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A novel modified polyoxometalate, {PMo12O40[Cu(2,2′-bpy)]}[Cu(2,2′-bpy)(en)(H2O)]2 [2,2′-bpy is 2,2′-bipyridyl (C10H8N2) and en is ethyl­enedi­amine (C2H8N2)], has been synthesized hydro­thermally and structurally characterized by elemental analysis, TG, IR, XPS and single-crystal X-ray diffraction. The structural analysis reveals that the com­pound contains the reduced Keggin polyanion [PMo12O40]6− as the parent unit, which is monocapped by [Cu(2,2′-bpy)]2+ fragments via four bridging O atoms on an {Mo4O4} pit and bi-supported by two [Cu(2,2′-bpy)(en)(H2O)]2+ coordination cations simultaneously. There exist strong intra­molecular π–π stacking between the capping and supporting units, which play a stabilizing role during the crystallization of the com­pound. Adjacent POM clusters are further aggregated to form a three-dimensional supra­molecular network through noncovalent forces, hydrogen bonding and π–π stacking inter­actions. In addition, the photocatalytic properties were investigated in detail, and the results indicated that the com­pound can be used as a photocatalyst towards the decom­position of the organic pollutant methyl­ene blue (MB).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229619011999/qp3028sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229619011999/qp3028Isup2.hkl
Contains datablock I

CCDC reference: 1910111

Computing details top

Data collection: APEX2 (Bruker, 2012); cell refinement: SAINT (Bruker, 2012); data reduction: SAINT (Bruker, 2012); program(s) used to solve structure: SHELXS2014 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: pubCIF (Westrip, 2010).

(I) top
Crystal data top
{[PMo12O40]Cu(C10H8N2)}[Cu(C10H8N2)(C2H8N2)(H2O)]2F(000) = 5040
Mr = 2637.69Dx = 2.732 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C2ycCell parameters from 9970 reflections
a = 18.9465 (8) Åθ = 2.2–26.1°
b = 14.7806 (6) ŵ = 3.36 mm1
c = 24.5444 (10) ÅT = 296 K
β = 111.093 (1)°Prism, black
V = 6412.9 (5) Å30.36 × 0.27 × 0.21 mm
Z = 4
Data collection top
Bruker APEXII CCD
diffractometer
6363 independent reflections
Radiation source: fine-focus sealed tube5864 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.018
φ and ω scansθmax = 26.1°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2012)
h = 2223
Tmin = 0.377, Tmax = 0.539k = 1718
17366 measured reflectionsl = 2130
