# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Jones, Matthew' _publ_contact_author_name 'Matthew Jones' _publ_contact_author_address ; ; _publ_contact_author_email mj205@bath.ac.uk # Attachment '- All.CIF' data_MeOH _database_code_depnum_ccdc_archive 'CCDC 804589' #TrackingRef '- All.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration ad _chemical_formula_moiety ? _chemical_formula_sum 'C20.70 H22.80 Cu F6 N4 O6.70 S2' _chemical_formula_weight 676.49 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 Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.8600(5) _cell_length_b 11.2890(5) _cell_length_c 14.6510(7) _cell_angle_alpha 80.751(3) _cell_angle_beta 86.603(2) _cell_angle_gamma 69.248(3) _cell_volume 1352.51(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 81171 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 687 _exptl_absorpt_coefficient_mu 1.050 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8175 _exptl_absorpt_correction_T_max 0.9023 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995 ; _exptl_special_details ; ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25918 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11526 _reflns_number_gt 8834 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0830P)^2^+0.8116P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.027(13) _refine_ls_number_reflns 11526 _refine_ls_number_parameters 750 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1481 _refine_ls_wR_factor_gt 0.1296 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 1.23414(6) 0.78457(5) 0.84283(4) 0.03554(18) Uani 1 1 d . . . S1 S 1.2115(2) 0.54646(16) 1.03961(11) 0.0456(4) Uani 1 1 d . . . F1 F 1.4095(7) 0.4132(5) 0.9267(4) 0.0892(16) Uani 1 1 d . . . O1 O 1.1654(6) 0.6517(4) 0.9655(3) 0.0464(11) Uani 1 1 d . . . N1 N 1.2097(6) 0.6643(5) 0.7580(3) 0.0349(11) Uani 1 1 d . . . C1 C 1.3168(8) 0.5618(6) 0.7275(4) 0.0393(14) Uani 1 1 d . . . H1 H 1.4281 0.5446 0.7369 0.047 Uiso 1 1 calc R . . Cu2 Cu 0.89207(6) 0.64717(5) 1.39059(4) 0.03698(18) Uani 1 1 d . . . S2 S 1.42929(18) 0.94090(14) 0.64935(10) 0.0367(3) Uani 1 1 d . . . F2 F 1.1709(7) 0.4039(5) 0.9267(4) 0.0884(15) Uani 1 1 d . . . O2 O 1.3438(8) 0.5350(6) 1.0937(5) 0.088(2) Uani 1 1 d . . . N2 N 1.4607(6) 0.7394(5) 0.8840(4) 0.0354(12) Uani 1 1 d . . . C2 C 1.2752(9) 0.4801(6) 0.6837(4) 0.0427(15) Uani 1 1 d . . . H2 H 1.3562 0.4093 0.6621 0.051 Uiso 1 1 calc R . . S3 S 0.69899(18) 0.50594(15) 1.57702(11) 0.0412(4) Uani 1 1 d . . . F3 F 1.3339(8) 0.2988(4) 1.0393(3) 0.0958(18) Uani 1 1 d . . . O3 O 1.0770(6) 0.5297(5) 1.0927(3) 0.0645(14) Uani 1 1 d . . . N3 N 1.1917(7) 0.9311(5) 0.9169(4) 0.0397(13) Uani 1 1 d . . . H3A H 1.1697 0.9036 0.9778 0.048 Uiso 1 1 calc R . . C3 C 1.1140(8) 0.5017(6) 0.6711(4) 0.0426(15) Uani 1 1 d . . . H3 H 1.0823 0.4436 0.6434 0.051 Uiso 1 1 calc R . . S4 S 0.9217(2) 0.85720(17) 1.17171(11) 0.0480(4) Uani 1 1 d . . . F4 F 1.2307(7) 1.1716(5) 0.5884(4) 0.0968(19) Uani 1 1 d . . . O4 O 1.2942(5) 0.9174(4) 0.6998(3) 0.0418(10) Uani 1 1 d . . . N4 N 1.0018(6) 0.8622(5) 0.8205(4) 0.0354(11) Uani 1 1 d . . . C4 C 0.9985(8) 0.6100(6) 0.6996(4) 0.0388(14) Uani 1 1 d . . . H4 H 0.8868 0.6291 0.6895 0.047 Uiso 1 1 calc R . . F5 F 1.4789(6) 1.1555(5) 0.5908(4) 0.0783(14) Uani 1 1 d . . . O5 O 1.5740(6) 0.9002(5) 0.7013(4) 0.0609(14) Uani 1 1 d . . . N5 N 0.6725(7) 0.6996(5) 1.3363(4) 0.0401(13) Uani 1 1 d . . . C5 C 1.0499(8) 0.6880(6) 0.7424(4) 0.0357(14) Uani 1 1 d . . . F6 F 1.3441(8) 1.1574(4) 0.7173(4) 0.0978(19) Uani 1 1 d . . . O6 O 1.4425(6) 0.9180(6) 0.5549(4) 0.0602(14) Uani 1 1 d . . . N6 N 0.9232(6) 0.7815(5) 1.4594(3) 0.0336(11) Uani 1 1 d . . . C6 C 0.9391(8) 0.8028(6) 0.7752(4) 0.0349(13) Uani 1 1 d . . . F7 F 0.7779(8) 0.3291(6) 1.4719(6) 0.120(2) Uani 1 1 d . . . O7 O 1.3510(6) 1.0407(5) 0.9740(3) 0.0512(11) Uani 1 1 d . . . N7 N 1.1201(6) 0.5627(5) 1.4214(3) 0.0341(11) Uani 1 1 d . . . C7 C 0.9171(7) 0.9743(5) 0.8647(4) 0.0367(13) Uani 1 1 d . . . H7 H 0.8843 0.9436 0.9280 0.044 Uiso 1 1 calc R . . F8 F 0.9100(6) 0.2751(5) 1.6024(6) 0.127(3) Uani 1 1 d . . . O8 O 0.8233(6) 0.5476(5) 1.5308(3) 0.0479(11) Uani 1 1 d . . . N8 N 0.9381(8) 0.5042(7) 1.3190(5) 0.067(2) Uani 1 1 d . B . H8 H 0.9118 0.4446 1.3622 0.080 Uiso 0.40 1 calc PR A 1 C8 C 0.7691(9) 1.0684(7) 0.8165(6) 0.0567(19) Uani 1 1 d . . . H8A H 0.6897 1.0260 0.8124 0.068 Uiso 1 1 calc R . . H8B H 0.7975 1.0983 0.7527 0.068 Uiso 1 1 calc R . . F9 F 0.6678(6) 0.2817(5) 1.6017(6) 0.111(2) Uani 1 1 d . . . O9 O 0.5425(6) 0.5579(5) 1.5323(3) 0.0517(12) Uani 1 1 d . . . C9 C 0.6936(10) 1.1833(7) 0.8678(7) 0.066(2) Uani 1 1 d . . . H9A H 0.6533 1.1552 0.9288 0.080 Uiso 1 1 calc R . . H9B H 0.6009 1.2474 0.8321 0.080 Uiso 1 1 calc R . . F10 F 0.7163(8) 0.9963(6) 1.2797(4) 0.111(2) Uani 1 1 d . . . O10 O 0.6964(6) 0.5016(5) 1.6754(4) 0.0589(13) Uani 1 1 d . . . C10 C 0.8212(9) 1.2454(6) 0.8812(6) 0.067(2) Uani 1 1 d . . . H10A H 0.8529 1.2814 0.8201 0.080 Uiso 1 1 calc R . . H10B H 0.7726 1.3166 0.9176 0.080 Uiso 1 1 calc R . . F11 F 0.9443(11) 1.0375(7) 1.2541(6) 0.143(3) Uani 1 1 d . . . O11 O 0.9918(6) 0.7676(5) 1.2524(3) 0.0519(12) Uani 1 1 d . . . C11 C 0.9677(9) 1.1496(6) 0.9300(5) 0.0539(18) Uani 1 1 d . . . H11A H 0.9374 1.1174 0.9927 0.065 Uiso 1 1 calc R . . H11B H 1.0471 1.1911 0.9366 0.065 Uiso 1 1 calc R . . F12 F 0.7580(10) 1.1015(5) 1.1491(4) 0.137(3) Uani 1 1 d . . . O12 O 0.7849(7) 0.8404(7) 1.1350(4) 0.0815(18) Uani 1 1 d . . . C12 C 1.0437(6) 1.0377(5) 0.8761(4) 0.0346(11) Uani 1 1 d . . . H12 H 1.0724 1.0727 0.8131 0.042 Uiso 1 1 calc R . . O13 O 1.0356(7) 0.8800(5) 1.1047(4) 0.0685(15) Uani 1 1 d . . . C13 C 1.3396(7) 0.9591(5) 0.9146(4) 0.0389(12) Uani 1 1 d . . . H13 H 1.3461 1.0042 0.8507 0.047 Uiso 1 1 calc R . . O14 O 0.7791(15) 0.4229(10) 1.2330(7) 0.048(3) Uani 0.40 1 d P B 1 C14 C 1.4803(7) 0.8325(6) 0.9220(4) 0.0378(12) Uani 1 1 d . . . C15 C 1.6273(8) 0.8165(6) 0.9611(5) 0.0498(15) Uani 1 1 d . . . H15 H 1.6405 0.8838 0.9875 0.060 Uiso 1 1 calc R . . C16 C 1.7527(9) 0.7023(8) 0.9609(6) 0.0580(19) Uani 1 1 d . . . H16 H 1.8516 0.6878 0.9904 0.070 Uiso 1 1 calc R . . C17 C 1.7342(10) 0.6099(8) 0.9181(6) 0.061(2) Uani 1 1 d . . . H17 H 1.8220 0.5327 0.9133 0.073 Uiso 1 1 calc R . . C18 C 1.5844(8) 0.6309(7) 0.8815(5) 0.0492(17) Uani 1 1 d . . . H18 H 1.5699 0.5652 0.8536 0.059 Uiso 1 1 calc R . . C19 C 1.3384(10) 1.0009(8) 1.0694(5) 0.0637(19) Uani 1 1 d . . . H19A H 1.2247 1.0169 1.0858 0.096 Uiso 1 1 calc R . . H19B H 1.3813 1.0489 1.1044 0.096 Uiso 1 1 calc R . . H19C H 1.4002 0.9091 1.0843 0.096 Uiso 1 1 calc R . . C20 C 1.2846(11) 0.4061(6) 0.9819(5) 0.059(2) Uani 1 1 d . . . C21 C 1.3690(10) 1.1152(8) 0.6369(5) 0.0580(19) Uani 1 1 d . . . C22 C 0.5342(9) 0.7900(7) 1.3553(5) 0.0503(17) Uani 1 1 d . . . H22 H 0.5343 0.8425 1.3999 0.060 Uiso 1 1 calc R . . C23 C 0.3901(8) 0.8097(8) 1.3118(6) 0.062(2) Uani 1 1 d . . . H23 H 0.2939 0.8757 1.3259 0.075 Uiso 1 1 calc R . . C24 C 0.3878(11) 0.7332(11) 1.2486(6) 0.073(3) Uani 1 1 d . . . H24 H 0.2896 0.7446 1.2194 0.087 Uiso 1 1 calc R . . C25 C 0.5273(9) 0.6409(8) 1.2277(5) 0.062(2) Uani 1 1 d . . . H25 H 0.5273 0.5883 1.1832 0.075 Uiso 1 1 calc R . . C26 C 0.6716(7) 0.6236(6) 1.2724(4) 0.0427(14) Uani 1 1 d . B . C27 C 0.8260(7) 0.5273(6) 1.2528(4) 0.0427(13) Uani 1 1 d . . . H27 H 0.8679 0.5626 1.1938 0.051 Uiso 1 1 calc R B 1 C28 C 0.784(3) 0.407(2) 1.1327(11) 0.071(6) Uani 0.40 1 d P B 1 H28A H 0.6798 0.4596 1.1040 0.107 Uiso 0.40 1 calc PR B 1 H28B H 0.8070 0.3171 1.1277 0.107 Uiso 0.40 1 calc PR B 1 H28C H 0.8691 0.4352 1.1010 0.107 Uiso 0.40 1 calc PR B 1 C29 C 1.1119(7) 0.4350(6) 1.3058(4) 0.0475(14) Uani 1 1 d . . . H29 H 1.1517 0.4871 1.2550 0.057 Uiso 1 1 calc R B . C30 C 1.1593(10) 0.3014(7) 1.2824(5) 0.0546(18) Uani 1 1 d . B . H30A H 1.1073 0.3039 1.2238 0.065 Uiso 1 1 calc R . . H30B H 1.1221 0.2472 1.3318 0.065 Uiso 1 1 calc R . . C31 C 1.3422(9) 0.2443(7) 1.2725(5) 0.066(2) Uani 1 1 d . . . H31A H 1.3736 0.1548 1.2606 0.079 Uiso 1 1 calc R B . H31B H 1.3780 0.2938 1.2191 0.079 Uiso 1 1 calc R . . C32 C 1.4247(11) 0.2471(8) 1.3607(5) 0.065(2) Uani 1 1 d . B . H32A H 1.3976 0.1894 1.4120 0.078 Uiso 1 1 calc R . . H32B H 1.5430 0.2132 1.3515 0.078 Uiso 1 1 calc R . . C33 C 1.3778(8) 0.3791(7) 1.3888(5) 0.0527(18) Uani 1 1 d . . . H33A H 1.4170 0.4356 1.3423 0.063 Uiso 1 1 calc R B . H33B H 1.4261 0.3731 1.4494 0.063 Uiso 1 1 calc R . . C34 C 1.1916(7) 0.4336(6) 1.3951(4) 0.0398(13) Uani 1 1 d . B . H34 H 1.1591 0.3742 1.4438 0.048 Uiso 1 1 calc R . . C35 C 1.1899(8) 0.6247(6) 1.4560(4) 0.0386(15) Uani 1 1 d . . . C36 C 1.0816(8) 0.7498(6) 1.4801(4) 0.0368(14) Uani 1 1 d . . . C37 C 1.1381(9) 0.8269(7) 1.5228(5) 0.0463(16) Uani 1 1 d . . . H37 H 1.2499 0.8034 1.5348 0.056 Uiso 1 1 calc R . . C38 C 1.0274(9) 0.9390(7) 1.5475(5) 0.0521(18) Uani 1 1 d . . . H38 H 1.0623 0.9952 1.5754 0.063 Uiso 1 1 calc R . . C39 C 0.8662(9) 0.9677(7) 1.5309(5) 0.0492(16) Uani 1 1 d . . . H39 H 0.7879 1.0425 1.5494 0.059 Uiso 1 1 calc R . . C40 C 0.8189(8) 0.8857(6) 1.4866(4) 0.0430(15) Uani 1 1 d . . . H40 H 0.7073 0.9059 1.4757 0.052 Uiso 1 1 calc R . . C41 C 0.7697(10) 0.3370(8) 1.5607(9) 0.084(3) Uani 1 1 d . . . C42 C 0.8332(12) 1.0041(10) 1.2159(7) 0.084(3) Uani 1 1 d . . . H2A H 1.287(9) 0.599(6) 1.486(4) 0.046(18) Uiso 1 1 d . . . H6A H 0.818(7) 0.827(5) 0.777(4) 0.029(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0231(4) 0.0335(3) 0.0530(4) -0.0117(3) -0.0048(3) -0.0107(3) S1 0.0461(9) 0.0456(8) 0.0429(8) -0.0071(7) -0.0082(7) -0.0118(7) F1 0.079(4) 0.069(3) 0.098(4) -0.017(3) 0.031(3) -0.001(2) O1 0.041(3) 0.043(2) 0.052(2) -0.0048(19) 0.0086(19) -0.0122(19) N1 0.026(3) 0.035(3) 0.045(3) -0.007(2) 0.002(2) -0.012(2) C1 0.031(3) 0.041(3) 0.048(3) -0.012(3) 0.004(3) -0.014(3) Cu2 0.0240(4) 0.0430(4) 0.0449(4) -0.0109(3) -0.0049(3) -0.0104(3) S2 0.0257(8) 0.0425(8) 0.0452(8) -0.0069(6) -0.0010(6) -0.0158(6) F2 0.110(4) 0.080(3) 0.087(3) -0.025(3) -0.024(3) -0.038(3) O2 0.072(4) 0.092(4) 0.103(5) -0.027(3) -0.051(3) -0.017(3) N2 0.022(3) 0.037(3) 0.046(3) -0.001(2) -0.004(2) -0.010(2) C2 0.045(4) 0.040(3) 0.048(3) -0.016(3) 0.004(3) -0.019(3) S3 0.0252(8) 0.0446(8) 0.0560(9) -0.0039(7) -0.0051(7) -0.0159(7) F3 0.144(5) 0.042(2) 0.075(3) -0.006(2) -0.007(3) -0.002(3) O3 0.053(3) 0.071(3) 0.052(3) 0.009(2) 0.010(2) -0.011(2) N3 0.035(3) 0.035(3) 0.052(3) -0.011(2) -0.002(2) -0.013(2) C3 0.045(4) 0.043(3) 0.045(3) -0.014(3) 0.000(3) -0.018(3) S4 0.0367(8) 0.0600(10) 0.0435(8) -0.0047(7) -0.0008(7) -0.0135(7) F4 0.057(3) 0.067(3) 0.143(5) 0.037(3) -0.008(3) -0.014(2) O4 0.033(2) 0.048(2) 0.048(2) 0.0015(18) -0.0010(18) -0.0236(19) N4 0.028(3) 0.032(3) 0.047(3) -0.004(2) -0.006(2) -0.012(2) C4 0.031(3) 0.044(3) 0.049(3) -0.011(3) -0.005(3) -0.019(3) F5 0.073(3) 0.067(3) 0.105(3) 0.012(2) 0.002(3) -0.046(2) O5 0.033(3) 0.075(3) 0.075(3) 0.003(3) -0.015(2) -0.023(2) N5 0.032(3) 0.045(3) 0.046(3) -0.004(2) 0.001(2) -0.018(3) C5 0.026(3) 0.050(4) 0.037(3) -0.004(3) -0.002(2) -0.021(3) F6 0.157(6) 0.048(2) 0.097(4) -0.033(3) 0.032(4) -0.041(3) O6 0.044(3) 0.094(4) 0.057(3) -0.025(3) 0.008(2) -0.038(3) N6 0.029(3) 0.044(3) 0.030(2) -0.003(2) -0.0018(19) -0.016(2) C6 0.025(4) 0.042(3) 0.040(3) -0.006(3) -0.001(3) -0.015(3) F7 0.115(5) 0.109(5) 0.173(6) -0.093(5) 0.030(4) -0.056(4) O7 0.054(3) 0.055(3) 0.054(3) -0.010(2) -0.004(2) -0.029(2) N7 0.029(3) 0.038(3) 0.033(2) -0.002(2) -0.001(2) -0.010(2) C7 0.022(3) 0.037(3) 0.051(3) -0.011(3) 0.002(2) -0.009(2) F8 0.033(3) 0.052(3) 0.284(9) -0.023(4) -0.018(4) 0.002(2) O8 0.032(2) 0.065(3) 0.053(2) -0.007(2) -0.0023(19) -0.025(2) N8 0.047(4) 0.072(4) 0.069(4) -0.037(3) -0.026(3) 0.008(3) C8 0.038(4) 0.044(4) 0.084(5) -0.018(3) -0.011(3) -0.005(3) F9 0.058(3) 0.055(3) 0.229(7) -0.006(4) -0.015(4) -0.036(2) O9 0.026(2) 0.060(3) 0.068(3) -0.001(2) -0.018(2) -0.013(2) C9 0.035(4) 0.046(4) 0.104(6) -0.031(4) -0.007(4) 0.012(3) F10 0.101(4) 0.091(4) 0.087(4) -0.007(3) 0.041(3) 0.023(3) O10 0.038(3) 0.082(4) 0.062(3) -0.008(3) 0.004(2) -0.029(3) C10 0.068(5) 0.035(3) 0.085(5) -0.017(3) -0.008(4) 0.002(3) F11 0.168(8) 0.118(5) 0.179(8) -0.074(5) 0.015(6) -0.072(6) O11 0.036(2) 0.070(3) 0.041(2) 0.001(2) 0.0012(18) -0.012(2) C11 0.050(4) 0.041(3) 0.071(4) -0.023(3) 0.000(3) -0.011(3) F12 0.163(7) 0.069(3) 0.105(4) 0.016(3) 0.042(4) 0.030(4) O12 0.063(4) 0.109(5) 0.081(4) -0.010(3) -0.033(3) -0.037(3) C12 0.029(3) 0.031(3) 0.046(3) -0.009(2) -0.003(2) -0.012(2) O13 0.069(4) 0.069(3) 0.057(3) 0.000(2) 0.020(3) -0.019(3) C13 0.042(3) 0.042(3) 0.040(3) -0.008(2) -0.006(2) -0.022(2) O14 0.068(8) 0.044(6) 0.042(6) -0.013(5) -0.009(5) -0.029(5) C14 0.032(3) 0.044(3) 0.041(3) -0.002(2) -0.003(2) -0.019(2) C15 0.047(4) 0.052(4) 0.059(4) -0.004(3) -0.010(3) -0.027(3) C16 0.033(4) 0.065(5) 0.078(5) -0.002(4) -0.015(3) -0.020(3) C17 0.036(5) 0.068(5) 0.077(5) -0.013(4) -0.013(4) -0.013(4) C18 0.030(4) 0.047(4) 0.072(5) -0.018(3) -0.009(3) -0.009(3) C19 0.062(5) 0.082(5) 0.054(4) -0.016(4) -0.002(3) -0.032(4) C20 0.075(5) 0.036(3) 0.052(4) -0.002(3) -0.006(4) -0.001(3) C21 0.051(4) 0.063(5) 0.062(4) -0.005(3) 0.005(3) -0.024(4) C22 0.030(4) 0.062(4) 0.057(4) 0.004(3) 0.000(3) -0.018(3) C23 0.020(4) 0.075(5) 0.075(5) 0.022(4) -0.006(3) -0.010(3) C24 0.044(5) 0.115(7) 0.063(5) 0.023(5) -0.027(4) -0.045(5) C25 0.057(5) 0.086(5) 0.057(4) 0.008(4) -0.024(3) -0.047(4) C26 0.040(3) 0.058(4) 0.041(3) 0.002(3) -0.009(3) -0.034(3) C27 0.046(3) 0.048(3) 0.041(3) -0.008(2) -0.003(2) -0.025(3) C28 0.117(18) 0.082(13) 0.037(9) -0.002(9) -0.005(10) -0.066(13) C29 0.046(3) 0.047(3) 0.044(3) -0.011(3) -0.002(3) -0.007(3) C30 0.054(5) 0.049(4) 0.053(4) -0.020(3) -0.012(3) -0.002(3) C31 0.060(4) 0.060(4) 0.057(4) -0.023(3) -0.007(3) 0.013(3) C32 0.057(5) 0.063(5) 0.059(4) -0.010(4) -0.004(4) -0.002(4) C33 0.027(3) 0.065(4) 0.057(4) -0.018(3) 0.000(3) -0.001(3) C34 0.036(3) 0.041(3) 0.040(3) -0.008(2) 0.001(2) -0.010(2) C35 0.025(4) 0.049(4) 0.038(3) -0.002(3) -0.004(3) -0.010(3) C36 0.035(4) 0.035(3) 0.043(3) -0.001(3) -0.005(3) -0.017(3) C37 0.038(4) 0.060(4) 0.050(4) -0.013(3) -0.004(3) -0.024(3) C38 0.049(4) 0.056(4) 0.064(4) -0.012(3) -0.013(3) -0.030(4) C39 0.042(4) 0.049(4) 0.059(4) -0.017(3) 0.003(3) -0.016(3) C40 0.033(4) 0.048(3) 0.048(3) -0.012(3) -0.003(3) -0.012(3) C41 0.044(5) 0.049(4) 0.168(11) -0.029(6) -0.001(5) -0.021(4) C42 0.072(6) 0.083(6) 0.091(7) -0.031(5) 0.023(5) -0.016(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 1.955(5) . ? Cu1 N2 1.993(5) . ? Cu1 N3 2.035(5) . ? Cu1 N1 2.054(5) . ? Cu1 O1 2.346(4) . ? S1 O2 1.410(6) . ? S1 O1 1.432(5) . ? S1 O3 1.436(5) . ? S1 C20 1.812(7) . ? F1 C20 1.349(10) . ? N1 C1 1.333(8) . ? N1 C5 1.371(8) . ? C1 C2 1.362(9) . ? C1 H1 0.9500 . ? Cu2 N7 1.949(5) . ? Cu2 N8 1.974(6) . ? Cu2 N5 1.996(6) . ? Cu2 N6 2.053(5) . ? Cu2 O8 2.334(4) . ? S2 O5 1.421(5) . ? S2 O6 1.438(5) . ? S2 O4 1.452(4) . ? S2 C21 1.828(8) . ? F2 C20 1.337(10) . ? N2 C18 1.328(9) . ? N2 C14 1.332(8) . ? C2 C3 1.380(10) . ? C2 H2 0.9500 . ? S3 O10 1.433(5) . ? S3 O8 1.439(5) . ? S3 O9 1.450(5) . ? S3 C41 1.836(8) . ? F3 C20 1.307(8) . ? N3 C13 1.450(7) . ? N3 C12 1.506(7) . ? N3 H3A 0.9300 . ? C3 C4 1.395(9) . ? C3 H3 0.9500 . ? S4 O13 1.426(5) . ? S4 O11 1.437(5) . ? S4 O12 1.438(6) . ? S4 C42 1.774(9) . ? F4 C21 1.348(10) . ? N4 C6 1.284(8) . ? N4 C7 1.455(8) . ? C4 C5 1.369(9) . ? C4 H4 0.9500 . ? F5 C21 1.323(8) . ? N5 C22 1.336(9) . ? N5 C26 1.370(8) . ? C5 C6 1.455(9) . ? F6 C21 1.318(9) . ? N6 C40 1.316(8) . ? N6 C36 1.360(8) . ? C6 H6A 1.01(6) . ? F7 C41 1.314(13) . ? O7 C13 1.397(7) . ? O7 C19 1.408(8) . ? N7 C35 1.260(8) . ? N7 C34 1.473(8) . ? C7 C8 1.493(9) . ? C7 C12 1.557(8) . ? C7 H7 1.0000 . ? F8 C41 1.320(11) . ? N8 C27 1.358(8) . ? N8 C29 1.476(9) . ? N8 H8 0.9300 . ? C8 C9 1.528(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? F9 C41 1.335(10) . ? C9 C10 1.563(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? F10 C42 1.370(11) . ? C10 C11 1.494(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? F11 C42 1.349(13) . ? C11 C12 1.526(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? F12 C42 1.350(12) . ? C12 H12 1.0000 . ? C13 C14 1.521(8) . ? C13 H13 1.0000 . ? O14 C27 1.455(12) . ? O14 C28 1.504(19) . ? C14 C15 1.395(8) . ? C15 C16 1.372(10) . ? C15 H15 0.9500 . ? C16 C17 1.360(11) . ? C16 H16 0.9500 . ? C17 C18 1.388(10) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C22 C23 1.392(11) . ? C22 H22 0.9500 . ? C23 C24 1.370(13) . ? C23 H23 0.9500 . ? C24 C25 1.360(13) . ? C24 H24 0.9500 . ? C25 C26 1.408(9) . ? C25 H25 0.9500 . ? C26 C27 1.462(9) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.507(9) . ? C29 C34 1.518(9) . ? C29 H29 1.0000 . ? C30 C31 1.524(10) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.532(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.517(11) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.546(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34 1.0000 . ? C35 C36 1.484(9) . ? C35 H2A 0.92(7) . ? C36 C37 1.385(9) . ? C37 C38 1.386(10) . ? C37 H37 0.9500 . ? C38 C39 1.375(10) . ? C38 H38 0.9500 . ? C39 C40 1.399(10) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? 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_3 _geom_angle_publ_flag N4 Cu1 N2 166.1(2) . . ? N4 Cu1 N3 83.0(2) . . ? N2 Cu1 N3 83.1(2) . . ? N4 Cu1 N1 80.9(2) . . ? N2 Cu1 N1 113.1(2) . . ? N3 Cu1 N1 163.7(2) . . ? N4 Cu1 O1 85.24(19) . . ? N2 Cu1 O1 95.29(19) . . ? N3 Cu1 O1 93.87(19) . . ? N1 Cu1 O1 86.78(18) . . ? O2 S1 O1 116.5(4) . . ? O2 S1 O3 114.0(4) . . ? O1 S1 O3 113.4(3) . . ? O2 S1 C20 103.7(4) . . ? O1 S1 C20 104.1(3) . . ? O3 S1 C20 103.0(4) . . ? S1 O1 Cu1 150.5(3) . . ? C1 N1 C5 117.1(5) . . ? C1 N1 Cu1 131.6(4) . . ? C5 N1 Cu1 110.6(4) . . ? N1 C1 C2 123.6(6) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? N7 Cu2 N8 82.2(2) . . ? N7 Cu2 N5 164.9(2) . . ? N8 Cu2 N5 82.8(2) . . ? N7 Cu2 N6 80.8(2) . . ? N8 Cu2 N6 161.4(3) . . ? N5 Cu2 N6 113.8(2) . . ? N7 Cu2 O8 89.95(18) . . ? N8 Cu2 O8 98.2(3) . . ? N5 Cu2 O8 94.14(19) . . ? N6 Cu2 O8 89.10(18) . . ? O5 S2 O6 117.7(3) . . ? O5 S2 O4 114.6(3) . . ? O6 S2 O4 114.5(3) . . ? O5 S2 C21 101.8(4) . . ? O6 S2 C21 102.6(4) . . ? O4 S2 C21 102.4(3) . . ? C18 N2 C14 119.2(6) . . ? C18 N2 Cu1 128.7(5) . . ? C14 N2 Cu1 112.0(4) . . ? C1 C2 C3 119.1(6) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? O10 S3 O8 114.0(3) . . ? O10 S3 O9 115.6(3) . . ? O8 S3 O9 115.9(3) . . ? O10 S3 C41 104.2(5) . . ? O8 S3 C41 101.7(4) . . ? O9 S3 C41 102.8(4) . . ? C13 N3 C12 116.9(5) . . ? C13 N3 Cu1 106.8(4) . . ? C12 N3 Cu1 106.8(4) . . ? C13 N3 H3A 108.7 . . ? C12 N3 H3A 108.7 . . ? Cu1 N3 H3A 108.7 . . ? C2 C3 C4 119.0(6) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? O13 S4 O11 114.7(3) . . ? O13 S4 O12 115.3(4) . . ? O11 S4 O12 114.5(4) . . ? O13 S4 C42 104.4(4) . . ? O11 S4 C42 103.0(4) . . ? O12 S4 C42 102.6(5) . . ? C6 N4 C7 127.2(5) . . ? C6 N4 Cu1 116.6(4) . . ? C7 N4 Cu1 116.0(4) . . ? C5 C4 C3 118.3(6) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C22 N5 C26 118.8(6) . . ? C22 N5 Cu2 130.4(5) . . ? C26 N5 Cu2 110.8(4) . . ? C4 C5 N1 122.8(6) . . ? C4 C5 C6 122.6(6) . . ? N1 C5 C6 114.6(5) . . ? C40 N6 C36 118.1(5) . . ? C40 N6 Cu2 131.4(5) . . ? C36 N6 Cu2 110.4(4) . . ? N4 C6 C5 116.4(6) . . ? N4 C6 H6A 118(3) . . ? C5 C6 H6A 124(3) . . ? C13 O7 C19 116.7(5) . . ? C35 N7 C34 128.0(6) . . ? C35 N7 Cu2 118.0(4) . . ? C34 N7 Cu2 113.9(4) . . ? N4 C7 C8 115.9(5) . . ? N4 C7 C12 106.1(4) . . ? C8 C7 C12 111.5(5) . . ? N4 C7 H7 107.7 . . ? C8 C7 H7 107.7 . . ? C12 C7 H7 107.7 . . ? S3 O8 Cu2 143.4(3) . . ? C27 N8 C29 123.0(6) . . ? C27 N8 Cu2 112.9(5) . . ? C29 N8 Cu2 113.9(5) . . ? C27 N8 H8 100.7 . . ? C29 N8 H8 100.7 . . ? Cu2 N8 H8 100.7 . . ? C7 C8 C9 111.1(6) . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C10 110.2(6) . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 111.3(6) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 110.5(6) . . ? C10 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? C10 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? N3 C12 C11 117.2(5) . . ? N3 C12 C7 106.2(4) . . ? C11 C12 C7 109.2(5) . . ? N3 C12 H12 108.0 . . ? C11 C12 H12 108.0 . . ? C7 C12 H12 108.0 . . ? O7 C13 N3 117.7(5) . . ? O7 C13 C14 113.8(5) . . ? N3 C13 C14 107.8(4) . . ? O7 C13 H13 105.5 . . ? N3 C13 H13 105.5 . . ? C14 C13 H13 105.5 . . ? C27 O14 C28 115.5(10) . . ? N2 C14 C15 121.1(6) . . ? N2 C14 C13 116.9(5) . . ? C15 C14 C13 121.9(5) . . ? C16 C15 C14 119.1(6) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C17 C16 C15 119.5(7) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 118.6(8) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? N2 C18 C17 122.3(7) . . ? N2 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? O7 C19 H19A 109.5 . . ? O7 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O7 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? F3 C20 F2 109.3(7) . . ? F3 C20 F1 108.3(7) . . ? F2 C20 F1 106.5(6) . . ? F3 C20 S1 113.1(5) . . ? F2 C20 S1 110.8(5) . . ? F1 C20 S1 108.6(6) . . ? F6 C21 F5 108.5(7) . . ? F6 C21 F4 107.4(7) . . ? F5 C21 F4 106.7(6) . . ? F6 C21 S2 112.5(5) . . ? F5 C21 S2 111.2(6) . . ? F4 C21 S2 110.3(6) . . ? N5 C22 C23 122.0(8) . . ? N5 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C24 C23 C22 119.5(8) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C25 C24 C23 119.5(7) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C26 119.8(8) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? N5 C26 C25 120.4(7) . . ? N5 C26 C27 116.9(5) . . ? C25 C26 C27 122.7(6) . . ? N8 C27 O14 119.6(7) . . ? N8 C27 C26 112.5(5) . . ? O14 C27 C26 102.9(7) . . ? N8 C27 H27 107.0 . . ? O14 C27 H27 107.0 . . ? C26 C27 H27 107.0 . . ? N8 C29 C30 116.9(6) . . ? N8 C29 C34 105.3(5) . . ? C30 C29 C34 110.6(5) . . ? N8 C29 H29 107.9 . . ? C30 C29 H29 107.9 . . ? C34 C29 H29 107.9 . . ? C29 C30 C31 109.7(6) . . ? C29 C30 H30A 109.7 . . ? C31 C30 H30A 109.7 . . ? C29 C30 H30B 109.7 . . ? C31 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? C32 C31 C30 110.3(6) . . ? C32 C31 H31A 109.6 . . ? C30 C31 H31A 109.6 . . ? C32 C31 H31B 109.6 . . ? C30 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? C33 C32 C31 114.3(7) . . ? C33 C32 H32A 108.7 . . ? C31 C32 H32A 108.7 . . ? C33 C32 H32B 108.7 . . ? C31 C32 H32B 108.7 . . ? H32A C32 H32B 107.6 . . ? C32 C33 C34 107.3(6) . . ? C32 C33 H33A 110.3 . . ? C34 C33 H33A 110.3 . . ? C32 C33 H33B 110.3 . . ? C34 C33 H33B 110.3 . . ? H33A C33 H33B 108.5 . . ? N7 C34 C29 107.5(5) . . ? N7 C34 C33 116.2(5) . . ? C29 C34 C33 112.2(5) . . ? N7 C34 H34 106.8 . . ? C29 C34 H34 106.8 . . ? C33 C34 H34 106.8 . . ? N7 C35 C36 114.8(6) . . ? N7 C35 H2A 132(4) . . ? C36 C35 H2A 110(4) . . ? N6 C36 C37 122.7(6) . . ? N6 C36 C35 115.2(5) . . ? C37 C36 C35 122.1(6) . . ? C38 C37 C36 118.4(7) . . ? C38 C37 H37 120.8 . . ? C36 C37 H37 120.8 . . ? C39 C38 C37 118.9(6) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C38 C39 C40 119.3(7) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.4 . . ? N6 C40 C39 122.5(6) . . ? N6 C40 H40 118.8 . . ? C39 C40 H40 118.8 . . ? F7 C41 F8 112.2(9) . . ? F7 C41 F9 109.4(8) . . ? F8 C41 F9 106.1(9) . . ? F7 C41 S3 109.7(7) . . ? F8 C41 S3 109.6(6) . . ? F9 C41 S3 109.7(7) . . ? F12 C42 F11 107.0(9) . . ? F12 C42 F10 105.8(8) . . ? F11 C42 F10 109.9(9) . . ? F12 C42 S4 111.8(7) . . ? F11 C42 S4 111.8(7) . . ? F10 C42 S4 110.3(7) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.681 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.118 #===END data_EtOH _database_code_depnum_ccdc_archive 'CCDC 804590' #TrackingRef '- All.