Diaqua­bis­(propane-1,3-diamine)­copper(II) bis­[diamminetetra­kis­(thio­cyanato-κN)chromate(III)] dimethyl sulfoxide octa­solvate

Nikitina, V.M.; Nesterova, O.V.; Zubatyuk, R.I.; Shishkin, O.V.; Rusanova, J.A.

doi:10.1107/S160053681102023X

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 7| July 2011| Pages m849-m850

doi:10.1107/S160053681102023X

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Diaquabis(propane-1,3-diamine)copper(II) bis[diamminetetrakis(thiocyanato-κN)chromate(III)] dimethyl sulfoxide octasolvate

Vitalina M. Nikitina,^a Oksana V. Nesterova,^a Roman I. Zubatyuk,^b Oleg V. Shishkin ^b and Julia A. Rusanova ^a ^*

^aNational Taras Shevchenko University, Department of Chemistry, Volodymyrska Str. 64, 01033 Kyiv, Ukraine, and ^bInstitute for Scintillation Materials, "Institute for Single Crystals", National Academy of Sciences of Ukraine, Lenina ave. 60, Kharkov 61001, Ukraine
^*Correspondence e-mail: rusanova_j@yahoo.com

(Received 11 May 2011; accepted 26 May 2011; online 4 June 2011)

The ionic title complex, [Cu(C₃H₁₀N₂)₂(H₂O)₂][Cr(NCS)₄(NH₃)₂]·8C₂H₆OS, consists of complex [Cu(dipr)₂(H₂O)₂]²⁺ copper cations (dipr is propane-1,3-diamine), complex [Cr(NCS)₄(NH₃)₂]⁻ anions and uncoordinated solvent dimethyl sulfoxide (DMSO) molecules. All the metal atoms lie on crystallographic centers of symmetry. The cations are connected to the anions through N—H⋯O hydrogen bonds between the NH₃ molecules of the anion and the water molecules of the cation. The DMSO molecules are involved in hydrogen-bonded linkage of the [Cr(NCS)₄(NH₃)₂]⁻ anions into supramolecular chains through bridging O atoms. A network of hydrogen bonds as well as short S⋯S contacts [3.5159 (12) and 3.4880 (12) Å] between the NCS groups of the complex anions link the molecules into a three-dimensional supramolecular network.

Related literature

For background to direct synthesis see: Nesterov et al. (2004 , 2006 ); Kovbasyuk et al. (1997 , 1998 ); Vassilyeva et al. (1997 ). For the stuctures of related compexes, see: Zhang et al. (2001 ); Cucos et al. (2006 ); Cherkasova & Gorunova (2003 ); Kolotilov et al. (2010 ).

Experimental

Crystal data

[Cu(C₃H₁₀N₂)₂(H₂O)₂]·[Cr(NCS)₄(NH₃)₂]·8(C₂H₆OS)
M_r = 1509.63
Triclinic, $[P \overline 1]$
a = 12.2609 (11) Å
b = 12.2772 (12) Å
c = 13.8578 (12) Å
α = 72.466 (8)°
β = 89.664 (7)°
γ = 61.535 (10)°
V = 1724.9 (3) Å³
Z = 1
Mo Kα radiation
μ = 1.15 mm⁻¹
T = 100 K
0.6 × 0.4 × 0.3 mm

Data collection

Oxford Diffraction Xcalibur Sapphire3 diffractometer
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2010 $[Oxford Diffraction (2010). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.]$ ) T_min = 0.58, T_max = 0.71
15229 measured reflections
8482 independent reflections
6966 reflections with I > 2σ(I)
R_int = 0.020

Refinement

R[F² > 2σ(F²)] = 0.037
wR(F²) = 0.097
S = 1.08
8482 reflections
353 parameters
H-atom parameters constrained
Δρ_max = 0.76 e Å⁻³
Δρ_min = −0.56 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1E⋯O2ⁱ	0.87	1.88	2.732 (2)	165
O1—H1E⋯S5ⁱ	0.87	2.87	3.5905 (18)	142
O1—H1F⋯O4	0.87	1.98	2.786 (2)	153
N1—H1A⋯O2ⁱⁱ	0.92	2.10	2.995 (3)	163
N1—H1B⋯S4ⁱⁱⁱ	0.92	2.70	3.490 (2)	145
N2—H2A⋯O4	0.92	2.33	3.052 (2)	135
N2—H2B⋯O3	0.92	2.24	3.091 (3)	153
N5—H5A⋯O2	0.91	2.11	3.003 (2)	167
N5—H5B⋯O3^iv	0.91	2.21	3.079 (2)	161
N5—H5C⋯O5^v	0.91	2.09	2.966 (2)	160
N8—H8A⋯O1ⁱⁱⁱ	0.91	2.08	2.956 (2)	162
N8—H8B⋯O5^vi	0.91	2.19	3.054 (2)	159
N8—H8C⋯O3^vii	0.91	2.10	2.981 (2)	162
Symmetry codes: (i) -x+1, -y+1, -z; (ii) x-1, y+1, z; (iii) -x, -y+1, -z; (iv) x+1, y-1, z; (v) -x+1, -y+1, -z+1; (vi) -x, -y+1, -z+1; (vii) x, y-1, z.

