW8	0.43958 (14)	0.16397 (14)	0.53259 (9)	0.0411 (3)
H8A	0.5199 (10)	0.171 (2)	0.5308 (14)	0.059 (8)*
H8	0.420 (3)	0.2323 (15)	0.528 (2)	0.128 (15)*
O9	1.35138 (11)	0.61691 (10)	0.55042 (6)	0.0201 (2)
OW9	0.38688 (17)	0.15083 (14)	0.16474 (9)	0.0424 (4)
H9A	0.3190 (17)	0.0997 (19)	0.1617 (13)	0.077 (9)*
H9	0.398 (2)	0.153 (2)	0.1231 (7)	0.067 (9)*
O10	1.26017 (11)	0.54659 (10)	0.40279 (6)	0.0203 (2)
OW10	−0.12799 (16)	−0.02705 (13)	−0.14543 (8)	0.0371 (3)
H10A	−0.122 (3)	0.0247 (17)	−0.1126 (11)	0.091 (11)*
H10	−0.099 (2)	−0.0836 (14)	−0.1268 (11)	0.051 (7)*
O11	0.89035 (11)	0.17946 (10)	0.46197 (6)	0.0215 (2)
OW11	0.92060 (19)	0.00011 (15)	0.36414 (10)	0.0529 (4)
H11A	0.885 (3)	−0.0632 (12)	0.3769 (15)	0.077 (10)*
H11	0.901 (3)	0.0538 (15)	0.3879 (14)	0.086 (11)*
O12	1.08229 (11)	0.36480 (10)	0.43845 (6)	0.0172 (2)
OW12	0.5765 (2)	0.84410 (16)	0.32161 (10)	0.0543 (4)
H12A	0.585 (4)	0.863 (3)	0.3649 (6)	0.109 (14)*
H12	0.591 (3)	0.9078 (14)	0.3037 (13)	0.069 (9)*
O13	0.98414 (11)	0.24860 (10)	0.60770 (6)	0.0206 (2)
OW13	0.5991 (2)	0.04561 (16)	0.23666 (10)	0.0593 (4)
H13A	0.5371 (17)	0.080 (2)	0.2263 (16)	0.097 (12)*
H13	0.6593 (17)	0.0880 (19)	0.2662 (12)	0.074 (10)*
O14	0.72198 (11)	0.22051 (10)	0.54372 (6)	0.0213 (2)
O15	0.16851 (12)	0.19023 (11)	0.01731 (7)	0.0256 (3)
O16	0.17107 (13)	0.73950 (11)	−0.18860 (7)	0.0291 (3)
O17	−0.09494 (11)	0.17913 (10)	−0.04646 (6)	0.0201 (2)
O18	0.36438 (12)	0.86336 (11)	0.10787 (7)	0.0314 (3)
O19	−0.17957 (11)	0.34289 (10)	−0.13134 (6)	0.0189 (2)
O20	0.36424 (11)	0.41002 (10)	−0.00808 (7)	0.0228 (2)
O21	−0.08613 (10)	0.40435 (9)	0.01380 (5)	0.0148 (2)
O22	0.17311 (10)	0.42933 (9)	0.06961 (6)	0.0152 (2)
O23	−0.00626 (11)	0.53888 (10)	−0.15901 (6)	0.0189 (2)
O24	0.26323 (11)	0.79347 (10)	−0.03960 (6)	0.0200 (2)
O25	0.34844 (11)	0.63047 (10)	0.04986 (6)	0.0191 (2)
O26	0.08739 (10)	0.37592 (9)	−0.06618 (6)	0.0152 (2)
O27	0.00026 (11)	0.23902 (10)	0.10095 (6)	0.0197 (2)
O28	0.25577 (11)	0.56861 (10)	−0.09873 (6)	0.0191 (2)
N101	0.2055 (2)	0.01177 (15)	0.41814 (10)	0.0432 (4)
H1C	0.220 (2)	−0.0602 (11)	0.4335 (11)	0.043 (6)*
H1D	0.1168 (10)	0.009 (2)	0.4044 (13)	0.067 (9)*
H1E	0.250 (2)	0.0624 (18)	0.4577 (9)	0.070 (8)*
N301	0.14397 (17)	0.33193 (15)	0.28628 (9)	0.0290 (3)
H3C	0.0686 (15)	0.352 (2)	0.2608 (11)	0.045 (6)*
H3D	0.204 (2)	0.351 (2)	0.2595 (13)	0.065 (8)*
H3E	0.170 (2)	0.3797 (17)	0.3282 (8)	0.042 (6)*
N401	0.66343 (18)	0.98385 (15)	0.09662 (11)	0.0395 (4)
