Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806049750/cv2148sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806049750/cv2148Isup2.hkl |
CCDC reference: 619832
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- R factor = 0.035
- wR factor = 0.094
- Data-to-parameter ratio = 18.7
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 3 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cu1 - Cl1 .. 7.41 su
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2006).
[Cu2Cl2(C16H13N2P)2] | F(000) = 736 |
Mr = 726.49 | Dx = 1.519 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 3120 reflections |
a = 9.305 (1) Å | θ = 2.3–26.0° |
b = 10.857 (1) Å | µ = 1.64 mm−1 |
c = 15.746 (2) Å | T = 293 K |
β = 93.033 (1)° | Block, yellow |
V = 1588.5 (3) Å3 | 0.34 × 0.14 × 0.10 mm |
Z = 2 |
Bruker APEX area-detector diffractometer | 3548 independent reflections |
Radiation source: fine-focus sealed tube | 2901 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
φ and ω scans | θmax = 27.5°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −12→11 |
Tmin = 0.760, Tmax = 0.849 | k = −14→12 |
9241 measured reflections | l = −17→20 |
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.094 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0513P)2 + 0.1517P] where P = (Fo2 + 2Fc2)/3 |
3548 reflections | (Δ/σ)max = 0.001 |
190 parameters | Δρmax = 0.44 e Å−3 |
0 restraints | Δρmin = −0.24 e Å−3 |
Experimental. CH&N elemental analysis. Calculated for C32H26N4P2Cl2Cu2: C 52.91, H 3.61, N 7.71%. Found: C 53.20, H 3.66, N 7.61%. |
x | y | z | Uiso*/Ueq | ||
Cu1 | 0.58631 (3) | 0.34424 (2) | 0.50471 (2) | 0.0328 (1) | |
Cl1 | 0.69581 (7) | 0.15323 (5) | 0.51186 (4) | 0.0376 (2) | |
P1 | 0.36520 (7) | 0.52998 (5) | 0.59746 (4) | 0.0308 (2) | |
N1 | 0.3716 (2) | 0.3057 (2) | 0.5191 (1) | 0.0328 (4) | |
N2 | 0.6208 (2) | 0.4115 (2) | 0.6268 (1) | 0.0327 (4) | |
C1 | 0.2869 (2) | 0.3813 (2) | 0.5618 (1) | 0.0318 (5) | |
C2 | 0.1432 (3) | 0.3537 (2) | 0.5721 (2) | 0.0483 (7) | |
C3 | 0.0864 (3) | 0.2448 (3) | 0.5386 (2) | 0.0571 (8) | |
C4 | 0.1743 (3) | 0.1664 (3) | 0.4975 (2) | 0.0531 (7) | |
C5 | 0.3150 (3) | 0.1991 (2) | 0.4889 (2) | 0.0442 (6) | |
C6 | 0.5297 (2) | 0.4895 (2) | 0.6619 (1) | 0.0311 (5) | |