Data collection: CrysAlis PRO (Oxford Diffraction, 2010 $[Oxford Diffraction (2010). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.]$ ); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053681102023X/br2167sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053681102023X/br2167Isup2.hkl

checkCIF report

Comment top

It has been shown that direct synthesis is an efficient method to obtained novel homo- and heterometallic complexes (Nesterov et al. (2004, 2006); Kovbasyuk et al. (1997, 1998); Vassilyeva et al. (1997)). Continuing our investigations in this paper we present a novel Cu/Cr heterometallic ionic complex which has been synthesized using zerovalent copper, Reinecke's salt and 1,3-propilenediamine as starting materials. As it shown on Fig. 1 Cu atoms in complex cations are in square bypiramidal coordination environment with four N atoms in equatorial position and two O atoms of the H₂O molecules in axial position. The Cr centers are coordinated to six N atoms - four NCS-groups in equatorial position and two NH₃ molecules in axial position. The bond distances and angles in the title molecule agree well with the corresponding bond distances and angles reported in closely related compounds (Zhang et al., 2001, Cucos et al., 2006; Cherkasova et al., 2003; Kolotilov et al., 2010). There are short interanionic S···S contacts between NCS-groups of the complex anions with the distances 3.5159 (12) and 3.4880 (12) Å whereas sum of standard Van-der-Vaals radius of the sulfur atom is 3.68 Å. The crystal packing of the title compound is presented on Fig 2.

Related literature top

For background to direct synthesis see: Nesterov et al. (2004, 2006); Kovbasyuk et al. (1997, 1998); Vassilyeva et al. (1997). For the stuctures of related compexes, see: Zhang et al. (2001); Cucos et al. (2006); Cherkasova & Gorunova (2003); Kolotilov et al. (2010).

Experimental top

For the preparation of the title compound, copper powder 0.04 g (0.63 mmol), NH₄[Cr(NCS)₄(NH₃)₂]^.H₂O 0.45 g (1.26 mmol), 0.11 ml (1.26 mmol) 1,3-propilenediamine (dipr), 20 ml of DMSO, were heated to 323–333 K and stirred magnetically for 15 min, until total dissolution of the copper powder was observed. Addition of a few ml of the PrⁱOH to the cooled solution leads to precipitation within few days of the dark violet crystals suitable for X-ray analysis. They were collected by filter-suction, washed with dry PrⁱOH and finally dried in vacuo at room temperature (yield: 0.59 g, 69%).

Computing details top

Data collection: CrysAlis PRO (Oxford Diffraction, 2010); cell refinement: CrysAlis PRO (Oxford Diffraction, 2010); data reduction: CrysAlis PRO (Oxford Diffraction, 2010); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

	Fig. 1. Molecular view of the title compound. DMSO molecules are omitted for clarity. Displacement ellipsoids are drawn at the 50% probability level.
	Fig. 2. Crystal packing of the title compound along b axis.

Diaquabis(propane-1,3-diamine)copper(II) bis[diamminetetrakis(thiocyanato-κN)chromate(III)] dimethyl sulfoxide octasolvate top

Crystal data top

[Cu(C₃H₁₀N₂)₂(H₂O)₂]·[Cr(NCS)₄(NH₃)₂]·8(C₂H₆OS)	Z = 1
M_r = 1509.63	F(000) = 789
Triclinic, P1	D_x = 1.453 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 12.2609 (11) Å	Cell parameters from 4303 reflections
b = 12.2772 (12) Å	θ = 2.9–25.0°
c = 13.8578 (12) Å	µ = 1.15 mm⁻¹
α = 72.466 (8)°	T = 100 K
β = 89.664 (7)°	Block, violet
γ = 61.535 (10)°	0.6 × 0.4 × 0.3 mm
V = 1724.9 (3) Å³

