Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803022104/ww6114sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803022104/ww6114Isup2.hkl |
CCDC reference: 226664
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.009 Å
- H-atom completeness 96%
- Disorder in solvent or counterion
- R factor = 0.059
- wR factor = 0.136
- Data-to-parameter ratio = 13.5
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT432_ALERT_2_B Short Inter X...Y Contact O8 .. C73' = 2.76 Ang.
Alert level C PLAT026_ALERT_3_C Ratio Observed / Unique Reflections too Low .... 48 Perc. PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.28 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.67 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.64 Ratio PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C33 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C43 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C63 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C15 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C31 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C45 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C51 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C61 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C72 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl3 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl4 PLAT301_ALERT_3_C Main Residue Disorder ......................... 2.00 Perc. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 46.00 Perc. PLAT331_ALERT_2_C Small Av. Phenyl C-C Dist. C61 - C66 = 1.37 Ang. PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9 PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1 ... ?
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C90 H80 Cl6 Cu2 N6 O8 P4 Atom count from the _atom_site data: C90 H76 Cl6 Cu2 N6 O8 P4 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C90 H80 Cl6 Cu2 N6 O8 P4 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 180.00 180.00 0.00 H 160.00 152.00 8.00 Cl 12.00 12.00 0.00 Cu 4.00 4.00 0.00 N 12.00 12.00 0.00 O 16.00 16.00 0.00 P 8.00 8.00 0.00
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 24 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 15 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 3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SHELXTL (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Cu2(C15H13ClP)4(C30H28N2)](ClO4)2 | F(000) = 1892.0 |
Mr = 1837.28 | Dx = 1.376 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 873 reflections |
a = 13.507 (3) Å | θ = 2.5–23.5° |
b = 18.359 (4) Å | µ = 0.79 mm−1 |
c = 17.968 (4) Å | T = 298 K |
β = 95.409 (5)° | Block, colourless |
V = 4435.7 (15) Å3 | 0.35 × 0.25 × 0.20 mm |
Z = 2 |
