catena-Poly[[[bis­(acetonitrile)(1,10-phenanthroline-κ²N,N′)copper(II)]-μ-perchlorato-κ²O:O′] perchlorate]

In the title complex {[Cu(ClO₄)(C₁₂H₈N₂)(CH₃CN)₂]ClO₄}_n, the Cu cations have an N₄O₂ octa­hedral coordination geometry, being bridged by the perchlorate, chelated by the phenanthroline heterocycles and also coordinated by two acetonitrile ligands. One perchlorate anion acts both as a bridging bis-monodentate ligand between a metal cation and its symmetry equivalents, forming an infinite one-dimensional chain in the b-axis direction, and as a counter-ion to balance the charge.

Key indicators

• Single-crystal X-ray study
• T = 130 K
• Mean [sigma](C-C) = 0.006 Å
• R factor = 0.031
• wR factor = 0.073
• Data-to-parameter ratio = 15.6

checkCIF/PLATON results

No syntax errors found



Alert level C
STRVA01_ALERT_4_C           Flack test results are ambiguous.
           From the CIF: _refine_ls_abs_structure_Flack    0.390
           From the CIF: _refine_ls_abs_structure_Flack_su    0.020
PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero .......       0.39
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.97
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       2.54 Ratio
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        Cl2

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           28.30
           From the CIF: _reflns_number_total               4255
           Count of symmetry unique reflns         2709
           Completeness (_total/calc)            157.07%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      1546
           Fraction of Friedel pairs measured     0.571
           Are heavy atom types Z>Si present        yes

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   6 ALERT level C = Check and explain
   1 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
   5 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: SMART (Bruker, 2001); cell refinement: SAINT-Plus (Bruker, 1999); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97.

catena-Poly[[[bis(acetonitrile)(1,10-phenanthroline- κ²N,N')copper(II)]-µ-perchlorato-κ²O:O'] perchlorate]

Crystal data

[Cu(ClO4)(C12H8N2)(C2H3N)2]ClO4	F(000) = 530
Mr = 524.75	Dx = 1.729 Mg m^−3
Monoclinic, P21	Mo Kα radiation, λ = 0.71073 Å
a = 11.578 (3) Å	Cell parameters from 8096 reflections
b = 6.943 (2) Å	θ = 1.6–28.3°
c = 12.542 (4) Å	µ = 1.40 mm^−1
β = 90.018 (3)°	T = 130 K
V = 1008.2 (5) Å^3	Fragment, light blue
Z = 2	0.37 × 0.35 × 0.31 mm

Data collection

Bruker SMART APEX CCD diffractometer	4255 independent reflections
Radiation source: fine-focus sealed tube	4195 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.051
ω scans	θmax = 28.3°, θmin = 1.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −11→15
Tmin = 0.625, Tmax = 0.670	k = −9→8
6720 measured reflections	l = −16→16

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.031	H-atom parameters constrained
wR(F^2) = 0.073	w = 1/[σ^2(Fo^2) + (0.0511P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.01	(Δ/σ)max < 0.001
4444 reflections	Δρmax = 0.76 e Å^−3
285 parameters	Δρmin = −0.62 e Å^−3
1 restraint	Absolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.39 (2)

Special details

Experimental. The values of Tmin and Tmax are 0.748636 and 1.000000 from SADABS.

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 (Ų)