Data collection top

Oxford Diffraction Xcalibur Sapphire3 diffractometer	8482 independent reflections
Radiation source: Enhance (Mo) X-ray Source	6966 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.020
Detector resolution: 16.1827 pixels mm^-1	θ_max = 29.9°, θ_min = 2.9°
ω and ϕ scans	h = −16→16
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2010)	k = −16→15
T_min = 0.58, T_max = 0.71	l = −19→19
15229 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)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.097	H-atom parameters constrained
S = 1.08	w = 1/[σ²(F_o²) + (0.0448P)² + 1.0385P] where P = (F_o² + 2F_c²)/3
8482 reflections	(Δ/σ)_max = 0.001
353 parameters	Δρ_max = 0.76 e Å⁻³
0 restraints	Δρ_min = −0.56 e Å⁻³

Crystal data top

[Cu(C₃H₁₀N₂)₂(H₂O)₂]·[Cr(NCS)₄(NH₃)₂]·8(C₂H₆OS)	γ = 61.535 (10)°
M_r = 1509.63	V = 1724.9 (3) Å³
Triclinic, P1	Z = 1
a = 12.2609 (11) Å	Mo Kα radiation
b = 12.2772 (12) Å	µ = 1.15 mm⁻¹
c = 13.8578 (12) Å	T = 100 K
α = 72.466 (8)°	0.6 × 0.4 × 0.3 mm
β = 89.664 (7)°

Data collection top

Oxford Diffraction Xcalibur Sapphire3 diffractometer	8482 independent reflections
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2010)	6966 reflections with I > 2σ(I)
T_min = 0.58, T_max = 0.71	R_int = 0.020
15229 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	0 restraints
wR(F²) = 0.097	H-atom parameters constrained
S = 1.08	Δρ_max = 0.76 e Å⁻³
8482 reflections	Δρ_min = −0.56 e Å⁻³
353 parameters

Special details top

Experimental. Xcalibur; Oxford Diffraction, (2010) CrysAlisPro, Oxford Diffraction (2010). Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.

