Poly[bis­[bis­(ethyl­enediamine)copper(II)]-tetra-μ-cyano-[tetra­cyano­molybdate(IV)]]

Zhan, S.-Z.; Wang, J.-G.; Zhao, B.-T.; Huang, Z.-Y.; Cai, M.-L

doi:10.1107/S1600536806026535

Poly[bis[bis(ethylenediamine)copper(II)]-tetra-μ-cyano-[tetracyanomolybdate(IV)]]

S.-Z. Zhan, J.-G. Wang, B.-T. Zhao, Z.-Y. Huang and M.-L Cai

The title cyano-bridged heteronuclear coordination polymer, [Cu₂Mo(CN)₈(C₂H₈N₂)₄]_n, was synthesized by the reaction of [CuL₂]²⁺ (L is ethylenediamine) and [Mo(CN)₈]⁴⁻ in an aqueous solution. The structure is a three-dimensional polymer; the Cu sits on a position with twofold symmetry and the Mo sits on a position with $\overline{4}$ symmetry.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806026535/om2025sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806026535/om2025Isup2.hkl Contains datablock I

CCDC reference: 618299

checkCIF report

Key indicators

Single-crystal X-ray study
T = 291 K
Mean (C-C) = 0.004 Å
R factor = 0.026
wR factor = 0.059
Data-to-parameter ratio = 19.0

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT420_ALERT_2_C D-H Without Acceptor       N1     -   H1B    ...          ?
PLAT420_ALERT_2_C D-H Without Acceptor       N2     -   H2B    ...          ?
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          1
            N2  -CU1 -N1  -C1    122.20  0.50   2.565   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          5
            N1  -CU1 -N2  -C2     96.50  0.50   2.565   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         10
            C4  -MO1 -C3  -N3    135.00  4.00   2.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         11
            C4  -MO1 -C3  -N3     34.00  4.00   8.656   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         12
            C4  -MO1 -C3  -N3   -146.00  4.00   7.566   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         13
            C4  -MO1 -C3  -N3    -68.00  4.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         14
            C3  -MO1 -C3  -N3   -147.00  4.00   2.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         15
            C3  -MO1 -C3  -N3     84.00  4.00   8.656   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         16
            C3  -MO1 -C3  -N3    -19.00  4.00   7.566   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         17
            C4  -MO1 -C4  -N4     16.00  6.00   2.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         18
            C4  -MO1 -C4  -N4    -91.00  6.00   8.656   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         19
            C4  -MO1 -C4  -N4    123.00  6.00   7.566   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         20
            C3  -MO1 -C4  -N4    -23.00  6.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         21
            C3  -MO1 -C4  -N4     55.00  6.00   2.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         22
            C3  -MO1 -C4  -N4   -163.00  6.00   8.656   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         23
            C3  -MO1 -C4  -N4   -165.00  6.00   7.566   1.555   1.555   1.555

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

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

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: APEX2; data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1995); software used to prepare material for publication: SHELXTL.

Poly[bis[bis(ethylenediamine)copper(II)]-tetra-µ-cyano- [tetracyanomolybdate(IV)]] top

Crystal data top

[Cu₂Mo(CN)₈(C₂H₈N₂)₄]	D_x = 1.670 Mg m⁻³
M_r = 671.60	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P4₂/n	Cell parameters from 2278 reflections
a = 9.2676 (7) Å	θ = 2.6–27.9°
c = 15.550 (2) Å	µ = 2.08 mm⁻¹
V = 1335.6 (2) Å³	T = 291 K
Z = 2	Block, blue
F(000) = 680	0.36 × 0.17 × 0.08 mm

Data collection top

Bruker SMART APEX-II diffractometer	1524 independent reflections
Radiation source: fine-focus sealed tube	1215 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.072
Detector resolution: 8.3 pixels mm^-1	θ_max = 27.5°, θ_min = 2.6°
φ and ω scans	h = −12→8
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −7→12
T_min = 0.524, T_max = 0.848	l = −20→20
5810 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.027	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.059	H-atom parameters constrained
S = 0.96	w = 1/[σ²(F_o²) + (0.0203P)²] where P = (F_o² + 2F_c²)/3
1524 reflections	(Δ/σ)_max < 0.001
80 parameters	Δρ_max = 0.52 e Å⁻³
0 restraints	Δρ_min = −0.50 e Å⁻³

Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)

are estimated using the full covariance matrix. The cell e.s.d.'s are taken

into account individually in the estimation of e.s.d.'s in distances, angles

and torsion angles; correlations between e.s.d.'s in cell parameters are only

used when they are defined by crystal symmetry. An approximate (isotropic)

treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and

goodness of fit S are based on F², conventional R-factors R are based

on F, with F set to zero for negative F². The threshold expression of

F² > σ(F²) is used only for calculating R-factors(gt) etc. and is

not relevant to the choice of reflections for refinement. R-factors based

on F² are statistically about twice as large as those based on F, and R-

factors based on ALL data will be even larger.

