The 3,4-connected layered hybrid oxide poly[tetra­kis(μ-2,4′-bipyridine-κ2N:N′)(μ4-β-octa­molybdato-κ4O:O′:O′′:O′′′)tetra­copper(I)]

Ochalek, C.E.; LaDuca, R.L.

doi:10.1107/S1600536807003583

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The 3,4-connected layered hybrid oxide poly[tetrakis(μ-2,4′-bipyridine-κ²N:N′)(μ₄-β-octamolybdato-κ⁴O:O′:O′′:O′′′)tetracopper(I)]

The title compound, [Cu₄(β-Mo₈O₂₆)(C₁₀H₈N₂)₄]_n, is a two-dimensional 3,4-connected network coordination polymer containing two crystallographically distinct T-coordinated Cu^I atoms, each of which is bound to two N atoms from two bridging 2,4′-bipyridine ligands and a terminal O atom belonging to a centrosymmetric β-octamolybdate anion. Rippled cationic [Cu(2,4′-bpy)]_nⁿ⁺ chain motifs are linked into `brick-wall' two-dimensional layers by exo-tetradentate β-octamolybdate anions. The layers stack via C—H

O interactions to form a three-dimensional structure.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807003583/ng2210sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536807003583/ng2210Isup2.hkl Contains datablock I

CCDC reference: 636767

checkCIF report

Key indicators

Single-crystal X-ray study
T = 173 K
Mean (C-C) = 0.005 Å
R factor = 0.023
wR factor = 0.059
Data-to-parameter ratio = 15.3

checkCIF/PLATON results

No syntax errors found



Alert level A
DIFF020_ALERT_1_A  _diffrn_standards_interval_count and
            _diffrn_standards_interval_time are missing. Number of measurements
            between standards or time (min) between standards.

Author Response: CCD detector used


Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       2.00 Ratio
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000)         300 Deg.
PLAT747_ALERT_1_C D...A   Calc    3.073(4), Rep     3.07000 ......    Missing su
              C4   -O5      1.555   1.445
PLAT747_ALERT_1_C D...A   Calc    3.030(4), Rep     3.03000 ......    Missing su
              C7   -O1      1.555   2.667
PLAT747_ALERT_1_C D...A   Calc    3.252(4), Rep     3.25000 ......    Missing su
              C10  -O4      1.555   2.666
PLAT747_ALERT_1_C D...A   Calc    3.462(4), Rep     3.46000 ......    Missing su
              C12  -O9      1.555   2.656
PLAT747_ALERT_1_C D...A   Calc    3.116(4), Rep     3.12000 ......    Missing su
              C14  -O10     1.555   2.766
PLAT747_ALERT_1_C D...A   Calc    3.016(4), Rep     3.02000 ......    Missing su
              C16  -O3      1.555   2.656

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

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

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: CrystalMaker (Palmer, 2005); software used to prepare material for publication: SHELXL97.

poly[tetrakis(µ-2,4'-bipyridine-κ²N:N')(µ₄-β-octamolybdato- κ⁴-O:O':O'':O''')tetracopper(I)] top

Crystal data top

[Cu₄Mo₈O₂₆(C₁₀H₈N₂)₄]	Z = 1
M_r = 2062.46	F(000) = 988
Triclinic, P1	D_x = 2.682 Mg m⁻³
a = 10.631 (2) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.948 (2) Å	Cell parameters from 15119 reflections
c = 12.701 (3) Å	θ = 1.8–28.3°
α = 99.427 (3)°	µ = 3.62 mm⁻¹
β = 114.082 (3)°	T = 173 K
γ = 100.871 (3)°	Block, orange
V = 1276.7 (5) Å³	0.40 × 0.20 × 0.16 mm

Data collection top

Bruker SMART 1K diffractometer	5945 independent reflections
Radiation source: fine-focus sealed tube	5371 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.020
ω scans	θ_max = 28.3°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −14→14
T_min = 0.412, T_max = 0.560	k = −14→14
15119 measured reflections	l = −16→16

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.023	H-atom parameters constrained
wR(F²) = 0.059	w = 1/[σ²(F_o²) + (0.026P)² + 2.0526P] where P = (F_o² + 2F_c²)/3
S = 1.09	(Δ/σ)_max = 0.001
5945 reflections	Δρ_max = 1.61 e Å⁻³
389 parameters	Δρ_min = −0.86 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00123 (13)