H4C	0.687 (2)	1.0526 (13)	0.0762 (11)	0.053 (7)*
H4D	0.6177 (19)	0.9931 (19)	0.1308 (9)	0.050 (7)*
H4E	0.622 (2)	0.9290 (17)	0.0587 (10)	0.070 (8)*
N601	0.88151 (17)	0.66528 (15)	0.21742 (9)	0.0294 (3)
H6C	0.9542 (14)	0.6421 (19)	0.2427 (11)	0.040 (6)*
H6D	0.816 (2)	0.649 (2)	0.2407 (14)	0.066 (8)*
H6E	0.862 (2)	0.6187 (17)	0.1754 (8)	0.043 (6)*
C1	0.2677 (2)	0.04157 (17)	0.35450 (12)	0.0398 (5)
H1A	0.2173	−0.0123	0.3108	0.048*
H1B	0.3596	0.0272	0.3662	0.048*
C2	0.26924 (19)	0.17390 (16)	0.33745 (11)	0.0346 (4)
H2A	0.3066	0.2264	0.3834	0.042*
H2B	0.3290	0.1946	0.3045	0.042*
C3	0.13226 (19)	0.20131 (16)	0.30187 (10)	0.0322 (4)
H3A	0.0936	0.1493	0.2558	0.039*
H3B	0.0722	0.1833	0.3349	0.039*
C4	0.79540 (19)	0.95429 (16)	0.13511 (11)	0.0359 (4)
H4A	0.8377	1.0133	0.1778	0.043*
H4B	0.8552	0.9593	0.1015	0.043*
C5	0.77358 (18)	0.82740 (16)	0.16017 (11)	0.0308 (4)
H5A	0.7364	0.7685	0.1170	0.037*
H5B	0.7084	0.8212	0.1907	0.037*
C6	0.90388 (18)	0.79617 (17)	0.20427 (10)	0.0324 (4)
H6A	0.9737	0.8137	0.1770	0.039*
H6B	0.9340	0.8460	0.2515	0.039*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cu1	0.01615 (12)	0.02568 (13)	0.01415 (12)	0.00619 (8)	0.00203 (8)	0.00328 (8)
V1	0.01902 (15)	0.02064 (15)	0.01920 (15)	0.00255 (10)	0.00150 (11)	0.00157 (11)
V2	0.01999 (15)	0.02317 (15)	0.01620 (14)	0.00618 (10)	0.00530 (10)	0.00572 (10)
V3	0.01529 (14)	0.01979 (14)	0.01130 (14)	0.00613 (10)	0.00186 (10)	0.00183 (10)
V4	0.01504 (14)	0.02144 (14)	0.01684 (14)	0.00784 (10)	0.00413 (10)	0.00435 (10)
V5	0.01748 (14)	0.01800 (14)	0.02008 (15)	0.00739 (10)	0.00430 (10)	0.00393 (10)
V6	0.01758 (15)	0.01806 (14)	0.01978 (15)	0.00013 (10)	0.00210 (11)	0.00048 (10)
V7	0.01345 (14)	0.01715 (14)	0.01098 (13)	0.00381 (10)	0.00158 (9)	0.00150 (10)
V8	0.02034 (15)	0.02046 (15)	0.01700 (15)	0.00303 (10)	0.00636 (10)	0.00549 (10)
V9	0.01286 (14)	0.01843 (14)	0.01784 (14)	0.00485 (10)	0.00431 (10)	0.00273 (10)
V10	0.01562 (14)	0.01604 (14)	0.02011 (15)	0.00541 (10)	0.00423 (10)	0.00344 (10)
O1	0.0270 (7)	0.0298 (7)	0.0339 (7)	−0.0019 (5)	0.0003 (5)	−0.0038 (5)
OW1	0.0321 (8)	0.0438 (8)	0.0328 (7)	0.0223 (6)	−0.0029 (6)	−0.0007 (6)
O2	0.0317 (7)	0.0401 (7)	0.0237 (6)	0.0129 (5)	0.0111 (5)	0.0141 (5)
OW2	0.0368 (8)	0.0528 (9)	0.0301 (8)	0.0277 (7)	−0.0024 (6)	−0.0027 (7)
O3	0.0258 (6)	0.0247 (6)	0.0325 (7)	0.0131 (5)	0.0082 (5)	0.0066 (5)
OW3	0.0281 (7)	0.0469 (8)	0.0174 (6)	0.0104 (6)	0.0064 (5)	0.0059 (6)
O4	0.0212 (6)	0.0280 (6)	0.0293 (6)	0.0123 (5)	0.0072 (5)	0.0060 (5)
