# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_120809 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C61 H76 Cu1.50 F6 N3 O3 Sb ' _chemical_formula_moiety ? _chemical_formula_weight 1230.35 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 33.657(3) _cell_length_b 17.489(1) _cell_length_c 19.991(2) _cell_angle_alpha 90 _cell_angle_beta 96.718(3) _cell_angle_gamma 90 _cell_volume 11686(1) _cell_formula_units_Z 8 _cell_measurement_reflns_used 12607 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 133.2 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.010 _exptl_crystal_size_min 0.010 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5084.00 _exptl_absorpt_coefficient_mu 1.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.284 _exptl_absorpt_correction_T_max 0.989 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_ambient_temperature 133.2 _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 57494 _diffrn_reflns_av_R_equivalents 0.184 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9960 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9960 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement was carried out using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 13357 _reflns_number_gt 12474 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1686 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 13357 _refine_ls_number_parameters 681 _refine_ls_goodness_of_fit_ref 0.561 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0005 _refine_diff_density_max 3.83 _refine_diff_density_min -2.55 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cu Cu 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Sb Sb -0.587 1.546 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb(1) Sb 0.14257(2) 0.90862(5) 0.45598(4) 0.0532(3) Uani 1.00 1 d . . . Cu(2) Cu 0.06778(4) 0.01433(7) 0.12205(6) 0.0367(4) Uani 1.00 1 d . . . Cu(3) Cu 0.0000 0.1905(1) 0.2500 0.0360(6) Uani 1.00 2 d S . . F(1) F 0.0999(2) 0.9172(5) 0.3894(3) 0.111(3) Uani 1.00 1 d . . . F(2) F 0.1098(2) 0.9486(4) 0.5182(2) 0.066(2) Uani 1.00 1 d . . . F(3) F 0.1573(2) 1.0074(4) 0.4353(3) 0.101(3) Uani 1.00 1 d . . . F(4) F 0.1844(2) 0.9018(4) 0.5250(3) 0.077(2) Uani 1.00 1 d . . . F(5) F 0.1734(2) 0.8661(4) 0.3946(3) 0.084(3) Uani 1.00 1 d . . . F(6) F 0.1252(2) 0.8098(4) 0.4779(3) 0.085(3) Uani 1.00 1 d . . . O(1) O 0.0803(2) -0.0902(4) 0.1181(3) 0.038(2) Uani 1.00 1 d . . . O(2) O 0.1167(2) 0.0379(4) 0.1776(3) 0.037(2) Uani 1.00 1 d . . . O(3) O 0.0404(2) 0.2651(4) 0.2487(3) 0.037(2) Uani 1.00 1 d . . . N(1) N 0.0127(2) 0.0014(5) 0.0890(3) 0.035(3) Uani 1.00 1 d . . . N(2) N 0.0552(2) 0.1217(4) 0.1127(3) 0.029(3) Uani 1.00 1 d . . . N(3) N 0.0384(2) 0.1084(4) 0.2668(3) 0.031(3) Uani 1.00 1 d . . . C(1) C 0.0543(3) -0.1469(6) 0.1144(4) 0.036(4) Uani 1.00 1 d . . . C(2) C 0.0130(3) -0.1377(7) 0.0901(5) 0.038(4) Uani 1.00 1 d . . . C(3) C -0.0119(3) -0.2023(7) 0.0830(5) 0.042(4) Uani 1.00 1 d . . . C(4) C 0.0419(4) -0.2801(6) 0.1237(5) 0.050(4) Uani 1.00 1 d . . . C(5) C 0.0693(3) -0.2217(6) 0.1339(5) 0.038(4) Uani 1.00 1 d . . . C(6) C 0.1126(3) -0.2377(6) 0.1626(5) 0.039(3) Uani 1.00 1 d . . . C(7) C 0.1241(3) -0.1864(6) 0.2251(5) 0.050(4) Uani 1.00 1 d . . . C(8) C 0.1395(3) -0.2218(6) 0.1076(5) 0.043(4) Uani 1.00 1 d . . . C(9) C 0.1201(3) -0.3204(6) 0.1858(5) 0.064(4) Uani 1.00 1 d . . . C(10) C -0.0052(3) -0.0653(7) 0.0786(5) 0.043(4) Uani 1.00 1 d . . . C(11) C -0.0087(3) 0.0707(6) 0.0785(4) 0.034(3) Uani 1.00 1 d . . . C(12) C -0.0493(3) 0.0776(6) 0.0540(4) 0.037(3) Uani 1.00 1 d . . . C(13) C -0.0668(3) 0.1498(7) 0.0497(4) 0.042(4) Uani 1.00 1 d . . . C(14) C -0.0439(3) 0.2144(6) 0.0689(5) 0.041(4) Uani 1.00 1 d . . . C(15) C -0.0038(3) 0.2092(6) 0.0911(4) 0.039(4) Uani 1.00 1 d . . . C(16) C 0.0141(3) 0.1365(6) 0.0947(4) 0.033(3) Uani 1.00 1 d . . . C(17) C 0.0811(3) 0.1780(6) 0.1246(4) 0.033(3) Uani 1.00 1 d . . . C(18) C 0.1231(3) 0.1678(6) 0.1456(4) 0.039(4) Uani 1.00 1 d . . . C(19) C 0.1481(3) 0.2298(6) 0.1406(5) 0.040(4) Uani 1.00 1 d . . . C(20) C 0.1891(3) 0.2242(6) 0.1531(4) 0.030(3) Uani 1.00 1 d . . . C(21) C 0.2054(3) 0.1516(7) 0.1753(4) 0.033(3) Uani 1.00 1 d . . . C(22) C 0.1820(3) 0.0882(6) 0.1824(4) 0.036(3) Uani 1.00 1 d . . . C(23) C 0.2173(3) 0.2913(6) 0.1404(5) 0.038(3) Uani 1.00 1 d . . . C(24) C 0.1968(3) 0.3668(6) 0.1457(5) 0.058(4) Uani 1.00 1 d . . . C(25) C 0.2278(3) 0.2772(6) 0.0690(5) 0.056(4) Uani 1.00 1 d . . . C(26) C 0.2557(3) 0.2887(6) 0.1897(5) 0.060(4) Uani 1.00 1 d . . . C(27) C 0.2017(3) 0.0121(6) 0.2073(5) 0.042(4) Uani 1.00 1 d . . . C(28) C 0.2469(3) 0.0173(6) 0.2207(5) 0.052(4) Uani 1.00 1 d . . . C(29) C 0.1857(3) -0.0110(6) 0.2730(5) 0.049(4) Uani 1.00 1 d . . . C(30) C 0.1917(3) -0.0490(6) 0.1529(5) 0.048(4) Uani 1.00 1 d . . . C(31) C 0.1394(3) 0.0943(6) 0.1664(4) 0.030(3) Uani 1.00 1 d . . . C(33) C 0.0778(3) 0.2620(6) 0.2757(5) 0.034(3) Uani 1.00 1 d . . . C(34) C 0.1017(3) 0.3278(6) 0.2835(5) 0.035(3) Uani 1.00 1 d . . . C(35) C 0.1397(3) 0.3231(6) 0.3162(4) 0.036(3) Uani 1.00 1 d . . . C(36) C 0.1570(3) 0.2547(6) 0.3429(5) 0.041(4) Uani 1.00 1 d . . . C(37) C 0.1349(3) 0.1894(6) 0.3315(4) 0.033(3) Uani 1.00 1 d . . . C(38) C 0.0951(3) 0.1910(6) 0.2980(5) 0.037(3) Uani 1.00 1 d . . . C(39) C 0.0755(3) 0.1191(6) 0.2904(4) 0.037(3) Uani 1.00 1 d . . . C(40) C 0.0843(3) 0.4047(6) 0.2580(5) 0.039(3) Uani 1.00 1 d . . . C(41) C 0.0691(3) 0.4035(6) 0.1838(5) 0.055(4) Uani 1.00 1 d . . . C(42) C 0.1150(3) 