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
O1	0.13010 (15)	0.77778 (15)	−0.02683 (12)	0.0259 (3)
H1E	0.1484	0.8037	−0.0871	0.039*
H1F	0.1991	0.7425	0.0160	0.039*
Cu1	0.0000	1.0000	0.0000	0.01782 (9)
Cr1	1.0000	0.0000	0.5000	0.01666 (10)
Cr2	0.0000	0.5000	0.0000	0.01895 (11)
S1	1.22765 (6)	0.19198 (6)	0.58717 (5)	0.03186 (14)
S2	0.60022 (5)	0.32965 (5)	0.52979 (4)	0.02642 (13)
S3	0.28491 (6)	0.43926 (7)	0.26932 (6)	0.03845 (16)
S4	0.34351 (5)	0.12439 (6)	−0.04325 (5)	0.02791 (13)
S5	0.64253 (5)	0.22031 (5)	0.19080 (4)	0.02553 (12)
S6	0.30881 (5)	1.08392 (5)	0.23806 (4)	0.02493 (12)
S7	0.47022 (5)	0.58296 (6)	0.11082 (4)	0.02518 (12)
S8	0.17949 (5)	0.48082 (5)	0.67464 (4)	0.02321 (12)
O2	0.78274 (14)	0.13337 (16)	0.19770 (12)	0.0264 (3)
O3	0.18069 (15)	1.09692 (16)	0.22392 (13)	0.0276 (3)
O4	0.36425 (15)	0.72167 (16)	0.05789 (12)	0.0275 (3)
O5	0.16592 (15)	0.58928 (15)	0.71241 (12)	0.0263 (3)
N1	−0.10137 (17)	0.93537 (17)	0.09092 (14)	0.0220 (4)
H1A	−0.1522	1.0008	0.1162	0.026*
H1B	−0.1535	0.9272	0.0496	0.026*
N2	0.13971 (17)	0.92577 (18)	0.12042 (13)	0.0212 (4)
H2A	0.2133	0.9049	0.0940	0.025*
H2B	0.1236	0.9936	0.1440	0.025*
N3	1.08964 (17)	0.08516 (17)	0.53719 (13)	0.0209 (4)
N4	0.83883 (17)	0.13557 (17)	0.52307 (14)	0.0220 (4)
N5	0.96720 (16)	0.11943 (17)	0.34908 (13)	0.0186 (3)
H5A	0.9124	0.1123	0.3108	0.022*
H5B	1.0410	0.0939	0.3241	0.022*
H5C	0.9338	0.2046	0.3460	0.022*
N6	0.12608 (17)	0.47359 (18)	0.10717 (15)	0.0242 (4)
N7	0.13479 (17)	0.35414 (18)	−0.03865 (15)	0.0239 (4)
N8	−0.03243 (17)	0.36323 (17)	0.10530 (14)	0.0213 (4)
H8A	−0.0753	0.3381	0.0719	0.026*
H8B	−0.0786	0.3996	0.1501	0.026*
H8C	0.0423	0.2917	0.1403	0.026*
C1	−0.0366 (2)	0.8106 (2)	0.17926 (17)	0.0254 (5)
H1C	0.0134	0.7365	0.1541	0.031*
H1D	−0.0998	0.7942	0.2157	0.031*
C2	0.0489 (2)	0.8171 (2)	0.25237 (17)	0.0266 (5)
H2C	0.0741	0.7434	0.3179	0.032*
H2D	0.0018	0.9003	0.2669	0.032*
C3	0.1658 (2)	0.8099 (2)	0.21183 (16)	0.0256 (5)
H3A	0.2224	0.8027	0.2669	0.031*
H3B	0.2103	0.7291	0.1935	0.031*
C4	1.1462 (2)	0.1305 (2)	0.55823 (16)	0.0215 (4)
C5	0.7391 (2)	0.2164 (2)	0.52692 (16)	0.0207 (4)
C6	0.1937 (2)	0.4591 (2)	0.17413 (18)	0.0240 (4)
C7	0.2218 (2)	0.2583 (2)	−0.04054 (16)	0.0219 (4)
C8	0.5722 (2)	0.1351 (3)	0.1611 (2)	0.0333 (5)
H8D	0.5821	0.1333	0.0913	0.050*
H8E	0.4826	0.1801	0.1659	0.050*
H8F	0.6131	0.0447	0.2098	0.050*
C9	0.6182 (3)	0.1991 (3)	0.3196 (2)	0.0557 (10)
H9A	0.6514	0.1053	0.3578	0.084*
H9B	0.5280	0.2480	0.3214	0.084*
H9C	0.6619	0.2323	0.3511	0.084*
C10	0.4189 (2)	0.9225 (2)	0.2392 (2)	0.0311 (5)
H10A	0.4043	0.8578	0.2903	0.047*
H10B	0.5046	0.9045	0.2568	0.047*
H10C	0.4083	0.9167	0.1712	0.047*
C11	0.3450 (3)	1.0572 (3)	0.3702 (2)	0.0402 (6)
H11A	0.2926	1.1390	0.3842	0.060*
H11B	0.4340	1.0294	0.3870	0.060*
H11C	0.3285	0.9883	0.4122	0.060*
C12	0.6073 (2)	0.5762 (3)	0.0626 (2)	0.0329 (5)
H12A	0.6020	0.5784	−0.0086	0.049*
H12B	0.6818	0.4946	0.1046	0.049*
H12C	0.6135	0.6520	0.0652	0.049*
C13	0.5117 (2)	0.5740 (3)	0.23673 (19)	0.0354 (6)
H13A	0.5284	0.6457	0.2328	0.053*
H13B	0.5873	0.4892	0.2718	0.053*
H13C	0.4423	0.5824	0.2750	0.053*
C14	0.0292 (2)	0.4947 (3)	0.6669 (2)	0.0331 (5)
H14A	0.0074	0.4758	0.7358	0.050*
