Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803027752/ac6072sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803027752/ac6072Isup2.hkl |
CCDC reference: 231832
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.006 Å
- R factor = 0.034
- wR factor = 0.077
- Data-to-parameter ratio = 18.3
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT213_ALERT_2_A Atom C41B has ADP max/min Ratio ............. 6.00 oblate
Alert level B PLAT061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.71 PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.93 Ratio PLAT241_ALERT_2_B Check High U(eq) as Compared to Neighbors .... C3AB
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.232 0.400 Tmin' and Tmax expected: 0.299 0.400 RR' = 0.776 Please check that your absorption correction is appropriate. SHFSU01_ALERT_2_C The absolute value of parameter shift to su ratio > 0.05 Absolute value of the parameter shift to su ratio given 0.052 Additional refinement cycles may be required. PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT213_ALERT_2_C Atom C12A has ADP max/min Ratio ............. 3.30 oblate PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.25 Ratio PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... N1A PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... N4A PLAT301_ALERT_3_C Main Residue Disorder ......................... 20.00 Perc. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 16 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 15.70 Deg. C12B -N1A -C11A 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 9.10 Deg. C11B -N1A -C12A 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 31.70 Deg. C2AA -N1A -C2AB 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 16.20 Deg. C42A -N4A -C42B 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 10.80 Deg. C41A -N4A -C41B 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 28.90 Deg. C3AB -N4A -C3AA 1.555 1.555 1.555
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 28.35 From the CIF: _reflns_number_total 5275 Count of symmetry unique reflns 2845 Completeness (_total/calc) 185.41% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 2430 Fraction of Friedel pairs measured 0.854 Are heavy atom types Z>Si present yes
1 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 15 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 13 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, 2001); cell refinement: SMART; data reduction: SAINT (Sheldrick, 1999); program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Cu3Cl5(C6H16N2)(C6H13N2)] | Dx = 1.823 Mg m−3 |