0.4696(6) 0.2676(5) 0.055(4) Uani 1.00 1 d . . . C(43) C 0.0500(3) 0.4263(6) 0.2987(5) 0.062(4) Uani 1.00 1 d . . . C(44) C 0.1978(3) 0.2540(6) 0.3862(5) 0.039(4) Uani 1.00 1 d . . . C(45) C 0.2200(3) 0.3294(7) 0.3853(5) 0.068(4) Uani 1.00 1 d . . . C(46) C 0.2246(3) 0.1923(7) 0.3648(6) 0.067(4) Uani 1.00 1 d . . . C(47) C 0.1902(3) 0.2385(7) 0.4589(5) 0.067(4) Uani 1.00 1 d . . . C(48) C 0.0205(3) 0.0351(6) 0.2595(4) 0.033(3) Uani 1.00 1 d . . . C(49) C 0.0416(3) -0.0354(6) 0.2662(4) 0.035(3) Uani 1.00 1 d . . . C(50) C 0.0211(2) -0.1042(6) 0.2571(4) 0.038(3) Uani 1.00 1 d . . . C(51) C 0.3251(4) 0.8837(9) 0.6017(7) 0.105(6) Uani 1.00 1 d . . . C(52) C 0.3180(5) 0.9461(7) 0.5522(6) 0.061(5) Uani 1.00 1 d . . . C(53) C 0.2806(4) 0.9640(8) 0.5231(7) 0.072(5) Uani 1.00 1 d . . . C(54) C 0.2749(5) 1.0177(10) 0.4742(8) 0.087(6) Uani 1.00 1 d . . . C(55) C 0.3082(6) 1.0558(8) 0.4560(7) 0.086(6) Uani 1.00 1 d . . . C(56) C 0.3465(4) 1.0384(9) 0.4864(7) 0.082(6) Uani 1.00 1 d . . . C(57) C 0.3517(4) 0.9816(9) 0.5336(7) 0.076(5) Uani 1.00 1 d . . . C(58) C 0.0012(4) -0.2749(7) 0.0978(5) 0.048(4) Uani 1.00 1 d . . . C(59) C -0.0269(3) -0.3424(7) 0.0883(6) 0.053(4) Uani 1.00 1 d . . . C(60) C -0.0542(4) -0.3411(7) 0.1436(6) 0.082(5) Uani 1.00 1 d . . . C(61) C -0.0534(5) -0.3392(8) 0.0219(6) 0.112(6) Uani 1.00 1 d . . . C(62) C -0.0049(4) -0.4183(7) 0.0934(7) 0.100(6) Uani 1.00 1 d . . . H(1) H -0.0412 -0.1951 0.0658 0.0507 Uiso 1.00 1 calc . . . H(2) H 0.0520 -0.3325 0.1355 0.0604 Uiso 1.00 1 calc . . . H(3) H -0.0352 -0.0647 0.0606 0.0610 Uiso 1.00 1 calc . . . H(4) H -0.0651 0.0312 0.0381 0.0493 Uiso 1.00 1 calc . . . H(5) H -0.0956 0.1564 0.0344 0.0523 Uiso 1.00 1 calc . . . H(6) H -0.0568 0.2663 0.0666 0.0532 Uiso 1.00 1 calc . . . H(7) H 0.0123 0.2560 0.1041 0.0455 Uiso 1.00 1 calc . . . H(8) H 0.0701 0.2310 0.1191 0.0425 Uiso 1.00 1 calc . . . H(9) H 0.1362 0.2799 0.1270 0.0474 Uiso 1.00 1 calc . . . H(10) H 0.2347 0.1467 0.1844 0.0400 Uiso 1.00 1 calc . . . H(11) H 0.1515 -0.1937 0.2452 0.0551 Uiso 1.00 1 calc . . . H(12) H 0.1211 -0.1326 0.2151 0.0551 Uiso 1.00 1 calc . . . H(13) H 0.1074 -0.1970 0.2606 0.0551 Uiso 1.00 1 calc . . . H(14) H 0.1677 -0.2298 0.1228 0.0484 Uiso 1.00 1 calc . . . H(15) H 0.1332 -0.2531 0.0683 0.0484 Uiso 1.00 1 calc . . . H(16) H 0.1373 -0.1688 0.0923 0.0484 Uiso 1.00 1 calc . . . H(17) H 0.1030 -0.3351 0.2204 0.0729 Uiso 1.00 1 calc . . . H(18) H 0.1137 -0.3578 0.1497 0.0729 Uiso 1.00 1 calc . . . H(19) H 0.1470 -0.3312 0.2049 0.0729 Uiso 1.00 1 calc . . . H(20) H 0.2142 0.4098 0.1381 0.0639 Uiso 1.00 1 calc . . . H(21) H 0.1734 0.3725 0.1127 0.0639 Uiso 1.00 1 calc . . . H(22) H 0.1880 0.3750 0.1892 0.0639 Uiso 1.00 1 calc . . . H(23) H 0.2410 0.2287 0.0656 0.0698 Uiso 1.00 1 calc . . . H(24) H 0.2043 0.2769 0.0363 0.0698 Uiso 1.00 1 calc . . . H(25) H 0.2455 0.3160 0.0551 0.0698 Uiso 1.00 1 calc . . . H(26) H 0.2684 0.2386 0.1880 0.0688 Uiso 1.00 1 calc . . . H(27) H 0.2749 0.3257 0.1791 0.0688 Uiso 1.00 1 calc . . . H(28) H 0.2505 0.2964 0.2352 0.0688 Uiso 1.00 1 calc . . . H(29) H 0.2589 -0.0304 0.2357 0.0600 Uiso 1.00 1 calc . . . H(30) H 0.2587 0.0325 0.1809 0.0600 Uiso 1.00 1 calc . . . H(31) H 0.2551 0.0550 0.2550 0.0600 Uiso 1.00 1 calc . . . H(32) H 0.1914 0.0294 0.3076 0.0608 Uiso 1.00 1 calc . . . H(33) H 0.1572 -0.0166 0.2674 0.0608 Uiso 1.00 1 calc . . . H(34) H 0.1973 -0.0566 0.2925 0.0608 Uiso 1.00 1 calc . . . H(35) H 0.1635 -0.0566 0.1439 0.0585 Uiso 1.00 1 calc . . . H(36) H 0.2013 -0.0342 0.1107 0.0585 Uiso 1.00 1 calc . . . H(37) H 0.2039 -0.0974 0.1655 0.0585 Uiso 1.00 1 calc . . . H(38) H -0.0692 -0.2928 0.1419 0.0913 Uiso 1.00 1 calc . . . H(39) H -0.0735 -0.3811 0.1403 0.0913 Uiso 1.00 1 calc . . . H(40) H -0.0391 -0.3431 0.1873 0.0913 Uiso 1.00 1 calc . . . H(41) H -0.0682 -0.2915 0.0180 0.1102 Uiso 1.00 1 calc . . . H(42) H -0.0376 -0.3410 -0.0152 0.1102 Uiso 1.00 1 calc . . . H(43) H -0.0725 -0.3798 0.0163 0.1102 Uiso 1.00 1 calc . . . H(44) H -0.0224 -0.4625 0.0896 0.1043 Uiso 1.00 1 calc . . . H(45) H 0.0128 -0.4237 0.0589 0.1043 Uiso 1.00 1 calc . . . H(46) H 0.0118 -0.4235 0.1363 0.1043 Uiso 1.00 1 calc . . . H(47) H 0.1559 0.3699 0.3228 0.0460 Uiso 1.00 1 calc . . . H(48) H 0.1468 0.1397 0.3478 0.0430 Uiso 1.00 1 calc . . . H(49) H 0.0920 0.0732 0.3049 0.0488 Uiso 1.00 1 calc . . . H(50) H 0.0713 -0.0354 0.2773 0.0450 Uiso 1.00 1 calc . . . H(51) H 0.0569 0.4500 0.1671 0.0636 Uiso 1.00 1 calc . . . H(52) H 0.0907 0.3928 0.1560 0.0636 Uiso 1.00 1 calc . . . H(53) H 0.0496 0.3627 0.1728 0.0636 Uiso 1.00 1 calc . . . H(54) H 0.1259 0.4755 0.3136 0.0660 Uiso 1.00 1 calc . . . H(55) H 0.1373 0.4609 0.2417 0.0660 Uiso 1.00 1 calc . . . H(56) H 0.1037 0.5187 0.2525 0.0660 Uiso 1.00 1 calc . . . H(57) H 0.0593 0.4311 0.3467 0.0721 Uiso 1.00 1 calc . . . H(58) H 0.0376 0.4748 0.2855 0.0721 Uiso 1.00 1 calc . . . H(59) H 0.0290 0.3887 0.2953 0.0721 Uiso 1.00 1 calc . . . H(60) H 0.2447 0.3295 0.4141 0.0782 Uiso 1.00 1 calc . . . H(61) H 0.2259 0.3421 0.3403 0.0782 Uiso 1.00 1 calc . . . H(62) H 0.2037 0.3706 0.3993 0.0782 Uiso 1.00 1 calc . . . H(63) H 0.2112 0.1424 0.3646 0.0779 Uiso 1.00 1 calc . . . H(64) H 0.2304 0.2003 0.3191 0.0779 Uiso 1.00 1 calc . . . H(65) H 0.2489 0.1881 0.3931 0.0779 Uiso 1.00 1 calc . . . H(66) H 0.1738 0.2772 0.4752 0.0712 Uiso 1.00 1 calc . . . H(67) H 0.1761 0.1898 0.4627 0.0712 Uiso 1.00 1 calc . . . H(68) H 0.2144 0.2348 0.4892 0.0712 Uiso 1.00 1 calc . . . H(69) H 0.2999 