Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email KELLERS@MISSOURI.EDU _publ_contact_author_name 'Dr Steven Keller' _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_address ; Department of Chemistry Univerisity of Missouri 125 Chemistry 601 South College Ave. Columbia MO 65211 UNITED STATES OF AMERICA ; _publ_section_title ; Supermolecular Coordination Isomers: Synthesis and Crystal Structures of Four New One-Dimensional Copper(I) Coordination Polymers with 1,3-Dithiane ; loop_ _publ_author_name 'Steven Keller' 'Jacqueline M. Knaust' data_c:\manusc~1\dithiane\jmk_ii~1\work\pcba _database_code_depnum_ccdc_archive 'CCDC 212583' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H14 B Cu F4 N2 S2' _chemical_formula_weight 352.68 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' B B 0.0013 0.0007 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.893(5) _cell_length_b 11.621(4) _cell_length_c 19.044(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2853.3(18) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.850 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16362 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.12 _reflns_number_total 3152 _reflns_number_gt 2583 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1000P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.0000(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3152 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 0.815 _refine_ls_restrained_S_all 0.815 _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 0.21197(2) 0.23077(2) 0.489722(16) 0.02950(13) Uani 1 1 d . . . S1 S 0.36994(4) 0.14247(5) 0.47746(3) 0.02712(16) Uani 1 1 d . . . S2 S 0.25188(4) -0.07939(4) 0.45791(3) 0.02407(15) Uani 1 1 d . . . F1 F 0.29671(12) 0.02435(15) 0.68859(9) 0.0528(4) Uani 1 1 d . . . F2 F 0.43955(13) 0.11275(16) 0.64637(9) 0.0546(4) Uani 1 1 d . . . F3 F 0.35808(13) 0.18558(15) 0.74139(9) 0.0521(4) Uani 1 1 d . . . F4 F 0.44738(15) 0.01914(16) 0.74974(10) 0.0706(6) Uani 1 1 d . . . N1 N 0.08858(16) 0.17541(17) 0.43624(11) 0.0360(5) Uani 1 1 d . . . N2 N 0.16832(17) 0.23498(17) 0.58988(12) 0.0359(5) Uani 1 1 d . . . C1 C 0.35577(17) -0.00749(19) 0.50263(12) 0.0259(4) Uani 1 1 d . . . H1A H 0.4215 -0.0484 0.4926 0.031 Uiso 1 1 calc R . . H1B H 0.3433 -0.0117 0.5539 0.031 Uiso 1 1 calc R . . C2 C 0.29827(19) -0.0649(2) 0.36817(12) 0.0310(5) Uani 1 1 d . . . H2A H 0.3664 -0.1036 0.3641 0.037 Uiso 1 1 calc R . . H2B H 0.2494 -0.1047 0.3363 0.037 Uiso 1 1 calc R . . C3 C 0.30949(19) 0.0599(2) 0.34473(12) 0.0340(5) Uani 1 1 d . . . H3A H 0.3252 0.0615 0.2939 0.041 Uiso 1 1 calc R . . H3B H 0.2426 0.0999 0.3519 0.041 Uiso 1 1 calc R . . C4 C 0.39383(19) 0.1244(2) 