Bruker SMART CCD area-detector diffractometer | 7801 independent reflections |
Radiation source: fine-focus sealed tube | 3755 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.084 |
φ and ω scans | θmax = 25.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −16→14 |
Tmin = 0.797, Tmax = 0.858 | k = −21→20 |
18343 measured reflections | l = −18→21 |
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)] = 0.059 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.136 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0451P)2] where P = (Fo2 + 2Fc2)/3 |
7801 reflections | (Δ/σ)max = 0.002 |
578 parameters | Δρmax = 0.73 e Å−3 |
44 restraints | Δρmin = −0.32 e Å−3 |
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 > 2σ(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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cu1 | 0.56194 (4) | 0.10326 (3) | 0.79291 (3) | 0.0551 (2) | |
P1 | 0.54495 (10) | 0.06136 (7) | 0.67462 (7) | 0.0537 (4) | |
P2 | 0.47531 (11) | 0.19685 (7) | 0.83627 (7) | 0.0594 (4) | |
N1 | 0.6770 (3) | 0.0631 (3) | 0.8640 (2) | 0.0572 (12) | |
C1 | 0.6602 (4) | −0.0072 (3) | 0.9010 (3) | 0.0638 (14) | |
H1A | 0.7209 | −0.0218 | 0.9303 | 0.077* | |
H1B | 0.6444 | −0.0442 | 0.8631 | 0.077* | |
C2 | 0.5766 (4) | −0.0028 (2) | 0.9513 (3) | 0.0539 (13) | |
C3 | 0.4797 (4) | −0.0232 (2) | 0.9256 (3) | 0.0535 (13) | |
C4 | 0.4539 (4) | −0.0459 (3) | 0.8501 (3) | 0.0653 (14) | |
H4A | 0.5030 | −0.0470 | 0.8171 | 0.078* | |
C5 | 0.3603 (5) | −0.0657 (3) | 0.8253 (3) | 0.0775 (16) | |
H5A | 0.3458 | −0.0799 | 0.7758 | 0.093* | |
C6 | 0.2841 (4) | −0.0649 (3) | 0.8743 (3) | 0.0788 (17) | |
H6A | 0.2197 | −0.0787 | 0.8572 | 0.095* | |
C7 | 0.3057 (4) | −0.0440 (3) | 0.9463 (3) | 0.0701 (15) | |
H7A | 0.2554 | −0.0445 | 0.9783 | 0.084* | |
C8 | 0.4017 (4) | −0.0214 (3) | 0.9744 (3) | 0.0540 (13) | |
N2 | 0.6283 (3) | −0.0659 (2) | 0.7091 (2) | 0.0689 (12) | |
C11 | 0.6246 (4) | −0.0148 (3) | 0.6550 (3) | 0.0574 (13) | |
C12 | 0.6784 (4) | −0.0221 (3) | 0.5946 (3) | 0.0728 (16) | |
H12A | 0.6764 | 0.0143 | 0.5585 | 0.087* | |
C13 | 0.7358 (4) | −0.0833 (4) | 0.5874 (4) | 0.0879 (19) | |
H13A | 0.7724 | −0.0886 | 0.5464 | 0.105* | |
C14 | 0.7380 (4) | −0.1354 (4) | 0.6403 (4) | 0.093 (2) | |
H14A | 0.7755 | −0.1776 | 0.6371 | 0.111* | |
C15 | 0.6821 (5) | −0.1231 (3) | 0.6994 (3) | 0.0858 (18) | |
Cl1 | 0.6853 (2) | −0.18756 (11) | 0.77109 (12) | 0.1707 (11) | |
C21 | 0.4220 (4) | 0.0264 (3) | 0.6484 (3) | 0.0566 (13) | |
C22 | 0.3405 (4) | 0.0677 (4) | 0.6658 (3) | 0.0871 (18) | |
H22A | 0.3518 | 0.1121 | 0.6900 | 0.104* | |
C23 | 0.2454 (5) | 0.0451 (5) | 0.6485 (4) | 0.109 (2) | |
H23A | 0.1927 | 0.0746 | 0.6594 | 0.130* | |
C24 | 0.2273 (5) | −0.0213 (5) | 0.6149 (4) | 0.101 (2) | |
