Di-μ-chlorido-bis­[dichlorido(3,3′,5,5′-tetra­methyl-4,4′-bipyrazol-1-ium-κN2′)copper(II)] dihydrate

Kurawa, M.A.; Adams, C.J.; Orpen, A.G.

doi:10.1107/S1600536808022605

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 8| August 2008| Pages m1053-m1054

doi:10.1107/S1600536808022605

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Di-μ-chlorido-bis[dichlorido(3,3′,5,5′-tetramethyl-4,4′-bipyrazol-1-ium-κN^2′)copper(II)] dihydrate

Mukhtar A. Kurawa,^a Christopher J. Adams ^a and A. Guy Orpen ^a ^*

^aSchool of Chemistry, University of Bristol, Bristol BS8 1TS, England
^*Correspondence e-mail: guy.orpen@bris.ac.uk

(Received 26 June 2008; accepted 18 July 2008; online 23 July 2008)

The structure of the centrosymmetric title compound, [Cu₂Cl₆(C₁₀H₁₅N₄)₂]·2H₂O, consists of a dimeric [{(HMe₄bpz)CuCl₃}₂] unit (HMe₄bpz is 3,3′,5,5′-tetramethyl-4,4′-bipyrazol-1-ium) with two solvent water molecules. Each [HMe₄bpz]⁺ cation is bonded to a CuCl₃ unit through a Cu—N dative bond, effectively making square-planar geometry at the Cu atom. Two of these units then undergo a face-to-face dimerization so that the Cu atoms have a Jahn–Teller distorted square-pyramidal geometry with three chlorides and an N atom in the basal plane and one chloride weakly bound in the apical position. Several N—H⋯Cl, O—H⋯Cl and N—H⋯O hydrogen bonds form a three-dimensional network.

Related literature

We have been unable to find any references in the literature to any other compound containing a monoprotonated 3,3′,5,5′- tetramethylbipyrazole ligand coordinated only to one metal atom through a single nitrogen donor, but Komarchuk et al. (2004 ) reported a compound containing two unprotonated tetramethylbipyrazole ligands acting as ligands to a single copper atom. For an exploration of N—H⋯Cl interactions in the design and synthesis of crystal structures with desired properties such as unit-cell metrics or defined reactivity, see: Adams et al. (2005 ).

Experimental

Crystal data

[Cu₂Cl₆(C₁₀H₁₅N₄)₂]·2H₂O
M_r = 758.35
Triclinic, $[P \overline 1]$
a = 8.2837 (4) Å
b = 10.5907 (6) Å
c = 10.9058 (6) Å
α = 102.4385 (9)°
β = 108.4401 (9)°
γ = 110.2613 (8)°
V = 792.70 (7) Å³
Z = 1
Mo Kα radiation
μ = 1.88 mm⁻¹
T = 173 (2) K
0.2 × 0.13 × 0.07 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2008a ) T_min = 0.787, T_max = 0.87
8466 measured reflections
3609 independent reflections
3242 reflections with I > 2σ(I)
R_int = 0.023

Refinement

R[F² > 2σ(F²)] = 0.024
wR(F²) = 0.064
S = 1.04
3609 reflections
182 parameters
2 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.39 e Å⁻³
Δρ_min = −0.34 e Å⁻³

Table 1
Selected bond lengths (Å)

Cu1—N2	1.9834 (13)
Cu1—Cl1	2.2684 (5)
Cu1—Cl3	2.2988 (4)
Cu1—Cl2	2.3345 (4)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯Cl1ⁱ	0.88	2.43	3.2625 (14)	157
N3—H3A⋯O1ⁱⁱ	0.88	1.80	2.6786 (19)	173
N4—H4A⋯Cl3ⁱⁱⁱ	0.88	2.26	3.1435 (14)	179
O1—H11⋯Cl1^iv	0.811 (15)	2.519 (17)	3.2640 (14)	153 (2)
O1—H11⋯Cl3^iv	0.811 (15)	2.74 (2)	3.3031 (14)	128.5 (19)
O1—H12⋯Cl2^v	0.800 (15)	2.404 (16)	3.1923 (14)	169 (2)
Symmetry codes: (i) -x+2, -y+3, -z+1; (ii) x, y, z-1; (iii) x, y-1, z; (iv) -x+2, -y+2, -z+1; (v) x-1, y-1, z.