0.8591 0.6145 0.1098 Uiso 1.00 1 calc . . . H(70) H 0.3393 0.8383 0.5855 0.1098 Uiso 1.00 1 calc . . . H(71) H 0.3400 0.8958 0.6447 0.1098 Uiso 1.00 1 calc . . . H(72) H 0.2565 0.9376 0.5390 0.0923 Uiso 1.00 1 calc . . . H(73) H 0.2480 1.0287 0.4520 0.1120 Uiso 1.00 1 calc . . . H(74) H 0.3040 1.0952 0.4198 0.1065 Uiso 1.00 1 calc . . . H(75) H 0.3708 1.0695 0.4746 0.1101 Uiso 1.00 1 calc . . . H(76) H 0.3779 0.9635 0.5515 0.0948 Uiso 1.00 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sb(1) 0.0456(5) 0.0764(7) 0.0387(4) 0.0182(5) 0.0096(4) 0.0111(5) Cu(2) 0.0377(8) 0.0374(9) 0.0354(7) -0.0001(7) 0.0064(6) -0.0010(7) Cu(3) 0.035(1) 0.036(1) 0.037(1) 0.0000 0.0033(9) 0.0000 F(1) 0.071(5) 0.227(9) 0.033(3) 0.063(6) -0.006(3) 0.021(5) F(2) 0.069(5) 0.093(5) 0.041(4) 0.041(4) 0.030(3) 0.025(3) F(3) 0.128(7) 0.077(6) 0.109(6) 0.000(5) 0.055(5) 0.034(5) F(4) 0.052(4) 0.125(6) 0.051(4) 0.006(5) 0.001(3) 0.011(4) F(5) 0.082(5) 0.127(7) 0.050(4) 0.052(5) 0.035(4) 0.021(4) F(6) 0.092(6) 0.080(6) 0.084(5) -0.039(5) 0.015(4) -0.015(4) O(1) 0.039(4) 0.030(5) 0.045(4) 0.020(4) 0.009(3) 0.002(4) O(2) 0.031(4) 0.041(5) 0.037(4) -0.001(4) 0.002(3) 0.006(3) O(3) 0.031(4) 0.041(5) 0.038(4) 0.007(4) 0.003(3) 0.008(3) N(1) 0.040(6) 0.046(7) 0.020(4) -0.007(5) 0.005(4) -0.003(4) N(2) 0.027(5) 0.025(5) 0.034(5) -0.004(4) 0.001(4) -0.001(4) N(3) 0.035(5) 0.033(6) 0.022(4) -0.006(4) -0.001(4) -0.013(4) C(1) 0.055(8) 0.027(7) 0.029(6) -0.008(6) 0.022(6) -0.002(5) C(2) 0.033(7) 0.045(8) 0.039(7) -0.002(6) 0.013(5) 0.000(6) C(3) 0.039(7) 0.046(8) 0.043(7) -0.006(6) 0.009(5) 0.002(6) C(4) 0.059(9) 0.045(8) 0.048(7) 0.003(7) 0.022(6) 0.008(6) C(5) 0.050(8) 0.030(7) 0.040(6) -0.003(6) 0.030(6) -0.001(5) C(6) 0.043(7) 0.030(7) 0.045(7) 0.013(6) 0.009(6) 0.008(5) C(7) 0.044(7) 0.049(8) 0.056(7) 0.006(6) -0.002(6) 0.002(6) C(8) 0.040(7) 0.039(7) 0.055(7) 0.012(6) 0.020(6) 0.001(6) C(9) 0.068(9) 0.041(8) 0.083(9) 0.009(7) 0.009(7) 0.022(7) C(10) 0.045(8) 0.054(9) 0.029(6) -0.012(7) 0.003(5) -0.014(6) C(11) 0.049(8) 0.026(7) 0.030(6) 0.001(6) 0.014(5) 0.000(5) C(12) 0.032(7) 0.054(9) 0.027(5) -0.000(6) 0.006(5) -0.007(5) C(13) 0.032(7) 0.066(9) 0.026(6) 0.018(7) -0.006(5) -0.005(6) C(14) 0.039(7) 0.043(8) 0.039(6) -0.003(6) 0.001(5) -0.002(6) C(15) 0.043(8) 0.045(8) 0.030(6) -0.009(6) 0.004(5) 0.001(5) C(16) 0.038(7) 0.034(7) 0.026(6) -0.007(6) 0.004(5) 0.006(5) C(17) 0.044(7) 0.031(7) 0.029(6) 0.002(6) 0.020(5) 0.009(5) C(18) 0.050(8) 0.042(8) 0.028(6) 0.013(7) 0.016(5) 0.002(5) C(19) 0.052(8) 0.027(7) 0.045(7) 0.005(6) 0.024(6) 0.012(5) C(20) 0.024(6) 0.048(8) 0.021(5) 0.004(6) 0.017(5) -0.013(5) C(21) 0.019(6) 0.057(8) 0.024(5) -0.008(6) -0.004(4) -0.009(6) C(22) 0.044(7) 0.033(7) 0.033(6) -0.009(6) 0.012(5) -0.005(6) C(23) 0.037(7) 0.032(7) 0.046(7) -0.005(6) 0.005(6) 0.000(5) C(24) 0.055(8) 0.039(8) 0.086(9) 0.001(7) 0.034(7) 0.000(7) C(25) 0.067(8) 0.059(8) 0.045(7) -0.011(7) 0.020(6) -0.011(6) C(26) 0.049(8) 0.059(9) 0.067(8) -0.021(7) -0.008(6) 0.003(7) C(27) 0.033(7) 0.036(7) 0.060(7) -0.001(6) 0.015(6) -0.006(6) C(28) 0.050(8) 0.049(8) 0.058(7) 0.006(6) 0.013(6) -0.006(6) C(29) 0.044(7) 0.055(8) 0.049(7) -0.006(6) 0.010(6) 0.011(6) C(30) 0.052(8) 0.036(7) 0.058(7) -0.001(6) 0.014(6) 0.008(6) C(31) 0.033(6) 0.034(7) 0.026(5) -0.020(6) 0.010(5) -0.012(5) C(33) 0.029(7) 0.041(8) 0.033(6) -0.000(6) 0.007(5) 0.005(5) C(34) 0.028(7) 0.035(7) 0.039(6) -0.001(6) -0.002(5) -0.005(5) C(35) 0.048(7) 0.032(7) 0.030(6) -0.014(6) 0.010(5) -0.023(5) C(36) 0.033(7) 0.041(8) 0.048(7) -0.004(6) -0.001(6) -0.004(6) C(37) 0.039(7) 0.036(7) 0.026(6) -0.004(6) 0.008(5) 0.001(5) C(38) 0.044(7) 0.031(7) 0.035(6) -0.001(6) 0.004(5) -0.006(5) C(39) 0.044(7) 0.039(8) 0.027(6) 0.005(6) 0.003(5) 0.005(5) C(40) 0.032(6) 0.041(7) 0.044(6) -0.018(6) 0.006(5) -0.008(6) C(41) 0.059(8) 0.037(7) 0.066(7) -0.004(6) -0.007(6) 0.009(6) C(42) 0.048(8) 0.041(8) 0.075(8) -0.002(6) 0.007(6) 0.004(6) C(43) 0.061(8) 0.057(9) 0.066(8) 0.007(7) -0.001(7) -0.009(7) C(44) 0.040(7) 0.049(8) 0.032(6) -0.011(6) 0.017(5) -0.001(5) C(45) 0.041(8) 0.10(1) 0.063(8) -0.027(7) -0.009(6) -0.012(7) C(46) 0.052(8) 0.08(1) 0.069(8) -0.000(8) -0.011(7) 0.004(7) C(47) 0.044(8) 0.11(1) 0.045(7) -0.008(8) 0.003(6) -0.004(7) C(48) 0.036(7) 0.043(7) 0.020(5) 0.010(5) 0.003(5) -0.010(5) C(49) 0.027(6) 0.047(8) 0.033(6) 0.015(6) 0.012(5) -0.002(5) C(50) 0.033(6) 0.062(8) 0.021(5) -0.016(6) 0.015(5) 0.002(5) C(51) 0.09(1) 0.11(1) 0.12(1) 0.002(10) 0.031(9) -0.02(1) C(52) 0.09(1) 0.042(9) 0.048(8) 0.004(8) 0.008(8) -0.002(6) C(53) 0.053(10) 0.09(1) 0.074(10) 0.027(8) -0.008(8) -0.028(9) C(54) 0.10(1) 0.08(1) 0.08(1) 0.03(1) -0.03(1) -0.038(10) C(55) 0.12(1) 0.06(1) 0.08(1) -0.00(1) -0.01(1) -0.002(8) C(56) 0.07(1) 0.09(1) 0.08(1) -0.004(9) -0.004(9) -0.018(9) C(57) 0.07(1) 0.09(1) 0.071(10) 0.021(10) 0.006(8) 0.028(9) C(58) 0.055(9) 0.043(8) 0.050(7) -0.017(7) 0.021(6) -0.004(6) C(59) 0.051(8) 0.051(9) 0.058(8) -0.026(7) 0.015(7) 0.008(7) C(60) 0.09(1) 0.08(1) 0.082(10) -0.037(8) 0.019(8) -0.007(8) C(61) 0.16(2) 0.09(1) 0.074(10) -0.09(1) -0.031(10) 0.009(8) C(62) 0.10(1) 0.029(9) 0.18(1) -0.025(8) 0.03(1) -0.024(9) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 2.0' _computing_structure_solution SHELXS97 _computing_structure_refinement 'teXsan Ver. 2.0' _computing_publication_material 'teXsan Ver. 2.0' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb(1) F(1) 1.848(5) . . yes Sb(1) F(2) 1.889(5) . . yes Sb(1) F(3) 1.857(7) . . yes Sb(1) F(4) 1.855(5) . . yes Sb(1) F(5) 1.853(6) . . yes Sb(1) F(6) 1.892(6) . . yes Cu(2) O(1) 1.880(7) . . yes Cu(2) O(2) 1.919(6) . . yes Cu(2) N(1) 1.907(8) . . yes Cu(2) N(2) 1.928(7) . . yes Cu(3) O(3) 1.886(6) . . yes Cu(3) O(3) 1.886(6) . 