	x	y	z	Uiso*/Ueq
Cu1	0.77228 (3)	0.46932 (6)	0.28035 (3)	0.01514 (9)
Cl1	0.73197 (7)	0.97776 (16)	0.23489 (5)	0.01578 (14)
O1	0.7563 (3)	0.8176 (4)	0.3057 (2)	0.0276 (7)
O3	0.7433 (2)	0.9184 (4)	0.12494 (19)	0.0246 (6)
O2	0.8158 (2)	1.1291 (4)	0.2568 (2)	0.0219 (6)
O4	0.6169 (2)	1.0494 (4)	0.2546 (2)	0.0242 (6)
N3	0.6574 (3)	0.4364 (5)	0.3962 (2)	0.0190 (7)
N4	0.8924 (2)	0.4680 (7)	0.3946 (2)	0.0205 (6)
N2	0.8834 (3)	0.5048 (5)	0.1587 (2)	0.0155 (7)
N1	0.6557 (2)	0.4773 (6)	0.1640 (2)	0.0154 (6)
C15	0.9381 (3)	0.4555 (7)	0.4745 (3)	0.0184 (7)
C16	0.9967 (4)	0.4458 (9)	0.5768 (3)	0.0268 (10)
H16A	1.0744	0.3929	0.5667	0.040*
H16B	0.9530	0.3625	0.6252	0.040*
H16C	1.0023	0.5754	0.6073	0.040*
C13	0.6087 (4)	0.4208 (7)	0.4727 (3)	0.0263 (10)
C14	0.5447 (5)	0.4026 (9)	0.5751 (4)	0.0408 (14)
H14A	0.5572	0.5183	0.6182	0.061*
H14B	0.5726	0.2894	0.6140	0.061*
H14C	0.4620	0.3879	0.5604	0.061*
C2	0.8274 (3)	0.5133 (5)	0.0638 (3)	0.0161 (8)
C6	0.8856 (4)	0.5366 (6)	−0.0346 (3)	0.0217 (8)
C9	0.6407 (4)	0.5103 (6)	−0.0294 (3)	0.0242 (10)
C4	1.0622 (4)	0.5420 (7)	0.0669 (4)	0.0271 (9)
H4	1.1440	0.5505	0.0707	0.032*
C1	0.7049 (3)	0.4960 (6)	0.0666 (3)	0.0171 (8)
C3	0.9977 (3)	0.5192 (6)	0.1603 (3)	0.0210 (9)
H3	1.0369	0.5139	0.2268	0.025*
C5	1.0080 (4)	0.5522 (7)	−0.0299 (3)	0.0266 (10)
H5	1.0516	0.5695	−0.0934	0.032*
C12	0.5408 (3)	0.4672 (8)	0.1713 (3)	0.0209 (7)
H12	0.5062	0.4518	0.2394	0.025*
C11	0.4699 (3)	0.4788 (10)	0.0805 (3)	0.0282 (8)
H11	0.3883	0.4732	0.0875	0.034*
C7	0.8186 (4)	0.5519 (7)	−0.1291 (3)	0.0313 (10)
H7	0.8562	0.5744	−0.1953	0.038*
C8	0.7022 (4)	0.5350 (7)	−0.1266 (3)	0.0320 (11)
H8	0.6603	0.5397	−0.1917	0.038*
C10	0.5195 (4)	0.4984 (7)	−0.0182 (3)	0.0266 (11)
H10	0.4718	0.5039	−0.0798	0.032*
Cl2	0.25589 (7)	0.44708 (18)	0.36263 (7)	0.02623 (19)
O5	0.3674 (3)	0.3691 (8)	0.3817 (4)	0.0767 (18)
O6	0.2581 (4)	0.5355 (6)	0.2593 (3)	0.0625 (12)
O7	0.2284 (6)	0.5863 (7)	0.4418 (4)	0.092 (2)
O8	0.1703 (3)	0.2997 (6)	0.3659 (3)	0.0505 (10)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cu1	0.01348 (15)	0.01747 (18)	0.01447 (14)	−0.0004 (3)	−0.00207 (14)	0.0010 (2)