H24A | 0.1623 | −0.0376 | 0.6041 | 0.121* | |
C25 | 0.3053 (6) | −0.0634 (4) | 0.5976 (3) | 0.0890 (18) | |
H25A | 0.2933 | −0.1084 | 0.5747 | 0.107* | |
C26 | 0.4022 (4) | −0.0393 (3) | 0.6141 (3) | 0.0707 (15) | |
H26A | 0.4547 | −0.0682 | 0.6015 | 0.085* | |
C31 | 0.5662 (4) | 0.1281 (3) | 0.6037 (3) | 0.0578 (13) | |
C32 | 0.6545 (5) | 0.1647 (4) | 0.6102 (3) | 0.107 (2) | |
H32A | 0.7037 | 0.1515 | 0.6475 | 0.128* | |
C33 | 0.6725 (7) | 0.2226 (5) | 0.5609 (4) | 0.130 (3) | |
H33A | 0.7331 | 0.2470 | 0.5656 | 0.155* | |
C35 | 0.5148 (6) | 0.2033 (4) | 0.4982 (4) | 0.105 (2) | |
H35A | 0.4668 | 0.2151 | 0.4596 | 0.126* | |
C36 | 0.4969 (5) | 0.1465 (3) | 0.5454 (3) | 0.0815 (17) | |
H36A | 0.4378 | 0.1204 | 0.5378 | 0.098* | |
C34 | 0.5998 (8) | 0.2421 (4) | 0.5064 (5) | 0.118 (3) | |
H34A | 0.6089 | 0.2816 | 0.4754 | 0.142* | |
N3 | 0.6092 (4) | 0.2210 (2) | 0.9513 (2) | 0.0709 (12) | |
C41 | 0.5115 (5) | 0.2125 (3) | 0.9359 (3) | 0.0615 (14) | |
C42 | 0.4481 (5) | 0.2115 (4) | 0.9903 (3) | 0.100 (2) | |
H42A | 0.3803 | 0.2042 | 0.9788 | 0.120* | |
C43 | 0.4880 (8) | 0.2219 (5) | 1.0639 (4) | 0.130 (3) | |
H43A | 0.4462 | 0.2210 | 1.1022 | 0.156* | |
C44 | 0.5859 (7) | 0.2331 (4) | 1.0804 (4) | 0.111 (2) | |
H44A | 0.6135 | 0.2406 | 1.1292 | 0.133* | |
C45 | 0.6416 (5) | 0.2328 (3) | 1.0223 (4) | 0.0859 (18) | |
Cl2 | 0.76821 (15) | 0.24629 (12) | 1.04098 (11) | 0.1391 (8) | |
C51 | 0.3410 (4) | 0.1923 (3) | 0.8296 (3) | 0.0607 (14) | |
C52 | 0.2954 (5) | 0.1288 (3) | 0.8480 (4) | 0.094 (2) | |
H52A | 0.3347 | 0.0889 | 0.8629 | 0.113* | |
C53 | 0.1948 (6) | 0.1223 (4) | 0.8450 (4) | 0.109 (2) | |
H53A | 0.1665 | 0.0791 | 0.8598 | 0.131* | |
C54 | 0.1362 (6) | 0.1779 (5) | 0.8207 (4) | 0.112 (2) | |
H54A | 0.0675 | 0.1726 | 0.8171 | 0.134* | |
C55 | 0.1769 (5) | 0.2422 (5) | 0.8012 (4) | 0.110 (2) | |
H55A | 0.1360 | 0.2809 | 0.7851 | 0.131* | |
C56 | 0.2796 (5) | 0.2498 (3) | 0.8056 (3) | 0.0901 (18) | |
H56A | 0.3073 | 0.2938 | 0.7923 | 0.108* | |
C61 | 0.4980 (4) | 0.2846 (3) | 0.7934 (3) | 0.0595 (13) | |
C62 | 0.5032 (5) | 0.2860 (3) | 0.7168 (3) | 0.0907 (19) | |
H62A | 0.5020 | 0.2425 | 0.6901 | 0.109* | |
C63 | 0.5102 (6) | 0.3508 (4) | 0.6801 (4) | 0.117 (3) | |
H63A | 0.5128 | 0.3513 | 0.6286 | 0.141* | |
C64 | 0.5133 (5) | 0.4140 (3) | 0.7184 (4) | 0.095 (2) | |
H64A | 0.5178 | 0.4580 | 0.6933 | 0.115* | |
C65 | 0.5099 (5) | 0.4135 (3) | 0.7942 (4) | 0.0919 (19) | |
H65A | 0.5127 | 0.4572 | 0.8204 | 0.110* | |
C66 | 0.5022 (4) | 0.3492 (3) | 0.8316 (3) | 0.0758 (16) | |
H66A | 0.4999 | 0.3494 | 0.8832 | 0.091* | |
C71 | 0.7703 (4) | 0.0595 (3) | 0.8269 (3) | 0.0778 (16) | |
H71A | 0.8223 | 0.0385 | 0.8613 | 0.093* | |
H71B | 0.7604 | 0.0275 | 0.7838 | 0.093* | |