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration ad _chemical_formula_moiety ? _chemical_formula_sum 'C21.70 H25.10 Cu F6 N4 O6.85 S2' _chemical_formula_weight 693.22 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 Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.8420(3) _cell_length_b 11.6520(4) _cell_length_c 14.8430(5) _cell_angle_alpha 98.123(2) _cell_angle_beta 93.505(2) _cell_angle_gamma 111.186(2) _cell_volume 1401.10(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 38553 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 706 _exptl_absorpt_coefficient_mu 1.016 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8226 _exptl_absorpt_correction_T_max 0.9509 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18888 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0786 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.20 _diffrn_reflns_theta_max 27.47 _reflns_number_total 10538 _reflns_number_gt 8907 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+2.3290P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.017(15) _refine_ls_number_reflns 10538 _refine_ls_number_parameters 760 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1449 _refine_ls_wR_factor_gt 0.1340 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.60733(7) 0.17426(6) 1.04584(5) 0.03075(18) Uani 1 1 d . . . S1 S 0.8208(2) 0.39536(16) 1.24696(11) 0.0377(4) Uani 1 1 d . . . F1 F 0.7676(6) 0.5259(4) 1.1283(3) 0.0625(13) Uani 1 1 d . . . O1 O 0.8003(6) 0.2982(5) 1.1694(3) 0.0393(11) Uani 1 1 d . . . N1 N 0.7442(6) 0.2898(6) 0.9637(4) 0.0316(12) Uani 1 1 d . . . C1 C 0.7336(8) 0.3907(7) 0.9357(4) 0.0348(14) Uani 1 1 d . . . H1 H 0.6378 0.4083 0.9431 0.042 Uiso 1 1 calc R . . Cu2 Cu 1.07595(7) 0.30496(6) 0.60554(5) 0.03227(18) Uani 1 1 d . . . S2 S 0.25865(19) 0.00878(16) 0.85458(11) 0.0341(4) Uani 1 1 d . . . F2 F 1.0207(7) 0.5545(6) 1.1597(5) 0.0812(18) Uani 1 1 d . . . N2 N 0.4217(6) 0.2206(6) 1.0842(4) 0.0327(12) Uani 1 1 d . . . C2 C 0.8599(9) 0.4716(7) 0.8954(5) 0.0399(15) Uani 1 1 d . . . H2 H 0.8492 0.5431 0.8764 0.048 Uiso 1 1 calc R . . S3 S 1.41009(19) 0.45579(17) 0.79087(12) 0.0357(4) Uani 1 1 d . . . F3 F 0.9024(8) 0.6373(4) 1.2555(4) 0.0740(15) Uani 1 1 d . . . O3 O 0.9588(8) 0.4172(6) 1.3117(4) 0.0590(15) Uani 1 1 d . . . N3 N 0.5186(6) 0.0359(5) 1.1195(4) 0.0299(11) Uani 1 1 d . . . H3A H 0.5688 0.0646 1.1796 0.036 Uiso 1 1 calc R . . C3 C 0.9989(8) 0.4472(7) 0.8837(5) 0.0397(16) Uani 1 1 d . . . H3 H 1.0865 0.5027 0.8583 0.048 Uiso 1 1 calc R . . S4 S 0.86619(18) 0.11412(16) 0.37848(11) 0.0339(3) Uani 1 1 d . . . F4 F 0.2164(7) -0.2208(6) 0.7830(5) 0.093(2) Uani 1 1 d . . . O4 O 0.2613(7) 0.0308(7) 0.7631(4) 0.0617(17) Uani 1 1 d . . . N4 N 0.7668(7) 0.0972(5) 1.0232(4) 0.0303(11) Uani 1 1 d . . . C4 C 1.0092(8) 0.3406(7) 0.9094(5) 0.0362(15) Uani 1 1 d . . . H4 H 1.1029 0.3206 0.9001 0.043 Uiso 1 1 calc R . . F5 F -0.0066(6) -0.1937(5) 0.8054(4) 0.0670(14) Uani 1 1 d . . . O5 O 0.4148(6) 0.0274(5) 0.9025(3) 0.0408(11) Uani 1 1 d . . . N6 N 0.9196(6) 0.1737(6) 0.6703(4) 0.0324(12) Uani 1 1 d . . . C5 C 0.8824(8) 0.2633(7) 0.9486(4) 0.0308(13) Uani 1 1 d . . . F6 F 0.1494(8) -0.2009(5) 0.9185(5) 0.097(2) Uani 1 1 d . . . O6 O 0.1595(6) 0.0562(6) 0.9082(4) 0.0503(13) Uani 1 1 d . . . N5 N 1.2472(7) 0.2518(6) 0.5542(4) 0.0353(13) Uani 1 1 d . . . C6 C 0.8824(8) 0.1503(7) 0.9805(5) 0.0339(14) Uani 1 1 d . . . H6 H 0.9659 0.1187 0.9692 0.041 Uiso 1 1 calc R . . F7 F 1.5060(7) 0.6338(6) 0.6948(4) 0.0837(18) Uani 1 1 d . . . O7 O 0.2611(5) -0.0639(5) 1.1807(3) 0.0386(10) Uani 1 1 d . . . N8 N 1.1724(8) 0.4484(7) 0.5405(5) 0.0476(16) Uani 1 1 d . . . H7A H 1.2569 0.5079 0.5818 0.057 Uiso 0.70 1 calc PR . . C7 C 0.7467(7) -0.0112(6) 1.0686(4) 0.0305(13) Uani 1 1 d . . . H7 H 0.8084 0.0204 1.1315 0.037 Uiso 1 1 calc R . . F8 F 1.6707(6) 0.6636(5) 0.8153(4) 0.0705(15) Uani 1 1 d . . . O8 O 1.2485(6) 0.4266(6) 0.7437(3) 0.0459(13) Uani 1 1 d . . . N7 N 0.9252(7) 0.3882(6) 0.6365(4) 0.0326(12) Uani 1 1 d . . . C8 C 0.8057(9) -0.1093(7) 1.0196(5) 0.0433(16) Uani 1 1 d . . . H8A H 0.7481 -0.1404 0.9565 0.052 Uiso 1 1 calc R . . H8B H 0.9242 -0.0704 1.0154 0.052 Uiso 1 1 calc R . . F9 F 1.4477(7) 0.6921(5) 0.8279(5) 0.0843(18) Uani 1 1 d . . . O9 O 1.5084(6) 0.3947(5) 0.7448(4) 0.0475(13) Uani 1 1 d . . . C9 C 0.7739(11) -0.2175(8) 1.0708(6) 0.052(2) Uani 1 1 d . . . H9A H 0.8396 -0.1878 1.1319 0.062 Uiso 1 1 calc R . . H9B H 0.8076 -0.2818 1.0366 0.062 Uiso 1 1 calc R . . F10 F 0.9397(8) -0.0267(5) 0.4825(4) 0.0761(16) Uani 1 1 d . . . O10 O 1.4145(6) 0.4593(5) 0.8885(4) 0.0433(12) Uani 1 1 d . . . C10 C 0.5908(9) -0.2755(7) 1.0824(5) 0.0482(16) Uani 1 1 d . . . H10A H 0.5262 -0.3115 1.0213 0.058 Uiso 1 1 calc R . . H10B H 0.5727 -0.3442 1.1180 0.058 Uiso 1 1 calc R . . F11 F 0.6824(8) -0.0625(6) 0.4586(4) 0.0825(18) Uani 1 1 d . . . O11 O 0.7283(6) 0.0893(5) 0.3124(3) 0.0481(12) Uani 1 1 d . . . C11 C 0.5317(9) -0.1773(7) 1.1321(5) 0.0381(15) Uani 1 1 d . . . H11A H 0.4133 -0.2158 1.1366 0.046 Uiso 1 1 calc R . . H11B H 0.5902 -0.1453 1.1949 0.046 Uiso 1 1 calc R . . F12 F 0.8053(7) -0.1257(5) 0.3502(4) 0.0722(14) Uani 1 1 d . . . O12 O 1.0179(6) 0.1340(6) 0.3418(4) 0.0542(13) Uani 1 1 d . . . C12 C 0.5646(7) -0.0699(6) 1.0784(4) 0.0320(12) Uani 1 1 d . . . H12 H 0.5032 -0.1045 1.0156 0.038 Uiso 1 1 calc R . . O13 O 0.8769(6) 0.1981(5) 0.4605(3) 0.0408(11) Uani 1 1 d . . . C13 C 0.3420(6) 0.0084(6) 1.1189(4) 0.0328(12) Uani 1 1 d . . . H13 H 0.2901 -0.0404 1.0566 0.039 Uiso 1 1 calc R . . O14 O 1.3745(7) 0.5123(6) 0.4409(4) 0.0332(13) Uani 0.70 1 d P . . C14 C 0.3164(7) 0.1332(6) 1.1247(4) 0.0344(13) Uani 1 1 d . . . C15 C 0.1873(7) 0.1514(7) 1.1632(5) 0.0399(14) Uani 1 1 d . . . H15 H 0.1145 0.0885 1.1912 0.048 Uiso 1 1 calc R . . C16 C 0.1647(9) 0.2619(8) 1.1606(5) 0.0454(18) Uani 1 1 d . . . H16 H 0.0788 0.2773 1.1890 0.054 Uiso 1 1 calc R . . C17 C 0.2689(9) 0.3508(8) 1.1161(6) 0.0460(18) Uani 1 1 d . . . H17 H 0.2522 0.4258 1.1107 0.055 Uiso 1 1 calc R . . C18 C 0.3994(9) 0.3268(7) 1.0795(5) 0.0384(15) Uani 1 1 d . . . H18 H 0.4737 0.3879 1.0507 0.046 Uiso 1 1 calc R . . C19 C 0.3181(9) -0.0164(8) 1.2769(5) 0.0490(18) Uani 1 1 d . . . H19A H 0.3034 0.0636 1.2953 0.059 Uiso 1 1 calc R . . H19B H 0.4358 -0.0012 1.2889 0.059 Uiso 1 1 calc R . . C20 C 0.2232(15) -0.1095(10) 1.3292(7) 0.084(3) Uani 1 1 d . . . H20A H 0.1075 -0.1215 1.3187 0.126 Uiso 1 1 calc R . . H20B H 0.2625 -0.0804 1.3946 0.126 Uiso 1 1 calc R . . H20C H 0.2360 -0.1890 1.3091 0.126 Uiso 1 1 calc R . . C21 C 0.8810(10) 0.5351(7) 1.1946(5) 0.0435(16) Uani 1 1 d . . . C22 C 0.1497(11) -0.1597(9) 0.8412(6) 0.057(2) Uani 1 1 d . . . C23 C 0.9217(8) 0.0675(7) 0.6907(5) 0.0404(16) Uani 1 1 d . . . H23 H 1.0116 0.0450 0.6762 0.049 Uiso 1 1 calc R . . C24 C 0.7987(9) -0.0142(8) 0.7328(6) 0.0457(17) Uani 1 1 d . . . H24 H 0.8063 -0.0887 0.7476 0.055 Uiso 1 1 calc R . . C25 C 0.6668(9) 0.0177(8) 0.7517(5) 0.0430(17) Uani 1 1 d . . . H25 H 0.5791 -0.0364 0.7779 0.052 Uiso 1 1 calc R . . C26 C 0.6636(8) 0.1306(8) 0.7320(5) 0.0396(16) Uani 1 1 d . . . H26 H 0.5752 0.1555 0.7458 0.048 Uiso 1 1 calc R . . C27 C 0.7916(8) 0.2052(7) 0.6920(4) 0.0336(14) Uani 1 1 d . . . C28 C 0.7974(8) 0.3275(7) 0.6709(5) 0.0324(14) Uani 1 1 d . . . H28 H 0.7130 0.3581 0.6821 0.039 Uiso 1 1 calc R . . C29 C 0.9684(8) 0.5112(6) 0.6124(4) 0.0343(13) Uani 1 1 d . . . H29 H 1.0527 0.5719 0.6619 0.041 Uiso 1 1 calc R . . C30 C 0.8287(9) 0.5581(7) 0.6015(5) 0.0433(16) Uani 1 1 d . . . H30A H 0.7820 0.5638 0.6601 0.052 Uiso 1 1 calc R . . H30B H 0.7412 0.4985 0.5542 0.052 Uiso 1 1 calc R . . C31 C 0.8935(12) 0.6880(8) 0.5729(6) 0.052(2) Uani 1 1 d . . . H31A H 0.8016 0.7160 0.5627 0.063 Uiso 1 1 calc R . . H31B H 0.9731 0.7490 0.6230 0.063 Uiso 1 1 calc R . . C32 C 0.9752(11) 0.6848(8) 0.4859(5) 0.0545(18) Uani 1 1 d . . . H32A H 1.0191 0.7699 0.4707 0.065 Uiso 1 1 calc R . . H32B H 0.8931 0.6296 0.4344 0.065 Uiso 1 1 calc R . . C33 C 1.1152(10) 0.6366(7) 0.4975(6) 0.0459(17) Uani 1 1 d . . . H33A H 1.1633 0.6318 0.4392 0.055 Uiso 1 1 calc R . . H33B H 1.2020 0.6955 0.5454 0.055 Uiso 1 1 calc R . . C34 C 1.0499(8) 0.5073(6) 0.5245(5) 0.0381(13) Uani 1 1 d . . . H34 H 0.9643 0.4500 0.4743 0.046 Uiso 1 1 calc R . . C35 C 1.2465(7) 0.4136(6) 0.4667(4) 0.0359(13) Uani 1 1 d . . . H35 H 1.1610 0.3730 0.4126 0.043 Uiso 1 1 calc R . . C36 C 1.3162(7) 0.3201(7) 0.4898(4) 0.0394(15) Uani 1 1 d . . . C37 C 1.4443(8) 0.3009(8) 0.4475(5) 0.0522(19) Uani 1 1 d . . . H37 H 1.4949 0.3499 0.4038 0.063 Uiso 1 1 calc R . . C38 C 1.4965(10) 0.2067(10) 0.4715(6) 0.060(2) Uani 1 1 d . . . H38 H 1.5800 0.1891 0.4420 0.073 Uiso 1 1 calc R . . C39 C 1.4275(9) 0.1425(9) 0.5360(6) 0.052(2) Uani 1 1 d . . . H39 H 1.4637 0.0805 0.5535 0.063 Uiso 1 1 calc R . . C40 C 1.3043(9) 0.1665(7) 0.5767(5) 0.0408(16) Uani 1 1 d . . . H40 H 1.2576 0.1206 0.6228 0.049 Uiso 1 1 calc R . . C41 C 1.3659(12) 0.5145(10) 0.3454(6) 0.040(2) Uani 0.70 1 d P . . H41A H 1.2581 0.5138 0.3222 0.048 Uiso 0.70 1 calc PR . . H41B H 1.3803 0.4401 0.3119 0.048 Uiso 0.70 1 calc PR . . C42 C 1.4997(14) 0.6317(12) 0.3311(9) 0.058(3) Uani 0.70 1 d P . . H42A H 1.4793 0.7048 0.3602 0.087 Uiso 0.70 1 calc PR . . H42B H 1.5023 0.6324 0.2652 0.087 Uiso 0.70 1 calc PR . . H42C H 1.6050 0.6345 0.3585 0.087 Uiso 0.70 1 calc PR . . C43 C 1.5132(10) 0.6196(8) 0.7823(6) 0.053(2) Uani 1 1 d . . . C44 C 0.8189(11) -0.0329(8) 0.4207(6) 0.0536(19) Uani 1 1 d . . . O2 O 0.6705(8) 0.3900(6) 1.2831(5) 0.0705(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0219(3) 0.0350(4) 0.0390(4) 0.0091(3) 0.0082(3) 0.0133(3) S1 0.0430(8) 0.0397(9) 0.0336(8) 0.0053(7) 0.0053(6) 0.0195(7) F1 0.081(3) 0.051(3) 0.059(3) 0.009(2) -0.019(2) 0.033(2) O1 0.036(2) 0.047(3) 0.037(2) 0.002(2) -0.0008(18) 0.022(2) N1 0.021(2) 0.043(3) 0.030(3) 0.005(2) 0.0015(19) 0.012(2) C1 0.031(3) 0.044(4) 0.035(3) 0.009(3) 0.004(2) 0.020(3) Cu2 0.0236(4) 0.0425(4) 0.0354(4) 0.0092(3) 0.0076(3) 0.0163(3) S2 0.0231(7) 0.0440(9) 0.0376(8) 0.0082(7) 0.0039(6) 0.0152(7) F2 0.058(3) 0.077(4) 0.120(5) 0.049(4) 0.041(3) 0.022(3) N2 0.020(2) 0.042(3) 0.035(3) 0.005(2) 0.001(2) 0.011(2) C2 0.039(3) 0.043(4) 0.040(4) 0.012(3) 0.007(3) 0.016(3) S3 0.0214(7) 0.0462(10) 0.0403(9) 0.0043(7) 0.0036(6) 0.0149(7) F3 0.110(4) 0.037(2) 0.069(3) 0.001(2) -0.005(3) 0.026(3) O3 0.075(4) 0.053(3) 0.045(3) 0.000(2) -0.022(3) 0.027(3) N3 0.021(2) 0.033(3) 0.034(3) 0.001(2) 0.004(2) 0.009(2) C3 0.029(3) 0.043(4) 0.041(4) 0.010(3) 0.006(3) 0.005(3) S4 0.0271(7) 0.0406(9) 0.0335(8) 0.0026(6) 0.0013(6) 0.0137(6) F4 0.071(4) 0.079(4) 0.121(5) -0.044(4) -0.033(3) 0.051(3) O4 0.042(3) 0.109(5) 0.045(3) 0.029(3) 0.009(2) 0.035(3) N4 0.025(3) 0.030(3) 0.033(3) 0.002(2) 0.001(2) 0.008(2) C4 0.026(3) 0.047(4) 0.034(3) 0.007(3) 0.007(3) 0.012(3) F5 0.036(2) 0.060(3) 0.087(4) 0.002(3) -0.011(2) 0.004(2) O5 0.027(2) 0.057(3) 0.038(3) 0.004(2) 0.0007(18) 0.018(2) N6 0.019(2) 0.045(3) 0.035(3) 0.006(2) 0.002(2) 0.014(2) C5 0.022(3) 0.042(4) 0.031(3) 0.003(3) 0.004(2) 0.016(3) F6 0.111(5) 0.051(3) 0.092(4) 0.031(3) -0.038(4) -0.012(3) O6 0.031(2) 0.058(3) 0.064(3) -0.001(3) 0.009(2) 0.023(2) N5 0.025(3) 0.042(3) 0.039(3) 0.001(2) 0.000(2) 0.015(2) C6 0.022(3) 0.043(4) 0.037(3) 0.003(3) 0.004(3) 0.014(3) F7 0.065(3) 0.090(4) 0.095(4) 0.053(4) 0.011(3) 0.014(3) O7 0.028(2) 0.046(3) 0.034(2) 0.007(2) 0.0043(17) 0.0056(19) N8 0.049(4) 0.048(4) 0.057(4) 0.020(3) 0.021(3) 0.025(3) C7 0.027(3) 0.033(3) 0.036(3) 0.008(3) 0.005(2) 0.015(2) F8 0.030(2) 0.054(3) 0.115(5) 0.002(3) 0.001(2) 0.007(2) O8 0.023(2) 0.070(4) 0.044(3) 0.004(2) -0.0003(19) 0.019(2) N7 0.024(3) 0.050(3) 0.026(3) 0.006(2) 0.002(2) 0.017(2) C8 0.039(4) 0.041(4) 0.057(4) 0.008(3) 0.015(3) 0.021(3) F9 0.065(3) 0.059(3) 0.141(6) 0.013(3) 0.012(3) 0.038(3) O9 0.032(2) 0.052(3) 0.062(3) -0.003(2) 0.008(2) 0.023(2) C9 0.059(5) 0.046(4) 0.066(5) 0.019(4) 0.019(4) 0.032(4) F10 0.106(4) 0.069(3) 0.062(3) 0.009(3) -0.022(3) 0.049(3) O10 0.030(2) 0.059(3) 0.045(3) 0.008(2) 0.001(2) 0.022(2) C10 0.059(4) 0.039(4) 0.055(4) 0.014(3) 0.012(3) 0.026(3) F11 0.079(4) 0.064(3) 0.097(4) 0.028(3) 0.038(3) 0.008(3) O11 0.043(3) 0.055(3) 0.042(3) 0.004(2) -0.012(2) 0.017(2) C11 0.039(3) 0.037(4) 0.036(3) 0.005(3) 0.004(3) 0.012(3) F12 0.092(4) 0.046(3) 0.075(3) -0.007(2) -0.009(3) 0.031(3) O12 0.037(2) 0.062(4) 0.063(3) 0.003(3) 0.013(2) 0.020(2) C12 0.028(3) 0.033(3) 0.031(3) -0.002(2) 0.000(2) 0.010(2) O13 0.037(2) 0.049(3) 0.035(2) 0.002(2) 0.0003(19) 0.017(2) C13 0.022(2) 0.038(3) 0.035(3) 0.008(2) 0.004(2) 0.007(2) O14 0.027(3) 0.032(3) 0.036(3) 0.007(3) 0.007(2) 0.005(2) C14 0.025(3) 0.044(4) 0.030(3) 0.002(3) 0.003(2) 0.010(3) C15 0.022(3) 0.053(4) 0.040(3) 0.005(3) 0.001(2) 0.010(3) C16 0.027(3) 0.056(5) 0.053(4) 0.000(3) 0.010(3) 0.018(3) C17 0.036(4) 0.050(4) 0.057(5) 0.009(4) 0.010(3) 0.021(3) C18 0.029(3) 0.041(4) 0.048(4) 0.009(3) 0.005(3) 0.017(3) C19 0.036(3) 0.062(5) 0.041(4) 0.011(3) 0.007(3) 0.008(3) C20 0.103(8) 0.068(7) 0.049(5) 0.012(5) 0.014(5) -0.007(6) C21 0.054(4) 0.039(4) 0.039(4) 0.009(3) 0.004(3) 0.019(3) C22 0.052(5) 0.063(5) 0.056(5) 0.002(4) -0.012(4) 0.026(4) C23 0.027(3) 0.053(4) 0.049(4) 0.016(3) 0.009(3) 0.020(3) C24 0.041(4) 0.050(4) 0.056(4) 0.019(3) 0.015(3) 0.024(3) C25 0.035(3) 0.056(5) 0.044(4) 0.015(3) 0.015(3) 0.020(3) C26 0.023(3) 0.053(4) 0.046(4) 0.010(3) 0.011(3) 0.017(3) C27 0.026(3) 0.045(4) 0.030(3) 0.005(3) 0.003(2) 0.015(3) C28 0.022(3) 0.046(4) 0.031(3) 0.000(3) -0.001(2) 0.018(3) C29 0.033(3) 0.036(3) 0.034(3) 0.001(3) 0.000(2) 0.016(3) C30 0.041(4) 0.051(4) 0.048(4) 0.014(3) 0.011(3) 0.027(3) C31 0.072(6) 0.050(5) 0.054(5) 0.015(4) 0.016(4) 0.041(4) C32 0.077(5) 0.056(5) 0.045(4) 0.017(3) 0.014(4) 0.038(4) C33 0.048(4) 0.040(4) 0.056(4) 0.012(3) 0.013(3) 0.021(3) C34 0.043(3) 0.037(3) 0.039(3) 0.007(3) 0.013(3) 0.018(3) C35 0.028(3) 0.045(3) 0.031(3) 0.009(3) 0.007(2) 0.007(2) C36 0.020(3) 0.057(4) 0.034(3) -0.004(3) 0.003(2) 0.011(3) C37 0.025(3) 0.076(5) 0.047(4) -0.006(4) 0.010(3) 0.013(3) C38 0.032(4) 0.084(6) 0.063(5) -0.022(5) -0.001(3) 0.033(4) C39 0.033(4) 0.075(6) 0.052(5) -0.011(4) -0.006(3) 0.036(4) C40 0.030(3) 0.048(4) 0.046(4) -0.005(3) -0.002(3) 0.023(3) C41 0.035(4) 0.049(6) 0.033(5) 0.007(4) 0.005(4) 0.012(4) C42 0.053(6) 0.052(7) 0.071(8) 0.029(6) 0.030(6) 0.013(5) C43 0.036(4) 0.050(5) 0.075(6) 0.013(4) 0.005(4) 0.018(3) C44 0.064(5) 0.051(5) 0.046(4) 0.010(4) -0.004(4) 0.023(4) O2 0.075(4) 0.065(4) 0.091(5) 0.024(3) 0.051(4) 0.040(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 1.948(6) . ? Cu1 N2 1.994(6) . ? Cu1 N3 2.024(5) . ? Cu1 N1 2.056(5) . ? Cu1 O1 2.335(5) . ? S1 O3 1.428(6) . ? S1 O2 1.447(6) . ? S1 O1 1.448(5) . ? S1 C21 1.822(7) . ? F1 C21 1.326(8) . ? N1 C1 1.334(9) . ? N1 C5 1.387(8) . ? C1 C2 1.404(10) . ? C1 H1 0.9500 . ? Cu2 N7 1.952(6) . ? Cu2 N5 1.985(6) . ? Cu2 N8 1.995(6) . ? Cu2 N6 2.055(5) . ? Cu2 O8 2.403(5) . ? S2 O4 1.417(6) . ? S2 O6 1.421(6) . ? S2 O5 1.442(5) . ? S2 C22 1.822(10) . ? F2 C21 1.325(9) . ? N2 C18 1.332(9) . ? N2 C14 1.350(8) . ? C2 C3 1.374(10) . ? C2 H2 0.9500 . ? S3 O10 1.442(6) . ? S3 O8 1.451(5) . ? S3 O9 1.453(5) . ? S3 C43 1.821(9) . ? F3 C21 1.335(9) . ? N3 C13 1.475(7) . ? N3 C12 1.497(8) . ? N3 H3A 0.9300 . ? C3 C4 1.381(10) . ? C3 H3 0.9500 . ? S4 O13 1.425(5) . ? S4 O12 1.431(5) . ? S4 O11 1.432(5) . ? S4 C44 1.821(8) . ? F4 C22 1.339(11) . ? N4 C6 1.251(9) . ? N4 C7 1.475(8) . ? C4 C5 1.381(9) . ? C4 H4 0.9500 . ? F5 C22 1.343(9) . ? N6 C23 1.320(9) . ? N6 C27 1.353(9) . ? C5 C6 1.460(9) . ? F6 C22 1.305(10) . ? N5 C40 1.339(9) . ? N5 C36 1.362(9) . ? C6 H6 0.9500 . ? F7 C43 1.333(11) . ? O7 C13 1.388(7) . ? O7 C19 1.444(9) . ? N8 C35 1.395(9) . ? N8 C34 1.501(9) . ? N8 H7A 0.9300 . ? C7 C12 1.530(8) . ? C7 C8 1.533(9) . ? C7 H7 1.0000 . ? F8 C43 1.331(9) . ? N7 C28 1.278(9) . ? N7 C29 1.447(9) . ? C8 C9 1.513(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? F9 C43 1.321(11) . ? C9 C10 1.544(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? F10 C44 1.340(9) . ? C10 C11 1.538(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? F11 C44 1.316(10) . ? C11 C12 1.528(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? F12 C44 1.360(10) . ? C12 H12 1.0000 . ? C13 C14 1.543(9) . ? C13 H13 1.0000 . ? O14 C35 1.409(8) . ? O14 C41 1.420(11) . ? C14 C15 1.377(9) . ? C15 C16 1.377(11) . ? C15 H15 0.9500 . ? C16 C17 1.391(12) . ? C16 H16 0.9500 . ? C17 C18 1.404(11) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.464(12) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C23 C24 1.408(10) . ? C23 H23 0.9500 . ? C24 C25 1.379(10) . ? C24 H24 0.9500 . ? C25 C26 1.397(11) . ? C25 H25 0.9500 . ? C26 C27 1.381(9) . ? C26 H26 0.9500 . ? C27 C28 1.485(10) . ? C28 H28 0.9500 . ? C29 C30 1.529(9) . ? C29 C34 1.531(9) . ? C29 H29 1.0000 . ? C30 C31 1.544(11) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.520(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.543(10) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.528(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34 1.0000 . ? C35 C36 1.500(10) . ? C35 H35 1.0000 . ? C36 C37 1.399(9) . ? C37 C38 1.414(13) . ? C37 H37 0.9500 . ? C38 C39 1.339(14) . ? C38 H38 0.9500 . ? C39 C40 1.373(11) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.502(14) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? 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_3 _geom_angle_publ_flag N4 Cu1 N2 166.8(2) . . ? N4 Cu1 N3 82.8(2) . . ? N2 Cu1 N3 84.0(2) . . ? N4 Cu1 N1 80.6(2) . . ? N2 Cu1 N1 112.5(2) . . ? N3 Cu1 N1 163.4(2) . . ? N4 Cu1 O1 83.8(2) . . ? N2 Cu1 O1 97.2(2) . . ? N3 Cu1 O1 91.1(2) . . ? N1 Cu1 O1 87.6(2) . . ? O3 S1 O2 117.2(4) . . ? O3 S1 O1 113.0(3) . . ? O2 S1 O1 114.4(4) . . ? O3 S1 C21 103.7(4) . . ? O2 S1 C21 104.1(4) . . ? O1 S1 C21 102.1(3) . . ? S1 O1 Cu1 140.1(3) . . ? C1 N1 C5 117.9(6) . . ? C1 N1 Cu1 131.4(5) . . ? C5 N1 Cu1 110.0(4) . . ? N1 C1 C2 121.9(6) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? N7 Cu2 N5 165.8(2) . . ? N7 Cu2 N8 83.1(3) . . ? N5 Cu2 N8 82.8(3) . . ? N7 Cu2 N6 80.9(2) . . ? N5 Cu2 N6 112.9(2) . . ? N8 Cu2 N6 163.2(2) . . ? N7 Cu2 O8 87.8(2) . . ? N5 Cu2 O8 94.2(2) . . ? N8 Cu2 O8 89.7(3) . . ? N6 Cu2 O8 94.9(2) . . ? O4 S2 O6 115.9(4) . . ? O4 S2 O5 115.4(3) . . ? O6 S2 O5 114.2(3) . . ? O4 S2 C22 103.4(4) . . ? O6 S2 C22 102.4(4) . . ? O5 S2 C22 102.7(3) . . ? C18 N2 C14 119.5(6) . . ? C18 N2 Cu1 127.9(5) . . ? C14 N2 Cu1 112.4(4) . . ? C3 C2 C1 119.9(6) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? O10 S3 O8 114.2(3) . . ? O10 S3 O9 115.9(3) . . ? O8 S3 O9 115.5(3) . . ? O10 S3 C43 102.8(4) . . ? O8 S3 C43 102.1(4) . . ? O9 S3 C43 103.7(4) . . ? C13 N3 C12 116.1(5) . . ? C13 N3 Cu1 107.2(4) . . ? C12 N3 Cu1 106.9(4) . . ? C13 N3 H3A 108.8 . . ? C12 N3 H3A 108.8 . . ? Cu1 N3 H3A 108.8 . . ? C2 C3 C4 118.9(6) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? O13 S4 O12 114.7(3) . . ? O13 S4 O11 115.2(3) . . ? O12 S4 O11 115.3(3) . . ? O13 S4 C44 101.4(3) . . ? O12 S4 C44 104.5(4) . . ? O11 S4 C44 103.2(3) . . ? C6 N4 C7 126.8(6) . . ? C6 N4 Cu1 117.9(5) . . ? C7 N4 Cu1 114.9(4) . . ? C5 C4 C3 119.5(7) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C23 N6 C27 117.5(6) . . ? C23 N6 Cu2 131.8(5) . . ? C27 N6 Cu2 110.7(4) . . ? C4 C5 N1 121.9(6) . . ? C4 C5 C6 124.1(6) . . ? N1 C5 C6 114.0(6) . . ? C40 N5 C36 119.0(6) . . ? C40 N5 Cu2 129.7(5) . . ? C36 N5 Cu2 111.2(5) . . ? N4 C6 C5 116.6(6) . . ? N4 C6 H6 121.7 . . ? C5 C6 H6 121.7 . . ? C13 O7 C19 117.1(5) . . ? C35 N8 C34 119.1(6) . . ? C35 N8 Cu2 110.3(5) . . ? C34 N8 Cu2 109.4(4) . . ? C35 N8 H7A 105.7 . . ? C34 N8 H7A 105.7 . . ? Cu2 N8 H7A 105.7 . . ? N4 C7 C12 106.1(5) . . ? N4 C7 C8 115.5(5) . . ? C12 C7 C8 110.5(5) . . ? N4 C7 H7 108.1 . . ? C12 C7 H7 108.1 . . ? C8 C7 H7 108.1 . . ? S3 O8 Cu2 140.6(3) . . ? C28 N7 C29 127.3(6) . . ? C28 N7 Cu2 117.7(5) . . ? C29 N7 Cu2 114.9(4) . . ? C9 C8 C7 110.7(6) . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C10 110.4(6) . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 111.3(7) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 109.1(5) . . ? C12 C11 H11A 109.9 . . ? C10 C11 H11A 109.9 . . ? C12 C11 H11B 109.9 . . ? C10 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? N3 C12 C11 115.7(5) . . ? N3 C12 C7 105.6(5) . . ? C11 C12 C7 110.6(5) . . ? N3 C12 H12 108.2 . . ? C11 C12 H12 108.2 . . ? C7 C12 H12 108.2 . . ? O7 C13 N3 117.6(5) . . ? O7 C13 C14 113.0(5) . . ? N3 C13 C14 107.8(5) . . ? O7 C13 H13 105.8 . . ? N3 C13 H13 105.8 . . ? C14 C13 H13 105.8 . . ? C35 O14 C41 114.6(6) . . ? N2 C14 C15 121.8(6) . . ? N2 C14 C13 115.9(5) . . ? C15 C14 C13 122.1(6) . . ? C14 C15 C16 119.3(6) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C15 C16 C17 119.4(7) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C16 C17 C18 118.2(8) . . ? C16 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? N2 C18 C17 121.6(7) . . ? N2 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? O7 C19 C20 108.1(7) . . ? O7 C19 H19A 110.1 . . ? C20 C19 H19A 110.1 . . ? O7 C19 H19B 110.1 . . ? C20 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? F2 C21 F1 108.5(6) . . ? F2 C21 F3 107.0(7) . . ? F1 C21 F3 107.2(6) . . ? F2 C21 S1 111.3(5) . . ? F1 C21 S1 111.0(5) . . ? F3 C21 S1 111.7(5) . . ? F6 C22 F4 107.8(8) . . ? F6 C22 F5 107.6(8) . . ? F4 C22 F5 106.2(7) . . ? F6 C22 S2 112.8(6) . . ? F4 C22 S2 110.9(7) . . ? F5 C22 S2 111.3(6) . . ? N6 C23 C24 123.8(6) . . ? N6 C23 H23 118.1 . . ? C24 C23 H23 118.1 . . ? C25 C24 C23 117.7(7) . . ? C25 C24 H24 121.1 . . ? C23 C24 H24 121.1 . . ? C24 C25 C26 119.2(7) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C27 C26 C25 118.5(7) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? N6 C27 C26 123.1(7) . . ? N6 C27 C28 115.6(6) . . ? C26 C27 C28 121.3(6) . . ? N7 C28 C27 114.6(6) . . ? N7 C28 H28 122.7 . . ? C27 C28 H28 122.7 . . ? N7 C29 C30 116.0(5) . . ? N7 C29 C34 106.2(5) . . ? C30 C29 C34 111.5(5) . . ? N7 C29 H29 107.6 . . ? C30 C29 H29 107.6 . . ? C34 C29 H29 107.6 . . ? C29 C30 C31 109.6(6) . . ? C29 C30 H30A 109.8 . . ? C31 C30 H30A 109.8 . . ? C29 C30 H30B 109.8 . . ? C31 C30 H30B 109.8 . . ? H30A C30 H30B 108.2 . . ? C32 C31 C30 111.4(7) . . ? C32 C31 H31A 109.4 . . ? C30 C31 H31A 109.4 . . ? C32 C31 H31B 109.4 . . ? C30 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C31 C32 C33 111.1(6) . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32B 109.4 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 109.9(6) . . ? C34 C33 H33A 109.7 . . ? C32 C33 H33A 109.7 . . ? C34 C33 H33B 109.7 . . ? C32 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? N8 C34 C33 116.5(6) . . ? N8 C34 C29 106.4(5) . . ? C33 C34 C29 110.7(6) . . ? N8 C34 H34 107.6 . . ? C33 C34 H34 107.6 . . ? C29 C34 H34 107.6 . . ? N8 C35 O14 115.1(6) . . ? N8 C35 C36 109.4(5) . . ? O14 C35 C36 107.1(5) . . ? N8 C35 H35 108.3 . . ? O14 C35 H35 108.3 . . ? C36 C35 H35 108.3 . . ? N5 C36 C37 120.5(7) . . ? N5 C36 C35 116.7(5) . . ? C37 C36 C35 122.8(6) . . ? C36 C37 C38 118.3(8) . . ? C36 C37 H37 120.8 . . ? C38 C37 H37 120.8 . . ? C39 C38 C37 119.6(8) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C40 119.8(9) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? N5 C40 C39 122.7(8) . . ? N5 C40 H40 118.6 . . ? C39 C40 H40 118.6 . . ? O14 C41 C42 107.7(9) . . ? O14 C41 H41A 110.2 . . ? C42 C41 H41A 110.2 . . ? O14 C41 H41B 110.2 . . ? C42 C41 H41B 110.2 . . ? H41A C41 H41B 108.5 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? F9 C43 F8 106.8(8) . . ? F9 C43 F7 108.3(7) . . ? F8 C43 F7 106.9(7) . . ? F9 C43 S3 112.2(6) . . ? F8 C43 S3 112.2(6) . . ? F7 C43 S3 110.2(6) . . ? F11 C44 F10 108.6(7) . . ? F11 C44 F12 109.4(7) . . ? F10 C44 F12 106.6(7) . . ? F11 C44 S4 111.5(6) . . ? F10 C44 S4 111.0(6) . . ? F12 C44 S4 109.6(5) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.736 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.080 #===END data_IPA _database_code_depnum_ccdc_archive 'CCDC 804591' #TrackingRef '- All.