Mr = 597.26 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pca21 | Cell parameters from 6021 reflections |
a = 15.5111 (14) Å | θ = 2.6–28.3° |
b = 11.0313 (9) Å | µ = 3.52 mm−1 |
c = 12.7192 (12) Å | T = 293 K |
V = 2176.4 (3) Å3 | Irregular block, blue |
Z = 4 | 0.33 × 0.31 × 0.26 mm |
F(000) = 1204 |
CCD area detector diffractometer | 5275 independent reflections |
Radiation source: fine-focus sealed tube | 4598 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
phi and ω scans | θmax = 28.4°, θmin = 2.3° |
Absorption correction: multi-scan (Sheldrick, 1999) | h = −20→20 |
Tmin = 0.232, Tmax = 0.400 | k = −14→13 |
18409 measured reflections | l = −16→16 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.034 | H-atom parameters constrained |
wR(F2) = 0.077 | w = 1/[σ2(Fo2) + (0.0379P)2 + 0.3117P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.052 |
5275 reflections | Δρmax = 0.54 e Å−3 |
288 parameters | Δρmin = −0.27 e Å−3 |
15 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.017 (12) |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cu1 | 0.62357 (2) | 0.07008 (3) | 0.92580 (3) | 0.02979 (7) | |
Cu2 | 0.65647 (3) | 0.32725 (4) | 1.07471 (4) | 0.04394 (10) | |
Cu3 | 0.45850 (3) | 0.28353 (5) | 0.96767 (4) | 0.05975 (13) | |
Cl1 | 0.57821 (5) | 0.14248 (7) | 1.09129 (6) | 0.04402 (19) | |
Cl2 | 0.72776 (5) | 0.21749 (7) | 0.92582 (8) | 0.0500 (2) | |
Cl3 | 0.50657 (6) | 0.18489 (8) | 0.82119 (7) | 0.0473 (2) | |
Cl4 | 0.54790 (5) | 0.45402 (7) | 0.99835 (7) | 0.0474 (2) | |
Cl5 | 0.32628 (6) | 0.28503 (9) | 1.03141 (8) | 0.0532 (2) | |
N1A | 0.68079 (12) | −0.01642 (19) | 0.79921 (18) | 0.0409 (7) | |
C11A | 0.6836 (5) | 0.0622 (5) | 0.7057 (3) | 0.0513 (18) | 0.645 (5) |
H11A | 0.7005 | 0.0152 | 0.6456 | 0.077* | 0.645 (5) |
H11B | 0.7246 | 0.1261 | 0.7169 | 0.077* | 0.645 (5) |
H11C | 0.6276 | 0.0965 | 0.6938 | 0.077* | 0.645 (5) |
C12A | 0.7699 (2) | −0.0539 (6) | 0.8221 (6) | 0.057 (2) | 0.645 (5) |
H12A | 0.7907 | −0.1048 | 0.7663 | 0.085* | 0.645 (5) |
H12B | 0.7713 | −0.0980 | 0.8871 | 0.085* | 0.645 (5) |
H12C | 0.8059 | 0.0166 | 0.8277 | 0.085* | 0.645 (5) |
C11B | 0.7738 (3) | −0.0399 (15) | 0.8091 (14) | 0.124 (10) | 0.355 (5) |
H11D | 0.7866 | −0.1193 | 0.7824 | 0.185* | 0.355 (5) |
H11E | 0.7903 | −0.0354 | 0.8817 | 0.185* | 0.355 (5) |
H11F | 0.8053 | 0.0196 | 0.7696 | 0.185* | 0.355 (5) |
C12B | 0.6672 (11) | 0.0371 (10) | 0.6946 (4) | 0.079 (5) | 0.355 (5) |
H12D | 0.6893 | −0.0167 | 0.6417 | 0.118* | 0.355 (5) |