C72 | 0.8031 (5) | 0.1315 (4) | 0.8024 (4) | 0.103 (2) | |
C73 | 0.8536 (12) | 0.1667 (8) | 0.8737 (10) | 0.143 (6) | 0.50 |
H73A | 0.8759 | 0.2147 | 0.8624 | 0.215* | 0.50 |
H73B | 0.9095 | 0.1376 | 0.8926 | 0.215* | 0.50 |
H73C | 0.8070 | 0.1697 | 0.9107 | 0.215* | 0.50 |
C73' | 0.8841 (9) | 0.1223 (8) | 0.7521 (9) | 0.139 (6) | 0.50 |
H73D | 0.8570 | 0.1018 | 0.7054 | 0.209* | 0.50 |
H73E | 0.9342 | 0.0903 | 0.7752 | 0.209* | 0.50 |
H73F | 0.9132 | 0.1689 | 0.7433 | 0.209* | 0.50 |
Cl3 | 0.5000 | 0.5000 | 0.5000 | 0.208 (3) | |
O4 | 0.522 (2) | 0.5655 (10) | 0.532 (2) | 0.37 (2) | 0.50 |
O1 | 0.4203 (7) | 0.4627 (15) | 0.5204 (16) | 0.292 (14) | 0.50 |
O2 | 0.5167 (16) | 0.4938 (15) | 0.4253 (7) | 0.215 (9) | 0.50 |
O3 | 0.5889 (6) | 0.4501 (6) | 0.5330 (5) | 0.135 (4) | 0.50 |
Cl4 | 0.9644 (3) | 0.0733 (2) | 0.5520 (2) | 0.0972 (11) | 0.50 |
O5 | 0.9440 (8) | −0.0040 (5) | 0.5479 (5) | 0.156 (4) | 0.50 |
O6 | 0.8770 (5) | 0.1194 (4) | 0.5304 (5) | 0.108 (3) | 0.50 |
O7 | 1.0453 (8) | 0.0885 (6) | 0.5054 (6) | 0.178 (5) | 0.50 |
O8 | 0.9988 (5) | 0.0971 (4) | 0.6356 (5) | 0.150 (5) | 0.50 |
H1 | 0.677 (3) | 0.093 (2) | 0.897 (3) | 0.059 (17)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0666 (4) | 0.0596 (4) | 0.0392 (3) | −0.0010 (3) | 0.0054 (3) | 0.0008 (3) |
P1 | 0.0624 (8) | 0.0606 (8) | 0.0378 (7) | 0.0045 (7) | 0.0035 (7) | −0.0016 (6) |
P2 | 0.0788 (10) | 0.0577 (9) | 0.0422 (8) | 0.0007 (7) | 0.0082 (7) | −0.0001 (6) |
N1 | 0.058 (3) | 0.069 (3) | 0.044 (3) | −0.010 (2) | 0.007 (2) | 0.000 (3) |
C1 | 0.072 (4) | 0.071 (4) | 0.050 (3) | 0.004 (3) | 0.013 (3) | 0.008 (3) |
C2 | 0.066 (4) | 0.053 (3) | 0.042 (3) | −0.001 (3) | 0.003 (3) | 0.012 (2) |
C3 | 0.065 (3) | 0.050 (3) | 0.045 (3) | −0.004 (3) | 0.002 (3) | 0.008 (2) |
C4 | 0.076 (4) | 0.071 (4) | 0.048 (3) | −0.007 (3) | 0.001 (3) | 0.007 (3) |
C5 | 0.107 (5) | 0.079 (4) | 0.043 (3) | −0.018 (4) | −0.010 (4) | −0.001 (3) |
C6 | 0.082 (4) | 0.085 (4) | 0.066 (4) | −0.022 (3) | −0.012 (4) | 0.014 (3) |
C7 | 0.081 (4) | 0.081 (4) | 0.049 (4) | −0.010 (3) | 0.005 (3) | 0.010 (3) |
C8 | 0.058 (3) | 0.059 (3) | 0.045 (3) | −0.002 (3) | 0.002 (3) | 0.015 (2) |
N2 | 0.090 (3) | 0.064 (3) | 0.054 (3) | 0.018 (3) | 0.014 (2) | 0.000 (2) |
C11 | 0.061 (3) | 0.066 (3) | 0.045 (3) | 0.000 (3) | 0.002 (3) | −0.002 (3) |
C12 | 0.085 (4) | 0.080 (4) | 0.056 (4) | 0.011 (3) | 0.018 (3) | 0.001 (3) |
C13 | 0.090 (5) | 0.099 (5) | 0.080 (5) | 0.012 (4) | 0.034 (4) | −0.012 (4) |
C14 | 0.089 (5) | 0.090 (5) | 0.100 (5) | 0.027 (4) | 0.010 (4) | −0.023 (4) |
C15 | 0.115 (5) | 0.074 (4) | 0.067 (4) | 0.021 (4) | 0.005 (4) | 0.001 (3) |
Cl1 | 0.290 (3) | 0.1068 (15) | 0.1247 (18) | 0.0962 (17) | 0.0704 (19) | 0.0408 (13) |