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration ad _chemical_formula_moiety ? _chemical_formula_sum 'C23 H28 Cu F6 N4 O7 S2' _chemical_formula_weight 714.15 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 Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.5699(3) _cell_length_b 11.4168(3) _cell_length_c 13.9033(4) _cell_angle_alpha 76.376(2) _cell_angle_beta 82.0610(10) _cell_angle_gamma 88.3080(10) _cell_volume 1462.14(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 57521 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 730 _exptl_absorpt_coefficient_mu 0.977 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8286 _exptl_absorpt_correction_T_max 0.9086 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27768 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.49 _reflns_number_total 12531 _reflns_number_gt 9930 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+1.8143P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.022(13) _refine_ls_number_reflns 12531 _refine_ls_number_parameters 775 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1343 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 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 Cu1 Cu 0.67623(6) 0.42376(5) 0.97972(4) 0.03441(18) Uani 1 1 d . . . S1 S 0.81443(17) 0.62545(16) 0.11644(12) 0.0386(4) Uani 1 1 d . . . F1 F 0.8245(7) 0.7434(5) -0.0686(3) 0.0873(18) Uani 1 1 d . . . O1 O 0.7799(7) 0.6612(5) 0.2091(4) 0.0659(16) Uani 1 1 d . . . N1 N 0.8590(5) 0.4683(5) 0.8881(4) 0.0313(12) Uani 1 1 d . . . C1 C 0.8852(7) 0.5531(6) 0.8007(4) 0.0339(13) Uani 1 1 d . . . H1 H 0.8108 0.6044 0.7779 0.041 Uiso 1 1 calc R . . Cu2 Cu 0.18317(6) 0.52603(5) 0.41108(4) 0.03366(18) Uani 1 1 d . . . S2 S 0.48682(17) 0.24569(15) 0.84963(12) 0.0364(4) Uani 1 1 d . . . F2 F 0.8865(6) 0.8458(4) 0.0248(4) 0.0902(19) Uani 1 1 d . . . O2 O 0.9575(5) 0.5911(6) 0.0934(5) 0.081(2) Uani 1 1 d . . . N2 N 0.5086(6) 0.5343(5) 0.9511(4) 0.0367(13) Uani 1 1 d . . . C2 C 1.0171(8) 0.5669(6) 0.7440(5) 0.0394(15) Uani 1 1 d . . . H2 H 1.0322 0.6263 0.6829 0.047 Uiso 1 1 calc R . . S3 S 0.04849(16) 0.30153(14) 0.28395(11) 0.0340(3) Uani 1 1 d . . . F3 F 0.6695(6) 0.8093(5) 0.0305(5) 0.114(3) Uani 1 1 d . . . O3 O 0.7104(6) 0.5459(5) 0.0994(4) 0.0480(11) Uani 1 1 d . . . N3 N 0.5316(5) 0.3321(5) 1.0794(4) 0.0348(11) Uani 1 1 d . . . C3 C 1.1253(7) 0.4944(6) 0.7765(5) 0.0370(15) Uani 1 1 d . . . H3 H 1.2162 0.5034 0.7382 0.044 Uiso 1 1 calc R . . S4 S 0.36871(17) 0.69632(15) 0.53438(12) 0.0355(3) Uani 1 1 d . . . F4 F 0.6288(7) 0.0546(5) 0.9218(5) 0.101(2) Uani 1 1 d . . . O4 O 0.4298(6) 0.2829(5) 0.7568(3) 0.0594(14) Uani 1 1 d . . . N4 N 0.7984(5) 0.2999(4) 1.0487(4) 0.0302(11) Uani 1 1 d . . . C4 C 1.1020(7) 0.4069(7) 0.8664(5) 0.0376(15) Uani 1 1 d . . . H4 H 1.1762 0.3563 0.8907 0.045 Uiso 1 1 calc R . . F5 F 0.6599(7) 0.1117(5) 0.7598(5) 0.104(2) Uani 1 1 d . . . O5 O 0.3829(5) 0.2175(4) 0.9377(3) 0.0418(10) Uani 1 1 d . . . N5 N 0.3503(5) 0.4153(5) 0.4370(4) 0.0323(12) Uani 1 1 d . . . C5 C 0.9652(7) 0.3963(6) 0.9195(5) 0.0340(14) Uani 1 1 d . . . F6 F 0.4696(7) 0.0219(4) 0.8379(5) 0.096(2) Uani 1 1 d . . . O6 O 0.6100(5) 0.3147(4) 0.8553(4) 0.0440(11) Uani 1 1 d . . . N6 N -0.0032(5) 0.4780(5) 0.5018(4) 0.0319(12) Uani 1 1 d . . . C6 C 0.9278(6) 0.3051(6) 1.0125(5) 0.0342(13) Uani 1 1 d . . . H6 H 0.9961 0.2531 1.0436 0.041 Uiso 1 1 calc R . . F7 F 0.2194(5) 0.1512(4) 0.3827(4) 0.0663(12) Uani 1 1 d . . . O7 O 0.1005(5) 0.2627(4) 0.1932(3) 0.0406(10) Uani 1 1 d . . . N7 N 0.0701(5) 0.6664(4) 0.3589(3) 0.0309(11) Uani 1 1 d . . . C7 C 0.7325(5) 0.2222(5) 1.1426(4) 0.0334(11) Uani 1 1 d . . . H7 H 0.7352 0.2654 1.1970 0.040 Uiso 1 1 calc R . . F8 F 0.0311(6) 0.1848(4) 0.4733(3) 0.0675(13) Uani 1 1 d . . . O8 O -0.1018(5) 0.3131(4) 0.3025(3) 0.0473(11) Uani 1 1 d . . . N8 N 0.3127(5) 0.5966(5) 0.2910(4) 0.0327(11) Uani 1 1 d . . . C8 C 0.7961(8) 0.0996(6) 1.1743(5) 0.0414(16) Uani 1 1 d . . . H8A H 0.8956 0.1078 1.1840 0.050 Uiso 1 1 calc R . . H8B H 0.7943 0.0545 1.1218 0.050 Uiso 1 1 calc R . . F9 F 0.0240(5) 0.0711(4) 0.3714(3) 0.0655(12) Uani 1 1 d . . . O9 O 0.1327(6) 0.3952(4) 0.3001(4) 0.0449(11) Uani 1 1 d . . . C9 C 0.7116(7) 0.0309(6) 1.2721(5) 0.0570(18) Uani 1 1 d . . . H9A H 0.7214 0.0723 1.3259 0.068 Uiso 1 1 calc R . . H9B H 0.7500 -0.0515 1.2913 0.068 Uiso 1 1 calc R . . F10 F 0.2111(5) 0.8158(4) 0.6445(4) 0.0653(12) Uani 1 1 d . . . O10 O 0.4535(6) 0.7305(5) 0.4395(4) 0.0554(13) Uani 1 1 d . . . C10 C 0.5525(7) 0.0234(6) 1.2607(5) 0.0605(18) Uani 1 1 d . . . H10A H 0.5421 -0.0249 1.2116 0.073 Uiso 1 1 calc R . . H10B H 0.4996 -0.0178 1.3256 0.073 Uiso 1 1 calc R . . F11 F 0.3859(6) 0.9182(4) 0.5537(5) 0.0842(16) Uani 1 1 d . . . O11 O 0.4459(5) 0.6553(4) 0.6179(4) 0.0452(11) Uani 1 1 d . . . C11 C 0.4912(8) 0.1476(7) 1.2265(5) 0.0455(17) Uani 1 1 d . . . H11A H 0.4955 0.1948 1.2773 0.055 Uiso 1 1 calc R . . H11B H 0.3912 0.1407 1.2175 0.055 Uiso 1 1 calc R . . F12 F 0.2059(7) 0.8809(6) 0.4880(5) 0.106(2) Uani 1 1 d . . . O12 O 0.2499(5) 0.6225(4) 0.5355(3) 0.0430(11) Uani 1 1 d . . . C12 C 0.5761(5) 0.2107(5) 1.1281(4) 0.0362(11) Uani 1 1 d . . . H12 H 0.5734 0.1582 1.0801 0.043 Uiso 1 1 calc R . . C13 C 0.4079(6) 0.3748(6) 1.0853(5) 0.0392(14) Uani 1 1 d . . . H13 H 0.3317 0.3349 1.1314 0.047 Uiso 1 1 calc R . . C14 C 0.3922(6) 0.4898(6) 1.0158(5) 0.0363(15) Uani 1 1 d . . . C15 C 0.2611(8) 0.5481(6) 1.0123(6) 0.0421(17) Uani 1 1 d . . . H15 H 0.1801 0.5171 1.0580 0.051 Uiso 1 1 calc R . . C16 C 0.2559(7) 0.6550(7) 0.9376(5) 0.0447(18) Uani 1 1 d . . . H16 H 0.1689 0.6965 0.9318 0.054 Uiso 1 1 calc R . . C17 C 0.3712(8) 0.6993(7) 0.8744(6) 0.0464(17) Uani 1 1 d . . . H17 H 0.3662 0.7715 0.8244 0.056 Uiso 1 1 calc R . . C18 C 0.4980(8) 0.6381(6) 0.8833(5) 0.0417(16) Uani 1 1 d . . . H18 H 0.5800 0.6709 0.8398 0.050 Uiso 1 1 calc R . . C19 C 0.3655(7) 0.3222(7) 0.5125(5) 0.0409(16) Uani 1 1 d . . . H19 H 0.2877 0.2980 0.5632 0.049 Uiso 1 1 calc R . . C20 C 0.4927(8) 0.2582(7) 0.5198(5) 0.0441(17) Uani 1 1 d . . . H20 H 0.5011 0.1924 0.5750 0.053 Uiso 1 1 calc R . . C21 C 0.6069(8) 0.2926(7) 0.4446(6) 0.0477(18) Uani 1 1 d . . . H21 H 0.6934 0.2496 0.4464 0.057 Uiso 1 1 calc R . . C22 C 0.5899(8) 0.3901(7) 0.3685(6) 0.0441(17) Uani 1 1 d . . . H22 H 0.6664 0.4164 0.3173 0.053 Uiso 1 1 calc R . . C23 C 0.4641(7) 0.4506(6) 0.3650(5) 0.0350(14) Uani 1 1 d . . . C24 C 0.4358(6) 0.5526(6) 0.2837(5) 0.0375(14) Uani 1 1 d . . . H24 H 0.5057 0.5838 0.2288 0.045 Uiso 1 1 calc R . . C25 C 0.2534(5) 0.6948(5) 0.2202(4) 0.0364(11) Uani 1 1 d . . . H25 H 0.1968 0.6577 0.1797 0.044 Uiso 1 1 calc R . . C26 C 0.3592(8) 0.7816(6) 0.1475(5) 0.0472(17) Uani 1 1 d . . . H26A H 0.4182 0.7378 0.1032 0.057 Uiso 1 1 calc R . . H26B H 0.4219 0.8156 0.1850 0.057 Uiso 1 1 calc R . . C27 C 0.2790(7) 0.8838(5) 0.0846(5) 0.0523(15) Uani 1 1 d . . . H27A H 0.3481 0.9432 0.0415 0.063 Uiso 1 1 calc R . . H27B H 0.2269 0.8500 0.0405 0.063 Uiso 1 1 calc R . . C28 C 0.1744(7) 0.9489(6) 0.1484(5) 0.0495(15) Uani 1 1 d . . . H28A H 0.1222 1.0104 0.1043 0.059 Uiso 1 1 calc R . . H28B H 0.2268 0.9905 0.1873 0.059 Uiso 1 1 calc R . . C29 C 0.0681(8) 0.8574(6) 0.2210(5) 0.0426(17) Uani 1 1 d . . . H29A H 0.0049 0.8992 0.2647 0.051 Uiso 1 1 calc R . . H29B H 0.0095 0.8206 0.1826 0.051 Uiso 1 1 calc R . . C30 C 0.1509(5) 0.7618(5) 0.2830(4) 0.0336(11) Uani 1 1 d . . . H30 H 0.2091 0.8035 0.3193 0.040 Uiso 1 1 calc R . . C31 C -0.0608(7) 0.6600(6) 0.3868(5) 0.0372(14) Uani 1 1 d . . . H31 H -0.1246 0.7176 0.3563 0.045 Uiso 1 1 calc R . . C32 C -0.1089(6) 0.5567(6) 0.4704(5) 0.0339(14) Uani 1 1 d . . . C33 C -0.2463(7) 0.5444(6) 0.5170(5) 0.0414(16) Uani 1 1 d . . . H33 H -0.3168 0.5990 0.4919 0.050 Uiso 1 1 calc R . . C34 C -0.2800(7) 0.4531(7) 0.5996(5) 0.0442(17) Uani 1 1 d . . . H34 H -0.3738 0.4438 0.6333 0.053 Uiso 1 1 calc R . . C35 C -0.1735(8) 0.3732(7) 0.6341(5) 0.0447(17) Uani 1 1 d . . . H35 H -0.1934 0.3094 0.6919 0.054 Uiso 1 1 calc R . . C36 C -0.0355(7) 0.3902(6) 0.5805(5) 0.0414(16) Uani 1 1 d . . . H36 H 0.0364 0.3354 0.6027 0.050 Uiso 1 1 calc R . . C37 C 0.7987(8) 0.7611(6) 0.0220(5) 0.0441(16) Uani 1 1 d . . . C38 C 0.5658(9) 0.1000(7) 0.8444(7) 0.062(2) Uani 1 1 d . . . C39 C 0.0835(8) 0.1694(6) 0.3829(5) 0.0448(16) Uani 1 1 d . . . C40 C 0.2901(9) 0.8327(7) 0.5578(6) 0.0553(19) Uani 1 1 d . . . O50 O 0.6798(12) 0.7566(11) 0.6810(8) 0.061(3) Uani 0.779(10) 1 d P A 1 H50 H 0.6106 0.7403 0.6552 0.091 Uiso 0.779(10) 1 calc PR A 1 C50 C 0.7188(9) 0.8692(6) 0.6413(11) 0.080(4) Uani 0.779(10) 1 d P A 1 H50A H 0.6392 0.9237 0.6563 0.096 Uiso 0.779(10) 1 calc PR A 1 C51 C 0.8449(8) 0.9030(8) 0.6792(6) 0.052(2) Uani 0.779(10) 1 d P A 1 H51A H 0.8259 0.8908 0.7519 0.078 Uiso 0.779(10) 1 calc PR A 1 H51B H 0.8677 0.9880 0.6490 0.078 Uiso 0.779(10) 1 calc PR A 1 H51C H 0.9246 0.8527 0.6617 0.078 Uiso 0.779(10) 1 calc PR A 1 C52 C 0.7586(11) 0.8909(11) 0.5221(7) 0.082(4) Uani 0.779(10) 1 d P A 1 H52A H 0.6774 0.8702 0.4933 0.123 Uiso 0.779(10) 1 calc PR A 1 H52B H 0.8388 0.8398 0.5069 0.123 Uiso 0.779(10) 1 calc PR A 1 H52C H 0.7838 0.9757 0.4935 0.123 Uiso 0.779(10) 1 calc PR A 1 O60 O 0.1658(9) 0.2137(7) 0.7259(6) 0.099(2) Uiso 1 1 d D . . H60 H 0.2014 0.1963 0.6724 0.149 Uiso 1 1 calc R . . C60 C 0.1110(17) 0.0991(15) 0.8016(13) 0.177(7) Uiso 1 1 d D . . H60A H 0.1747 0.0883 0.8543 0.213 Uiso 1 1 calc R . . C61 C -0.0369(7) 0.1108(6) 0.8580(5) 0.0492(15) Uiso 1 1 d D . . H61A H -0.0442 0.1881 0.8774 0.074 Uiso 1 1 calc R . . H61B H -0.0525 0.0448 0.9179 0.074 Uiso 1 1 calc R . . H61C H -0.1082 0.1069 0.8145 0.074 Uiso 1 1 calc R . . C62 C 0.171(2) 0.0217(14) 0.7376(15) 0.206(8) Uiso 1 1 d D . . H62A H 0.2685 0.0472 0.7102 0.308 Uiso 1 1 calc R . . H62B H 0.1152 0.0275 0.6828 0.308 Uiso 1 1 calc R . . H62C H 0.1711 -0.0619 0.7766 0.308 Uiso 1 1 calc R . . O50A O 0.699(3) 0.742(2) 0.662(2) 0.014(5) Uiso 0.221(10) 1 d P A 2 H50B H 0.6403 0.6931 0.6528 0.020 Uiso 0.221(10) 1 calc PR A 2 C50A C 0.7291(19) 0.840(2) 0.569(2) 0.028(5) Uiso 0.221(10) 1 d PD A 2 H50C H 0.6881 0.8249 0.5109 0.033 Uiso 0.221(10) 1 calc PR A 2 C51A C 0.8930(17) 0.8225(17) 0.5620(14) 0.018(5) Uiso 0.221(10) 1 d PD A 2 H51D H 0.9180 0.7444 0.5466 0.026 Uiso 0.221(10) 1 calc PR A 2 H51E H 0.9239 0.8251 0.6257 0.026 Uiso 0.221(10) 1 calc PR A 2 H51F H 0.9395 0.8872 0.5089 0.026 Uiso 0.221(10) 1 calc PR A 2 C52A C 0.687(2) 0.953(2) 0.5940(18) 0.035(6) Uiso 0.221(10) 1 d P A 2 H52D H 0.5844 0.9549 0.6102 0.052 Uiso 0.221(10) 1 calc PR A 2 H52E H 0.7179 1.0195 0.5367 0.052 Uiso 0.221(10) 1 calc PR A 2 H52F H 0.7313 0.9615 0.6516 0.052 Uiso 0.221(10) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0221(4) 0.0405(4) 0.0349(4) -0.0006(3) 0.0013(3) 0.0012(3) S1 0.0261(8) 0.0498(9) 0.0371(8) -0.0063(7) -0.0010(6) -0.0040(6) F1 0.149(5) 0.072(3) 0.038(2) -0.005(2) -0.012(3) -0.018(3) O1 0.087(4) 0.070(3) 0.041(3) -0.012(2) 0.000(3) -0.037(3) N1 0.027(3) 0.038(3) 0.030(3) -0.010(2) -0.001(2) 0.000(2) C1 0.030(3) 0.038(3) 0.028(3) -0.002(2) 0.008(2) 0.004(2) Cu2 0.0213(4) 0.0413(4) 0.0339(4) -0.0036(3) 0.0028(3) 0.0004(3) S2 0.0318(9) 0.0434(8) 0.0340(8) -0.0106(7) -0.0003(7) -0.0041(7) F2 0.129(5) 0.069(3) 0.066(3) 0.012(2) -0.025(3) -0.062(3) O2 0.019(2) 0.091(4) 0.105(4) 0.020(3) 0.010(2) 0.009(2) N2 0.027(3) 0.049(3) 0.035(3) -0.014(3) 0.002(2) 0.001(2) C2 0.038(3) 0.037(3) 0.043(4) -0.007(3) -0.004(3) -0.007(3) S3 0.0217(7) 0.0435(8) 0.0379(8) -0.0137(6) -0.0003(6) -0.0033(6) F3 0.060(3) 0.078(3) 0.159(6) 0.035(4) 0.021(3) 0.025(3) O3 0.046(3) 0.050(3) 0.049(3) -0.018(2) -0.002(2) -0.006(2) N3 0.030(2) 0.043(3) 0.032(2) -0.009(2) -0.0044(19) -0.007(2) C3 0.025(3) 0.049(4) 0.036(3) -0.011(3) 0.003(2) -0.006(3) S4 0.0272(8) 0.0422(8) 0.0366(8) -0.0095(7) -0.0017(7) -0.0017(6) F4 0.090(4) 0.057(3) 0.128(5) 0.018(3) 0.005(3) 0.030(3) O4 0.062(3) 0.077(4) 0.037(2) -0.006(2) -0.011(2) -0.020(3) N4 0.029(2) 0.029(2) 0.032(2) -0.0063(19) -0.0029(19) -0.0012(18) C4 0.024(3) 0.049(4) 0.044(4) -0.020(3) -0.004(3) 0.008(3) F5 0.098(4) 0.066(3) 0.131(5) -0.038(3) 0.067(4) 0.001(3) O5 0.025(2) 0.061(3) 0.039(2) -0.014(2) 0.0004(17) -0.0031(18) N5 0.023(3) 0.041(3) 0.033(3) -0.009(2) -0.005(2) 0.005(2) C5 0.029(3) 0.039(3) 0.034(3) -0.010(3) 0.000(3) -0.003(3) F6 0.110(5) 0.050(3) 0.124(5) -0.034(3) 0.036(4) -0.026(3) O6 0.030(2) 0.057(3) 0.049(3) -0.022(2) 0.001(2) -0.008(2) N6 0.026(3) 0.039(3) 0.032(3) -0.015(2) 0.004(2) -0.002(2) C6 0.022(3) 0.042(3) 0.039(3) -0.009(3) -0.005(2) 0.006(2) F7 0.045(2) 0.073(3) 0.074(3) 0.001(2) -0.018(2) 0.008(2) O7 0.033(2) 0.053(2) 0.036(2) -0.0173(19) 0.0050(17) -0.0063(17) N7 0.026(2) 0.039(3) 0.026(2) -0.0079(19) 0.0001(18) -0.0001(19) C7 0.031(3) 0.031(3) 0.036(3) -0.003(2) -0.004(2) -0.006(2) F8 0.088(3) 0.070(3) 0.038(2) -0.0064(19) 0.003(2) 0.004(2) O8 0.026(2) 0.062(3) 0.053(3) -0.014(2) -0.0013(18) 0.0022(18) N8 0.021(2) 0.041(3) 0.035(2) -0.010(2) -0.0002(18) -0.0019(18) C8 0.040(4) 0.043(4) 0.039(3) -0.002(3) -0.010(3) 0.006(3) F9 0.090(3) 0.044(2) 0.061(2) -0.0058(18) -0.010(2) -0.012(2) O9 0.047(3) 0.046(2) 0.045(2) -0.015(2) -0.012(2) -0.011(2) C9 0.053(4) 0.050(4) 0.055(4) 0.018(3) -0.010(3) -0.011(3) F10 0.054(3) 0.078(3) 0.072(3) -0.041(2) 0.003(2) 0.008(2) O10 0.044(3) 0.072(3) 0.047(3) -0.017(2) 0.014(2) -0.013(2) C10 0.058(4) 0.050(4) 0.063(4) 0.011(3) -0.012(3) -0.021(3) F11 0.086(4) 0.050(3) 0.116(4) -0.031(3) 0.010(3) -0.010(3) O11 0.038(2) 0.049(3) 0.052(3) -0.013(2) -0.019(2) 0.0097(19) C11 0.039(3) 0.049(4) 0.044(3) -0.001(3) -0.001(3) -0.016(3) F12 0.121(5) 0.101(4) 0.104(4) -0.023(3) -0.054(4) 0.064(4) O12 0.035(3) 0.058(3) 0.039(2) -0.017(2) -0.001(2) -0.006(2) C12 0.029(2) 0.047(3) 0.031(3) -0.006(2) -0.003(2) -0.009(2) C13 0.026(3) 0.052(4) 0.041(3) -0.018(3) 0.004(2) -0.005(2) C14 0.017(3) 0.060(4) 0.038(3) -0.024(3) -0.002(2) 0.002(3) C15 0.025(3) 0.046(4) 0.060(4) -0.024(3) -0.003(3) 0.001(3) C16 0.029(4) 0.066(5) 0.049(4) -0.028(4) -0.017(3) 0.015(3) C17 0.038(4) 0.054(4) 0.050(4) -0.017(3) -0.012(3) 0.013(3) C18 0.039(4) 0.047(4) 0.038(3) -0.007(3) -0.009(3) 0.009(3) C19 0.026(3) 0.056(4) 0.040(3) -0.015(3) 0.006(3) 0.000(3) C20 0.042(4) 0.052(4) 0.038(3) -0.009(3) -0.008(3) 0.011(3) C21 0.036(4) 0.053(4) 0.055(4) -0.019(4) -0.001(3) 0.011(3) C22 0.023(3) 0.058(4) 0.052(4) -0.017(4) 0.003(3) 0.000(3) C23 0.033(4) 0.037(3) 0.036(3) -0.013(3) -0.002(3) -0.002(3) C24 0.029(3) 0.043(3) 0.040(3) -0.013(3) 0.006(2) -0.006(2) C25 0.032(3) 0.040(3) 0.036(3) -0.006(2) -0.004(2) -0.005(2) C26 0.045(4) 0.046(4) 0.042(3) -0.003(3) 0.014(3) -0.012(3) C27 0.056(4) 0.041(3) 0.050(3) 0.003(3) 0.008(3) -0.009(3) C28 0.051(4) 0.040(3) 0.055(4) -0.010(3) -0.003(3) 0.001(3) C29 0.054(5) 0.029(3) 0.042(4) -0.005(3) -0.004(3) -0.005(3) C30 0.036(3) 0.034(3) 0.033(3) -0.013(2) -0.004(2) -0.004(2) C31 0.036(4) 0.041(3) 0.035(3) -0.009(3) -0.004(3) 0.006(3) C32 0.018(3) 0.050(4) 0.035(3) -0.014(3) -0.002(3) 0.001(3) C33 0.024(3) 0.047(4) 0.050(4) -0.011(3) 0.005(3) -0.006(3) C34 0.022(3) 0.062(4) 0.047(4) -0.015(3) 0.006(3) -0.002(3) C35 0.038(4) 0.056(4) 0.035(3) -0.010(3) 0.011(3) -0.007(3) C36 0.034(4) 0.050(4) 0.044(4) -0.015(3) -0.012(3) 0.002(3) C37 0.037(3) 0.045(3) 0.046(4) -0.007(3) 0.002(3) -0.008(3) C38 0.054(5) 0.040(4) 0.080(6) -0.004(4) 0.016(4) 0.006(3) C39 0.041(4) 0.044(3) 0.046(4) -0.008(3) 0.001(3) -0.003(3) C40 0.061(5) 0.047(4) 0.058(4) -0.015(3) -0.004(4) 0.010(4) O50 0.041(5) 0.079(7) 0.049(6) 0.012(5) -0.004(4) -0.014(4) C50 0.046(5) 0.019(4) 0.183(12) -0.011(5) -0.067(6) -0.008(3) C51 0.045(4) 0.062(5) 0.055(5) -0.019(4) -0.017(3) 0.000(4) C52 0.091(7) 0.108(8) 0.037(5) 0.011(5) -0.012(4) -0.066(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.950(5) . ? Cu1 N4 1.965(5) . ? Cu1 N1 2.018(5) . ? Cu1 N2 2.036(6) . ? S1 O2 1.427(5) . ? S1 O1 1.434(6) . ? S1 O3 1.446(5) . ? S1 C37 1.797(7) . ? F1 C37 1.310(8) . ? N1 C5 1.343(9) . ? N1 C1 1.361(7) . ? C1 C2 1.385(9) . ? C1 H1 0.9500 . ? Cu2 N8 1.956(5) . ? Cu2 N7 1.958(5) . ? Cu2 N5 2.028(5) . ? Cu2 N6 2.045(5) . ? Cu2 O12 2.420(4) . ? S2 O4 1.438(5) . ? S2 O5 1.445(5) . ? S2 O6 1.459(5) . ? S2 C38 1.819(8) . ? F2 C37 1.311(8) . ? N2 C18 1.341(9) . ? N2 C14 1.360(8) . ? C2 C3 1.364(10) . ? C2 H2 0.9500 . ? S3 O9 1.434(5) . ? S3 O8 1.433(5) . ? S3 O7 1.454(5) . ? S3 C39 1.844(7) . ? F3 C37 1.340(9) . ? N3 C13 1.266(8) . ? N3 C12 1.471(8) . ? C3 C4 1.399(10) . ? C3 H3 0.9500 . ? S4 O10 1.425(5) . ? S4 O12 1.431(5) . ? S4 O11 1.440(5) . ? S4 C40 1.788(8) . ? F4 C38 1.299(11) . ? N4 C6 1.268(8) . ? N4 C7 1.466(7) . ? C4 C5 1.405(9) . ? C4 H4 0.9500 . ? F5 C38 1.361(9) . ? N5 C19 1.326(9) . ? N5 C23 1.373(8) . ? C5 C6 1.464(8) . ? F6 C38 1.326(10) . ? N6 C36 1.306(8) . ? N6 C32 1.380(9) . ? C6 H6 0.9500 . ? F7 C39 1.311(8) . ? N7 C31 1.258(8) . ? N7 C30 1.476(7) . ? C7 C8 1.502(8) . ? C7 C12 1.551(7) . ? C7 H7 1.0000 . ? F8 C39 1.337(8) . ? N8 C24 1.268(8) . ? N8 C25 1.464(7) . ? C8 C9 1.532(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? F9 C39 1.325(8) . ? C9 C10 1.559(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? F10 C40 1.308(9) . ? C10 C11 1.514(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? F11 C40 1.344(10) . ? C11 C12 1.521(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? F12 C40 1.353(10) . ? C12 H12 1.0000 . ? C13 C14 1.453(10) . ? C13 H13 0.9500 . ? C14 C15 1.404(9) . ? C15 C16 1.409(10) . ? C15 H15 0.9500 . ? C16 C17 1.342(11) . ? C16 H16 0.9500 . ? C17 C18 1.387(10) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.405(10) . ? C19 H19 0.9500 . ? C20 C21 1.399(10) . ? C20 H20 0.9500 . ? C21 C22 1.366(10) . ? C21 H21 0.9500 . ? C22 C23 1.371(10) . ? C22 H22 0.9500 . ? C23 C24 1.467(9) . ? C24 H24 0.9500 . ? C25 C26 1.527(8) . ? C25 C30 1.530(7) . ? C25 H25 1.0000 . ? C26 C27 1.538(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.538(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.558(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.503(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30 1.0000 . ? C31 C32 1.480(9) . ? C31 H31 0.9500 . ? C32 C33 1.379(9) . ? C33 C34 1.365(10) . ? C33 H33 0.9500 . ? C34 C35 1.406(11) . ? C34 H34 0.9500 . ? C35 C36 1.419(10) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? O50 C50 1.317(14) . ? O50 H50 0.8400 . ? C50 C51 1.476(10) . ? C50 C52 1.610(17) . ? C50 H50A 1.0000 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? O60 C60 1.528(14) . ? O60 H60 0.8400 . ? C60 C62 1.450(15) . ? C60 C61 1.538(14) . ? C60 H60A 1.0000 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? O50A C50A 1.49(4) . ? O50A H50B 0.8400 . ? C50A C52A 1.45(3) . ? C50A C51A 1.567(17) . ? C50A H50C 1.0000 . ? C51A H51D 0.9800 . ? C51A H51E 0.9800 . ? C51A H51F 0.9800 . ? C52A H52D 0.9800 . ? C52A H52E 0.9800 . ? C52A H52F 0.9800 . ? 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_3 _geom_angle_publ_flag N3 Cu1 N4 81.7(2) . . ? N3 Cu1 N1 161.6(2) . . ? N4 Cu1 N1 81.1(2) . . ? N3 Cu1 N2 80.9(2) . . ? N4 Cu1 N2 161.4(2) . . ? N1 Cu1 N2 116.9(2) . . ? O2 S1 O1 116.0(4) . . ? O2 S1 O3 114.8(4) . . ? O1 S1 O3 113.2(3) . . ? O2 S1 C37 102.7(3) . . ? O1 S1 C37 104.6(4) . . ? O3 S1 C37 103.5(3) . . ? C5 N1 C1 118.4(5) . . ? C5 N1 Cu1 111.7(4) . . ? C1 N1 Cu1 129.9(4) . . ? N1 C1 C2 122.1(6) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? N8 Cu2 N7 81.7(2) . . ? N8 Cu2 N5 81.1(2) . . ? N7 Cu2 N5 161.5(2) . . ? N8 Cu2 N6 159.1(2) . . ? N7 Cu2 N6 81.0(2) . . ? N5 Cu2 N6 117.2(2) . . ? N8 Cu2 O12 103.56(18) . . ? N7 Cu2 O12 90.55(18) . . ? N5 Cu2 O12 86.80(19) . . ? N6 Cu2 O12 88.18(18) . . ? O4 S2 O5 115.0(3) . . ? O4 S2 O6 114.1(3) . . ? O5 S2 O6 116.9(3) . . ? O4 S2 C38 103.7(4) . . ? O5 S2 C38 103.2(3) . . ? O6 S2 C38 101.2(4) . . ? C18 N2 C14 118.8(6) . . ? C18 N2 Cu1 131.2(5) . . ? C14 N2 Cu1 110.0(5) . . ? C3 C2 C1 119.5(6) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? O9 S3 O8 117.4(3) . . ? O9 S3 O7 113.1(3) . . ? O8 S3 O7 114.9(3) . . ? O9 S3 C39 103.7(3) . . ? O8 S3 C39 102.5(3) . . ? O7 S3 C39 102.6(3) . . ? C13 N3 C12 127.1(5) . . ? C13 N3 Cu1 117.9(5) . . ? C12 N3 Cu1 114.2(4) . . ? C2 C3 C4 119.9(7) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? O10 S4 O12 114.1(3) . . ? O10 S4 O11 115.1(3) . . ? O12 S4 O11 114.1(3) . . ? O10 S4 C40 105.6(4) . . ? O12 S4 C40 103.5(4) . . ? O11 S4 C40 102.6(3) . . ? C6 N4 C7 127.6(5) . . ? C6 N4 Cu1 116.0(4) . . ? C7 N4 Cu1 115.9(4) . . ? C3 C4 C5 117.8(7) . . ? C3 C4 H4 121.1 . . ? C5 C4 H4 121.1 . . ? C19 N5 C23 118.4(6) . . ? C19 N5 Cu2 130.1(5) . . ? C23 N5 Cu2 111.4(4) . . ? N1 C5 C4 122.4(6) . . ? N1 C5 C6 115.2(6) . . ? C4 C5 C6 122.4(6) . . ? C36 N6 C32 117.9(6) . . ? C36 N6 Cu2 131.7(5) . . ? C32 N6 Cu2 110.4(4) . . ? N4 C6 C5 115.8(6) . . ? N4 C6 H6 122.1 . . ? C5 C6 H6 122.1 . . ? C31 N7 C30 128.6(5) . . ? C31 N7 Cu2 117.2(4) . . ? C30 N7 Cu2 113.9(3) . . ? N4 C7 C8 116.8(5) . . ? N4 C7 C12 105.0(4) . . ? C8 C7 C12 110.4(5) . . ? N4 C7 H7 108.1 . . ? C8 C7 H7 108.1 . . ? C12 C7 H7 108.1 . . ? C24 N8 C25 128.2(5) . . ? C24 N8 Cu2 116.9(4) . . ? C25 N8 Cu2 114.9(4) . . ? C7 C8 C9 109.3(6) . . ? C7 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? C7 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.3 . . ? C8 C9 C10 110.9(5) . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 111.2(5) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 108.7(6) . . ? C10 C11 H11A 110.0 . . ? C12 C11 H11A 110.0 . . ? C10 C11 H11B 110.0 . . ? C12 C11 H11B 110.0 . . ? H11A C11 H11B 108.3 . . ? S4 O12 Cu2 131.4(3) . . ? N3 C12 C11 117.9(5) . . ? N3 C12 C7 106.3(4) . . ? C11 C12 C7 109.9(5) . . ? N3 C12 H12 107.5 . . ? C11 C12 H12 107.5 . . ? C7 C12 H12 107.5 . . ? N3 C13 C14 114.4(6) . . ? N3 C13 H13 122.8 . . ? C14 C13 H13 122.8 . . ? N2 C14 C15 122.0(7) . . ? N2 C14 C13 116.7(6) . . ? C15 C14 C13 121.3(6) . . ? C14 C15 C16 116.5(7) . . ? C14 C15 H15 121.8 . . ? C16 C15 H15 121.8 . . ? C17 C16 C15 121.4(7) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C18 119.0(7) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? N2 C18 C17 122.3(7) . . ? N2 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? N5 C19 C20 122.1(6) . . ? N5 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C21 C20 C19 119.1(7) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C22 C21 C20 117.8(7) . . ? C22 C21 H21 121.1 . . ? C20 C21 H21 121.1 . . ? C21 C22 C23 121.0(7) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 N5 121.5(6) . . ? C22 C23 C24 124.2(6) . . ? N5 C23 C24 114.2(6) . . ? N8 C24 C23 116.1(6) . . ? N8 C24 H24 121.9 . . ? C23 C24 H24 121.9 . . ? N8 C25 C26 116.4(5) . . ? N8 C25 C30 106.3(4) . . ? C26 C25 C30 111.2(5) . . ? N8 C25 H25 107.6 . . ? C26 C25 H25 107.6 . . ? C30 C25 H25 107.6 . . ? C25 C26 C27 109.4(6) . . ? C25 C26 H26A 109.8 . . ? C27 C26 H26A 109.8 . . ? C25 C26 H26B 109.8 . . ? C27 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? C28 C27 C26 113.0(5) . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27B 109.0 . . ? C26 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C27 C28 C29 110.6(5) . . ? C27 C28 H28A 109.5 . . ? C29 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? C30 C29 C28 108.2(6) . . ? C30 C29 H29A 110.1 . . ? C28 C29 H29A 110.1 . . ? C30 C29 H29B 110.1 . . ? C28 C29 H29B 110.1 . . ? H29A C29 H29B 108.4 . . ? N7 C30 C29 117.2(5) . . ? N7 C30 C25 105.2(4) . . ? C29 C30 C25 113.1(5) . . ? N7 C30 H30 106.9 . . ? C29 C30 H30 106.9 . . ? C25 C30 H30 106.9 . . ? N7 C31 C32 115.6(6) . . ? N7 C31 H31 122.2 . . ? C32 C31 H31 122.2 . . ? N6 C32 C33 122.8(6) . . ? N6 C32 C31 114.4(5) . . ? C33 C32 C31 122.6(6) . . ? C34 C33 C32 119.3(7) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 118.9(7) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? C34 C35 C36 118.4(7) . . ? C34 C35 H35 120.8 . . ? C36 C35 H35 120.8 . . ? N6 C36 C35 122.7(7) . . ? N6 C36 H36 118.6 . . ? C35 C36 H36 118.6 . . ? F1 C37 F2 105.8(6) . . ? F1 C37 F3 106.7(7) . . ? F2 C37 F3 106.0(7) . . ? F1 C37 S1 112.5(5) . . ? F2 C37 S1 112.8(5) . . ? F3 C37 S1 112.5(5) . . ? F4 C38 F6 108.6(7) . . ? F4 C38 F5 109.4(8) . . ? F6 C38 F5 105.6(7) . . ? F4 C38 S2 112.2(7) . . ? F6 C38 S2 111.2(6) . . ? F5 C38 S2 109.6(5) . . ? F7 C39 F9 109.1(6) . . ? F7 C39 F8 107.2(6) . . ? F9 C39 F8 107.3(6) . . ? F7 C39 S3 111.0(5) . . ? F9 C39 S3 110.9(5) . . ? F8 C39 S3 111.2(5) . . ? F10 C40 F11 107.8(7) . . ? F10 C40 F12 106.7(7) . . ? F11 C40 F12 106.0(7) . . ? F10 C40 S4 112.6(5) . . ? F11 C40 S4 112.8(6) . . ? F12 C40 S4 110.5(6) . . ? O50 C50 C51 112.7(9) . . ? O50 C50 C52 110.5(10) . . ? C51 C50 C52 106.4(8) . . ? O50 C50 H50A 109.0 . . ? C51 C50 H50A 109.0 . . ? C52 C50 H50A 109.0 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C60 O60 H60 109.5 . . ? C62 C60 C61 133.9(16) . . ? C62 C60 O60 92.9(11) . . ? C61 C60 O60 114.5(12) . . ? C62 C60 H60A 104.0 . . ? C61 C60 H60A 104.1 . . ? O60 C60 H60A 104.1 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C50A O50A H50B 109.5 . . ? C52A C50A O50A 108(2) . . ? C52A C50A C51A 111.2(19) . . ? O50A C50A C51A 94.3(18) . . ? C52A C50A H50C 113.8 . . ? O50A C50A H50C 113.8 . . ? C51A C50A H50C 113.8 . . ? C50A C51A H51D 109.5 . . ? C50A C51A H51E 109.5 . . ? H51D C51A H51E 109.5 . . ? C50A C51A H51F 109.5 . . ? H51D C51A H51F 109.5 . . ? H51E C51A H51F 109.5 . . ? C50A C52A H52D 109.5 . . ? C50A C52A H52E 109.5 . . ? H52D C52A H52E 109.5 . . ? C50A C52A H52F 109.5 . . ? H52D C52A H52F 109.5 . . ? H52E C52A H52F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.459 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.079 #===END data_MeOCH2CH2OH _database_code_depnum_ccdc_archive 'CCDC 804592' #TrackingRef '- All.