2_555 yes Cu(3) N(3) 1.935(8) . . yes Cu(3) N(3) 1.935(8) . 2_555 yes O(1) C(1) 1.32(1) . . yes O(2) C(31) 1.284(10) . . yes O(3) C(33) 1.313(10) . . yes N(1) C(10) 1.32(1) . . yes N(1) C(11) 1.41(1) . . yes N(2) C(16) 1.41(1) . . yes N(2) C(17) 1.32(1) . . yes N(3) C(39) 1.30(1) . . yes N(3) C(48) 1.42(1) . . yes C(1) C(2) 1.43(1) . . yes C(1) C(5) 1.44(1) . . yes C(2) C(3) 1.40(1) . . yes C(2) C(10) 1.42(1) . . yes C(3) C(58) 1.36(1) . . yes C(4) C(5) 1.37(1) . . yes C(4) C(58) 1.41(1) . . yes C(5) C(6) 1.53(1) . . yes C(6) C(7) 1.55(1) . . yes C(6) C(8) 1.53(1) . . yes C(6) C(9) 1.53(1) . . yes C(11) C(12) 1.40(1) . . yes C(11) C(16) 1.40(1) . . yes C(12) C(13) 1.39(1) . . yes C(13) C(14) 1.40(1) . . yes C(14) C(15) 1.37(1) . . yes C(15) C(16) 1.40(1) . . yes C(17) C(18) 1.44(1) . . yes C(18) C(19) 1.38(1) . . yes C(18) C(31) 1.44(1) . . yes C(19) C(20) 1.38(1) . . yes C(20) C(21) 1.43(1) . . yes C(20) C(23) 1.55(1) . . yes C(21) C(22) 1.38(1) . . yes C(22) C(27) 1.54(1) . . yes C(22) C(31) 1.44(1) . . yes C(23) C(24) 1.50(1) . . yes C(23) C(25) 1.53(1) . . yes C(23) C(26) 1.53(1) . . yes C(27) C(28) 1.52(1) . . yes C(27) C(29) 1.53(1) . . yes C(27) C(30) 1.53(1) . . yes C(33) C(34) 1.40(1) . . yes C(33) C(38) 1.42(1) . . yes C(34) C(35) 1.37(1) . . yes C(34) C(40) 1.53(1) . . yes C(35) C(36) 1.41(1) . . yes C(36) C(37) 1.37(1) . . yes C(36) C(44) 1.53(1) . . yes C(37) C(38) 1.43(1) . . yes C(38) C(39) 1.42(1) . . yes C(40) C(41) 1.51(1) . . yes C(40) C(42) 1.53(1) . . yes C(40) C(43) 1.54(1) . . yes C(44) C(45) 1.52(1) . . yes C(44) C(46) 1.50(1) . . yes C(44) C(47) 1.53(1) . . yes C(48) C(48) 1.39(2) . 2_555 yes C(48) C(49) 1.42(1) . . yes C(49) C(50) 1.39(1) . . yes C(50) C(50) 1.41(2) . 2_555 yes C(51) C(52) 1.47(2) . . yes C(52) C(53) 1.36(2) . . yes C(52) C(57) 1.38(2) . . yes C(53) C(54) 1.35(2) . . yes C(54) C(55) 1.39(2) . . yes C(55) C(56) 1.39(2) . . yes C(56) C(57) 1.37(2) . . yes C(58) C(59) 1.51(1) . . yes C(59) C(60) 1.52(2) . . yes C(59) C(61) 1.51(1) . . yes C(59) C(62) 1.52(2) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F(1) Sb(1) F(2) 88.8(3) . . . yes F(1) Sb(1) F(3) 88.2(4) . . . yes F(1) Sb(1) F(4) 177.9(3) . . . yes F(1) Sb(1) F(5) 90.2(3) . . . yes F(1) Sb(1) F(6) 90.3(3) . . . yes F(2) Sb(1) F(3) 89.6(3) . . . yes F(2) Sb(1) F(4) 89.1(2) . . . yes F(2) Sb(1) F(5) 177.8(3) . . . yes F(2) Sb(1) F(6) 88.1(3) . . . yes F(3) Sb(1) F(4) 91.5(3) . . . yes F(3) Sb(1) F(5) 92.4(3) . . . yes F(3) Sb(1) F(6) 177.3(3) . . . yes F(4) Sb(1) F(5) 91.8(3) . . . yes F(4) Sb(1) F(6) 89.8(3) . . . yes F(5) Sb(1) F(6) 89.9(3) . . . yes O(1) Cu(2) O(2) 93.0(3) . . . yes O(1) Cu(2) N(1) 94.8(3) . . . yes O(1) Cu(2) N(2) 172.0(3) . . . yes O(2) Cu(2) N(1) 163.5(3) . . . yes O(2) Cu(2) N(2) 90.6(3) . . . yes N(1) Cu(2) N(2) 83.6(4) . . . yes O(3) Cu(3) O(3) 92.5(4) . . 2_555 yes O(3) Cu(3) N(3) 92.8(3) . . . yes O(3) Cu(3) N(3) 168.1(3) . . 2_555 yes O(3) Cu(3) N(3) 168.1(3) 2_555 . . yes O(3) Cu(3) N(3) 92.8(3) 2_555 . 2_555 yes N(3) Cu(3) N(3) 84.1(5) . . 2_555 yes Cu(2) O(1) C(1) 125.6(6) . . . yes Cu(2) O(2) C(31) 123.5(6) . . . yes Cu(3) O(3) C(33) 128.7(6) . . . yes Cu(2) N(1) C(10) 124.7(8) . . . yes Cu(2) N(1) C(11) 114.0(7) . . . yes C(10) N(1) C(11) 121.3(9) . . . yes Cu(2) N(2) C(16) 113.7(6) . . . yes Cu(2) N(2) C(17) 125.2(7) . . . yes C(16) N(2) C(17) 121.0(8) . . . yes Cu(3) N(3) C(39) 123.5(7) . . . yes Cu(3) N(3) C(48) 112.7(6) . . . yes C(39) N(3) C(48) 123.3(8) . . . yes O(1) C(1) C(2) 123.3(10) . . . yes O(1) C(1) C(5) 117.2(10) . . . yes C(2) C(1) C(5) 119.5(10) . . . yes C(1) C(2) C(3) 119(1) . . . yes C(1) C(2) C(10) 122(1) . . . yes C(3) C(2) C(10) 117.5(10) . . . yes C(2) C(3) C(58) 123(1) . . . yes C(5) C(4) C(58) 127(1) . . . yes C(1) C(5) C(4) 115(1) . . . yes C(1) C(5) C(6) 123.9(10) . . . yes C(4) C(5) C(6) 120.8(10) . . . yes C(5) C(6) C(7) 109.5(8) . . . yes C(5) C(6) C(8) 108.5(8) . . . yes C(5) C(6) C(9) 113.9(9) . . . yes C(7) C(6) C(8) 111.1(9) . . . yes C(7) C(6) C(9) 106.6(8) . . . yes C(8) C(6) C(9) 107.3(9) . . . yes N(1) C(10) C(2) 125.7(10) . . . yes N(1) C(11) C(12) 125.8(9) . . . yes N(1) C(11) C(16) 114.6(10) . . . yes C(12) C(11) C(16) 119.7(10) . . . yes C(11) C(12) C(13) 119.2(9) . . . yes C(12) C(13) C(14) 120.1(9) . . . yes C(13) C(14) C(15) 121(1) . . . yes C(14) C(15) C(16) 118.6(10) . . . yes N(2) C(16) C(11) 113.6(9) . . . yes N(2) C(16) C(15) 125.7(9) . . . yes C(11) C(16) C(15) 120.7(9) . . . yes N(2) C(17) C(18) 124.5(9) . . . yes C(17) C(18) C(19) 117.8(10) . . . yes C(17) C(18) C(31) 121.6(10) . . . yes C(19) C(18) C(31) 120.4(10) . . . yes C(18) C(19) C(20) 122.4(10) . . . yes C(19) C(20) C(21) 117.4(9) . . . yes C(19) C(20) C(23) 122.4(10) . . . yes C(21) C(20) C(23) 120.1(9) . . . yes C(20) C(21) C(22) 122.7(9) . . . yes C(21) C(22) C(27) 119.8(9) . . . yes C(21) C(22) C(31) 119.1(10) . . . yes C(27) C(22) C(31) 121.1(9) . . . yes C(20) C(23) C(24) 111.1(9) . . . yes C(20) C(23) C(25) 104.1(8) . . . yes C(20) C(23) C(26) 111.0(8) . . . yes C(24) C(23) C(25) 111.5(9) . . . yes C(24) C(23) C(26) 110.0(9) . . . yes C(25) C(23) C(26) 108.9(9) . . . yes C(22) C(27) C(28) 112.9(9) . . . yes C(22) C(27) C(29) 108.8(8) . . . yes C(22) C(27) C(30) 108.9(8) . . . yes