0.38386(12) 0.0335(5) Uani 1 1 d . . . H4A H 0.4019 0.2015 0.3623 0.040 Uiso 1 1 calc R . . H4B H 0.4602 0.0828 0.3777 0.040 Uiso 1 1 calc R . . C5 C 0.01482(19) 0.1425(2) 0.41026(12) 0.0323(5) Uani 1 1 d . . . C6 C -0.07939(19) 0.0996(2) 0.37728(15) 0.0431(6) Uani 1 1 d . . . H6A H -0.0612 0.0536 0.3359 0.065 Uiso 1 1 calc R . . H6B H -0.1229 0.1646 0.3629 0.065 Uiso 1 1 calc R . . H6C H -0.1176 0.0515 0.4108 0.065 Uiso 1 1 calc R . . C7 C 0.14592(19) 0.2401(2) 0.64741(13) 0.0320(5) Uani 1 1 d . . . C8 C 0.1170(2) 0.2464(2) 0.72119(14) 0.0404(6) Uani 1 1 d . . . H8A H 0.0780 0.3175 0.7297 0.061 Uiso 1 1 calc R . . H8B H 0.1797 0.2461 0.7502 0.061 Uiso 1 1 calc R . . H8C H 0.0738 0.1800 0.7333 0.061 Uiso 1 1 calc R . . B1 B 0.3848(2) 0.0854(2) 0.70657(15) 0.0350(6) 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 0.0324(2) 0.02272(19) 0.0333(2) -0.00100(11) 0.00033(11) 0.00305(11) S1 0.0260(3) 0.0187(3) 0.0366(3) -0.0008(2) -0.0033(2) -0.0005(2) S2 0.0249(3) 0.0207(3) 0.0265(3) -0.0008(2) -0.0009(2) -0.0018(2) F1 0.0440(9) 0.0529(10) 0.0616(11) 0.0019(9) -0.0081(8) -0.0147(8) F2 0.0535(10) 0.0616(10) 0.0485(10) -0.0071(8) 0.0172(8) -0.0066(8) F3 0.0531(10) 0.0492(10) 0.0540(10) -0.0145(8) 0.0115(8) 0.0011(8) F4 0.0776(13) 0.0526(11) 0.0816(14) 0.0150(9) -0.0398(11) 0.0032(9) N1 0.0292(10) 0.0332(11) 0.0457(12) -0.0052(9) -0.0014(9) 0.0045(8) N2 0.0381(12) 0.0324(11) 0.0373(13) 0.0042(9) -0.0002(10) 0.0021(9) C1 0.0292(11) 0.0188(10) 0.0298(11) 0.0007(8) -0.0047(8) 0.0015(9) C2 0.0373(12) 0.0331(12) 0.0227(11) -0.0051(9) 0.0006(9) 0.0006(9) C3 0.0398(12) 0.0384(13) 0.0238(12) 0.0057(10) 0.0032(9) 0.0056(11) C4 0.0342(12) 0.0279(11) 0.0385(13) 0.0068(10) 0.0106(10) 0.0007(10) C5 0.0315(12) 0.0293(11) 0.0363(12) -0.0033(9) 0.0040(10) 0.0043(10) C6 0.0306(12) 0.0509(15) 0.0478(15) -0.0112(12) -0.0001(11) -0.0049(11) C7 0.0306(12) 0.0294(11) 0.0360(14) 0.0072(10) -0.0002(10) 0.0009(9) C8 0.0416(15) 0.0495(15) 0.0302(13) 0.0068(11) 0.0028(11) 0.0024(11) B1 0.0342(14) 0.0376(15) 0.0333(14) 0.0032(11) -0.0024(11) 0.0011(11) _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 1.989(2) . ? Cu1 N1 1.995(2) . ? Cu1 S1 2.2925(9) . ? Cu1 S2 2.3349(10) 7_665 ? S1 C1 1.817(2) . ? S1 C4 1.821(2) . ? S2 C1 1.794(2) . ? S2 C2 1.818(2) . ? S2 Cu1 2.3349(10) 7_655 ? F1 B1 1.382(3) . ? F2 B1 1.384(3) . ? F3 B1 1.383(3) . ? F4 B1 1.386(3) . ? N1 C5 1.138(3) . ? N2 C7 1.135(3) . ? C2 C3 1.524(3) . ? C3 C4 1.517(3) . ? C5 C6 1.456(3) . ? C7 C8 1.456(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 N2 Cu1 N1 105.77(9) . . ? N2 Cu1 S1 111.10(7) . . ? N1 Cu1 S1 120.79(6) . . ? N2 Cu1 S2 106.38(6) . 7_665 ? N1 Cu1 S2 109.35(6) . 7_665 ? S1 Cu1 S2 102.66(3) . 