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration ad _chemical_formula_moiety ? _chemical_formula_sum 'C21 H22.50 Cu F6 N4 O6.50 S2' _chemical_formula_weight 676.59 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 Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.8900(2) _cell_length_b 11.4790(3) _cell_length_c 15.4820(5) _cell_angle_alpha 111.6200(10) _cell_angle_beta 101.1990(10) _cell_angle_gamma 93.6650(10) _cell_volume 1424.80(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30643 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 687 _exptl_absorpt_coefficient_mu 0.996 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26438 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 27.47 _reflns_number_total 12251 _reflns_number_gt 8863 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0719P)^2^+1.4966P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 12251 _refine_ls_number_parameters 717 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1559 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.51035(8) 0.32729(7) 0.85871(6) 0.0308(3) Uani 1 1 d . . . S1 S 0.2753(3) 0.1246(2) 0.92617(18) 0.0326(5) Uani 1 1 d . . . F1 F 0.1855(10) -0.0019(8) 0.7414(5) 0.077(2) Uani 1 1 d . . . O1 O 0.4142(8) 0.1768(6) 0.9100(5) 0.0414(17) Uani 1 1 d . . . N1 N 0.3017(9) 0.3813(7) 0.8366(6) 0.0329(19) Uani 1 1 d . . . C1 C 0.2294(12) 0.4600(9) 0.8993(7) 0.035(2) Uani 1 1 d . . . H1 H 0.2799 0.4961 0.9652 0.042 Uiso 1 1 calc R . . Cu2 Cu 0.10382(8) 0.28862(7) 0.28999(5) 0.0313(3) Uani 1 1 d . . . S2 S 0.5805(3) 0.5321(2) 0.74003(17) 0.0335(5) Uani 1 1 d . . . F2 F 0.3251(8) -0.0980(6) 0.8141(6) 0.072(2) Uani 1 1 d . . . O2 O 0.1461(8) 0.1901(7) 0.9185(6) 0.0435(17) Uani 1 1 d . . . N2 N 0.6566(9) 0.4234(8) 0.9899(6) 0.0332(19) Uani 1 1 d . . . C2 C 0.0813(11) 0.4901(9) 0.8699(7) 0.039(2) Uani 1 1 d . . . H2 H 0.0355 0.5487 0.9148 0.047 Uiso 1 1 calc R . . S3 S 0.3434(3) 0.4891(2) 0.22282(18) 0.0348(6) Uani 1 1 d . . . F3 F 0.0893(9) -0.0921(6) 0.8241(6) 0.071(2) Uani 1 1 d . . . O3 O 0.3027(8) 0.0877(7) 1.0069(5) 0.0420(16) Uani 1 1 d . . . N3 N 0.6875(9) 0.2391(7) 0.8392(5) 0.0297(16) Uani 1 1 d . . . C3 C 0.0034(11) 0.4322(9) 0.7733(8) 0.039(2) Uani 1 1 d . . . H3 H -0.0953 0.4513 0.7507 0.047 Uiso 1 1 calc R . . S4 S 0.0303(3) 0.0906(2) 0.41259(17) 0.0344(5) Uani 1 1 d . . . F4 F 0.6112(11) 0.7308(8) 0.6980(7) 0.096(3) Uani 1 1 d . . . O4 O 0.6353(8) 0.5099(7) 0.8253(5) 0.0469(19) Uani 1 1 d . . . N4 N 0.4394(9) 0.2295(7) 0.7201(6) 0.0337(17) Uani 1 1 d . . . C4 C 0.0745(12) 0.3475(9) 0.7132(8) 0.037(2) Uani 1 1 d . . . H4 H 0.0214 0.3030 0.6482 0.045 Uiso 1 1 calc R . . F5 F 0.6173(11) 0.7715(6) 0.8451(6) 0.087(2) Uani 1 1 d . . . O5 O 0.4182(8) 0.5313(8) 0.7132(6) 0.060(2) Uani 1 1 d . . . N5 N -0.0405(9) 0.1927(7) 0.1587(5) 0.0282(17) Uani 1 1 d . . . C5 C 0.2213(10) 0.3247(9) 0.7441(7) 0.029(2) Uani 1 1 d . . . F6 F 0.8108(10) 0.7128(8) 0.7899(7) 0.096(3) Uani 1 1 d . . . O6 O 0.6479(10) 0.4617(7) 0.6622(6) 0.053(2) Uani 1 1 d . . . N6 N 0.3138(9) 0.2283(7) 0.3106(5) 0.0299(17) Uani 1 1 d . . . C6 C 0.3058(11) 0.2415(8) 0.6790(7) 0.0323(18) Uani 1 1 d . . . H6 H 0.2643 0.2003 0.6121 0.039 Uiso 1 1 calc R . . F7 F 0.5361(8) 0.6968(6) 0.3185(5) 0.0660(19) Uani 1 1 d . . . O7 O 0.3201(9) 0.5240(7) 0.1427(6) 0.0482(18) Uani 1 1 d . . . N7 N 0.1888(9) 0.4066(7) 0.4219(5) 0.0315(16) Uani 1 1 d . . . C7 C 0.5572(7) 0.1618(6) 0.6740(5) 0.0343(14) Uani 1 1 d . . . H7 H 0.6234 0.2251 0.6618 0.041 Uiso 1 1 calc R . . F8 F 0.2986(10) 0.7161(7) 0.3245(6) 0.076(2) Uani 1 1 d . . . O8 O 0.4700(8) 0.4179(6) 0.2337(6) 0.0495(19) Uani 1 1 d . . . N8 N -0.0855(9) 0.3594(7) 0.3158(6) 0.0320(17) Uani 1 1 d . . . C8 C 0.5018(12) 0.0521(9) 0.5815(8) 0.046(3) Uani 1 1 d . . . H8A H 0.4402 0.0797 0.5340 0.055 Uiso 1 1 calc R . . H8B H 0.4341 -0.0130 0.5898 0.055 Uiso 1 1 calc R . . F9 F 0.4346(8) 0.6265(7) 0.4068(5) 0.0631(18) Uani 1 1 d . . . O9 O 0.1998(8) 0.4422(6) 0.2399(5) 0.0396(17) Uani 1 1 d . . . C9 C 0.6392(9) -0.0044(8) 0.5456(5) 0.0452(17) Uani 1 1 d . . . H9A H 0.6993 0.0575 0.5297 0.054 Uiso 1 1 calc R . . H9B H 0.6005 -0.0813 0.4864 0.054 Uiso 1 1 calc R . . F10 F 0.0241(11) -0.1527(7) 0.3120(7) 0.086(2) Uani 1 1 d . . . O10 O -0.0236(9) 0.1044(7) 0.3236(5) 0.0474(18) Uani 1 1 d . . . C10 C 0.7471(11) -0.0394(9) 0.6211(7) 0.052(2) Uani 1 1 d . . . H10A H 0.6907 -0.1084 0.6316 0.063 Uiso 1 1 calc R . . H10B H 0.8383 -0.0704 0.5971 0.063 Uiso 1 1 calc R . . F11 F -0.1916(9) -0.1003(6) 0.3524(6) 0.080(2) Uani 1 1 d . . . O11 O -0.0471(9) 0.1542(7) 0.4864(5) 0.0476(17) Uani 1 1 d . . . C11 C 0.8019(12) 0.0761(9) 0.7166(8) 0.038(2) Uani 1 1 d . . . H11A H 0.8643 0.0508 0.7653 0.045 Uiso 1 1 calc R . . H11B H 0.8674 0.1423 0.7083 0.045 Uiso 1 1 calc R . . F12 F 0.0063(12) -0.1074(8) 0.4556(6) 0.101(3) Uani 1 1 d . . . O12 O 0.1965(9) 0.1053(8) 0.4434(5) 0.0526(18) Uani 1 1 d . . . C12 C 0.6599(8) 0.1276(7) 0.7493(5) 0.0349(15) Uani 1 1 d . . . H12 H 0.5978 0.0581 0.7573 0.042 Uiso 1 1 calc R . . C13 C 0.8126(11) 0.2832(8) 0.9021(7) 0.0296(19) Uani 1 1 d . . . H13 H 0.9067 0.2512 0.8928 0.036 Uiso 1 1 calc R . . C14 C 0.8036(11) 0.3907(8) 0.9938(7) 0.031(2) Uani 1 1 d . . . C15 C 0.9224(11) 0.4433(9) 1.0683(7) 0.034(2) Uani 1 1 d . . . H15 H 1.0200 0.4146 1.0662 0.041 Uiso 1 1 calc R . . C16 C 0.9042(13) 0.5401(11) 1.1493(9) 0.052(3) Uani 1 1 d . . . H16 H 0.9893 0.5846 1.2020 0.062 Uiso 1 1 calc R . . C17 C 0.7474(13) 0.5704(11) 1.1498(8) 0.045(3) Uani 1 1 d . . . H17 H 0.7236 0.6285 1.2057 0.054 Uiso 1 1 calc R . . C18 C 0.6365(12) 0.5123(10) 1.0670(7) 0.037(2) Uani 1 1 d . . . H18 H 0.5371 0.5384 1.0652 0.044 Uiso 1 1 calc R . . C19 C 0.2177(14) -0.0242(11) 0.8220(9) 0.056(3) Uani 1 1 d . . . C20 C 0.6614(17) 0.7019(10) 0.7734(10) 0.057(3) Uani 1 1 d . . . C21 C -0.0131(12) 0.1120(9) 0.0797(7) 0.037(2) Uani 1 1 d . . . H21 H 0.0896 0.0950 0.0777 0.044 Uiso 1 1 calc R . . C22 C -0.1370(12) 0.0492(10) -0.0036(8) 0.042(2) Uani 1 1 d . . . H22 H -0.1181 -0.0142 -0.0589 0.050 Uiso 1 1 calc R . . C23 C -0.2761(11) 0.0797(8) -0.0029(6) 0.033(2) Uani 1 1 d . . . H23 H -0.3559 0.0419 -0.0597 0.039 Uiso 1 1 calc R . . C24 C -0.3102(12) 0.1650(9) 0.0775(8) 0.039(2) Uani 1 1 d . . . H24 H -0.4128 0.1834 0.0780 0.047 Uiso 1 1 calc R . . C25 C -0.1849(11) 0.2254(9) 0.1612(7) 0.033(2) Uani 1 1 d . . . C26 C -0.2067(11) 0.3148(9) 0.2470(8) 0.036(2) Uani 1 1 d . . . H26 H -0.3048 0.3404 0.2535 0.043 Uiso 1 1 calc R . . C27 C -0.0737(8) 0.4432(7) 0.4166(5) 0.0342(15) Uani 1 1 d . . . H27 H -0.0947 0.3871 0.4506 0.041 Uiso 1 1 calc R . . C28 C -0.1854(13) 0.5397(10) 0.4350(8) 0.040(3) Uani 1 1 d . . . H28A H -0.1702 0.5964 0.4012 0.048 Uiso 1 1 calc R . . H28B H -0.2935 0.4955 0.4100 0.048 Uiso 1 1 calc R . . C29 C -0.1577(10) 0.6172(8) 0.5408(6) 0.047(2) Uani 1 1 d . . . H29A H -0.2218 0.6863 0.5510 0.056 Uiso 1 1 calc R . . H29B H -0.1916 0.5626 0.5723 0.056 Uiso 1 1 calc R . . C30 C 0.0089(10) 0.6734(7) 0.5867(6) 0.0505(19) Uani 1 1 d . . . H30A H 0.0205 0.7152 0.6567 0.061 Uiso 1 1 calc R . . H30B H 0.0366 0.7397 0.5635 0.061 Uiso 1 1 calc R . . C31 C 0.1246(12) 0.5772(8) 0.5675(6) 0.036(2) Uani 1 1 d . . . H31A H 0.2325 0.6219 0.5937 0.043 Uiso 1 1 calc R . . H31B H 0.1091 0.5171 0.5983 0.043 Uiso 1 1 calc R . . C32 C 0.0945(7) 0.5060(6) 0.4588(5) 0.0354(14) Uani 1 1 d . . . H32 H 0.1121 0.5705 0.4312 0.042 Uiso 1 1 calc R . . C33 C 0.3211(11) 0.3953(8) 0.4620(6) 0.0325(19) Uani 1 1 d . . . H33 H 0.3699 0.4486 0.5263 0.039 Uiso 1 1 calc R . . C34 C 0.3970(12) 0.2922(9) 0.4020(7) 0.032(2) Uani 1 1 d . . . C35 C 0.5391(11) 0.2660(10) 0.4362(8) 0.035(2) Uani 1 1 d . . . H35 H 0.5943 0.3102 0.5008 0.042 Uiso 1 1 calc R . . C36 C 0.5999(13) 0.1694(10) 0.3703(8) 0.045(3) Uani 1 1 d . . . H36 H 0.7002 0.1497 0.3888 0.055 Uiso 1 1 calc R . . C37 C 0.5130(12) 0.1068(11) 0.2816(9) 0.053(3) Uani 1 1 d . . . H37 H 0.5512 0.0405 0.2374 0.063 Uiso 1 1 calc R . . C38 C 0.3708(10) 0.1364(9) 0.2537(7) 0.037(2) Uani 1 1 d . . . H38 H 0.3110 0.0885 0.1907 0.045 Uiso 1 1 calc R . . C39 C 0.4076(12) 0.6417(9) 0.3230(8) 0.044(2) Uani 1 1 d . . . C40 C -0.0350(14) -0.0696(10) 0.3828(9) 0.050(3) Uani 1 1 d . . . C100 C 0.484(2) -0.1026(16) 0.0411(15) 0.188(8) Uiso 1 1 d D . . H10C H 0.4511 -0.1314 -0.0286 0.282 Uiso 1 1 calc R . . H10D H 0.5977 -0.0823 0.0608 0.282 Uiso 1 1 calc R . . H10E H 0.4386 -0.0269 0.0714 0.282 Uiso 1 1 calc R . . C101 C 0.4326(14) -0.2043(13) 0.0709(10) 0.111(4) Uiso 1 1 d D . . H10F H 0.4865 -0.1892 0.1372 0.134 Uiso 1 1 calc R . . H10G H 0.4459 -0.2891 0.0270 0.134 Uiso 1 1 calc R . . O102 O 0.2595(16) -0.187(2) 0.0622(15) 0.222(6) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0209(6) 0.0397(6) 0.0300(6) 0.0118(5) 0.0036(5) 0.0092(5) S1 0.0194(12) 0.0350(11) 0.0439(15) 0.0169(11) 0.0056(11) 0.0048(9) F1 0.079(6) 0.095(5) 0.043(4) 0.020(4) 0.003(4) -0.010(4) O1 0.028(4) 0.051(4) 0.051(5) 0.033(4) -0.002(3) -0.001(3) N1 0.028(4) 0.038(4) 0.044(5) 0.025(4) 0.016(4) 0.014(3) C1 0.035(5) 0.038(4) 0.036(5) 0.017(4) 0.011(4) 0.008(3) Cu2 0.0210(6) 0.0400(6) 0.0267(6) 0.0073(5) 0.0020(5) 0.0073(4) S2 0.0285(13) 0.0404(12) 0.0334(13) 0.0179(11) 0.0049(11) 0.0039(10) F2 0.056(4) 0.048(3) 0.095(5) 0.003(3) 0.020(4) 0.024(3) O2 0.029(4) 0.048(4) 0.057(5) 0.023(4) 0.011(4) 0.017(3) N2 0.021(4) 0.048(5) 0.039(5) 0.023(4) 0.012(4) 0.014(3) C2 0.029(4) 0.046(5) 0.045(5) 0.013(4) 0.018(4) 0.017(3) S3 0.0244(13) 0.0403(13) 0.0408(15) 0.0177(12) 0.0065(12) 0.0058(10) F3 0.057(4) 0.048(3) 0.082(5) -0.001(3) 0.017(4) -0.015(3) O3 0.030(4) 0.055(4) 0.047(4) 0.026(4) 0.008(3) 0.005(3) N3 0.030(4) 0.032(3) 0.028(3) 0.013(3) 0.004(3) 0.008(3) C3 0.023(5) 0.044(5) 0.053(6) 0.025(5) 0.004(4) 0.009(4) S4 0.0258(13) 0.0388(12) 0.0372(14) 0.0161(11) 0.0013(11) 0.0044(10) F4 0.131(8) 0.072(5) 0.124(7) 0.074(6) 0.042(6) 0.021(5) O4 0.039(5) 0.065(5) 0.045(4) 0.037(4) -0.001(4) 0.002(4) N4 0.032(4) 0.039(4) 0.031(4) 0.014(3) 0.007(3) 0.011(3) C4 0.027(6) 0.038(5) 0.041(6) 0.012(5) 0.003(5) 0.000(4) F5 0.122(6) 0.038(3) 0.089(5) -0.003(3) 0.052(5) 0.019(3) O5 0.022(3) 0.082(5) 0.086(6) 0.048(5) 0.000(4) 0.011(3) N5 0.026(4) 0.029(4) 0.022(4) 0.009(3) -0.005(3) -0.004(3) C5 0.015(4) 0.035(5) 0.038(6) 0.014(4) 0.007(4) 0.004(4) F6 0.065(6) 0.075(5) 0.131(8) 0.025(5) 0.026(5) -0.026(4) O6 0.062(5) 0.046(4) 0.047(5) 0.010(4) 0.019(4) 0.003(3) N6 0.023(4) 0.032(4) 0.026(4) 0.006(3) -0.002(3) -0.003(3) C6 0.029(4) 0.039(4) 0.031(4) 0.019(3) 0.002(3) 0.007(3) F7 0.052(4) 0.044(3) 0.086(5) 0.008(3) 0.021(4) -0.013(3) O7 0.048(5) 0.055(4) 0.053(5) 0.032(4) 0.017(4) 0.010(3) N7 0.029(4) 0.034(3) 0.027(3) 0.008(3) 0.005(3) 0.009(3) C7 0.031(3) 0.036(3) 0.039(4) 0.015(3) 0.014(3) 0.010(3) F8 0.078(5) 0.060(4) 0.081(5) 0.011(4) 0.027(4) 0.025(4) O8 0.022(4) 0.041(4) 0.080(6) 0.021(4) 0.004(4) 0.007(3) N8 0.024(3) 0.036(3) 0.038(4) 0.014(3) 0.010(3) 0.003(3) C8 0.038(5) 0.043(5) 0.056(7) 0.020(5) 0.005(5) 0.011(4) F9 0.052(4) 0.077(4) 0.045(4) 0.012(3) 0.004(3) 0.001(3) O9 0.021(4) 0.052(4) 0.053(5) 0.027(4) 0.012(3) 0.009(3) C9 0.048(4) 0.049(4) 0.035(4) 0.009(3) 0.015(3) 0.016(3) F10 0.103(5) 0.069(4) 0.097(6) 0.027(4) 0.052(5) 0.044(4) O10 0.049(5) 0.050(4) 0.043(4) 0.022(4) 0.002(4) 0.012(3) C10 0.044(5) 0.052(5) 0.063(6) 0.019(4) 0.020(4) 0.015(4) F11 0.064(5) 0.050(4) 0.102(6) 0.005(4) 0.022(5) -0.017(3) O11 0.040(4) 0.055(4) 0.034(4) 0.004(3) 0.002(3) 0.015(3) C11 0.031(6) 0.039(5) 0.041(6) 0.012(5) 0.009(5) 0.010(4) F12 0.162(10) 0.075(5) 0.109(7) 0.064(6) 0.067(7) 0.039(6) O12 0.033(4) 0.079(5) 0.050(4) 0.035(4) 0.001(3) 0.000(3) C12 0.034(4) 0.040(4) 0.037(4) 0.021(3) 0.011(3) 0.011(3) C13 0.024(4) 0.031(4) 0.031(4) 0.009(3) 0.005(4) 0.007(3) C14 0.029(5) 0.027(4) 0.043(6) 0.017(4) 0.014(4) 0.011(4) C15 0.019(5) 0.045(5) 0.034(5) 0.018(4) -0.005(4) -0.003(4) C16 0.024(5) 0.061(6) 0.063(8) 0.028(6) -0.011(5) -0.003(4) C17 0.042(7) 0.057(6) 0.038(6) 0.021(5) 0.006(5) 0.008(5) C18 0.030(5) 0.044(5) 0.035(6) 0.014(5) 0.008(4) 0.002(4) C19 0.042(7) 0.059(7) 0.069(8) 0.026(6) 0.019(6) -0.004(5) C20 0.075(8) 0.028(4) 0.064(7) 0.012(5) 0.019(6) -0.002(4) C21 0.030(5) 0.044(5) 0.034(5) 0.013(4) 0.005(4) 0.010(4) C22 0.036(6) 0.047(6) 0.030(5) 0.003(5) 0.001(5) 0.010(5) C23 0.037(5) 0.033(4) 0.019(4) 0.007(4) -0.003(4) -0.003(4) C24 0.033(6) 0.040(5) 0.047(7) 0.021(5) 0.005(5) 0.009(4) C25 0.022(5) 0.049(5) 0.030(5) 0.023(4) -0.005(4) -0.003(4) C26 0.016(4) 0.041(4) 0.055(6) 0.023(4) 0.007(4) 0.007(3) C27 0.039(4) 0.041(4) 0.028(3) 0.013(3) 0.017(3) 0.017(3) C28 0.036(6) 0.042(5) 0.052(7) 0.024(5) 0.019(5) 0.018(5) C29 0.050(5) 0.043(5) 0.043(4) 0.004(4) 0.022(4) 0.023(4) C30 0.066(5) 0.037(4) 0.042(4) 0.006(3) 0.015(4) 0.013(4) C31 0.044(5) 0.035(4) 0.020(4) 0.000(3) 0.011(4) 0.003(4) C32 0.036(4) 0.035(3) 0.039(4) 0.015(3) 0.013(3) 0.014(3) C33 0.031(4) 0.036(4) 0.028(4) 0.011(3) 0.004(3) 0.003(3) C34 0.030(5) 0.035(5) 0.035(6) 0.020(4) 0.006(5) 0.001(4) C35 0.026(5) 0.045(5) 0.037(6) 0.023(5) 0.001(5) 0.006(4) C36 0.028(5) 0.058(6) 0.043(6) 0.013(5) 0.003(4) 0.015(4) C37 0.034(5) 0.057(6) 0.056(6) 0.013(5) 0.003(4) 0.016(4) C38 0.021(4) 0.046(4) 0.032(4) 0.003(4) 0.001(3) 0.010(3) C39 0.030(5) 0.042(5) 0.046(6) 0.003(5) 0.005(4) 0.011(4) C40 0.057(7) 0.047(5) 0.056(6) 0.022(5) 0.030(5) 0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.939(8) . ? Cu1 N4 1.968(8) . ? Cu1 N1 2.000(8) . ? Cu1 N2 2.043(9) . ? Cu1 O1 2.331(6) . ? S1 O2 1.423(7) . ? S1 O1 1.443(7) . ? S1 O3 1.444(7) . ? S1 C19 1.821(13) . ? F1 C19 1.346(14) . ? N1 C5 1.357(12) . ? N1 C1 1.357(12) . ? C1 C2 1.414(14) . ? C1 H1 0.9500 . ? Cu2 N7 1.952(8) . ? Cu2 N8 1.963(8) . ? Cu2 N5 2.037(7) . ? Cu2 N6 2.040(8) . ? Cu2 O9 2.347(6) . ? S2 O5 1.420(8) . ? S2 O4 1.435(7) . ? S2 O6 1.445(8) . ? S2 C20 1.875(10) . ? F2 C19 1.311(13) . ? N2 C18 1.306(13) . ? N2 C14 1.379(11) . ? C2 C3 1.401(15) . ? C2 H2 0.9500 . ? S3 O7 1.421(7) . ? S3 O8 1.452(7) . ? S3 O9 1.462(6) . ? S3 C39 1.824(10) . ? F3 C19 1.353(12) . ? N3 C13 1.259(12) . ? N3 C12 1.465(10) . ? C3 C4 1.361(14) . ? C3 H3 0.9500 . ? S4 O10 1.437(7) . ? S4 O11 1.438(8) . ? S4 O12 1.440(8) . ? S4 C40 1.751(11) . ? F4 C20 1.331(15) . ? N4 C6 1.275(11) . ? N4 C7 1.482(10) . ? C4 C5 1.377(13) . ? C4 H4 0.9500 . ? F5 C20 1.257(14) . ? N5 C21 1.312(13) . ? N5 C25 1.364(12) . ? C5 C6 1.473(13) . ? F6 C20 1.292(15) . ? N6 C38 1.305(12) . ? N6 C34 1.359(12) . ? C6 H6 0.9500 . ? F7 C39 1.297(12) . ? N7 C33 1.257(11) . ? N7 C32 1.469(9) . ? C7 C8 1.481(12) . ? C7 C12 1.522(9) . ? C7 H7 1.0000 . ? F8 C39 1.330(11) . ? N8 C26 1.280(12) . ? N8 C27 1.479(10) . ? C8 C9 1.524(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? F9 C39 1.350(12) . ? C9 C10 1.553(12) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? F10 C40 1.380(12) . ? C10 C11 1.541(14) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? F11 C40 1.358(14) . ? C11 C12 1.524(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? F12 C40 1.347(13) . ? C12 H12 1.0000 . ? C13 C14 1.520(12) . ? C13 H13 0.9500 . ? C14 C15 1.320(13) . ? C15 C16 1.382(16) . ? C15 H15 0.9500 . ? C16 C17 1.458(15) . ? C16 H16 0.9500 . ? C17 C18 1.362(15) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C21 C22 1.434(14) . ? C21 H21 0.9500 . ? C22 C23 1.308(14) . ? C22 H22 0.9500 . ? C23 C24 1.374(13) . ? C23 H23 0.9500 . ? C24 C25 1.442(14) . ? C24 H24 0.9500 . ? C25 C26 1.405(14) . ? C26 H26 0.9500 . ? C27 C28 1.521(11) . ? C27 C32 1.523(10) . ? C27 H27 1.0000 . ? C28 C29 1.509(14) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.499(12) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.546(12) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.534(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32 1.0000 . ? C33 C34 1.501(13) . ? C33 H33 0.9500 . ? C34 C35 1.369(13) . ? C35 C36 1.422(15) . ? C35 H35 0.9500 . ? C36 C37 1.337(16) . ? C36 H36 0.9500 . ? C37 C38 1.361(13) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C100 C101 1.483(9) . ? C100 H10C 0.9800 . ? C100 H10D 0.9800 . ? C100 H10E 0.9800 . ? C101 O102 1.550(9) . ? C101 H10F 0.9900 . ? C101 H10G 0.9900 . ? 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_3 _geom_angle_publ_flag N3 Cu1 N4 81.6(3) . . ? N3 Cu1 N1 162.1(3) . . ? N4 Cu1 N1 80.7(3) . . ? N3 Cu1 N2 80.9(3) . . ? N4 Cu1 N2 160.0(3) . . ? N1 Cu1 N2 116.9(3) . . ? N3 Cu1 O1 88.8(3) . . ? N4 Cu1 O1 98.2(3) . . ? N1 Cu1 O1 91.2(3) . . ? N2 Cu1 O1 91.1(3) . . ? O2 S1 O1 115.5(4) . . ? O2 S1 O3 115.1(4) . . ? O1 S1 O3 113.9(4) . . ? O2 S1 C19 103.5(5) . . ? O1 S1 C19 101.8(5) . . ? O3 S1 C19 104.7(5) . . ? S1 O1 Cu1 143.0(4) . . ? C5 N1 C1 117.0(8) . . ? C5 N1 Cu1 112.7(6) . . ? C1 N1 Cu1 130.2(7) . . ? N1 C1 C2 122.3(10) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? N7 Cu2 N8 81.7(3) . . ? N7 Cu2 N5 162.9(3) . . ? N8 Cu2 N5 81.3(3) . . ? N7 Cu2 N6 81.8(3) . . ? N8 Cu2 N6 160.9(3) . . ? N5 Cu2 N6 115.4(3) . . ? N7 Cu2 O9 88.5(3) . . ? N8 Cu2 O9 96.4(3) . . ? N5 Cu2 O9 91.2(3) . . ? N6 Cu2 O9 92.7(3) . . ? O5 S2 O4 116.1(5) . . ? O5 S2 O6 114.4(6) . . ? O4 S2 O6 113.2(5) . . ? O5 S2 C20 102.7(6) . . ? O4 S2 C20 103.9(5) . . ? O6 S2 C20 104.4(5) . . ? C18 N2 C14 116.1(9) . . ? C18 N2 Cu1 131.4(7) . . ? C14 N2 Cu1 112.3(6) . . ? C3 C2 C1 118.9(9) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? O7 S3 O8 116.8(5) . . ? O7 S3 O9 113.7(4) . . ? O8 S3 O9 114.6(4) . . ? O7 S3 C39 102.5(5) . . ? O8 S3 C39 103.6(5) . . ? O9 S3 C39 103.1(5) . . ? C13 N3 C12 127.0(7) . . ? C13 N3 Cu1 118.2(6) . . ? C12 N3 Cu1 114.8(5) . . ? C4 C3 C2 117.4(9) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? O10 S4 O11 114.9(5) . . ? O10 S4 O12 114.3(4) . . ? O11 S4 O12 115.0(5) . . ? O10 S4 C40 102.2(5) . . ? O11 S4 C40 102.8(5) . . ? O12 S4 C40 105.4(5) . . ? C6 N4 C7 127.4(8) . . ? C6 N4 Cu1 117.3(7) . . ? C7 N4 Cu1 114.9(5) . . ? C3 C4 C5 121.7(11) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C21 N5 C25 120.7(8) . . ? C21 N5 Cu2 130.5(7) . . ? C25 N5 Cu2 108.8(6) . . ? N1 C5 C4 122.4(9) . . ? N1 C5 C6 114.8(8) . . ? C4 C5 C6 122.8(10) . . ? C38 N6 C34 118.4(8) . . ? C38 N6 Cu2 130.5(6) . . ? C34 N6 Cu2 110.8(6) . . ? N4 C6 C5 114.4(9) . . ? N4 C6 H6 122.8 . . ? C5 C6 H6 122.8 . . ? C33 N7 C32 127.9(8) . . ? C33 N7 Cu2 117.0(6) . . ? C32 N7 Cu2 114.8(5) . . ? C8 C7 N4 117.8(7) . . ? C8 C7 C12 112.5(6) . . ? N4 C7 C12 105.9(6) . . ? C8 C7 H7 106.6 . . ? N4 C7 H7 106.6 . . ? C12 C7 H7 106.6 . . ? C26 N8 C27 128.5(8) . . ? C26 N8 Cu2 116.0(7) . . ? C27 N8 Cu2 114.9(5) . . ? C7 C8 C9 110.1(8) . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.2 . . ? S3 O9 Cu2 140.1(4) . . ? C8 C9 C10 111.7(7) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 111.0(7) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 108.6(8) . . ? C12 C11 H11A 110.0 . . ? C10 C11 H11A 110.0 . . ? C12 C11 H11B 110.0 . . ? C10 C11 H11B 110.0 . . ? H11A C11 H11B 108.3 . . ? N3 C12 C7 106.3(6) . . ? N3 C12 C11 117.2(7) . . ? C7 C12 C11 111.3(6) . . ? N3 C12 H12 107.2 . . ? C7 C12 H12 107.2 . . ? C11 C12 H12 107.2 . . ? N3 C13 C14 115.8(8) . . ? N3 C13 H13 122.1 . . ? C14 C13 H13 122.1 . . ? C15 C14 N2 124.8(9) . . ? C15 C14 C13 123.4(8) . . ? N2 C14 C13 111.8(9) . . ? C14 C15 C16 119.8(9) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C17 116.5(10) . . ? C15 C16 H16 121.7 . . ? C17 C16 H16 121.7 . . ? C18 C17 C16 117.4(11) . . ? C18 C17 H17 121.3 . . ? C16 C17 H17 121.3 . . ? N2 C18 C17 124.9(10) . . ? N2 C18 H18 117.5 . . ? C17 C18 H18 117.5 . . ? F2 C19 F1 107.2(10) . . ? F2 C19 F3 106.6(9) . . ? F1 C19 F3 107.4(10) . . ? F2 C19 S1 113.1(9) . . ? F1 C19 S1 110.3(8) . . ? F3 C19 S1 111.9(8) . . ? F5 C20 F6 111.5(12) . . ? F5 C20 F4 111.3(11) . . ? F6 C20 F4 107.9(11) . . ? F5 C20 S2 109.7(8) . . ? F6 C20 S2 108.9(8) . . ? F4 C20 S2 107.4(9) . . ? N5 C21 C22 120.6(9) . . ? N5 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 119.5(10) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 122.0(9) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C23 C24 C25 117.7(9) . . ? C23 C24 H24 121.2 . . ? C25 C24 H24 121.2 . . ? N5 C25 C26 118.3(8) . . ? N5 C25 C24 119.3(9) . . ? C26 C25 C24 122.4(9) . . ? N8 C26 C25 115.6(8) . . ? N8 C26 H26 122.2 . . ? C25 C26 H26 122.2 . . ? N8 C27 C28 116.9(7) . . ? N8 C27 C32 107.1(5) . . ? C28 C27 C32 111.7(7) . . ? N8 C27 H27 106.9 . . ? C28 C27 H27 106.9 . . ? C32 C27 H27 106.9 . . ? C29 C28 C27 110.1(8) . . ? C29 C28 H28A 109.6 . . ? C27 C28 H28A 109.6 . . ? C29 C28 H28B 109.6 . . ? C27 C28 H28B 109.6 . . ? H28A C28 H28B 108.2 . . ? C30 C29 C28 112.9(7) . . ? C30 C29 H29A 109.0 . . ? C28 C29 H29A 109.0 . . ? C30 C29 H29B 109.0 . . ? C28 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C29 C30 C31 114.6(7) . . ? C29 C30 H30A 108.6 . . ? C31 C30 H30A 108.6 . . ? C29 C30 H30B 108.6 . . ? C31 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? C32 C31 C30 107.4(7) . . ? C32 C31 H31A 110.2 . . ? C30 C31 H31A 110.2 . . ? C32 C31 H31B 110.2 . . ? C30 C31 H31B 110.2 . . ? H31A C31 H31B 108.5 . . ? N7 C32 C27 105.9(6) . . ? N7 C32 C31 118.0(6) . . ? C27 C32 C31 110.9(6) . . ? N7 C32 H32 107.2 . . ? C27 C32 H32 107.2 . . ? C31 C32 H32 107.2 . . ? N7 C33 C34 115.8(9) . . ? N7 C33 H33 122.1 . . ? C34 C33 H33 122.1 . . ? N6 C34 C35 122.8(9) . . ? N6 C34 C33 114.4(9) . . ? C35 C34 C33 122.7(10) . . ? C34 C35 C36 116.7(10) . . ? C34 C35 H35 121.7 . . ? C36 C35 H35 121.7 . . ? C37 C36 C35 118.6(10) . . ? C37 C36 H36 120.7 . . ? C35 C36 H36 120.7 . . ? C36 C37 C38 121.1(11) . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? N6 C38 C37 122.2(10) . . ? N6 C38 H38 118.9 . . ? C37 C38 H38 118.9 . . ? F7 C39 F8 110.1(9) . . ? F7 C39 F9 107.1(9) . . ? F8 C39 F9 107.5(9) . . ? F7 C39 S3 111.0(7) . . ? F8 C39 S3 110.4(7) . . ? F9 C39 S3 110.7(7) . . ? F12 C40 F11 106.2(9) . . ? F12 C40 F10 102.7(8) . . ? F11 C40 F10 105.8(10) . . ? F12 C40 S4 113.5(9) . . ? F11 C40 S4 113.3(8) . . ? F10 C40 S4 114.4(7) . . ? C101 C100 H10C 109.5 . . ? C101 C100 H10D 109.5 . . ? H10C C100 H10D 109.5 . . ? C101 C100 H10E 109.5 . . ? H10C C100 H10E 109.5 . . ? H10D C100 H10E 109.5 . . ? C100 C101 O102 98.6(13) . . ? C100 C101 H10F 112.0 . . ? O102 C101 H10F 112.0 . . ? C100 C101 H10G 112.0 . . ? O102 C101 H10G 112.0 . . ? H10F C101 H10G 109.7 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.219 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.091 #===END data_CF3CH2OH _database_code_depnum_ccdc_archive 'CCDC 804593' #TrackingRef '- All.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_absolute_configuration ad _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H21 Cu F9 N4 O7 S2' _chemical_formula_weight 752.09 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 Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.5450(8) _cell_length_b 11.4260(10) _cell_length_c 13.6980(12) _cell_angle_alpha 78.636(6) _cell_angle_beta 83.184(5) _cell_angle_gamma 88.992(5) _cell_volume 1454.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 35753 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 24.11 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 758 _exptl_absorpt_coefficient_mu 1.001 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9065 _exptl_absorpt_correction_T_max 0.9516 _exptl_absorpt_process_details ? _exptl_special_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995 ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kapp ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10765 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.16 _diffrn_reflns_theta_max 24.16 _reflns_number_total 7741 _reflns_number_gt 5792 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+3.1719P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(2) _refine_ls_number_reflns 7741 _refine_ls_number_parameters 811 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.65256(11) 0.70465(11) 0.97408(9) 0.0392(4) Uani 1 1 d . . . S1 S 0.5186(3) 0.4776(3) 0.8458(3) 0.0407(8) Uani 1 1 d . . . F1 F 0.5248(8) 0.3686(7) 1.0344(6) 0.057(2) Uani 1 1 d . . . O1 O 0.6064(10) 0.5720(9) 0.8627(8) 0.053(2) Uani 1 1 d . . . N1 N 0.8214(10) 0.5956(9) 1.0013(8) 0.033(3) Uani 1 1 d . . . C1 C 0.8390(14) 0.5055(13) 1.0740(11) 0.043(3) Uani 1 1 d . . . H1 H 0.7639 0.4818 1.1260 0.052 Uiso 1 1 calc R . . Cu2 Cu 0.14435(11) 0.59202(10) 0.54901(9) 0.0387(4) Uani 1 1 d . . . S2 S 0.8412(3) 0.8768(3) 1.1064(2) 0.0405(8) Uani 1 1 d . . . F2 F 0.6963(8) 0.3244(8) 0.9345(7) 0.072(2) Uani 1 1 d . . . O2 O 0.3690(9) 0.4901(9) 0.8710(7) 0.055(2) Uani 1 1 d . . . N2 N 0.4674(10) 0.6610(11) 1.0652(9) 0.041(3) Uani 1 1 d . . . C2 C 0.9636(14) 0.4449(14) 1.0764(11) 0.050(4) Uani 1 1 d . . . H2 H 0.9713 0.3787 1.1296 0.061 Uiso 1 1 calc R . . S3 S 0.2833(3) 0.8010(3) 0.6826(3) 0.0428(8) Uani 1 1 d . . . F3 F 0.4924(9) 0.2511(7) 0.9350(6) 0.070(2) Uani 1 1 d . . . O3 O 0.5594(9) 0.4364(8) 0.7540(7) 0.049(2) Uani 1 1 d . . . N3 N 0.5413(10) 0.8458(9) 0.9255(7) 0.036(2) Uani 1 1 d . . . C3 C 1.0770(14) 0.4747(14) 1.0064(11) 0.049(4) Uani 1 1 d . . . H3 H 1.1637 0.4330 1.0107 0.059 Uiso 1 1 calc R . . S4 S -0.0550(3) 0.4140(3) 0.4099(3) 0.0423(8) Uani 1 1 d . . . F4 F 0.8687(9) 1.0983(8) 1.1282(8) 0.078(3) Uani 1 1 d . . . O4 O 0.9203(10) 0.8421(8) 1.1902(7) 0.052(2) Uani 1 1 d . . . N4 N 0.7810(9) 0.7735(8) 0.8567(7) 0.034(2) Uani 1 1 d . . . C4 C 1.0593(13) 0.5702(13) 0.9275(10) 0.044(3) Uani 1 1 d . . . H4 H 1.1332 0.5929 0.8745 0.053 Uiso 1 1 calc R . . F5 F 0.6832(10) 1.0072(8) 1.2099(7) 0.072(3) Uani 1 1 d . . . O5 O 0.9271(9) 0.9043(9) 1.0116(7) 0.053(2) Uani 1 1 d . . . N5 N 0.3237(11) 0.6363(9) 0.4537(8) 0.034(3) Uani 1 1 d . . . C5 C 0.9355(13) 0.6299(11) 0.9276(10) 0.036(3) Uani 1 1 d . . . F6 F 0.6944(10) 1.0689(8) 1.0513(8) 0.078(3) Uani 1 1 d . . . O6 O 0.7202(9) 0.8072(8) 1.1061(7) 0.048(2) Uani 1 1 d . . . N6 N -0.0262(11) 0.6942(10) 0.5247(9) 0.039(3) Uani 1 1 d . . . C6 C 0.9047(11) 0.7302(10) 0.8459(8) 0.036(3) Uani 1 1 d . . . H6 H 0.9720 0.7597 0.7900 0.044 Uiso 1 1 calc R . . F7 F 0.3517(8) 1.0207(7) 0.5941(6) 0.066(2) Uani 1 1 d . . . O7 O 0.1773(9) 0.7215(8) 0.6638(7) 0.045(2) Uani 1 1 d . . . N7 N 0.0008(10) 0.4965(9) 0.6465(7) 0.038(2) Uani 1 1 d . . . C7 C 0.7199(9) 0.8706(9) 0.7857(7) 0.042(2) Uani 1 1 d . . . H7 H 0.6610 0.8329 0.7445 0.050 Uiso 1 1 calc R . . F8 F 0.1342(9) 0.9837(9) 0.6072(8) 0.098(3) Uani 1 1 d . . . O8 O 0.4253(9) 0.7700(9) 0.6566(9) 0.072(3) Uani 1 1 d . . . N8 N 0.2676(10) 0.4675(9) 0.6093(8) 0.037(2) Uani 1 1 d . . . C8 C 0.8286(14) 0.9525(12) 0.7137(10) 0.051(3) Uani 1 1 d . . . H8A H 0.8852 0.9070 0.6686 0.061 Uiso 1 1 calc R . . H8B H 0.8932 0.9877 0.7516 0.061 Uiso 1 1 calc R . . F9 F 0.2780(11) 0.9176(8) 0.4979(6) 0.078(3) Uani 1 1 d . . . O9 O 0.2507(11) 0.8371(9) 0.7785(7) 0.062(3) Uani 1 1 d . . . C9 C 0.7438(12) 1.0519(9) 0.6521(8) 0.058(3) Uani 1 1 d . . . H9A H 0.8105 1.1090 0.6066 0.070 Uiso 1 1 calc R . . H9B H 0.6861 1.0156 0.6103 0.070 Uiso 1 1 calc R . . F10 F 0.0914(10) 0.2252(8) 0.4754(7) 0.074(3) Uani 1 1 d . . . O10 O 0.0686(9) 0.4875(9) 0.4128(7) 0.053(3) Uani 1 1 d . . . C10 C 0.6475(14) 1.1194(10) 0.7183(10) 0.055(3) Uani 1 1 d . . . H10A H 0.5947 1.1805 0.6756 0.066 Uiso 1 1 calc R . . H10B H 0.7054 1.1610 0.7564 0.066 Uiso 1 1 calc R . . F11 F -0.0698(9) 0.1908(8) 0.3881(7) 0.073(3) Uani 1 1 d . . . O11 O -0.1533(9) 0.3863(9) 0.4995(7) 0.048(2) Uani 1 1 d . . . C11 C 0.5408(13) 1.0337(12) 0.7931(11) 0.046(4) Uani 1 1 d . . . H11A H 0.4850 1.0785 0.8392 0.056 Uiso 1 1 calc R . . H11B H 0.4749 0.9988 0.7559 0.056 Uiso 1 1 calc R . . F12 F 0.1202(8) 0.2836(8) 0.3150(7) 0.065(2) Uani 1 1 d . . . O12 O -0.1179(9) 0.4497(9) 0.3163(7) 0.053(2) Uani 1 1 d . . . C12 C 0.6219(10) 0.9372(8) 0.8514(7) 0.036(2) Uani 1 1 d . . . H12 H 0.6835 0.9773 0.8893 0.044 Uiso 1 1 calc R . . F13 F 0.2640(12) 0.2106(9) 0.1252(10) 0.111(4) Uani 1 1 d . . . O13 O 0.6228(11) 0.3810(9) 0.2762(8) 0.064(3) Uani 1 1 d . . . H13A H 0.6671 0.3943 0.3224 0.077 Uiso 1 1 calc R . . C13 C 0.4102(13) 0.8471(11) 0.9571(10) 0.037(3) Uani 1 1 d . . . H13 H 0.3478 0.9081 0.9313 0.044 Uiso 1 1 calc R . . F14 F 0.2035(12) 0.0671(9) 0.0602(7) 0.101(4) Uani 1 1 d . . . O14 O 0.1605(10) -0.0827(8) 0.2475(7) 0.050(2) Uani 1 1 d . . . H14 H 0.1228 -0.0999 0.1997 0.059 Uiso 1 1 calc R . . C14 C 0.3659(12) 0.7456(11) 1.0367(10) 0.034(3) Uani 1 1 d . . . F15 F 0.3911(11) 0.0553(13) 0.1306(11) 0.123(5) Uani 1 1 d . . . C15 C 0.2278(14) 0.7308(13) 1.0871(10) 0.042(3) Uani 1 1 d . . . H15 H 0.1565 0.7869 1.0682 0.051 Uiso 1 1 calc R . . F16 F 0.5156(16) 0.0841(11) 0.3895(10) 0.145(6) Uani 1 1 d . . . C16 C 0.1970(17) 0.6323(15) 1.1657(13) 0.059(5) Uani 1 1 d . . . H16 H 0.1040 0.6210 1.1996 0.071 Uiso 1 1 calc R . . F17 F 0.4045(12) 0.2436(16) 0.3930(12) 0.143(6) Uani 1 1 d . . . C17 C 0.3007(14) 0.5525(15) 1.1936(12) 0.049(3) Uani 1 1 d . . . H17 H 0.2813 0.4867 1.2477 0.058 Uiso 1 1 calc R . . F18 F 0.5861(11) 0.2191(11) 0.4592(8) 0.101(4) Uani 1 1 d . . . C18 C 0.4360(13) 0.5700(14) 1.1406(11) 0.045(4) Uani 1 1 d . . . H18 H 0.5079 0.5144 1.1594 0.055 Uiso 1 1 calc R . . C19 C 0.3518(14) 0.7228(12) 0.3745(10) 0.038(3) Uani 1 1 d . . . H19 H 0.2787 0.7771 0.3557 0.046 Uiso 1 1 calc R . . C20 C 0.4811(15) 0.7383(14) 0.3178(12) 0.044(3) Uani 1 1 d . . . H20 H 0.4965 0.8019 0.2614 0.053 Uiso 1 1 calc R . . C21 C 0.5895(13) 0.6592(12) 0.3444(10) 0.041(3) Uani 1 1 d . . . H21 H 0.6796 0.6669 0.3060 