H14B	0.0302	0.4317	0.6367	0.050*
H14C	−0.0334	0.5844	0.6239	0.050*
C15	0.1823 (3)	0.5356 (3)	0.54062 (19)	0.0348 (6)
H15A	0.1095	0.6237	0.5080	0.052*
H15B	0.1791	0.4744	0.5104	0.052*
H15C	0.2599	0.5389	0.5298	0.052*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
O1	0.0239 (8)	0.0248 (8)	0.0277 (8)	−0.0124 (7)	0.0004 (6)	−0.0066 (6)
Cu1	0.01624 (17)	0.01650 (17)	0.01893 (17)	−0.00831 (14)	0.00019 (13)	−0.00339 (13)
Cr1	0.0145 (2)	0.0143 (2)	0.0189 (2)	−0.00612 (17)	0.00164 (17)	−0.00447 (17)
Cr2	0.0162 (2)	0.0144 (2)	0.0248 (2)	−0.00683 (18)	0.00464 (18)	−0.00617 (18)
S1	0.0354 (3)	0.0315 (3)	0.0385 (3)	−0.0230 (3)	0.0043 (3)	−0.0136 (3)
S2	0.0196 (3)	0.0210 (3)	0.0285 (3)	−0.0031 (2)	0.0046 (2)	−0.0073 (2)
S3	0.0249 (3)	0.0358 (3)	0.0474 (4)	−0.0128 (3)	−0.0097 (3)	−0.0085 (3)
S4	0.0189 (3)	0.0210 (3)	0.0415 (3)	−0.0054 (2)	0.0044 (2)	−0.0154 (2)
S5	0.0205 (3)	0.0208 (3)	0.0282 (3)	−0.0047 (2)	−0.0019 (2)	−0.0087 (2)
S6	0.0225 (3)	0.0225 (3)	0.0303 (3)	−0.0126 (2)	0.0066 (2)	−0.0071 (2)
S7	0.0186 (3)	0.0235 (3)	0.0323 (3)	−0.0096 (2)	0.0007 (2)	−0.0095 (2)
S8	0.0230 (3)	0.0177 (2)	0.0258 (3)	−0.0086 (2)	0.0018 (2)	−0.0060 (2)
O2	0.0186 (8)	0.0266 (8)	0.0288 (8)	−0.0080 (6)	−0.0002 (6)	−0.0083 (7)
O3	0.0203 (8)	0.0248 (8)	0.0363 (9)	−0.0109 (7)	0.0059 (7)	−0.0093 (7)
O4	0.0193 (8)	0.0240 (8)	0.0304 (8)	−0.0060 (6)	0.0000 (6)	−0.0061 (6)
O5	0.0292 (8)	0.0210 (8)	0.0282 (8)	−0.0115 (7)	0.0020 (7)	−0.0093 (6)
N1	0.0193 (9)	0.0189 (9)	0.0257 (9)	−0.0096 (7)	0.0015 (7)	−0.0046 (7)
N2	0.0185 (8)	0.0228 (9)	0.0208 (8)	−0.0095 (7)	0.0018 (7)	−0.0065 (7)
N3	0.0192 (9)	0.0166 (8)	0.0228 (8)	−0.0069 (7)	0.0025 (7)	−0.0048 (7)
N4	0.0202 (9)	0.0183 (9)	0.0233 (9)	−0.0078 (7)	0.0020 (7)	−0.0046 (7)
N5	0.0183 (8)	0.0173 (8)	0.0191 (8)	−0.0081 (7)	0.0033 (7)	−0.0059 (6)
N6	0.0192 (9)	0.0208 (9)	0.0308 (10)	−0.0094 (7)	0.0033 (8)	−0.0076 (8)
N7	0.0201 (9)	0.0198 (9)	0.0306 (9)	−0.0089 (7)	0.0064 (7)	−0.0085 (7)
N8	0.0205 (9)	0.0168 (8)	0.0269 (9)	−0.0100 (7)	0.0041 (7)	−0.0067 (7)
C1	0.0270 (11)	0.0196 (10)	0.0251 (10)	−0.0115 (9)	0.0022 (9)	−0.0018 (8)
C2	0.0279 (12)	0.0238 (11)	0.0197 (10)	−0.0085 (9)	0.0026 (9)	−0.0041 (8)
C3	0.0235 (11)	0.0232 (11)	0.0197 (10)	−0.0073 (9)	−0.0039 (8)	−0.0012 (8)
C4	0.0215 (10)	0.0176 (10)	0.0212 (10)	−0.0078 (8)	0.0026 (8)	−0.0045 (8)
C5	0.0222 (10)	0.0176 (10)	0.0204 (9)	−0.0096 (8)	0.0020 (8)	−0.0046 (8)
C6	0.0176 (10)	0.0173 (10)	0.0324 (11)	−0.0073 (8)	0.0041 (9)	−0.0046 (9)
C7	0.0194 (10)	0.0235 (11)	0.0267 (10)	−0.0122 (9)	0.0067 (8)	−0.0110 (9)
C8	0.0254 (12)	0.0302 (12)	0.0427 (14)	−0.0155 (10)	0.0030 (10)	−0.0075 (11)
C9	0.0343 (15)	0.064 (2)	0.0323 (14)	0.0075 (14)	0.0003 (12)	−0.0237 (14)
C10	0.0228 (11)	0.0241 (11)	0.0393 (13)	−0.0085 (9)	0.0057 (10)	−0.0070 (10)
C11	0.0467 (16)	0.0494 (17)	0.0368 (14)	−0.0317 (14)	0.0075 (12)	−0.0169 (12)
C12	0.0197 (11)	0.0330 (13)	0.0436 (14)	−0.0112 (10)	0.0056 (10)	−0.0133 (11)
C13	0.0267 (12)	0.0367 (14)	0.0314 (12)	−0.0080 (11)	−0.0039 (10)	−0.0101 (11)
C14	0.0312 (13)	0.0326 (13)	0.0399 (13)	−0.0195 (11)	0.0069 (11)	−0.0119 (11)
C15	0.0510 (16)	0.0367 (14)	0.0314 (12)	−0.0301 (13)	0.0165 (11)	−0.0166 (11)

