[mu]-Terephthalato-bis­[bis(1,10-phenanthroline)copper(I)] diperchlorate

The title compound, [Cu₂(C₈H₄O₄)(C₁₂H₈N₂)₄](ClO₄)₂, was prepared from the hydro­thermal reaction of CuCl₂, 1,4-di­cyano­benzene, 1,10-phenanthroline and water at 443 K. The compound is a dimer in which the cation lies about an inversion center. The terephthalate moiety acts as a bridging ligand and the phenanthrolines as terminal ligands. The unique Cu atom is coordinated by two O and four N atoms in a distorted octahedral geometry, with Cu-O distances of 1.955 (2) and 2.815 (2) Å, and Cu-N distances of 2.008 (2) to 2.216 (2) Å.

Computing details

Data collection: SMART (Siemens, 1994); cell refinement: SMART; data reduction: SMART; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: SHELXL97.

Bis[copper(I)-di-1,10-phenanthroline)]terephthalate bisperchlorate

Crystal data

[Cu2(C8H4O4)(C12H8N2)4](ClO4)2	Dx = 1.625 Mg m^−3
Mr = 1210.91	Melting point: not measured K
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 21.0780 (4) Å	Cell parameters from 6459 reflections
b = 15.0708 (4) Å	θ = 1.7–25.0°
c = 15.9811 (3) Å	µ = 1.05 mm^−1
β = 102.823 (1)°	T = 293 K
V = 4949.98 (19) Å^3	Rectangle, blue
Z = 4	0.3 × 0.25 × 0.2 mm
F(000) = 2464

Data collection

Siemens Smart CCD diffractometer	4337 independent reflections
Radiation source: fine-focus sealed tube	3590 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.022
ω scans	θmax = 25.0°, θmin = 1.7°
Absorption correction: empirical (using intensity measurements) empirical (using intensity measurements) from equivalent reflections (XEMP in SHELXTL; Siemens, 1994)	h = −25→22
Tmin = 0.745, Tmax = 0.818	k = −11→17
9568 measured reflections	l = −19→11

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)] = 0.039	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.106	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0517P)^2 + 6.9792P] where P = (Fo^2 + 2Fc^2)/3
4337 reflections	(Δ/σ)max = 0.001
361 parameters	Δρmax = 0.54 e Å^−3
0 restraints	Δρmin = −0.43 e Å^−3