0.050 Uiso 1 1 calc R . . C22 C 0.5624(14) 0.5706(13) 0.4271(11) 0.044(4) Uani 1 1 d . . . H22 H 0.6339 0.5154 0.4476 0.052 Uiso 1 1 calc R . . C23 C 0.4322(14) 0.5625(12) 0.4793(11) 0.040(3) Uani 1 1 d . . . C24 C 0.3932(13) 0.4695(11) 0.5677(10) 0.039(3) Uani 1 1 d . . . H24 H 0.4601 0.4125 0.5931 0.047 Uiso 1 1 calc R . . C25 C 0.2063(9) 0.3884(8) 0.7035(7) 0.036(2) Uani 1 1 d . . . H25 H 0.2117 0.4322 0.7594 0.043 Uiso 1 1 calc R . . C26 C 0.2699(15) 0.2654(11) 0.7345(10) 0.045(4) Uani 1 1 d . . . H26A H 0.2699 0.2202 0.6798 0.053 Uiso 1 1 calc R . . H26B H 0.3687 0.2736 0.7475 0.053 Uiso 1 1 calc R . . C27 C 0.1862(12) 0.2009(12) 0.8255(10) 0.057(3) Uani 1 1 d . . . H27A H 0.2003 0.2406 0.8817 0.069 Uiso 1 1 calc R . . H27B H 0.2238 0.1189 0.8416 0.069 Uiso 1 1 calc R . . C28 C 0.0277(10) 0.1922(9) 0.8204(8) 0.051(2) Uani 1 1 d . . . H28A H 0.0105 0.1415 0.7721 0.061 Uiso 1 1 calc R . . H28B H -0.0202 0.1547 0.8871 0.061 Uiso 1 1 calc R . . C29 C -0.0322(13) 0.3166(12) 0.7875(10) 0.045(3) Uani 1 1 d . . . H29A H -0.1330 0.3101 0.7785 0.054 Uiso 1 1 calc R . . H29B H -0.0255 0.3641 0.8400 0.054 Uiso 1 1 calc R . . C30 C 0.0492(8) 0.3786(8) 0.6899(7) 0.034(2) Uani 1 1 d . . . H30 H 0.0431 0.3266 0.6398 0.041 Uiso 1 1 calc R . . C31 C -0.1225(10) 0.5366(10) 0.6518(8) 0.033(3) Uani 1 1 d . . . H31 H -0.1983 0.4955 0.6956 0.039 Uiso 1 1 calc R . . C32 C -0.1405(12) 0.6509(12) 0.5859(10) 0.040(3) Uani 1 1 d . . . C33 C -0.2739(14) 0.7117(13) 0.5817(11) 0.043(3) Uani 1 1 d . . . H33 H -0.3545 0.6804 0.6262 0.051 Uiso 1 1 calc R . . C34 C -0.2827(15) 0.8132(13) 0.5141(11) 0.045(4) Uani 1 1 d . . . H34 H -0.3704 0.8538 0.5120 0.054 Uiso 1 1 calc R . . C35 C -0.1701(14) 0.8597(12) 0.4484(11) 0.043(3) Uani 1 1 d . . . H35 H -0.1772 0.9299 0.3990 0.052 Uiso 1 1 calc R . . C36 C -0.0427(14) 0.7976(13) 0.4582(10) 0.043(3) Uani 1 1 d . . . H36 H 0.0384 0.8303 0.4150 0.052 Uiso 1 1 calc R . . C37 C 0.5587(14) 0.3482(13) 0.9406(11) 0.047(3) Uani 1 1 d . . . C38 C 0.7679(15) 1.0182(14) 1.1267(11) 0.051(4) Uani 1 1 d . . . C39 C 0.2614(14) 0.9348(13) 0.5894(12) 0.048(3) Uani 1 1 d . . . C40 C 0.0266(16) 0.2694(13) 0.3996(11) 0.051(4) Uani 1 1 d . . . C41 C 0.259(2) 0.0886(15) 0.1425(14) 0.074(5) Uani 1 1 d . . . C42 C 0.1695(16) 0.0383(13) 0.2361(11) 0.055(4) Uani 1 1 d . . . C43 C 0.5305(17) 0.2000(17) 0.3835(14) 0.069(5) Uani 1 1 d . . . C44 C 0.6067(16) 0.2531(13) 0.2850(12) 0.059(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0226(8) 0.0499(10) 0.0426(9) -0.0056(8) -0.0001(7) 0.0030(7) S1 0.0269(16) 0.0498(19) 0.048(2) -0.0160(16) -0.0024(14) -0.0023(14) F1 0.063(5) 0.063(5) 0.044(4) -0.009(4) -0.003(4) -0.001(4) O1 0.045(5) 0.052(5) 0.064(6) -0.008(5) -0.013(4) -0.018(4) N1 0.020(6) 0.040(6) 0.037(6) -0.009(5) -0.002(5) 0.003(5) C1 0.028(7) 0.053(8) 0.045(8) -0.010(7) 0.006(6) -0.002(6) Cu2 0.0251(9) 0.0470(10) 0.0408(9) -0.0029(8) -0.0014(7) 0.0019(7) S2 0.0341(18) 0.0477(19) 0.0404(19) -0.0095(16) -0.0061(15) 0.0004(15) F2 0.047(4) 0.094(6) 0.069(5) -0.002(4) -0.007(4) 0.020(4) O2 0.033(5) 0.072(6) 0.060(6) -0.011(5) -0.002(4) 0.001(4) N2 0.010(5) 0.058(7) 0.051(7) -0.005(6) -0.001(5) 0.003(5) C2 0.035(8) 0.070(10) 0.046(8) -0.009(7) -0.008(7) 0.000(7) S3 0.0252(17) 0.058(2) 0.0449(19) -0.0112(16) -0.0019(14) -0.0047(14) F3 0.101(6) 0.045(4) 0.066(5) -0.016(3) -0.011(4) -0.011(4) O3 0.045(5) 0.061(5) 0.045(5) -0.018(4) -0.004(4) -0.009(4) N3 0.033(5) 0.046(6) 0.028(5) -0.014(4) 0.002(4) 0.006(4) C3 0.029(7) 0.071(10) 0.053(10) -0.024(9) -0.006(7) 0.017(7) S4 0.0297(17) 0.053(2) 0.047(2) -0.0170(17) -0.0058(15) 0.0024(15) F4 0.067(6) 0.051(5) 0.122(8) -0.031(5) -0.021(6) -0.002(4) O4 0.059(6) 0.051(5) 0.050(5) -0.008(4) -0.024(4) 0.001(4) N4 0.024(4) 0.033(5) 0.047(5) -0.007(4) -0.006(4) -0.008(4) C4 0.024(6) 0.071(9) 0.039(7) -0.013(7) 0.000(5) 0.002(6) F5 0.080(7) 0.069(6) 0.070(6) -0.024(5) 0.002(5) 0.007(5) O5 0.037(4) 0.071(6) 0.052(5) -0.017(5) 0.001(4) -0.002(4) N5 0.037(6) 0.039(6) 0.029(6) -0.010(5) -0.008(5) -0.005(5) C5 0.031(7) 0.034(7) 0.049(8) -0.021(6) -0.006(6) -0.001(5) F6 0.065(6) 0.074(6) 0.100(8) -0.009(6) -0.037(6) 0.017(5) O6 0.043(5) 0.061(6) 0.043(5) -0.016(5) -0.007(4) -0.002(4) N6 0.028(6) 0.048(7) 0.044(7) -0.014(6) -0.006(6) -0.001(6) C6 0.029(5) 0.048(6) 0.032(6) -0.011(5) 0.004(4) -0.006(5) F7 0.073(5) 0.064(5) 0.056(4) 0.004(3) -0.008(3) -0.034(4) O7 0.038(5) 0.054(5) 0.043(5) -0.016(4) 0.001(4) -0.008(4) N7 0.035(5) 0.045(5) 0.033(5) -0.010(4) 0.000(4) -0.004(4) C7 0.041(5) 0.051(6) 0.032(5) -0.004(4) -0.010(4) -0.005(4) F8 0.052(5) 0.077(5) 0.140(9) 0.025(5) 0.010(5) 0.013(4) O8 0.017(4) 0.066(6) 0.119(8) 0.008(5) 0.002(4) 0.005(4) N8 0.031(5) 0.036(5) 0.044(6) -0.006(4) -0.014(4) 0.004(4) C8 0.039(6) 0.056(8) 0.047(7) 0.009(6) 0.007(5) -0.011(6) F9 0.120(8) 0.066(5) 0.051(5) -0.014(4) -0.018(5) -0.021(5) O9 0.074(6) 0.067(6) 0.041(5) -0.007(4) 0.002(5) -0.029(5) C9 0.071(7) 0.043(6) 0.057(7) 0.000(5) -0.008(6) -0.003(5) F10 0.080(6) 0.071(6) 0.068(6) -0.007(5) -0.013(5) 0.031(5) O10 0.029(5) 0.061(6) 0.072(7) -0.023(5) 0.001(5) -0.015(4) C10 0.062(8) 0.034(6) 0.068(8) -0.006(5) -0.010(6) 0.005(6) F11 0.058(6) 0.062(6) 0.099(7) -0.022(5) -0.002(5) -0.011(4) O11 0.029(4) 0.070(6) 0.046(5) -0.012(4) -0.006(4) 0.003(4) C11 0.035(7) 0.050(8) 0.054(9) -0.010(7) -0.002(6) -0.012(6) F12 0.048(5) 0.071(6) 0.078(6) -0.033(5) 0.011(4) 0.012(4) O12 0.046(5) 0.074(6) 0.042(5) -0.018(4) -0.007(4) 0.005(5) C12 0.035(5) 0.034(5) 0.042(6) -0.006(4) -0.009(4) -0.005(4) F13 0.122(9) 0.060(6) 0.128(10) 0.022(6) 0.011(7) -0.016(6) O13 0.058(6) 0.059(6) 0.079(7) -0.008(6) -0.034(6) 0.008(5) C13 0.032(6) 0.036(6) 0.043(7) -0.007(5) -0.011(5) 0.002(5) F14 0.142(10) 0.103(8) 0.050(6) -0.002(6) -0.002(7) -0.001(7) O14 0.056(5) 0.049(6) 0.041(5) -0.001(4) -0.006(4) -0.003(4) C14 0.017(6) 0.039(7) 0.047(8) -0.017(6) 0.000(5) 0.000(5) F15 0.040(6) 0.170(14) 0.141(12) -0.007(10) 0.023(7) -0.006(7) C15 0.026(7) 0.049(8) 0.051(8) -0.008(7) -0.002(6) -0.008(6) F16 0.216(15) 0.092(8) 0.113(10) -0.021(7) 0.056(9) -0.086(10) C16 0.041(8) 0.073(11) 0.067(10) -0.030(9) 0.007(7) -0.014(8) F17 0.046(7) 0.210(18) 0.149(13) 0.005(12) 0.018(8) -0.004(9) C17 0.028(7) 0.063(9) 0.050(8) -0.007(7) 0.009(5) -0.015(6) F18 0.096(8) 0.140(10) 0.058(6) 0.009(6) -0.017(6) -0.019(7) C18 0.023(7) 0.063(9) 0.056(9) -0.021(8) -0.009(6) 0.001(6) C19 0.038(8) 0.035(7) 0.038(7) -0.003(6) -0.001(6) -0.001(6) C20 0.045(7) 0.045(7) 0.050(8) -0.021(6) -0.010(6) -0.002(6) C21 0.020(6) 0.059(9) 0.048(8) -0.022(7) 0.006(5) -0.005(6) C22 0.030(7) 0.051(8) 0.057(9) -0.026(8) -0.007(7) 0.018(6) C23 0.032(7) 0.045(7) 0.049(8) -0.019(6) -0.010(6) -0.002(6) C24 0.028(6) 0.039(6) 0.051(7) -0.010(6) -0.005(5) 0.009(5) C25 0.029(5) 0.036(5) 0.043(6) -0.009(4) -0.003(4) -0.002(4) C26 0.056(8) 0.035(7) 0.044(8) -0.002(6) -0.022(6) 0.015(6) C27 0.044(6) 0.055(8) 0.063(8) 0.012(6) -0.007(6) -0.003(6) C28 0.046(6) 0.048(6) 0.050(6) 0.009(5) -0.005(5) -0.014(5) C29 0.034(6) 0.051(7) 0.051(7) -0.013(6) 0.003(5) -0.002(5) C30 0.024(4) 0.037(5) 0.040(5) -0.004(4) -0.007(4) 0.004(4) C31 0.022(5) 0.047(6) 0.031(6) -0.014(5) 0.004(4) -0.004(4) C32 0.019(6) 0.050(8) 0.052(8) -0.013(7) 0.000(6) 0.002(6) C33 0.026(6) 0.053(8) 0.055(8) -0.024(7) -0.008(6) 0.001(5) C34 0.035(8) 0.047(9) 0.058(10) -0.016(8) -0.012(7) 0.009(7) C35 0.044(8) 0.036(7) 0.047(8) -0.001(6) -0.011(7) 0.017(6) C36 0.032(7) 0.063(9) 0.035(7) -0.012(7) -0.001(6) 0.002(6) C37 0.031(7) 0.054(8) 0.052(8) -0.010(6) 0.006(5) 0.002(6) C38 0.042(8) 0.067(10) 0.047(9) -0.012(8) -0.015(8) -0.002(7) C39 0.034(7) 0.056(8) 0.058(9) -0.021(7) 0.000(6) 0.000(6) C40 0.054(9) 0.046(8) 0.052(10) -0.013(7) 0.002(8) 0.009(7) C41 0.086(13) 0.062(11) 0.067(12) 0.009(9) -0.013(10) 0.004(9) C42 0.062(9) 0.052(9) 0.057(10) -0.025(8) -0.002(7) -0.010(7) C43 0.042(9) 0.097(14) 0.064(11) -0.014(10) 0.012(8) -0.031(9) C44 0.046(8) 0.043(8) 0.073(10) 0.017(7) 0.005(7) -0.009(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 1.942(10) . ? Cu1 N3 1.964(11) . ? Cu1 N1 2.044(10) . ? Cu1 N2 2.047(11) . ? Cu1 O1 2.432(9) . ? S1 O3 1.437(9) . ? S1 O2 1.441(9) . ? S1 O1 1.447(9) . ? S1 C37 1.833(16) . ? F1 C37 1.352(16) . ? N1 C1 1.307(18) . ? N1 C5 1.398(16) . ? C1 C2 1.366(19) . ? C1 H1 0.9500 . ? Cu2 N8 1.949(10) . ? Cu2 N7 1.974(10) . ? Cu2 N6 2.008(11) . ? Cu2 N5 2.032(11) . ? Cu2 O7 2.410(8) . ? S2 O6 1.414(9) . ? S2 O5 1.432(10) . ? S2 O4 1.436(9) . ? S2 C38 1.807(16) . ? F2 C37 1.334(15) . ? N2 C18 1.324(18) . ? N2 C14 1.390(17) . ? C2 C3 1.36(2) . ? C2 H2 0.9500 . ? S3 O8 1.417(9) . ? S3 O7 1.450(8) . ? S3 O9 1.451(10) . ? S3 C39 1.814(16) . ? F3 C37 1.307(14) . ? N3 C13 1.275(16) . ? N3 C12 1.462(14) . ? C3 C4 1.40(2) . ? C3 H3 0.9500 . ? S4 O11 1.439(10) . ? S4 O12 1.462(9) . ? S4 O10 1.469(8) . ? S4 C40 1.838(14) . ? F4 C38 1.344(15) . ? N4 C6 1.276(14) . ? N4 C7 1.484(13) . ? C4 C5 1.354(18) . ? C4 H4 0.9500 . ? F5 C38 1.303(18) . ? N5 C19 1.321(16) . ? N5 C23 1.359(17) . ? C5 C6 1.487(17) . ? F6 C38 1.349(16) . ? N6 C32 1.333(16) . ? N6 C36 1.362(18) . ? C6 H6 0.9500 . ? F7 C39 1.333(14) . ? N7 C31 1.254(13) . ? N7 C30 1.453(13) . ? C7 C12 1.520(13) . ? C7 C8 1.534(15) . ? C7 H7 1.0000 . ? F8 C39 1.344(16) . ? N8 C24 1.263(16) . ? N8 C25 1.484(14) . ? C8 C9 1.553(17) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? F9 C39 1.298(16) . ? C9 C10 1.521(15) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? F10 C40 1.285(16) . ? C10 C11 1.561(18) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? F11 C40 1.341(15) . ? C11 C12 1.491(17) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? F12 C40 1.361(16) . ? C12 H12 1.0000 . ? F13 C41 1.368(19) . ? O13 C44 1.452(17) . ? O13 H13A 0.8400 . ? C13 C14 1.457(18) . ? C13 H13 0.9500 . ? F14 C41 1.367(19) . ? O14 C42 1.363(16) . ? O14 H14 0.8400 . ? C14 C15 1.410(17) . ? F15 C41 1.31(2) . ? C15 C16 1.40(2) . ? C15 H15 0.9500 . ? F16 C43 1.32(2) . ? C16 C17 1.37(2) . ? C16 H16 0.9500 . ? F17 C43 1.30(2) . ? C17 C18 1.402(18) . ? C17 H17 0.9500 . ? F18 C43 1.276(18) . ? C18 H18 0.9500 . ? C19 C20 1.37(2) . ? C19 H19 0.9500 . ? C20 C21 1.39(2) . ? C20 H20 0.9500 . ? C21 C22 1.37(2) . ? C21 H21 0.9500 . ? C22 C23 1.354(18) . ? C22 H22 0.9500 . ? C23 C24 1.460(19) . ? C24 H24 0.9500 . ? C25 C26 1.523(15) . ? C25 C30 1.541(11) . ? C25 H25 1.0000 . ? C26 C27 1.469(19) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.529(13) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.526(17) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.514(16) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30 1.0000 . ? C31 C32 1.454(17) . ? C31 H31 0.9500 . ? C32 C33 1.441(17) . ? C33 C34 1.34(2) . ? C33 H33 0.9500 . ? C34 C35 1.36(2) . ? C34 H34 0.9500 . ? C35 C36 1.404(19) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C42 1.47(2) . ? C43 C44 1.48(2) . ? 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_3 _geom_angle_publ_flag N4 Cu1 N3 81.7(4) . . ? N4 Cu1 N1 81.4(4) . . ? N3 Cu1 N1 160.9(4) . . ? N4 Cu1 N2 159.7(4) . . ? N3 Cu1 N2 80.7(5) . . ? N1 Cu1 N2 117.3(5) . . ? N4 Cu1 O1 80.4(3) . . ? N3 Cu1 O1 102.1(4) . . ? N1 Cu1 O1 83.9(4) . . ? N2 Cu1 O1 93.3(4) . . ? O3 S1 O2 115.2(5) . . ? O3 S1 O1 114.9(6) . . ? O2 S1 O1 116.0(6) . . ? O3 S1 C37 102.1(6) . . ? O2 S1 C37 101.8(6) . . ? O1 S1 C37 104.0(6) . . ? S1 O1 Cu1 146.8(7) . . ? C1 N1 C5 117.9(11) . . ? C1 N1 Cu1 131.4(9) . . ? C5 N1 Cu1 110.6(8) . . ? N1 C1 C2 121.0(13) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? N8 Cu2 N7 81.7(4) . . ? N8 Cu2 N6 161.4(5) . . ? N7 Cu2 N6 80.0(5) . . ? N8 Cu2 N5 81.0(5) . . ? N7 Cu2 N5 160.8(4) . . ? N6 Cu2 N5 117.6(5) . . ? N8 Cu2 O7 94.4(4) . . ? N7 Cu2 O7 91.7(3) . . ? N6 Cu2 O7 82.8(4) . . ? N5 Cu2 O7 97.9(3) . . ? O6 S2 O5 114.2(5) . . ? O6 S2 O4 116.3(6) . . ? O5 S2 O4 113.7(6) . . ? O6 S2 C38 103.2(6) . . ? O5 S2 C38 105.0(7) . . ? O4 S2 C38 102.2(6) . . ? C18 N2 C14 120.5(11) . . ? C18 N2 Cu1 130.3(9) . . ? C14 N2 Cu1 109.2(9) . . ? C3 C2 C1 123.2(15) . . ? C3 C2 H2 118.4 . . ? C1 C2 H2 118.4 . . ? O8 S3 O7 115.7(6) . . ? O8 S3 O9 116.6(7) . . ? O7 S3 O9 112.5(6) . . ? O8 S3 C39 102.3(7) . . ? O7 S3 C39 102.4(6) . . ? O9 S3 C39 105.1(6) . . ? C13 N3 C12 127.4(11) . . ? C13 N3 Cu1 118.9(10) . . ? C12 N3 Cu1 113.6(7) . . ? C2 C3 C4 116.5(14) . . ? C2 C3 H3 121.8 . . ? C4 C3 H3 121.8 . . ? O11 S4 O12 115.6(5) . . ? O11 S4 O10 117.5(5) . . ? O12 S4 O10 112.1(6) . . ? O11 S4 C40 103.6(7) . . ? O12 S4 C40 103.8(6) . . ? O10 S4 C40 101.7(6) . . ? C6 N4 C7 126.6(10) . . ? C6 N4 Cu1 118.7(8) . . ? C7 N4 Cu1 114.7(7) . . ? C5 C4 C3 119.2(13) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C19 N5 C23 116.3(11) . . ? C19 N5 Cu2 131.6(9) . . ? C23 N5 Cu2 112.0(9) . . ? C4 C5 N1 122.2(12) . . ? C4 C5 C6 123.3(12) . . ? N1 C5 C6 114.3(11) . . ? C32 N6 C36 116.5(11) . . ? C32 N6 Cu2 112.4(9) . . ? C36 N6 Cu2 131.1(10) . . ? N4 C6 C5 114.8(11) . . ? N4 C6 H6 122.6 . . ? C5 C6 H6 122.6 . . ? S3 O7 Cu2 139.4(6) . . ? C31 N7 C30 128.4(10) . . ? C31 N7 Cu2 117.1(9) . . ? C30 N7 Cu2 113.6(7) . . ? N4 C7 C12 105.0(8) . . ? N4 C7 C8 114.9(8) . . ? C12 C7 C8 113.0(9) . . ? N4 C7 H7 107.9 . . ? C12 C7 H7 107.9 . . ? C8 C7 H7 107.9 . . ? C24 N8 C25 127.7(10) . . ? C24 N8 Cu2 115.9(10) . . ? C25 N8 Cu2 116.1(7) . . ? C7 C8 C9 106.5(10) . . ? C7 C8 H8A 110.4 . . ? C9 C8 H8A 110.4 . . ? C7 C8 H8B 110.4 . . ? C9 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? C10 C9 C8 112.6(10) . . ? C10 C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C9 C10 C11 111.6(9) . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 108.5(10) . . ? C12 C11 H11A 110.0 . . ? C10 C11 H11A 110.0 . . ? C12 C11 H11B 110.0 . . ? C10 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? N3 C12 C11 117.4(9) . . ? N3 C12 C7 106.2(8) . . ? C11 C12 C7 113.4(9) . . ? N3 C12 H12 106.4 . . ? C11 C12 H12 106.4 . . ? C7 C12 H12 106.4 . . ? C44 O13 H13A 109.5 . . ? N3 C13 C14 113.1(12) . . ? N3 C13 H13 123.4 . . ? C14 C13 H13 123.4 . . ? C42 O14 H14 109.5 . . ? N2 C14 C15 119.0(13) . . ? N2 C14 C13 117.4(11) . . ? C15 C14 C13 123.5(12) . . ? C16 C15 C14 119.2(13) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 120.1(14) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 118.6(15) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? N2 C18 C17 122.4(14) . . ? N2 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? N5 C19 C20 123.4(14) . . ? N5 C19 H19 118.3 . . ? C20 C19 H19 118.3 . . ? C19 C20 C21 119.0(15) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? C22 C21 C20 118.2(13) . . ? C22 C21 H21 120.9 . . ? C20 C21 H21 120.9 . . ? C23 C22 C21 119.0(13) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C22 C23 N5 124.1(14) . . ? C22 C23 C24 122.8(13) . . ? N5 C23 C24 113.1(12) . . ? N8 C24 C23 117.9(11) . . ? N8 C24 H24 121.1 . . ? C23 C24 H24 121.1 . . ? N8 C25 C26 119.0(9) . . ? N8 C25 C30 103.9(8) . . ? C26 C25 C30 111.0(8) . . ? N8 C25 H25 107.4 . . ? C26 C25 H25 107.4 . . ? C30 C25 H25 107.4 . . ? C27 C26 C25 109.2(11) . . ? C27 C26 H26A 109.8 . . ? C25 C26 H26A 109.8 . . ? C27 C26 H26B 109.8 . . ? C25 C26 H26B 109.8 . . ? H26A C26 H26B 108.3 . . ? C26 C27 C28 116.0(10) . . ? C26 C27 H27A 108.3 . . ? C28 C27 H27A 108.3 . . ? C26 C27 H27B 108.3 . . ? C28 C27 H27B 108.3 . . ? H27A C27 H27B 107.4 . . ? C29 C28 C27 109.9(9) . . ? C29 C28 H28A 109.7 . . ? C27 C28 H28A 109.7 . . ? C29 C28 H28B 109.7 . . ? C27 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? C30 C29 C28 110.0(9) . . ? C30 C29 H29A 109.7 . . ? C28 C29 H29A 109.7 . . ? C30 C29 H29B 109.7 . . ? C28 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? N7 C30 C29 116.6(8) . . ? N7 C30 C25 108.2(7) . . ? C29 C30 C25 109.8(8) . . ? N7 C30 H30 107.3 . . ? C29 C30 H30 107.3 . . ? C25 C30 H30 107.3 . . ? N7 C31 C32 114.9(10) . . ? N7 C31 H31 122.5 . . ? C32 C31 H31 122.5 . . ? N6 C32 C33 121.3(13) . . ? N6 C32 C31 115.5(11) . . ? C33 C32 C31 123.1(12) . . ? C34 C33 C32 119.0(14) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C33 C34 C35 122.0(14) . . ? C33 C34 H34 119.0 . . ? C35 C34 H34 119.0 . . ? C34 C35 C36 116.0(13) . . ? C34 C35 H35 122.0 . . ? C36 C35 H35 122.0 . . ? N6 C36 C35 125.1(13) . . ? N6 C36 H36 117.4 . . ? C35 C36 H36 117.4 . . ? F3 C37 F2 107.7(12) . . ? F3 C37 F1 107.4(12) . . ? F2 C37 F1 104.7(11) . . ? F3 C37 S1 113.2(9) . . ? F2 C37 S1 111.9(10) . . ? F1 C37 S1 111.4(10) . . ? F5 C38 F4 108.4(11) . . ? F5 C38 F6 107.5(13) . . ? F4 C38 F6 105.1(12) . . ? F5 C38 S2 112.3(11) . . ? F4 C38 S2 112.1(10) . . ? F6 C38 S2 111.1(9) . . ? F9 C39 F7 107.1(13) . . ? F9 C39 F8 108.9(12) . . ? F7 C39 F8 103.8(11) . . ? F9 C39 S3 113.8(10) . . ? F7 C39 S3 111.8(9) . . ? F8 C39 S3 111.0(11) . . ? F10 C40 F11 109.4(13) . . ? F10 C40 F12 108.9(12) . . ? F11 C40 F12 105.6(10) . . ? F10 C40 S4 112.6(10) . . ? F11 C40 S4 110.9(10) . . ? F12 C40 S4 109.1(10) . . ? F15 C41 F13 105.0(15) . . ? F15 C41 F14 104.9(16) . . ? F13 C41 F14 102.5(13) . . ? F15 C41 C42 119.2(16) . . ? F13 C41 C42 112.0(15) . . ? F14 C41 C42 111.7(14) . . ? O14 C42 C41 110.2(12) . . ? F18 C43 F17 105.0(16) . . ? F18 C43 F16 109.8(18) . . ? F17 C43 F16 106.7(14) . . ? F18 C43 C44 115.2(12) . . ? F17 C43 C44 110.5(18) . . ? F16 C43 C44 109.3(14) . . ? O13 C44 C43 110.3(14) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 24.16 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.419 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.073 #===END data_secPh-alcohol _database_code_depnum_ccdc_archive 'CCDC 804594' #TrackingRef '- All.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration ad _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 Cu F6 N4 O8 S2' _chemical_formula_weight 898.38 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 Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P43212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+3/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+1/4' 'x+1/2, -y+1/2, -z+1/4' '-x+1/2, y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 21.106(5) _cell_length_b 21.106(5) _cell_length_c 8.547(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3807.5(20) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9754 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 26.6 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1852 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9481 _exptl_absorpt_correction_T_max 0.9773 _exptl_absorpt_process_details ; 'Jacobson, R. (1998) Private communication' ; _exptl_special_details ; ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type Synchrotron _diffrn_source Synchrotron _diffrn_radiation_monochromator Synchrotron _diffrn_measurement_device_type Synchrotron _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37331 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 26.74 _reflns_number_total 4433 _reflns_number_gt 4232 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009) ; _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+2.0997P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.101(14) _refine_ls_number_reflns 4433 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.272290(15) 0.272290(15) 0.0000 0.03547(13) Uani 1 2 d S . . S1 S 0.00899(4) 0.21534(3) -0.11888(9) 0.03829(17) Uani 1 1 d . . . F1 F -0.00660(9) 0.09709(8) -0.2016(2) 0.0491(5) Uani 1 1 d . . . O1 O 0.17847(12) 0.32156(11) -0.1520(3) 0.0328(5) Uani 0.75 1 d P A 1 H1A H 0.1436 0.3027 -0.1432 0.09(2) Uiso 0.75 1 calc PR A 1 N1 N 0.26473(10) 0.20963(9) -0.1795(2) 0.0275(4) Uani 1 1 d . . . C1 C 0.22973(14) 0.15731(12) -0.1922(3) 0.0343(6) Uani 1 1 d . . . H1 H 0.2051 0.1438 -0.1054 0.041 Uiso 1 1 calc R . . F2 F 0.04249(10) 0.15328(10) -0.3700(2) 0.0559(5) Uani 1 1 d . . . O2 O 0.05387(13) 0.26141(11) -0.1747(3) 0.0627(7) Uani 1 1 d . . . N2 N 0.33279(10) 0.31107(10) -0.1449(3) 0.0310(5) Uani 1 1 d . . . C2 C 0.22839(14) 0.12200(13) -0.3301(3) 0.0384(6) Uani 1 1 d . . . H2 H 0.2028 0.0851 -0.3371 0.046 Uiso 1 1 calc R . . F3 F 0.08963(9) 0.12274(10) -0.1618(3) 0.0595(6) Uani 1 1 d . . . O3 O 0.01458(10) 0.20025(10) 0.0439(2) 0.0419(5) Uani 1 1 d . . . C3 C 0.26419(14) 0.14090(12) -0.4550(3) 0.0364(6) Uani 1 1 d . . . H3 H 0.2627 0.1182 -0.5510 0.044 Uiso 1 1 calc R . . O4 O -0.05470(12) 0.22313(13) -0.1741(3) 0.0624(7) Uani 1 1 d . . . C4 C 0.30278(13) 0.19383(13) -0.4392(3) 0.0329(6) Uani 1 1 d . . . H4 H 0.3294 0.2071 -0.5227 0.039 Uiso 1 1 calc R . . C5 C 0.30169(12) 0.22659(12) -0.3007(3) 0.0281(5) Uani 1 1 d . . . C6 C 0.34020(12) 0.28401(12) -0.2748(3) 0.0301(5) Uani 1 1 d . . . H6 H 0.3688 0.2996 -0.3514 0.036 Uiso 1 1 calc R . . C7 C 0.36234(12) 0.36946(12) -0.0890(3) 0.0299(5) Uani 1 1 d . . . H7 H 0.3319 0.4049 -0.1085 0.036 Uiso 1 1 calc R . . C8 C 0.42513(14) 0.38817(13) -0.1606(3) 0.0366(6) Uani 1 1 d . . . H8A H 0.4204 0.3932 -0.2752 0.044 Uiso 1 1 calc R . . H8B H 0.4570 0.3547 -0.1409 0.044 Uiso 1 1 calc R . . C9 C 0.44726(14) 0.45037(13) -0.0887(3) 0.0381(6) Uani 1 1 d . . . H9A H 0.4897 0.4610 -0.1302 0.046 Uiso 1 1 calc R . . H9B H 0.4178 0.4846 -0.1200 0.046 Uiso 1 1 calc R . . C10 C 0.03504(13) 0.14402(14) -0.2182(3) 0.0368(6) Uani 1 1 d . . . C11 C 0.1681(2) 0.38951(19) -0.1462(5) 0.0322(8) Uani 0.75 1 d P A 1 H11 H 0.2078 0.4114 -0.1806 0.039 Uiso 0.75 1 calc PR A 1 C12 C 0.15343(13) 0.40931(13) 0.0224(3) 0.0344(6) Uani 1 1 d . . . C13 C 0.19594(14) 0.45136(14) 0.0877(4) 0.0411(7) Uani 1 1 d . A . H13 H 0.2316 0.4648 0.0288 0.049 Uiso 1 1 calc R . . C14 C 0.18733(19) 0.47386(13) 0.2360(4) 0.0511(8) Uani 1 1 d . . . H14 H 0.2176 0.5019 0.2803 0.061 Uiso 1 1 calc R A . C15 C 0.1351(2) 0.45610(15) 0.3218(4) 0.0596(11) Uani 1 1 d . A . H15 H 0.1286 0.4724 0.4241 0.072 Uiso 1 1 calc R . . C16 C 0.09162(18) 0.41378(16) 0.2564(4) 0.0538(9) Uani 1 1 d . . . H16 H 0.0553 0.4011 0.3142 0.065 Uiso 1 1 calc R A . C17 C 0.10150(15) 0.39048(14) 0.1079(4) 0.0426(7) Uani 1 1 d . A . H17 H 0.0723 0.3612 0.0642 0.051 Uiso 1 1 calc R . . C18 C 0.1144(9) 0.4099(9) -0.252(2) 0.043(4) Uani 0.75 1 d P A 1 H18A H 0.1201 0.3910 -0.3558 0.065 Uiso 0.75 1 calc PR A 1 H18B H 0.1142 0.4562 -0.2612 0.065 Uiso 0.75 1 calc PR A 1 H18C H 0.0740 0.3957 -0.2076 0.065 Uiso 0.75 1 calc PR A 1 O1A O 0.2104(5) 0.3544(5) -0.1725(12) 0.050(2) Uiso 0.25 1 d P A 2 H1A1 H 0.2306 0.3859 -0.2060 0.060 Uiso 0.25 1 calc PR A 2 C11A C 0.1491(7) 0.3738(7) -0.1246(18) 0.036(3) Uiso 0.25 1 d P A 2 H11A H 0.1246 0.3343 -0.1012 0.043 Uiso 0.25 1 calc PR A 2 C18A C 0.117(3) 0.405(3) -0.256(6) 0.040(11) Uiso 0.25 1 d P A 2 H18D H 0.1447 0.4050 -0.3478 0.060 Uiso 0.25 1 calc PR A 2 H18E H 0.1066 0.4488 -0.2273 0.060 Uiso 0.25 1 calc PR A 2 H18F H 0.0777 0.3821 -0.2808 0.060 Uiso 0.25 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.04084(17) 0.04084(17) 0.0247(2) -0.00737(15) 0.00737(15) -0.0126(2) S1 0.0449(4) 0.0316(3) 0.0384(4) 0.0034(3) -0.0029(3) -0.0022(3) F1 0.0558(11) 0.0369(9) 0.0545(11) -0.0039(8) 0.0065(9) -0.0136(8) O1 0.0364(13) 0.0279(11) 0.0340(15) -0.0015(10) 0.0012(11) 0.0083(10) N1 0.0289(10) 0.0278(10) 0.0257(11) -0.0021(8) 0.0019(8) 0.0003(8) C1 0.0342(13) 0.0331(13) 0.0354(14) -0.0053(11) 0.0048(12) -0.0068(11) F2 0.0706(13) 0.0668(12) 0.0304(10) -0.0025(9) 0.0043(9) -0.0176(10) O2 0.0879(19) 0.0405(12) 0.0597(16) 0.0050(11) 0.0073(14) -0.0282(12) N2 0.0391(12) 0.0290(10) 0.0248(11) -0.0005(9) 0.0016(9) -0.0044(9) C2 0.0378(14) 0.0320(13) 0.0453(17) -0.0092(11) 0.0005(13) -0.0059(11) F3 0.0407(10) 0.0745(13) 0.0633(13) -0.0099(11) -0.0071(9) 0.0168(9) O3 0.0477(12) 0.0441(11) 0.0339(11) -0.0026(9) 0.0011(9) -0.0047(9) C3 0.0440(15) 0.0318(13) 0.0334(15) -0.0084(11) -0.0007(12) 0.0019(11) O4 0.0525(14) 0.0636(15) 0.0710(17) 0.0010(14) -0.0180(12) 0.0223(12) C4 0.0379(14) 0.0334(13) 0.0273(14) -0.0035(11) 0.0029(11) 0.0031(10) C5 0.0321(12) 0.0273(11) 0.0250(12) 0.0000(10) 0.0018(9) 0.0040(10) C6 0.0368(13) 0.0288(12) 0.0247(14) 0.0007(10) 0.0013(10) -0.0015(10) C7 0.0353(13) 0.0289(12) 0.0255(14) -0.0006(10) 0.0012(10) -0.0039(9) C8 0.0444(15) 0.0337(13) 0.0319(15) 0.0015(11) 0.0051(12) -0.0086(11) C9 0.0417(15) 0.0349(14) 0.0377(16) 0.0064(12) -0.0043(12) -0.0120(11) C10 0.0329(13) 0.0442(15) 0.0334(16) 0.0035(12) -0.0032(11) -0.0054(11) C11 0.035(2) 0.0266(18) 0.035(2) 0.0051(15) 0.0096(17) 0.0015(16) C12 0.0355(13) 0.0334(13) 0.0344(15) -0.0007(11) -0.0096(11) 0.0046(10) C13 0.0386(14) 0.0402(15) 0.0445(18) 0.0077(13) -0.0103(13) -0.0044(11) C14 0.081(2) 0.0294(14) 0.0430(19) 0.0029(13) -0.0256(18) -0.0067(14) C15 0.118(3) 0.0341(16) 0.0264(16) -0.0004(13) 0.0022(19) 0.0144(19) C16 0.068(2) 0.0462(17) 0.047(2) 0.0144(16) 0.0160(18) 0.0032(15) C17 0.0465(16) 0.0383(15) 0.0430(18) 0.0029(13) -0.0027(14) -0.0038(12) C18 0.058(5) 0.044(5) 0.027(3) -0.002(3) -0.008(2) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.958(2) 7 ? Cu1 N2 1.958(2) . ? Cu1 N1 2.032(2) . ? Cu1 N1 2.032(2) 7 ? S1 O3 1.432(2) . ? S1 O4 1.434(2) . ? S1 O2 1.439(2) . ? S1 C10 1.813(3) . ? F1 C10 1.332(3) . ? O1 C11 1.452(4) . ? O1 H1A 0.8400 . ? N1 C1 1.333(3) . ? N1 C5 1.345(3) . ? C1 C2 1.394(4) . ? C1 H1 0.9500 . ? F2 C10 1.322(4) . ? N2 C6 1.258(3) . ? N2 C7 1.462(3) . ? C2 C3 1.368(4) . ? C2 H2 0.9500 . ? F3 C10 1.327(3) . ? C3 C4 1.389(4) . ? C3 H3 0.9500 . ? C4 C5 1.371(4) . ? C4 H4 0.9500 . ? C5 C6 1.476(3) . ? C6 H6 0.9500 . ? C7 C8 1.512(4) . ? C7 C7 1.536(5) 7 ? C7 H7 1.0000 . ? C8 C9 1.523(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C9 1.519(6) 7 ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C18 1.514(19) . ? C11 C12 1.532(5) . ? C11 H11 1.0000 . ? C12 C17 1.376(4) . ? C12 C13 1.380(4) . ? C12 C11A 1.466(15) . ? C13 C14 1.366(5) . ? C13 H13 0.9500 . ? C14 C15 1.376(6) . ? C14 H14 0.9500 . ? C15 C16 1.397(5) . ? C15 H15 0.9500 . ? C16 C17 1.377(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O1A C11A 1.418(16) . ? O1A H1A1 0.8400 . ? C11A C18A 1.47(6) . ? C11A H11A 1.0000 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? 