OW4	0.0246 (6)	0.0318 (7)	0.0189 (6)	0.0056 (5)	−0.0012 (5)	0.0039 (5)
O5	0.0163 (5)	0.0183 (5)	0.0150 (5)	0.0062 (4)	0.0034 (4)	0.0030 (4)
OW5	0.0268 (6)	0.0392 (7)	0.0166 (6)	0.0119 (5)	0.0047 (5)	0.0064 (5)
O6	0.0209 (6)	0.0243 (6)	0.0154 (5)	0.0049 (4)	0.0007 (4)	−0.0005 (4)
OW6	0.0241 (6)	0.0283 (6)	0.0184 (6)	0.0052 (5)	−0.0020 (5)	0.0031 (5)
O7	0.0155 (5)	0.0196 (5)	0.0146 (5)	0.0065 (4)	0.0016 (4)	0.0040 (4)
OW7	0.0235 (7)	0.0384 (8)	0.0619 (10)	0.0126 (6)	0.0141 (7)	0.0165 (7)
O8	0.0213 (6)	0.0265 (6)	0.0143 (5)	0.0092 (4)	0.0040 (4)	0.0045 (4)
OW8	0.0301 (8)	0.0430 (8)	0.0552 (9)	0.0129 (6)	0.0145 (7)	0.0123 (7)
O9	0.0156 (5)	0.0230 (5)	0.0213 (6)	0.0055 (4)	0.0019 (4)	0.0036 (4)
OW9	0.0456 (9)	0.0351 (8)	0.0452 (9)	0.0086 (7)	0.0079 (7)	0.0015 (7)
O10	0.0186 (5)	0.0271 (6)	0.0184 (5)	0.0088 (4)	0.0069 (4)	0.0051 (4)
OW10	0.0502 (9)	0.0289 (7)	0.0342 (7)	0.0108 (6)	0.0119 (6)	0.0034 (6)
O11	0.0216 (6)	0.0185 (5)	0.0237 (6)	0.0054 (4)	0.0030 (5)	0.0000 (4)
OW11	0.0827 (12)	0.0302 (8)	0.0547 (10)	0.0064 (8)	0.0386 (9)	0.0017 (7)
O12	0.0185 (5)	0.0198 (5)	0.0149 (5)	0.0080 (4)	0.0041 (4)	0.0013 (4)
OW12	0.0807 (13)	0.0405 (9)	0.0433 (10)	0.0205 (9)	0.0115 (9)	0.0022 (8)
O13	0.0209 (6)	0.0223 (6)	0.0201 (6)	0.0077 (4)	0.0041 (4)	0.0077 (4)
OW13	0.0730 (13)	0.0544 (10)	0.0473 (10)	0.0196 (10)	0.0028 (9)	0.0004 (8)
O14	0.0191 (5)	0.0219 (6)	0.0235 (6)	0.0043 (4)	0.0053 (4)	0.0060 (4)
O15	0.0243 (6)	0.0244 (6)	0.0319 (6)	0.0121 (5)	0.0080 (5)	0.0064 (5)
O16	0.0348 (7)	0.0323 (7)	0.0253 (6)	0.0089 (5)	0.0141 (5)	0.0122 (5)
O17	0.0201 (5)	0.0170 (5)	0.0220 (6)	0.0032 (4)	0.0031 (4)	−0.0003 (4)
O18	0.0247 (6)	0.0264 (6)	0.0359 (7)	−0.0032 (5)	0.0005 (5)	−0.0052 (5)
O19	0.0187 (5)	0.0213 (5)	0.0145 (5)	0.0030 (4)	0.0006 (4)	−0.0014 (4)
O20	0.0186 (6)	0.0257 (6)	0.0273 (6)	0.0095 (4)	0.0075 (5)	0.0048 (5)
O21	0.0137 (5)	0.0164 (5)	0.0143 (5)	0.0033 (4)	0.0025 (4)	0.0025 (4)
O22	0.0137 (5)	0.0175 (5)	0.0143 (5)	0.0047 (4)	0.0015 (4)	0.0023 (4)
O23	0.0198 (5)	0.0240 (6)	0.0138 (5)	0.0060 (4)	0.0044 (4)	0.0039 (4)
O24	0.0177 (5)	0.0190 (5)	0.0233 (6)	0.0015 (4)	0.0060 (4)	0.0053 (4)
O25	0.0140 (5)	0.0212 (5)	0.0208 (5)	0.0026 (4)	0.0020 (4)	0.0017 (4)
O26	0.0151 (5)	0.0175 (5)	0.0136 (5)	0.0055 (4)	0.0032 (4)	0.0013 (4)
O27	0.0201 (6)	0.0201 (5)	0.0201 (6)	0.0060 (4)	0.0045 (4)	0.0067 (4)
O28	0.0184 (5)	0.0231 (5)	0.0189 (5)	0.0064 (4)	0.0080 (4)	0.0049 (4)
