catena-Poly­[[bis(μ-1,10-phenanthrolin-2-olato-κ³N,N′:O)­dicopper(I,II)(Cu—Cu)]-μ-chlorocopper(I)-μ-chloro]

In the crystal structure of the title compound, [Cu₃(C₁₂H₇N₂O)₂Cl₂]_n, the mixed-valence Cu^I/Cu^II cation and the cuprate(I) anion both lie on centres of inversion. The O atom of one half of the planar N,N′-chelated dinuclear copper cation binds to the Cu atom of the other half; the geometry around the metal atom is square-planar, owing to the symmetry-related metal atom at a distance of 2.3945 (5) Å. The dinuclear cations are bridged through the anions to form an infinite linear chain.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.032
• wR factor = 0.091
• Data-to-parameter ratio = 15.0

checkCIF/PLATON results

No syntax errors found



Alert level C
ABSTM02_ALERT_3_C  The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
            Tmin and Tmax reported:      0.374     0.585
            Tmin' and Tmax expected:      0.401     0.548
            RR' =      0.875
            Please check that your absorption correction is appropriate.
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.96
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large .............       0.82
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.94

Alert level G
ABSTM02_ALERT_3_G  When printed, the submitted absorption T values will be
            replaced by the scaled T values. Since the ratio of scaled T's
            is identical to the ratio of reported T values, the scaling
            does not imply a change to the absorption corrections used in
            the study.
            Ratio of Tmax expected/reported      0.937
            Tmax scaled      0.548 Tmin scaled      0.351

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

   1 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
   4 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

catena-Poly[[bis(µ-1,10-phenanthrolin-2-olato- κ³N,N':O)dicopper(I,II)(Cu—Cu)]-µ-chloro-copper(I)-µ-chloro]

Crystal data

[Cu3(C12H7N2O)2Cl2]	Z = 1
Mr = 651.91	F(000) = 323
Triclinic, P1	Dx = 1.976 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.0588 (6) Å	Cell parameters from 2232 reflections
b = 8.3638 (6) Å	θ = 2.7–28.1°
c = 10.5690 (8) Å	µ = 3.16 mm^−1
α = 112.301 (1)°	T = 295 K
β = 94.096 (1)°	Block, dark blue
γ = 104.930 (1)°	0.28 × 0.26 × 0.19 mm
V = 547.73 (7) Å^3

Data collection

Bruker APEX area-detector diffractometer	2407 independent reflections
Radiation source: fine-focus sealed tube	2155 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.017
φ and ω scans	θmax = 27.5°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Bruker, 2002)	h = −9→9
Tmin = 0.374, Tmax = 0.585	k = −10→10
4698 measured reflections	l = −13→13