Special details

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
Cu	0.680262 (16)	0.34580 (2)	0.65914 (2)	0.03530 (13)
N1	0.62443 (12)	0.47160 (16)	0.64272 (16)	0.0409 (6)
N2	0.58937 (11)	0.30010 (16)	0.65442 (15)	0.0378 (5)
N3	0.76488 (11)	0.39913 (15)	0.64647 (14)	0.0363 (5)
N4	0.67278 (11)	0.32028 (15)	0.53091 (14)	0.0327 (5)
O5	0.70553 (11)	0.34571 (14)	0.78450 (13)	0.0471 (5)
O6	0.71800 (13)	0.20095 (17)	0.77030 (14)	0.0649 (7)
C1	0.64252 (17)	0.5549 (2)	0.6379 (2)	0.0542 (8)
H1A	0.6865	0.5670	0.6437	0.065*
C2	0.5989 (2)	0.6254 (2)	0.6246 (3)	0.0688 (11)
H2A	0.6135	0.6831	0.6204	0.083*
C3	0.5347 (2)	0.6085 (3)	0.6179 (3)	0.0761 (12)
H3A	0.5050	0.6550	0.6100	0.091*
C4	0.51305 (17)	0.5207 (2)	0.6230 (3)	0.0609 (9)
C5	0.44648 (19)	0.4957 (3)	0.6153 (3)	0.0834 (14)
H5A	0.4148	0.5397	0.6076	0.100*
C6	0.42847 (18)	0.4103 (3)	0.6190 (3)	0.0781 (12)
H6A	0.3848	0.3965	0.6138	0.094*
C7	0.47558 (16)	0.3408 (2)	0.6306 (2)	0.0528 (8)
C8	0.46011 (17)	0.2507 (3)	0.6320 (2)	0.0618 (9)
H8A	0.4168	0.2332	0.6237	0.074*
C9	0.50778 (18)	0.1886 (2)	0.6454 (2)	0.0575 (9)
H9A	0.4974	0.1286	0.6466	0.069*
C10	0.57212 (16)	0.2152 (2)	0.6572 (2)	0.0480 (8)
H10A	0.6045	0.1722	0.6675	0.058*
C11	0.56036 (14)	0.4538 (2)	0.63503 (19)	0.0421 (7)
C12	0.54158 (14)	0.3629 (2)	0.64021 (18)	0.0397 (7)
C13	0.81211 (15)	0.4344 (2)	0.7061 (2)	0.0477 (7)
H13A	0.8089	0.4321	0.7631	0.057*
C14	0.86648 (16)	0.4750 (2)	0.6861 (2)	0.0578 (9)
H14A	0.8990	0.4982	0.7297	0.069*
C15	0.87192 (15)	0.4807 (2)	0.6033 (2)	0.0508 (8)
H15A	0.9077	0.5085	0.5898	0.061*
C16	0.82309 (14)	0.44438 (18)	0.5384 (2)	0.0396 (7)
C17	0.82428 (16)	0.4451 (2)	0.4490 (2)	0.0481 (8)
H17A	0.8585	0.4728	0.4314	0.058*
C18	0.77685 (16)	0.40634 (19)	0.3902 (2)	0.0449 (7)
H18A	0.7785	0.4091	0.3326	0.054*
C19	0.72389 (14)	0.36100 (17)	0.41421 (18)	0.0358 (6)
C20	0.67540 (15)	0.3138 (2)	0.35692 (18)	0.0422 (7)
H20A	0.6756	0.3115	0.2988	0.051*
C21	0.62802 (15)	0.2713 (2)	0.38759 (19)	0.0425 (7)
H21A	0.5960	0.2393	0.3504	0.051*
C22	0.62776 (14)	0.27613 (19)	0.47474 (18)	0.0382 (6)
H22A	0.5948	0.2473	0.4943	0.046*
C23	0.77063 (13)	0.40385 (17)	0.56310 (17)	0.0328 (6)
C24	0.72068 (13)	0.36150 (17)	0.50109 (17)	0.0319 (6)
C25	0.71892 (14)	0.2678 (2)	0.81511 (18)	0.0411 (7)
C26	0.73523 (12)	0.25939 (18)	0.91110 (16)	0.0330 (6)
C27	0.75253 (15)	0.33273 (19)	0.96350 (18)	0.0395 (7)
H27A	0.7541	0.3886	0.9393	0.047*
C28	0.73255 (15)	0.17707 (19)	0.94855 (18)	0.0403 (7)
H28A	0.7205	0.1276	0.9139	0.048*
Cl	1.04567 (5)	0.37609 (6)	0.60455 (6)	0.0632 (3)
O1	1.0955 (2)	0.3628 (3)	0.5613 (4)	0.159 (2)
O2	0.9880 (2)	0.3467 (3)	0.5537 (3)	0.1428 (18)
O3	1.04204 (14)	0.46793 (18)	0.62343 (19)	0.0790 (8)
O4	1.0575 (4)	0.3264 (3)	0.6798 (3)	0.182 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cu	0.0362 (2)	0.0416 (2)	0.0295 (2)	0.00264 (15)	0.01031 (14)	0.00448 (14)