N101	0.0717 (14)	0.0233 (8)	0.0365 (10)	0.0120 (8)	0.0137 (10)	0.0074 (7)
N301	0.0359 (9)	0.0319 (8)	0.0216 (8)	0.0137 (7)	0.0058 (7)	0.0032 (6)
N401	0.0386 (10)	0.0284 (8)	0.0531 (12)	0.0078 (7)	0.0103 (9)	0.0193 (8)
N601	0.0345 (9)	0.0371 (9)	0.0200 (7)	0.0187 (7)	0.0040 (6)	0.0035 (6)
C1	0.0489 (12)	0.0316 (10)	0.0436 (11)	0.0146 (9)	0.0145 (9)	0.0070 (8)
C2	0.0355 (10)	0.0284 (9)	0.0393 (10)	0.0049 (7)	0.0074 (8)	0.0104 (8)
C3	0.0354 (10)	0.0284 (9)	0.0323 (10)	0.0045 (7)	0.0078 (8)	0.0040 (7)
C4	0.0338 (10)	0.0274 (9)	0.0450 (11)	0.0040 (7)	0.0067 (8)	0.0080 (8)
C5	0.0317 (9)	0.0265 (9)	0.0347 (10)	0.0069 (7)	0.0063 (8)	0.0091 (7)
C6	0.0319 (10)	0.0331 (9)	0.0296 (9)	0.0047 (7)	0.0037 (8)	0.0014 (7)

Geometric parameters (Å, º)

Cu1—OW1	2.0399 (14)	OW2—HW2	0.84 (2)
Cu1—OW5	2.0702 (13)	OW3—HW3A	0.86 (2)
Cu1—OW3	2.0798 (13)	OW3—HW3	0.84 (2)
Cu1—OW2	2.0983 (15)	OW4—HW4A	0.84 (2)
Cu1—OW6	2.1110 (15)	OW4—HW4	0.83 (2)
Cu1—OW4	2.1388 (15)	O5—V3^i	2.0963 (14)
V1—O1	1.5933 (14)	O5—V4^i	2.2276 (12)
V1—O11	1.8454 (12)	OW5—HW5A	0.85 (2)
V1—O14	1.8656 (12)	OW5—HW5	0.85 (2)
V1—O9^i	1.8926 (12)	OW6—HW6A	0.84 (2)
V1—O6	2.0170 (13)	OW6—HW6	0.83 (2)
V1—O5	2.3600 (15)	O7—V3^i	1.9510 (12)
V2—O2	1.5997 (12)	OW7—H7A	0.80 (2)
V2—O14	1.8243 (14)	OW7—H7	0.80 (2)
V2—O10^i	1.8709 (12)	O8—V2^i	2.0823 (15)
V2—O13	1.8935 (12)	OW8—H8A	0.83 (2)
V2—O8^i	2.0823 (15)	OW8—H8	0.82 (2)
V2—O5	2.2990 (12)	O9—V1^i	1.8926 (12)
V3—O8	1.6813 (12)	OW9—H9A	0.81 (2)
V3—O6	1.7083 (13)	OW9—H9	0.81 (2)
V3—O12	1.8744 (12)	O10—V2^i	1.8709 (12)
V3—O7^i	1.9510 (12)	OW10—H10A	0.80 (2)
V3—O5^i	2.0963 (14)	OW10—H10	0.80 (2)
V3—O5	2.1325 (11)	OW11—H11A	0.81 (2)
V4—O4	1.6093 (12)	OW11—H11	0.81 (2)
V4—O9	1.8023 (14)	OW12—H12A	0.80 (2)
V4—O10	1.8390 (12)	OW12—H12	0.80 (2)
V4—O7	1.9998 (12)	OW13—H13A	0.80 (2)
V4—O12	2.0306 (14)	OW13—H13	0.80 (2)
V4—O5^i	2.2276 (12)	O17—V6^ii	1.8439 (12)
V5—O3	1.6104 (12)	O19—V6^ii	2.0181 (13)
V5—O13	1.7965 (12)	O21—V7^ii	2.1013 (14)
V5—O11	1.8401 (14)	O21—V9^ii	2.2117 (11)
V5—O7	1.9984 (14)	O21—V8^ii	2.2855 (12)
V5—O12	2.0213 (12)	O21—V6^ii	2.3641 (15)
V5—O5	2.2355 (12)	O22—V7^ii	1.9319 (11)
V6—O18	1.5943 (14)	O27—V8^ii	1.8732 (12)
V6—O17^ii	1.8439 (12)	N101—C1	1.491 (3)
V6—O24	1.8657 (12)	N101—H1C	0.89 (2)
V6—O25	1.9007 (12)	N101—H1D	0.89 (2)
V6—O19^ii	2.0181 (13)	N101—H1E	0.89 (2)
V6—O21^ii	2.3641 (15)	N301—C3	1.484 (2)
V7—O23	1.6865 (12)	N301—H3C	0.89 (2)
V7—O19	1.6985 (13)	N301—H3D	0.88 (2)
V7—O26	1.8917 (12)	N301—H3E	0.88 (2)
V7—O22^ii	1.9319 (11)	N401—C4	1.490 (2)