Special details top

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

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Cu1	0.92753 (4)	0.15492 (4)	0.54966 (3)	0.02286 (9)
Cu2	0.44983 (4)	0.64784 (4)	0.55367 (4)	0.02306 (9)
Mo1	0.82417 (2)	0.49216 (2)	0.98953 (2)	0.01207 (6)
Mo2	0.82994 (3)	0.69789 (2)	0.80942 (2)	0.01429 (6)
Mo3	0.88800 (2)	0.22326 (2)	0.92594 (2)	0.01346 (6)
Mo4	0.91292 (2)	0.43053 (2)	0.74899 (2)	0.01305 (6)
O1	0.7082 (2)	0.4166 (2)	1.03470 (19)	0.0198 (4)
O2	0.9983 (2)	0.58343 (18)	0.92660 (17)	0.0135 (4)
O3	0.7964 (2)	0.35321 (19)	0.85871 (17)	0.0137 (4)
O4	0.7724 (2)	0.52242 (19)	0.71177 (17)	0.0154 (4)
O5	0.9288 (2)	0.7630 (2)	0.7448 (2)	0.0242 (5)
O6	0.9389 (2)	0.80487 (19)	0.96915 (18)	0.0177 (4)
O7	0.7305 (2)	0.58341 (19)	0.90242 (17)	0.0155 (4)
O8	0.6773 (2)	0.7463 (2)	0.75378 (19)	0.0216 (5)
O9	0.7710 (2)	0.1627 (2)	0.97684 (19)	0.0210 (4)
O10	1.0293 (2)	0.5091 (2)	0.70574 (19)	0.0222 (5)
O11	0.8213 (2)	0.2887 (2)	0.63790 (18)	0.0204 (4)
O12	1.0465 (2)	0.36520 (19)	0.87257 (17)	0.0146 (4)
O13	0.8385 (2)	0.1130 (2)	0.79525 (19)	0.0211 (4)
N1	0.0852 (3)	0.1425 (2)	0.6878 (2)	0.0174 (5)
N2	0.7862 (2)	0.1423 (2)	0.3920 (2)	0.0156 (5)
N3	0.3618 (3)	0.5250 (2)	0.6102 (2)	0.0197 (5)
N4	0.5271 (3)	−0.2306 (2)	0.4895 (2)	0.0174 (5)
C1	0.2139 (3)	0.2337 (3)	0.7557 (3)	0.0158 (6)
C2	0.3021 (3)	0.2302 (3)	0.8704 (3)	0.0201 (6)
H2	0.3903	0.2924	0.9156	0.024*
C3	0.2599 (3)	0.1350 (3)	0.9178 (3)	0.0221 (6)
H3	0.3162	0.1356	0.9965	0.027*
C4	0.1325 (3)	0.0387 (3)	0.8468 (3)	0.0215 (6)
H4	0.1038	−0.0292	0.8750	0.026*
C5	0.0495 (3)	0.0459 (3)	0.7333 (3)	0.0206 (6)
H5	−0.0358	−0.0192	0.6852	0.025*
C6	0.4125 (3)	0.5402 (3)	0.7288 (3)	0.0205 (6)
H6	0.4837	0.6155	0.7802	0.025*
C7	0.3649 (3)	0.4508 (3)	0.7779 (3)	0.0187 (6)
H7	0.4028	0.4668	0.8607	0.022*
C8	0.2587 (3)	0.3350 (3)	0.7035 (3)	0.0156 (5)
C9	0.2053 (3)	0.3197 (3)	0.5802 (3)	0.0183 (6)
H9	0.1348	0.2448	0.5267	0.022*
C10	0.2572 (3)	0.4153 (3)	0.5377 (3)	0.0207 (6)
H10	0.2183	0.4037	0.4554	0.025*
C11	0.6556 (3)	0.0529 (3)	0.3289 (3)	0.0155 (5)
C12	0.5644 (3)	0.0510 (3)	0.2128 (3)	0.0214 (6)
H12	0.4737	−0.0081	0.1721	0.026*
C13	0.6090 (3)	0.1375 (3)	0.1576 (3)	0.0232 (7)
H13	0.5510	0.1335	0.0783	0.028*
C14	0.7404 (3)	0.2291 (3)	0.2222 (3)	0.0212 (6)
H14	0.7717	0.2893	0.1879	0.025*
C15	0.8246 (3)	0.2301 (3)	0.3388 (3)	0.0190 (6)
H15	0.9117	0.2940	0.3829	0.023*
C16	0.4813 (3)	−0.2554 (3)	0.3702 (3)	0.0170 (6)
H16	0.4199	−0.3364	0.3221	0.020*
C17	0.5210 (3)	−0.1666 (3)	0.3166 (3)	0.0176 (6)
H17	0.4865	−0.1880	0.2339	0.021*
C18	0.6136 (3)	−0.0437 (3)	0.3866 (3)	0.0151 (5)
C19	0.6602 (3)	−0.0182 (3)	0.5101 (3)	0.0168 (6)
H19	0.7206	0.0624	0.5601	0.020*
C20	0.6168 (3)	−0.1124 (3)	0.5580 (3)	0.0181 (6)
H20	0.6505	−0.0939	0.6405	0.022*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.01678 (18)	0.0241 (2)	0.01801 (19)	−0.00234 (15)	0.00133 (15)	0.00818 (16)
Cu2	0.02266 (19)	0.01944 (19)	0.0292 (2)	0.00161 (15)	0.01384 (17)	0.01121 (16)
Mo1	0.00955 (11)	0.01353 (12)	0.01002 (11)	0.00113 (9)	0.00287 (9)	0.00193 (9)