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

	x	y	z	U_iso*/U_eq
Mo1	0.2500	0.2500	0.2500	0.02093 (11)
Cu1	0.2500	0.7500	0.09307 (2)	0.04140 (14)
N1	0.40382 (18)	0.7090 (2)	0.18087 (12)	0.0365 (4)
H1A	0.3910	0.7653	0.2274	0.044*
H1B	0.3991	0.6162	0.1976	0.044*
N2	0.4131 (2)	0.7441 (2)	0.00870 (14)	0.0442 (5)
H2A	0.3889	0.6889	−0.0367	0.053*
H2B	0.4324	0.8337	−0.0104	0.053*
N3	0.1776 (2)	0.4604 (2)	0.08210 (13)	0.0483 (5)
N4	0.5659 (2)	0.3711 (2)	0.18150 (13)	0.0460 (5)
C1	0.5451 (3)	0.7388 (3)	0.14150 (18)	0.0488 (6)
H1C	0.6210	0.6908	0.1736	0.059*
H1D	0.5642	0.8417	0.1418	0.059*
C2	0.5408 (3)	0.6839 (3)	0.05162 (17)	0.0549 (7)
H2C	0.6276	0.7126	0.0212	0.066*
H2D	0.5358	0.5793	0.0517	0.066*
C3	0.2014 (2)	0.3849 (2)	0.13860 (14)	0.0314 (5)
C4	0.4571 (2)	0.3286 (2)	0.20683 (13)	0.0309 (5)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.02120 (13)	0.02120 (13)	0.02039 (17)	0.000	0.000	0.000
Cu1	0.0372 (2)	0.0621 (3)	0.0249 (2)	0.0079 (2)	0.000	0.000
N1	0.0355 (10)	0.0400 (11)	0.0341 (10)	0.0038 (8)	−0.0009 (8)	−0.0060 (9)
N2	0.0584 (14)	0.0367 (11)	0.0374 (11)	−0.0037 (10)	0.0134 (10)	−0.0030 (9)
N3	0.0660 (15)	0.0408 (12)	0.0381 (12)	0.0147 (10)	0.0023 (10)	0.0083 (9)
N4	0.0353 (11)	0.0684 (14)	0.0344 (11)	−0.0139 (10)	0.0011 (9)	0.0030 (10)
C1	0.0361 (14)	0.0500 (16)	0.0602 (17)	−0.0053 (12)	−0.0003 (12)	−0.0029 (13)
C2	0.0468 (16)	0.0641 (18)	0.0538 (17)	0.0086 (14)	0.0198 (13)	−0.0013 (14)
C3	0.0375 (12)	0.0261 (11)	0.0306 (11)	0.0041 (9)	0.0021 (9)	−0.0033 (9)
C4	0.0319 (11)	0.0378 (12)	0.0231 (11)	−0.0028 (10)	−0.0019 (9)	0.0011 (9)

Geometric parameters (Å, º) top

Mo1—C4ⁱ	2.160 (2)	N1—H1A	0.9000
Mo1—C4ⁱⁱ	2.160 (2)	N1—H1B	0.9000
Mo1—C4ⁱⁱⁱ	2.160 (2)	N2—C2	1.469 (3)
Mo1—C4	2.160 (2)	N2—H2A	0.9000
Mo1—C3	2.183 (2)	N2—H2B	0.9000
Mo1—C3ⁱ	2.183 (2)	N3—C3	1.145 (3)
Mo1—C3ⁱⁱ	2.183 (2)	N4—C4	1.152 (3)
Mo1—C3ⁱⁱⁱ	2.183 (2)	C1—C2	1.488 (4)
Cu1—N2^iv	2.003 (2)	C1—H1C	0.9700
Cu1—N2	2.003 (2)	C1—H1D	0.9700
Cu1—N1^iv	2.0100 (18)	C2—H2C	0.9700
Cu1—N1	2.0101 (18)	C2—H2D	0.9700
N1—C1	1.472 (3)