Data collection: SMART (Bruker, 2001 ); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008b ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008b); molecular graphics: SHELXTL (Sheldrick, 2008b); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808022605/rn2046sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808022605/rn2046Isup2.hkl

checkCIF report

Comment top

We have sought to explore N—H···Cl interactions in designing and synthesizing crystal structures with desired properties such as unit cell metrics or defined reactivity (Adams et al., 2005). We aimed to utilize these interactions by reacting 3,3',5,5'- tetramethylbipyrazole dihydrochloride and copper(II) chloride dihydrate in a 1:1 ratio to synthesize (C₁₀H₁₆N₄)[CuCl₄]. However, the title compound I was obtained instead, crystallizing in the triclinic system with the P1 space group, with a [HMe₄bpz]⁺ cation bonded to a CuCl₃^-unit through a Cu—N bond, forming a zwitterion. In the crystal structure, water molecules bridge adjacent [{(HMe₄bpz)CuCl₃}₂] dimers through O—H···Cl hydrogen bonds forming a hydrogen bonded ribbon (Fig. 2) along the a-axis.

Related literature top

We have been unable to find any references in the literature to any other compound containing a monoprotonated 3,3',5,5'- tetramethylbipyrazole ligand coordinated only to one metal atom through a single nitrogen donor, but Komarchuk et al. (2004) reported a compound containing two unprotonated tetramethylbipyrazole ligands acting as ligands to a single copper atom.

For related literature, see: Adams et al. (2005).

Experimental top

An attempt to synthesize tetramethylbipyrazolium tetrachlorocuprate(II) by slow evaporation at room temperature of a solution of equimolar amounts of tetramethylbipyrazole hydrochloride and copper(II) chloride dihydrate in concentrated HCl resulted in the formation of the title compound as a by-product in the form of pale green, plate-like crystals.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008b); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008b); molecular graphics: SHELXTL (Sheldrick, 2008b); software used to prepare material for publication: SHELXTL (Sheldrick, 2008b).

Figures top

	Fig. 1. The molecular structure of I with atom labels and 50% probability displacement ellipsoids for non-H atoms. [Symmetry codes: (A) -x + 2, -y + 3, -z + 1; (B) x, y - 1, z]
	Fig. 2. Packing of I viewed down the c axis, with O—H···Cl bonds connecting the dimeric units.

Di-µ-chlorido-bis[dichlorido(3,3',5,5'- tetramethyl-4,4'-bipyrazol-1-ium-κN^2')copper(II)] dihydrate top

Crystal data top

[Cu₂Cl₆(C₁₀H₁₅N₄)₂]·2H₂O	Z = 1
M_r = 758.35	F(000) = 386
Triclinic, P1	D_x = 1.589 Mg m⁻³
a = 8.2837 (4) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.5907 (6) Å	Cell parameters from 5647 reflections
c = 10.9058 (6) Å	θ = 2.4–27.5°
α = 102.4385 (9)°	µ = 1.88 mm⁻¹
β = 108.4401 (9)°	T = 173 K
γ = 110.2613 (8)°	Plate, green
V = 792.70 (7) Å³	0.2 × 0.13 × 0.08 mm

Data collection top

Bruker SMART CCD area-detector diffractometer	3609 independent reflections
Radiation source: fine-focus sealed tube	3242 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.023
ϕ and ω scans	θ_max = 27.5°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 2008a)	h = −10→10
T_min = 0.787, T_max = 0.87	k = −13→13
8466 measured reflections	l = −14→14

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)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.064	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ²(F_o²) + (0.0305P)² + 0.3154P] where P = (F_o² + 2F_c²)/3
3609 reflections	(Δ/σ)_max = 0.002
182 parameters	Δρ_max = 0.39 e Å⁻³
2 restraints	Δρ_min = −0.34 e Å⁻³