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.019Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.047H atoms treated by a mixture of independent and constrained refinement
S = 1.08 w = 1/[σ2(Fo2) + (0.0198P)2 + 10.7248P]
where P = (Fo2 + 2Fc2)/3
6363 reflections(Δ/σ)max = 0.002
545 parametersΔρmax = 0.55 e Å3
2 restraintsΔρmin = 0.48 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
P10.50000.11132 (6)0.25000.00891 (18)
Mo10.336787 (13)0.118060 (14)0.120477 (10)0.01141 (6)
Mo20.474146 (13)0.279639 (14)0.142142 (10)0.01214 (6)
Mo30.358431 (13)0.282904 (15)0.221090 (10)0.01269 (6)
Mo40.486698 (13)0.054521 (14)0.142939 (9)0.01100 (6)
Mo50.623739 (13)0.106362 (15)0.169174 (10)0.01289 (6)
Mo60.642343 (13)0.058302 (14)0.269812 (10)0.01166 (6)
Cu10.50000.18894 (3)0.25000.01527 (10)
Cu20.570050 (19)0.20825 (2)0.060638 (14)0.01556 (8)
O10.26363 (11)0.09360 (12)0.05829 (8)0.0162 (4)
O20.47990 (11)0.35763 (12)0.09361 (8)0.0166 (4)
O30.29622 (11)0.36381 (12)0.22123 (8)0.0170 (4)
O40.45804 (11)0.13263 (12)0.08892 (8)0.0181 (4)
O50.67732 (11)0.12651 (12)0.12867 (8)0.0192 (4)
O60.70752 (11)0.13955 (12)0.29626 (8)0.0171 (4)
O70.39043 (10)0.21110 (12)0.09244 (8)0.0140 (4)
O80.29887 (10)0.21498 (11)0.15387 (8)0.0134 (4)
O90.32482 (10)0.03216 (12)0.17340 (8)0.0135 (4)
O100.41312 (10)0.03319 (11)0.11632 (7)0.0129 (4)
O110.40624 (10)0.33943 (11)0.17236 (8)0.0140 (4)
O120.55398 (10)0.31369 (12)0.21251 (8)0.0152 (4)
O130.53959 (10)0.18767 (12)0.13468 (8)0.0149 (4)
O140.55650 (10)0.01209 (11)0.12071 (8)0.0142 (4)
O150.57115 (11)0.11712 (11)0.19952 (8)0.0141 (4)
O160.43503 (10)0.09580 (11)0.19692 (8)0.0136 (4)
O170.67675 (10)0.00923 (11)0.21756 (8)0.0139 (4)
O180.65857 (10)0.19045 (12)0.23001 (8)0.0148 (4)
O190.44260 (10)0.17127 (11)0.20388 (7)0.0116 (4)
O200.54325 (10)0.05232 (11)0.22112 (7)0.0114 (4)
O1W0.64402 (15)0.28826 (19)0.01833 (11)0.0365 (6)
N10.44137 (14)0.29168 (15)0.20129 (11)0.0206 (5)
N20.48147 (13)0.28857 (15)0.01977 (10)0.0170 (5)
N30.58804 (13)0.30346 (15)0.12243 (10)0.0174 (5)
N40.66253 (15)0.13739 (18)0.10498 (11)0.0192 (5)
N50.55660 (16)0.11531 (16)0.00292 (11)0.0180 (5)
C10.38204 (18)0.2855 (2)0.15137 (14)0.0240 (7)
C20.3461 (2)0.3610 (2)0.12065 (17)0.0338 (8)
C30.3731 (2)0.4453 (2)0.14171 (17)0.0386 (9)
H30.35010.49690.12130.046*
C40.4336 (2)0.4530 (2)0.19247 (17)0.0335 (8)
C50.46789 (17)0.37479 (18)0.22252 (14)0.0233 (7)
C60.42231 (17)0.2719 (2)0.02902 (13)0.0209 (6)
C70.36729 (18)0.3347 (2)0.05551 (13)0.0268 (7)