H12E | 0.6967 | 0.1135 | 0.6904 | 0.118* | 0.355 (5) |
H12F | 0.6066 | 0.0495 | 0.6833 | 0.118* | 0.355 (5) |
C2AA | 0.6130 (3) | −0.1109 (4) | 0.7685 (3) | 0.0600 (18) | 0.645 (5) |
H2AA | 0.5620 | −0.0719 | 0.7403 | 0.072* | 0.645 (5) |
H2AB | 0.6358 | −0.1661 | 0.7161 | 0.072* | 0.645 (5) |
C3AA | 0.5925 (4) | −0.1760 (3) | 0.8659 (3) | 0.0601 (19) | 0.645 (5) |
H3AA | 0.6438 | −0.2168 | 0.8913 | 0.072* | 0.645 (5) |
H3AB | 0.5492 | −0.2372 | 0.8514 | 0.072* | 0.645 (5) |
C2AB | 0.6483 (3) | −0.1476 (3) | 0.8070 (9) | 0.047 (3) | 0.355 (5) |
H2AC | 0.6533 | −0.1879 | 0.7395 | 0.057* | 0.355 (5) |
H2AD | 0.6818 | −0.1925 | 0.8583 | 0.057* | 0.355 (5) |
C3AB | 0.5577 (4) | −0.1409 (8) | 0.8395 (4) | 0.079 (5) | 0.355 (5) |
H3AC | 0.5313 | −0.2205 | 0.8381 | 0.095* | 0.355 (5) |
H3AD | 0.5255 | −0.0873 | 0.7936 | 0.095* | 0.355 (5) |
N4A | 0.55992 (12) | −0.0923 (2) | 0.94860 (16) | 0.0409 (7) | |
C41A | 0.46539 (18) | −0.0810 (6) | 0.9496 (7) | 0.057 (2) | 0.645 (5) |
H41A | 0.4403 | −0.1568 | 0.9706 | 0.086* | 0.645 (5) |
H41B | 0.4454 | −0.0600 | 0.8806 | 0.086* | 0.645 (5) |
H41C | 0.4488 | −0.0189 | 0.9985 | 0.086* | 0.645 (5) |
C42A | 0.5787 (4) | −0.1472 (5) | 1.0515 (3) | 0.0537 (19) | 0.645 (5) |
H42A | 0.5503 | −0.2242 | 1.0566 | 0.080* | 0.645 (5) |
H42B | 0.5584 | −0.0947 | 1.1064 | 0.080* | 0.645 (5) |
H42C | 0.6398 | −0.1584 | 1.0587 | 0.080* | 0.645 (5) |
C41B | 0.4683 (3) | −0.0617 (13) | 0.963 (2) | 0.117 (10) | 0.355 (5) |
H41D | 0.4338 | −0.1327 | 0.9517 | 0.175* | 0.355 (5) |
H41E | 0.4521 | −0.0001 | 0.9134 | 0.175* | 0.355 (5) |
H41F | 0.4593 | −0.0323 | 1.0332 | 0.175* | 0.355 (5) |
C42B | 0.5974 (6) | −0.1650 (8) | 1.0342 (6) | 0.051 (3) | 0.355 (5) |
H42D | 0.5767 | −0.2468 | 1.0293 | 0.077* | 0.355 (5) |
H42E | 0.5808 | −0.1311 | 1.1007 | 0.077* | 0.355 (5) |
H42F | 0.6591 | −0.1646 | 1.0283 | 0.077* | 0.355 (5) |
C1B | 0.72636 (18) | 0.4115 (2) | 1.1724 (2) | 0.0310 (7) | |
N2B | 0.80876 (17) | 0.4242 (2) | 1.1827 (2) | 0.0340 (6) | |
C21B | 0.8727 (2) | 0.3689 (3) | 1.1141 (3) | 0.0490 (9) | |
H21A | 0.8444 | 0.3174 | 1.0640 | 0.074* | |
H21B | 0.9121 | 0.3216 | 1.1554 | 0.074* | |
H21C | 0.9039 | 0.4312 | 1.0776 | 0.074* | |
C3B | 0.8394 (2) | 0.5047 (3) | 1.2665 (3) | 0.0517 (9) | |
H3BA | 0.8579 | 0.5824 | 1.2387 | 0.062* | |
H3BB | 0.8866 | 0.4684 | 1.3055 | 0.062* | |
C4B | 0.7617 (3) | 0.5175 (3) | 1.3327 (3) | 0.0508 (9) | |
H4BA | 0.7573 | 0.5988 | 1.3612 | 0.061* | |
H4BB | 0.7623 | 0.4597 | 1.3902 | 0.061* | |
N5B | 0.68794 (18) | 0.4914 (2) | 1.2572 (2) | 0.0373 (6) | |