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.091	H-atom parameters constrained
S = 1.01	w = 1/[σ^2(Fo^2) + (0.0614P)^2] where P = (Fo^2 + 2Fc^2)/3
2407 reflections	(Δ/σ)max = 0.001
160 parameters	Δρmax = 0.40 e Å^−3
0 restraints	Δρmin = −0.30 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Cu1	−0.02079 (5)	0.55892 (4)	0.61873 (3)	0.0406 (1)
Cu2	0.5000	0.5000	0.5000	0.0545 (2)
Cl1	0.3858 (1)	0.5625 (1)	0.6850 (1)	0.0594 (2)
O1	0.0716 (3)	0.8031 (2)	0.64009 (16)	0.0449 (4)
N1	0.1318 (3)	0.6921 (3)	0.4204 (2)	0.0364 (4)
N2	0.1079 (3)	0.4013 (3)	0.1938 (2)	0.0405 (4)
C1	0.1404 (3)	0.8331 (3)	0.5396 (2)	0.0379 (5)
C2	0.2247 (3)	1.0136 (3)	0.5498 (2)	0.0437 (6)
C3	0.2929 (4)	1.0435 (3)	0.4422 (3)	0.0453 (5)
C4	0.2833 (3)	0.8939 (3)	0.3153 (3)	0.0409 (5)
C5	0.3542 (4)	0.9094 (4)	0.1959 (3)	0.0515 (6)
C6	0.3433 (4)	0.7608 (4)	0.0800 (3)	0.0502 (6)
C7	0.2610 (3)	0.5826 (4)	0.0734 (3)	0.0433 (5)
C8	0.2450 (4)	0.4200 (4)	−0.0416 (3)	0.0498 (6)
C9	0.1664 (4)	0.2566 (4)	−0.0355 (3)	0.0542 (7)
C10	0.0978 (4)	0.2531 (3)	0.0850 (3)	0.0497 (6)
C11	0.1903 (3)	0.5651 (3)	0.1895 (2)	0.0371 (5)
C12	0.2019 (3)	0.7223 (3)	0.3115 (2)	0.0360 (5)
H2	0.2325	1.1121	0.6321	0.052*
H3	0.3464	1.1618	0.4506	0.054*
H5	0.4090	1.0242	0.1978	0.062*
H6	0.3901	0.7751	0.0037	0.060*
H8	0.2880	0.4241	−0.1218	0.060*
H9	0.1585	0.1490	−0.1102	0.065*
H10	0.0428	0.1412	0.0880	0.060*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cu1	0.0612 (2)	0.0301 (2)	0.0304 (2)	0.0123 (1)	0.0115 (1)	0.0129 (1)
Cu2	0.0685 (3)	0.0440 (3)	0.0514 (3)	0.0093 (2)	0.0137 (2)	0.0249 (2)
Cl1	0.0625 (4)	0.0654 (5)	0.0559 (4)	0.0173 (3)	0.0156 (3)	0.0319 (4)
O1	0.066 (1)	0.033 (1)	0.035 (1)	0.016 (1)	0.013 (1)	0.013 (1)
N1	0.044 (1)	0.030 (1)	0.034 (1)	0.009 (1)	0.005 (1)	0.014 (1)
N2	0.050 (1)	0.037 (1)	0.033 (1)	0.009 (1)	0.010 (1)	0.014 (1)
C1	0.043 (1)	0.033 (1)	0.037 (1)	0.013 (1)	0.005 (1)	0.013 (1)
C2	0.048 (1)	0.031 (1)	0.046 (2)	0.011 (1)	0.005 (1)	0.011 (1)
C3	0.046 (1)	0.033 (1)	0.056 (2)	0.007 (1)	0.009 (1)	0.021 (1)
C4	0.037 (1)	0.040 (1)	0.046 (1)	0.008 (1)	0.007 (1)	0.020 (1)
C5	0.050 (1)	0.051 (2)	0.059 (2)	0.007 (1)	0.011 (1)	0.034 (1)
C6	0.050 (1)	0.061 (2)	0.050 (2)	0.013 (1)	0.020 (1)	0.033 (1)
C7	0.038 (1)	0.054 (1)	0.041 (1)	0.012 (1)	0.009 (1)	0.023 (1)
C8	0.050 (1)	0.063 (2)	0.037 (1)	0.016 (1)	0.017 (1)	0.021 (1)
C9	0.064 (2)	0.053 (2)	0.039 (1)	0.018 (1)	0.016 (1)	0.012 (1)
C10	0.064 (2)	0.038 (1)	0.041 (1)	0.012 (1)	0.014 (1)	0.012 (1)
C11	0.037 (1)	0.039 (1)	0.036 (1)	0.011 (1)	0.007 (1)	0.018 (1)
C12	0.035 (1)	0.038 (1)	0.037 (1)	0.010 (1)	0.005 (1)	0.018 (1)

Geometric parameters (Å, º)