V7—O21^ii	2.1013 (14)	N401—H4C	0.89 (2)
V7—O21	2.1338 (11)	N401—H4D	0.89 (2)
V8—O16	1.6075 (12)	N401—H4E	0.89 (2)
V8—O24	1.8283 (14)	N601—C6	1.474 (2)
V8—O27^ii	1.8732 (12)	N601—H6C	0.88 (2)
V8—O28	1.8949 (12)	N601—H6D	0.88 (2)
V8—O23	2.0570 (14)	N601—H6E	0.88 (2)
V8—O21^ii	2.2855 (12)	C1—C2	1.518 (2)
V9—O20	1.6105 (12)	C1—H1A	0.9700
V9—O25	1.8027 (13)	C1—H1B	0.9700
V9—O28	1.8365 (12)	C2—C3	1.512 (3)
V9—O22	1.9996 (12)	C2—H2A	0.9700
V9—O26	2.0296 (14)	C2—H2B	0.9700
V9—O21^ii	2.2117 (11)	C3—H3A	0.9700
V10—O15	1.6032 (12)	C3—H3B	0.9700
V10—O27	1.8232 (12)	C4—C5	1.502 (2)
V10—O17	1.8333 (14)	C4—H4A	0.9700
V10—O26	2.0041 (12)	C4—H4B	0.9700
V10—O22	2.0097 (13)	C5—C6	1.516 (2)
V10—O21	2.2461 (12)	C5—H5A	0.9700
OW1—HW1	0.83 (2)	C5—H5B	0.9700
OW1—HW1A	0.82 (2)	C6—H6A	0.9700
OW2—HW2A	0.83 (2)	C6—H6B	0.9700
OW1—Cu1—OW5	90.00 (6)	O15—V10—O26	99.82 (6)
OW1—Cu1—OW3	90.00 (6)	O27—V10—O26	154.70 (5)
OW5—Cu1—OW3	179.26 (4)	O17—V10—O26	90.30 (5)
OW1—Cu1—OW2	175.88 (6)	O15—V10—O22	99.90 (6)
OW5—Cu1—OW2	92.83 (6)	O27—V10—O22	89.26 (5)
OW3—Cu1—OW2	87.21 (6)	O17—V10—O22	155.14 (5)
OW1—Cu1—OW6	92.17 (6)	O26—V10—O22	76.23 (5)
OW5—Cu1—OW6	86.81 (6)	O15—V10—O21	174.24 (5)
OW3—Cu1—OW6	92.45 (6)	O27—V10—O21	80.30 (5)
OW2—Cu1—OW6	90.98 (6)	O17—V10—O21	81.23 (5)
OW1—Cu1—OW4	88.18 (6)	O26—V10—O21	76.06 (5)
OW5—Cu1—OW4	92.77 (6)	O22—V10—O21	75.33 (5)
OW3—Cu1—OW4	87.97 (6)	Cu1—OW1—HW1	125.3 (14)
OW2—Cu1—OW4	88.69 (6)	Cu1—OW1—HW1A	127.9 (15)
OW6—Cu1—OW4	179.45 (4)	HW1—OW1—HW1A	106.4 (14)
O1—V1—O11	103.16 (6)	Cu1—OW2—HW2A	125 (2)
O1—V1—O14	103.74 (7)	Cu1—OW2—HW2	119.7 (15)
O11—V1—O14	90.62 (6)	HW2A—OW2—HW2	106 (3)
O1—V1—O9^i	102.48 (6)	Cu1—OW3—HW3A	119.6 (14)
O11—V1—O9^i	153.42 (5)	Cu1—OW3—HW3	123 (2)
O14—V1—O9^i	90.02 (6)	HW3A—OW3—HW3	107 (2)
O1—V1—O6	101.08 (6)	Cu1—OW4—HW4A	113.2 (13)
O11—V1—O6	84.97 (5)	Cu1—OW4—HW4	114.7 (16)
O14—V1—O6	155.15 (5)	HW4A—OW4—HW4	108.9 (14)
O9^i—V1—O6	83.37 (5)	V3^i—O5—V3	101.94 (5)
O1—V1—O5	175.55 (6)	V3^i—O5—V4^i	93.61 (5)
O11—V1—O5	77.48 (5)	V3—O5—V4^i	93.89 (5)
O14—V1—O5	80.63 (5)	V3^i—O5—V5	94.25 (5)
O9^i—V1—O5	76.42 (5)	V3—O5—V5	92.16 (5)
O6—V1—O5	74.54 (5)	V4^i—O5—V5	168.89 (6)
O2—V2—O14	105.04 (7)	V3^i—O5—V2	88.56 (4)
O2—V2—O10^i	103.84 (6)	V3—O5—V2	169.48 (6)
O14—V2—O10^i	93.48 (6)	V4^i—O5—V2	85.97 (4)
O2—V2—O13	99.10 (6)	V5—O5—V2	86.39 (4)
O14—V2—O13	91.31 (6)	V3^i—O5—V1	171.42 (5)
O10^i—V2—O13	154.44 (5)	V3—O5—V1	86.64 (5)
O2—V2—O8^i	97.53 (7)	V4^i—O5—V1	85.73 (4)
O14—V2—O8^i	157.28 (5)	V5—O5—V1	85.33 (4)