C80.37382 (19)0.4197 (2)0.03069 (14)0.0292 (7)
C90.43438 (19)0.4383 (2)0.01986 (14)0.0268 (7)
C100.48744 (17)0.37155 (18)0.04455 (12)0.0192 (6)
C110.55105 (17)0.38108 (18)0.10072 (13)0.0191 (6)
C120.5718 (2)0.4614 (2)0.13141 (15)0.0284 (7)
C130.62931 (19)0.4621 (2)0.18492 (15)0.0302 (7)
C140.66387 (18)0.3817 (2)0.20864 (14)0.0255 (7)
C150.64171 (17)0.3036 (2)0.17582 (13)0.0199 (6)
C160.68363 (18)0.0805 (2)0.06350 (13)0.0217 (6)
C170.61254 (17)0.04111 (19)0.01998 (12)0.0188 (6)
H17B0.6255 (16)0.0119 (19)0.0115 (13)0.015 (7)*
H16B0.7085 (18)0.1196 (19)0.0465 (13)0.018 (8)*
H70.3280 (14)0.322 (2)0.0884 (10)0.026 (9)*
H17A0.5901 (17)0.002 (2)0.0407 (13)0.020 (8)*
H120.548 (2)0.511 (2)0.1182 (15)0.036 (10)*
H60.4182 (18)0.214 (2)0.0444 (14)0.027 (9)*
H90.4394 (19)0.4929 (15)0.0374 (14)0.038 (10)*
H150.6651 (16)0.251 (2)0.1913 (12)0.015 (7)*
H4A0.6539 (19)0.101 (2)0.1319 (15)0.028 (9)*
H140.7045 (18)0.3757 (19)0.2436 (14)0.021 (8)*
H80.337 (2)0.460 (2)0.0478 (15)0.032 (9)*
H16A0.7176 (17)0.0341 (19)0.0826 (12)0.012 (7)*
H10.3666 (18)0.226 (2)0.1397 (14)0.026 (9)*
H130.6432 (19)0.515 (2)0.2027 (14)0.029 (9)*
H40.454 (2)0.508 (3)0.2084 (16)0.046 (11)*
H4B0.6956 (19)0.170 (2)0.1202 (14)0.023 (10)*
H20.303 (2)0.357 (2)0.0877 (16)0.036 (10)*
H2W0.639 (3)0.268 (3)0.019 (2)0.080 (16)*
H1W0.673 (3)0.323 (3)0.0301 (19)0.053 (14)*
H5A0.5611 (19)0.138 (2)0.0330 (15)0.028 (9)*
H5B0.515 (2)0.097 (2)0.0170 (14)0.016 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
P10.0104 (5)0.0076 (4)0.0097 (4)0.0000.0048 (4)0.000
Mo10.01247 (12)0.01077 (11)0.01030 (11)0.00017 (8)0.00327 (9)0.00066 (8)
Mo20.01642 (12)0.00973 (11)0.01031 (11)0.00097 (9)0.00486 (9)0.00107 (8)
Mo30.01332 (12)0.01225 (11)0.01191 (12)0.00303 (9)0.00383 (9)0.00129 (8)
Mo40.01399 (12)0.00961 (11)0.01051 (11)0.00084 (8)0.00575 (9)0.00102 (8)
Mo50.01486 (12)0.01301 (11)0.01261 (12)0.00004 (9)0.00713 (9)0.00125 (8)
Mo60.01353 (12)0.01025 (11)0.01242 (11)0.00187 (8)0.00614 (9)0.00060 (8)
Cu10.0200 (3)0.0089 (2)0.0169 (2)0.0000.0066 (2)0.000
Cu20.01852 (18)0.01345 (16)0.01318 (16)0.00004 (13)0.00387 (13)0.00072 (13)
O10.0171 (10)0.0143 (9)0.0153 (10)0.0011 (8)0.0036 (8)0.0002 (7)
O20.0217 (11)0.0130 (9)0.0145 (10)0.0015 (8)0.0056 (8)0.0014 (7)
O30.0182 (10)0.0177 (9)0.0144 (10)0.0036 (8)0.0052 (8)0.0009 (8)
O40.0232 (11)0.0155 (9)0.0178 (10)0.0005 (8)0.0102 (8)0.0045 (8)
O50.0220 (11)0.0202 (10)0.0188 (10)0.0000 (8)0.0114 (9)0.0022 (8)
O60.0196 (10)0.0154 (9)0.0176 (10)0.0034 (8)0.0083 (8)0.0027 (8)