Mo2	0.01283 (11)	0.01307 (12)	0.01159 (12)	−0.00015 (9)	0.00239 (9)	0.00252 (9)
Mo3	0.01235 (11)	0.01125 (12)	0.01076 (12)	−0.00003 (9)	0.00158 (9)	0.00143 (9)
Mo4	0.01278 (11)	0.01352 (12)	0.00906 (11)	0.00109 (9)	0.00302 (9)	0.00162 (9)
O1	0.0188 (10)	0.0225 (11)	0.0191 (10)	0.0037 (8)	0.0101 (9)	0.0069 (9)
O2	0.0120 (9)	0.0128 (9)	0.0110 (9)	0.0006 (7)	0.0031 (7)	0.0004 (7)
O3	0.0117 (9)	0.0144 (9)	0.0094 (9)	0.0002 (7)	0.0019 (7)	0.0012 (7)
O4	0.0130 (9)	0.0163 (10)	0.0107 (9)	0.0017 (8)	0.0008 (8)	0.0029 (8)
O5	0.0258 (11)	0.0192 (11)	0.0217 (11)	−0.0036 (9)	0.0106 (9)	0.0023 (9)
O6	0.0161 (10)	0.0143 (10)	0.0152 (10)	0.0032 (8)	0.0015 (8)	0.0015 (8)
O7	0.0126 (9)	0.0182 (10)	0.0148 (10)	0.0035 (8)	0.0051 (8)	0.0057 (8)
O8	0.0190 (10)	0.0195 (11)	0.0192 (11)	0.0033 (8)	0.0025 (9)	0.0067 (9)
O9	0.0193 (10)	0.0207 (11)	0.0191 (11)	0.0011 (8)	0.0065 (9)	0.0070 (9)
O10	0.0197 (10)	0.0258 (12)	0.0204 (11)	0.0015 (9)	0.0100 (9)	0.0072 (9)
O11	0.0221 (11)	0.0196 (11)	0.0132 (10)	0.0028 (9)	0.0047 (9)	0.0012 (8)
O12	0.0138 (9)	0.0136 (9)	0.0123 (9)	0.0031 (7)	0.0033 (8)	0.0013 (8)
O13	0.0227 (11)	0.0155 (10)	0.0156 (10)	0.0022 (8)	0.0030 (9)	−0.0008 (8)
N1	0.0155 (11)	0.0167 (12)	0.0165 (12)	0.0019 (10)	0.0047 (10)	0.0052 (10)
N2	0.0136 (11)	0.0161 (12)	0.0134 (11)	0.0010 (9)	0.0044 (9)	0.0033 (9)
N3	0.0173 (12)	0.0199 (13)	0.0224 (13)	0.0037 (10)	0.0087 (10)	0.0095 (11)
N4	0.0120 (11)	0.0166 (12)	0.0193 (12)	0.0006 (9)	0.0044 (10)	0.0053 (10)
C1	0.0149 (13)	0.0169 (14)	0.0161 (14)	0.0042 (11)	0.0080 (11)	0.0040 (11)
C2	0.0156 (14)	0.0229 (15)	0.0178 (14)	0.0023 (12)	0.0050 (12)	0.0060 (12)
C3	0.0195 (14)	0.0291 (17)	0.0170 (14)	0.0076 (13)	0.0057 (12)	0.0103 (13)
C4	0.0226 (15)	0.0202 (15)	0.0260 (16)	0.0072 (12)	0.0122 (13)	0.0125 (13)
C5	0.0193 (14)	0.0183 (15)	0.0209 (15)	0.0020 (12)	0.0074 (12)	0.0051 (12)
C6	0.0165 (14)	0.0174 (14)	0.0236 (15)	0.0015 (11)	0.0079 (12)	0.0023 (12)
C7	0.0166 (13)	0.0203 (15)	0.0148 (14)	0.0015 (11)	0.0057 (11)	0.0019 (12)
C8	0.0145 (13)	0.0172 (14)	0.0160 (14)	0.0054 (11)	0.0068 (11)	0.0063 (11)
C9	0.0153 (13)	0.0196 (15)	0.0139 (14)	0.0000 (11)	0.0035 (11)	0.0030 (11)
C10	0.0201 (14)	0.0224 (15)	0.0160 (14)	0.0019 (12)	0.0062 (12)	0.0058 (12)
C11	0.0129 (13)	0.0164 (14)	0.0153 (13)	0.0023 (11)	0.0061 (11)	0.0020 (11)
C12	0.0150 (13)	0.0243 (16)	0.0189 (15)	0.0011 (12)	0.0033 (12)	0.0078 (13)
C13	0.0190 (14)	0.0299 (17)	0.0174 (15)	0.0055 (13)	0.0035 (12)	0.0123 (13)
C14	0.0206 (15)	0.0225 (15)	0.0214 (15)	0.0041 (12)	0.0094 (12)	0.0109 (13)
C15	0.0165 (13)	0.0168 (14)	0.0205 (15)	−0.0003 (11)	0.0076 (12)	0.0048 (12)
C16	0.0102 (12)	0.0161 (14)	0.0173 (14)	−0.0009 (10)	0.0022 (11)	0.0020 (11)
C17	0.0130 (13)	0.0197 (14)	0.0145 (13)	0.0009 (11)	0.0034 (11)	0.0020 (11)
C18	0.0095 (12)	0.0167 (14)	0.0165 (13)	0.0017 (10)	0.0048 (11)	0.0034 (11)
C19	0.0137 (13)	0.0157 (14)	0.0156 (14)	−0.0011 (11)	0.0041 (11)	0.0037 (11)
C20	0.0164 (13)	0.0190 (14)	0.0157 (14)	0.0013 (11)	0.0056 (11)	0.0055 (12)