O10^i—V2—O8^i	83.51 (5)	V2—O5—V1	82.86 (4)
O13—V2—O8^i	82.44 (5)	Cu1—OW5—HW5A	124.3 (15)
O2—V2—O5	171.15 (6)	Cu1—OW5—HW5	121.1 (19)
O14—V2—O5	83.17 (5)	HW5A—OW5—HW5	105 (2)
O10^i—V2—O5	78.56 (5)	V3—O6—V1	111.64 (6)
O13—V2—O5	77.10 (5)	Cu1—OW6—HW6A	119.5 (13)
O8^i—V2—O5	74.16 (5)	Cu1—OW6—HW6	115.3 (18)
O8—V3—O6	106.46 (6)	HW6A—OW6—HW6	105 (2)
O8—V3—O12	98.80 (6)	V3^i—O7—V5	107.05 (5)
O6—V3—O12	98.50 (6)	V3^i—O7—V4	107.52 (5)
O8—V3—O7^i	96.21 (5)	V5—O7—V4	101.34 (5)
O6—V3—O7^i	95.46 (5)	H7A—OW7—H7	107.2 (15)
O12—V3—O7^i	155.66 (5)	V3—O8—V2^i	108.97 (6)
O8—V3—O5^i	88.26 (6)	H8A—OW8—H8	106.4 (15)
O6—V3—O5^i	165.06 (5)	V4—O9—V1^i	115.33 (6)
O12—V3—O5^i	81.31 (5)	H9A—OW9—H9	105.9 (15)
O7^i—V3—O5^i	80.11 (5)	V4—O10—V2^i	112.61 (6)
O8—V3—O5	166.14 (5)	H10A—OW10—H10	107.4 (15)
O6—V3—O5	87.12 (6)	V5—O11—V1	115.43 (6)
O12—V3—O5	81.50 (5)	H11A—OW11—H11	105.3 (15)
O7^i—V3—O5	79.39 (5)	V3—O12—V5	107.71 (6)
O5^i—V3—O5	78.06 (5)	V3—O12—V4	107.65 (5)
O4—V4—O9	103.33 (6)	V5—O12—V4	99.50 (5)
O4—V4—O10	102.89 (6)	H12A—OW12—H12	105 (3)
O9—V4—O10	96.33 (6)	V5—O13—V2	114.51 (6)
O4—V4—O7	98.81 (6)	H13A—OW13—H13	109.8 (16)
O9—V4—O7	90.68 (6)	V2—O14—V1	113.35 (6)
O10—V4—O7	154.94 (5)	V10—O17—V6^ii	115.41 (6)
O4—V4—O12	99.38 (6)	V7—O19—V6^ii	112.21 (6)
O9—V4—O12	155.15 (5)	V7^ii—O21—V7	101.74 (5)
O10—V4—O12	88.25 (6)	V7^ii—O21—V9^ii	94.20 (5)
O7—V4—O12	75.89 (5)	V7—O21—V9^ii	93.29 (5)
O4—V4—O5^i	173.00 (5)	V7^ii—O21—V10	94.08 (5)
O9—V4—O5^i	81.72 (5)	V7—O21—V10	91.94 (5)
O10—V4—O5^i	81.13 (5)	V9^ii—O21—V10	169.10 (5)
O7—V4—O5^i	76.11 (5)	V7^ii—O21—V8^ii	88.09 (4)
O12—V4—O5^i	74.85 (5)	V7—O21—V8^ii	170.12 (5)
O3—V5—O13	102.98 (6)	V9^ii—O21—V8^ii	86.88 (4)
O3—V5—O11	103.00 (6)	V10—O21—V8^ii	86.33 (4)
O13—V5—O11	94.96 (6)	V7^ii—O21—V6^ii	171.60 (5)
O3—V5—O7	99.62 (6)	V7—O21—V6^ii	86.63 (5)
O13—V5—O7	90.19 (6)	V9^ii—O21—V6^ii	86.02 (4)
O11—V5—O7	155.00 (5)	V10—O21—V6^ii	84.75 (4)
O3—V5—O12	99.76 (6)	V8^ii—O21—V6^ii	83.53 (4)
O13—V5—O12	155.13 (5)	V7^ii—O22—V9	106.98 (5)
O11—V5—O12	89.59 (6)	V7^ii—O22—V10	107.70 (5)
O7—V5—O12	76.13 (5)	V9—O22—V10	100.81 (5)
O3—V5—O5	174.23 (5)	V7—O23—V8	108.86 (6)
O13—V5—O5	80.71 (5)	V8—O24—V6	113.97 (6)
O11—V5—O5	80.93 (5)	V9—O25—V6	114.97 (6)
O7—V5—O5	75.78 (5)	V7—O26—V10	107.88 (5)
O12—V5—O5	75.88 (5)	V7—O26—V9	107.35 (5)
O18—V6—O17^ii	103.76 (6)	V10—O26—V9	99.97 (5)
O18—V6—O24	103.28 (7)	V10—O27—V8^ii	114.00 (6)
O17^ii—V6—O24	91.64 (6)	V9—O28—V8	111.95 (6)
O18—V6—O25	101.96 (6)	C1—N101—H1C	110.7 (14)