O70.0165 (10)0.0144 (9)0.0101 (9)0.0006 (7)0.0036 (8)0.0002 (7)
O80.0145 (10)0.0133 (9)0.0128 (9)0.0004 (7)0.0054 (8)0.0027 (7)
O90.0129 (10)0.0136 (9)0.0157 (9)0.0003 (7)0.0074 (8)0.0010 (7)
O100.0171 (10)0.0122 (8)0.0114 (9)0.0005 (7)0.0078 (8)0.0002 (7)
O110.0174 (10)0.0105 (9)0.0142 (9)0.0016 (7)0.0060 (8)0.0004 (7)
O120.0164 (10)0.0137 (9)0.0134 (9)0.0000 (7)0.0028 (8)0.0015 (7)
O130.0171 (10)0.0145 (9)0.0133 (9)0.0006 (8)0.0057 (8)0.0013 (7)
O140.0177 (10)0.0137 (9)0.0131 (9)0.0008 (7)0.0078 (8)0.0007 (7)
O150.0173 (10)0.0121 (9)0.0142 (9)0.0015 (7)0.0072 (8)0.0015 (7)
O160.0171 (10)0.0105 (8)0.0138 (9)0.0003 (7)0.0064 (8)0.0010 (7)
O170.0142 (10)0.0143 (9)0.0146 (9)0.0019 (7)0.0069 (8)0.0007 (7)
O180.0146 (10)0.0146 (9)0.0151 (9)0.0013 (7)0.0053 (8)0.0027 (7)
O190.0138 (9)0.0104 (8)0.0106 (9)0.0008 (7)0.0043 (7)0.0006 (7)
O200.0127 (9)0.0102 (8)0.0123 (9)0.0008 (7)0.0058 (7)0.0001 (7)
O1W0.0399 (15)0.0494 (16)0.0176 (12)0.0300 (13)0.0074 (11)0.0031 (11)
N10.0249 (14)0.0123 (11)0.0285 (14)0.0023 (10)0.0143 (11)0.0020 (10)
N20.0212 (13)0.0166 (11)0.0146 (12)0.0005 (10)0.0081 (10)0.0022 (9)
N30.0194 (13)0.0143 (11)0.0187 (12)0.0002 (9)0.0069 (10)0.0000 (9)
N40.0196 (14)0.0200 (12)0.0159 (13)0.0012 (11)0.0037 (11)0.0019 (11)
N50.0192 (14)0.0190 (13)0.0140 (13)0.0029 (11)0.0040 (11)0.0011 (10)
C10.0265 (17)0.0188 (15)0.0282 (17)0.0024 (13)0.0117 (14)0.0057 (13)
C20.0266 (19)0.0324 (18)0.042 (2)0.0051 (15)0.0113 (16)0.0129 (16)
C30.036 (2)0.0216 (17)0.059 (2)0.0106 (15)0.0174 (18)0.0165 (16)
C40.034 (2)0.0128 (15)0.056 (2)0.0033 (14)0.0200 (18)0.0050 (15)
C50.0262 (17)0.0133 (13)0.0360 (18)0.0019 (12)0.0179 (14)0.0016 (12)
C60.0237 (16)0.0222 (15)0.0172 (15)0.0007 (12)0.0078 (12)0.0007 (12)
C70.0217 (17)0.0377 (18)0.0181 (15)0.0008 (14)0.0036 (13)0.0013 (14)
C80.0274 (18)0.0301 (17)0.0286 (17)0.0103 (15)0.0080 (14)0.0078 (14)
C90.0301 (18)0.0187 (15)0.0306 (18)0.0044 (13)0.0098 (14)0.0001 (13)
C100.0225 (16)0.0176 (13)0.0190 (15)0.0013 (12)0.0093 (12)0.0014 (11)
C110.0228 (16)0.0155 (13)0.0208 (15)0.0008 (11)0.0101 (12)0.0002 (11)
C120.0342 (19)0.0159 (15)0.0325 (18)0.0023 (14)0.0089 (15)0.0040 (13)
C130.0328 (19)0.0215 (16)0.0349 (19)0.0038 (14)0.0103 (15)0.0129 (14)
C140.0201 (16)0.0307 (17)0.0232 (17)0.0013 (13)0.0047 (13)0.0116 (13)
C150.0199 (15)0.0190 (14)0.0204 (15)0.0004 (12)0.0068 (12)0.0009 (12)
C160.0220 (16)0.0230 (15)0.0218 (15)0.0038 (13)0.0102 (13)0.0003 (13)