Geometric parameters (Å, º) top

Cu1—N2	1.913 (2)	N4—C16	1.349 (4)
Cu1—N1ⁱ	1.916 (2)	N4—C20	1.353 (4)
Cu1—O11	2.408 (2)	C1—C2	1.386 (4)
Cu2—N3	1.895 (3)	C1—C8	1.482 (4)
Cu2—N4ⁱⁱ	1.897 (3)	C2—C3	1.378 (4)
Cu2—O8	2.564 (2)	C2—H2	0.9300
Mo1—O1	1.697 (2)	C3—C4	1.383 (4)
Mo1—O7	1.747 (2)	C3—H3	0.9300
Mo1—O12ⁱⁱⁱ	1.930 (2)	C4—C5	1.374 (4)
Mo1—O3	1.940 (2)	C4—H4	0.9300
Mo1—O2ⁱⁱⁱ	2.149 (2)	C5—H5	0.9300
Mo1—O2	2.416 (2)	C6—C7	1.369 (4)
Mo2—O5	1.703 (2)	C6—H6	0.9300
Mo2—O8	1.710 (2)	C7—C8	1.404 (4)
Mo2—O6	1.903 (2)	C7—H7	0.9300
Mo2—O4	1.939 (2)	C8—C9	1.399 (4)
Mo2—O7	2.256 (2)	C9—C10	1.378 (4)
Mo2—O2	2.504 (2)	C9—H9	0.9300
Mo3—O13	1.697 (2)	C10—H10	0.9300
Mo3—O9	1.700 (2)	C11—C12	1.389 (4)
Mo3—O6ⁱⁱⁱ	1.898 (2)	C11—C18	1.482 (4)
Mo3—O3	1.986 (2)	C12—C13	1.390 (4)
Mo3—O2ⁱⁱⁱ	2.310 (2)	C12—H12	0.9300
Mo3—O12	2.450 (2)	C13—C14	1.378 (4)
Mo4—O10	1.697 (2)	C13—H13	0.9300
Mo4—O11	1.715 (2)	C14—C15	1.379 (4)
Mo4—O4	1.901 (2)	C14—H14	0.9300
Mo4—O12	1.981 (2)	C15—H15	0.9300
Mo4—O2	2.288 (2)	C16—C17	1.372 (4)
Mo4—O3	2.365 (2)	C16—H16	0.9300
N1—C5	1.350 (4)	C17—C18	1.401 (4)
N1—C1	1.361 (4)	C17—H17	0.9300
N2—C15	1.355 (4)	C18—C19	1.399 (4)
N2—C11	1.361 (4)	C19—C20	1.378 (4)
N3—C6	1.345 (4)	C19—H19	0.9300
N3—C10	1.351 (4)	C20—H20	0.9300