N1	0.0416 (14)	0.0376 (14)	0.0439 (14)	0.0036 (11)	0.0107 (11)	0.0025 (11)
N2	0.0426 (14)	0.0393 (14)	0.0347 (13)	0.0010 (11)	0.0155 (10)	0.0023 (10)
N3	0.0353 (12)	0.0388 (13)	0.0340 (12)	0.0037 (10)	0.0060 (10)	0.0010 (10)
N4	0.0328 (12)	0.0335 (12)	0.0327 (12)	0.0028 (10)	0.0088 (10)	0.0045 (10)
O5	0.0558 (13)	0.0553 (14)	0.0296 (10)	−0.0005 (10)	0.0082 (9)	0.0069 (10)
O6	0.0955 (19)	0.0639 (16)	0.0333 (12)	0.0197 (14)	0.0099 (12)	−0.0105 (11)
C1	0.0501 (19)	0.0449 (19)	0.067 (2)	−0.0017 (15)	0.0111 (16)	0.0013 (16)
C2	0.068 (3)	0.0396 (19)	0.096 (3)	0.0060 (17)	0.012 (2)	0.0037 (19)
C3	0.065 (3)	0.049 (2)	0.110 (4)	0.0220 (19)	0.010 (2)	0.003 (2)
C4	0.049 (2)	0.054 (2)	0.078 (3)	0.0137 (16)	0.0119 (18)	0.0001 (18)
C5	0.046 (2)	0.071 (3)	0.133 (4)	0.021 (2)	0.019 (2)	0.006 (3)
C6	0.0370 (19)	0.084 (3)	0.115 (4)	0.0066 (19)	0.020 (2)	0.003 (3)
C7	0.0401 (17)	0.061 (2)	0.059 (2)	−0.0029 (15)	0.0144 (15)	0.0007 (16)
C8	0.047 (2)	0.070 (2)	0.070 (2)	−0.0162 (18)	0.0156 (17)	−0.0031 (19)
C9	0.063 (2)	0.051 (2)	0.061 (2)	−0.0156 (18)	0.0196 (18)	−0.0025 (17)
C10	0.0547 (19)	0.0441 (18)	0.0495 (19)	−0.0013 (15)	0.0212 (15)	0.0009 (14)
C11	0.0397 (16)	0.0447 (17)	0.0425 (16)	0.0091 (13)	0.0102 (13)	0.0042 (13)
C12	0.0368 (15)	0.0480 (18)	0.0356 (15)	0.0018 (13)	0.0111 (12)	0.0004 (13)
C13	0.0461 (17)	0.0527 (19)	0.0402 (17)	0.0009 (15)	0.0007 (14)	−0.0006 (14)
C14	0.0483 (19)	0.057 (2)	0.060 (2)	−0.0099 (16)	−0.0064 (16)	−0.0031 (17)
C15	0.0400 (17)	0.0457 (19)	0.066 (2)	−0.0077 (14)	0.0099 (15)	0.0000 (16)
C16	0.0416 (16)	0.0289 (14)	0.0511 (18)	0.0015 (12)	0.0164 (13)	0.0024 (13)
C17	0.0566 (19)	0.0367 (16)	0.060 (2)	−0.0052 (14)	0.0335 (17)	−0.0004 (15)
C18	0.063 (2)	0.0372 (16)	0.0434 (17)	0.0023 (14)	0.0300 (15)	0.0005 (14)
C19	0.0480 (16)	0.0261 (14)	0.0367 (15)	0.0070 (12)	0.0170 (13)	0.0023 (11)
C20	0.0588 (19)	0.0386 (16)	0.0303 (15)	0.0106 (14)	0.0120 (13)	0.0007 (13)
C21	0.0438 (16)	0.0406 (17)	0.0408 (16)	0.0056 (13)	0.0042 (13)	−0.0056 (13)
C22	0.0375 (15)	0.0355 (15)	0.0420 (16)	0.0022 (12)	0.0097 (13)	−0.0005 (12)
C23	0.0370 (14)	0.0278 (14)	0.0352 (15)	0.0059 (11)	0.0111 (11)	0.0018 (11)
C24	0.0356 (14)	0.0276 (14)	0.0340 (14)	0.0065 (11)	0.0108 (11)	0.0027 (11)
C25	0.0401 (16)	0.0528 (19)	0.0315 (15)	0.0059 (13)	0.0104 (12)	0.0016 (14)
C26	0.0327 (14)	0.0398 (16)	0.0271 (13)	0.0004 (11)	0.0078 (11)	−0.0001 (12)
C27	0.0512 (17)	0.0339 (15)	0.0340 (15)	−0.0037 (13)	0.0105 (13)	0.0050 (12)
C28	0.0506 (17)	0.0369 (16)	0.0333 (15)	−0.0039 (13)	0.0086 (13)	−0.0059 (12)
Cl	0.0626 (6)	0.0543 (5)	0.0737 (6)	−0.0197 (4)	0.0173 (5)	−0.0134 (4)
O1	0.114 (3)	0.108 (3)	0.296 (7)	−0.032 (2)	0.132 (4)	−0.058 (3)
O2	0.096 (3)	0.173 (4)	0.157 (4)	−0.074 (3)	0.023 (3)	−0.075 (3)
O3	0.091 (2)	0.0528 (16)	0.088 (2)	−0.0011 (14)	0.0086 (16)	−0.0060 (14)
O4	0.366 (8)	0.067 (2)	0.098 (3)	−0.004 (4)	0.017 (4)	0.010 (2)