C170.0274 (17)0.0169 (14)0.0144 (14)0.0007 (12)0.0103 (13)0.0003 (11)
Geometric parameters (Å, º) top
P1—O201.5337 (17)Cu2—N41.995 (3)
P1—O20i1.5337 (17)Cu2—N22.005 (2)
P1—O191.5373 (17)Cu2—N32.006 (2)
P1—O19i1.5373 (17)Cu2—N52.025 (2)
Mo1—O11.6909 (19)Cu2—O1W2.343 (2)
Mo1—O91.8874 (17)Cu2—O42.7008 (19)
Mo1—O81.9142 (17)O9—Mo6i1.8692 (18)
Mo1—O101.9447 (17)O12—Mo3i1.9158 (18)
Mo1—O71.9751 (18)O16—Mo6i1.9962 (18)
Mo1—O192.4237 (17)O18—Mo3i1.9209 (18)
Mo1—Mo33.3874 (3)O1W—H2W0.93 (5)
Mo1—Mo23.4298 (3)O1W—H1W0.74 (4)
Mo2—O21.6891 (18)N1—C11.335 (4)
Mo2—O131.8927 (18)N1—C51.358 (4)
Mo2—O71.9073 (18)N2—C61.336 (4)
Mo2—O121.9089 (18)N2—C101.356 (3)
Mo2—O111.9167 (17)N3—C151.339 (4)
Mo2—O192.4229 (17)N3—C111.350 (3)
Mo2—Mo33.4090 (3)N4—C161.482 (4)
Mo3—O31.6800 (18)N4—H4A0.91 (3)
Mo3—O81.9140 (18)N4—H4B0.77 (3)
Mo3—O12i1.9158 (18)N5—C171.488 (4)
Mo3—O18i1.9209 (18)N5—H5A0.84 (3)
Mo3—O111.9309 (17)N5—H5B0.79 (3)
Mo3—O192.4350 (17)C1—C21.381 (4)
Mo4—O41.6934 (18)C1—H10.93 (3)
Mo4—O101.8427 (18)C2—C31.376 (5)
Mo4—O141.8803 (18)C2—H20.92 (4)
Mo4—O151.9353 (18)C3—C41.361 (5)
Mo4—O162.0049 (17)C3—H30.9300
Mo4—O202.4175 (17)C4—C51.399 (4)
Mo4—Cu13.2310 (4)C4—H40.92 (4)
Mo4—Mo53.4070 (3)C5—C5i1.456 (6)
Mo4—Mo63.4332 (3)C6—C71.372 (4)
Mo5—O51.6833 (18)C6—H60.92 (3)
Mo5—O181.8710 (18)C7—C81.382 (5)
Mo5—O171.9031 (18)C7—H70.898 (18)
Mo5—O131.9317 (18)C8—C91.381 (5)
Mo5—O141.9720 (18)C8—H80.91 (3)
Mo5—O202.4472 (17)C9—C101.382 (4)
Mo5—Mo63.3945 (3)C9—H90.904 (18)
Mo6—O61.6768 (18)C10—C111.476 (4)
Mo6—O9i1.8692 (18)C11—C121.385 (4)
Mo6—O171.9152 (17)C12—C131.372 (5)
Mo6—O151.9690 (18)C12—H120.86 (3)
Mo6—O16i1.9962 (18)C13—C141.381 (5)
Mo6—O202.4519 (17)C13—H130.89 (3)
Mo6—Cu13.2085 (4)C14—C151.384 (4)
Cu1—O161.9883 (18)C14—H140.93 (3)
Cu1—O16i1.9883 (18)C15—H150.91 (3)
Cu1—N1i2.003 (2)C16—C171.503 (4)
Cu1—N12.003 (2)C16—H16B0.93 (3)
Cu1—O152.3834 (18)C16—H16A0.94 (3)
Cu1—O15i2.3835 (18)C17—H17B0.99 (3)
Cu1—Mo6i3.2085 (4)C17—H17A1.00 (3)
Cu1—Mo4i3.2310 (4)
O20—P1—O20i110.70 (13)O20—Mo6—Mo546.08 (4)
O20—P1—O19109.96 (9)Cu1—Mo6—Mo5117.369 (9)
O20i—P1—O19108.31 (9)O6—Mo6—Mo4129.44 (7)
O20—P1—O19i108.31 (9)O9i—Mo6—Mo4127.70 (5)
O20i—P1—O19i109.96 (9)O17—Mo6—Mo476.84 (5)
O19—P1—O19i109.60 (14)O15—Mo6—Mo428.17 (5)
O1—Mo1—O9102.41 (8)O16i—Mo6—Mo481.84 (5)
O1—Mo1—O8103.56 (8)O20—Mo6—Mo444.76 (4)
O9—Mo1—O892.99 (7)Cu1—Mo6—Mo458.100 (6)
O1—Mo1—O10101.43 (8)Mo5—Mo6—Mo459.864 (7)
O9—Mo1—O1083.00 (7)O16—Cu1—O16i92.36 (10)
O8—Mo1—O10154.96 (8)O16—Cu1—N1i174.51 (9)