C51B | 0.6138 (2) | 0.4304 (3) | 1.3093 (3) | 0.0539 (10) | |
H51A | 0.5697 | 0.4143 | 1.2583 | 0.081* | |
H51D | 0.5911 | 0.4821 | 1.3634 | 0.081* | |
H51B | 0.6328 | 0.3555 | 1.3399 | 0.081* | |
C52B | 0.6575 (2) | 0.6065 (3) | 1.2055 (3) | 0.0491 (9) | |
H52D | 0.6160 | 0.5873 | 1.1520 | 0.074* | |
H52A | 0.7058 | 0.6475 | 1.1742 | 0.074* | |
H52B | 0.6314 | 0.6582 | 1.2572 | 0.074* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.02837 (14) | 0.02991 (13) | 0.03108 (16) | −0.00184 (13) | 0.00207 (16) | −0.00280 (15) |
Cu2 | 0.03597 (18) | 0.04584 (18) | 0.0500 (2) | −0.00367 (17) | −0.00458 (19) | −0.01197 (19) |
Cu3 | 0.0499 (2) | 0.0686 (3) | 0.0607 (3) | 0.0115 (2) | 0.0106 (2) | 0.0019 (2) |
Cl1 | 0.0494 (4) | 0.0454 (4) | 0.0372 (4) | −0.0101 (3) | 0.0095 (3) | −0.0044 (3) |
Cl2 | 0.0465 (4) | 0.0450 (3) | 0.0586 (5) | −0.0172 (3) | 0.0189 (4) | −0.0176 (4) |
Cl3 | 0.0469 (4) | 0.0578 (4) | 0.0372 (4) | 0.0193 (4) | −0.0039 (4) | −0.0014 (4) |
Cl4 | 0.0390 (4) | 0.0504 (4) | 0.0526 (5) | 0.0112 (3) | −0.0046 (4) | −0.0048 (4) |
Cl5 | 0.0403 (4) | 0.0717 (5) | 0.0477 (5) | 0.0060 (4) | 0.0048 (4) | 0.0030 (4) |
N1A | 0.0399 (14) | 0.0397 (13) | 0.0431 (15) | −0.0016 (12) | 0.0097 (12) | −0.0080 (12) |
C11A | 0.050 (3) | 0.075 (4) | 0.029 (3) | 0.015 (3) | 0.002 (3) | −0.005 (3) |
C12A | 0.030 (3) | 0.066 (4) | 0.074 (5) | 0.034 (2) | 0.012 (3) | 0.003 (3) |
C11B | 0.26 (3) | 0.071 (10) | 0.036 (8) | 0.039 (14) | −0.031 (12) | −0.003 (7) |
C12B | 0.092 (12) | 0.100 (10) | 0.044 (8) | 0.025 (9) | 0.015 (7) | −0.034 (7) |
C2AA | 0.062 (4) | 0.069 (4) | 0.049 (3) | −0.007 (3) | 0.004 (3) | −0.028 (3) |
C3AA | 0.085 (5) | 0.033 (2) | 0.062 (4) | −0.020 (3) | 0.026 (4) | −0.015 (3) |
C2AB | 0.049 (6) | 0.025 (4) | 0.067 (7) | −0.012 (4) | 0.001 (5) | −0.020 (4) |
C3AB | 0.131 (13) | 0.054 (7) | 0.052 (8) | −0.043 (8) | −0.001 (8) | 0.000 (6) |
N4A | 0.0462 (14) | 0.0379 (12) | 0.0385 (16) | −0.0112 (11) | 0.0086 (12) | −0.0006 (11) |
C41A | 0.036 (3) | 0.048 (3) | 0.088 (6) | −0.014 (2) | −0.011 (3) | 0.017 (3) |
C42A | 0.046 (3) | 0.050 (3) | 0.065 (4) | −0.003 (3) | 0.010 (3) | 0.009 (3) |
C41B | 0.056 (8) | 0.089 (9) | 0.21 (3) | −0.063 (7) | −0.010 (12) | −0.015 (12) |
C42B | 0.038 (6) | 0.051 (6) | 0.064 (8) | 0.006 (5) | 0.013 (5) | 0.031 (6) |
C1B | 0.0331 (15) | 0.0256 (11) | 0.0343 (15) | 0.0041 (10) | 0.0034 (13) | 0.0014 (11) |
N2B | 0.0311 (12) | 0.0335 (11) | 0.0373 (14) | −0.0019 (10) | −0.0027 (11) | 0.0013 (11) |
C21B | 0.0345 (17) | 0.0580 (19) | 0.055 (2) | 0.0032 (15) | 0.0029 (15) | −0.0047 (17) |