C(28) C(27) C(29) 108.1(8) . . . yes C(28) C(27) C(30) 107.4(8) . . . yes C(29) C(27) C(30) 110.8(9) . . . yes O(2) C(31) C(18) 121.5(9) . . . yes O(2) C(31) C(22) 120.2(10) . . . yes C(18) C(31) C(22) 117.8(10) . . . yes O(3) C(33) C(34) 121.5(9) . . . yes O(3) C(33) C(38) 120.1(9) . . . yes C(34) C(33) C(38) 118.4(9) . . . yes C(33) C(34) C(35) 119.7(10) . . . yes C(33) C(34) C(40) 119.6(9) . . . yes C(35) C(34) C(40) 120.7(9) . . . yes C(34) C(35) C(36) 123.6(9) . . . yes C(35) C(36) C(37) 117.0(9) . . . yes C(35) C(36) C(44) 121.5(9) . . . yes C(37) C(36) C(44) 121.4(10) . . . yes C(36) C(37) C(38) 121.7(9) . . . yes C(33) C(38) C(37) 119.4(9) . . . yes C(33) C(38) C(39) 125.1(9) . . . yes C(37) C(38) C(39) 115.6(9) . . . yes N(3) C(39) C(38) 125.6(9) . . . yes C(34) C(40) C(41) 112.9(8) . . . yes C(34) C(40) C(42) 112.7(8) . . . yes C(34) C(40) C(43) 108.7(8) . . . yes C(41) C(40) C(42) 106.2(8) . . . yes C(41) C(40) C(43) 109.4(8) . . . yes C(42) C(40) C(43) 106.7(9) . . . yes C(36) C(44) C(45) 113.4(9) . . . yes C(36) C(44) C(46) 112.0(8) . . . yes C(36) C(44) C(47) 107.4(8) . . . yes C(45) C(44) C(46) 107.9(9) . . . yes C(45) C(44) C(47) 107.6(9) . . . yes C(46) C(44) C(47) 108.4(9) . . . yes N(3) C(48) C(48) 115.2(5) . . 2_555 yes N(3) C(48) C(49) 124.9(8) . . . yes C(48) C(48) C(49) 119.8(6) 2_555 . . yes C(48) C(49) C(50) 120.2(9) . . . yes C(49) C(50) C(50) 119.9(6) . . 2_555 yes C(51) C(52) C(53) 121(1) . . . yes C(51) C(52) C(57) 116(1) . . . yes C(53) C(52) C(57) 122(1) . . . yes C(52) C(53) C(54) 120(1) . . . yes C(53) C(54) C(55) 118(1) . . . yes C(54) C(55) C(56) 121(1) . . . yes C(55) C(56) C(57) 119(1) . . . yes C(52) C(57) C(56) 117(1) . . . yes C(3) C(58) C(4) 114.5(10) . . . yes C(3) C(58) C(59) 121(1) . . . yes C(4) C(58) C(59) 124(1) . . . yes C(58) C(59) C(60) 108.6(10) . . . yes C(58) C(59) C(61) 112.2(9) . . . yes C(58) C(59) C(62) 112(1) . . . yes C(60) C(59) C(61) 107(1) . . . yes C(60) C(59) C(62) 107(1) . . . yes C(61) C(59) C(62) 108(1) . . . yes #-----------------------------------------------------------------------END _database_code_depnum_ccdc_archive 'CCDC 957252' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_120617 #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C35 H13 Cl2 Cu F6 N2 O4 Sb' _chemical_formula_moiety 'C35 H13 Cl2 Cu F6 N2 O4 Sb' _chemical_formula_weight 895.69 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 10.8962(17) _cell_length_b 12.008(2) _cell_length_c 13.632(3) _cell_angle_alpha 89.710(4) _cell_angle_beta 81.617(4) _cell_angle_gamma 84.038(4) _cell_volume 1755.0(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6659 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.50 _cell_measurement_temperature 173 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.010 _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874.00 _exptl_absorpt_coefficient_mu 1.599 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 173 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 17378 _diffrn_reflns_av_R_equivalents 0.1015 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7965 _reflns_number_gt 4368 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0857 _refine_ls_wR_factor_ref 0.2547 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 7965 _refine_ls_number_parameters 424 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 4.450 _refine_diff_density_min -1.870 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.3201 1.2651 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Sb Sb -0.5866 1.5461 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.30980(5) 0.45776(5) 0.33729(5) 0.0373(3) Uani 1.0 2 d . . . Cu3 Cu 0.26255(8) 0.79268(8) 0.42709(7) 0.0268(3) Uani 1.0 2 d . . . Cl45 Cl 0.8507(5) 0.5348(4) -0.0065(3) 0.0961(13) Uani 1.0 2 d . . . Cl46 Cl 0.7636(5) 0.7443(5) -0.0776(4) 0.1298(18) Uani 1.0 2 d . . . F7 F 0.3427(6) 0.6064(5) 0.3479(5) 0.0557(17) Uani 1.0 2 d . . . F8 F 0.1837(6) 0.4789(5) 0.4473(5) 0.0640(19) Uani 1.0 2 d . . . F9 F 0.4323(6) 0.4345(6) 0.2274(5) 0.0668(19) Uani 1.0 2 d . . . F10 F 0.2690(7) 0.3098(5) 0.3296(6) 0.075(2) Uani 1.0 2 d . . . F11 F 0.1915(6) 0.5046(6) 0.2553(5) 0.0645(18) Uani 1.0 2 d . . . F12 F 0.4258(7) 0.4141(6) 0.4186(6) 0.075(2) Uani 1.0 2 d . . . O2 O 0.3937(5) 0.8607(5) 0.3536(4) 0.0298(13) Uani 1.0 2 d . . . O4 O 0.1698(5) 0.8080(5) 0.3139(5) 0.0338(14) Uani 1.0 2 d . . . O5 O 0.8413(5) 0.9590(6) 0.4648(5) 0.0393(16) Uani 1.0 2 d . . . O6 O -0.2529(6) 0.6452(6) 0.2411(5) 0.0390(15) Uani 1.0 2 d . . . N13 N 0.3384(6) 0.7780(6) 0.5458(5) 0.0268(15) Uani 1.0 2 d . . . N14 N 0.1249(6) 0.7281(6) 0.5085(5) 0.0261(15) Uani 1.0 2 d . . . C15 C 0.4986(7) 0.8816(7) 0.3806(7) 0.0280(18) Uani 1.0 2 d . . . C16 C 0.5934(8) 0.9316(7) 0.3126(6) 0.0280(19) Uani 1.0 2 d . . . C17 C 0.7017(7) 0.9536(7) 0.3453(7) 0.031(2) Uani 1.0 2 d . . . C18 C 0.7281(7) 0.9299(7) 0.4403(6) 0.0277(18) Uani 1.0 2 d . . . C19 C 0.6411(8) 0.8817(7) 0.5080(7) 0.033(2) Uani 1.0 2 d . . . C20 C 0.5288(7) 0.8569(7) 0.4784(6) 0.0267(18) Uani 1.0 2 d . . . C21 C 0.8633(8) 0.9362(8) 0.5638(7) 0.036(2) Uani 1.0 2 d . . . C22 C 0.4485(8) 0.8092(6) 0.5549(7) 0.0283(18) Uani 1.0 2 d . . . C23 C 0.2632(8) 0.7314(7) 0.6252(6) 0.0288(19) Uani 1.0 2 d . . . C24 C 0.2978(8) 0.7083(7) 0.7209(6) 0.0308(19) Uani 1.0 2 d . . . C25 C 0.2144(9) 0.6634(8) 0.7919(7) 0.035(2) Uani 1.0 2 d . . . C26 C 0.0980(9) 0.6407(9) 0.7723(7) 0.043(3) Uani 1.0 2 d . . . C27 C 0.0650(8) 0.6597(8) 