C7 | 0.5637 (3) | 0.5455 (3) | 0.7401 (2) | 0.0450 (6) | |
C8 | 0.6908 (3) | 0.5163 (3) | 0.7840 (2) | 0.0541 (8) | |
C9 | 0.7802 (3) | 0.4313 (3) | 0.7498 (2) | 0.0555 (8) | |
C10 | 0.7428 (3) | 0.3818 (3) | 0.6719 (2) | 0.0439 (6) | |
C11 | 0.2416 (3) | 0.5753 (2) | 0.6775 (1) | 0.0335 (5) | |
C12 | 0.1556 (3) | 0.6772 (2) | 0.6629 (2) | 0.0410 (6) | |
C13 | 0.0562 (3) | 0.7095 (2) | 0.7222 (2) | 0.0496 (7) | |
C14 | 0.0461 (3) | 0.6444 (2) | 0.7955 (2) | 0.0490 (7) | |
C15 | 0.1313 (3) | 0.5436 (3) | 0.8107 (2) | 0.0477 (7) | |
C16 | 0.2278 (3) | 0.5069 (2) | 0.7519 (2) | 0.0432 (6) | |
H2 | 0.0855 | 0.4077 | 0.6010 | 0.058* | |
H3 | −0.0100 | 0.2254 | 0.5440 | 0.069* | |
H4 | 0.1391 | 0.0920 | 0.4757 | 0.064* | |
H5 | 0.3742 | 0.1453 | 0.4608 | 0.053* | |
H7 | 0.5009 | 0.6022 | 0.7624 | 0.054* | |
H8 | 0.7157 | 0.5535 | 0.8359 | 0.065* | |
H9 | 0.8651 | 0.4077 | 0.7792 | 0.067* | |
H10 | 0.8046 | 0.3249 | 0.6489 | 0.053* | |
H12 | 0.1638 | 0.7240 | 0.6140 | 0.049* | |
H13 | −0.0042 | 0.7767 | 0.7115 | 0.060* | |
H14 | −0.0189 | 0.6685 | 0.8352 | 0.059* | |
H15 | 0.1245 | 0.4995 | 0.8610 | 0.057* | |
H16 | 0.2835 | 0.4368 | 0.7618 | 0.052* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0392 (2) | 0.0305 (2) | 0.0297 (2) | 0.0043 (1) | 0.0101 (1) | 0.0020 (1) |
Cl1 | 0.0450 (4) | 0.0299 (3) | 0.0385 (3) | 0.0087 (2) | 0.0069 (3) | 0.0034 (2) |
P1 | 0.0376 (3) | 0.0271 (3) | 0.0287 (3) | 0.0043 (2) | 0.0115 (2) | 0.0002 (2) |
N1 | 0.035 (1) | 0.033 (1) | 0.031 (1) | 0.003 (1) | 0.004 (1) | −0.002 (1) |
N2 | 0.033 (1) | 0.032 (1) | 0.033 (1) | −0.003 (1) | 0.006 (1) | −0.002 (1) |
C1 | 0.034 (1) | 0.032 (1) | 0.030 (1) | 0.004 (1) | 0.004 (1) | 0.002 (1) |
C2 | 0.036 (2) | 0.052 (2) | 0.058 (2) | 0.003 (1) | 0.010 (1) | −0.013 (1) |
C3 | 0.035 (2) | 0.061 (2) | 0.076 (2) | −0.010 (1) | 0.004 (13) | −0.014 (2) |
C4 | 0.048 (2) | 0.047 (2) | 0.065 (2) | −0.008 (1) | 0.000 (1) | −0.014 (1) |
C5 | 0.046 (2) | 0.039 (1) | 0.048 (2) | 0.003 (1) | 0.001 (12) | −0.010 (1) |
C6 | 0.036 (1) | 0.027 (1) | 0.031 (1) | −0.006 (1) | 0.008 (1) | 0.000 (1) |
C7 | 0.050 (2) | 0.041 (1) | 0.044 (2) | −0.007 (1) | 0.008 (1) | −0.012 (1) |
C8 | 0.059 (2) | 0.064 (2) | 0.040 (2) | −0.019 (2) | −0.002 (1) | −0.017 (1) |
C9 | 0.044 (2) | 0.069 (2) | 0.052 (2) | −0.011 (2) | −0.012 (1) | −0.007 (2) |