Geometric parameters (Å, º) top

O1—H1E	0.8692	N4—C5	1.165 (3)
O1—H1F	0.8704	N5—H5A	0.9100
Cu1—O1	2.5655 (16)	N5—H5B	0.9100
Cu1—N1	2.0202 (18)	N5—H5C	0.9100
Cu1—N1ⁱ	2.0202 (18)	N6—C6	1.162 (3)
Cu1—N2ⁱ	2.0442 (17)	N7—C7	1.159 (3)
Cu1—N2	2.0442 (17)	N8—H8A	0.9100
Cr1—N4	1.9888 (18)	N8—H8B	0.9100
Cr1—N4ⁱⁱ	1.9888 (18)	N8—H8C	0.9100
Cr1—N3ⁱⁱ	1.9983 (19)	C1—C2	1.508 (3)
Cr1—N3	1.9983 (19)	C1—H1C	0.9900
Cr1—N5	2.0702 (17)	C1—H1D	0.9900
Cr1—N5ⁱⁱ	2.0702 (17)	C2—C3	1.509 (3)
Cr2—N6	1.9898 (19)	C2—H2C	0.9900
Cr2—N6ⁱⁱⁱ	1.9898 (19)	C2—H2D	0.9900
Cr2—N7ⁱⁱⁱ	1.9928 (18)	C3—H3A	0.9900
Cr2—N7	1.9928 (19)	C3—H3B	0.9900
Cr2—N8	2.0640 (17)	C8—H8D	0.9800
Cr2—N8ⁱⁱⁱ	2.0641 (17)	C8—H8E	0.9800
S1—C4	1.623 (2)	C8—H8F	0.9800
S2—C5	1.615 (2)	C9—H9A	0.9800
S3—C6	1.617 (2)	C9—H9B	0.9800
S4—C7	1.622 (2)	C9—H9C	0.9800
S5—O2	1.5149 (16)	C10—H10A	0.9800
S5—C8	1.769 (3)	C10—H10B	0.9800
S5—C9	1.770 (3)	C10—H10C	0.9800
S6—O3	1.5090 (17)	C11—H11A	0.9800
S6—C11	1.780 (3)	C11—H11B	0.9800
S6—C10	1.783 (2)	C11—H11C	0.9800
S7—O4	1.5086 (16)	C12—H12A	0.9800
S7—C13	1.777 (3)	C12—H12B	0.9800
S7—C12	1.779 (2)	C12—H12C	0.9800
S8—O5	1.5108 (17)	C13—H13A	0.9800
S8—C14	1.769 (3)	C13—H13B	0.9800
S8—C15	1.781 (2)	C13—H13C	0.9800
N1—C1	1.483 (3)	C14—H14A	0.9800
N1—H1A	0.9200	C14—H14B	0.9800
N1—H1B	0.9200	C14—H14C	0.9800
N2—C3	1.489 (3)	C15—H15A	0.9800
N2—H2A	0.9200	C15—H15B	0.9800
N2—H2B	0.9200	C15—H15C	0.9800
N3—C4	1.159 (3)