N2—Cu1—N1ⁱ	166.67 (11)	Mo3ⁱⁱⁱ—O6—Mo2	120.41 (11)
N2—Cu1—O11	91.17 (9)	Mo1—O7—Mo2	119.82 (10)
N1ⁱ—Cu1—O11	102.16 (9)	Mo2—O8—Cu2	129.30 (11)
N3—Cu2—N4ⁱⁱ	176.59 (11)	Mo4—O11—Cu1	125.50 (11)
N3—Cu2—O8	94.60 (9)	Mo1ⁱⁱⁱ—O12—Mo4	109.24 (9)
N4ⁱⁱ—Cu2—O8	88.62 (9)	Mo1ⁱⁱⁱ—O12—Mo3	109.26 (9)
O1—Mo1—O7	104.13 (10)	Mo4—O12—Mo3	103.53 (8)
O1—Mo1—O12ⁱⁱⁱ	103.31 (10)	C5—N1—C1	118.1 (3)
O7—Mo1—O12ⁱⁱⁱ	96.53 (9)	C5—N1—Cu1^iv	113.7 (2)
O1—Mo1—O3	100.14 (10)	C1—N1—Cu1^iv	126.6 (2)
O7—Mo1—O3	97.28 (9)	C15—N2—C11	118.2 (2)
O12ⁱⁱⁱ—Mo1—O3	148.88 (8)	C15—N2—Cu1	115.35 (19)
O1—Mo1—O2ⁱⁱⁱ	99.67 (9)	C11—N2—Cu1	126.5 (2)
O7—Mo1—O2ⁱⁱⁱ	156.20 (8)	C6—N3—C10	116.9 (3)
O12ⁱⁱⁱ—Mo1—O2ⁱⁱⁱ	78.25 (8)	C6—N3—Cu2	119.3 (2)
O3—Mo1—O2ⁱⁱⁱ	77.88 (8)	C10—N3—Cu2	123.5 (2)
O1—Mo1—O2	174.83 (9)	C16—N4—C20	117.5 (3)
O7—Mo1—O2	80.44 (8)	C16—N4—Cu2^v	119.9 (2)
O12ⁱⁱⁱ—Mo1—O2	78.32 (8)	C20—N4—Cu2^v	122.2 (2)
O3—Mo1—O2	76.68 (7)	N1—C1—C2	120.5 (3)
O2ⁱⁱⁱ—Mo1—O2	75.76 (8)	N1—C1—C8	118.6 (3)
O5—Mo2—O8	104.36 (11)	C2—C1—C8	120.9 (3)
O5—Mo2—O6	99.98 (10)	C3—C2—C1	120.4 (3)
O8—Mo2—O6	104.48 (10)	C3—C2—H2	119.8
O5—Mo2—O4	95.52 (10)	C1—C2—H2	119.8
O8—Mo2—O4	103.74 (9)	C2—C3—C4	119.0 (3)
O6—Mo2—O4	143.10 (8)	C2—C3—H3	120.5
O5—Mo2—O7	167.53 (10)	C4—C3—H3	120.5
O8—Mo2—O7	87.49 (9)	C5—C4—C3	118.2 (3)
O6—Mo2—O7	80.38 (8)	C5—C4—H4	120.9
O4—Mo2—O7	77.61 (8)	C3—C4—H4	120.9
O5—Mo2—O2	98.17 (9)	N1—C5—C4	123.5 (3)
O8—Mo2—O2	157.44 (9)	N1—C5—H5	118.2
O6—Mo2—O2	72.29 (8)	C4—C5—H5	118.2
O4—Mo2—O2	72.49 (7)	N3—C6—C7	123.6 (3)
O7—Mo2—O2	69.95 (7)	N3—C6—H6	118.2
O13—Mo3—O9	104.51 (11)	C7—C6—H6	118.2
O13—Mo3—O6ⁱⁱⁱ	102.70 (10)	C6—C7—C8	120.0 (3)
O9—Mo3—O6ⁱⁱⁱ	102.48 (10)	C6—C7—H7	120.0
O13—Mo3—O3	98.40 (9)	C8—C7—H7	120.0
O9—Mo3—O3	98.37 (9)	C9—C8—C7	116.3 (3)
O6ⁱⁱⁱ—Mo3—O3	145.35 (8)	C9—C8—C1	123.2 (3)
O13—Mo3—O2ⁱⁱⁱ	158.49 (9)	C7—C8—C1	120.4 (3)
O9—Mo3—O2ⁱⁱⁱ	96.39 (9)	C10—C9—C8	120.1 (3)
O6ⁱⁱⁱ—Mo3—O2ⁱⁱⁱ	77.18 (8)	C10—C9—H9	120.0
O3—Mo3—O2ⁱⁱⁱ	73.23 (8)	C8—C9—H9	120.0
O13—Mo3—O12	87.46 (9)	N3—C10—C9	123.1 (3)
O9—Mo3—O12	164.60 (9)	N3—C10—H10	118.5
O6ⁱⁱⁱ—Mo3—O12	83.87 (8)	C9—C10—H10	118.5
O3—Mo3—O12	69.86 (7)	N2—C11—C12	120.9 (3)
O2ⁱⁱⁱ—Mo3—O12	71.10 (7)	N2—C11—C18	118.3 (2)
O10—Mo4—O11	103.78 (11)	C12—C11—C18	120.7 (3)
O10—Mo4—O4	101.69 (10)	C11—C12—C13	119.9 (3)
O11—Mo4—O4	101.11 (9)	C11—C12—H12	120.0
O10—Mo4—O12	99.31 (10)	C13—C12—H12	120.0
O11—Mo4—O12	98.94 (9)	C14—C13—C12	118.9 (3)
O4—Mo4—O12	146.43 (8)	C14—C13—H13	120.5
O10—Mo4—O2	94.67 (9)	C12—C13—H13	120.5
O11—Mo4—O2	161.16 (9)	C13—C14—C15	118.8 (3)
O4—Mo4—O2	78.47 (8)	C13—C14—H14	120.6
O12—Mo4—O2	73.96 (8)	C15—C14—H14	120.6
O10—Mo4—O3	165.25 (9)	N2—C15—C14	123.1 (3)
O11—Mo4—O3	89.49 (9)	N2—C15—H15	118.5
O4—Mo4—O3	81.66 (8)	C14—C15—H15	118.5
O12—Mo4—O3	71.85 (8)	N4—C16—C17	123.0 (3)
O2—Mo4—O3	71.76 (7)	N4—C16—H16	118.5
Mo1ⁱⁱⁱ—O2—Mo4	91.84 (7)	C17—C16—H16	118.5
Mo1ⁱⁱⁱ—O2—Mo3ⁱⁱⁱ	91.42 (7)	C16—C17—C18	119.9 (3)
Mo4—O2—Mo3ⁱⁱⁱ	161.75 (10)	C16—C17—H17	120.0
Mo1ⁱⁱⁱ—O2—Mo1	104.24 (8)	C18—C17—H17	120.0
Mo4—O2—Mo1	97.94 (7)	C19—C18—C17	116.8 (3)
Mo3ⁱⁱⁱ—O2—Mo1	98.65 (7)	C19—C18—C11	123.1 (3)
Mo1ⁱⁱⁱ—O2—Mo2	165.98 (10)	C17—C18—C11	120.1 (3)
Mo4—O2—Mo2	86.10 (6)	C20—C19—C18	120.1 (3)
Mo3ⁱⁱⁱ—O2—Mo2	86.40 (7)	C20—C19—H19	119.9
Mo1—O2—Mo2	89.78 (6)	C18—C19—H19	119.9
Mo1—O3—Mo3	108.88 (9)	N4—C20—C19	122.6 (3)
Mo1—O3—Mo4	110.68 (9)	N4—C20—H20	118.7
Mo3—O3—Mo4	106.49 (8)	C19—C20—H20	118.7
Mo4—O4—Mo2	117.04 (10)