O17^ii—V6—O25	153.35 (5)	C1—N101—H1D	109.9 (16)
O24—V6—O25	89.18 (6)	H1C—N101—H1D	109 (2)
O18—V6—O19^ii	102.74 (6)	C1—N101—H1E	109.3 (17)
O17^ii—V6—O19^ii	84.52 (5)	H1C—N101—H1E	101 (2)
O24—V6—O19^ii	153.87 (5)	H1D—N101—H1E	116 (2)
O25—V6—O19^ii	83.12 (5)	C3—N301—H3C	115.4 (15)
O18—V6—O21^ii	176.45 (6)	C3—N301—H3D	110.5 (17)
O17^ii—V6—O21^ii	77.83 (5)	H3C—N301—H3D	105 (2)
O24—V6—O21^ii	79.77 (5)	C3—N301—H3E	110.2 (14)
O25—V6—O21^ii	76.12 (5)	H3C—N301—H3E	106 (2)
O19^ii—V6—O21^ii	74.15 (5)	H3D—N301—H3E	109 (2)
O23—V7—O19	106.69 (6)	C4—N401—H4C	103.9 (15)
O23—V7—O26	98.22 (6)	C4—N401—H4D	107.4 (14)
O19—V7—O26	97.61 (5)	H4C—N401—H4D	113 (2)
O23—V7—O22^ii	96.52 (5)	C4—N401—H4E	111.0 (16)
O19—V7—O22^ii	96.63 (5)	H4C—N401—H4E	105 (2)
O26—V7—O22^ii	155.61 (5)	H4D—N401—H4E	116 (2)
O23—V7—O21^ii	88.05 (5)	C6—N601—H6C	113.5 (14)
O19—V7—O21^ii	165.23 (5)	C6—N601—H6D	109.5 (18)
O26—V7—O21^ii	80.77 (5)	H6C—N601—H6D	110 (2)
O22^ii—V7—O21^ii	80.42 (5)	C6—N601—H6E	111.0 (14)
O23—V7—O21	166.24 (5)	H6C—N601—H6E	102.8 (19)
O19—V7—O21	86.98 (6)	H6D—N601—H6E	110 (2)
O26—V7—O21	81.17 (5)	N101—C1—C2	111.72 (16)
O22^ii—V7—O21	79.92 (5)	N101—C1—H1A	109.3
O21^ii—V7—O21	78.26 (5)	C2—C1—H1A	109.3
O16—V8—O24	103.98 (6)	N101—C1—H1B	109.3
O16—V8—O27^ii	101.23 (6)	C2—C1—H1B	109.3
O24—V8—O27^ii	91.81 (6)	H1A—C1—H1B	107.9
O16—V8—O28	101.34 (6)	C3—C2—C1	114.52 (16)
O24—V8—O28	91.45 (5)	C3—C2—H2A	108.6
O27^ii—V8—O28	155.67 (5)	C1—C2—H2A	108.6
O16—V8—O23	98.34 (6)	C3—C2—H2B	108.6
O24—V8—O23	157.67 (5)	C1—C2—H2B	108.6
O27^ii—V8—O23	84.04 (5)	H2A—C2—H2B	107.6
O28—V8—O23	83.85 (5)	N301—C3—C2	110.68 (15)
O16—V8—O21^ii	173.33 (6)	N301—C3—H3A	109.5
O24—V8—O21^ii	82.69 (5)	C2—C3—H3A	109.5
O27^ii—V8—O21^ii	78.25 (5)	N301—C3—H3B	109.5
O28—V8—O21^ii	78.26 (5)	C2—C3—H3B	109.5
O23—V8—O21^ii	74.99 (5)	H3A—C3—H3B	108.1
O20—V9—O25	103.27 (6)	N401—C4—C5	109.86 (15)
O20—V9—O28	103.14 (6)	N401—C4—H4A	109.7
O25—V9—O28	96.50 (6)	C5—C4—H4A	109.7
O20—V9—O22	97.66 (6)	N401—C4—H4B	109.7
O25—V9—O22	91.03 (5)	C5—C4—H4B	109.7
O28—V9—O22	155.55 (5)	H4A—C4—H4B	108.2
O20—V9—O26	98.61 (6)	C4—C5—C6	111.86 (15)
O25—V9—O26	155.83 (5)	C4—C5—H5A	109.2
O28—V9—O26	88.32 (5)	C6—C5—H5A	109.2
O22—V9—O26	75.88 (5)	C4—C5—H5B	109.2
O20—V9—O21^ii	172.35 (5)	C6—C5—H5B	109.2
O25—V9—O21^ii	82.10 (5)	H5A—C5—H5B	107.9
O28—V9—O21^ii	81.42 (5)	N601—C6—C5	109.67 (15)
O22—V9—O21^ii	76.61 (5)	N601—C6—H6A	109.7
O26—V9—O21^ii	75.21 (5)	C5—C6—H6A	109.7
O15—V10—O27	103.06 (6)	N601—C6—H6B	109.7