H1E—O1—H1F	105.3	Cr2—N8—H8B	109.5
N1—Cu1—N1ⁱ	180.00 (11)	H8A—N8—H8B	109.5
N1—Cu1—N2ⁱ	87.84 (7)	Cr2—N8—H8C	109.5
N1ⁱ—Cu1—N2ⁱ	92.16 (7)	H8A—N8—H8C	109.5
N1—Cu1—N2	92.16 (7)	H8B—N8—H8C	109.5
N1ⁱ—Cu1—N2	87.84 (7)	N1—C1—C2	110.69 (19)
N2ⁱ—Cu1—N2	180.0	N1—C1—H1C	109.5
N1—Cu1—O1	92.27 (6)	C2—C1—H1C	109.5
N1ⁱ—Cu1—O1	87.73 (6)	N1—C1—H1D	109.5
N2ⁱ—Cu1—O1	94.59 (6)	C2—C1—H1D	109.5
N2—Cu1—O1	85.41 (6)	H1C—C1—H1D	108.1
N4—Cr1—N4ⁱⁱ	180.00 (10)	C1—C2—C3	113.34 (19)
N4—Cr1—N3ⁱⁱ	89.65 (8)	C1—C2—H2C	108.9
N4ⁱⁱ—Cr1—N3ⁱⁱ	90.35 (8)	C3—C2—H2C	108.9
N4—Cr1—N3	90.35 (8)	C1—C2—H2D	108.9
N4ⁱⁱ—Cr1—N3	89.65 (8)	C3—C2—H2D	108.9
N3ⁱⁱ—Cr1—N3	180.00 (6)	H2C—C2—H2D	107.7
N4—Cr1—N5	90.24 (7)	N2—C3—C2	113.53 (18)
N4ⁱⁱ—Cr1—N5	89.76 (7)	N2—C3—H3A	108.9
N3ⁱⁱ—Cr1—N5	91.87 (7)	C2—C3—H3A	108.9
N3—Cr1—N5	88.13 (7)	N2—C3—H3B	108.9
N4—Cr1—N5ⁱⁱ	89.76 (7)	C2—C3—H3B	108.9
N4ⁱⁱ—Cr1—N5ⁱⁱ	90.24 (7)	H3A—C3—H3B	107.7
N3ⁱⁱ—Cr1—N5ⁱⁱ	88.13 (7)	N3—C4—S1	178.9 (2)
N3—Cr1—N5ⁱⁱ	91.87 (7)	N4—C5—S2	178.86 (19)
N5—Cr1—N5ⁱⁱ	180.000 (1)	N6—C6—S3	178.4 (2)
N6—Cr2—N6ⁱⁱⁱ	180.0	N7—C7—S4	179.9 (3)
N6—Cr2—N7ⁱⁱⁱ	90.37 (8)	S5—C8—H8D	109.5
N6ⁱⁱⁱ—Cr2—N7ⁱⁱⁱ	89.63 (8)	S5—C8—H8E	109.5
N6—Cr2—N7	89.63 (8)	H8D—C8—H8E	109.5
N6ⁱⁱⁱ—Cr2—N7	90.37 (8)	S5—C8—H8F	109.5
N7ⁱⁱⁱ—Cr2—N7	180.00 (10)	H8D—C8—H8F	109.5
N6—Cr2—N8	89.48 (8)	H8E—C8—H8F	109.5
N6ⁱⁱⁱ—Cr2—N8	90.52 (8)	S5—C9—H9A	109.5
N7ⁱⁱⁱ—Cr2—N8	91.17 (7)	S5—C9—H9B	109.5
N7—Cr2—N8	88.83 (7)	H9A—C9—H9B	109.5
N6—Cr2—N8ⁱⁱⁱ	90.52 (8)	S5—C9—H9C	109.5
N6ⁱⁱⁱ—Cr2—N8ⁱⁱⁱ	89.48 (8)	H9A—C9—H9C	109.5
N7ⁱⁱⁱ—Cr2—N8ⁱⁱⁱ	88.83 (7)	H9B—C9—H9C	109.5
N7—Cr2—N8ⁱⁱⁱ	91.17 (7)	S6—C10—H10A	109.5
N8—Cr2—N8ⁱⁱⁱ	180.00 (14)	S6—C10—H10B	109.5
O2—S5—C8	105.70 (11)	H10A—C10—H10B	109.5
O2—S5—C9	104.89 (11)	S6—C10—H10C	109.5
C8—S5—C9	98.98 (17)	H10A—C10—H10C	109.5
O3—S6—C11	105.98 (12)	H10B—C10—H10C	109.5
O3—S6—C10	105.91 (11)	S6—C11—H11A	109.5
C11—S6—C10	97.80 (13)	S6—C11—H11B	109.5
O4—S7—C13	106.08 (11)	H11A—C11—H11B	109.5
O4—S7—C12	106.13 (11)	S6—C11—H11C	109.5
C13—S7—C12	97.55 (13)	H11A—C11—H11C	109.5
O5—S8—C14	105.80 (11)	H11B—C11—H11C	109.5
O5—S8—C15	106.19 (11)	S7—C12—H12A	109.5
C14—S8—C15	97.93 (13)	S7—C12—H12B	109.5
C1—N1—Cu1	120.07 (14)	H12A—C12—H12B	109.5
C1—N1—H1A	107.3	S7—C12—H12C	109.5
Cu1—N1—H1A	107.3	H12A—C12—H12C	109.5
C1—N1—H1B	107.3	H12B—C12—H12C	109.5
Cu1—N1—H1B	107.3	S7—C13—H13A	109.5
H1A—N1—H1B	106.9	S7—C13—H13B	109.5
C3—N2—Cu1	121.96 (14)	H13A—C13—H13B	109.5
C3—N2—H2A	106.8	S7—C13—H13C	109.5
Cu1—N2—H2A	106.8	H13A—C13—H13C	109.5
C3—N2—H2B	106.8	H13B—C13—H13C	109.5
Cu1—N2—H2B	106.8	S8—C14—H14A	109.5
H2A—N2—H2B	106.7	S8—C14—H14B	109.5
C4—N3—Cr1	177.22 (18)	H14A—C14—H14B	109.5
C5—N4—Cr1	173.03 (18)	S8—C14—H14C	109.5
Cr1—N5—H5A	109.5	H14A—C14—H14C	109.5
Cr1—N5—H5B	109.5	H14B—C14—H14C	109.5
H5A—N5—H5B	109.5	S8—C15—H15A	109.5
Cr1—N5—H5C	109.5	S8—C15—H15B	109.5
H5A—N5—H5C	109.5	H15A—C15—H15B	109.5
H5B—N5—H5C	109.5	S8—C15—H15C	109.5
C6—N6—Cr2	175.38 (19)	H15A—C15—H15C	109.5
C7—N7—Cr2	166.49 (18)	H15B—C15—H15C	109.5
Cr2—N8—H8A	109.5