7_665 ? C1 S1 C4 99.49(11) . . ? C1 S1 Cu1 108.25(7) . . ? C4 S1 Cu1 107.54(8) . . ? C1 S2 C2 99.06(11) . . ? C1 S2 Cu1 99.66(7) . 7_655 ? C2 S2 Cu1 105.40(8) . 7_655 ? C5 N1 Cu1 175.1(2) . . ? C7 N2 Cu1 177.7(2) . . ? S2 C1 S1 113.37(11) . . ? C3 C2 S2 113.23(16) . . ? C4 C3 C2 113.3(2) . . ? C3 C4 S1 114.62(16) . . ? N1 C5 C6 179.6(3) . . ? N2 C7 C8 179.9(3) . . ? F1 B1 F3 110.3(2) . . ? F1 B1 F2 109.4(2) . . ? F3 B1 F2 109.3(2) . . ? F1 B1 F4 109.9(2) . . ? F3 B1 F4 109.2(2) . . ? F2 B1 F4 108.8(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.404 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.062 data_d:\jackie\sulfur\196b\work\196b _database_code_depnum_ccdc_archive 'CCDC 212584' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cu2 C16 H28 N4 S4 B2 F8' _chemical_formula_weight 705.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 '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' B B 0.0013 0.0007 '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' 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' _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 6.671(2) _cell_length_b 16.939(8) _cell_length_c 12.941(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.88(3) _cell_angle_gamma 90.00 _cell_volume 1459.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4050 _cell_measurement_theta_min 2.8755 _cell_measurement_theta_max 23.251 _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 1.808 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.832046 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; Data were collected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 3663 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2917 _reflns_number_gt 2609 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart (Bruker 1998)' _computing_cell_refinement 'Smart (Bruker 1998)' _computing_data_reduction 'Saint (Bruker 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0721P)^2^+0.1233P] 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 0.02(2) _refine_ls_number_reflns 2917 _refine_ls_number_parameters 329 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.60580(14) 0.87919(6) 0.77735(5) 0.0429(3) Uani 1 1 d . . . S1 S 0.8156(3) 0.88182(15) 0.92547(11) 0.0363(4) Uani 1 1 d . . . F1 F 0.7195(10) 1.0815(4) 0.9533(5) 0.100(2) Uani 1 1 d . . . N1 N 0.5093(11) 0.7723(5) 0.7325(4) 0.0445(17) Uani 1 1 d . . . C1 C 0.6459(10) 0.8911(6) 1.0272(4) 0.0339(16) Uani 1 1 d . . . H1A H 0.5493 0.8482 1.0221 0.041 Uiso 1 1 calc R . . H1B H 0.5725 0.9404 1.0190 0.041 Uiso 1 1 calc R . . B1 B 0.5954(13) 1.1287(6) 1.0071(5) 0.033(2) Uani 1 1 d . . . Cu2 Cu 0.55016(13) 0.89077(6) 1.27789(5) 0.0366(3) Uani 1 1 d . . . S2 S 0.7804(2) 0.88882(14) 