Cl1	0.0157 (3)	0.0131 (3)	0.0185 (3)	−0.0008 (5)	−0.0024 (3)	0.0008 (4)
O1	0.042 (2)	0.0128 (13)	0.0279 (12)	−0.0026 (13)	−0.0142 (14)	0.0030 (9)
O3	0.0252 (14)	0.0238 (15)	0.0247 (11)	−0.0007 (10)	−0.0005 (11)	−0.0040 (9)
O2	0.0176 (12)	0.0116 (12)	0.0367 (14)	−0.0026 (10)	−0.0046 (12)	−0.0005 (11)
O4	0.0162 (13)	0.0298 (14)	0.0267 (14)	0.0003 (10)	0.0013 (10)	0.0009 (12)
N3	0.0230 (15)	0.0174 (19)	0.0165 (13)	0.0001 (14)	−0.0001 (11)	0.0010 (13)
N4	0.0183 (13)	0.0204 (16)	0.0228 (13)	−0.004 (2)	−0.0010 (11)	0.002 (2)
N2	0.0171 (14)	0.0103 (17)	0.0193 (14)	−0.0001 (11)	−0.0014 (11)	0.0025 (12)
N1	0.0161 (12)	0.0120 (14)	0.0181 (12)	0.0024 (17)	−0.0016 (9)	−0.0003 (17)
C15	0.0156 (15)	0.0145 (18)	0.0250 (17)	0.0010 (19)	−0.0032 (12)	−0.005 (2)
C16	0.0283 (19)	0.029 (3)	0.0228 (16)	0.007 (2)	−0.0085 (14)	−0.005 (2)
C13	0.029 (2)	0.022 (2)	0.028 (2)	0.0043 (16)	−0.0066 (17)	−0.0006 (15)
C14	0.036 (3)	0.052 (4)	0.034 (2)	0.002 (2)	0.016 (2)	0.004 (2)
C2	0.0216 (18)	0.010 (2)	0.0164 (15)	0.0023 (13)	−0.0002 (13)	0.0016 (12)
C6	0.025 (2)	0.0157 (18)	0.0244 (19)	0.0035 (15)	0.0075 (16)	0.0001 (15)
C9	0.030 (2)	0.020 (2)	0.0224 (18)	0.0007 (16)	−0.0071 (14)	−0.0012 (15)
C4	0.017 (2)	0.020 (2)	0.044 (2)	0.0017 (15)	0.0079 (17)	0.0054 (18)
C1	0.0183 (18)	0.013 (2)	0.0199 (15)	0.0000 (15)	−0.0009 (11)	−0.0003 (14)
C3	0.0200 (18)	0.017 (2)	0.0259 (18)	0.0012 (13)	−0.0007 (14)	0.0000 (14)
C5	0.035 (3)	0.017 (2)	0.027 (2)	0.0074 (18)	0.0129 (18)	0.0054 (16)
C12	0.0204 (16)	0.0176 (18)	0.0249 (15)	−0.005 (2)	−0.0013 (12)	0.001 (2)
C11	0.0166 (17)	0.028 (2)	0.0401 (19)	−0.001 (3)	−0.0098 (14)	0.003 (3)
C7	0.050 (3)	0.027 (2)	0.0167 (18)	0.004 (2)	0.0040 (19)	0.0012 (16)
C8	0.044 (3)	0.033 (2)	0.0189 (18)	0.0044 (18)	−0.0117 (17)	0.0023 (16)
C10	0.028 (2)	0.026 (3)	0.0258 (19)	0.0006 (19)	−0.0133 (16)	0.0046 (18)
Cl2	0.0171 (4)	0.0312 (5)	0.0303 (3)	−0.0029 (5)	−0.0017 (3)	−0.0016 (4)
O5	0.0216 (18)	0.119 (5)	0.090 (4)	0.015 (2)	0.000 (2)	0.051 (3)
O6	0.041 (2)	0.095 (3)	0.0512 (18)	−0.004 (2)	−0.0016 (17)	0.031 (2)
O7	0.123 (5)	0.061 (3)	0.092 (3)	−0.050 (3)	0.060 (4)	−0.044 (3)
O8	0.048 (2)	0.054 (2)	0.049 (2)	−0.0260 (18)	0.0132 (18)	−0.0143 (19)