C10 | 0.034 (1) | 0.049 (2) | 0.049 (2) | −0.001 (1) | 0.001 (1) | −0.003 (1) |
C11 | 0.038 (1) | 0.031 (1) | 0.032 (1) | 0.003 (1) | 0.012 (1) | −0.004 (1) |
C12 | 0.047 (2) | 0.035 (1) | 0.042 (1) | 0.005 (1) | 0.015 (1) | 0.001 (1) |
C13 | 0.048 (2) | 0.037 (1) | 0.066 (2) | 0.008 (1) | 0.021 (1) | −0.007 (1) |
C14 | 0.049 (2) | 0.052 (2) | 0.049 (2) | −0.008 (1) | 0.024 (1) | −0.019 (1) |
C15 | 0.050 (2) | 0.060 (2) | 0.035 (1) | −0.006 (1) | 0.016 (1) | 0.001 (1) |
C16 | 0.047 (2) | 0.044 (2) | 0.040 (1) | 0.004 (1) | 0.013 (1) | 0.005 (1) |
Cu1—N1 | 2.065 (2) | C11—C12 | 1.377 (3) |
Cu1—N2 | 2.066 (2) | C11—C16 | 1.399 (3) |
Cu1—P1i | 2.1757 (7) | C12—C13 | 1.394 (4) |
Cu1—Cl1 | 2.3107 (6) | C13—C14 | 1.361 (4) |
P1—C11 | 1.818 (2) | C14—C15 | 1.365 (4) |
P1—C6 | 1.844 (2) | C15—C16 | 1.382 (3) |
P1—C1 | 1.847 (2) | C2—H2 | 0.93 |
N1—C1 | 1.343 (3) | C3—H3 | 0.93 |
N1—C5 | 1.348 (3) | C4—H4 | 0.93 |
N2—C6 | 1.338 (3) | C5—H5 | 0.93 |
N2—C10 | 1.345 (3) | C7—H7 | 0.93 |
C1—C2 | 1.388 (4) | C8—H8 | 0.93 |
C2—C3 | 1.388 (4) | C9—H9 | 0.93 |
C3—C4 | 1.366 (4) | C10—H10 | 0.93 |
C4—C5 | 1.371 (4) | C12—H12 | 0.93 |
C6—C7 | 1.396 (3) | C13—H13 | 0.93 |
C7—C8 | 1.375 (4) | C14—H14 | 0.93 |
C8—C9 | 1.371 (4) | C15—H15 | 0.93 |
C9—C10 | 1.368 (4) | C16—H16 | 0.93 |
N1—Cu1—N2 | 94.18 (7) | C12—C11—P1 | 119.1 (2) |
N1—Cu1—P1i | 116.63 (6) | C16—C11—P1 | 121.8 (2) |
N1—Cu1—Cl1 | 103.84 (6) | C11—C12—C13 | 119.5 (2) |
N2—Cu1—P1i | 115.99 (6) | C14—C13—C12 | 121.0 (3) |
N2—Cu1—Cl1 | 103.04 (6) | C13—C14—C15 | 120.0 (2) |
P1i—Cu1—Cl1 | 119.42 (3) | C14—C15—C16 | 120.3 (3) |
C11—P1—C6 | 102.7 (1) | C15—C16—C11 | 120.0 (2) |
C11—P1—C1 | 101.1 (1) | C3—C2—H2 | 120.4 |
C6—P1—C1 | 105.2 (1) | C1—C2—H2 | 120.4 |
C11—P1—Cu1i | 120.41 (8) | C4—C3—H3 | 120.5 |
C6—P1—Cu1i | 110.95 (7) | C2—C3—H3 | 120.5 |
C1—P1—Cu1i | 114.72 (8) | C5—C4—H4 | 120.5 |
C1—N1—C5 | 118.2 (2) | C3—C4—H4 | 120.5 |
C1—N1—Cu1 | 121.9 (2) | N1—C5—H5 | 118.5 |
C5—N1—Cu1 | 119.8 (2) | C4—C5—H5 | 118.5 |
C6—N2—C10 | 118.0 (2) | C8—C7—H7 | 120.3 |
C6—N2—Cu1 | 122.5 (2) | C6—C7—H7 | 120.3 |
C10—N2—Cu1 | 119.4 (2) | C9—C8—H8 | 120.6 |
N1—C1—C2 | 121.4 (2) | C7—C8—H8 | 120.6 |
N1—C1—P1 | 117.0 (2) | C8—C9—H9 | 120.5 |
C2—C1—P1 | 121.4 (2) | C10—C9—H9 | 120.5 |