O15—V10—O17	102.98 (6)	C5—C6—H6B	109.7
O27—V10—O17	94.92 (6)	H6A—C6—H6B	108.2

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
OW1—HW1···O19^ii	0.83 (2)	1.95 (2)	2.756 (3)	163 (2)
OW1—HW1A···OW12	0.82 (2)	2.01 (2)	2.731 (3)	146 (2)
OW2—HW2A···O16^iii	0.83 (3)	2.31 (3)	2.993 (3)	140 (2)
OW2—HW2A···O28^iii	0.83 (3)	2.58 (3)	3.293 (3)	144 (2)
OW2—HW2···O6	0.84 (2)	1.87 (2)	2.712 (3)	173 (2)
OW3—HW3A···O25	0.86 (2)	1.90 (2)	2.744 (3)	167 (2)
OW3—HW3···O28^iii	0.84 (3)	2.10 (3)	2.893 (3)	156 (1)
OW3—HW3···O20^iii	0.84 (3)	2.46 (3)	2.937 (3)	117 (1)
OW4—HW4A···O7^i	0.84 (2)	1.81 (2)	2.641 (3)	170 (2)
OW4—HW4···OW12	0.83 (2)	1.94 (2)	2.738 (3)	162 (2)
OW5—HW5A···O9^i	0.85 (3)	1.85 (2)	2.689 (3)	168 (2)
OW5—HW5···O10^iv	0.85 (3)	2.02 (3)	2.816 (3)	157 (2)
OW6—HW6A···O22	0.84 (2)	1.82 (2)	2.654 (3)	174 (2)
OW6—HW6···OW9	0.83 (2)	1.88 (2)	2.714 (3)	176 (3)
OW7—H7A···O24	0.80 (2)	2.06 (1)	2.812 (3)	157 (2)
OW7—H7···O20^iii	0.80 (2)	2.03 (2)	2.805 (3)	167 (2)
OW7—H7···O15^iii	0.80 (2)	2.59 (2)	2.961 (3)	110 (1)
OW8—H8A···O14	0.83 (2)	2.02 (1)	2.837 (3)	167 (2)
OW8—H8···O4^iv	0.82 (2)	2.03 (2)	2.844 (3)	171 (1)
OW9—H9···OW7^iii	0.81 (2)	2.03 (2)	2.816 (3)	166 (1)
OW10—H10A···O17	0.80 (2)	2.00 (2)	2.792 (3)	167 (2)
OW10—H10···O27^v	0.80 (2)	2.18 (2)	2.962 (3)	165 (2)
OW10—H10···O15^v	0.80 (2)	2.57 (2)	3.113 (3)	126 (2)
OW11—H11A···O3^vi	0.81 (2)	2.28 (2)	3.006 (3)	149 (2)
OW11—H11···O11	0.81 (2)	1.95 (2)	2.742 (3)	167 (3)
OW12—H12A···OW8^vii	0.80 (2)	2.00 (2)	2.750 (3)	156 (2)
OW12—H12···OW13^viii	0.80 (2)	2.02 (2)	2.804 (3)	166 (2)
N101—H1C···O14^ix	0.89 (2)	2.01 (1)	2.890 (3)	170 (2)
N101—H1C···O13^ix	0.89 (2)	2.65 (2)	3.148 (3)	117 (2)
N101—H1D···OW11^iv	0.89 (2)	1.98 (2)	2.868 (3)	175 (2)
N101—H1E···OW8	0.89 (2)	2.21 (2)	3.021 (3)	152 (2)
N101—H1E···O3^iv	0.89 (2)	2.35 (2)	2.956 (3)	125 (2)
N301—H3C···O23^ii	0.89 (2)	2.32 (2)	3.028 (3)	137 (2)
N301—H3C···O16^ii	0.89 (2)	2.54 (2)	3.288 (3)	142 (2)
N301—H3D···OW6	0.88 (2)	2.04 (2)	2.915 (3)	174 (2)
N301—H3E···O10^iv	0.88 (2)	2.19 (2)	3.024 (3)	158
N301—H3E···O12^iv	0.88 (2)	2.42 (2)	3.050 (3)	129
N401—H4C···O24^x	0.89 (2)	1.90 (2)	2.788 (3)	176 (2)
N401—H4D···OW13^viii	0.89 (2)	2.08 (2)	2.904 (3)	154 (2)
N401—H4E···OW7	0.88 (2)	2.01 (2)	2.892 (3)	176 (2)
N601—H6C···O8	0.88 (2)	2.30 (2)	2.983 (3)	135 (2)
N601—H6D···OW4	0.88 (2)	2.02 (2)	2.892 (3)	170 (2)
N601—H6E···O26^iii	0.88 (2)	2.20 (2)	2.918 (3)	138 (2)

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