Crystal data top

[Cu₂Cl₆(C₁₀H₁₅N₄)₂]·2H₂O	γ = 110.2613 (8)°
M_r = 758.35	V = 792.70 (7) Å³
Triclinic, P1	Z = 1
a = 8.2837 (4) Å	Mo Kα radiation
b = 10.5907 (6) Å	µ = 1.88 mm⁻¹
c = 10.9058 (6) Å	T = 173 K
α = 102.4385 (9)°	0.2 × 0.13 × 0.08 mm
β = 108.4401 (9)°

Data collection top

Bruker SMART CCD area-detector diffractometer	3609 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2008a)	3242 reflections with I > 2σ(I)
T_min = 0.787, T_max = 0.87	R_int = 0.023
8466 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.024	2 restraints
wR(F²) = 0.064	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	Δρ_max = 0.39 e Å⁻³
3609 reflections	Δρ_min = −0.34 e Å⁻³
182 parameters

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	1.11358 (3)	1.463916 (19)	0.381212 (19)	0.01706 (7)
Cl1	1.38009 (6)	1.67695 (4)	0.47299 (5)	0.02431 (10)
Cl2	1.16045 (6)	1.45959 (4)	0.60262 (4)	0.02086 (9)
Cl3	1.04245 (6)	1.46073 (4)	0.15868 (4)	0.02189 (10)
N1	0.7878 (2)	1.19314 (14)	0.32487 (14)	0.0185 (3)
H1A	0.7400	1.2435	0.3637	0.022*
N2	0.9482 (2)	1.25267 (14)	0.30738 (14)	0.0178 (3)
N3	0.7030 (2)	0.64464 (15)	0.01465 (15)	0.0210 (3)
H3A	0.6352	0.5632	−0.0579	0.025*
N4	0.8615 (2)	0.67473 (15)	0.12509 (15)	0.0217 (3)
H4A	0.9136	0.6159	0.1356	0.026*
C1	0.5323 (3)	0.9567 (2)	0.2828 (2)	0.0291 (4)
H1B	0.5223	1.0103	0.3631	0.044*
H1C	0.5358	0.8677	0.2923	0.044*
H1D	0.4220	0.9325	0.1977	0.044*
C2	0.7099 (2)	1.04760 (17)	0.27573 (17)	0.0185 (3)
C3	0.8267 (2)	1.01087 (17)	0.22334 (16)	0.0167 (3)
C4	0.9734 (2)	1.14256 (17)	0.24501 (16)	0.0172 (3)
C5	1.1377 (3)	1.16715 (19)	0.2077 (2)	0.0261 (4)
H5A	1.1436	1.2324	0.1559	0.039*
H5B	1.1210	1.0746	0.1501	0.039*
H5C	1.2561	1.2106	0.2926	0.039*
C6	0.4994 (3)	0.7602 (2)	−0.0706 (2)	0.0310 (4)
H6A	0.4776	0.7067	−0.1642	0.047*
H6B	0.5248	0.8602	−0.0607	0.047*
H6C	0.3862	0.7144	−0.0553	0.047*
C7	0.6656 (2)	0.75913 (17)	0.03346 (17)	0.0192 (3)
C8	0.8057 (2)	0.86539 (17)	0.16027 (17)	0.0171 (3)
C9	0.9272 (2)	0.80751 (17)	0.21604 (18)	0.0194 (3)
C10	1.0961 (3)	0.8699 (2)	0.3517 (2)	0.0290 (4)
H10A	1.1679	0.8134	0.3499	0.044*
H10B	1.0542	0.8671	0.4260	0.044*
H10C	1.1775	0.9703	0.3684	0.044*
O1	0.50412 (19)	0.40901 (14)	0.78153 (14)	0.0258 (3)
H11	0.570 (3)	0.402 (2)	0.741 (2)	0.031*
H12	0.413 (3)	0.410 (2)	0.729 (2)	0.031*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.02091 (11)	0.01281 (11)	0.01527 (11)	0.00629 (8)	0.00744 (8)	0.00371 (8)
Cl1	0.0229 (2)	0.01816 (19)	0.0263 (2)	0.00477 (16)	0.01237 (17)	0.00262 (16)
Cl2	0.0242 (2)	0.0218 (2)	0.0157 (2)	0.01139 (16)	0.00700 (16)	0.00580 (15)
Cl3	0.0302 (2)	0.0242 (2)	0.0190 (2)	0.01682 (18)	0.01283 (17)	0.01042 (16)
N1	0.0212 (7)	0.0162 (7)	0.0193 (7)	0.0090 (6)	0.0104 (6)	0.0050 (5)
N2	0.0208 (7)	0.0148 (6)	0.0168 (7)	0.0072 (6)	0.0085 (6)	0.0045 (5)
N3	0.0246 (7)	0.0150 (7)	0.0197 (7)	0.0082 (6)	0.0085 (6)	0.0026 (6)
N4	0.0265 (7)	0.0186 (7)	0.0239 (8)	0.0138 (6)	0.0112 (6)	0.0080 (6)
C1	0.0264 (9)	0.0215 (9)	0.0384 (11)	0.0074 (7)	0.0192 (8)	0.0069 (8)
C2	0.0202 (8)	0.0166 (8)	0.0171 (8)	0.0085 (7)	0.0068 (6)	0.0051 (6)
C3	0.0180 (7)	0.0152 (7)	0.0144 (8)	0.0074 (6)	0.0049 (6)	0.0042 (6)
C4	0.0204 (8)	0.0157 (7)	0.0145 (8)	0.0087 (6)	0.0061 (6)	0.0047 (6)
C5	0.0269 (9)	0.0202 (8)	0.0331 (10)	0.0099 (7)	0.0172 (8)	0.0075 (7)
C6	0.0270 (9)	0.0258 (9)	0.0267 (10)	0.0127 (8)	−0.0001 (8)	0.0012 (8)
C7	0.0214 (8)	0.0163 (8)	0.0197 (8)	0.0084 (6)	0.0093 (7)	0.0056 (6)
C8	0.0194 (7)	0.0148 (7)	0.0183 (8)	0.0081 (6)	0.0086 (6)	0.0065 (6)
C9	0.0217 (8)	0.0177 (8)	0.0206 (8)	0.0094 (7)	0.0095 (7)	0.0087 (7)
C10	0.0264 (9)	0.0269 (9)	0.0284 (10)	0.0125 (8)	0.0040 (8)	0.0110 (8)
O1	0.0243 (7)	0.0271 (7)	0.0245 (7)	0.0119 (6)	0.0117 (6)	0.0043 (5)