0.6800(7) 0.039(3) Uani 1.0 2 d . . . C28 C 0.1481(8) 0.7057(7) 0.6061(6) 0.0280(18) Uani 1.0 2 d . . . C29 C 0.0258(8) 0.6955(7) 0.4770(6) 0.0283(18) Uani 1.0 2 d . . . C30 C -0.0027(8) 0.7115(7) 0.3781(7) 0.0305(19) Uani 1.0 2 d . . . C31 C 0.0719(8) 0.7679(7) 0.2992(7) 0.032(2) Uani 1.0 2 d . . . C32 C 0.0310(8) 0.7770(8) 0.2015(7) 0.034(2) Uani 1.0 2 d . . . C33 C -0.0744(8) 0.7343(7) 0.1886(7) 0.033(2) Uani 1.0 2 d . . . C34 C -0.1489(8) 0.6806(8) 0.2665(7) 0.034(2) Uani 1.0 2 d . . . C35 C -0.1138(8) 0.6714(7) 0.3599(7) 0.033(2) Uani 1.0 2 d . . . C36 C -0.3398(8) 0.5973(9) 0.3183(8) 0.045(3) Uani 1.0 2 d . . . C37 C 0.5677(8) 0.9568(7) 0.2061(6) 0.0299(18) Uani 1.0 2 d . . . C38 C 0.5498(9) 0.8480(8) 0.1545(7) 0.042(3) Uani 1.0 2 d . . . C39 C 0.4515(9) 1.0419(8) 0.2048(8) 0.046(3) Uani 1.0 2 d . . . C40 C 0.6771(8) 1.0071(9) 0.1436(7) 0.044(3) Uani 1.0 2 d . . . C41 C 0.1101(8) 0.8336(8) 0.1167(7) 0.038(3) Uani 1.0 2 d . . . C42 C 0.2424(9) 0.7662(10) 0.0969(8) 0.052(3) Uani 1.0 2 d . . . C43 C 0.1238(11) 0.9543(9) 0.1455(8) 0.051(3) Uani 1.0 2 d . . . C44 C 0.0517(9) 0.8329(9) 0.0225(7) 0.045(3) Uani 1.0 2 d . . . C47 C 0.712(2) 0.6157(14) -0.0322(13) 0.139(10) Uani 1.0 2 d . . . H17 H 0.7620 0.9870 0.3004 0.0377 Uiso 1.0 2 calc R . . H19 H 0.6576 0.8658 0.5735 0.0398 Uiso 1.0 2 calc R . . H21A H 0.8629 0.8558 0.5762 0.0437 Uiso 1.0 2 calc R . . H21B H 0.7976 0.9777 0.6104 0.0437 Uiso 1.0 2 calc R . . H21C H 0.9445 0.9594 0.5729 0.0437 Uiso 1.0 2 calc R . . H22 H 0.4764 0.7991 0.6175 0.0339 Uiso 1.0 2 calc R . . H24 H 0.3771 0.7238 0.7353 0.0370 Uiso 1.0 2 calc R . . H25 H 0.2370 0.6476 0.8556 0.0424 Uiso 1.0 2 calc R . . H26 H 0.0411 0.6118 0.8231 0.0519 Uiso 1.0 2 calc R . . H27 H -0.0137 0.6418 0.6661 0.0462 Uiso 1.0 2 calc R . . H29 H -0.0307 0.6589 0.5227 0.0339 Uiso 1.0 2 calc R . . H33 H -0.1008 0.7399 0.1252 0.0395 Uiso 1.0 2 calc R . . H35 H -0.1650 0.6380 0.4119 0.0394 Uiso 1.0 2 calc R . . H36A H -0.3691 0.6531 0.3710 0.0536 Uiso 1.0 2 calc R . . H36B H -0.2972 0.5312 0.3460 0.0536 Uiso 1.0 2 calc R . . H36C H -0.4112 0.5755 0.2894 0.0536 Uiso 1.0 2 calc R . . H38A H 0.4751 0.8175 0.1884 0.0508 Uiso 1.0 2 calc R . . H38B H 0.6229 0.7936 0.1570 0.0508 Uiso 1.0 2 calc R . . H38C H 0.5401 0.8632 0.0853 0.0508 Uiso 1.0 2 calc R . . H39A H 0.4665 1.1138 0.2321 0.0547 Uiso 1.0 2 calc R . . H39B H 0.3794 1.0137 0.2451 0.0547 Uiso 1.0 2 calc R . . H39C H 0.4348 1.0522 0.1365 0.0547 Uiso 1.0 2 calc R . . H40A H 0.6566 1.0235 0.0770 0.0529 Uiso 1.0 2 calc R . . H40B H 0.7520 0.9535 0.1387 0.0529 Uiso 1.0 2 calc R . . H40C H 0.6926 1.0765 0.1751 0.0529 Uiso 1.0 2 calc R . . H42A H 0.2832 0.7691 0.1562 0.0620 Uiso 1.0 2 calc R . . H42B H 0.2929 0.7991 0.0410 0.0620 Uiso 1.0 2 calc R . . H42C H 0.2339 0.6880 0.0813 0.0620 Uiso 1.0 2 calc R . . H43A H 0.1616 0.9933 0.0873 0.0610 Uiso 1.0 2 calc R . . H43B H 0.1771 0.9539 0.1975 0.0610 Uiso 1.0 2 calc R . . H43C H 0.0414 0.9928 0.1701 0.0610 Uiso 1.0 2 calc R . . H44A H 0.1046 0.8675 -0.0310 0.0537 Uiso 1.0 2 calc R . . H44B H -0.0311 0.8752 0.0335 0.0537 Uiso 1.0 2 calc R . . H44C H 0.0438 0.7555 0.0039 0.0537 Uiso 1.0 2 calc R . . H47A H 0.6501 0.6281 0.0288 0.1668 Uiso 1.0 2 calc R . . H47B H 0.6733 0.5780 -0.0826 0.1668 Uiso 1.0 2 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sb1 0.0364(4) 0.0278(4) 0.0473(4) -0.0040(3) -0.0038(3) 0.0034(3) Cu3 0.0239(5) 0.0262(6) 0.0305(6) -0.0071(4) -0.0017(5) 0.0054(4) Cl45 0.120(4) 0.099(3) 0.073(3) -0.038(3) -0.007(3) 0.008(2) Cl46 0.130(4) 0.129(5) 0.123(4) 0.013(4) -0.015(4) -0.008(4) F7 0.054(4) 0.026(3) 0.082(5) -0.006(3) 0.010(4) -0.005(3) F8 0.065(4) 0.054(4) 0.068(5) -0.009(3) 0.006(4) 0.019(4) F9 0.059(4) 0.072(5) 0.064(5) -0.002(4) 0.006(4) -0.015(4) F10 0.096(5) 0.031(4) 0.102(6) -0.017(4) -0.020(5) 0.001(4) F11 0.062(4) 0.062(5) 0.069(5) 0.001(4) -0.014(4) 0.017(4) F12 0.089(5) 0.055(5) 0.084(5) 0.012(4) -0.036(5) -0.004(4) O2 0.025(3) 0.035(4) 0.029(3) -0.010(3) 0.002(3) 0.002(3) O4 0.028(3) 0.037(4) 0.037(4) -0.013(3) 0.001(3) 0.011(3) O5 0.023(3) 0.050(4) 0.048(4) -0.014(3) -0.007(3) 0.008(3) O6 0.033(3) 0.050(4) 0.039(4) -0.019(3) -0.010(3) 0.005(3) N13 0.022(3) 0.023(4) 0.034(4) -0.009(3) 0.004(3) 0.003(3) N14 0.030(4) 0.028(4) 0.021(4) -0.006(3) -0.002(3) -0.003(3) C15 0.027(4) 0.020(4) 0.038(5) -0.006(3) -0.002(4) -0.000(4) C16 0.029(4) 0.022(4) 0.031(5) -0.006(4) 0.005(4) 0.001(4) C17 0.023(4) 0.027(5) 0.043(5) -0.007(4) 0.003(4) 0.000(4) C18 0.024(4) 0.031(5) 0.031(5) -0.006(4) -0.012(4) 0.011(4) C19 0.034(5) 0.027(5) 0.037(5) -0.010(4) 0.004(4) -0.001(4) C20 0.023(4) 0.024(4) 0.032(5) -0.001(3) -0.001(4) -0.002(4) C21 0.024(4) 0.038(5) 0.046(6) -0.004(4) -0.002(4) 0.008(5) C22 0.034(5) 0.018(4) 0.031(5) -0.001(4) -0.003(4) -0.000(4) C23 0.031(4) 0.024(5) 0.031(5) -0.006(4) 0.001(4) -0.001(4) C24 0.034(5) 0.036(5) 0.026(5) -0.012(4) -0.012(4) 0.007(4) C25 0.044(5) 0.042(6) 0.022(4) -0.011(4) -0.007(4) 0.004(4) C26 0.042(6) 0.057(7) 0.031(5) -0.010(5) -0.002(5) 0.011(5) C27 0.022(4) 0.053(6) 0.040(5) -0.011(4) 0.002(4) 0.007(5) C28 0.034(5) 0.033(5) 0.017(4) -0.004(4) -0.006(4) 0.003(4) C29 0.031(4) 0.032(5) 0.025(4) -0.012(4) -0.010(4) 0.008(4) C30 0.035(5) 0.017(4) 0.040(5) -0.008(4) -0.005(4) 0.002(4) C31 0.025(4) 0.033(5) 0.038(5) -0.009(4) 0.005(4) 0.001(4) C32 0.036(5) 0.033(5) 0.034(5) -0.007(4) -0.008(4) 0.004(4) C33 0.031(5) 0.038(5) 0.034(5) -0.013(4) -0.012(4) 0.010(4) C34 0.031(5) 0.035(5) 0.036(5) -0.008(4) -0.008(4) 