C3B | 0.053 (2) | 0.053 (2) | 0.049 (2) | −0.0090 (17) | −0.0163 (17) | −0.0056 (17) |
C4B | 0.067 (2) | 0.0488 (17) | 0.0366 (18) | −0.0041 (18) | −0.0093 (17) | −0.0107 (16) |
N5B | 0.0443 (14) | 0.0305 (11) | 0.0371 (14) | 0.0032 (11) | 0.0065 (12) | −0.0027 (11) |
C51B | 0.049 (2) | 0.060 (2) | 0.053 (2) | 0.0036 (17) | 0.0215 (18) | 0.0030 (17) |
C52B | 0.059 (2) | 0.0331 (14) | 0.055 (2) | 0.0162 (15) | 0.0042 (18) | −0.0010 (15) |
Cu1—N4A | 2.065 (2) | C3AB—H3AC | 0.9700 |
Cu1—N1A | 2.071 (2) | C3AB—H3AD | 0.9700 |
Cu1—Cl2 | 2.2926 (8) | N4A—C42A | 1.472 (3) |
Cu1—Cl1 | 2.3588 (9) | N4A—C41A | 1.472 (3) |
Cu1—Cl3 | 2.5822 (9) | N4A—C42B | 1.472 (3) |
Cu2—C1B | 1.893 (3) | N4A—C41B | 1.472 (3) |
Cu2—Cl1 | 2.3817 (9) | C41A—H41A | 0.9600 |
Cu2—Cl4 | 2.3949 (9) | C41A—H41B | 0.9600 |
Cu2—Cl2 | 2.5050 (10) | C41A—H41C | 0.9600 |
Cu3—Cl5 | 2.2054 (10) | C42A—H42A | 0.9600 |
Cu3—Cl3 | 2.2828 (10) | C42A—H42B | 0.9600 |
Cu3—Cl4 | 2.3690 (10) | C42A—H42C | 0.9600 |
N1A—C12B | 1.471 (3) | C41B—H41D | 0.9600 |
N1A—C11B | 1.472 (3) | C41B—H41E | 0.9600 |
N1A—C11A | 1.472 (3) | C41B—H41F | 0.9600 |
N1A—C12A | 1.473 (3) | C42B—H42D | 0.9600 |
N1A—C2AA | 1.531 (3) | C42B—H42E | 0.9600 |
N1A—C2AB | 1.536 (3) | C42B—H42F | 0.9600 |
C11A—H11A | 0.9600 | C1B—N2B | 1.292 (4) |
C11A—H11B | 0.9600 | C1B—N5B | 1.515 (4) |
C11A—H11C | 0.9600 | N2B—C21B | 1.456 (4) |
C12A—H12A | 0.9600 | N2B—C3B | 1.467 (4) |
C12A—H12B | 0.9600 | C21B—H21A | 0.9600 |
C12A—H12C | 0.9600 | C21B—H21B | 0.9600 |
C11B—H11D | 0.9600 | C21B—H21C | 0.9600 |
C11B—H11E | 0.9600 | C3B—C4B | 1.478 (6) |
C11B—H11F | 0.9600 | C3B—H3BA | 0.9700 |
C12B—H12D | 0.9600 | C3B—H3BB | 0.9700 |
C12B—H12E | 0.9600 | C4B—N5B | 1.520 (5) |
C12B—H12F | 0.9600 | C4B—H4BA | 0.9700 |
C2AA—C3AA | 1.466 (4) | C4B—H4BB | 0.9700 |
C2AA—H2AA | 0.9700 | N5B—C51B | 1.488 (4) |
C2AA—H2AB | 0.9700 | N5B—C52B | 1.507 (4) |
C3AA—N4A | 1.488 (3) | C51B—H51A | 0.9600 |
C3AA—H3AA | 0.9700 | C51B—H51D | 0.9600 |
C3AA—H3AB | 0.9700 | C51B—H51B | 0.9600 |
C2AB—C3AB | 1.467 (4) | C52B—H52D | 0.9600 |
C2AB—H2AC | 0.9700 | C52B—H52A | 0.9600 |
C2AB—H2AD | 0.9700 | C52B—H52B | 0.9600 |
C3AB—N4A | 1.488 (4) | ||
N4A—Cu1—N1A | 85.10 (8) | N4A—C3AB—H3AD | 110.7 |
N4A—Cu1—Cl2 | 162.16 (6) | H3AC—C3AB—H3AD | 108.8 |
N1A—Cu1—Cl2 | 91.42 (6) | C42A—N4A—C41A | 103.0 (4) |
N4A—Cu1—Cl1 | 91.47 (6) | C42A—N4A—C42B | 16.2 (5) |
N1A—Cu1—Cl1 | 167.81 (6) | C41A—N4A—C42B | 115.7 (5) |
Cl2—Cu1—Cl1 | 88.28 (3) | C42A—N4A—C41B | 100.1 (11) |
N4A—Cu1—Cl3 | 99.31 (6) | C41A—N4A—C41B | 10.8 (8) |