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1E···O2^iv	0.87	1.88	2.732 (2)	165
O1—H1E···S5^iv	0.87	2.87	3.5905 (18)	142
O1—H1F···O4	0.87	1.98	2.786 (2)	153
N1—H1A···O2^v	0.92	2.10	2.995 (3)	163
N1—H1B···S4ⁱⁱⁱ	0.92	2.70	3.490 (2)	145
N2—H2A···O4	0.92	2.33	3.052 (2)	135
N2—H2B···O3	0.92	2.24	3.091 (3)	153
N5—H5A···O2	0.91	2.11	3.003 (2)	167
N5—H5B···O3^vi	0.91	2.21	3.079 (2)	161
N5—H5C···O5^vii	0.91	2.09	2.966 (2)	160
N8—H8A···O1ⁱⁱⁱ	0.91	2.08	2.956 (2)	162
N8—H8B···O5^viii	0.91	2.19	3.054 (2)	159
N8—H8C···O3^ix	0.91	2.10	2.981 (2)	162

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

Experimental details

Crystal data
Chemical formula	[Cu(C₃H₁₀N₂)₂(H₂O)₂]·[Cr(NCS)₄(NH₃)₂]·8(C₂H₆OS)
M_r	1509.63
Crystal system, space group	Triclinic, P1
Temperature (K)	100
a, b, c (Å)	12.2609 (11), 12.2772 (12), 13.8578 (12)
α, β, γ (°)	72.466 (8), 89.664 (7), 61.535 (10)
V (Å³)	1724.9 (3)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	1.15
Crystal size (mm)	0.6 × 0.4 × 0.3

Data collection
Diffractometer	Oxford Diffraction Xcalibur Sapphire3 diffractometer
Absorption correction	Multi-scan (CrysAlis PRO; Oxford Diffraction, 2010)
T_min, T_max	0.58, 0.71
No. of measured, independent and observed [I > 2σ(I)] reflections	15229, 8482, 6966
R_int	0.020
(sin θ/λ)_max (Å⁻¹)	0.701

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.097, 1.08
No. of reflections	8482
No. of parameters	353
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.76, −0.56

Computer programs: CrysAlis PRO (Oxford Diffraction, 2010), SHELXTL (Sheldrick, 2008), publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1E···O2ⁱ	0.87	1.88	2.732 (2)	165
O1—H1E···S5ⁱ	0.87	2.87	3.5905 (18)	142
O1—H1F···O4	0.87	1.98	2.786 (2)	153
N1—H1A···O2ⁱⁱ	0.92	2.10	2.995 (3)	163
N1—H1B···S4ⁱⁱⁱ	0.92	2.70	3.490 (2)	145
N2—H2A···O4	0.92	2.33	3.052 (2)	135
N2—H2B···O3	0.92	2.24	3.091 (3)	153
N5—H5A···O2	0.91	2.11	3.003 (2)	167
N5—H5B···O3^iv	0.91	2.21	3.079 (2)	161
N5—H5C···O5^v	0.91	2.09	2.966 (2)	160
N8—H8A···O1ⁱⁱⁱ	0.91	2.08	2.956 (2)	162
N8—H8B···O5^vi	0.91	2.19	3.054 (2)	159
N8—H8C···O3^vii	0.91	2.10	2.981 (2)	162

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

Acknowledgements

The authors gratefully acknowledge the Ukrainian State Fund for Fundamental Researchers (SFFR) for financial support of the Research Program (Chemistry).

References

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Volume 67| Part 7| July 2011| Pages m849-m850

doi:10.1107/S160053681102023X

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Di­aqua­bis­­(propane-1,3-di­amine)­copper(II) bis­­[diammine­tetra­kis­(thio­cyanato-κN)chromate(III)] di­methyl sulfoxide octa­solvate

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Diaquabis(propane-1,3-diamine)copper(II) bis[diamminetetrakis(thiocyanato-κN)chromate(III)] dimethyl sulfoxide octasolvate