C21 | 0.062 (3) | 0.070 (4) | 0.037 (3) | −0.002 (3) | 0.007 (3) | −0.003 (3) |
C22 | 0.064 (4) | 0.111 (5) | 0.085 (5) | 0.002 (4) | 0.000 (4) | −0.023 (4) |
C23 | 0.066 (5) | 0.147 (7) | 0.111 (6) | 0.008 (4) | 0.001 (4) | −0.026 (5) |
C24 | 0.066 (5) | 0.153 (7) | 0.082 (5) | −0.027 (5) | 0.004 (4) | −0.007 (5) |
C25 | 0.098 (5) | 0.101 (5) | 0.066 (4) | −0.031 (4) | −0.002 (4) | −0.014 (4) |
C26 | 0.074 (4) | 0.079 (4) | 0.059 (4) | −0.004 (3) | 0.005 (3) | −0.007 (3) |
C31 | 0.072 (4) | 0.063 (3) | 0.039 (3) | 0.001 (3) | 0.006 (3) | 0.000 (2) |
C32 | 0.122 (6) | 0.145 (6) | 0.053 (4) | −0.041 (5) | 0.001 (4) | 0.024 (4) |
C33 | 0.157 (7) | 0.152 (7) | 0.081 (6) | −0.070 (6) | 0.016 (6) | 0.010 (5) |
C35 | 0.128 (6) | 0.114 (6) | 0.074 (5) | 0.030 (5) | 0.008 (5) | 0.038 (4) |
C36 | 0.095 (4) | 0.086 (4) | 0.063 (4) | 0.010 (3) | 0.004 (4) | 0.017 (3) |
C34 | 0.176 (9) | 0.104 (6) | 0.080 (6) | −0.010 (6) | 0.038 (6) | 0.024 (5) |
N3 | 0.095 (4) | 0.071 (3) | 0.045 (3) | −0.011 (3) | −0.002 (3) | 0.004 (2) |
C41 | 0.076 (4) | 0.066 (4) | 0.043 (3) | 0.001 (3) | 0.008 (3) | 0.000 (2) |
C42 | 0.101 (5) | 0.146 (6) | 0.054 (4) | 0.015 (4) | 0.019 (4) | 0.001 (4) |
C43 | 0.155 (8) | 0.195 (9) | 0.043 (5) | 0.023 (7) | 0.030 (5) | 0.003 (5) |
C44 | 0.148 (7) | 0.133 (6) | 0.051 (5) | 0.000 (6) | 0.003 (5) | −0.005 (4) |
C45 | 0.114 (5) | 0.077 (4) | 0.063 (4) | −0.015 (4) | −0.010 (4) | 0.009 (3) |
Cl2 | 0.1477 (17) | 0.1631 (18) | 0.0970 (15) | −0.0625 (14) | −0.0392 (13) | 0.0204 (13) |
C51 | 0.074 (4) | 0.054 (3) | 0.055 (3) | 0.005 (3) | 0.016 (3) | −0.002 (3) |
C52 | 0.081 (5) | 0.073 (5) | 0.132 (6) | 0.000 (4) | 0.028 (4) | 0.009 (4) |
C53 | 0.099 (6) | 0.084 (5) | 0.149 (7) | −0.013 (5) | 0.036 (5) | 0.000 (5) |
C54 | 0.091 (6) | 0.123 (7) | 0.122 (7) | −0.014 (6) | 0.014 (5) | −0.014 (5) |
C55 | 0.074 (5) | 0.122 (7) | 0.131 (7) | 0.020 (5) | 0.001 (4) | 0.009 (5) |
C56 | 0.090 (5) | 0.083 (5) | 0.098 (5) | 0.005 (4) | 0.012 (4) | 0.007 (4) |
C61 | 0.080 (4) | 0.051 (3) | 0.048 (3) | 0.002 (3) | 0.010 (3) | 0.000 (3) |
C62 | 0.156 (6) | 0.065 (4) | 0.055 (4) | −0.002 (4) | 0.029 (4) | 0.000 (3) |
C63 | 0.205 (8) | 0.077 (5) | 0.076 (5) | 0.007 (5) | 0.050 (5) | 0.020 (4) |
C64 | 0.119 (5) | 0.070 (5) | 0.100 (6) | 0.000 (4) | 0.025 (5) | 0.021 (4) |
C65 | 0.128 (5) | 0.057 (4) | 0.089 (5) | −0.007 (3) | 0.004 (4) | −0.003 (4) |
C66 | 0.111 (5) | 0.060 (4) | 0.057 (4) | 0.001 (3) | 0.013 (3) | −0.006 (3) |
C71 | 0.059 (4) | 0.107 (5) | 0.067 (4) | −0.006 (3) | 0.002 (3) | 0.012 (3) |
C72 | 0.104 (5) | 0.111 (5) | 0.094 (5) | −0.042 (4) | 0.017 (4) | 0.011 (4) |
C73 | 0.164 (15) | 0.124 (13) | 0.148 (16) | −0.025 (11) | 0.045 (13) | −0.037 (11) |