N1A—Cu1—Cl3 | 97.27 (6) | C42B—N4A—C41B | 114.5 (11) |
Cl2—Cu1—Cl3 | 98.49 (3) | C42A—N4A—C3AB | 133.3 (5) |
Cl1—Cu1—Cl3 | 94.82 (3) | C41A—N4A—C3AB | 90.9 (4) |
C1B—Cu2—Cl1 | 130.83 (9) | C42B—N4A—C3AB | 120.1 (6) |
C1B—Cu2—Cl4 | 112.48 (8) | C41B—N4A—C3AB | 100.2 (10) |
Cl1—Cu2—Cl4 | 100.21 (3) | C42A—N4A—C3AA | 107.8 (3) |
C1B—Cu2—Cl2 | 118.74 (9) | C41A—N4A—C3AA | 113.4 (4) |
Cl1—Cu2—Cl2 | 83.01 (3) | C42B—N4A—C3AA | 92.9 (5) |
Cl4—Cu2—Cl2 | 106.62 (4) | C41B—N4A—C3AA | 123.9 (9) |
Cl5—Cu3—Cl3 | 127.40 (4) | C3AB—N4A—C3AA | 28.9 (4) |
Cl5—Cu3—Cl4 | 118.54 (4) | C42A—N4A—Cu1 | 112.8 (3) |
Cl3—Cu3—Cl4 | 108.76 (4) | C41A—N4A—Cu1 | 113.8 (3) |
Cu1—Cl1—Cu2 | 93.37 (3) | C42B—N4A—Cu1 | 112.8 (4) |
Cu1—Cl2—Cu2 | 91.82 (3) | C41B—N4A—Cu1 | 106.3 (6) |
Cu3—Cl3—Cu1 | 92.46 (3) | C3AB—N4A—Cu1 | 101.1 (4) |
Cu3—Cl4—Cu2 | 90.85 (3) | C3AA—N4A—Cu1 | 106.1 (2) |
C12B—N1A—C11B | 106.8 (10) | N4A—C41A—H41A | 109.5 |
C12B—N1A—C11A | 15.7 (7) | N4A—C41A—H41B | 109.5 |
C11B—N1A—C11A | 98.2 (7) | N4A—C41A—H41C | 109.5 |
C12B—N1A—C12A | 115.3 (7) | N4A—C42A—H42A | 109.5 |
C11B—N1A—C12A | 9.1 (8) | N4A—C42A—H42B | 109.5 |
C11A—N1A—C12A | 107.3 (4) | N4A—C42A—H42C | 109.5 |
C12B—N1A—C2AA | 86.8 (6) | N4A—C41B—H41D | 109.5 |
C11B—N1A—C2AA | 125.1 (7) | N4A—C41B—H41E | 109.5 |
C11A—N1A—C2AA | 102.4 (3) | H41D—C41B—H41E | 109.5 |
C12A—N1A—C2AA | 120.3 (4) | N4A—C41B—H41F | 109.5 |
C12B—N1A—C2AB | 112.9 (7) | H41D—C41B—H41F | 109.5 |
C11B—N1A—C2AB | 98.6 (7) | H41E—C41B—H41F | 109.5 |
C11A—N1A—C2AB | 128.1 (5) | N4A—C42B—H42D | 109.5 |
C12A—N1A—C2AB | 91.7 (3) | N4A—C42B—H42E | 109.5 |
C2AA—N1A—C2AB | 31.7 (3) | H42D—C42B—H42E | 109.5 |
C12B—N1A—Cu1 | 117.2 (5) | N4A—C42B—H42F | 109.5 |
C11B—N1A—Cu1 | 115.8 (7) | H42D—C42B—H42F | 109.5 |
C11A—N1A—Cu1 | 111.7 (3) | H42E—C42B—H42F | 109.5 |
C12A—N1A—Cu1 | 112.2 (3) | N2B—C1B—N5B | 104.7 (2) |
C2AA—N1A—Cu1 | 102.6 (2) | N2B—C1B—Cu2 | 133.3 (2) |
C2AB—N1A—Cu1 | 104.1 (4) | N5B—C1B—Cu2 | 121.9 (2) |
N1A—C11A—H11A | 109.5 | C1B—N2B—C21B | 124.6 (3) |
N1A—C11A—H11B | 109.5 | C1B—N2B—C3B | 117.4 (3) |
N1A—C11A—H11C | 109.5 | C21B—N2B—C3B | 117.9 (3) |
N1A—C12A—H12A | 109.5 | N2B—C21B—H21A | 109.5 |
N1A—C12A—H12B | 109.5 | N2B—C21B—H21B | 109.5 |
N1A—C12A—H12C | 109.5 | H21A—C21B—H21B | 109.5 |
N1A—C11B—H11D | 109.5 | N2B—C21B—H21C | 109.5 |
N1A—C11B—H11E | 109.5 | H21A—C21B—H21C | 109.5 |
H11D—C11B—H11E | 109.5 | H21B—C21B—H21C | 109.5 |
N1A—C11B—H11F | 109.4 | N2B—C3B—C4B | 101.9 (3) |
H11D—C11B—H11F | 109.5 | N2B—C3B—H3BA | 111.4 |
H11E—C11B—H11F | 109.5 | C4B—C3B—H3BA | 111.4 |
N1A—C12B—H12D | 109.5 | N2B—C3B—H3BB | 111.4 |