Geometric parameters (Å, º)

Cu—O5	1.955 (2)	C8—C9	1.355 (5)
Cu—O6	2.815 (2)	C9—C10	1.386 (5)
Cu—N3	2.007 (2)	C11—C12	1.433 (4)
Cu—N2	2.022 (2)	C13—C14	1.397 (5)
Cu—N4	2.056 (2)	C14—C15	1.356 (5)
Cu—N1	2.216 (2)	C15—C16	1.401 (4)
N1—C1	1.319 (4)	C16—C23	1.395 (4)
N1—C11	1.356 (4)	C16—C17	1.434 (4)
N2—C10	1.334 (4)	C17—C18	1.344 (5)
N2—C12	1.364 (4)	C18—C19	1.432 (4)
N3—C13	1.327 (4)	C19—C24	1.405 (4)
N3—C23	1.366 (3)	C19—C20	1.405 (4)
N4—C22	1.331 (4)	C20—C21	1.366 (4)
N4—C24	1.359 (3)	C21—C22	1.396 (4)
O5—C25	1.280 (4)	C23—C24	1.427 (4)
O6—C25	1.233 (4)	C25—C26	1.501 (4)
C1—C2	1.390 (5)	C26—C28	1.384 (4)
C2—C3	1.358 (6)	C26—C27	1.386 (4)
C3—C4	1.408 (5)	C27—C28^i	1.378 (4)
C4—C11	1.402 (4)	C28—C27^i	1.378 (4)
C4—C5	1.432 (5)	Cl—O2	1.376 (4)
C5—C6	1.346 (6)	Cl—O4	1.391 (4)
C6—C7	1.427 (5)	Cl—O1	1.394 (4)
C7—C8	1.399 (5)	Cl—O3	1.422 (3)
C7—C12	1.405 (4)
O5—Cu—N3	93.30 (9)	C4—C11—C12	119.9 (3)
O5—Cu—N2	94.49 (9)	N2—C12—C7	122.1 (3)
N3—Cu—N2	171.39 (9)	N2—C12—C11	118.0 (3)
O5—Cu—N4	164.59 (9)	C7—C12—C11	119.9 (3)
N3—Cu—N4	81.24 (9)	N3—C13—C14	122.3 (3)
N2—Cu—N4	92.10 (9)	C15—C14—C13	120.1 (3)
O5—Cu—N1	97.97 (9)	C14—C15—C16	119.4 (3)
N3—Cu—N1	96.08 (9)	C23—C16—C15	117.4 (3)
N2—Cu—N1	79.23 (9)	C23—C16—C17	118.4 (3)
N4—Cu—N1	96.93 (9)	C15—C16—C17	124.2 (3)
C1—N1—C11	118.6 (3)	C18—C17—C16	121.3 (3)
C1—N1—Cu	131.9 (2)	C17—C18—C19	121.5 (3)
C11—N1—Cu	109.46 (19)	C24—C19—C20	117.3 (3)
C10—N2—C12	118.3 (3)	C24—C19—C18	118.3 (3)
C10—N2—Cu	126.1 (2)	C20—C19—C18	124.4 (3)
C12—N2—Cu	115.39 (19)	C21—C20—C19	119.2 (3)
C13—N3—C23	117.7 (3)	C20—C21—C22	119.9 (3)
C13—N3—Cu	129.1 (2)	N4—C22—C21	122.6 (3)
C23—N3—Cu	113.10 (18)	N3—C23—C16	123.1 (3)
C22—N4—C24	117.8 (2)	N3—C23—C24	116.3 (2)
C22—N4—Cu	130.64 (19)	C16—C23—C24	120.6 (3)
C24—N4—Cu	111.43 (18)	N4—C24—C19	123.1 (3)
C25—O5—Cu	112.28 (19)	N4—C24—C23	116.9 (2)
N1—C1—C2	123.1 (3)	C19—C24—C23	119.9 (2)
C3—C2—C1	118.9 (4)	O6—C25—O5	123.6 (3)
C2—C3—C4	120.1 (3)	O6—C25—C26	119.7 (3)
C11—C4—C3	117.1 (3)	O5—C25—C26	116.7 (3)
C11—C4—C5	118.4 (3)	C28—C26—C27	119.0 (2)
C3—C4—C5	124.5 (3)	C28—C26—C25	119.7 (2)
C6—C5—C4	121.9 (4)	C27—C26—C25	121.4 (3)
C5—C6—C7	120.8 (4)	C28^i—C27—C26	120.0 (3)
C8—C7—C12	117.2 (3)	C27^i—C28—C26	121.0 (3)
C8—C7—C6	123.9 (3)	O2—Cl—O4	107.7 (4)
C12—C7—C6	118.9 (3)	O2—Cl—O1	108.9 (3)
C9—C8—C7	120.4 (3)	O4—Cl—O1	109.9 (4)
C8—C9—C10	119.3 (3)	O2—Cl—O3	110.9 (3)
N2—C10—C9	122.6 (3)	O4—Cl—O3	110.3 (2)
N1—C11—C4	122.2 (3)	O1—Cl—O3	109.1 (2)
N1—C11—C12	117.8 (3)

Symmetry code: (i) −x+3/2, −y+1/2, −z+2.