O10—Mo4—O2—Mo1ⁱⁱⁱ	−80.59 (10)	O2—Mo2—O6—Mo3ⁱⁱⁱ	17.38 (10)
O11—Mo4—O2—Mo1ⁱⁱⁱ	87.8 (3)	O1—Mo1—O7—Mo2	−176.80 (11)
O4—Mo4—O2—Mo1ⁱⁱⁱ	178.41 (9)	O12ⁱⁱⁱ—Mo1—O7—Mo2	77.67 (12)
O12—Mo4—O2—Mo1ⁱⁱⁱ	17.77 (7)	O3—Mo1—O7—Mo2	−74.37 (12)
O3—Mo4—O2—Mo1ⁱⁱⁱ	93.50 (8)	O2ⁱⁱⁱ—Mo1—O7—Mo2	2.1 (3)
O10—Mo4—O2—Mo3ⁱⁱⁱ	19.6 (3)	O2—Mo1—O7—Mo2	0.73 (10)
O11—Mo4—O2—Mo3ⁱⁱⁱ	−172.0 (3)	O5—Mo2—O7—Mo1	17.5 (5)
O4—Mo4—O2—Mo3ⁱⁱⁱ	−81.4 (3)	O8—Mo2—O7—Mo1	179.57 (13)
O12—Mo4—O2—Mo3ⁱⁱⁱ	117.9 (3)	O6—Mo2—O7—Mo1	−75.28 (12)
O3—Mo4—O2—Mo3ⁱⁱⁱ	−166.3 (3)	O4—Mo2—O7—Mo1	74.92 (12)
Mo1ⁱⁱⁱ—Mo4—O2—Mo3ⁱⁱⁱ	100.2 (3)	O2—Mo2—O7—Mo1	−0.74 (10)
O10—Mo4—O2—Mo1	174.76 (9)	O5—Mo2—O8—Cu2	82.41 (15)
O11—Mo4—O2—Mo1	−16.9 (3)	O6—Mo2—O8—Cu2	−173.06 (12)
O4—Mo4—O2—Mo1	73.76 (8)	O4—Mo2—O8—Cu2	−17.07 (16)
O12—Mo4—O2—Mo1	−86.88 (8)	O7—Mo2—O8—Cu2	−93.66 (14)
O3—Mo4—O2—Mo1	−11.15 (6)	O2—Mo2—O8—Cu2	−94.4 (2)
Mo1ⁱⁱⁱ—Mo4—O2—Mo1	−104.65 (9)	N3—Cu2—O8—Mo2	85.51 (16)
O10—Mo4—O2—Mo2	85.53 (9)	N4ⁱⁱ—Cu2—O8—Mo2	−95.62 (16)
O11—Mo4—O2—Mo2	−106.1 (3)	O10—Mo4—O11—Cu1	44.08 (15)
O4—Mo4—O2—Mo2	−15.47 (7)	O4—Mo4—O11—Cu1	149.19 (12)
O12—Mo4—O2—Mo2	−176.11 (8)	O12—Mo4—O11—Cu1	−57.88 (14)
O3—Mo4—O2—Mo2	−100.39 (7)	O2—Mo4—O11—Cu1	−124.0 (2)
Mo1ⁱⁱⁱ—Mo4—O2—Mo2	166.12 (9)	O3—Mo4—O11—Cu1	−129.41 (12)
O7—Mo1—O2—Mo1ⁱⁱⁱ	179.45 (10)	Mo1ⁱⁱⁱ—Mo4—O11—Cu1	−55.35 (16)
O12ⁱⁱⁱ—Mo1—O2—Mo1ⁱⁱⁱ	80.67 (9)	N2—Cu1—O11—Mo4	−132.28 (14)
O3—Mo1—O2—Mo1ⁱⁱⁱ	−80.65 (9)	N1ⁱ—Cu1—O11—Mo4	47.80 (15)
O2ⁱⁱⁱ—Mo1—O2—Mo1ⁱⁱⁱ	0.0	O10—Mo4—O12—Mo1ⁱⁱⁱ	71.13 (12)
O7—Mo1—O2—Mo4	−86.60 (9)	O11—Mo4—O12—Mo1ⁱⁱⁱ	176.80 (10)
O12ⁱⁱⁱ—Mo1—O2—Mo4	174.62 (9)	O4—Mo4—O12—Mo1ⁱⁱⁱ	−57.07 (18)
O3—Mo1—O2—Mo4	13.31 (7)	O2—Mo4—O12—Mo1ⁱⁱⁱ	−21.09 (9)
O2ⁱⁱⁱ—Mo1—O2—Mo4	93.95 (9)	O3—Mo4—O12—Mo1ⁱⁱⁱ	−96.70 (10)
O7—Mo1—O2—Mo3ⁱⁱⁱ	85.76 (9)	O10—Mo4—O12—Mo3	−172.55 (9)
O12ⁱⁱⁱ—Mo1—O2—Mo3ⁱⁱⁱ	−13.02 (8)	O11—Mo4—O12—Mo3	−66.88 (10)
O3—Mo1—O2—Mo3ⁱⁱⁱ	−174.34 (9)	O4—Mo4—O12—Mo3	59.25 (17)
O2ⁱⁱⁱ—Mo1—O2—Mo3ⁱⁱⁱ	−93.69 (9)	O2—Mo4—O12—Mo3	95.23 (8)
O7—Mo1—O2—Mo2	−0.57 (8)	O3—Mo4—O12—Mo3	19.61 (7)