0.003(4) C35 0.027(4) 0.028(5) 0.044(6) -0.004(4) -0.004(4) 0.001(4) C36 0.028(5) 0.055(7) 0.052(6) -0.020(4) 0.002(5) 0.005(5) C37 0.032(5) 0.033(5) 0.025(4) -0.005(4) -0.004(4) 0.001(4) C38 0.048(6) 0.044(6) 0.038(5) -0.009(5) -0.014(5) 0.005(5) C39 0.049(6) 0.043(6) 0.041(6) -0.005(5) 0.006(5) 0.008(5) C40 0.032(5) 0.061(7) 0.039(6) -0.013(5) 0.002(5) 0.008(5) C41 0.032(5) 0.037(6) 0.048(6) -0.012(4) -0.005(5) 0.011(5) C42 0.039(5) 0.079(8) 0.040(6) -0.007(5) -0.016(5) 0.019(6) C43 0.064(7) 0.044(6) 0.047(6) -0.016(5) -0.011(6) 0.017(5) C44 0.048(6) 0.060(7) 0.030(5) -0.023(5) -0.009(5) 0.011(5) C47 0.21(3) 0.092(13) 0.087(12) -0.036(14) 0.073(15) -0.029(10) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Sb1 F7 1.867(6) yes . . Sb1 F8 1.879(6) yes . . Sb1 F9 1.857(6) yes . . Sb1 F10 1.883(7) yes . . Sb1 F11 1.869(7) yes . . Sb1 F12 1.835(8) yes . . Cu3 O2 1.879(6) yes . . Cu3 O4 1.962(7) yes . . Cu3 N13 1.922(7) yes . . Cu3 N14 1.957(7) yes . . Cl45 C47 1.79(3) yes . . Cl46 C47 1.777(19) yes . . O2 C15 1.300(11) yes . . O4 C31 1.256(11) yes . . O5 C18 1.402(11) yes . . O5 C21 1.425(12) yes . . O6 C34 1.342(12) yes . . O6 C36 1.467(11) yes . . N13 C22 1.316(11) yes . . N13 C23 1.409(10) yes . . N14 C28 1.409(11) yes . . N14 C29 1.315(12) yes . . C15 C16 1.459(11) yes . . C15 C20 1.441(13) yes . . C16 C17 1.371(12) yes . . C16 C37 1.541(12) yes . . C17 C18 1.389(13) yes . . C18 C19 1.393(12) yes . . C19 C20 1.404(12) yes . . C20 C22 1.418(11) yes . . C23 C24 1.428(12) yes . . C23 C28 1.382(13) yes . . C24 C25 1.376(12) yes . . C25 C26 1.388(14) yes . . C26 C27 1.370(14) yes . . C27 C28 1.405(12) yes . . C29 C30 1.434(13) yes . . C30 C31 1.459(12) yes . . C30 C35 1.403(13) yes . . C31 C32 1.466(13) yes . . C32 C33 1.339(13) yes . . C32 C41 1.538(13) yes . . C33 C34 1.433(12) yes . . C34 C35 1.382(14) yes . . C37 C38 1.530(13) yes . . C37 C39 1.544(13) yes . . C37 C40 1.537(12) yes . . C41 C42 1.566(13) yes . . C41 C43 1.531(14) yes . . C41 C44 1.514(14) yes . . C17 H17 0.950 no . . C19 H19 0.950 no . . C21 H21A 0.980 no . . C21 H21B 0.980 no . . C21 H21C 0.980 no . . C22 H22 0.950 no . . C24 H24 0.950 no . . C25 H25 0.950 no . . C26 H26 0.950 no . . C27 H27 0.950 no . . C29 H29 0.950 no . . C33 H33 0.950 no . . C35 H35 0.950 no . . C36 H36A 0.980 no . . C36 H36B 0.980 no . . C36 H36C 0.980 no . . C38 H38A 0.980 no . . C38 H38B 0.980 no . . C38 H38C 0.980 no . . C39 H39A 0.980 no . . C39 H39B 0.980 no . . C39 H39C 0.980 no . . C40 H40A 0.980 no . . C40 H40B 0.980 no . . C40 H40C 0.980 no . . C42 H42A 0.980 no . . C42 H42B 0.980 no . . C42 H42C 0.980 no . . C43 H43A 0.980 no . . C43 H43B 0.980 no . . C43 H43C 0.980 no . . C44 H44A 0.980 no . . C44 H44B 0.980 no . . C44 H44C 0.980 no . . C47 H47A 0.990 no . . C47 H47B 0.990 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 F7 Sb1 F8 90.1(3) yes . . . F7 Sb1 F9 91.0(3) yes . . . F7 Sb1 F10 177.3(3) yes . . . F7 Sb1 F11 88.9(3) yes . . . F7 Sb1 F12 90.2(3) yes . . . F8 Sb1 F9 178.7(3) yes . . . F8 Sb1 F10 87.5(3) yes . . . F8 Sb1 F11 88.9(3) yes . . . F8 Sb1 F12 90.8(3) yes . . . F9 Sb1 F10 91.4(3) yes . . . F9 Sb1 F11 90.4(3) yes . . . F9 Sb1 F12 89.9(3) yes . . . F10 Sb1 F11 89.9(4) yes . . . F10 Sb1 F12 90.9(4) yes . . . F11 Sb1 F12 179.0(3) yes . . . O2 Cu3 O4 89.8(3) yes . . . O2 Cu3 N13 95.0(3) yes . . . O2 Cu3 N14 177.1(3) yes . . . O4 Cu3 N13 174.6(3) yes . . . O4 Cu3 N14 91.6(3) yes . . . N13 Cu3 N14 83.5(3) yes . . . Cu3 O2 C15 128.3(6) yes . . . Cu3 O4 C31 130.5(6) yes . . . C18 O5 C21 116.2(7) yes . . . C34 O6 C36 118.3(8) yes . . . Cu3 N13 C22 124.6(6) yes . . . Cu3 N13 C23 113.3(6) yes . . . C22 N13 C23 122.1(8) yes . . . Cu3 N14 C28 112.8(6) yes . . . Cu3 N14 C29 126.0(6) yes . . . C28 N14 C29 120.7(7) yes . . . O2 C15 C16 121.4(8) yes . . . O2 C15 C20 122.5(7) yes . . . C16 C15 C20 116.1(8) yes . . . C15 C16 C17 119.1(8) yes . . . C15 C16 C37 118.3(8) yes . . . C17 C16 C37 122.5(8) yes . . . C16 C17 C18 123.7(8) yes . . . O5 C18 C17 117.9(7) yes . . . O5 C18 C19 122.6(8) yes . . . C17 C18 C19 119.5(8) yes . . . C18 C19 C20 119.2(9) yes . . . C15 C20 C19 122.3(8) yes . . . C15 C20 C22 124.4(8) yes . . . C19 C20 C22 113.2(8) yes . . . N13 C22 C20 125.1(8) yes . . . N13 C23 C24 125.0(8) yes . . . N13 C23 C28 115.9(8) yes . . . C24 C23 C28 119.0(8) yes . . . C23 C24 C25 118.9(8) yes . . . C24 C25 C26 121.4(9) yes . . . C25 C26 C27 120.3(9) yes . . . C26 C27 C28 119.6(9) yes . . . N14 C28 C23 114.5(7) yes . . . N14 C28 C27 124.7(8) yes . . . C23 C28 C27 120.8(8) yes . . . N14 C29 C30 124.4(8) yes . . . C29 C30 C31 125.2(8) yes . . . C29 C30 C35 115.4(8) yes . . . C31 C30 C35 119.4(9) yes . . . O4 C31 C30 121.1(8) yes . . . O4 C31 C32 120.1(8) yes . . . C30 C31 C32 118.8(8) yes . . . C31 C32 C33 118.5(8) yes . . . C31 C32 C41 119.5(8) yes . . . C33 C32 C41 121.9(9) yes . . . C32 C33 C34 122.7(9) yes . . . O6 C34 C33 114.7(8) yes . . . O6 C34 C35 125.0(8) yes . . . C33 C34 C35 120.3(9) yes . . . C30 C35 C34 120.1(8) yes . . . C16 C37 C38 109.6(7) yes . . . C16 C37 C39 111.7(7) yes . . . C16 C37 C40 111.9(8) yes . . . C38 C37 C39 109.7(8) yes . . . C38 C37 C40 107.1(7) yes . . . C39 C37 C40 106.7(7) yes . . . C32 C41 C42 108.4(8) yes . . . C32 C41 C43 110.3(8) yes . . . C32 C41 C44 110.8(8) yes . . . C42 C41 C43 109.2(9) yes . . . C42 C41 C44 108.5(8) yes . . . C43 C41 C44 109.7(8) yes . . . Cl45 C47 Cl46 104.2(12) yes . . . C16 C17 H17 118.154 no . . . C18 C17 H17 118.159 no . . . C18 C19 H19 120.392 