Geometric parameters (Å, º) top

Cu1—N2	1.9834 (13)	C2—C3	1.388 (2)
Cu1—Cl1	2.2684 (5)	C3—C4	1.407 (2)
Cu1—Cl3	2.2988 (4)	C3—C8	1.470 (2)
Cu1—Cl2	2.3345 (4)	C4—C5	1.495 (2)
Cu1—Cl2ⁱ	2.7029 (5)	C5—H5A	0.9800
Cl2—Cu1ⁱ	2.7029 (5)	C5—H5B	0.9800
N1—C2	1.348 (2)	C5—H5C	0.9800
N1—N2	1.3538 (19)	C6—C7	1.487 (2)
N1—H1A	0.8800	C6—H6A	0.9800
N2—C4	1.335 (2)	C6—H6B	0.9800
N3—C7	1.342 (2)	C6—H6C	0.9800
N3—N4	1.349 (2)	C7—C8	1.391 (2)
N3—H3A	0.8800	C8—C9	1.400 (2)
N4—C9	1.336 (2)	C9—C10	1.487 (2)
N4—H4A	0.8800	C10—H10A	0.9800
C1—C2	1.490 (2)	C10—H10B	0.9800
C1—H1B	0.9800	C10—H10C	0.9800
C1—H1C	0.9800	O1—H11	0.811 (15)
C1—H1D	0.9800	O1—H12	0.800 (15)