Cu1—Cu1^i	2.3945 (5)	C4—C5	1.429 (3)
Cu1—Cl1	2.8947 (8)	C5—C6	1.354 (4)
Cu1—O1	1.894 (2)	C6—C7	1.426 (3)
Cu1—N1^i	1.908 (2)	C7—C11	1.400 (3)
Cu1—N2^i	2.048 (2)	C7—C8	1.410 (4)
Cu2—Cl1	2.1009 (7)	C8—C9	1.364 (4)
Cu2—Cl1^ii	2.1009 (7)	C9—C10	1.402 (3)
O1—C1	1.281 (3)	C11—C12	1.429 (3)
N1—C1	1.344 (3)	C2—H2	0.93
N1—C12	1.369 (3)	C3—H3	0.93
N2—C10	1.313 (3)	C5—H5	0.93
N2—C11	1.363 (3)	C6—H6	0.93
C1—C2	1.431 (3)	C8—H8	0.93
C2—C3	1.349 (3)	C9—H9	0.93
C3—C4	1.427 (4)	C10—H10	0.93
C4—C12	1.385 (3)
Cl1—Cu1—O1	90.51 (6)	C5—C6—C7	120.9 (2)
Cl1—Cu1—N1^i	93.70 (6)	C11—C7—C8	116.6 (2)
Cl1—Cu1—N2^i	100.65 (6)	C11—C7—C6	118.3 (2)
O1—Cu1—N1^i	173.96 (7)	C8—C7—C6	125.1 (2)
O1—Cu1—N2^i	99.69 (7)	C9—C8—C7	120.1 (2)
N1^i—Cu1—N2^i	83.80 (8)	C8—C9—C10	119.1 (2)
O1—Cu1—Cu1^i	92.97 (5)	N2—C10—C9	122.8 (2)
N1^i—Cu1—Cu1^i	83.07 (6)	N2—C11—C7	123.1 (2)
N2^i—Cu1—Cu1^i	165.92 (6)	N2—C11—C12	116.3 (2)
Cu1^i—Cu1—Cl1	85.27 (2)	C7—C11—C12	120.6 (2)
Cl1—Cu2—Cl1^ii	180	N1—C12—C4	123.6 (2)
Cu2—Cl1—Cu1	107.52 (3)	N1—C12—C11	116.5 (2)
C1—O1—Cu1	117.9 (1)	C4—C12—C11	119.9 (2)
C1—N1—C12	120.1 (2)	C3—C2—H2	119.4
C1—N1—Cu1^i	126.2 (2)	C1—C2—H2	119.4
C12—N1—Cu1^i	113.7 (1)	C2—C3—H3	119.9
C10—N2—C11	118.4 (2)	C4—C3—H3	119.9
C10—N2—Cu1^i	132.0 (2)	C6—C5—H5	119.3
C11—N2—Cu1^i	109.6 (2)	C4—C5—H5	119.3
O1—C1—N1	119.5 (2)	C5—C6—H6	119.6
O1—C1—C2	121.8 (2)	C7—C6—H6	119.6
N1—C1—C2	118.7 (2)	C9—C8—H8	120.0
C3—C2—C1	121.2 (2)	C7—C8—H8	120.0
C2—C3—C4	120.1 (2)	C8—C9—H9	120.5
C12—C4—C5	118.8 (2)	C10—C9—H9	120.5
C12—C4—C3	116.2 (2)	N2—C10—H10	118.6
C5—C4—C3	124.9 (2)	C9—C10—H10	118.6
C6—C5—C4	121.5 (2)
O1—Cu1—Cl1—Cu2	−85.03 (6)	C7—C8—C9—C10	1.6 (4)
N1^i—Cu1—Cl1—Cu2	90.63 (6)	C11—N2—C10—C9	−0.6 (4)
N2^i—Cu1—Cl1—Cu2	175.01 (6)	Cu1^i—N2—C10—C9	179.5 (2)
Cu1^i—Cu1—Cl1—Cu2	7.91 (3)	C8—C9—C10—N2	−0.9 (4)
N2^i—Cu1—O1—C1	179.9 (2)	C10—N2—C11—C7	1.3 (3)
Cu1^i—Cu1—O1—C1	−6.2 (2)	Cu1^i—N2—C11—C7	−178.8 (2)
Cl1—Cu1—O1—C1	79.1 (2)	C10—N2—C11—C12	−178.7 (2)
Cu1—O1—C1—N1	4.7 (3)	Cu1^i—N2—C11—C12	1.2 (2)
Cu1—O1—C1—C2	−176.1 (2)	C8—C7—C11—N2	−0.5 (3)
C12—N1—C1—O1	179.0 (2)	C6—C7—C11—N2	179.6 (2)
Cu1^i—N1—C1—O1	0.9 (3)	C8—C7—C11—C12	179.4 (2)
C12—N1—C1—C2	−0.3 (3)	C6—C7—C11—C12	−0.4 (3)
Cu1^i—N1—C1—C2	−178.4 (2)	C1—N1—C12—C4	−0.3 (3)
O1—C1—C2—C3	−178.6 (2)	Cu1^i—N1—C12—C4	178.1 (2)
N1—C1—C2—C3	0.6 (3)	C1—N1—C12—C11	179.0 (2)
C1—C2—C3—C4	−0.4 (4)	Cu1^i—N1—C12—C11	−2.7 (3)
C2—C3—C4—C12	−0.1 (3)	C5—C4—C12—N1	179.2 (2)
C2—C3—C4—C5	−178.8 (2)	C3—C4—C12—N1	0.5 (3)
C12—C4—C5—C6	0.0 (4)	C5—C4—C12—C11	0.0 (3)
C3—C4—C5—C6	178.7 (2)	C3—C4—C12—C11	−178.7 (2)
C4—C5—C6—C7	−0.3 (4)	N2—C11—C12—N1	0.9 (3)
C5—C6—C7—C11	0.5 (4)	C7—C11—C12—N1	−179.1 (2)
C5—C6—C7—C8	−179.4 (2)	N2—C11—C12—C4	−179.9 (2)
C11—C7—C8—C9	−0.9 (4)	C7—C11—C12—C4	0.2 (3)
C6—C7—C8—C9	178.9 (2)

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