O1—Mo1—O7101.06 (8)O16i—Cu1—N1i93.11 (9)
O9—Mo1—O7155.84 (8)O16—Cu1—N193.11 (9)
O8—Mo1—O787.00 (7)O16i—Cu1—N1174.51 (9)
O10—Mo1—O786.86 (7)N1i—Cu1—N181.42 (14)
O1—Mo1—O19172.75 (7)O16—Cu1—O1571.55 (7)
O9—Mo1—O1984.54 (7)O16i—Cu1—O1572.52 (7)
O8—Mo1—O1973.70 (7)N1i—Cu1—O15110.61 (8)
O10—Mo1—O1981.31 (7)N1—Cu1—O15108.86 (8)
O7—Mo1—O1972.26 (6)O16—Cu1—O15i72.52 (7)
O1—Mo1—Mo3131.05 (6)O16i—Cu1—O15i71.55 (7)
O9—Mo1—Mo389.72 (5)N1i—Cu1—O15i108.86 (8)
O8—Mo1—Mo327.77 (5)N1—Cu1—O15i110.61 (8)
O10—Mo1—Mo3127.23 (5)O15—Cu1—O15i127.10 (8)
O7—Mo1—Mo379.09 (5)O16—Cu1—Mo6i36.45 (5)
O19—Mo1—Mo345.94 (4)O16i—Cu1—Mo6i88.34 (5)
O1—Mo1—Mo2128.21 (6)N1i—Cu1—Mo6i143.32 (7)
O9—Mo1—Mo2129.35 (6)N1—Cu1—Mo6i96.34 (7)
O8—Mo1—Mo278.07 (5)O15—Cu1—Mo6i104.77 (4)
O10—Mo1—Mo285.42 (5)O15i—Cu1—Mo6i37.72 (4)
O7—Mo1—Mo227.41 (5)O16—Cu1—Mo688.34 (5)
O19—Mo1—Mo244.95 (4)O16i—Cu1—Mo636.45 (5)
Mo3—Mo1—Mo260.006 (7)N1i—Cu1—Mo696.34 (7)
O2—Mo2—O13102.19 (8)N1—Cu1—Mo6143.32 (7)
O2—Mo2—O799.28 (8)O15—Cu1—Mo637.72 (4)
O13—Mo2—O788.83 (8)O15i—Cu1—Mo6104.77 (4)
O2—Mo2—O12103.12 (8)Mo6i—Cu1—Mo6105.998 (15)
O13—Mo2—O1286.76 (8)O16—Cu1—Mo436.16 (5)
O7—Mo2—O12157.60 (7)O16i—Cu1—Mo487.47 (5)
O2—Mo2—O11100.43 (8)N1i—Cu1—Mo4144.65 (7)
O13—Mo2—O11157.37 (7)N1—Cu1—Mo496.69 (7)
O7—Mo2—O1188.45 (8)O15—Cu1—Mo436.54 (4)
O12—Mo2—O1187.25 (8)O15i—Cu1—Mo4104.82 (4)
O2—Mo2—O19170.14 (8)Mo6i—Cu1—Mo472.023 (9)
O13—Mo2—O1984.45 (7)Mo6—Cu1—Mo464.435 (8)
O7—Mo2—O1973.34 (7)O16—Cu1—Mo4i87.47 (5)
O12—Mo2—O1984.37 (7)O16i—Cu1—Mo4i36.16 (5)
O11—Mo2—O1973.25 (6)N1i—Cu1—Mo4i96.69 (7)
O2—Mo2—Mo3127.53 (6)N1—Cu1—Mo4i144.65 (7)
O13—Mo2—Mo3130.01 (5)O15—Cu1—Mo4i104.82 (4)
O7—Mo2—Mo379.29 (5)O15i—Cu1—Mo4i36.54 (4)
O12—Mo2—Mo386.81 (6)Mo6i—Cu1—Mo4i64.435 (8)
O11—Mo2—Mo327.73 (5)Mo6—Cu1—Mo4i72.023 (9)
O19—Mo2—Mo345.58 (4)Mo4—Cu1—Mo4i104.107 (15)
O2—Mo2—Mo1127.14 (6)N4—Cu2—N2175.23 (10)
O13—Mo2—Mo188.39 (5)N4—Cu2—N394.52 (10)
O7—Mo2—Mo128.48 (5)N2—Cu2—N381.19 (9)
O12—Mo2—Mo1129.33 (5)N4—Cu2—N584.63 (10)
O11—Mo2—Mo178.67 (5)N2—Cu2—N599.54 (10)
O19—Mo2—Mo144.97 (4)N3—Cu2—N5176.79 (11)
Mo3—Mo2—Mo159.380 (7)N4—Cu2—O1W87.64 (11)
O3—Mo3—O8100.29 (8)N2—Cu2—O1W90.34 (9)
O3—Mo3—O12i102.87 (8)N3—Cu2—O1W90.86 (9)
O8—Mo3—O12i156.83 (8)N5—Cu2—O1W86.01 (11)
O3—Mo3—O18i103.27 (8)N4—Cu2—O4105.05 (9)
O8—Mo3—O18i89.20 (7)N2—Cu2—O477.29 (8)
O12i—Mo3—O18i85.76 (8)N3—Cu2—O491.80 (8)
O3—Mo3—O11100.32 (8)N5—Cu2—O491.41 (9)
O8—Mo3—O1187.45 (8)O1W—Cu2—O4166.78 (8)
O12i—Mo3—O1188.19 (8)Mo4—O4—Cu2115.04 (9)