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_3 _geom_angle_publ_flag N2 Cu1 N2 81.67(13) 7 . ? N2 Cu1 N1 159.21(9) 7 . ? N2 Cu1 N1 81.11(9) . . ? N2 Cu1 N1 81.11(9) 7 7 ? N2 Cu1 N1 159.21(9) . 7 ? N1 Cu1 N1 117.90(12) . 7 ? O3 S1 O4 115.00(15) . . ? O3 S1 O2 114.73(15) . . ? O4 S1 O2 115.48(17) . . ? O3 S1 C10 104.19(13) . . ? O4 S1 C10 103.01(14) . . ? O2 S1 C10 101.89(15) . . ? C1 N1 C5 118.6(2) . . ? C1 N1 Cu1 130.11(18) . . ? C5 N1 Cu1 111.26(16) . . ? N1 C1 C2 121.5(3) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C6 N2 C7 128.2(2) . . ? C6 N2 Cu1 116.70(18) . . ? C7 N2 Cu1 115.06(16) . . ? C3 C2 C1 119.5(2) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 118.8(3) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 118.7(3) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 122.7(2) . . ? N1 C5 C6 115.0(2) . . ? C4 C5 C6 122.3(2) . . ? N2 C6 C5 115.9(2) . . ? N2 C6 H6 122.0 . . ? C5 C6 H6 122.0 . . ? N2 C7 C8 117.5(2) . . ? N2 C7 C7 106.45(16) . 7 ? C8 C7 C7 109.92(19) . 7 ? N2 C7 H7 107.5 . . ? C8 C7 H7 107.5 . . ? C7 C7 H7 107.5 7 . ? C7 C8 C9 109.3(2) . . ? C7 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? C7 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.3 . . ? C9 C9 C8 112.3(2) 7 . ? C9 C9 H9A 109.1 7 . ? C8 C9 H9A 109.2 . . ? C9 C9 H9B 109.1 7 . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? F2 C10 F3 107.6(3) . . ? F2 C10 F1 107.0(2) . . ? F3 C10 F1 106.4(2) . . ? F2 C10 S1 111.9(2) . . ? F3 C10 S1 112.0(2) . . ? F1 C10 S1 111.6(2) . . ? O1 C11 C18 111.9(8) . . ? O1 C11 C12 109.4(3) . . ? C18 C11 C12 109.5(8) . . ? O1 C11 H11 108.7 . . ? C18 C11 H11 108.7 . . ? C12 C11 H11 108.7 . . ? C17 C12 C13 119.2(3) . . ? C17 C12 C11A 104.9(6) . . ? C13 C12 C11A 135.8(6) . . ? C17 C12 C11 125.6(3) . . ? C13 C12 C11 115.1(3) . . ? C11A C12 C11 21.1(5) . . ? C14 C13 C12 120.8(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.4(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 119.2(3) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C17 C16 C15 119.8(3) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C12 C17 C16 120.5(3) . . ? C12 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C11A O1A H1A1 109.5 . . ? O1A C11A C12 109.7(10) . . ? O1A C11A C18A 109(2) . . ? C12 C11A C18A 117(2) . . ? O1A C11A H11A 106.7 . . ? C12 C11A H11A 106.7 . . ? C18A C11A H11A 106.7 . . ? C11A C18A H18D 109.5 . . ? C11A C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C11A C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cu1 N1 C1 144.5(3) 7 . . . ? N2 Cu1 N1 C1 178.9(2) . . . . ? N1 Cu1 N1 C1 -10.0(2) 7 . . . ? N2 Cu1 N1 C5 -35.9(3) 7 . . . ? N2 Cu1 N1 C5 -1.49(17) . . . . ? N1 Cu1 N1 C5 169.61(19) 7 . . . ? C5 N1 C1 C2 -3.2(4) . . . . ? Cu1 N1 C1 C2 176.4(2) . . . . ? N2 Cu1 N2 C6 168.9(3) 7 . . . ? N1 Cu1 N2 C6 0.6(2) . . . . ? N1 Cu1 N2 C6 -156.8(2) 7 . . . ? N2 Cu1 N2 C7 -12.90(13) 7 . . . ? N1 Cu1 N2 C7 178.81(19) . . . . ? N1 Cu1 N2 C7 21.5(4) 7 . . . ? N1 C1 C2 C3 0.6(4) . . . . ? C1 C2 C3 C4 2.2(4) . . . . ? C2 C3 C4 C5 -2.5(4) . . . . ? C1 N1 C5 C4 2.9(4) . . . . ? Cu1 N1 C5 C4 -176.7(2) . . . . ? C1 N1 C5 C6 -178.3(2) . . . . ? Cu1 N1 C5 C6 2.1(3) . . . . ? C3 C4 C5 N1 -0.1(4) . . . . ? C3 C4 C5 C6 -178.8(3) . . . . ? C7 N2 C6 C5 -177.5(2) . . . . ? Cu1 N2 C6 C5 0.4(3) . . . . ? N1 C5 C6 N2 -1.7(3) . . . . ? C4 C5 C6 N2 177.1(2) . . . . ? C6 N2 C7 C8 -24.8(4) . . . . ? Cu1 N2 C7 C8 157.26(19) . . . . ? C6 N2 C7 C7 -148.4(3) . . . 7 ? Cu1 N2 C7 C7 33.6(3) . . . 7 ? N2 C7 C8 C9 179.2(2) . . . . ? C7 C7 C8 C9 -58.9(3) 7 . . . ? C7 C8 C9 C9 54.9(4) . . . 7 ? O3 S1 C10 F2 -169.85(19) . . . . ? O4 S1 C10 F2 69.8(2) . . . . ? O2 S1 C10 F2 -50.2(2) . . . . ? O3 S1 C10 F3 -48.9(2) . . . . ? O4 S1 C10 F3 -169.3(2) . . . . ? O2 S1 C10 F3 70.7(2) . . . . ? O3 S1 C10 F1 70.3(2) . . . . ? O4 S1 C10 F1 -50.1(2) . . . . ? O2 S1 C10 F1 -170.1(2) . . . . ? O1 C11 C12 C17 -63.6(4) . . . . ? C18 C11 C12 C17 59.3(8) . . . . ? O1 C11 C12 C13 118.7(3) . . . . ? C18 C11 C12 C13 -118.3(8) . . . . ? O1 C11 C12 C11A -50.7(17) . . . . ? C18 C11 C12 C11A 72.3(19) . . . . ? C17 C12 C13 C14 0.6(4) . . . . ? C11A C12 C13 C14 -176.1(9) . . . . ? C11 C12 C13 C14 178.4(3) . . . . ? C12 C13 C14 C15 -1.6(5) . . . . ? C13 C14 C15 C16 1.3(5) . . . . ? C14 C15 C16 C17 0.0(5) . . . . ? C13 C12 C17 C16 0.7(4) . . . . ? C11A C12 C17 C16 178.3(6) . . . . ? C11 C12 C17 C16 -176.9(3) . . . . ? C15 C16 C17 C12 -1.0(5) . . . . ? C17 C12 C11A O1A -141.4(9) . . . . ? C13 C12 C11A O1A 35.7(15) . . . . ? C11 C12 C11A O1A 49.5(13) . . . . ? C17 C12 C11A C18A 93(2) . . . . ? C13 C12 C11A C18A -90(2) . . . . ? C11 C12 C11A C18A -76(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.74 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.280 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.051 #===END data_1AcOH+MeOH _database_code_depnum_ccdc_archive 'CCDC 804595' #TrackingRef '- All.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H24 Cu F6 N4 O7 S2' _chemical_formula_weight 686.10 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 Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.8590(2) _cell_length_b 11.2530(3) _cell_length_c 14.7790(5) _cell_angle_alpha 80.1800(10) _cell_angle_beta 86.8560(10) _cell_angle_gamma 68.9600(10) _cell_volume 1354.92(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 33153 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 698 _exptl_absorpt_coefficient_mu 1.050 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19858 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 27.46 _reflns_number_total 10511 _reflns_number_gt 9486 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.7137P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.025(10) _refine_ls_number_reflns 10511 _refine_ls_number_parameters 742 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.1024 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.49286(4) 0.25201(4) 0.40127(3) 0.02845(11) Uani 1 1 d . . . S1 S 0.30028(13) 0.11046(11) 0.58999(7) 0.0345(2) Uani 1 1 d . . . F1 F 0.3815(6) -0.0777(4) 0.4955(3) 0.0893(13) Uani 1 1 d . . . O1 O 0.3881(5) 0.0269(4) 0.2434(2) 0.0523(9) Uani 1 1 d . . . N1 N 0.5235(5) 0.3869(3) 0.4679(2) 0.0289(7) Uani 1 1 d . . . C1 C 0.4192(6) 0.4939(5) 0.4938(3) 0.0376(10) Uani 1 1 d . . . H1 H 0.3074 0.5153 0.4820 0.045 Uiso 1 1 calc R . . Cu2 Cu 0.83742(5) 0.39023(4) 0.85005(3) 0.03126(12) Uani 1 1 d . . . S2 S 0.52341(13) 0.45682(10) 0.18015(7) 0.0318(2) Uani 1 1 d . . . F2 F 0.2628(5) -0.1124(3) 0.6243(3) 0.0805(12) Uani 1 1 d . . . O2 O 0.9583(5) 0.6427(4) 0.9830(2) 0.0509(9) Uani 1 1 d . . . N2 N 0.2728(5) 0.3076(3) 0.3484(2) 0.0317(8) Uani 1 1 d . . . C2 C 0.4649(7) 0.5761(5) 0.5374(4) 0.0441(11) Uani 1 1 d . . . H2 H 0.3861 0.6517 0.5545 0.053 Uiso 1 1 calc R . . S3 S 0.82457(14) 0.15438(11) 1.04796(7) 0.0362(2) Uani 1 1 d . . . F3 F 0.5088(5) -0.1248(4) 0.6279(4) 0.0910(14) Uani 1 1 d . . . O3 O 0.4288(4) 0.1458(3) 0.5421(2) 0.0392(7) Uani 1 1 d . . . N3 N 0.5308(5) 0.0966(4) 0.3399(3) 0.0366(8) Uani 1 1 d . . . H3A H 0.5041 0.0356 0.3818 0.044 Uiso 1 1 calc R . . C3 C 0.6281(6) 0.5454(5) 0.5554(3) 0.0415(11) Uani 1 1 d . . . H3 H 0.6632 0.6002 0.5844 0.050 Uiso 1 1 calc R . . S4 S 1.02901(13) 0.54776(10) 0.65782(7) 0.0311(2) Uani 1 1 d . . . F4 F 0.3604(5) 0.7040(3) 0.1587(3) 0.0823(12) Uani 1 1 d . . . O4 O 0.1463(5) 0.1602(4) 0.5443(2) 0.0464(8) Uani 1 1 d . . . N4 N 0.7216(5) 0.1680(3) 0.4310(2) 0.0293(7) Uani 1 1 d . . . C4 C 0.7378(6) 0.4342(4) 0.5303(3) 0.0363(10) Uani 1 1 d . . . H4 H 0.8499 0.4105 0.5424 0.044 Uiso 1 1 calc R . . F5 F 0.3180(5) 0.6000(3) 0.2865(2) 0.0708(10) Uani 1 1 d . . . O5 O 0.2987(5) 0.1102(4) 0.6874(2) 0.0498(9) Uani 1 1 d . . . N5 N 1.0642(4) 0.3438(3) 0.8906(2) 0.0259(7) Uani 1 1 d . . . C5 C 0.6834(5) 0.3572(4) 0.4872(3) 0.0297(9) Uani 1 1 d . . . F6 F 0.5408(7) 0.6360(4) 0.2655(3) 0.0960(15) Uani 1 1 d . . . O6 O 0.6427(5) 0.4819(3) 0.1177(2) 0.0480(8) Uani 1 1 d . . . N6 N 0.7957(5) 0.5355(4) 0.9242(3) 0.0378(9) Uani 1 1 d . . . H6A H 0.7745 0.5052 0.9844 0.045 Uiso 1 1 calc R . . C6 C 0.7908(6) 0.2329(4) 0.4640(3) 0.0319(9) Uani 1 1 d . . . H6 H 0.9046 0.2028 0.4729 0.038 Uiso 1 1 calc R . . F7 F 1.0054(5) 0.0199(4) 0.9300(3) 0.0871(14) Uani 1 1 d . . . O7 O 0.3887(5) 0.4419(4) 0.1400(3) 0.0562(9) Uani 1 1 d . . . N7 N 0.6040(5) 0.4690(3) 0.8288(2) 0.0291(7) Uani 1 1 d . . . C7 C 0.7977(5) 0.0392(4) 0.4070(3) 0.0349(9) Uani 1 1 d . . . H7 H 0.7741 -0.0230 0.4575 0.042 Uiso 1 1 calc R . . F8 F 0.7708(6) 0.0106(4) 0.9424(3) 0.0857(12) Uani 1 1 d . . . O8 O 0.5909(4) 0.3650(3) 0.2616(2) 0.0344(7) Uani 1 1 d . . . N8 N 0.8106(4) 0.2699(3) 0.7666(2) 0.0292(7) Uani 1 1 d . . . C8 C 0.9808(6) -0.0083(5) 0.3934(4) 0.0459(11) Uani 1 1 d . . . H8A H 1.0090 0.0523 0.3447 0.055 Uiso 1 1 calc R . . H8B H 1.0352 -0.0115 0.4510 0.055 Uiso 1 1 calc R . . F9 F 0.9469(6) -0.0957(3) 1.0485(2) 0.0884(13) Uani 1 1 d . . . O9 O 1.0447(5) 0.5238(5) 0.5650(3) 0.0600(11) Uani 1 1 d . . . C9 C 1.0381(8) -0.1415(5) 0.3665(4) 0.0572(15) Uani 1 1 d . . . H9A H 1.0201 -0.2035 0.4182 0.069 Uiso 1 1 calc R . . H9B H 1.1556 -0.1695 0.3542 0.069 Uiso 1 1 calc R . . F10 F 0.8275(5) 0.7767(4) 0.5947(4) 0.1038(18) Uani 1 1 d . . . O10 O 0.8957(4) 0.5231(3) 0.7077(2) 0.0415(8) Uani 1 1 d . . . C10 C 0.9483(7) -0.1433(5) 0.2807(3) 0.0594(14) Uani 1 1 d . . . H10A H 0.9861 -0.2322 0.2664 0.071 Uiso 1 1 calc R . . H10B H 0.9735 -0.0870 0.2275 0.071 Uiso 1 1 calc R . . F11 F 1.0730(5) 0.7648(4) 0.5983(3) 0.0810(12) Uani 1 1 d . . . O11 O 1.1757(5) 0.5068(4) 0.7096(3) 0.0609(11) Uani 1 1 d . . . C11 C 0.7634(7) -0.0961(5) 0.2959(3) 0.0483(13) Uani 1 1 d . . . H11A H 0.7074 -0.0948 0.2394 0.058 Uiso 1 1 calc R . . H11B H 0.7365 -0.1553 0.3463 0.058 Uiso 1 1 calc R . . F12 F 0.9379(8) 0.7660(4) 0.7215(3) 0.119(2) Uani 1 1 d . . . O12 O 0.7683(4) 0.2593(3) 0.9725(2) 0.0414(8) Uani 1 1 d . . . C12 C 0.7081(5) 0.0401(4) 0.3205(3) 0.0366(9) Uani 1 1 d . . . H12 H 0.7351 0.0983 0.2684 0.044 Uiso 1 1 calc R . . O13 O 0.9652(6) 0.1460(5) 1.0938(4) 0.0868(16) Uani 1 1 d . . . C13 C 0.4211(5) 0.1343(4) 0.2624(2) 0.0307(8) Uani 1 1 d . . . H13 H 0.4708 0.1705 0.2073 0.037 Uiso 1 1 calc R . . O14 O 0.6974(5) 0.1358(4) 1.1054(2) 0.0574(10) Uani 1 1 d . . . C14 C 0.2651(5) 0.2356(4) 0.2847(3) 0.0325(8) Uani 1 1 d . . . C15 C 0.1205(6) 0.2571(5) 0.2418(3) 0.0445(11) Uani 1 1 d . . . H15 H 0.1164 0.2058 0.1978 0.053 Uiso 1 1 calc R . . C16 C -0.0184(7) 0.3543(6) 0.2636(4) 0.0529(14) Uani 1 1 d . . . H16 H -0.1184 0.3705 0.2344 0.063 Uiso 1 1 calc R . . C17 C -0.0100(6) 0.4270(6) 0.3277(3) 0.0468(12) Uani 1 1 d . . . H17 H -0.1037 0.4945 0.3430 0.056 Uiso 1 1 calc R . . C18 C 0.1358(6) 0.4007(5) 0.3694(3) 0.0374(10) Uani 1 1 d . . . H18 H 0.1405 0.4498 0.4147 0.045 Uiso 1 1 calc R . . C19 C 0.3980(10) 0.0108(6) 0.1479(4) 0.0652(17) Uani 1 1 d . . . H19A H 0.2978 0.0687 0.1160 0.098 Uiso 1 1 calc R . . H19B H 0.4131 -0.0787 0.1438 0.098 Uiso 1 1 calc R . . H19C H 0.4897 0.0317 0.1192 0.098 Uiso 1 1 calc R . . C20 C 0.9179(6) 0.1692(4) 0.7359(3) 0.0318(9) Uani 1 1 d . . . H20 H 1.0297 0.1521 0.7443 0.038 Uiso 1 1 calc R . . C21 C 0.8724(6) 0.0872(4) 0.6915(3) 0.0348(9) Uani 1 1 d . . . H21 H 0.9520 0.0154 0.6703 0.042 Uiso 1 1 calc R . . C22 C 0.7115(6) 0.1117(4) 0.6790(3) 0.0359(10) Uani 1 1 d . . . H22 H 0.6784 0.0548 0.6512 0.043 Uiso 1 1 calc R . . C23 C 0.5962(6) 0.2205(4) 0.7072(3) 0.0341(9) Uani 1 1 d . . . H23 H 0.4840 0.2414 0.6970 0.041 Uiso 1 1 calc R . . C24 C 0.6513(5) 0.2965(4) 0.7505(3) 0.0273(8) Uani 1 1 d . . . C25 C 0.5381(5) 0.4128(4) 0.7849(3) 0.0289(9) Uani 1 1 d . . . H25 H 0.4246 0.4428 0.7749 0.035 Uiso 1 1 calc R . . C26 C 0.5215(5) 0.5783(4) 0.8765(3) 0.0301(8) Uani 1 1 d . . . H26 H 0.4940 0.5436 0.9396 0.036 Uiso 1 1 calc R . . C27 C 0.3674(6) 0.6749(5) 0.8309(4) 0.0459(12) Uani 1 1 d . . . H27A H 0.2883 0.6320 0.8279 0.055 Uiso 1 1 calc R . . H27B H 0.3907 0.7083 0.7673 0.055 Uiso 1 1 calc R . . C28 C 0.2958(7) 0.7866(6) 0.8848(5) 0.0615(16) Uani 1 1 d . . . H28A H 0.2003 0.8525 0.8515 0.074 Uiso 1 1 calc R . . H28B H 0.2595 0.7545 0.9455 0.074 Uiso 1 1 calc R . . C29 C 0.4195(7) 0.8483(5) 0.8984(4) 0.0569(13) Uani 1 1 d . . . H29A H 0.4448 0.8906 0.8381 0.068 Uiso 1 1 calc R . . H29B H 0.3720 0.9157 0.9376 0.068 Uiso 1 1 calc R . . C30 C 0.5733(6) 0.7505(5) 0.9424(3) 0.0412(11) Uani 1 1 d . . . H30A H 0.5504 0.7145 1.0052 0.049 Uiso 1 1 calc R . . H30B H 0.6522 0.7932 0.9470 0.049 Uiso 1 1 calc R . . C31 C 0.6459(5) 0.6417(4) 0.8862(3) 0.0315(8) Uani 1 1 d . . . H31 H 0.6703 0.6798 0.8234 0.038 Uiso 1 1 calc R . . C32 C 0.9427(5) 0.5610(4) 0.9249(3) 0.0399(9) Uani 1 1 d . . . H32 H 0.9500 0.6067 0.8615 0.048 Uiso 1 1 calc R . . C33 C 1.0841(5) 0.4341(4) 0.9319(3) 0.0347(9) Uani 1 1 d . . . C34 C 1.2322(6) 0.4180(5) 0.9698(3) 0.0450(10) Uani 1 1 d . . . H34 H 1.2448 0.4845 0.9971 0.054 Uiso 1 1 calc R . . C35 C 1.3591(6) 0.3049(5) 0.9671(4) 0.0440(11) Uani 1 1 d . . . H35 H 1.4590 0.2899 0.9959 0.053 Uiso 1 1 calc R . . C36 C 1.3412(6) 0.2138(5) 0.9227(3) 0.0421(11) Uani 1 1 d . . . H36 H 1.4302 0.1371 0.9169 0.051 Uiso 1 1 calc R . . C37 C 1.1916(6) 0.2350(5) 0.8862(3) 0.0397(11) Uani 1 1 d . . . H37 H 1.1784 0.1704 0.8570 0.048 Uiso 1 1 calc R . . C38 C 0.9471(8) 0.5984(6) 1.0785(4) 0.0596(14) Uani 1 1 d . . . H38A H 0.8330 0.6212 1.0958 0.089 Uiso 1 1 calc R . . H38B H 0.9993 0.6392 1.1140 0.089 Uiso 1 1 calc R . . H38C H 1.0011 0.5045 1.0915 0.089 Uiso 1 1 calc R . . C39 C 0.3671(7) -0.0601(5) 0.5840(5) 0.0563(15) Uani 1 1 d . . . C40 C 0.4327(7) 0.6056(5) 0.2259(4) 0.0536(14) Uani 1 1 d . . . C41 C 0.8918(8) 0.0131(5) 0.9914(4) 0.0533(13) Uani 1 1 d . . . C42 C 0.9644(8) 0.7219(6) 0.6436(4) 0.0550(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0201(3) 0.0362(2) 0.0309(2) -0.00933(18) -0.00339(18) -0.00996(19) S1 0.0256(6) 0.0428(6) 0.0376(5) -0.0019(4) -0.0033(4) -0.0168(5) F1 0.112(3) 0.093(3) 0.093(3) -0.055(2) 0.028(3) -0.058(3) O1 0.074(3) 0.0502(19) 0.0416(18) -0.0069(14) -0.0122(17) -0.0312(19) N1 0.0242(18) 0.0391(18) 0.0277(16) -0.0079(13) -0.0016(14) -0.0152(15) C1 0.025(2) 0.047(2) 0.045(2) -0.0150(19) -0.0021(18) -0.0137(19) Cu2 0.0191(3) 0.0310(2) 0.0472(3) -0.0122(2) -0.0044(2) -0.00971(19) S2 0.0278(5) 0.0377(5) 0.0291(5) -0.0040(4) -0.0031(4) -0.0108(4) F2 0.059(2) 0.0495(19) 0.137(3) 0.006(2) 0.000(2) -0.0334(18) O2 0.059(2) 0.055(2) 0.0461(18) -0.0117(15) -0.0043(16) -0.0274(18) N2 0.027(2) 0.0379(19) 0.0301(17) -0.0019(14) 0.0004(15) -0.0130(16) C2 0.040(3) 0.046(2) 0.053(3) -0.023(2) 0.003(2) -0.016(2) S3 0.0331(5) 0.0417(5) 0.0323(5) -0.0083(4) -0.0063(4) -0.0094(4) F3 0.037(2) 0.051(2) 0.164(4) -0.001(2) -0.009(2) 0.0029(16) O3 0.0315(18) 0.0586(19) 0.0369(15) -0.0051(14) -0.0029(13) -0.0281(15) N3 0.034(2) 0.0388(19) 0.0371(18) -0.0045(15) -0.0060(16) -0.0124(17) C3 0.041(3) 0.051(3) 0.045(2) -0.013(2) -0.002(2) -0.028(2) S4 0.0222(5) 0.0371(5) 0.0366(5) -0.0046(4) -0.0032(4) -0.0136(4) F4 0.100(3) 0.0361(15) 0.078(2) 0.0061(15) 0.018(2) 0.0056(17) O4 0.0294(19) 0.056(2) 0.0526(19) 0.0015(15) -0.0195(15) -0.0158(16) N4 0.0261(19) 0.0345(18) 0.0258(16) -0.0036(13) 0.0000(13) -0.0096(15) C4 0.031(3) 0.046(2) 0.038(2) -0.0066(19) -0.0040(18) -0.020(2) F5 0.067(2) 0.0574(18) 0.0630(19) -0.0111(15) 0.0281(17) 0.0050(16) O5 0.042(2) 0.073(3) 0.0462(18) -0.0167(17) 0.0048(16) -0.0307(19) N5 0.0215(18) 0.0344(17) 0.0254(15) -0.0043(13) -0.0032(13) -0.0139(15) C5 0.022(2) 0.044(2) 0.0283(19) -0.0053(16) -0.0011(16) -0.0180(18) F6 0.121(4) 0.083(3) 0.113(3) -0.059(3) 0.007(3) -0.053(3) O6 0.051(2) 0.0463(18) 0.0396(17) 0.0010(14) 0.0131(15) -0.0142(16) N6 0.026(2) 0.0330(19) 0.058(2) -0.0144(17) 0.0002(17) -0.0123(16) C6 0.020(2) 0.046(2) 0.0296(19) -0.0022(17) -0.0048(16) -0.0127(19) F7 0.085(3) 0.069(2) 0.073(2) -0.0184(18) 0.036(2) 0.011(2) O7 0.048(2) 0.073(2) 0.055(2) -0.0088(17) -0.0219(17) -0.0273(19) N7 0.0226(18) 0.0300(17) 0.0353(17) -0.0046(13) 0.0002(14) -0.0105(14) C7 0.031(2) 0.040(2) 0.0277(18) -0.0040(16) 0.0008(16) -0.0063(17) F8 0.105(3) 0.075(2) 0.090(3) -0.038(2) -0.024(2) -0.032(2) O8 0.0281(15) 0.0431(16) 0.0281(13) -0.0007(11) -0.0008(11) -0.0102(12) N8 0.0215(18) 0.0354(17) 0.0329(16) -0.0058(13) 0.0017(14) -0.0129(14) C8 0.025(2) 0.051(3) 0.049(3) -0.010(2) -0.0036(19) 0.0026(19) F9 0.138(4) 0.0397(16) 0.061(2) -0.0076(14) 0.002(2) 0.0008(19) O9 0.043(2) 0.107(3) 0.050(2) -0.041(2) 0.0145(18) -0.041(2) C9 0.046(4) 0.051(3) 0.057(3) -0.018(2) -0.007(3) 0.010(3) F10 0.044(2) 0.070(2) 0.164(4) 0.050(3) -0.006(3) -0.0101(19) O10 0.0351(19) 0.0531(19) 0.0380(16) 0.0076(13) -0.0009(14) -0.0242(15) C10 0.057(3) 0.056(3) 0.045(3) -0.020(2) -0.008(2) 0.011(2) F11 0.073(3) 0.069(2) 0.110(3) 0.014(2) -0.002(2) -0.049(2) O11 0.032(2) 0.078(3) 0.069(2) 0.014(2) -0.0189(18) -0.0245(19) C11 0.059(4) 0.039(2) 0.037(2) -0.0161(19) -0.008(2) 0.001(2) F12 0.198(6) 0.069(3) 0.104(3) -0.050(2) 0.053(4) -0.054(3) O12 0.0378(18) 0.0412(16) 0.0426(16) -0.0060(13) 0.0071(14) -0.0124(14) C12 0.033(2) 0.038(2) 0.033(2) -0.0088(16) -0.0030(17) -0.0042(17) O13 0.066(3) 0.089(3) 0.104(3) -0.032(3) -0.054(3) -0.011(2) C13 0.038(2) 0.0375(19) 0.0256(17) -0.0060(14) -0.0029(15) -0.0237(17) O14 0.059(2) 0.057(2) 0.0426(18) 0.0002(16) 0.0178(17) -0.0102(18) C14 0.031(2) 0.044(2) 0.0298(19) -0.0034(16) -0.0036(16) -0.0217(17) C15 0.043(3) 0.066(3) 0.037(2) -0.004(2) -0.010(2) -0.035(2) C16 0.035(3) 0.084(4) 0.043(2) 0.005(2) -0.014(2) -0.030(3) C17 0.022(3) 0.070(3) 0.044(3) -0.001(2) -0.002(2) -0.015(2) C18 0.025(2) 0.047(2) 0.037(2) -0.0025(18) -0.0053(18) -0.011(2) C19 0.099(5) 0.069(4) 0.041(3) -0.013(2) -0.011(3) -0.042(4) C20 0.026(2) 0.038(2) 0.034(2) -0.0106(16) 0.0019(16) -0.0122(17) C21 0.034(2) 0.036(2) 0.039(2) -0.0137(16) 0.0033(18) -0.0155(18) C22 0.037(3) 0.040(2) 0.039(2) -0.0130(18) 0.0012(19) -0.021(2) C23 0.028(2) 0.046(2) 0.035(2) -0.0085(17) -0.0022(17) -0.0184(19) C24 0.021(2) 0.036(2) 0.0268(18) -0.0015(15) -0.0004(15) -0.0138(17) C25 0.021(2) 0.036(2) 0.0304(19) -0.0035(16) 0.0004(16) -0.0114(17) C26 0.0262(19) 0.0322(19) 0.0328(19) -0.0089(15) -0.0003(16) -0.0098(15) C27 0.030(2) 0.047(3) 0.059(3) -0.018(2) -0.009(2) -0.005(2) C28 0.038(3) 0.054(3) 0.082(4) -0.027(3) -0.005(3) 0.006(3) C29 0.053(3) 0.043(3) 0.067(3) -0.022(2) -0.002(2) -0.002(2) C30 0.042(3) 0.038(2) 0.046(2) -0.0166(19) 0.006(2) -0.013(2) C31 0.0272(19) 0.0265(18) 0.042(2) -0.0093(16) 0.0018(16) -0.0089(15) C32 0.040(2) 0.040(2) 0.043(2) -0.0144(18) -0.0086(18) -0.0133(18) C33 0.034(2) 0.039(2) 0.033(2) -0.0027(16) -0.0074(17) -0.0167(18) C34 0.040(3) 0.052(3) 0.049(3) -0.010(2) -0.014(2) -0.021(2) C35 0.027(2) 0.056(3) 0.051(3) 0.003(2) -0.015(2) -0.020(2) C36 0.027(3) 0.053(3) 0.044(3) -0.005(2) -0.007(2) -0.012(2) C37 0.026(2) 0.049(3) 0.046(2) -0.015(2) -0.002(2) -0.011(2) C38 0.064(4) 0.074(4) 0.051(3) -0.019(3) 0.003(3) -0.033(3) C39 0.043(3) 0.047(3) 0.083(4) -0.007(3) 0.003(3) -0.022(2) C40 0.061(3) 0.040(3) 0.056(3) -0.016(2) 0.019(3) -0.012(2) C41 0.067(4) 0.035(2) 0.047(3) -0.011(2) -0.001(3) -0.002(2) C42 0.054(4) 0.050(3) 0.061(3) -0.001(2) 0.007(3) -0.023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 1.943(4) . ? Cu1 N2 1.982(4) . ? Cu1 N3 2.020(4) . ? Cu1 N1 2.045(4) . ? Cu1 O3 2.365(3) . ? S1 O4 1.433(4) . ? S1 O5 1.439(4) . ? S1 O3 1.447(3) . ? S1 C39 1.811(6) . ? F1 C39 1.348(8) . ? O1 C13 1.415(5) . ? O1 C19 1.448(6) . ? N1 C1 1.330(6) . ? N1 C5 1.369(6) . ? C1 C2 1.390(7) . ? C1 H1 0.9500 . ? Cu2 N7 1.955(4) . ? Cu2 N5 1.985(4) . ? Cu2 N6 2.035(4) . ? Cu2 N8 2.060(4) . ? Cu2 O12 2.332(3) . ? S2 O7 1.435(4) . ? S2 O6 1.437(3) . ? S2 O8 1.444(3) . ? S2 C40 1.807(5) . ? F2 C39 1.329(6) . ? O2 C32 1.405(5) . ? O2 C38 1.426(6) . ? N2 C18 1.350(6) . ? N2 C14 1.361(6) . ? C2 C3 1.390(7) . ? C2 H2 0.9500 . ? S3 O13 1.417(4) . ? S3 O14 1.427(4) . ? S3 O12 1.440(4) . ? S3 C41 1.817(5) . ? F3 C39 1.341(8) . ? N3 C13 1.448(5) . ? N3 C12 1.500(6) . ? N3 H3A 0.9300 . ? C3 C4 1.376(7) . ? C3 H3 0.9500 . ? S4 O11 1.431(4) . ? S4 O9 1.432(4) . ? S4 O10 1.444(3) . ? S4 C42 1.810(6) . ? F4 C40 1.345(7) . ? N4 C6 1.273(6) . ? N4 C7 1.460(5) . ? C4 C5 1.381(6) . ? C4 H4 0.9500 . ? F5 C40 1.329(6) . ? N5 C33 1.337(5) . ? N5 C37 1.343(6) . ? C5 C6 1.467(6) . ? F6 C40 1.320(8) . ? N6 C32 1.431(6) . ? N6 C31 1.490(6) . ? N6 H6A 0.9300 . ? C6 H6 0.9500 . ? F7 C41 1.332(7) . ? N7 C25 1.268(6) . ? N7 C26 1.462(5) . ? C7 C8 1.528(6) . ? C7 C12 1.538(6) . ? C7 H7 1.0000 . ? F8 C41 1.337(7) . ? N8 C20 1.322(5) . ? N8 C24 1.359(6) . ? C8 C9 1.516(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? F9 C41 1.309(6) . ? C9 C10 1.541(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? F10 C42 1.334(8) . ? C10 C11 1.546(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? F11 C42 1.326(6) . ? C11 C12 1.534(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? F12 C42 1.307(8) . ? C12 H12 1.0000 . ? C13 C14 1.505(6) . ? C13 H13 1.0000 . ? C14 C15 1.384(6) . ? C15 C16 1.387(8) . ? C15 H15 0.9500 . ? C16 C17 1.375(9) . ? C16 H16 0.9500 . ? C17 C18 1.373(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.395(6) . ? C20 H20 0.9500 . ? C21 C22 1.368(7) . ? C21 H21 0.9500 . ? C22 C23 1.395(6) . ? C22 H22 0.9500 . ? C23 C24 1.378(6) . ? C23 H23 0.9500 . ? C24 C25 1.485(6) . ? C25 H25 0.9500 . ? C26 C27 1.512(6) . ? C26 C31 1.536(5) . ? C26 H26 1.0000 . ? C27 C28 1.527(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.531(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.505(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.525(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31 1.0000 . ? C32 C33 1.516(6) . ? C32 H32 1.0000 . ? C33 C34 1.395(6) . ? C34 C35 1.367(7) . ? C34 H34 0.9500 . ? C35 C36 1.366(7) . ? C35 H35 0.9500 . ? C36 C37 1.383(7) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? 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_3 _geom_angle_publ_flag N4 Cu1 N2 165.65(14) . . ? N4 Cu1 N3 83.12(16) . . ? N2 Cu1 N3 83.13(16) . . ? N4 Cu1 N1 80.85(15) . . ? N2 Cu1 N1 112.71(15) . . ? N3 Cu1 N1 163.86(16) . . ? N4 Cu1 O3 89.88(13) . . ? N2 Cu1 O3 94.61(13) . . ? N3 Cu1 O3 91.73(14) . . ? N1 Cu1 O3 90.06(12) . . ? O4 S1 O5 116.7(2) . . ? O4 S1 O3 116.3(2) . . ? O5 S1 O3 114.1(2) . . ? O4 S1 C39 102.6(3) . . ? O5 S1 C39 102.1(3) . . ? O3 S1 C39 101.6(2) . . ? C13 O1 C19 115.8(4) . . ? C1 N1 C5 117.0(4) . . ? C1 N1 Cu1 132.2(3) . . ? C5 N1 Cu1 110.8(3) . . ? N1 C1 C2 123.6(5) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? N7 Cu2 N5 165.86(14) . . ? N7 Cu2 N6 82.79(16) . . ? N5 Cu2 N6 83.08(15) . . ? N7 Cu2 N8 80.89(15) . . ? N5 Cu2 N8 113.25(14) . . ? N6 Cu2 N8 163.64(16) . . ? N7 Cu2 O12 84.36(13) . . ? N5 Cu2 O12 95.65(13) . . ? N6 Cu2 O12 92.47(14) . . ? N8 Cu2 O12 87.13(13) . . ? O7 S2 O6 116.5(2) . . ? O7 S2 O8 115.0(2) . . ? O6 S2 O8 113.9(2) . . ? O7 S2 C40 103.4(3) . . ? O6 S2 C40 103.3(2) . . ? O8 S2 C40 102.1(2) . . ? C32 O2 C38 114.7(4) . . ? C18 N2 C14 118.6(4) . . ? C18 N2 Cu1 129.0(3) . . ? C14 N2 Cu1 112.3(3) . . ? C1 C2 C3 118.7(5) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? O13 S3 O14 116.0(3) . . ? O13 S3 O12 115.6(3) . . ? O14 S3 O12 113.4(2) . . ? O13 S3 C41 103.7(3) . . ? O14 S3 C41 102.7(3) . . ? O12 S3 C41 102.9(2) . . ? S1 O3 Cu1 142.8(2) . . ? C13 N3 C12 117.0(3) . . ? C13 N3 Cu1 108.6(3) . . ? C12 N3 Cu1 108.0(3) . . ? C13 N3 H3A 107.6 . . ? C12 N3 H3A 107.6 . . ? Cu1 N3 H3A 107.6 . . ? C4 C3 C2 118.6(4) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? O11 S4 O9 116.5(3) . . ? O11 S4 O10 114.8(2) . . ? O9 S4 O10 115.0(2) . . ? O11 S4 C42 102.6(3) . . ? O9 S4 C42 102.8(3) . . ? O10 S4 C42 102.2(2) . . ? C6 N4 C7 127.0(4) . . ? C6 N4 Cu1 117.3(3) . . ? C7 N4 Cu1 115.5(3) . . ? C5 C4 C3 119.4(5) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C33 N5 C37 118.3(4) . . ? C33 N5 Cu2 112.4(3) . . ? C37 N5 Cu2 129.2(3) . . ? N1 C5 C4 122.7(4) . . ? N1 C5 C6 114.5(4) . . ? C4 C5 C6 122.8(4) . . ? C32 N6 C31 119.0(3) . . ? C32 N6 Cu2 107.1(3) . . ? C31 N6 Cu2 107.1(3) . . ? C32 N6 H6A 107.7 . . ? C31 N6 H6A 107.7 . . ? Cu2 N6 H6A 107.7 . . ? N4 C6 C5 115.6(4) . . ? N4 C6 H6 122.2 . . ? C5 C6 H6 122.2 . . ? C25 N7 C26 126.8(4) . . ? C25 N7 Cu2 117.7(3) . . ? C26 N7 Cu2 115.0(3) . . ? N4 C7 C8 116.9(4) . . ? N4 C7 C12 105.6(3) . . ? C8 C7 C12 111.6(4) . . ? N4 C7 H7 107.4 . . ? C8 C7 H7 107.4 . . ? C12 C7 H7 107.4 . . ? C20 N8 C24 118.3(4) . . ? C20 N8 Cu2 131.0(3) . . ? C24 N8 Cu2 110.4(3) . . ? C9 C8 C7 109.7(5) . . ? C9 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? C9 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C8 C9 C10 111.7(5) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? C9 C10 C11 111.0(4) . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 108.6(5) . . ? C12 C11 H11A 110.0 . . ? C10 C11 H11A 110.0 . . ? C12 C11 H11B 110.0 . . ? C10 C11 H11B 110.0 . . ? H11A C11 H11B 108.3 . . ? S3 O12 Cu2 147.0(2) . . ? N3 C12 C11 114.3(4) . . ? N3 C12 C7 106.6(3) . . ? C11 C12 C7 110.2(4) . . ? N3 C12 H12 108.5 . . ? C11 C12 H12 108.5 . . ? C7 C12 H12 108.5 . . ? O1 C13 N3 110.5(3) . . ? O1 C13 C14 108.9(3) . . ? N3 C13 C14 109.1(3) . . ? O1 C13 H13 109.4 . . ? N3 C13 H13 109.4 . . ? C14 C13 H13 109.4 . . ? N2 C14 C15 121.1(4) . . ? N2 C14 C13 116.8(4) . . ? C15 C14 C13 122.2(4) . . ? C16 C15 C14 119.4(5) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 C16 C15 119.4(5) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C18 C17 C16 119.1(5) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? N2 C18 C17 122.5(5) . . ? N2 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? O1 C19 H19A 109.5 . . ? O1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N8 C20 C21 122.2(4) . . ? N8 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C22 C21 C20 119.1(4) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C21 C22 C23 119.8(4) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 117.4(4) . . ? C24 C23 H23 121.3 . . ? C22 C23 H23 121.3 . . ? N8 C24 C23 123.1(4) . . ? N8 C24 C25 115.3(4) . . ? C23 C24 C25 121.6(4) . . ? N7 C25 C24 115.1(4) . . ? N7 C25 H25 122.4 . . ? C24 C25 H25 122.4 . . ? N7 C26 C27 115.0(4) . . ? N7 C26 C31 106.2(3) . . ? C27 C26 C31 111.6(3) . . ? N7 C26 H26 108.0 . . ? C27 C26 H26 108.0 . . ? C31 C26 H26 108.0 . . ? C26 C27 C28 110.2(4) . . ? C26 C27 H27A 109.6 . . ? C28 C27 H27A 109.6 . . ? C26 C27 H27B 109.6 . . ? C28 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? C29 C28 C27 111.4(5) . . ? C29 C28 H28A 109.3 . . ? C27 C28 H28A 109.3 . . ? C29 C28 H28B 109.3 . . ? C27 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? C30 C29 C28 111.9(4) . . ? C30 C29 H29A 109.2 . . ? C28 C29 H29A 109.2 . . ? C30 C29 H29B 109.2 . . ? C28 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C29 C30 C31 110.7(4) . . ? C29 C30 H30A 109.5 . . ? C31 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? N6 C31 C30 116.2(4) . . ? N6 C31 C26 106.2(3) . . ? C30 C31 C26 109.4(3) . . ? N6 C31 H31 108.2 . . ? C30 C31 H31 108.2 . . ? C26 C31 H31 108.2 . . ? O2 C32 N6 119.9(4) . . ? O2 C32 C33 113.2(4) . . ? N6 C32 C33 108.7(3) . . ? O2 C32 H32 104.5 . . ? N6 C32 H32 104.5 . . ? C33 C32 H32 104.5 . . ? N5 C33 C34 121.8(4) . . ? N5 C33 C32 116.0(4) . . ? C34 C33 C32 121.8(4) . . ? C35 C34 C33 118.9(4) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? C36 C35 C34 119.5(5) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C35 C36 C37 118.9(5) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? N5 C37 C36 122.3(5) . . ? N5 C37 H37 118.8 . . ? C36 C37 H37 118.8 . . ? O2 C38 H38A 109.5 . . ? O2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? F2 C39 F1 108.2(5) . . ? F2 C39 F3 106.3(5) . . ? F1 C39 F3 109.8(5) . . ? F2 C39 S1 111.4(4) . . ? F1 C39 S1 109.9(4) . . ? F3 C39 S1 111.2(4) . . ? F6 C40 F5 108.5(5) . . ? F6 C40 F4 107.5(5) . . ? F5 C40 F4 106.1(5) . . ? F6 C40 S2 111.9(4) . . ? F5 C40 S2 111.9(4) . . ? F4 C40 S2 110.6(4) . . ? F9 C41 F7 109.2(5) . . ? F9 C41 F8 108.5(5) . . ? F7 C41 F8 104.8(5) . . ? F9 C41 S3 113.4(4) . . ? F7 C41 S3 110.3(4) . . ? F8 C41 S3 110.3(4) . . ? F12 C42 F11 107.4(6) . . ? F12 C42 F10 107.2(6) . . ? F11 C42 F10 106.6(5) . . ? F12 C42 S4 113.2(4) . . ? F11 C42 S4 111.6(4) . . ? F10 C42 S4 110.6(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.600 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.064 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 804596' #TrackingRef '- All.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_absolute_configuration ad _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H24 Cu F6 N4 O6 S2' _chemical_formula_weight 658.09 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 Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.5520(2) _cell_length_b 27.0250(10) _cell_length_c 10.1510(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.143(2) _cell_angle_gamma 90.00 _cell_volume 2600.07(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 51323 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 1.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8118 _exptl_absorpt_correction_T_max 0.8990 _exptl_absorpt_process_details ? _exptl_special_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34132 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0634 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11316 _reflns_number_gt 8946 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+1.2620P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(9) _refine_ls_number_reflns 11316 _refine_ls_number_parameters 735 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.12541(5) 0.312406(18) 0.63192(5) 0.02913(12) Uani 1 1 d . . . S1 S -0.16390(11) 0.22958(4) 0.50776(11) 0.0334(2) Uani 1 1 d . . . F1 F -0.0391(5) 0.23539(18) 0.2956(4) 0.1004(15) Uani 1 1 d . . . O1 O -0.1190(3) 0.27991(11) 0.5340(3) 0.0386(7) Uani 1 1 d . . . N1 N 0.0221(4) 0.37666(13) 0.6415(3) 0.0297(8) Uani 1 1 d . . . C1 C 0.1889(5) 0.33647(18) 0.3533(4) 0.0341(10) Uani 1 1 d . . . H1 H 0.1148 0.3602 0.3469 0.041 Uiso 1 1 calc R . . Cu2 Cu 0.38205(5) 0.502065(18) 0.40447(5) 0.03142(13) Uani 1 1 d . . . S2 S 0.45200(11) 0.35930(4) 0.86348(10) 0.0295(2) Uani 1 1 d . . . F2 F -0.1861(5) 0.17699(13) 0.2899(3) 0.0836(12) Uani 1 1 d . . . O2 O -0.0617(3) 0.19322(12) 0.5618(3) 0.0423(8) Uani 1 1 d . . . N2 N 0.2113(3) 0.30792(14) 0.4629(3) 0.0277(7) Uani 1 1 d . . . C2 C 0.2691(5) 0.33255(17) 0.2505(4) 0.0336(10) Uani 1 1 d . . . H2 H 0.2515 0.3536 0.1754 0.040 Uiso 1 1 calc R . . S3 S 0.68427(13) 0.57893(5) 0.51206(12) 0.0396(3) Uani 1 1 d . . . F3 F -0.2606(5) 0.25126(13) 0.2614(3) 0.0843(12) Uani 1 1 d . . . O3 O -0.3065(3) 0.21887(17) 0.5267(4) 0.0605(10) Uani 1 1 d . . . N3 N 0.2001(3) 0.24333(13) 0.6548(3) 0.0258(7) Uani 1 1 d . . . H2A H 0.1341 0.2221 0.6095 0.031 Uiso 1 1 calc R . . C3 C 0.3752(5) 0.29793(18) 0.2571(4) 0.0351(11) Uani 1 1 d . . . H3 H 0.4336 0.2954 0.1883 0.042 Uiso 1 1 calc R . . S4 S 0.02853(12) 0.45153(5) 0.15683(10) 0.0354(3) Uani 1 1 d . . . F4 F 0.6853(3) 0.32403(11) 0.9977(2) 0.0458(7) Uani 1 1 d . . . O4 O 0.3806(3) 0.34431(13) 0.7352(3) 0.0383(8) Uani 1 1 d . . . N4 N 0.0929(4) 0.30678(14) 0.8215(3) 0.0315(8) Uani 1 1 d . . . H3A H 0.1702 0.3207 0.8731 0.038 Uiso 1 1 calc R . . C4 C 0.3951(4) 0.26675(17) 0.3663(4) 0.0331(10) Uani 1 1 d . . . H4 H 0.4651 0.2416 0.3715 0.040 Uiso 1 1 calc R . . F5 F 0.5251(3) 0.26935(12) 0.9478(3) 0.0593(8) Uani 1 1 d . . . O5 O 0.3645(3) 0.35570(13) 0.9695(3) 0.0394(7) Uani 1 1 d . . . N5 N 0.4875(3) 0.43791(13) 0.3910(3) 0.0283(8) Uani 1 1 d . . . C5 C 0.3121(4) 0.27265(16) 0.4676(4) 0.0263(9) Uani 1 1 d . . . F6 F 0.6430(3) 0.29741(14) 0.7974(3) 0.0660(11) Uani 1 1 d . . . O6 O 0.5343(4) 0.40308(13) 0.8623(3) 0.0468(9) Uani 1 1 d . . . N6 N 0.4573(4) 0.51586(13) 0.2324(3) 0.0297(8) Uani 1 1 d . . . H6 H 0.5472 0.5292 0.2529 0.036 Uiso 1 1 calc R . . C6 C 0.3304(4) 0.24046(16) 0.5905(4) 0.0285(9) Uani 1 1 d . . . H6A H 0.3482 0.2058 0.5659 0.034 Uiso 1 1 calc R . . H6B H 0.4119 0.2521 0.6525 0.034 Uiso 1 1 calc R . . F7 F -0.0514(4) 0.54389(12) 0.1286(5) 0.0804(12) Uani 1 1 d . . . O7 O 0.8332(4) 0.57116(17) 0.5270(5) 0.0776(13) Uani 1 1 d . . . N7 N 0.2520(4) 0.55772(13) 0.3511(3) 0.0318(8) Uani 1 1 d . . . H7A H 0.1709 0.5441 0.3051 0.038 Uiso 1 1 calc R . . C7 C 0.2139(4) 0.23012(17) 0.7977(4) 0.0289(9) Uani 1 1 d . . . H7 H 0.3023 0.2456 0.8425 0.035 Uiso 1 1 calc R . . F8 F -0.1956(3) 0.49244(15) 0.0225(3) 0.0683(10) Uani 1 1 d . . . O8 O 0.6017(4) 0.53429(13) 0.5129(3) 0.0492(9) Uani 1 1 d . . . N8 N 0.2932(4) 0.50614(15) 0.5718(3) 0.0316(8) Uani 1 1 d . . . C8 C 0.2217(5) 0.17476(19) 0.8240(4) 0.0388(11) Uani 1 1 d . . . H8A H 0.3062 0.1609 0.7900 0.047 Uiso 1 1 calc R . . H8B H 0.1374 0.1584 0.7765 0.047 Uiso 1 1 calc R . . F9 F -0.1879(3) 0.49923(14) 0.2331(3) 0.0651(8) Uani 1 1 d . . . O9 O 0.6307(4) 0.61345(15) 0.4117(4) 0.0639(12) Uani 1 1 d . . . C9 C 0.2293(5) 0.1645(2) 0.9723(5) 0.0460(12) Uani 1 1 d . . . H9A H 0.3188 0.1778 1.0183 0.055 Uiso 1 1 calc R . . H9B H 0.2286 0.1283 0.9873 0.055 Uiso 1 1 calc R . . F10 F 0.6681(18) 0.5775(10) 0.775(2) 0.102(5) Uani 0.50 1 d P A 2 O10 O 0.1045(4) 0.45816(18) 0.0451(3) 0.0626(12) Uani 1 1 d . . . C10 C 0.1033(5) 0.18840(18) 1.0314(4) 0.0387(11) Uani 1 1 d . . . H10A H 0.0145 0.1723 0.9927 0.046 Uiso 1 1 calc R . . H10B H 0.1143 0.1829 1.1286 0.046 Uiso 1 1 calc R . . F11 F 0.690(3) 0.6485(10) 0.688(3) 0.091(6) Uani 0.50 1 d P A 2 O11 O 0.1069(4) 0.46477(14) 0.2823(3) 0.0472(9) Uani 1 1 d . . . C11 C 0.0946(5) 0.24331(18) 1.0034(4) 0.0372(10) Uani 1 1 d . . . H11A H 0.1778 0.2601 1.0517 0.045 Uiso 1 1 calc R . . H11B H 0.0090 0.2570 1.0357 0.045 Uiso 1 1 calc R . . F12 F 0.4935(15) 0.6140(9) 0.6732(17) 0.099(4) Uani 0.50 1 d P A 2 O12 O -0.0495(4) 0.40599(13) 0.1581(4) 0.0485(9) Uani 1 1 d . . . C12 C 0.0894(4) 0.25339(16) 0.8547(4) 0.0284(9) Uani 1 1 d . . . H12 H 0.0003 0.2389 0.8083 0.034 Uiso 1 1 calc R . . C13 C -0.0308(5) 0.33562(18) 0.8423(5) 0.0379(10) Uani 1 1 d . . . H13A H -0.0212 0.3477 0.9350 0.045 Uiso 1 1 calc R . . H13B H -0.1158 0.3144 0.8276 0.045 Uiso 1 1 calc R . . C14 C -0.0477(4) 0.37909(16) 0.7483(4) 0.0289(9) Uani 1 1 d . . . C15 C -0.1378(4) 0.41797(17) 0.7683(4) 0.0338(10) Uani 1 1 d . . . H15 H -0.1871 0.4184 0.8440 0.041 Uiso 1 1 calc R . . C16 C -0.1546(5) 0.45562(19) 0.6775(5) 0.0414(11) Uani 1 1 d . . . H16 H -0.2157 0.4825 0.6896 0.050 Uiso 1 1 calc R . . C17 C -0.0815(5) 0.45421(17) 0.5673(5) 0.0403(11) Uani 1 1 d . . . H17 H -0.0921 0.4799 0.5028 0.048 Uiso 1 1 calc R . . C18 C 0.0066(5) 0.41467(17) 0.5541(4) 0.0373(10) Uani 1 1 d . . . H18 H 0.0589 0.4140 0.4803 0.045 Uiso 1 1 calc R . . C19 C 0.5375(5) 0.40566(17) 0.4872(4) 0.0367(10) Uani 1 1 d . . . H19 H 0.5057 0.4088 0.5718 0.044 Uiso 1 1 calc R . . C20 C 0.6311(5) 0.36878(18) 0.4697(5) 0.0420(11) Uani 1 1 d . . . H20 H 0.6600 0.3462 0.5394 0.050 Uiso 1 1 calc R . . C21 C 0.6830(5) 0.36480(18) 0.3499(5) 0.0382(11) Uani 1 1 d . . . H21 H 0.7525 0.3408 0.3368 0.046 Uiso 1 1 calc R . . C22 C 0.6309(5) 0.39700(18) 0.2479(4) 0.0373(11) Uani 1 1 d . . . H22 H 0.6625 0.3945 0.1630 0.045 Uiso 1 1 calc R . . C23 C 0.5332(4) 0.43251(17) 0.2713(4) 0.0297(9) Uani 1 1 d . . . C24 C 0.4728(4) 0.46844(16) 0.1658(4) 0.0314(9) Uani 1 1 d . . . H24A H 0.5370 0.4720 0.0969 0.038 Uiso 1 1 calc R . . H24B H 0.3801 0.4567 0.1228 0.038 Uiso 1 1 calc R . . C25 C 0.3682(4) 0.55426(16) 0.1541(4) 0.0288(9) Uani 1 1 d . . . H25 H 0.2842 0.5375 0.1047 0.035 Uiso 1 1 calc R . . C26 C 0.4474(5) 0.58123(18) 0.0549(4) 0.0372(10) Uani 1 1 d . . . H26A H 0.4698 0.5578 -0.0146 0.045 Uiso 1 1 calc R . . H26B H 0.5373 0.5944 0.1006 0.045 Uiso 1 1 calc R . . C27 C 0.3574(6) 0.62412(19) -0.0097(5) 0.0454(12) Uani 1 1 d . . . H27A H 0.4147 0.6435 -0.0660 0.054 Uiso 1 1 calc R . . H27B H 0.2759 0.6103 -0.0679 0.054 Uiso 1 1 calc R . . C28 C 0.3042(5) 0.65790(17) 0.0902(5) 0.0421(11) Uani 1 1 d . . . H28A H 0.2425 0.6834 0.0433 0.051 Uiso 1 1 calc R . . H28B H 0.3852 0.6750 0.1414 0.051 Uiso 1 1 calc R . . C29 C 0.2212(5) 0.62943(17) 0.1866(4) 0.0375(10) Uani 1 1 d . . . H29A H 0.1904 0.6524 0.2534 0.045 Uiso 1 1 calc R . . H29B H 0.1363 0.6140 0.1373 0.045 Uiso 1 1 calc R . . C30 C 0.3175(5) 0.58950(17) 0.2554(4) 0.0333(10) Uani 1 1 d . . . H30 H 0.4019 0.6061 0.3044 0.040 Uiso 1 1 calc R . . C31 C 0.2094(5) 0.58271(18) 0.4678(5) 0.0414(11) Uani 1 1 d . . . H31A H 0.1129 0.5963 0.4465 0.050 Uiso 1 1 calc R . . H31B H 0.2744 0.6105 0.4941 0.050 Uiso 1 1 calc R . . C32 C 0.2126(4) 0.54666(16) 0.5787(4) 0.0291(9) Uani 1 1 d . . . C33 C 0.1395(5) 0.55526(17) 0.6873(4) 0.0350(10) Uani 1 1 d . . . H33 H 0.0825 0.5840 0.6902 0.042 Uiso 1 1 calc R . . C34 C 0.1509(5) 0.52145(19) 0.7909(4) 0.0388(11) Uani 1 1 d . . . H34 H 0.1007 0.5264 0.8649 0.047 Uiso 1 1 calc R . . C35 C 0.2364(5) 0.4803(2) 0.7849(5) 0.0439(12) Uani 1 1 d . . . H35 H 0.2474 0.4569 0.8552 0.053 Uiso 1 1 calc R . . C36 C 0.3049(5) 0.4743(2) 0.6749(5) 0.0447(12) Uani 1 1 d . . . H36 H 0.3638 0.4461 0.6712 0.054 Uiso 1 1 calc R . . C37 C -0.1632(7) 0.2228(2) 0.3301(5) 0.0555(14) Uani 1 1 d . . . C38 C 0.5833(5) 0.3102(2) 0.9041(4) 0.0414(11) Uani 1 1 d . . . C39 C 0.634(3) 0.6052(13) 0.677(3) 0.070(8) Uiso 0.50 1 d P A 2 C40 C -0.1078(5) 0.4990(2) 0.1328(5) 0.0453(11) Uani 1 1 d . . . F10A F 0.748(3) 0.6543(12) 0.667(4) 0.122(11) Uani 0.50 1 d P A 1 F11A F 0.7363(18) 0.5829(7) 0.7629(15) 0.097(5) Uani 0.50 1 d P A 1 F12A F 0.546(2) 0.6194(13) 0.662(3) 0.190(13) Uani 0.50 1 d P A 1 C39A C 0.669(4) 0.6108(10) 0.656(2) 0.084(9) Uani 0.50 1 d P A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0348(3) 0.0269(3) 0.0277(2) 0.0029(2) 0.01164(19) 0.0039(2) S1 0.0310(6) 0.0317(6) 0.0364(6) 0.0020(5) 0.0001(4) -0.0015(5) F1 0.129(4) 0.115(4) 0.068(2) -0.025(2) 0.056(2) -0.025(3) O1 0.0444(18) 0.0276(17) 0.0426(18) -0.0036(14) 0.0002(14) 0.0051(14) N1 0.032(2) 0.027(2) 0.0314(19) -0.0008(15) 0.0071(15) -0.0020(15) C1 0.046(3) 0.033(3) 0.024(2) 0.0026(18) 0.0047(18) 0.005(2) Cu2 0.0407(3) 0.0285(3) 0.0265(2) 0.0045(2) 0.0098(2) 0.0084(2) S2 0.0283(5) 0.0326(6) 0.0283(5) 0.0022(4) 0.0067(4) -0.0031(4) F2 0.141(4) 0.042(2) 0.059(2) -0.0200(16) -0.023(2) 0.012(2) O2 0.0386(18) 0.0292(18) 0.055(2) 0.0072(14) -0.0079(15) -0.0021(14) N2 0.0290(17) 0.026(2) 0.0296(18) 0.0004(15) 0.0087(13) 0.0002(16) C2 0.040(2) 0.038(3) 0.024(2) 0.0042(18) 0.0093(18) -0.002(2) S3 0.0442(7) 0.0308(6) 0.0401(6) 0.0000(5) -0.0093(5) -0.0028(5) F3 0.148(4) 0.056(2) 0.0418(18) 0.0051(16) -0.017(2) 0.022(2) O3 0.0300(18) 0.080(3) 0.072(3) 0.006(2) 0.0057(16) -0.0105(18) N3 0.0308(18) 0.0257(18) 0.0214(16) 0.0015(13) 0.0049(13) 0.0010(14) C3 0.034(2) 0.045(3) 0.028(2) -0.0052(18) 0.0097(17) -0.007(2) S4 0.0358(6) 0.0393(7) 0.0317(5) 0.0033(5) 0.0072(4) -0.0026(5) F4 0.0337(14) 0.057(2) 0.0437(15) -0.0094(13) -0.0084(11) 0.0046(13) O4 0.0387(17) 0.046(2) 0.0300(16) -0.0007(14) 0.0022(13) -0.0018(15) N4 0.0354(19) 0.027(2) 0.0332(19) -0.0010(16) 0.0078(14) -0.0009(16) C4 0.030(2) 0.037(3) 0.034(2) -0.0037(19) 0.0083(18) -0.0051(19) F5 0.0421(16) 0.0380(18) 0.094(2) 0.0077(16) -0.0059(15) 0.0039(14) O5 0.0343(16) 0.054(2) 0.0326(16) 0.0033(15) 0.0130(13) 0.0057(15) N5 0.0283(18) 0.027(2) 0.0302(18) 0.0009(15) 0.0065(14) 0.0021(15) C5 0.023(2) 0.029(2) 0.027(2) -0.0050(17) 0.0028(16) -0.0057(17) F6 0.0373(15) 0.106(3) 0.0551(18) -0.0366(17) 0.0083(13) 0.0151(16) O6 0.0435(19) 0.038(2) 0.058(2) 0.0060(16) 0.0017(16) -0.0130(16) N6 0.0286(18) 0.029(2) 0.0316(19) 0.0003(14) 0.0032(14) 0.0024(14) C6 0.027(2) 0.032(2) 0.028(2) 0.0013(17) 0.0073(16) 0.0048(17) F7 0.061(2) 0.040(2) 0.137(3) 0.022(2) 0.000(2) -0.0035(16) O7 0.046(2) 0.062(3) 0.119(4) 0.012(3) -0.013(2) -0.003(2) N7 0.037(2) 0.029(2) 0.0289(19) 0.0018(15) 0.0035(15) -0.0027(16) C7 0.026(2) 0.037(3) 0.023(2) 0.0042(17) 0.0024(15) -0.0015(18) F8 0.0559(19) 0.084(3) 0.0606(19) -0.0016(18) -0.0104(15) 0.0146(18) O8 0.056(2) 0.041(2) 0.047(2) 0.0015(15) -0.0073(16) -0.0153(17) N8 0.0335(19) 0.034(2) 0.0276(17) 0.0018(17) 0.0070(14) 0.0019(18) C8 0.042(3) 0.041(3) 0.036(2) 0.007(2) 0.012(2) 0.010(2) F9 0.063(2) 0.066(2) 0.069(2) -0.0115(18) 0.0219(16) 0.0110(18) O9 0.062(2) 0.058(3) 0.063(2) 0.0251(19) -0.0240(19) -0.015(2) C9 0.051(3) 0.051(3) 0.036(3) 0.016(2) 0.009(2) 0.015(2) F10 0.118(12) 0.140(13) 0.047(6) -0.001(7) 0.002(7) -0.020(10) O10 0.038(2) 0.112(4) 0.0412(19) 0.021(2) 0.0168(15) 0.008(2) C10 0.042(3) 0.045(3) 0.029(2) 0.005(2) 0.0038(19) 0.001(2) F11 0.125(16) 0.041(10) 0.089(8) -0.026(7) -0.053(10) -0.005(9) O11 0.053(2) 0.050(2) 0.0360(18) 0.0028(15) -0.0065(15) -0.0107(17) C11 0.040(2) 0.045(3) 0.026(2) 0.0007(19) 0.0049(18) -0.003(2) F12 0.057(7) 0.153(10) 0.093(8) -0.048(7) 0.033(6) 0.017(7) O12 0.044(2) 0.037(2) 0.065(2) -0.0043(16) 0.0082(16) -0.0058(16) C12 0.028(2) 0.032(2) 0.026(2) 0.0032(17) 0.0027(16) -0.0011(18) C13 0.039(2) 0.036(3) 0.042(3) 0.003(2) 0.018(2) 0.004(2) C14 0.026(2) 0.027(2) 0.034(2) -0.0076(18) 0.0066(17) -0.0074(17) C15 0.030(2) 0.028(2) 0.046(3) -0.0111(19) 0.0129(19) -0.0014(18) C16 0.038(3) 0.030(3) 0.055(3) -0.007(2) 0.001(2) 0.006(2) C17 0.050(3) 0.025(2) 0.043(3) -0.002(2) -0.006(2) 0.003(2) C18 0.045(3) 0.032(3) 0.036(2) -0.0005(19) 0.0057(19) 0.000(2) C19 0.046(3) 0.033(3) 0.033(2) 0.0044(19) 0.0110(19) 0.006(2) C20 0.050(3) 0.029(3) 0.046(3) 0.003(2) 0.001(2) 0.004(2) C21 0.032(2) 0.029(3) 0.054(3) -0.006(2) 0.007(2) 0.0036(19) C22 0.042(3) 0.032(3) 0.039(2) -0.007(2) 0.011(2) -0.002(2) C23 0.031(2) 0.030(2) 0.028(2) -0.0012(17) 0.0034(17) -0.0054(18) C24 0.036(2) 0.033(2) 0.026(2) -0.0024(17) 0.0105(17) 0.0024(19) C25 0.030(2) 0.030(2) 0.026(2) 0.0056(17) 0.0012(16) -0.0025(18) C26 0.043(3) 0.037(3) 0.034(2) 0.0071(19) 0.0105(19) -0.002(2) C27 0.058(3) 0.043(3) 0.036(3) 0.015(2) 0.008(2) -0.002(2) C28 0.046(3) 0.030(3) 0.048(3) 0.011(2) -0.003(2) -0.009(2) C29 0.039(3) 0.035(3) 0.038(2) 0.007(2) 0.0024(19) 0.005(2) C30 0.040(3) 0.030(2) 0.029(2) 0.0040(18) -0.0011(18) -0.0025(19) C31 0.054(3) 0.029(3) 0.044(3) 0.003(2) 0.016(2) 0.009(2) C32 0.029(2) 0.024(2) 0.034(2) -0.0028(17) 0.0033(17) 0.0011(17) C33 0.034(2) 0.035(3) 0.037(2) -0.0046(19) 0.0104(18) 0.0007(19) C34 0.042(3) 0.044(3) 0.032(2) -0.004(2) 0.0109(19) -0.003(2) C35 0.044(3) 0.058(3) 0.032(2) 0.012(2) 0.012(2) 0.007(3) C36 0.053(3) 0.048(3) 0.036(3) 0.011(2) 0.017(2) 0.019(2) C37 0.084(4) 0.041(3) 0.040(3) 0.001(2) 0.002(3) 0.007(3) C38 0.033(2) 0.046(3) 0.044(3) -0.009(2) -0.0010(19) -0.004(2) C40 0.044(3) 0.041(3) 0.050(3) 0.000(2) 0.003(2) -0.004(2) F10A 0.17(2) 0.045(7) 0.133(17) -0.031(8) -0.068(16) -0.024(13) F11A 0.176(17) 0.082(8) 0.026(5) -0.012(5) -0.015(8) -0.011(11) F12A 0.15(2) 0.25(3) 0.195(17) -0.116(17) 0.110(17) 0.04(2) C39A 0.16(3) 0.057(13) 0.033(9) -0.022(8) 0.022(11) -0.006(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 1.993(3) . ? Cu1 N2 1.995(3) . ? Cu1 N3 2.002(3) . ? Cu1 N1 2.006(4) . ? S1 O3 1.429(3) . ? S1 O1 1.441(3) . ? S1 O2 1.444(3) . ? S1 C37 1.814(5) . ? F1 C37 1.322(7) . ? N1 C14 1.343(5) . ? N1 C18 1.354(6) . ? C1 N2 1.349(5) . ? C1 C2 1.373(6) . ? C1 H1 0.9500 . ? Cu2 N7 1.983(4) . ? Cu2 N8 1.994(3) . ? Cu2 N6 2.005(3) . ? Cu2 N5 2.019(4) . ? Cu2 O8 2.408(3) . ? S2 O6 1.421(3) . ? S2 O5 1.446(3) . ? S2 O4 1.450(3) . ? S2 C38 1.837(5) . ? F2 C37 1.313(7) . ? N2 C5 1.352(5) . ? C2 C3 1.375(6) . ? C2 H2 0.9500 . ? S3 O7 1.428(4) . ? S3 O9 1.428(4) . ? S3 O8 1.442(4) . ? S3 C39A 1.719(19) . ? S3 C39 1.93(3) . ? F3 C37 1.335(7) . ? N3 C6 1.477(5) . ? N3 C7 1.484(5) . ? N3 H2A 0.9300 . ? C3 C4 1.386(6) . ? C3 H3 0.9500 . ? S4 O10 1.431(3) . ? S4 O12 1.440(4) . ? S4 O11 1.440(3) . ? S4 C40 1.824(6) . ? F4 C38 1.327(5) . ? N4 C13 1.453(5) . ? N4 C12 1.483(6) . ? N4 H3A 0.9300 . ? C4 C5 1.384(6) . ? C4 H4 0.9500 . ? F5 C38 1.337(6) . ? N5 C23 1.349(5) . ? N5 C19 1.351(6) . ? C5 C6 1.514(6) . ? F6 C38 1.331(5) . ? N6 C24 1.465(5) . ? N6 C25 1.505(5) . ? N6 H6 0.9300 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? F7 C40 1.329(6) . ? N7 C31 1.464(6) . ? N7 C30 1.491(5) . ? N7 H7A 0.9300 . ? C7 C8 1.520(7) . ? C7 C12 1.522(6) . ? C7 H7 1.0000 . ? F8 C40 1.325(5) . ? N8 C32 1.346(6) . ? N8 C36 1.349(6) . ? C8 C9 1.524(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? F9 C40 1.348(6) . ? C9 C10 1.551(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? F10 C39 1.26(3) . ? C10 C11 1.511(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? F11 C39 1.28(4) . ? C11 C12 1.528(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? F12 C39 1.36(4) . ? C12 H12 1.0000 . ? C13 C14 1.509(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.389(6) . ? C15 C16 1.369(7) . ? C15 H15 0.9500 . ? C16 C17 1.390(7) . ? C16 H16 0.9500 . ? C17 C18 1.377(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.365(7) . ? C19 H19 0.9500 . ? C20 C21 1.373(7) . ? C20 H20 0.9500 . ? C21 C22 1.396(7) . ? C21 H21 0.9500 . ? C22 C23 1.380(6) . ? C22 H22 0.9500 . ? C23 C24 1.506(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.519(5) . ? C25 C30 1.524(6) . ? C25 H25 1.0000 . ? C26 C27 1.540(7) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.500(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.540(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.529(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30 1.0000 . ? C31 C32 1.487(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.395(6) . ? C33 C34 1.387(7) . ? C33 H33 0.9500 . ? C34 C35 1.385(7) . ? C34 H34 0.9500 . ? C35 C36 1.372(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? F10A C39A 1.39(4) . ? F11A C39A 1.41(3) . ? F12A C39A 1.21(4) . ? 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_3 _geom_angle_publ_flag N4 Cu1 N2 162.91(14) . . ? N4 Cu1 N3 85.02(14) . . ? N2 Cu1 N3 82.20(14) . . ? N4 Cu1 N1 83.25(14) . . ? N2 Cu1 N1 110.59(14) . . ? N3 Cu1 N1 166.48(13) . . ? O3 S1 O1 115.7(2) . . ? O3 S1 O2 115.0(2) . . ? O1 S1 O2 113.62(19) . . ? O3 S1 C37 103.6(3) . . ? O1 S1 C37 104.0(2) . . ? O2 S1 C37 102.9(2) . . ? C14 N1 C18 117.9(4) . . ? C14 N1 Cu1 112.2(3) . . ? C18 N1 Cu1 129.7(3) . . ? N2 C1 C2 122.4(4) . . ? N2 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? N7 Cu2 N8 82.65(15) . . ? N7 Cu2 N6 84.34(14) . . ? N8 Cu2 N6 165.61(16) . . ? N7 Cu2 N5 159.09(14) . . ? N8 Cu2 N5 111.97(15) . . ? N6 Cu2 N5 82.21(14) . . ? N7 Cu2 O8 109.33(14) . . ? N8 Cu2 O8 91.68(14) . . ? N6 Cu2 O8 86.83(13) . . ? N5 Cu2 O8 85.87(13) . . ? O6 S2 O5 115.7(2) . . ? O6 S2 O4 115.1(2) . . ? O5 S2 O4 113.47(19) . . ? O6 S2 C38 103.9(2) . . ? O5 S2 C38 103.1(2) . . ? O4 S2 C38 103.4(2) . . ? C1 N2 C5 118.1(3) . . ? C1 N2 Cu1 129.4(3) . . ? C5 N2 Cu1 112.3(3) . . ? C1 C2 C3 119.5(4) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? O7 S3 O9 115.8(3) . . ? O7 S3 O8 114.5(2) . . ? O9 S3 O8 113.8(2) . . ? O7 S3 C39A 99.9(12) . . ? O9 S3 C39A 102.6(10) . . ? O8 S3 C39A 108.1(10) . . ? O7 S3 C39 108.3(10) . . ? O9 S3 C39 105.7(11) . . ? O8 S3 C39 96.2(9) . . ? C39A S3 C39 12.2(16) . . ? C6 N3 C7 116.2(3) . . ? C6 N3 Cu1 107.8(2) . . ? C7 N3 Cu1 108.9(3) . . ? C6 N3 H2A 107.9 . . ? C7 N3 H2A 107.9 . . ? Cu1 N3 H2A 107.9 . . ? C2 C3 C4 118.7(4) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? O10 S4 O12 115.3(2) . . ? O10 S4 O11 114.2(2) . . ? O12 S4 O11 114.7(2) . . ? O10 S4 C40 103.3(2) . . ? O12 S4 C40 103.9(2) . . ? O11 S4 C40 103.2(2) . . ? C13 N4 C12 116.6(3) . . ? C13 N4 Cu1 109.1(3) . . ? C12 N4 Cu1 107.7(2) . . ? C13 N4 H3A 107.7 . . ? C12 N4 H3A 107.7 . . ? Cu1 N4 H3A 107.7 . . ? C5 C4 C3 119.3(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C23 N5 C19 117.2(4) . . ? C23 N5 Cu2 112.0(3) . . ? C19 N5 Cu2 129.8(3) . . ? N2 C5 C4 121.8(4) . . ? N2 C5 C6 116.3(3) . . ? C4 C5 C6 121.9(4) . . ? C24 N6 C25 116.3(3) . . ? C24 N6 Cu2 107.9(2) . . ? C25 N6 Cu2 110.3(2) . . ? C24 N6 H6 107.3 . . ? C25 N6 H6 107.3 . . ? Cu2 N6 H6 107.3 . . ? N3 C6 C5 108.5(3) . . ? N3 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? N3 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? C31 N7 C30 116.3(4) . . ? C31 N7 Cu2 110.9(3) . . ? C30 N7 Cu2 108.4(3) . . ? C31 N7 H7A 106.9 . . ? C30 N7 H7A 106.9 . . ? Cu2 N7 H7A 106.9 . . ? N3 C7 C8 113.9(3) . . ? N3 C7 C12 107.1(3) . . ? C8 C7 C12 111.3(3) . . ? N3 C7 H7 108.1 . . ? C8 C7 H7 108.1 . . ? C12 C7 H7 108.1 . . ? S3 O8 Cu2 138.2(2) . . ? C32 N8 C36 118.1(4) . . ? C32 N8 Cu2 113.4(3) . . ? C36 N8 Cu2 128.5(3) . . ? C7 C8 C9 110.4(4) . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C10 111.2(4) . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 111.3(4) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 110.8(4) . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N4 C12 C7 105.9(3) . . ? N4 C12 C11 113.5(3) . . ? C7 C12 C11 111.8(3) . . ? N4 C12 H12 108.5 . . ? C7 C12 H12 108.5 . . ? C11 C12 H12 108.5 . . ? N4 C13 C14 110.6(3) . . ? N4 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N4 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N1 C14 C15 122.2(4) . . ? N1 C14 C13 116.6(4) . . ? C15 C14 C13 121.1(4) . . ? C16 C15 C14 119.1(4) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 119.5(4) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 118.3(4) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? N1 C18 C17 122.9(4) . . ? N1 C18 H18 118.6 . . ? C17 C18 H18 118.6 . . ? N5 C19 C20 123.7(4) . . ? N5 C19 H19 118.2 . . ? C20 C19 H19 118.2 . . ? C19 C20 C21 119.1(5) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C20 C21 C22 118.3(4) . . ? C20 C21 H21 120.9 . . ? C22 C21 H21 120.9 . . ? C23 C22 C21 119.4(4) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? N5 C23 C22 122.1(4) . . ? N5 C23 C24 115.6(4) . . ? C22 C23 C24 122.2(4) . . ? N6 C24 C23 106.7(3) . . ? N6 C24 H24A 110.4 . . ? C23 C24 H24A 110.4 . . ? N6 C24 H24B 110.4 . . ? C23 C24 H24B 110.4 . . ? H24A C24 H24B 108.6 . . ? N6 C25 C26 112.6(3) . . ? N6 C25 C30 106.3(3) . . ? C26 C25 C30 112.0(4) . . ? N6 C25 H25 108.6 . . ? C26 C25 H25 108.6 . . ? C30 C25 H25 108.6 . . ? C25 C26 C27 110.2(4) . . ? C25 C26 H26A 109.6 . . ? C27 C26 H26A 109.6 . . ? C25 C26 H26B 109.6 . . ? C27 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? C28 C27 C26 112.8(4) . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27B 109.0 . . ? C26 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C27 C28 C29 111.7(4) . . ? C27 C28 H28A 109.3 . . ? C29 C28 H28A 109.3 . . ? C27 C28 H28B 109.3 . . ? C29 C28 H28B 109.3 . . ? H28A C28 H28B 107.9 . . ? C30 C29 C28 108.3(4) . . ? C30 C29 H29A 110.0 . . ? C28 C29 H29A 110.0 . . ? C30 C29 H29B 110.0 . . ? C28 C29 H29B 110.0 . . ? H29A C29 H29B 108.4 . . ? N7 C30 C25 105.9(3) . . ? N7 C30 C29 115.3(4) . . ? C25 C30 C29 110.9(3) . . ? N7 C30 H30 108.2 . . ? C25 C30 H30 108.2 . . ? C29 C30 H30 108.2 . . ? N7 C31 C32 109.2(4) . . ? N7 C31 H31A 109.8 . . ? C32 C31 H31A 109.8 . . ? N7 C31 H31B 109.8 . . ? C32 C31 H31B 109.8 . . ? H31A C31 H31B 108.3 . . ? N8 C32 C33 121.5(4) . . ? N8 C32 C31 116.9(4) . . ? C33 C32 C31 121.6(4) . . ? C34 C33 C32 119.3(4) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 119.1(4) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C36 C35 C34 118.3(4) . . ? C36 C35 H35 120.8 . . ? C34 C35 H35 120.8 . . ? N8 C36 C35 123.6(5) . . ? N8 C36 H36 118.2 . . ? C35 C36 H36 118.2 . . ? F2 C37 F1 106.3(5) . . ? F2 C37 F3 107.6(5) . . ? F1 C37 F3 107.6(5) . . ? F2 C37 S1 112.5(4) . . ? F1 C37 S1 110.6(4) . . ? F3 C37 S1 111.8(4) . . ? F4 C38 F6 107.7(4) . . ? F4 C38 F5 107.1(4) . . ? F6 C38 F5 107.1(4) . . ? F4 C38 S2 112.2(4) . . ? F6 C38 S2 110.8(3) . . ? F5 C38 S2 111.8(3) . . ? F10 C39 F11 114(3) . . ? F10 C39 F12 106(2) . . ? F11 C39 F12 104(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.401 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.079 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 804597' #TrackingRef '- All.