no . . . C20 C19 H19 120.397 no . . . O5 C21 H21A 109.467 no . . . O5 C21 H21B 109.470 no . . . O5 C21 H21C 109.464 no . . . H21A C21 H21B 109.474 no . . . H21A C21 H21C 109.479 no . . . H21B C21 H21C 109.474 no . . . N13 C22 H22 117.458 no . . . C20 C22 H22 117.459 no . . . C23 C24 H24 120.564 no . . . C25 C24 H24 120.562 no . . . C24 C25 H25 119.316 no . . . C26 C25 H25 119.317 no . . . C25 C26 H26 119.858 no . . . C27 C26 H26 119.862 no . . . C26 C27 H27 120.199 no . . . C28 C27 H27 120.199 no . . . N14 C29 H29 117.824 no . . . C30 C29 H29 117.809 no . . . C32 C33 H33 118.626 no . . . C34 C33 H33 118.630 no . . . C30 C35 H35 119.938 no . . . C34 C35 H35 119.948 no . . . O6 C36 H36A 109.474 no . . . O6 C36 H36B 109.470 no . . . O6 C36 H36C 109.470 no . . . H36A C36 H36B 109.473 no . . . H36A C36 H36C 109.476 no . . . H36B C36 H36C 109.464 no . . . C37 C38 H38A 109.466 no . . . C37 C38 H38B 109.466 no . . . C37 C38 H38C 109.476 no . . . H38A C38 H38B 109.473 no . . . H38A C38 H38C 109.471 no . . . H38B C38 H38C 109.475 no . . . C37 C39 H39A 109.465 no . . . C37 C39 H39B 109.464 no . . . C37 C39 H39C 109.473 no . . . H39A C39 H39B 109.465 no . . . H39A C39 H39C 109.479 no . . . H39B C39 H39C 109.482 no . . . C37 C40 H40A 109.477 no . . . C37 C40 H40B 109.471 no . . . C37 C40 H40C 109.476 no . . . H40A C40 H40B 109.476 no . . . H40A C40 H40C 109.461 no . . . H40B C40 H40C 109.467 no . . . C41 C42 H42A 109.472 no . . . C41 C42 H42B 109.480 no . . . C41 C42 H42C 109.475 no . . . H42A C42 H42B 109.471 no . . . H42A C42 H42C 109.465 no . . . H42B C42 H42C 109.464 no . . . C41 C43 H43A 109.468 no . . . C41 C43 H43B 109.464 no . . . C41 C43 H43C 109.476 no . . . H43A C43 H43B 109.469 no . . . H43A C43 H43C 109.468 no . . . H43B C43 H43C 109.482 no . . . C41 C44 H44A 109.470 no . . . C41 C44 H44B 109.469 no . . . C41 C44 H44C 109.468 no . . . H44A C44 H44B 109.471 no . . . H44A C44 H44C 109.474 no . . . H44B C44 H44C 109.474 no . . . Cl45 C47 H47A 110.925 no . . . Cl45 C47 H47B 110.927 no . . . Cl46 C47 H47A 110.916 no . . . Cl46 C47 H47B 110.919 no . . . H47A C47 H47B 108.946 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O2 Cu3 O4 C31 170.0(5) no . . . . O4 Cu3 O2 C15 -179.7(5) no . . . . O2 Cu3 N13 C22 -1.2(5) no . . . . O2 Cu3 N13 C23 177.8(4) no . . . . N13 Cu3 O2 C15 2.8(5) no . . . . O4 Cu3 N14 C28 -177.4(4) no . . . . O4 Cu3 N14 C29 10.1(5) no . . . . N14 Cu3 O4 C31 -12.5(5) no . . . . N13 Cu3 N14 C28 0.4(4) no . . . . N13 Cu3 N14 C29 -172.1(6) no . . . . N14 Cu3 N13 C22 -178.6(5) no . . . . N14 Cu3 N13 C23 0.3(4) no . . . . Cu3 O2 C15 C16 177.7(4) no . . . . Cu3 O2 C15 C20 -2.2(10) no . . . . Cu3 O4 C31 C30 9.5(11) no . . . . Cu3 O4 C31 C32 -170.4(4) no . . . . C21 O5 C18 C17 178.3(6) no . . . . C21 O5 C18 C19 0.2(10) no . . . . C36 O6 C34 C33 -175.2(6) no . . . . C36 O6 C34 C35 2.8(11) no . . . . Cu3 N13 C22 C20 -1.0(10) no . . . . Cu3 N13 C23 C24 178.2(5) no . . . . Cu3 N13 C23 C28 -1.0(8) no . . . . C22 N13 C23 C24 -2.8(11) no . . . . C22 N13 C23 C28 178.0(6) no . . . . C23 N13 C22 C20 -179.8(6) no . . . . Cu3 N14 C28 C23 -1.1(8) no . . . . Cu3 N14 C28 C27 179.8(5) no . . . . Cu3 N14 C29 C30 -5.9(11) no . . . . C28 N14 C29 C30 -177.8(6) no . . . . C29 N14 C28 C23 171.9(6) no . . . . C29 N14 C28 C27 -7.2(11) no . . . . O2 C15 C16 C17 179.0(6) no . . . . O2 C15 C16 C37 -1.5(10) no . . . . O2 C15 C20 C19 -178.7(6) no . . . . O2 C15 C20 C22 -0.8(11) no . . . . C16 C15 C20 C19 1.5(10) no . . . . C16 C15 C20 C22 179.4(6) no . . . . C20 C15 C16 C17 -1.2(10) no . . . . C20 C15 C16 C37 178.3(6) no . . . . C15 C16 C17 C18 0.7(11) no . . . . C15 C16 C37 C38 -60.3(8) no . . . . C15 C16 C37 C39 61.5(9) no . . . . C15 C16 C37 C40 -178.9(6) no . . . . C17 C16 C37 C38 119.2(8) no . . . . C17 C16 C37 C39 -119.0(8) no . . . . C17 C16 C37 C40 0.6(10) no . . . . C37 C16 C17 C18 -178.8(6) no . . . . C16 C17 C18 O5 -178.6(7) no . . . . C16 C17 C18 C19 -0.5(12) no . . . . O5 C18 C19 C20 178.7(6) no . . . . C17 C18 C19 C20 0.7(11) no . . . . C18 C19 C20 C15 -1.3(11) no . . . . C18 C19 C20 C22 -179.4(7) no . . . . C15 C20 C22 N13 2.4(12) no . . . . C19 C20 C22 N13 -179.5(7) no . . . . N13 C23 C24 C25 179.5(6) no . . . . N13 C23 C28 N14 1.3(10) no . . . . N13 C23 C28 C27 -179.5(6) no . . . . C24 C23 C28 N14 -177.9(7) no . . . . C24 C23 C28 C27 1.2(11) no . . . . C28 C23 C24 C25 -1.3(11) no . . . . C23 C24 C25 C26 -0.2(12) no . . . . C24 C25 C26 C27 1.9(14) no . . . . C25 C26 C27 C28 -2.0(14) no . . . . C26 C27 C28 N14 179.5(8) no . . . . C26 C27 C28 C23 0.4(13) no . . . . N14 C29 C30 C31 -1.3(12) no . . . . N14 C29 C30 C35 -179.4(7) no . . . . C29 C30 C31 O4 -0.3(12) no . . . . C29 C30 C31 C32 179.6(7) no . . . . C29 C30 C35 C34 -178.7(6) no . . . . C31 C30 C35 C34 3.1(11) no . . . . C35 C30 C31 O4 177.7(7) no . . . . C35 C30 C31 C32 -2.4(11) no . . . . O4 C31 C32 C33 -179.4(7) no . . . . O4 C31 C32 C41 1.4(11) no . . . . C30 C31 C32 C33 0.7(11) no . . . . C30 C31 C32 C41 -178.5(6) no . . . . C31 C32 C33 C34 0.3(12) no . . . . C31 C32 C41 C42 60.5(10) no . . . . C31 C32 C41 C43 -59.0(9) no . . . . C31 C32 C41 C44 179.4(7) no . . . . C33 C32 C41 C42 -118.8(9) no . . . . C33 C32 C41 C43 121.8(9) no . . . . C33 C32 C41 C44 0.2(11) no . . . . C41 C32 C33 C34 179.5(7) no . . . . C32 C33 C34 O6 178.4(7) no . . . . C32 C33 C34 C35 0.4(12) no . . . . O6 C34 C35 C30 -180.0(7) no . . . . C33 C34 C35 C30 -2.1(12) no . . . . #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 957253'