O18i—Mo3—O11156.39 (7)Mo2—O7—Mo1124.11 (9)
O3—Mo3—O19170.58 (7)Mo3—O8—Mo1124.47 (10)
O8—Mo3—O1973.43 (7)Mo6i—O9—Mo1154.72 (10)
O12i—Mo3—O1983.55 (7)Mo4—O10—Mo1156.52 (10)
O18i—Mo3—O1983.91 (7)Mo2—O11—Mo3124.75 (9)
O11—Mo3—O1972.74 (6)Mo2—O12—Mo3i150.32 (10)
O3—Mo3—Mo1127.77 (6)Mo2—O13—Mo5150.52 (10)
O8—Mo3—Mo127.77 (5)Mo4—O14—Mo5124.34 (9)
O12i—Mo3—Mo1129.16 (5)Mo4—O15—Mo6123.12 (9)
O18i—Mo3—Mo186.57 (5)Mo4—O15—Cu196.30 (7)
O11—Mo3—Mo179.65 (5)Mo6—O15—Cu194.50 (7)
O19—Mo3—Mo145.66 (4)Cu1—O16—Mo6i107.27 (8)
O3—Mo3—Mo2127.34 (6)Cu1—O16—Mo4108.02 (8)
O8—Mo3—Mo278.63 (5)Mo6i—O16—Mo4142.27 (9)
O12i—Mo3—Mo287.11 (5)Mo5—O17—Mo6125.50 (9)
O18i—Mo3—Mo2129.18 (5)Mo5—O18—Mo3i151.76 (11)
O11—Mo3—Mo227.51 (5)P1—O19—Mo2124.98 (10)
O19—Mo3—Mo245.29 (4)P1—O19—Mo1125.86 (9)
Mo1—Mo3—Mo260.615 (6)Mo2—O19—Mo190.09 (6)
O4—Mo4—O10102.33 (9)P1—O19—Mo3126.64 (9)
O4—Mo4—O14100.98 (8)Mo2—O19—Mo389.14 (6)
O10—Mo4—O1492.87 (8)Mo1—O19—Mo388.40 (6)
O4—Mo4—O15100.67 (8)P1—O20—Mo4125.48 (10)
O10—Mo4—O15156.26 (7)P1—O20—Mo5126.30 (9)
O14—Mo4—O1588.42 (8)Mo4—O20—Mo588.91 (6)
O4—Mo4—O16102.40 (8)P1—O20—Mo6126.63 (9)
O10—Mo4—O1687.79 (7)Mo4—O20—Mo689.66 (5)
O14—Mo4—O16155.90 (8)Mo5—O20—Mo687.72 (6)
O15—Mo4—O1681.63 (8)Cu2—O1W—H2W114 (3)
O4—Mo4—O20172.98 (8)Cu2—O1W—H1W132 (3)
O10—Mo4—O2083.37 (7)H2W—O1W—H1W114 (4)
O14—Mo4—O2074.41 (7)C1—N1—C5119.1 (2)
O15—Mo4—O2074.15 (6)C1—N1—Cu1126.81 (19)
O16—Mo4—O2081.75 (7)C5—N1—Cu1114.0 (2)
O4—Mo4—Cu197.28 (6)C6—N2—C10118.5 (2)
O10—Mo4—Cu1123.28 (5)C6—N2—Cu2128.33 (19)
O14—Mo4—Cu1134.49 (6)C10—N2—Cu2113.06 (19)
O15—Mo4—Cu147.16 (5)C15—N3—C11119.3 (2)
O16—Mo4—Cu135.82 (5)C15—N3—Cu2127.12 (19)
O20—Mo4—Cu182.74 (4)C11—N3—Cu2112.01 (18)
O4—Mo4—Mo5129.17 (6)C16—N4—Cu2108.92 (18)
O10—Mo4—Mo590.22 (5)C16—N4—H4A109 (2)
O14—Mo4—Mo528.55 (5)Cu2—N4—H4A111 (2)
O15—Mo4—Mo579.69 (5)C16—N4—H4B108 (2)
O16—Mo4—Mo5127.42 (5)Cu2—N4—H4B110 (2)
O20—Mo4—Mo545.90 (4)H4A—N4—H4B110 (3)
Cu1—Mo4—Mo5116.385 (8)C17—N5—Cu2109.52 (18)
O4—Mo4—Mo6128.89 (7)C17—N5—H5A110 (2)
O10—Mo4—Mo6128.78 (5)Cu2—N5—H5A113 (2)
O14—Mo4—Mo678.90 (6)C17—N5—H5B112 (2)
O15—Mo4—Mo628.71 (5)Cu2—N5—H5B114 (2)
O16—Mo4—Mo681.95 (5)H5A—N5—H5B99 (3)
O20—Mo4—Mo645.58 (4)N1—C1—C2122.2 (3)
Cu1—Mo4—Mo657.464 (6)N1—C1—H1114 (2)
Mo5—Mo4—Mo659.504 (7)C2—C1—H1123 (2)
O5—Mo5—O18103.85 (9)C3—C2—C1118.9 (3)
O5—Mo5—O17101.94 (8)C3—C2—H2118 (2)
O18—Mo5—O1792.74 (8)C1—C2—H2123 (2)
O5—Mo5—O13102.07 (8)C4—C3—C2119.7 (3)
O18—Mo5—O1386.27 (8)C4—C3—H3120.1