O12ⁱⁱⁱ—Mo1—O2—Mo2	−99.35 (7)	O13—Mo3—O12—Mo1ⁱⁱⁱ	−167.66 (11)
O3—Mo1—O2—Mo2	99.33 (7)	O9—Mo3—O12—Mo1ⁱⁱⁱ	50.8 (3)
O2ⁱⁱⁱ—Mo1—O2—Mo2	179.98 (10)	O6ⁱⁱⁱ—Mo3—O12—Mo1ⁱⁱⁱ	−64.59 (10)
O5—Mo2—O2—Mo1ⁱⁱⁱ	4.3 (4)	O3—Mo3—O12—Mo1ⁱⁱⁱ	92.44 (10)
O8—Mo2—O2—Mo1ⁱⁱⁱ	−178.8 (3)	O2ⁱⁱⁱ—Mo3—O12—Mo1ⁱⁱⁱ	13.93 (8)
O6—Mo2—O2—Mo1ⁱⁱⁱ	−93.6 (4)	O13—Mo3—O12—Mo4	76.04 (10)
O4—Mo2—O2—Mo1ⁱⁱⁱ	97.5 (4)	O9—Mo3—O12—Mo4	−65.5 (3)
O7—Mo2—O2—Mo1ⁱⁱⁱ	−179.6 (4)	O6ⁱⁱⁱ—Mo3—O12—Mo4	179.11 (9)
O5—Mo2—O2—Mo4	−77.65 (9)	O3—Mo3—O12—Mo4	−23.87 (8)
O8—Mo2—O2—Mo4	99.2 (2)	O2ⁱⁱⁱ—Mo3—O12—Mo4	−102.37 (9)
O6—Mo2—O2—Mo4	−175.59 (9)	N1ⁱ—Cu1—N2—C15	−86.4 (5)
O4—Mo2—O2—Mo4	15.59 (7)	O11—Cu1—N2—C15	93.9 (2)
O7—Mo2—O2—Mo4	98.44 (7)	N1ⁱ—Cu1—N2—C11	91.6 (5)
O5—Mo2—O2—Mo3ⁱⁱⁱ	85.69 (9)	O11—Cu1—N2—C11	−88.1 (2)
O8—Mo2—O2—Mo3ⁱⁱⁱ	−97.4 (2)	O8—Cu2—N3—C6	15.9 (2)
O6—Mo2—O2—Mo3ⁱⁱⁱ	−12.24 (8)	O8—Cu2—N3—C10	−158.2 (2)
O4—Mo2—O2—Mo3ⁱⁱⁱ	178.93 (8)	C5—N1—C1—C2	−3.0 (4)
O7—Mo2—O2—Mo3ⁱⁱⁱ	−98.21 (7)	Cu1^iv—N1—C1—C2	161.5 (2)
O5—Mo2—O2—Mo1	−175.63 (8)	C5—N1—C1—C8	175.8 (3)
O8—Mo2—O2—Mo1	1.3 (2)	Cu1^iv—N1—C1—C8	−19.7 (4)
O6—Mo2—O2—Mo1	86.43 (8)	N1—C1—C2—C3	−0.8 (5)
O4—Mo2—O2—Mo1	−82.39 (8)	C8—C1—C2—C3	−179.5 (3)
O7—Mo2—O2—Mo1	0.46 (6)	C1—C2—C3—C4	4.0 (5)
O1—Mo1—O3—Mo3	−72.75 (11)	C2—C3—C4—C5	−3.3 (5)
O7—Mo1—O3—Mo3	−178.59 (9)	C1—N1—C5—C4	3.7 (5)
O12ⁱⁱⁱ—Mo1—O3—Mo3	65.72 (19)	Cu1^iv—N1—C5—C4	−162.7 (3)
O2ⁱⁱⁱ—Mo1—O3—Mo3	25.07 (9)	C3—C4—C5—N1	−0.5 (5)
O2—Mo1—O3—Mo3	103.08 (9)	C10—N3—C6—C7	0.7 (5)
O1—Mo1—O3—Mo4	170.53 (9)	Cu2—N3—C6—C7	−173.8 (2)
O7—Mo1—O3—Mo4	64.70 (10)	N3—C6—C7—C8	0.9 (5)
O12ⁱⁱⁱ—Mo1—O3—Mo4	−51.00 (19)	C6—C7—C8—C9	−1.2 (4)
O2ⁱⁱⁱ—Mo1—O3—Mo4	−91.65 (9)	C6—C7—C8—C1	175.7 (3)
O2—Mo1—O3—Mo4	−13.63 (7)	N1—C1—C8—C9	−22.9 (4)
O13—Mo3—O3—Mo1	176.59 (10)	C2—C1—C8—C9	155.9 (3)
O9—Mo3—O3—Mo1	70.46 (11)	N1—C1—C8—C7	160.5 (3)
O6ⁱⁱⁱ—Mo3—O3—Mo1	−56.21 (18)	C2—C1—C8—C7	−20.8 (4)
O2ⁱⁱⁱ—Mo3—O3—Mo1	−23.73 (8)	C7—C8—C9—C10	0.1 (4)
O12—Mo3—O3—Mo1	−99.26 (10)	C1—C8—C9—C10	−176.7 (3)
O13—Mo3—O3—Mo4	−64.05 (10)	C6—N3—C10—C9	−1.9 (5)