C4ⁱ—Mo1—C4ⁱⁱ	95.54 (3)	N2—Cu1—N1^iv	170.25 (8)
C4ⁱ—Mo1—C4ⁱⁱⁱ	95.54 (3)	N2^iv—Cu1—N1	170.26 (8)
C4ⁱⁱ—Mo1—C4ⁱⁱⁱ	143.79 (11)	N2—Cu1—N1	84.51 (8)
C4ⁱ—Mo1—C4	143.79 (11)	N1^iv—Cu1—N1	94.44 (10)
C4ⁱⁱ—Mo1—C4	95.54 (3)	C1—N1—Cu1	108.24 (15)
C4ⁱⁱⁱ—Mo1—C4	95.54 (3)	C1—N1—H1A	110.0
C4ⁱ—Mo1—C3	76.30 (8)	Cu1—N1—H1A	110.0
C4ⁱⁱ—Mo1—C3	70.62 (7)	C1—N1—H1B	110.0
C4ⁱⁱⁱ—Mo1—C3	145.59 (8)	Cu1—N1—H1B	110.0
C4—Mo1—C3	75.15 (8)	H1A—N1—H1B	108.4
C4ⁱ—Mo1—C3ⁱ	75.15 (8)	C2—N2—Cu1	108.72 (15)
C4ⁱⁱ—Mo1—C3ⁱ	145.59 (8)	C2—N2—H2A	109.9
C4ⁱⁱⁱ—Mo1—C3ⁱ	70.62 (7)	Cu1—N2—H2A	109.9
C4—Mo1—C3ⁱ	76.30 (8)	C2—N2—H2B	109.9
C3—Mo1—C3ⁱ	74.99 (11)	Cu1—N2—H2B	109.9
C4ⁱ—Mo1—C3ⁱⁱ	70.62 (7)	H2A—N2—H2B	108.3
C4ⁱⁱ—Mo1—C3ⁱⁱ	75.15 (8)	N1—C1—C2	107.6 (2)
C4ⁱⁱⁱ—Mo1—C3ⁱⁱ	76.30 (8)	N1—C1—H1C	110.2
C4—Mo1—C3ⁱⁱ	145.59 (8)	C2—C1—H1C	110.2
C3—Mo1—C3ⁱⁱ	129.02 (7)	N1—C1—H1D	110.2
C3ⁱ—Mo1—C3ⁱⁱ	129.02 (7)	C2—C1—H1D	110.2
C4ⁱ—Mo1—C3ⁱⁱⁱ	145.59 (8)	H1C—C1—H1D	108.5
C4ⁱⁱ—Mo1—C3ⁱⁱⁱ	76.30 (8)	N2—C2—C1	108.6 (2)
C4ⁱⁱⁱ—Mo1—C3ⁱⁱⁱ	75.15 (8)	N2—C2—H2C	110.0
C4—Mo1—C3ⁱⁱⁱ	70.62 (7)	C1—C2—H2C	110.0
C3—Mo1—C3ⁱⁱⁱ	129.02 (7)	N2—C2—H2D	110.0
C3ⁱ—Mo1—C3ⁱⁱⁱ	129.01 (7)	C1—C2—H2D	110.0
C3ⁱⁱ—Mo1—C3ⁱⁱⁱ	74.99 (11)	H2C—C2—H2D	108.4
N2^iv—Cu1—N2	98.14 (13)	N3—C3—Mo1	177.2 (2)
N2^iv—Cu1—N1^iv	84.51 (8)	N4—C4—Mo1	178.03 (19)

N2^iv—Cu1—N1—C1	122.2 (5)	C4—Mo1—C3—N3	−68 (4)
N2—Cu1—N1—C1	15.89 (15)	C3ⁱ—Mo1—C3—N3	−147 (4)
N1^iv—Cu1—N1—C1	−154.38 (17)	C3ⁱⁱ—Mo1—C3—N3	84 (4)
N2^iv—Cu1—N2—C2	−158.26 (19)	C3ⁱⁱⁱ—Mo1—C3—N3	−19 (4)
N1^iv—Cu1—N2—C2	96.5 (5)	C4ⁱ—Mo1—C4—N4	16 (6)
N1—Cu1—N2—C2	12.29 (16)	C4ⁱⁱ—Mo1—C4—N4	−91 (6)
Cu1—N1—C1—C2	−40.6 (2)	C4ⁱⁱⁱ—Mo1—C4—N4	123 (6)
Cu1—N2—C2—C1	−38.1 (2)	C3—Mo1—C4—N4	−23 (6)
N1—C1—C2—N2	52.3 (3)	C3ⁱ—Mo1—C4—N4	55 (6)
C4ⁱ—Mo1—C3—N3	135 (4)	C3ⁱⁱ—Mo1—C4—N4	−163 (6)
C4ⁱⁱ—Mo1—C3—N3	34 (4)	C3ⁱⁱⁱ—Mo1—C4—N4	−165 (6)
C4ⁱⁱⁱ—Mo1—C3—N3	−146 (4)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···N4^v	0.90	2.12	3.004 (3)	168
N2—H2A···N4^vi	0.90	2.36	3.150 (3)	147
N2—H2B···N3^iv	0.90	2.60	3.084 (3)	115

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

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Poly[bis­[bis­(ethyl­enediamine)copper(II)]-tetra-μ-cyano-[tetra­cyano­molybdate(IV)]]

Supporting information

Key indicators

checkCIF/PLATON results

Poly[bis[bis(ethylenediamine)copper(II)]-tetra-μ-cyano-[tetracyanomolybdate(IV)]]