C73' | 0.067 (8) | 0.185 (15) | 0.171 (15) | −0.014 (9) | 0.036 (10) | 0.075 (12) |
Cl3 | 0.143 (4) | 0.393 (10) | 0.083 (3) | −0.078 (6) | −0.022 (3) | 0.079 (4) |
O4 | 0.23 (3) | 0.51 (5) | 0.35 (5) | 0.18 (4) | −0.07 (3) | 0.08 (4) |
O1 | 0.059 (8) | 0.58 (4) | 0.24 (2) | −0.048 (15) | 0.042 (12) | 0.18 (2) |
O2 | 0.165 (15) | 0.35 (3) | 0.127 (13) | 0.034 (15) | 0.016 (11) | 0.121 (15) |
O3 | 0.094 (7) | 0.208 (11) | 0.095 (7) | −0.029 (7) | −0.038 (6) | 0.044 (7) |
Cl4 | 0.098 (3) | 0.110 (3) | 0.077 (2) | −0.018 (2) | −0.020 (2) | 0.026 (2) |
O5 | 0.204 (11) | 0.134 (10) | 0.121 (9) | −0.053 (9) | −0.034 (7) | 0.028 (7) |
O6 | 0.074 (5) | 0.100 (6) | 0.133 (8) | −0.014 (5) | −0.071 (5) | −0.024 (5) |
O7 | 0.167 (10) | 0.198 (13) | 0.178 (12) | 0.022 (9) | 0.060 (9) | 0.085 (10) |
O8 | 0.086 (6) | 0.108 (7) | 0.244 (13) | −0.020 (5) | −0.041 (7) | 0.131 (8) |
Cu1—N1 | 2.053 (4) | C34—H34A | 0.9300 |
Cu1—P1 | 2.2517 (14) | N3—C45 | 1.326 (7) |
Cu1—P2 | 2.2583 (15) | N3—C41 | 1.332 (6) |
P1—C21 | 1.801 (5) | C41—C42 | 1.359 (7) |
P1—C31 | 1.810 (5) | C42—C43 | 1.392 (9) |
P1—C11 | 1.818 (5) | C42—H42A | 0.9300 |
P2—C51 | 1.809 (5) | C43—C44 | 1.343 (9) |
P2—C61 | 1.823 (5) | C43—H43A | 0.9300 |
P2—C41 | 1.834 (5) | C44—C45 | 1.343 (8) |
N1—C1 | 1.480 (6) | C44—H44A | 0.9300 |
N1—C71 | 1.481 (6) | C45—Cl2 | 1.729 (7) |
N1—H1 | 0.80 (4) | C51—C52 | 1.372 (7) |
C1—C2 | 1.514 (6) | C51—C56 | 1.387 (7) |
C1—H1A | 0.9700 | C52—C53 | 1.361 (8) |
C1—H1B | 0.9700 | C52—H52A | 0.9300 |
C2—C3 | 1.397 (6) | C53—C54 | 1.340 (9) |
C2—C8i | 1.412 (6) | C53—H53A | 0.9300 |
C3—C4 | 1.431 (6) | C54—C55 | 1.361 (9) |
C3—C8 | 1.432 (6) | C54—H54A | 0.9300 |
C4—C5 | 1.350 (7) | C55—C56 | 1.389 (8) |
C4—H4A | 0.9300 | C55—H55A | 0.9300 |
C5—C6 | 1.417 (7) | C56—H56A | 0.9300 |
C5—H5A | 0.9300 | C61—C66 | 1.370 (6) |
C6—C7 | 1.354 (7) | C61—C62 | 1.386 (6) |
C6—H6A | 0.9300 | C62—C63 | 1.368 (7) |
C7—C8 | 1.409 (6) | C62—H62A | 0.9300 |
C7—H7A | 0.9300 | C63—C64 | 1.348 (8) |
C8—C2i | 1.412 (6) | C63—H63A | 0.9300 |
N2—C15 | 1.299 (6) | C64—C65 | 1.365 (8) |
N2—C11 | 1.348 (6) | C64—H64A | 0.9300 |
C11—C12 | 1.369 (6) | C65—C66 | 1.366 (7) |
C12—C13 | 1.378 (7) | C65—H65A | 0.9300 |
C12—H12A | 0.9300 | C66—H66A | 0.9300 |
C13—C14 | 1.347 (8) | C71—C72 | 1.475 (7) |
C13—H13A | 0.9300 | C71—H71A | 0.9700 |
C14—C15 | 1.379 (8) | C71—H71B | 0.9700 |
C14—H14A | 0.9300 | C72—C73' | 1.493 (13) |
C15—Cl1 | 1.747 (6) | C72—C73 | 1.536 (16) |
C21—C26 | 1.369 (6) | C73—H73A | 0.9600 |
C21—C22 | 1.396 (7) | C73—H73B | 0.9600 |
C22—C23 | 1.358 (7) | C73—H73C | 0.9600 |
C22—H22A | 0.9300 | C73'—H73D | 0.9600 |
C23—C24 | 1.372 (9) | C73'—H73E | 0.9600 |
C23—H23A | 0.9300 | C73'—H73F | 0.9600 |
C24—C25 | 1.366 (8) | Cl3—O4 | 1.352 (13) |