N2—Cu1—Cl1	159.99 (4)	C2—C3—C8	127.73 (15)
N2—Cu1—Cl3	90.16 (4)	C4—C3—C8	126.42 (14)
Cl1—Cu1—Cl3	92.769 (17)	N2—C4—C3	109.72 (14)
N2—Cu1—Cl2	87.45 (4)	N2—C4—C5	121.50 (15)
Cl1—Cu1—Cl2	90.762 (17)	C3—C4—C5	128.78 (14)
Cl3—Cu1—Cl2	175.537 (17)	C4—C5—H5A	109.5
N2—Cu1—Cl2ⁱ	95.31 (4)	C4—C5—H5B	109.5
Cl1—Cu1—Cl2ⁱ	104.333 (16)	H5A—C5—H5B	109.5
Cl3—Cu1—Cl2ⁱ	92.434 (14)	C4—C5—H5C	109.5
Cl2—Cu1—Cl2ⁱ	84.042 (14)	H5A—C5—H5C	109.5
Cu1—Cl2—Cu1ⁱ	95.958 (14)	H5B—C5—H5C	109.5
C2—N1—N2	111.89 (13)	C7—C6—H6A	109.5
C2—N1—H1A	124.1	C7—C6—H6B	109.5
N2—N1—H1A	124.1	H6A—C6—H6B	109.5
C4—N2—N1	106.26 (13)	C7—C6—H6C	109.5
C4—N2—Cu1	130.17 (11)	H6A—C6—H6C	109.5
N1—N2—Cu1	123.33 (10)	H6B—C6—H6C	109.5
C7—N3—N4	108.88 (13)	N3—C7—C8	107.84 (14)
C7—N3—H3A	125.6	N3—C7—C6	122.10 (15)
N4—N3—H3A	125.6	C8—C7—C6	130.06 (15)
C9—N4—N3	109.65 (13)	C7—C8—C9	106.25 (14)
C9—N4—H4A	125.2	C7—C8—C3	127.55 (14)
N3—N4—H4A	125.2	C9—C8—C3	126.19 (15)
C2—C1—H1B	109.5	N4—C9—C8	107.39 (15)
C2—C1—H1C	109.5	N4—C9—C10	122.58 (15)
H1B—C1—H1C	109.5	C8—C9—C10	130.00 (15)
C2—C1—H1D	109.5	C9—C10—H10A	109.5
H1B—C1—H1D	109.5	C9—C10—H10B	109.5
H1C—C1—H1D	109.5	H10A—C10—H10B	109.5
N1—C2—C3	106.28 (15)	C9—C10—H10C	109.5
N1—C2—C1	122.23 (15)	H10A—C10—H10C	109.5
C3—C2—C1	131.49 (15)	H10B—C10—H10C	109.5
C2—C3—C4	105.84 (14)	H11—O1—H12	107 (2)

N2—Cu1—Cl2—Cu1ⁱ	−95.61 (4)	N1—N2—C4—C5	179.50 (15)
Cl1—Cu1—Cl2—Cu1ⁱ	104.331 (16)	Cu1—N2—C4—C5	−6.1 (2)
Cl2ⁱ—Cu1—Cl2—Cu1ⁱ	0.0	C2—C3—C4—N2	0.31 (18)
C2—N1—N2—C4	0.25 (18)	C8—C3—C4—N2	−178.69 (15)
C2—N1—N2—Cu1	−174.59 (11)	C2—C3—C4—C5	−179.52 (17)
Cl1—Cu1—N2—C4	−27.4 (2)	C8—C3—C4—C5	1.5 (3)
Cl3—Cu1—N2—C4	71.20 (14)	N4—N3—C7—C8	0.06 (19)
Cl2—Cu1—N2—C4	−112.57 (14)	N4—N3—C7—C6	179.90 (16)
Cl2ⁱ—Cu1—N2—C4	163.66 (14)	N3—C7—C8—C9	−0.39 (19)
Cl1—Cu1—N2—N1	146.16 (10)	C6—C7—C8—C9	179.78 (18)
Cl3—Cu1—N2—N1	−115.29 (12)	N3—C7—C8—C3	178.39 (16)
Cl2—Cu1—N2—N1	60.94 (12)	C6—C7—C8—C3	−1.4 (3)
Cl2ⁱ—Cu1—N2—N1	−22.83 (12)	C2—C3—C8—C7	69.0 (3)
C7—N3—N4—C9	0.32 (19)	C4—C3—C8—C7	−112.3 (2)
N2—N1—C2—C3	−0.06 (18)	C2—C3—C8—C9	−112.5 (2)
N2—N1—C2—C1	179.98 (15)	C4—C3—C8—C9	66.3 (2)
N1—C2—C3—C4	−0.15 (18)	N3—N4—C9—C8	−0.56 (19)
C1—C2—C3—C4	179.81 (18)	N3—N4—C9—C10	177.32 (16)
N1—C2—C3—C8	178.83 (15)	C7—C8—C9—N4	0.58 (19)
C1—C2—C3—C8	−1.2 (3)	C3—C8—C9—N4	−178.22 (16)
N1—N2—C4—C3	−0.34 (17)	C7—C8—C9—C10	−177.09 (18)
Cu1—N2—C4—C3	174.02 (11)	C3—C8—C9—C10	4.1 (3)