Geometric parameters (Å, º)

Cu1—N1	1.989 (3)	C2—C6	1.414 (5)
Cu1—N3	1.983 (3)	C2—C1	1.424 (5)
Cu1—N4	1.997 (3)	C6—C5	1.423 (7)
Cu1—N2	2.010 (3)	C6—C7	1.421 (6)
Cu1—O2^i	2.433 (3)	C9—C10	1.412 (6)
Cl1—O3	1.445 (2)	C9—C1	1.419 (5)
Cl1—O4	1.443 (3)	C9—C8	1.422 (6)
Cl1—O1	1.451 (3)	C4—C5	1.369 (6)
Cl1—O2	1.457 (3)	C4—C3	1.398 (6)
O2—Cu1^ii	2.433 (3)	C4—H4	0.9500
N3—C13	1.118 (5)	C3—H3	0.9500
N4—C15	1.136 (5)	C5—H5	0.9500
N2—C3	1.328 (5)	C12—C11	1.406 (5)
N2—C2	1.357 (5)	C12—H12	0.9500
N1—C12	1.335 (4)	C11—C10	1.372 (6)
N1—C1	1.354 (4)	C11—H11	0.9500
C15—C16	1.452 (5)	C7—C8	1.353 (7)
C16—H16A	0.9800	C7—H7	0.9500
C16—H16B	0.9800	C8—H8	0.9500
C16—H16C	0.9800	C10—H10	0.9500
C13—C14	1.489 (6)	Cl2—O5	1.420 (4)
C14—H14A	0.9800	Cl2—O8	1.425 (4)
C14—H14B	0.9800	Cl2—O6	1.435 (3)
C14—H14C	0.9800	Cl2—O7	1.422 (4)
N1—Cu1—N3	94.89 (11)	C6—C2—C1	120.4 (4)
N1—Cu1—N4	178.08 (17)	C2—C6—C5	116.6 (4)
N3—Cu1—N4	86.62 (11)	C2—C6—C7	118.5 (4)
N1—Cu1—N2	82.77 (11)	C5—C6—C7	124.9 (4)
N3—Cu1—N2	177.63 (13)	C10—C9—C1	115.5 (4)
N4—Cu1—N2	95.71 (12)	C10—C9—C8	126.2 (4)
N1—Cu1—O2^i	94.51 (13)	C1—C9—C8	118.3 (4)
N3—Cu1—O2^i	96.65 (13)	C5—C4—C3	120.3 (4)
N4—Cu1—O2^i	86.47 (14)	C5—C4—H4	119.9
N2—Cu1—O2^i	83.93 (12)	C3—C4—H4	119.9
O3—Cl1—O4	110.20 (16)	N1—C1—C2	116.8 (3)
O3—Cl1—O1	110.40 (17)	N1—C1—C9	123.5 (3)
O4—Cl1—O1	109.78 (18)	C2—C1—C9	119.6 (4)
O3—Cl1—O2	108.98 (17)	N2—C3—C4	121.9 (4)
O4—Cl1—O2	109.51 (19)	N2—C3—H3	119.0
O1—Cl1—O2	107.93 (16)	C4—C3—H3	119.0
Cl1—O2—Cu1^ii	125.81 (16)	C4—C5—C6	119.3 (4)
C13—N3—Cu1	168.0 (3)	C4—C5—H5	120.4
C15—N4—Cu1	163.2 (3)	C6—C5—H5	120.4
C3—N2—C2	119.0 (3)	N1—C12—C11	121.5 (3)
C3—N2—Cu1	129.5 (3)	N1—C12—H12	119.2
C2—N2—Cu1	111.5 (2)	C11—C12—H12	119.2
C12—N1—C1	119.1 (3)	C10—C11—C12	119.5 (3)
C12—N1—Cu1	128.6 (2)	C10—C11—H11	120.3
C1—N1—Cu1	112.3 (2)	C12—C11—H11	120.3
N4—C15—C16	178.3 (5)	C8—C7—C6	121.2 (4)
C15—C16—H16A	109.5	C8—C7—H7	119.4
C15—C16—H16B	109.5	C6—C7—H7	119.4
H16A—C16—H16B	109.5	C7—C8—C9	121.9 (4)
C15—C16—H16C	109.5	C7—C8—H8	119.0
H16A—C16—H16C	109.5	C9—C8—H8	119.0
H16B—C16—H16C	109.5	C11—C10—C9	120.8 (3)
N3—C13—C14	179.2 (5)	C11—C10—H10	119.6
C13—C14—H14A	109.5	C9—C10—H10	119.6
C13—C14—H14B	109.5	O5—Cl2—O8	110.7 (3)
H14A—C14—H14B	109.5	O5—Cl2—O6	107.4 (3)
C13—C14—H14C	109.5	O8—Cl2—O6	110.2 (2)
H14A—C14—H14C	109.5	O5—Cl2—O7	110.2 (4)
H14B—C14—H14C	109.5	O8—Cl2—O7	108.2 (3)
N2—C2—C6	122.9 (4)	O6—Cl2—O7	110.1 (3)
N2—C2—C1	116.7 (3)

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