N1A—C12B—H12E | 109.5 | C4B—C3B—H3BB | 111.4 |
H12D—C12B—H12E | 109.5 | H3BA—C3B—H3BB | 109.3 |
N1A—C12B—H12F | 109.5 | C3B—C4B—N5B | 103.7 (3) |
H12D—C12B—H12F | 109.5 | C3B—C4B—H4BA | 111.0 |
H12E—C12B—H12F | 109.5 | N5B—C4B—H4BA | 111.0 |
C3AA—C2AA—N1A | 105.5 (3) | C3B—C4B—H4BB | 111.0 |
C3AA—C2AA—H2AA | 110.6 | N5B—C4B—H4BB | 111.0 |
N1A—C2AA—H2AA | 110.6 | H4BA—C4B—H4BB | 109.0 |
C3AA—C2AA—H2AB | 110.6 | C51B—N5B—C52B | 109.5 (3) |
N1A—C2AA—H2AB | 110.6 | C51B—N5B—C1B | 111.0 (2) |
H2AA—C2AA—H2AB | 108.8 | C52B—N5B—C1B | 107.6 (2) |
C2AA—C3AA—N4A | 111.5 (3) | C51B—N5B—C4B | 112.7 (3) |
C2AA—C3AA—H3AA | 109.3 | C52B—N5B—C4B | 110.6 (2) |
N4A—C3AA—H3AA | 109.3 | C1B—N5B—C4B | 105.3 (2) |
C2AA—C3AA—H3AB | 109.3 | N5B—C51B—H51A | 109.5 |
N4A—C3AA—H3AB | 109.3 | N5B—C51B—H51D | 109.5 |
H3AA—C3AA—H3AB | 108.0 | H51A—C51B—H51D | 109.5 |
C3AB—C2AB—N1A | 106.5 (5) | N5B—C51B—H51B | 109.5 |
C3AB—C2AB—H2AC | 110.4 | H51A—C51B—H51B | 109.5 |
N1A—C2AB—H2AC | 110.4 | H51D—C51B—H51B | 109.5 |
C3AB—C2AB—H2AD | 110.4 | N5B—C52B—H52D | 109.5 |
N1A—C2AB—H2AD | 110.4 | N5B—C52B—H52A | 109.5 |
H2AC—C2AB—H2AD | 108.6 | H52D—C52B—H52A | 109.5 |
C2AB—C3AB—N4A | 105.0 (6) | N5B—C52B—H52B | 109.5 |
C2AB—C3AB—H3AC | 110.7 | H52D—C52B—H52B | 109.5 |
N4A—C3AB—H3AC | 110.7 | H52A—C52B—H52B | 109.5 |
C2AB—C3AB—H3AD | 110.7 | ||
N4A—Cu1—Cl1—Cu2 | 177.00 (6) | Cu1—N1A—C2AB—C3AB | 39.0 (7) |
N1A—Cu1—Cl1—Cu2 | 103.6 (3) | N1A—C2AB—C3AB—N4A | −67.1 (8) |
Cl2—Cu1—Cl1—Cu2 | 14.85 (3) | C2AB—C3AB—N4A—C42A | −78.7 (7) |
Cl3—Cu1—Cl1—Cu2 | −83.53 (3) | C2AB—C3AB—N4A—C41A | 172.4 (6) |
C1B—Cu2—Cl1—Cu1 | −135.96 (11) | C2AB—C3AB—N4A—C42B | −66.9 (8) |
Cl4—Cu2—Cl1—Cu1 | 92.05 (4) | C2AB—C3AB—N4A—C41B | 166.9 (9) |
Cl2—Cu2—Cl1—Cu1 | −13.66 (3) | C2AB—C3AB—N4A—C3AA | −45.2 (5) |
N4A—Cu1—Cl2—Cu2 | −103.5 (2) | C2AB—C3AB—N4A—Cu1 | 57.9 (6) |
N1A—Cu1—Cl2—Cu2 | 178.11 (6) | C2AA—C3AA—N4A—C42A | −154.2 (5) |
Cl1—Cu1—Cl2—Cu2 | −14.08 (3) | C2AA—C3AA—N4A—C41A | 92.5 (5) |
Cl3—Cu1—Cl2—Cu2 | 80.54 (3) | C2AA—C3AA—N4A—C42B | −147.9 (6) |
C1B—Cu2—Cl2—Cu1 | 147.20 (10) | C2AA—C3AA—N4A—C41B | 89.8 (12) |
Cl1—Cu2—Cl2—Cu1 | 14.04 (3) | C2AA—C3AA—N4A—C3AB | 50.7 (7) |
Cl4—Cu2—Cl2—Cu1 | −84.57 (4) | C2AA—C3AA—N4A—Cu1 | −33.2 (5) |
Cl5—Cu3—Cl3—Cu1 | −123.83 (4) | N1A—Cu1—N4A—C42A | 119.3 (3) |
Cl4—Cu3—Cl3—Cu1 | 82.67 (4) | Cl2—Cu1—N4A—C42A | 40.0 (4) |
N4A—Cu1—Cl3—Cu3 | 97.91 (7) | Cl1—Cu1—N4A—C42A | −49.0 (3) |
N1A—Cu1—Cl3—Cu3 | −175.90 (6) | Cl3—Cu1—N4A—C42A | −144.1 (3) |
Cl2—Cu1—Cl3—Cu3 | −83.36 (4) | N1A—Cu1—N4A—C41A | −123.8 (4) |