C3—C2—C1 | 119.3 (3) | N2—C10—H10 | 118.4 |
C4—C3—C2 | 119.1 (3) | C9—C10—H10 | 118.4 |
C5—C4—C3 | 118.9 (3) | C11—C12—H12 | 120.3 |
N1—C5—C4 | 123.0 (3) | C13—C12—H12 | 120.3 |
N2—C6—C7 | 121.4 (2) | C14—C13—H13 | 119.5 |
N2—C6—P1 | 116.7 (2) | C12—C13—H13 | 119.5 |
C7—C6—P1 | 121.7 (2) | C13—C14—H14 | 120.0 |
C8—C7—C6 | 119.5 (3) | C15—C14—H14 | 120.0 |
C9—C8—C7 | 118.8 (2) | C14—C15—H15 | 119.8 |
C8—C9—C10 | 119.0 (3) | C16—C15—H15 | 119.8 |
N2—C10—C9 | 123.1 (3) | C15—C16—H16 | 120.0 |
C12—C11—C16 | 119.1 (2) | C11—C16—H16 | 120.0 |
N2—Cu1—N1—C1 | 39.4 (2) | Cu1—N2—C6—C7 | −172.0 (2) |
P1i—Cu1—N1—C1 | −82.5 (2) | C10—N2—C6—P1 | 179.0 (2) |
Cl1—Cu1—N1—C1 | 144.0 (2) | Cu1—N2—C6—P1 | 2.6 (2) |
N2—Cu1—N1—C5 | −137.2 (2) | C11—P1—C6—N2 | 156.0 (2) |
P1i—Cu1—N1—C5 | 100.9 (2) | C1—P1—C6—N2 | 50.6 (2) |
Cl1—Cu1—N1—C5 | −32.7 (2) | Cu1i—P1—C6—N2 | −74.0 (2) |
N1—Cu1—N2—C6 | −45.1 (2) | C11—P1—C6—C7 | −29.4 (2) |
P1i—Cu1—N2—C6 | 77.3 (2) | C1—P1—C6—C7 | −134.9 (2) |
Cl1—Cu1—N2—C6 | −150.4 (2) | Cu1i—P1—C6—C7 | 100.6 (2) |
N1—Cu1—N2—C10 | 138.6 (2) | N2—C6—C7—C8 | −2.7 (4) |
P1i—Cu1—N2—C10 | −99.1 (2) | P1—C6—C7—C8 | −177.1 (2) |
Cl1—Cu1—N2—C10 | 33.3 (2) | C6—C7—C8—C9 | −0.8 (4) |
C5—N1—C1—C2 | −2.5 (3) | C7—C8—C9—C10 | 2.4 (5) |
Cu1—N1—C1—C2 | −179.2 (2) | C6—N2—C10—C9 | −2.8 (4) |
C5—N1—C1—P1 | −176.9 (2) | Cu1—N2—C10—C9 | 173.7 (2) |
Cu1—N1—C1—P1 | 6.4 (2) | C8—C9—C10—N2 | −0.7 (5) |
C11—P1—C1—N1 | −162.6 (2) | C6—P1—C11—C12 | 138.0 (2) |
C6—P1—C1—N1 | −56.0 (2) | C1—P1—C11—C12 | −113.5 (2) |
Cu1i—P1—C1—N1 | 66.2 (2) | Cu1i—P1—C11—C12 | 14.1 (2) |
C11—P1—C1—C2 | 23.0 (2) | C6—P1—C11—C16 | −44.4 (2) |
C6—P1—C1—C2 | 129.6 (2) | C1—P1—C11—C16 | 64.2 (2) |
Cu1i—P1—C1—C2 | −108.2 (2) | Cu1i—P1—C11—C16 | −168.3 (2) |
N1—C1—C2—C3 | 1.0 (4) | C16—C11—C12—C13 | −0.4 (4) |
P1—C1—C2—C3 | 175.2 (2) | P1—C11—C12—C13 | 177.3 (2) |
C1—C2—C3—C4 | 1.0 (5) | C11—C12—C13—C14 | 2.2 (4) |
C2—C3—C4—C5 | −1.5 (5) | C12—C13—C14—C15 | −1.8 (4) |
C1—N1—C5—C4 | 2.0 (4) | C13—C14—C15—C16 | −0.3 (4) |
Cu1—N1—C5—C4 | 178.8 (2) | C14—C15—C16—C11 | 2.0 (4) |
C3—C4—C5—N1 | 0.0 (5) | C12—C11—C16—C15 | −1.6 (4) |
C10—N2—C6—C7 | 4.4 (3) | P1—C11—C16—C15 | −179.2 (2) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
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