C24—H24A | 0.9300 | Cl3—O4ii | 1.352 (13) |
C25—C26 | 1.387 (7) | Cl3—O1 | 1.354 (10) |
C25—H25A | 0.9300 | Cl3—O2 | 1.387 (12) |
C26—H26A | 0.9300 | Cl3—O3 | 1.580 (9) |
C31—C32 | 1.364 (7) | O4—O1ii | 1.38 (2) |
C31—C36 | 1.380 (7) | O4—O2ii | 1.46 (3) |
C32—C33 | 1.420 (9) | O1—O4ii | 1.38 (2) |
C32—H32A | 0.9300 | O1—O2ii | 1.47 (2) |
C33—C34 | 1.367 (9) | O2—O4ii | 1.46 (3) |
C33—H33A | 0.9300 | O2—O1ii | 1.47 (2) |
C35—C34 | 1.348 (9) | Cl4—O5 | 1.447 (8) |
C35—C36 | 1.379 (8) | Cl4—O7 | 1.466 (8) |
C35—H35A | 0.9300 | Cl4—O6 | 1.475 (7) |
C36—H36A | 0.9300 | Cl4—O8 | 1.591 (9) |
N1—Cu1—P1 | 117.91 (15) | C33—C34—H34A | 120.4 |
N1—Cu1—P2 | 116.44 (15) | C45—N3—C41 | 116.7 (5) |
P1—Cu1—P2 | 125.13 (5) | N3—C41—C42 | 122.1 (5) |
C21—P1—C31 | 105.1 (2) | N3—C41—P2 | 112.9 (4) |
C21—P1—C11 | 102.9 (2) | C42—C41—P2 | 124.9 (5) |
C31—P1—C11 | 104.4 (2) | C41—C42—C43 | 117.9 (6) |
C21—P1—Cu1 | 112.22 (16) | C41—C42—H42A | 121.1 |
C31—P1—Cu1 | 115.10 (17) | C43—C42—H42A | 121.1 |
C11—P1—Cu1 | 115.86 (17) | C44—C43—C42 | 121.0 (7) |
C51—P2—C61 | 102.8 (2) | C44—C43—H43A | 119.5 |
C51—P2—C41 | 104.2 (3) | C42—C43—H43A | 119.5 |
C61—P2—C41 | 103.6 (2) | C45—C44—C43 | 116.1 (7) |
C51—P2—Cu1 | 119.41 (17) | C45—C44—H44A | 121.9 |
C61—P2—Cu1 | 114.40 (16) | C43—C44—H44A | 121.9 |
C41—P2—Cu1 | 110.90 (18) | N3—C45—C44 | 126.1 (6) |
C1—N1—C71 | 109.6 (4) | N3—C45—Cl2 | 116.2 (5) |
C1—N1—Cu1 | 117.0 (3) | C44—C45—Cl2 | 117.7 (6) |
C71—N1—Cu1 | 111.3 (3) | C52—C51—C56 | 116.9 (5) |
C1—N1—H1 | 104 (4) | C52—C51—P2 | 119.6 (5) |
C71—N1—H1 | 115 (3) | C56—C51—P2 | 123.5 (4) |
Cu1—N1—H1 | 99 (4) | C53—C52—C51 | 122.3 (6) |
N1—C1—C2 | 112.1 (4) | C53—C52—H52A | 118.8 |
N1—C1—H1A | 109.2 | C51—C52—H52A | 118.8 |
C2—C1—H1A | 109.2 | C54—C53—C52 | 120.1 (7) |
N1—C1—H1B | 109.2 | C54—C53—H53A | 119.9 |
C2—C1—H1B | 109.2 | C52—C53—H53A | 119.9 |
H1A—C1—H1B | 107.9 | C53—C54—C55 | 120.3 (7) |
C3—C2—C8i | 120.1 (4) | C53—C54—H54A | 119.8 |
C3—C2—C1 | 121.1 (5) | C55—C54—H54A | 119.8 |
C8i—C2—C1 | 118.9 (4) | C54—C55—C56 | 119.9 (7) |
C2—C3—C4 | 121.9 (5) | C54—C55—H55A | 120.1 |
C2—C3—C8 | 120.8 (4) | C56—C55—H55A | 120.1 |
C4—C3—C8 | 117.3 (5) | C51—C56—C55 | 120.4 (6) |
C5—C4—C3 | 121.8 (5) | C51—C56—H56A | 119.8 |
C5—C4—H4A | 119.1 | C55—C56—H56A | 119.8 |
C3—C4—H4A | 119.1 | C66—C61—C62 | 118.6 (5) |
C4—C5—C6 | 120.3 (5) | C66—C61—P2 | 123.7 (4) |
C4—C5—H5A | 119.8 | C62—C61—P2 | 117.5 (4) |
C6—C5—H5A | 119.8 | C63—C62—C61 | 120.4 (5) |
C7—C6—C5 | 119.6 (5) | C63—C62—H62A | 119.8 |
C7—C6—H6A | 120.2 | C61—C62—H62A | 119.8 |
C5—C6—H6A | 120.2 | C64—C63—C62 | 120.3 (6) |
C6—C7—C8 | 122.2 (5) | C64—C63—H63A | 119.9 |
C6—C7—H7A | 118.9 | C62—C63—H63A | 119.9 |
C8—C7—H7A | 118.9 | C63—C64—C65 | 120.0 (6) |