Cl1—Cu1—Cl3—Cu3 | 5.62 (4) | Cl2—Cu1—N4A—C41A | 156.8 (4) |
Cl5—Cu3—Cl4—Cu2 | 124.87 (4) | Cl1—Cu1—N4A—C41A | 67.9 (4) |
Cl3—Cu3—Cl4—Cu2 | −78.93 (4) | Cl3—Cu1—N4A—C41A | −27.2 (4) |
C1B—Cu2—Cl4—Cu3 | −153.57 (10) | N1A—Cu1—N4A—C42B | 101.8 (4) |
Cl1—Cu2—Cl4—Cu3 | −11.06 (4) | Cl2—Cu1—N4A—C42B | 22.5 (5) |
Cl2—Cu2—Cl4—Cu3 | 74.62 (3) | Cl1—Cu1—N4A—C42B | −66.5 (4) |
N4A—Cu1—N1A—C12B | 120.2 (8) | Cl3—Cu1—N4A—C42B | −161.6 (4) |
Cl2—Cu1—N1A—C12B | −77.4 (8) | N1A—Cu1—N4A—C41B | −132.0 (11) |
Cl1—Cu1—N1A—C12B | −165.8 (8) | Cl2—Cu1—N4A—C41B | 148.7 (11) |
Cl3—Cu1—N1A—C12B | 21.4 (8) | Cl1—Cu1—N4A—C41B | 59.7 (11) |
N4A—Cu1—N1A—C11B | −112.4 (7) | Cl3—Cu1—N4A—C41B | −35.4 (11) |
Cl2—Cu1—N1A—C11B | 50.1 (7) | N1A—Cu1—N4A—C3AB | −27.8 (3) |
Cl1—Cu1—N1A—C11B | −38.3 (8) | Cl2—Cu1—N4A—C3AB | −107.2 (3) |
Cl3—Cu1—N1A—C11B | 148.9 (7) | Cl1—Cu1—N4A—C3AB | 163.9 (3) |
N4A—Cu1—N1A—C11A | 136.3 (3) | Cl3—Cu1—N4A—C3AB | 68.8 (3) |
Cl2—Cu1—N1A—C11A | −61.2 (3) | N1A—Cu1—N4A—C3AA | 1.5 (3) |
Cl1—Cu1—N1A—C11A | −149.6 (4) | Cl2—Cu1—N4A—C3AA | −77.8 (4) |
Cl3—Cu1—N1A—C11A | 37.6 (3) | Cl1—Cu1—N4A—C3AA | −166.7 (3) |
N4A—Cu1—N1A—C12A | −103.1 (3) | Cl3—Cu1—N4A—C3AA | 98.1 (3) |
Cl2—Cu1—N1A—C12A | 59.3 (3) | Cl1—Cu2—C1B—N2B | 104.6 (3) |
Cl1—Cu1—N1A—C12A | −29.1 (5) | Cl4—Cu2—C1B—N2B | −127.7 (3) |
Cl3—Cu1—N1A—C12A | 158.1 (3) | Cl2—Cu2—C1B—N2B | −2.2 (3) |
N4A—Cu1—N1A—C2AA | 27.3 (2) | Cl1—Cu2—C1B—N5B | −80.1 (2) |
Cl2—Cu1—N1A—C2AA | −170.2 (2) | Cl4—Cu2—C1B—N5B | 47.6 (2) |
Cl1—Cu1—N1A—C2AA | 101.3 (3) | Cl2—Cu2—C1B—N5B | 173.04 (17) |
Cl3—Cu1—N1A—C2AA | −71.5 (2) | N5B—C1B—N2B—C21B | −176.6 (3) |
N4A—Cu1—N1A—C2AB | −5.3 (3) | Cu2—C1B—N2B—C21B | −0.8 (5) |
Cl2—Cu1—N1A—C2AB | 157.2 (3) | N5B—C1B—N2B—C3B | 0.3 (4) |
Cl1—Cu1—N1A—C2AB | 68.7 (4) | Cu2—C1B—N2B—C3B | 176.1 (2) |
Cl3—Cu1—N1A—C2AB | −104.1 (3) | C1B—N2B—C3B—C4B | 16.2 (4) |
C12B—N1A—C2AA—C3AA | −168.9 (7) | C21B—N2B—C3B—C4B | −166.7 (3) |
C11B—N1A—C2AA—C3AA | 82.8 (9) | N2B—C3B—C4B—N5B | −24.3 (3) |
C11A—N1A—C2AA—C3AA | −167.7 (4) | N2B—C1B—N5B—C51B | −138.6 (3) |
C12A—N1A—C2AA—C3AA | 73.6 (5) | Cu2—C1B—N5B—C51B | 45.0 (3) |
C2AB—N1A—C2AA—C3AA | 44.8 (7) | N2B—C1B—N5B—C52B | 101.6 (3) |
Cu1—N1A—C2AA—C3AA | −51.8 (4) | Cu2—C1B—N5B—C52B | −74.8 (3) |
N1A—C2AA—C3AA—N4A | 58.6 (5) | N2B—C1B—N5B—C4B | −16.3 (3) |
C12B—N1A—C2AB—C3AB | −89.1 (9) | Cu2—C1B—N5B—C4B | 167.2 (2) |
C11B—N1A—C2AB—C3AB | 158.5 (9) | C3B—C4B—N5B—C51B | 146.8 (3) |
C11A—N1A—C2AB—C3AB | −93.9 (8) | C3B—C4B—N5B—C52B | −90.2 (3) |
C12A—N1A—C2AB—C3AB | 152.4 (7) | C3B—C4B—N5B—C1B | 25.7 (3) |
C2AA—N1A—C2AB—C3AB | −52.1 (4) |