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration ad _chemical_formula_moiety ? _chemical_formula_sum 'C23 H28 Cu F6 N4 O7 S2' _chemical_formula_weight 714.15 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 Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.6290(3) _cell_length_b 11.7880(5) _cell_length_c 13.8240(5) _cell_angle_alpha 99.918(2) _cell_angle_beta 105.773(2) _cell_angle_gamma 96.2200(10) _cell_volume 1467.40(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 34028 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 730 _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8291 _exptl_absorpt_correction_T_max 0.8291 _exptl_absorpt_process_details ? _exptl_special_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29086 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _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_reflns_theta_min 3.56 _diffrn_reflns_theta_max 27.55 _reflns_number_total 12630 _reflns_number_gt 11009 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+0.5954P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(8) _refine_ls_number_reflns 12630 _refine_ls_number_parameters 805 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0830 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu -0.40569(3) 0.31174(3) 1.41573(2) 0.02341(11) Uani 1 1 d . . . S1 S -0.48532(12) -0.00272(9) 1.57956(7) 0.0276(2) Uani 1 1 d . . . F1 F -0.5439(3) -0.0590(3) 1.74087(17) 0.0374(6) Uani 1 1 d . . . O1 O -0.4591(4) 0.3134(3) 1.5618(2) 0.0370(8) Uani 1 1 d . . . N1 N -0.6078(4) 0.2264(3) 1.3282(2) 0.0261(8) Uani 1 1 d . . . C1 C -0.7330(5) 0.2669(4) 1.3022(3) 0.0324(10) Uani 1 1 d . . . H1 H -0.7339 0.3477 1.3235 0.039 Uiso 1 1 calc R . . Cu2 Cu 0.12233(3) 0.20598(3) 0.97822(2) 0.02315(11) Uani 1 1 d . . . S2 S -0.34056(11) 0.00116(10) 1.08488(7) 0.0298(2) Uani 1 1 d . . . F2 F -0.5561(3) -0.2053(2) 1.62082(18) 0.0382(6) Uani 1 1 d . . . O2 O 0.1821(4) 0.2019(3) 0.8338(2) 0.0305(7) Uani 1 1 d . . . N2 N -0.3804(4) 0.4891(3) 1.4376(2) 0.0221(7) Uani 1 1 d . . . C2 C -0.8629(5) 0.1940(5) 1.2445(3) 0.0362(11) Uani 1 1 d . . . H2 H -0.9504 0.2255 1.2238 0.043 Uiso 1 1 calc R . . S3 S 0.04980(12) 0.51351(10) 1.29496(8) 0.0309(2) Uani 1 1 d . . . F3 F -0.7283(3) -0.1005(3) 1.6044(2) 0.0449(7) Uani 1 1 d . . . O3 O -0.3336(4) -0.0016(3) 1.6324(2) 0.0374(8) Uani 1 1 d . . . N3 N -0.1974(4) 0.3489(3) 1.4863(2) 0.0230(7) Uani 1 1 d . . . C3 C -0.8639(5) 0.0777(5) 1.2180(3) 0.0358(11) Uani 1 1 d . . . H3 H -0.9532 0.0276 1.1797 0.043 Uiso 1 1 calc R . . S4 S 0.20533(12) 0.52114(9) 0.80609(7) 0.0273(2) Uani 1 1 d . . . F4 F -0.2601(4) -0.1682(3) 1.1760(2) 0.0604(9) Uani 1 1 d . . . O4 O -0.5333(4) -0.0590(3) 1.4726(2) 0.0416(8) Uani 1 1 d . . . N4 N -0.3565(4) 0.1564(3) 1.3796(2) 0.0260(7) Uani 1 1 d . . . C4 C -0.7350(5) 0.0301(4) 1.2464(3) 0.0278(9) Uani 1 1 d . . . F5 F -0.1656(4) -0.1483(3) 1.0548(2) 0.0536(8) Uani 1 1 d . . . O5 O -0.5352(4) 0.1076(3) 1.6033(2) 0.0419(8) Uani 1 1 d . . . N5 N 0.1012(4) 0.0311(3) 0.9524(2) 0.0250(8) Uani 1 1 d . . . C5 C -0.6079(5) 0.1101(4) 1.3006(3) 0.0255(9) Uani 1 1 d . . . F6 F -0.3911(4) -0.2255(3) 1.0183(3) 0.0682(10) Uani 1 1 d . . . O6 O -0.4653(4) -0.0082(3) 1.1233(2) 0.0402(8) Uani 1 1 d . . . N6 N -0.0910(4) 0.1676(3) 0.9244(2) 0.0247(7) Uani 1 1 d . . . C6 C -0.4620(5) 0.0750(4) 1.3316(3) 0.0245(9) Uani 1 1 d . . . H6 H -0.444(3) -0.002(3) 1.309(2) 0.008(7) Uiso 1 1 d . . . F7 F -0.1202(3) 0.6697(3) 1.3177(2) 0.0505(7) Uani 1 1 d . . . O7 O -0.2133(4) 0.0777(3) 1.1543(3) 0.0560(10) Uani 1 1 d . . . N7 N 0.0790(4) 0.3640(3) 0.9918(2) 0.0230(7) Uani 1 1 d . . . C7 C -0.7330(5) -0.0990(4) 1.2203(3) 0.0339(10) Uani 1 1 d . . . H7A H -0.7085 -0.1289 1.2837 0.051 Uiso 1 1 calc R . . H7B H -0.6595 -0.1129 1.1845 0.051 Uiso 1 1 calc R . . H7C H -0.8295 -0.1390 1.1758 0.051 Uiso 1 1 calc R . . F8 F 0.1084(4) 0.7415(3) 1.3594(2) 0.0571(9) Uani 1 1 d . . . O8 O -0.3758(4) 0.0114(4) 0.9799(2) 0.0544(10) Uani 1 1 d . . . N8 N 0.3209(4) 0.2941(3) 1.0709(2) 0.0256(8) Uani 1 1 d . . . C8 C -0.2003(3) 0.1496(3) 1.4087(2) 0.0248(6) Uani 1 1 d . . . H8 H -0.1618 0.1698 1.3525 0.030 Uiso 1 1 calc R . . F9 F -0.0142(3) 0.6841(2) 1.20037(19) 0.0461(7) Uani 1 1 d . . . O9 O 0.0729(4) 0.5043(4) 1.3999(3) 0.0564(10) Uani 1 1 d . . . C9 C -0.1578(5) 0.0328(4) 1.4267(3) 0.0307(10) Uani 1 1 d . . . H9A H -0.2036 -0.0283 1.3636 0.037 Uiso 1 1 calc R . . H9B H -0.1926 0.0104 1.4829 0.037 Uiso 1 1 calc R . . F10 F 0.2759(3) 0.7211(2) 0.75891(18) 0.0379(6) Uani 1 1 d . . . O10 O -0.0755(4) 0.4392(3) 1.2215(3) 0.0509(9) Uani 1 1 d . . . C10 C 0.0093(4) 0.0435(3) 1.4553(3) 0.0342(8) Uani 1 1 d . . . H10A H 0.0381 -0.0306 1.4721 0.041 Uiso 1 1 calc R . . H10B H 0.0418 0.0565 1.3955 0.041 Uiso 1 1 calc R . . F11 F 0.4463(3) 0.6155(3) 0.77719(19) 0.0429(7) Uani 1 1 d . . . O11 O 0.1797(4) 0.5187(3) 1.2621(2) 0.0417(8) Uani 1 1 d . . . C11 C 0.0856(4) 0.1439(4) 1.5472(3) 0.0390(9) Uani 1 1 d . . . H11A H 0.1927 0.1508 1.5598 0.047 Uiso 1 1 calc R . . H11B H 0.0633 0.1254 1.6091 0.047 Uiso 1 1 calc R . . F12 F 0.2609(3) 0.5703(2) 0.64113(17) 0.0361(6) Uani 1 1 d . . . O12 O 0.2533(4) 0.4098(3) 0.7837(2) 0.0357(7) Uani 1 1 d . . . C12 C 0.0390(5) 0.2611(4) 1.5310(3) 0.0316(10) Uani 1 1 d . . . H12A H 0.0707 0.2853 1.4742 0.038 Uiso 1 1 calc R . . H12B H 0.0846 0.3220 1.5943 0.038 Uiso 1 1 calc R . . O13 O 0.2566(4) 0.5808(3) 0.9121(2) 0.0418(9) Uani 1 1 d . . . C13 C -0.1392(5) 0.4566(4) 1.5147(3) 0.0237(8) Uani 1 1 d . . . H13 H -0.038(5) 0.486(4) 1.556(3) 0.033(11) Uiso 1 1 d . . . O14 O 0.0540(3) 0.5223(3) 0.7553(2) 0.0349(7) Uani 1 1 d . . . C14 C -0.1282(3) 0.2456(3) 1.5047(2) 0.0257(6) Uani 1 1 d . . . H14 H -0.1554 0.2199 1.5634 0.031 Uiso 1 1 calc R . . C15 C -0.2401(5) 0.5393(4) 1.4907(3) 0.0241(9) Uani 1 1 d . . . C16 C -0.1974(5) 0.6612(4) 1.5210(3) 0.0270(9) Uani 1 1 d . . . C17 C -0.3059(5) 0.7283(4) 1.4951(3) 0.0292(9) Uani 1 1 d . . . H17 H -0.2825 0.8109 1.5155 0.035 Uiso 1 1 calc R . . C18 C -0.4478(5) 0.6767(4) 1.4401(3) 0.0322(10) Uani 1 1 d . . . H18 H -0.5207 0.7237 1.4212 0.039 Uiso 1 1 calc R . . C19 C -0.4831(5) 0.5564(4) 1.4128(3) 0.0284(9) Uani 1 1 d . . . H19 H -0.5811 0.5210 1.3762 0.034 Uiso 1 1 calc R . . C20 C -0.0448(5) 0.7156(4) 1.5806(3) 0.0364(10) Uani 1 1 d . . . H20A H -0.0227 0.6993 1.6498 0.055 Uiso 1 1 calc R . . H20B H -0.0338 0.8002 1.5854 0.055 Uiso 1 1 calc R . . H20C H 0.0228 0.6833 1.5459 0.055 Uiso 1 1 calc R . . C21 C -0.5521(6) 0.3883(5) 1.5939(4) 0.0455(13) Uani 1 1 d . . . H21A H -0.4947 0.4655 1.6288 0.068 Uiso 1 1 calc R . . H21B H -0.5958 0.3552 1.6412 0.068 Uiso 1 1 calc R . . H21C H -0.6297 0.3958 1.5337 0.068 Uiso 1 1 calc R . . C22 C 0.2023(5) -0.0364(4) 0.9724(3) 0.0306(10) Uani 1 1 d . . . H22 H 0.2991 -0.0006 1.0118 0.037 Uiso 1 1 calc R . . C23 C 0.1739(5) -0.1574(4) 0.9384(3) 0.0295(9) Uani 1 1 d . . . H23 H 0.2492 -0.2029 0.9550 0.035 Uiso 1 1 calc R . . C24 C 0.0351(5) -0.2090(4) 0.8807(3) 0.0311(9) Uani 1 1 d . . . H24 H 0.0136 -0.2912 0.8559 0.037 Uiso 1 1 calc R . . C25 C -0.0770(5) -0.1399(4) 0.8578(3) 0.0265(9) Uani 1 1 d . . . C26 C -0.0378(5) -0.0213(4) 0.8959(3) 0.0230(9) Uani 1 1 d . . . C27 C -0.2324(6) -0.1955(5) 0.7950(4) 0.0393(11) Uani 1 1 d . . . H27A H -0.2970 -0.1877 0.8389 0.059 Uiso 1 1 calc R . . H27B H -0.2350 -0.2784 0.7678 0.059 Uiso 1 1 calc R . . H27C H -0.2657 -0.1563 0.7379 0.059 Uiso 1 1 calc R . . C28 C -0.1440(5) 0.0622(4) 0.8830(3) 0.0247(9) Uani 1 1 d . . . H28 H -0.240(5) 0.038(4) 0.852(3) 0.019(10) Uiso 1 1 d . . . C29 C -0.1699(3) 0.2673(3) 0.9357(2) 0.0253(6) Uani 1 1 d . . . H29 H -0.1819 0.2795 1.0061 0.030 Uiso 1 1 calc R . . C30 C -0.3197(5) 0.2566(4) 0.8603(3) 0.0331(10) Uani 1 1 d . . . H30A H -0.3849 0.1880 0.8648 0.040 Uiso 1 1 calc R . . H30B H -0.3125 0.2459 0.7893 0.040 Uiso 1 1 calc R . . C31 C -0.3822(4) 0.3686(3) 0.8866(3) 0.0376(8) Uani 1 1 d . . . H31A H -0.4782 0.3643 0.8354 0.045 Uiso 1 1 calc R . . H31B H -0.3979 0.3743 0.9550 0.045 Uiso 1 1 calc R . . C32 C -0.2805(4) 0.4775(3) 0.8874(3) 0.0394(8) Uani 1 1 d . . . H32A H -0.3223 0.5475 0.9082 0.047 Uiso 1 1 calc R . . H32B H -0.2734 0.4759 0.8171 0.047 Uiso 1 1 calc R . . C33 C -0.1265(5) 0.4859(4) 0.9617(3) 0.0327(10) Uani 1 1 d . . . H33A H -0.0610 0.5543 0.9571 0.039 Uiso 1 1 calc R . . H33B H -0.1308 0.4955 1.0333 0.039 Uiso 1 1 calc R . . C34 C -0.0684(3) 0.3742(3) 0.9317(2) 0.0250(6) Uani 1 1 d . . . H34 H -0.0681 0.3674 0.8586 0.030 Uiso 1 1 calc R . . C35 C 0.1803(5) 0.4471(4) 1.0495(3) 0.0244(9) Uani 1 1 d . . . H35 H 0.175(4) 0.532(3) 1.056(2) 0.021(9) Uiso 1 1 d . . . C36 C 0.3221(5) 0.4117(4) 1.0922(3) 0.0245(9) Uani 1 1 d . . . C37 C 0.4490(5) 0.4915(4) 1.1464(3) 0.0286(10) Uani 1 1 d . . . C38 C 0.5778(5) 0.4471(4) 1.1789(3) 0.0323(10) Uani 1 1 d . . . H38 H 0.6663 0.4988 1.2161 0.039 Uiso 1 1 calc R . . C39 C 0.5781(5) 0.3272(4) 1.1573(3) 0.0329(10) Uani 1 1 d . . . H39 H 0.6663 0.2967 1.1784 0.039 Uiso 1 1 calc R . . C40 C 0.4471(5) 0.2529(4) 1.1041(3) 0.0300(9) Uani 1 1 d . . . H40 H 0.4463 0.1710 1.0908 0.036 Uiso 1 1 calc R . . C41 C 0.4451(6) 0.6210(4) 1.1662(3) 0.0356(11) Uani 1 1 d . . . H41A H 0.4133 0.6454 1.1005 0.053 Uiso 1 1 calc R . . H41B H 0.5430 0.6635 1.2054 0.053 Uiso 1 1 calc R . . H41C H 0.3765 0.6380 1.2056 0.053 Uiso 1 1 calc R . . C42 C 0.2805(5) 0.1302(4) 0.8069(3) 0.0326(10) Uani 1 1 d . . . H42A H 0.3683 0.1405 0.8657 0.049 Uiso 1 1 calc R . . H42B H 0.3079 0.1521 0.7485 0.049 Uiso 1 1 calc R . . H42C H 0.2332 0.0483 0.7878 0.049 Uiso 1 1 calc R . . C43 C -0.5839(5) -0.0969(4) 1.6391(3) 0.0300(9) Uani 1 1 d . . . C44 C -0.2877(6) -0.1420(5) 1.0839(3) 0.0388(11) Uani 1 1 d . . . C45 C 0.0039(5) 0.6604(4) 1.2938(3) 0.0364(11) Uani 1 1 d . . . C46 C 0.3026(5) 0.6115(4) 0.7423(3) 0.0258(9) Uani 1 1 d . . . H1A H -0.482(4) 0.228(3) 1.577(3) 0.035(11) Uiso 1 1 d . . . H2A H 0.192(5) 0.254(4) 0.824(3) 0.023(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0183(3) 0.0214(3) 0.0291(2) 0.00365(19) 0.00520(18) 0.0041(2) S1 0.0332(6) 0.0221(6) 0.0328(5) 0.0100(4) 0.0149(4) 0.0067(4) F1 0.0479(17) 0.0402(16) 0.0305(11) 0.0089(11) 0.0197(11) 0.0111(13) O1 0.046(2) 0.0326(19) 0.0424(15) 0.0103(14) 0.0265(14) 0.0115(16) N1 0.0230(19) 0.0230(19) 0.0313(16) 0.0045(14) 0.0072(13) 0.0035(15) C1 0.023(2) 0.037(2) 0.0350(19) 0.0086(17) 0.0056(16) 0.0040(18) Cu2 0.0181(3) 0.0210(3) 0.0299(2) 0.00505(19) 0.00655(18) 0.0038(2) S2 0.0214(5) 0.0354(6) 0.0335(5) 0.0086(4) 0.0084(4) 0.0058(4) F2 0.0550(17) 0.0223(14) 0.0468(13) 0.0131(10) 0.0266(12) 0.0086(12) O2 0.0405(19) 0.0199(17) 0.0395(15) 0.0095(13) 0.0211(13) 0.0107(14) N2 0.0219(18) 0.0226(19) 0.0214(14) 0.0048(13) 0.0052(13) 0.0055(15) C2 0.026(2) 0.050(3) 0.034(2) 0.011(2) 0.0086(17) 0.012(2) S3 0.0250(6) 0.0350(6) 0.0380(5) 0.0148(4) 0.0119(4) 0.0089(5) F3 0.0263(15) 0.0509(19) 0.0582(15) 0.0192(13) 0.0103(11) 0.0027(13) O3 0.0286(18) 0.041(2) 0.0477(16) 0.0137(15) 0.0162(14) 0.0081(15) N3 0.0232(16) 0.0214(16) 0.0245(13) 0.0049(12) 0.0062(11) 0.0059(12) C3 0.020(2) 0.053(3) 0.0290(19) 0.005(2) 0.0049(16) -0.006(2) S4 0.0318(6) 0.0230(6) 0.0299(4) 0.0084(4) 0.0114(4) 0.0059(4) F4 0.078(2) 0.068(2) 0.0592(15) 0.0376(15) 0.0337(15) 0.0393(17) O4 0.056(2) 0.041(2) 0.0293(14) 0.0104(13) 0.0133(14) 0.0036(17) N4 0.0241(16) 0.0267(17) 0.0266(14) 0.0030(12) 0.0076(12) 0.0055(13) C4 0.031(2) 0.027(2) 0.0245(18) 0.0040(16) 0.0092(16) -0.0003(19) F5 0.0529(18) 0.0554(19) 0.0664(16) 0.0107(14) 0.0358(14) 0.0248(14) O5 0.050(2) 0.0280(19) 0.0624(19) 0.0187(15) 0.0307(17) 0.0179(16) N5 0.0218(19) 0.028(2) 0.0275(16) 0.0082(14) 0.0097(14) 0.0059(16) C5 0.021(2) 0.034(3) 0.0217(17) 0.0067(17) 0.0070(15) 0.0008(18) F6 0.069(2) 0.045(2) 0.076(2) -0.0100(16) 0.0211(18) -0.0135(18) O6 0.0265(17) 0.058(2) 0.0450(16) 0.0180(15) 0.0177(13) 0.0166(16) N6 0.0190(15) 0.0241(17) 0.0336(15) 0.0061(13) 0.0113(12) 0.0061(12) C6 0.025(2) 0.025(2) 0.0231(16) 0.0055(15) 0.0070(15) 0.0032(17) F7 0.0475(17) 0.0466(17) 0.0695(17) 0.0151(13) 0.0306(13) 0.0203(13) O7 0.0307(19) 0.039(2) 0.078(2) -0.0064(17) -0.0029(16) 0.0012(16) N7 0.0188(15) 0.0225(16) 0.0272(14) 0.0048(12) 0.0060(11) 0.0042(12) C7 0.031(3) 0.030(2) 0.035(2) 0.0069(18) 0.0049(18) -0.006(2) F8 0.064(2) 0.0384(18) 0.0573(16) -0.0026(13) 0.0147(15) -0.0107(16) O8 0.060(2) 0.076(3) 0.0422(16) 0.0326(17) 0.0224(15) 0.0244(19) N8 0.0208(18) 0.032(2) 0.0241(14) 0.0076(14) 0.0060(13) 0.0055(15) C8 0.0202(14) 0.0265(15) 0.0278(15) 0.0034(13) 0.0077(12) 0.0059(11) F9 0.0603(18) 0.0384(15) 0.0472(12) 0.0213(11) 0.0190(12) 0.0133(12) O9 0.066(2) 0.074(3) 0.0508(17) 0.0369(17) 0.0307(17) 0.030(2) C9 0.032(3) 0.024(3) 0.038(2) 0.0067(18) 0.0103(19) 0.011(2) F10 0.0478(16) 0.0249(14) 0.0496(13) 0.0123(11) 0.0253(12) 0.0077(12) O10 0.0309(19) 0.035(2) 0.080(2) 0.0035(16) 0.0113(16) 0.0028(15) C10 0.0351(18) 0.0317(18) 0.0397(19) 0.0092(16) 0.0121(15) 0.0171(14) F11 0.0256(14) 0.0477(18) 0.0555(14) 0.0150(13) 0.0104(11) 0.0032(13) O11 0.0280(18) 0.061(2) 0.0442(16) 0.0187(15) 0.0158(13) 0.0150(16) C11 0.0268(18) 0.039(2) 0.045(2) 0.0051(18) 0.0006(16) 0.0147(15) F12 0.0420(15) 0.0391(16) 0.0315(11) 0.0114(11) 0.0148(10) 0.0078(12) O12 0.042(2) 0.0223(17) 0.0464(16) 0.0096(13) 0.0164(14) 0.0082(15) C12 0.019(2) 0.031(3) 0.043(2) 0.0073(19) 0.0052(17) 0.008(2) O13 0.065(2) 0.0340(19) 0.0270(14) 0.0092(13) 0.0127(14) 0.0066(17) C13 0.021(2) 0.023(2) 0.0257(17) 0.0038(16) 0.0065(15) 0.0044(18) O14 0.0272(17) 0.0341(19) 0.0459(16) 0.0096(14) 0.0147(13) 0.0034(14) C14 0.0238(15) 0.0242(15) 0.0296(16) 0.0051(13) 0.0076(12) 0.0078(11) C15 0.024(2) 0.026(2) 0.0229(17) 0.0033(16) 0.0086(15) 0.0035(18) C16 0.030(2) 0.024(2) 0.0286(17) 0.0060(15) 0.0122(15) 0.0032(16) C17 0.036(2) 0.0210(19) 0.0319(18) 0.0039(15) 0.0142(16) 0.0033(16) C18 0.039(2) 0.029(2) 0.0323(19) 0.0094(17) 0.0116(17) 0.0155(19) C19 0.025(2) 0.028(3) 0.0332(19) 0.0098(18) 0.0075(17) 0.0084(19) C20 0.034(2) 0.023(2) 0.044(2) 0.0016(17) 0.0017(17) -0.0020(18) C21 0.061(3) 0.042(3) 0.048(2) 0.010(2) 0.035(2) 0.019(3) C22 0.030(2) 0.035(3) 0.0279(18) 0.0073(18) 0.0069(16) 0.011(2) C23 0.032(2) 0.029(2) 0.0315(19) 0.0096(17) 0.0096(17) 0.0158(18) C24 0.041(2) 0.024(2) 0.0309(17) 0.0060(15) 0.0121(17) 0.0137(17) C25 0.030(2) 0.025(2) 0.0256(16) 0.0064(15) 0.0092(15) 0.0047(16) C26 0.024(2) 0.023(2) 0.0260(17) 0.0101(16) 0.0100(15) 0.0054(17) C27 0.040(3) 0.025(2) 0.046(2) 0.0037(18) 0.0053(19) -0.0001(19) C28 0.020(2) 0.028(2) 0.0267(18) 0.0056(17) 0.0095(16) 0.0012(18) C29 0.0192(14) 0.0240(15) 0.0339(16) 0.0052(13) 0.0086(12) 0.0080(11) C30 0.023(2) 0.031(3) 0.040(2) 0.006(2) 0.0005(18) 0.004(2) C31 0.0266(17) 0.038(2) 0.047(2) 0.0100(18) 0.0066(16) 0.0122(14) C32 0.0350(19) 0.0316(18) 0.049(2) 0.0089(17) 0.0042(17) 0.0152(14) C33 0.027(2) 0.023(3) 0.043(2) 0.0026(19) 0.0052(19) 0.007(2) C34 0.0230(14) 0.0244(15) 0.0280(15) 0.0046(13) 0.0080(12) 0.0061(11) C35 0.025(2) 0.024(2) 0.0264(17) 0.0065(16) 0.0113(15) 0.0024(17) C36 0.025(2) 0.023(2) 0.0254(18) 0.0045(16) 0.0088(16) 0.0028(18) C37 0.021(2) 0.041(3) 0.0244(18) 0.0076(18) 0.0095(16) -0.0019(19) C38 0.027(2) 0.038(3) 0.0301(19) 0.0066(18) 0.0078(17) -0.001(2) C39 0.019(2) 0.043(3) 0.0336(19) 0.0086(18) 0.0035(16) 0.0021(19) C40 0.025(2) 0.034(2) 0.0327(18) 0.0049(16) 0.0106(15) 0.0084(17) C41 0.036(3) 0.029(3) 0.033(2) 0.0021(18) 0.0039(18) -0.008(2) C42 0.030(2) 0.036(3) 0.038(2) 0.0081(18) 0.0160(17) 0.0124(19) C43 0.029(2) 0.032(3) 0.0309(19) 0.0087(17) 0.0093(16) 0.0094(19) C44 0.041(3) 0.040(3) 0.039(2) 0.009(2) 0.0179(19) 0.006(2) C45 0.034(3) 0.032(3) 0.045(2) 0.0079(19) 0.0145(19) 0.003(2) C46 0.025(2) 0.022(2) 0.0326(18) 0.0066(16) 0.0101(16) 0.0038(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.941(3) . ? Cu1 N4 1.957(4) . ? Cu1 N1 2.035(4) . ? Cu1 N2 2.038(4) . ? Cu1 O1 2.213(3) . ? S1 O4 1.437(3) . ? S1 O3 1.442(4) . ? S1 O5 1.450(3) . ? S1 C43 1.822(4) . ? F1 C43 1.334(4) . ? O1 C21 1.425(6) . ? O1 H1A 1.07(4) . ? N1 C1 1.326(6) . ? N1 C5 1.359(6) . ? C1 C2 1.388(7) . ? C1 H1 0.9500 . ? Cu2 N7 1.942(3) . ? Cu2 N6 1.957(3) . ? Cu2 N5 2.009(4) . ? Cu2 N8 2.039(4) . ? Cu2 O2 2.218(3) . ? S2 O8 1.428(3) . ? S2 O7 1.435(4) . ? S2 O6 1.441(3) . ? S2 C44 1.814(6) . ? F2 C43 1.330(5) . ? O2 C42 1.417(5) . ? O2 H2A 0.65(4) . ? N2 C19 1.343(6) . ? N2 C15 1.361(5) . ? C2 C3 1.356(7) . ? C2 H2 0.9500 . ? S3 O9 1.431(3) . ? S3 O10 1.432(4) . ? S3 O11 1.441(3) . ? S3 C45 1.834(5) . ? F3 C43 1.335(5) . ? N3 C13 1.278(5) . ? N3 C14 1.477(4) . ? C3 C4 1.404(7) . ? C3 H3 0.9500 . ? S4 O13 1.437(3) . ? S4 O14 1.438(3) . ? S4 O12 1.450(3) . ? S4 C46 1.829(4) . ? F4 C44 1.325(5) . ? N4 C6 1.263(5) . ? N4 C8 1.463(4) . ? C4 C5 1.399(6) . ? C4 C7 1.505(7) . ? F5 C44 1.348(6) . ? N5 C22 1.325(6) . ? N5 C26 1.367(5) . ? C5 C6 1.479(6) . ? F6 C44 1.331(6) . ? N6 C28 1.261(5) . ? N6 C29 1.476(4) . ? C6 H6 0.96(3) . ? F7 C45 1.334(6) . ? N7 C35 1.283(5) . ? N7 C34 1.467(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? F8 C45 1.321(5) . ? N8 C40 1.351(6) . ? N8 C36 1.365(6) . ? C8 C9 1.519(5) . ? C8 C14 1.528(4) . ? C8 H8 1.0000 . ? F9 C45 1.338(5) . ? C9 C10 1.534(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? F10 C46 1.338(5) . ? C10 C11 1.530(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? F11 C46 1.329(5) . ? C11 C12 1.532(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? F12 C46 1.332(4) . ? C12 C14 1.534(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C15 1.465(6) . ? C13 H13 0.97(5) . ? C14 H14 1.0000 . ? C15 C16 1.407(6) . ? C16 C17 1.385(7) . ? C16 C20 1.485(6) . ? C17 C18 1.382(6) . ? C17 H17 0.9500 . ? C18 C19 1.382(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.394(6) . ? C22 H22 0.9500 . ? C23 C24 1.367(6) . ? C23 H23 0.9500 . ? C24 C25 1.423(6) . ? C24 H24 0.9500 . ? C25 C26 1.378(6) . ? C25 C27 1.520(6) . ? C26 C28 1.492(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28 0.90(4) . ? C29 C30 1.510(5) . ? C29 C34 1.528(4) . ? C29 H29 1.0000 . ? C30 C31 1.537(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.524(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.539(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.522(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34 1.0000 . ? C35 C36 1.470(6) . ? C35 H35 1.00(4) . ? C36 C37 1.397(6) . ? C37 C38 1.390(7) . ? C37 C41 1.509(7) . ? C38 C39 1.394(7) . ? C38 H38 0.9500 . ? C39 C40 1.390(6) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? 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_3 _geom_angle_publ_flag N3 Cu1 N4 82.01(15) . . ? N3 Cu1 N1 163.11(15) . . ? N4 Cu1 N1 81.15(15) . . ? N3 Cu1 N2 80.83(14) . . ? N4 Cu1 N2 156.39(13) . . ? N1 Cu1 N2 114.90(14) . . ? N3 Cu1 O1 92.05(13) . . ? N4 Cu1 O1 104.48(13) . . ? N1 Cu1 O1 93.34(13) . . ? N2 Cu1 O1 92.25(12) . . ? O4 S1 O3 115.5(2) . . ? O4 S1 O5 115.0(2) . . ? O3 S1 O5 113.9(2) . . ? O4 S1 C43 104.0(2) . . ? O3 S1 C43 103.7(2) . . ? O5 S1 C43 102.5(2) . . ? C21 O1 Cu1 122.0(3) . . ? C21 O1 H1A 111(2) . . ? Cu1 O1 H1A 114(2) . . ? C1 N1 C5 119.0(4) . . ? C1 N1 Cu1 129.7(3) . . ? C5 N1 Cu1 111.2(3) . . ? N1 C1 C2 121.7(5) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? N7 Cu2 N6 81.79(14) . . ? N7 Cu2 N5 162.69(14) . . ? N6 Cu2 N5 81.00(15) . . ? N7 Cu2 N8 80.67(15) . . ? N6 Cu2 N8 157.71(14) . . ? N5 Cu2 N8 115.48(15) . . ? N7 Cu2 O2 95.84(12) . . ? N6 Cu2 O2 100.86(13) . . ? N5 Cu2 O2 89.30(12) . . ? N8 Cu2 O2 94.52(13) . . ? O8 S2 O7 116.3(3) . . ? O8 S2 O6 113.7(2) . . ? O7 S2 O6 114.5(2) . . ? O8 S2 C44 104.5(2) . . ? O7 S2 C44 103.0(3) . . ? O6 S2 C44 102.6(2) . . ? C42 O2 Cu2 122.0(3) . . ? C42 O2 H2A 113(4) . . ? Cu2 O2 H2A 112(4) . . ? C19 N2 C15 120.0(4) . . ? C19 N2 Cu1 128.5(3) . . ? C15 N2 Cu1 111.4(3) . . ? C3 C2 C1 119.5(5) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? O9 S3 O10 116.1(2) . . ? O9 S3 O11 114.8(2) . . ? O10 S3 O11 113.9(2) . . ? O9 S3 C45 103.5(2) . . ? O10 S3 C45 103.4(2) . . ? O11 S3 C45 102.8(2) . . ? C13 N3 C14 128.4(3) . . ? C13 N3 Cu1 117.8(3) . . ? C14 N3 Cu1 113.7(2) . . ? C2 C3 C4 121.0(4) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? O13 S4 O14 115.0(2) . . ? O13 S4 O12 115.2(2) . . ? O14 S4 O12 114.8(2) . . ? O13 S4 C46 103.77(19) . . ? O14 S4 C46 103.28(19) . . ? O12 S4 C46 102.34(19) . . ? C6 N4 C8 127.7(4) . . ? C6 N4 Cu1 116.7(3) . . ? C8 N4 Cu1 115.5(2) . . ? C5 C4 C3 115.9(4) . . ? C5 C4 C7 121.8(4) . . ? C3 C4 C7 122.3(4) . . ? C22 N5 C26 117.9(4) . . ? C22 N5 Cu2 129.8(3) . . ? C26 N5 Cu2 111.9(3) . . ? N1 C5 C4 122.9(4) . . ? N1 C5 C6 114.4(4) . . ? C4 C5 C6 122.7(4) . . ? C28 N6 C29 128.0(4) . . ? C28 N6 Cu2 116.7(3) . . ? C29 N6 Cu2 115.3(2) . . ? N4 C6 C5 116.0(4) . . ? N4 C6 H6 120.3(18) . . ? C5 C6 H6 123.1(18) . . ? C35 N7 C34 127.2(3) . . ? C35 N7 Cu2 118.0(3) . . ? C34 N7 Cu2 114.8(2) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C40 N8 C36 118.8(4) . . ? C40 N8 Cu2 129.1(3) . . ? C36 N8 Cu2 111.9(3) . . ? N4 C8 C9 116.9(3) . . ? N4 C8 C14 106.4(2) . . ? C9 C8 C14 110.7(3) . . ? N4 C8 H8 107.5 . . ? C9 C8 H8 107.5 . . ? C14 C8 H8 107.5 . . ? C8 C9 C10 108.9(3) . . ? C8 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? C8 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C11 C10 C9 111.9(3) . . ? C11 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? C11 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C10 C11 C12 112.9(3) . . ? C10 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? C10 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C12 C14 107.9(3) . . ? C11 C12 H12A 110.1 . . ? C14 C12 H12A 110.1 . . ? C11 C12 H12B 110.1 . . ? C14 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? N3 C13 C15 115.2(4) . . ? N3 C13 H13 125(3) . . ? C15 C13 H13 119(3) . . ? N3 C14 C8 106.1(3) . . ? N3 C14 C12 117.1(3) . . ? C8 C14 C12 110.8(3) . . ? N3 C14 H14 107.5 . . ? C8 C14 H14 107.5 . . ? C12 C14 H14 107.5 . . ? N2 C15 C16 122.0(4) . . ? N2 C15 C13 114.7(4) . . ? C16 C15 C13 123.2(4) . . ? C17 C16 C15 116.7(4) . . ? C17 C16 C20 121.4(4) . . ? C15 C16 C20 121.9(4) . . ? C18 C17 C16 120.9(4) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 119.7(5) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? N2 C19 C18 120.7(4) . . ? N2 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N5 C22 C23 123.3(4) . . ? N5 C22 H22 118.4 . . ? C23 C22 H22 118.4 . . ? C24 C23 C22 118.5(4) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C23 C24 C25 120.1(4) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 116.8(4) . . ? C26 C25 C27 122.1(4) . . ? C24 C25 C27 121.0(4) . . ? N5 C26 C25 123.4(4) . . ? N5 C26 C28 113.3(4) . . ? C25 C26 C28 123.3(4) . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N6 C28 C26 115.4(4) . . ? N6 C28 H28 122(3) . . ? C26 C28 H28 122(3) . . ? N6 C29 C30 117.2(3) . . ? N6 C29 C34 106.3(2) . . ? C30 C29 C34 110.8(3) . . ? N6 C29 H29 107.3 . . ? C30 C29 H29 107.3 . . ? C34 C29 H29 107.3 . . ? C29 C30 C31 108.5(3) . . ? C29 C30 H30A 110.0 . . ? C31 C30 H30A 110.0 . . ? C29 C30 H30B 110.0 . . ? C31 C30 H30B 110.0 . . ? H30A C30 H30B 108.4 . . ? C32 C31 C30 111.9(3) . . ? C32 C31 H31A 109.2 . . ? C30 C31 H31A 109.2 . . ? C32 C31 H31B 109.2 . . ? C30 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C31 C32 C33 111.8(3) . . ? C31 C32 H32A 109.3 . . ? C33 C32 H32A 109.3 . . ? C31 C32 H32B 109.3 . . ? C33 C32 H32B 109.3 . . ? H32A C32 H32B 107.9 . . ? C34 C33 C32 108.1(3) . . ? C34 C33 H33A 110.1 . . ? C32 C33 H33A 110.1 . . ? C34 C33 H33B 110.1 . . ? C32 C33 H33B 110.1 . . ? H33A C33 H33B 108.4 . . ? N7 C34 C33 117.5(3) . . ? N7 C34 C29 106.3(3) . . ? C33 C34 C29 110.9(3) . . ? N7 C34 H34 107.2 . . ? C33 C34 H34 107.2 . . ? C29 C34 H34 107.2 . . ? N7 C35 C36 115.0(4) . . ? N7 C35 H35 125(2) . . ? C36 C35 H35 119(2) . . ? N8 C36 C37 122.7(4) . . ? N8 C36 C35 114.3(4) . . ? C37 C36 C35 123.0(4) . . ? C38 C37 C36 117.4(5) . . ? C38 C37 C41 122.0(4) . . ? C36 C37 C41 120.6(4) . . ? C37 C38 C39 120.5(4) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C40 C39 C38 118.8(5) . . ? C40 C39 H39 120.6 . . ? C38 C39 H39 120.6 . . ? N8 C40 C39 121.8(4) . . ? N8 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? C37 C41 H41A 109.5 . . ? C37 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C37 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O2 C42 H42A 109.5 . . ? O2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? F2 C43 F1 107.4(3) . . ? F2 C43 F3 108.3(4) . . ? F1 C43 F3 107.3(3) . . ? F2 C43 S1 110.9(3) . . ? F1 C43 S1 111.0(3) . . ? F3 C43 S1 111.8(3) . . ? F4 C44 F6 107.9(4) . . ? F4 C44 F5 106.9(4) . . ? F6 C44 F5 106.6(4) . . ? F4 C44 S2 112.0(3) . . ? F6 C44 S2 111.8(4) . . ? F5 C44 S2 111.4(3) . . ? F8 C45 F7 108.3(4) . . ? F8 C45 F9 107.4(4) . . ? F7 C45 F9 107.7(4) . . ? F8 C45 S3 111.8(4) . . ? F7 C45 S3 111.1(3) . . ? F9 C45 S3 110.4(3) . . ? F11 C46 F12 108.0(3) . . ? F11 C46 F10 107.7(3) . . ? F12 C46 F10 107.8(3) . . ? F11 C46 S4 111.4(3) . . ? F12 C46 S4 111.1(3) . . ? F10 C46 S4 110.7(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.302 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.060