Symmetry code: (i) −x+2, −y+3, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···Cl1ⁱ	0.88	2.43	3.2625 (14)	157
N3—H3A···O1ⁱⁱ	0.88	1.80	2.6786 (19)	173
N4—H4A···Cl3ⁱⁱⁱ	0.88	2.26	3.1435 (14)	179
O1—H11···Cl1^iv	0.81 (2)	2.52 (2)	3.2640 (14)	153 (2)
O1—H11···Cl3^iv	0.81 (2)	2.74 (2)	3.3031 (14)	129 (2)
O1—H12···Cl2^v	0.80 (2)	2.40 (2)	3.1923 (14)	169 (2)

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

Experimental details

Crystal data
Chemical formula	[Cu₂Cl₆(C₁₀H₁₅N₄)₂]·2H₂O
M_r	758.35
Crystal system, space group	Triclinic, P1
Temperature (K)	173
a, b, c (Å)	8.2837 (4), 10.5907 (6), 10.9058 (6)
α, β, γ (°)	102.4385 (9), 108.4401 (9), 110.2613 (8)
V (Å³)	792.70 (7)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	1.88
Crystal size (mm)	0.2 × 0.13 × 0.08

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2008a)
T_min, T_max	0.787, 0.87
No. of measured, independent and observed [I > 2σ(I)] reflections	8466, 3609, 3242
R_int	0.023
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.024, 0.064, 1.04
No. of reflections	3609
No. of parameters	182
No. of restraints	2
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.39, −0.34

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008b), SHELXL97 (Sheldrick, 2008b), SHELXTL (Sheldrick, 2008b).

Selected bond lengths (Å) top

Cu1—N2	1.9834 (13)	Cu1—Cl3	2.2988 (4)
Cu1—Cl1	2.2684 (5)	Cu1—Cl2	2.3345 (4)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···Cl1ⁱ	0.88	2.43	3.2625 (14)	156.9
N3—H3A···O1ⁱⁱ	0.88	1.80	2.6786 (19)	173.2
N4—H4A···Cl3ⁱⁱⁱ	0.88	2.26	3.1435 (14)	178.8
O1—H11···Cl1^iv	0.811 (15)	2.519 (17)	3.2640 (14)	153 (2)
O1—H11···Cl3^iv	0.811 (15)	2.74 (2)	3.3031 (14)	128.5 (19)
O1—H12···Cl2^v	0.800 (15)	2.404 (16)	3.1923 (14)	169 (2)

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

Acknowledgements

MAK thanks Bayero University, Kano, Nigeria for funding.

References

Adams, C. J., Crawford, P. C., Orpen, A. G., Podesta, T. J. & Salt, B. (2005). Chem. Commun. pp. 2457–2458. Web of Science CSD CrossRef Google Scholar
Bruker (2001). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Komarchuk, V. V., Ponomarova, V. V., Krautscheid, H. & Domasevitch, K. V. (2004). Z. Anorg. Allg. Chem. 630, 1413–1418. Web of Science CSD CrossRef CAS Google Scholar
Sheldrick, G. M. (2008a). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008b). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar

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Volume 64| Part 8| August 2008| Pages m1053-m1054

doi:10.1107/S1600536808022605

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

Di-μ-chlorido-bis­­[di­chlorido(3,3′,5,5′-tetra­methyl-4,4′-bipyrazol-1-ium-κN2′)copper(II)] dihydrate

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Di-μ-chlorido-bis[dichlorido(3,3′,5,5′-tetramethyl-4,4′-bipyrazol-1-ium-κN^2′)copper(II)] dihydrate