O17—Mo5—O13155.48 (7)C2—C3—H3120.1
O5—Mo5—O1499.48 (8)C3—C4—C5119.5 (3)
O18—Mo5—O14156.42 (7)C3—C4—H4123 (2)
O17—Mo5—O1485.68 (7)C5—C4—H4117 (2)
O13—Mo5—O1485.59 (7)N1—C5—C4120.5 (3)
O5—Mo5—O20170.65 (8)N1—C5—C5i115.22 (17)
O18—Mo5—O2084.72 (7)C4—C5—C5i124.3 (2)
O17—Mo5—O2073.53 (7)N2—C6—C7123.3 (3)
O13—Mo5—O2081.99 (7)N2—C6—H6117 (2)
O14—Mo5—O2072.26 (6)C7—C6—H6120 (2)
O5—Mo5—Mo6129.03 (7)C6—C7—C8118.3 (3)
O18—Mo5—Mo688.91 (5)C6—C7—H7122 (2)
O17—Mo5—Mo627.35 (5)C8—C7—H7120 (2)
O13—Mo5—Mo6128.18 (5)C9—C8—C7119.4 (3)
O14—Mo5—Mo678.91 (5)C9—C8—H8123 (2)
O20—Mo5—Mo646.20 (4)C7—C8—H8118 (2)
O5—Mo5—Mo4126.32 (7)C8—C9—C10119.3 (3)
O18—Mo5—Mo4129.82 (5)C8—C9—H9121 (2)
O17—Mo5—Mo477.67 (5)C10—C9—H9120 (2)
O13—Mo5—Mo484.19 (5)N2—C10—C9121.2 (3)
O14—Mo5—Mo427.11 (5)N2—C10—C11114.4 (2)
O20—Mo5—Mo445.19 (4)C9—C10—C11124.2 (3)
Mo6—Mo5—Mo460.632 (7)N3—C11—C12120.6 (3)
O6—Mo6—O9i102.86 (9)N3—C11—C10114.9 (2)
O6—Mo6—O17104.58 (8)C12—C11—C10124.5 (3)
O9i—Mo6—O1791.40 (7)C13—C12—C11119.9 (3)
O6—Mo6—O15101.53 (8)C13—C12—H12119 (2)
O9i—Mo6—O15155.30 (7)C11—C12—H12121 (2)
O17—Mo6—O1586.23 (8)C12—C13—C14119.3 (3)
O6—Mo6—O16i100.94 (8)C12—C13—H13118 (2)
O9i—Mo6—O16i89.42 (7)C14—C13—H13123 (2)
O17—Mo6—O16i153.60 (7)C13—C14—C15118.3 (3)
O15—Mo6—O16i82.15 (7)C13—C14—H14125.6 (18)
O6—Mo6—O20173.92 (8)C15—C14—H14115.8 (19)
O9i—Mo6—O2082.96 (7)N3—C15—C14122.4 (3)
O17—Mo6—O2073.23 (7)N3—C15—H15119.4 (18)
O15—Mo6—O2072.81 (6)C14—C15—H15118.2 (18)
O16i—Mo6—O2080.69 (7)N4—C16—C17108.3 (2)
O6—Mo6—Cu195.13 (6)N4—C16—H16B105.1 (18)
O9i—Mo6—Cu1125.42 (5)C17—C16—H16B112.9 (19)
O17—Mo6—Cu1133.02 (5)N4—C16—H16A112.1 (17)
O15—Mo6—Cu147.78 (5)C17—C16—H16A110.4 (17)
O16i—Mo6—Cu136.28 (5)H16B—C16—H16A108 (3)
O20—Mo6—Cu182.71 (4)N5—C17—C16108.5 (2)
O6—Mo6—Mo5131.63 (6)N5—C17—H17B111.7 (17)
O9i—Mo6—Mo587.09 (5)C16—C17—H17B108.3 (17)
O17—Mo6—Mo527.16 (5)N5—C17—H17A106.6 (17)
O15—Mo6—Mo579.63 (5)C16—C17—H17A108.8 (17)
O16i—Mo6—Mo5126.69 (5)H17B—C17—H17A113 (2)
Symmetry code: (i) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N4—H4B···O3ii0.77 (3)2.58 (3)3.059 (3)122 (3)
N4—H4B···O8ii0.77 (3)2.50 (4)3.262 (3)171 (3)
N4—H4A···O140.91 (3)2.43 (3)3.102 (3)131 (3)
N4—H4A···O170.91 (3)2.57 (4)3.445 (3)161 (3)
N5—H5A···O7iii0.84 (3)2.26 (4)3.070 (3)162 (3)
O1W—H1W···O1ii0.74 (4)2.02 (5)2.747 (3)171 (5)
O1W—H2W···O7iii0.93 (5)1.89 (5)2.800 (3)166 (4)
Symmetry codes: (ii) x+1/2, y+1/2, z; (iii) x+1, y, z.
 

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