C7—C8—C2i | 122.2 (5) | C63—C64—H64A | 120.0 |
C7—C8—C3 | 118.7 (5) | C65—C64—H64A | 120.0 |
C2i—C8—C3 | 119.1 (4) | C64—C65—C66 | 120.5 (6) |
C15—N2—C11 | 116.7 (4) | C64—C65—H65A | 119.7 |
N2—C11—C12 | 121.1 (5) | C66—C65—H65A | 119.7 |
N2—C11—P1 | 112.2 (4) | C65—C66—C61 | 120.2 (5) |
C12—C11—P1 | 126.7 (4) | C65—C66—H66A | 119.9 |
C11—C12—C13 | 120.0 (5) | C61—C66—H66A | 119.9 |
C11—C12—H12A | 120.0 | C72—C71—N1 | 112.7 (5) |
C13—C12—H12A | 120.0 | C72—C71—H71A | 109.0 |
C14—C13—C12 | 119.2 (6) | N1—C71—H71A | 109.0 |
C14—C13—H13A | 120.4 | C72—C71—H71B | 109.0 |
C12—C13—H13A | 120.4 | N1—C71—H71B | 109.0 |
C13—C14—C15 | 116.7 (6) | H71A—C71—H71B | 107.8 |
C13—C14—H14A | 121.7 | C71—C72—C73' | 109.7 (8) |
C15—C14—H14A | 121.7 | C71—C72—C73 | 104.5 (8) |
N2—C15—C14 | 126.2 (6) | C73'—C72—C73 | 105.0 (9) |
N2—C15—Cl1 | 115.1 (5) | C72—C73—H73A | 109.5 |
C14—C15—Cl1 | 118.7 (5) | C72—C73—H73B | 109.5 |
C26—C21—C22 | 117.0 (5) | H73A—C73—H73B | 109.5 |
C26—C21—P1 | 124.6 (4) | C72—C73—H73C | 109.5 |
C22—C21—P1 | 118.3 (4) | H73A—C73—H73C | 109.5 |
C23—C22—C21 | 122.1 (6) | H73B—C73—H73C | 109.5 |
C23—C22—H22A | 118.9 | C72—C73'—H73D | 109.5 |
C21—C22—H22A | 118.9 | C72—C73'—H73E | 109.5 |
C22—C23—C24 | 119.8 (6) | H73D—C73'—H73E | 109.5 |
C22—C23—H23A | 120.1 | C72—C73'—H73F | 109.5 |
C24—C23—H23A | 120.1 | H73D—C73'—H73F | 109.5 |
C25—C24—C23 | 119.6 (6) | H73E—C73'—H73F | 109.5 |
C25—C24—H24A | 120.2 | O4—Cl3—O4ii | 180.0 (7) |
C23—C24—H24A | 120.2 | O4—Cl3—O1 | 118.7 (11) |
C24—C25—C26 | 120.3 (6) | O4ii—Cl3—O1 | 61.3 (11) |
C24—C25—H25A | 119.9 | O4—Cl3—O2 | 115.7 (11) |
C26—C25—H25A | 119.9 | O4ii—Cl3—O2 | 64.3 (11) |
C21—C26—C25 | 121.1 (5) | O1—Cl3—O2 | 115.2 (9) |
C21—C26—H26A | 119.4 | O4—Cl3—O3 | 103.3 (8) |
C25—C26—H26A | 119.4 | O4ii—Cl3—O3 | 76.7 (8) |
C32—C31—C36 | 118.0 (5) | O1—Cl3—O3 | 101.6 (8) |
C32—C31—P1 | 118.0 (4) | O2—Cl3—O3 | 97.4 (7) |
C36—C31—P1 | 124.0 (4) | Cl3—O4—O1ii | 59.4 (8) |
C31—C32—C33 | 121.0 (7) | Cl3—O4—O2ii | 59.0 (8) |
C31—C32—H32A | 119.5 | O1ii—O4—O2ii | 109.4 (14) |
C33—C32—H32A | 119.5 | Cl3—O1—O4ii | 59.3 (8) |
C34—C33—C32 | 119.2 (7) | Cl3—O1—O2ii | 58.7 (7) |
C34—C33—H33A | 120.4 | O4ii—O1—O2ii | 109.0 (12) |
C32—C33—H33A | 120.4 | Cl3—O2—O4ii | 56.7 (8) |
C34—C35—C36 | 122.0 (7) | Cl3—O2—O1ii | 56.5 (7) |
C34—C35—H35A | 119.0 | O4ii—O2—O1ii | 105.5 (12) |
C36—C35—H35A | 119.0 | O5—Cl4—O7 | 107.9 (6) |
C35—C36—C31 | 120.4 (6) | O5—Cl4—O6 | 113.9 (5) |
C35—C36—H36A | 119.8 | O7—Cl4—O6 | 111.2 (5) |
C31—C36—H36A | 119.8 | O5—Cl4—O8 | 110.8 (5) |
C35—C34—C33 | 119.2 (7) | O7—Cl4—O8 | 108.6 (6) |
C35—C34—H34A | 120.4 | O6—Cl4—O8 | 104.3 (5) |
Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x+1, −y+1, −z+1. |
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