O9—Mo3—O3—Mo4	−170.18 (9)	Cu2—N3—C10—C9	172.3 (2)
O6ⁱⁱⁱ—Mo3—O3—Mo4	63.15 (17)	C8—C9—C10—N3	1.5 (5)
O2ⁱⁱⁱ—Mo3—O3—Mo4	95.63 (8)	C15—N2—C11—C12	0.4 (4)
O12—Mo3—O3—Mo4	20.10 (7)	Cu1—N2—C11—C12	−177.5 (2)
O10—Mo4—O3—Mo1	38.6 (4)	C15—N2—C11—C18	179.7 (3)
O11—Mo4—O3—Mo1	−167.07 (11)	Cu1—N2—C11—C18	1.7 (4)
O4—Mo4—O3—Mo1	−65.76 (10)	N2—C11—C12—C13	3.0 (5)
O12—Mo4—O3—Mo1	93.35 (10)	C18—C11—C12—C13	−176.2 (3)
O2—Mo4—O3—Mo1	14.77 (8)	C11—C12—C13—C14	−3.9 (5)
Mo1ⁱⁱⁱ—Mo4—O3—Mo1	58.02 (7)	C12—C13—C14—C15	1.4 (5)
O10—Mo4—O3—Mo3	−79.6 (4)	C11—N2—C15—C14	−3.1 (4)
O11—Mo4—O3—Mo3	74.75 (10)	Cu1—N2—C15—C14	175.1 (2)
O4—Mo4—O3—Mo3	176.05 (9)	C13—C14—C15—N2	2.2 (5)
O12—Mo4—O3—Mo3	−24.84 (8)	C20—N4—C16—C17	−0.3 (4)
O2—Mo4—O3—Mo3	−103.41 (9)	Cu2^v—N4—C16—C17	173.0 (2)
Mo1ⁱⁱⁱ—Mo4—O3—Mo3	−60.17 (7)	N4—C16—C17—C18	0.2 (4)
O10—Mo4—O4—Mo2	−69.74 (13)	C16—C17—C18—C19	−0.5 (4)
O11—Mo4—O4—Mo2	−176.51 (11)	C16—C17—C18—C11	−179.4 (3)
O12—Mo4—O4—Mo2	57.89 (19)	N2—C11—C18—C19	30.6 (4)
O2—Mo4—O4—Mo2	22.70 (10)	C12—C11—C18—C19	−150.1 (3)
O3—Mo4—O4—Mo2	95.67 (11)	N2—C11—C18—C17	−150.5 (3)
Mo1ⁱⁱⁱ—Mo4—O4—Mo2	23.95 (13)	C12—C11—C18—C17	28.7 (4)
O5—Mo2—O4—Mo4	75.61 (13)	C17—C18—C19—C20	1.0 (4)
O8—Mo2—O4—Mo4	−178.13 (11)	C11—C18—C19—C20	179.9 (3)
O6—Mo2—O4—Mo4	−39.1 (2)	C16—N4—C20—C19	0.9 (4)
O7—Mo2—O4—Mo4	−93.86 (11)	C18—C19—C20—N4	−1.2 (5)
O2—Mo2—O4—Mo4	−21.24 (9)	C17—C18—C19—C20	1.0 (4)
O5—Mo2—O6—Mo3ⁱⁱⁱ	−78.09 (14)	C11—C18—C19—C20	179.9 (3)
O8—Mo2—O6—Mo3ⁱⁱⁱ	174.12 (12)	C16—N4—C20—C19	0.9 (4)
O4—Mo2—O6—Mo3ⁱⁱⁱ	35.3 (2)	C18—C19—C20—N4	−1.2 (5)
O7—Mo2—O6—Mo3ⁱⁱⁱ	89.26 (12)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C4—H4···O5^vi	0.93	2.46	3.07	124
C7—H7···O1^vii	0.93	2.47	3.03	119
C10—H10···O4^viii	0.93	2.42	3.25	148
C12—H12···O9^ix	0.93	2.55	3.46	168
C14—H14···O10^x	0.93	2.47	3.12	127
C16—H16···O3^ix	0.93	2.45	3.02	120

Symmetry codes: (vi) x−1, y−1, z; (vii) −x+1, −y+1, −z+2; (viii) −x+1, −y+1, −z+1; (ix) −x+1, −y, −z+1; (x) −x+2, −y+1, −z+1.

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