1.15278(10) 0.0352(4) Uani 1 1 d . . . F2 F 0.5077(12) 1.1796(5) 0.9370(6) 0.119(3) Uani 1 1 d . . . N2 N 0.3822(11) 0.9528(5) 0.7972(5) 0.0457(18) Uani 1 1 d . . . C2 C 0.8766(14) 0.7895(5) 1.1488(5) 0.051(2) Uani 1 1 d . . . H2A H 0.9503 0.7782 1.2143 0.061 Uiso 1 1 calc R . . H2B H 0.7642 0.7532 1.1415 0.061 Uiso 1 1 calc R . . B2 B 0.8189(17) 0.6380(7) 0.4915(7) 0.052(3) Uani 1 1 d . . . S3 S 0.7610(3) 0.93592(11) 1.41596(12) 0.0318(4) Uani 1 1 d . . . F3 F 0.7017(10) 1.1680(4) 1.0822(4) 0.092(2) Uani 1 1 d . . . N3 N 0.4444(10) 0.7828(5) 1.3011(5) 0.0441(17) Uani 1 1 d . . . C3 C 1.0151(13) 0.7741(6) 1.0608(5) 0.052(2) Uani 1 1 d . . . H3A H 1.1272 0.8107 1.0672 0.063 Uiso 1 1 calc R . . H3B H 1.0688 0.7210 1.0676 0.063 Uiso 1 1 calc R . . S4 S 0.7933(3) 0.92786(12) 1.64716(12) 0.0345(5) Uani 1 1 d . . . F4 F 0.4527(10) 1.0802(4) 1.0454(5) 0.095(2) Uani 1 1 d . . . N4 N 0.3282(10) 0.9640(4) 1.2409(4) 0.0403(16) Uani 1 1 d . . . C4 C 0.9079(13) 0.7832(6) 0.9544(5) 0.048(2) Uani 1 1 d . . . H4A H 0.7954 0.7468 0.9487 0.058 Uiso 1 1 calc R . . H4B H 0.9996 0.7683 0.9027 0.058 Uiso 1 1 calc R . . F5 F 0.7240(9) 0.5673(4) 0.4889(6) 0.105(2) Uani 1 1 d . . . C5 C 0.6336(10) 0.9117(5) 1.5304(4) 0.0316(19) Uani 1 1 d . . . H5A H 0.5923 0.8568 1.5272 0.038 Uiso 1 1 calc R . . H5B H 0.5137 0.9439 1.5326 0.038 Uiso 1 1 calc R . . F6 F 0.8870(18) 0.6473(7) 0.4010(9) 0.204(6) Uani 1 1 d . . . C6 C 0.9810(11) 0.8524(5) 1.6247(5) 0.040(2) Uani 1 1 d . . . H6A H 1.0783 0.8502 1.6838 0.049 Uiso 1 1 calc R . . H6B H 0.9157 0.8013 1.6181 0.049 Uiso 1 1 calc R . . F7 F 0.6792(7) 0.6975(3) 0.5039(3) 0.0540(13) Uani 1 1 d . . . C7 C 1.0868(10) 0.8689(6) 1.5295(5) 0.045(2) Uani 1 1 d . . . H7A H 1.1994 0.8328 1.5273 0.054 Uiso 1 1 calc R . . H7B H 1.1410 0.9220 1.5343 0.054 Uiso 1 1 calc R . . F8 F 0.9501(17) 0.6409(7) 0.5650(9) 0.233(7) Uani 1 1 d . . . C8 C 0.9570(10) 0.8615(5) 1.4278(5) 0.0352(19) Uani 1 1 d . . . H8A H 0.8959 0.8095 1.4241 0.042 Uiso 1 1 calc R . . H8B H 1.0418 0.8665 1.3701 0.042 Uiso 1 1 calc R . . C9 C 0.4606(13) 0.7117(6) 0.7078(6) 0.044(2) Uani 1 1 d . . . C10 C 0.3878(13) 0.6332(5) 0.6738(6) 0.054(2) Uani 1 1 d . . . H10A H 0.3656 0.6014 0.7333 0.081 Uiso 1 1 calc R . . H10B H 0.4862 0.6083 0.6339 0.081 Uiso 1 1 calc R . . H10C H 0.2640 0.6388 0.6321 0.081 Uiso 1 1 calc R . . C11 C 0.2697(13) 1.0011(5) 0.8123(6) 0.043(2) Uani 1 1 d . . . C12 C 0.1292(14) 1.0642(6) 0.8323(7) 0.066(3) Uani 1 1 d . . . H12A H 0.1897 1.0994 0.8836 0.099 Uiso 1 1 calc R . . H12B H 0.0091 1.0420 0.8572 0.099 Uiso 1 1 calc R . . H12C H 0.0961 1.0928 0.7695 0.099 Uiso 1 1 calc R . . C13 C 0.4019(13) 0.7195(6) 1.3104(5) 0.041(2) Uani 1 1 d . . . C14 C 0.3491(13) 0.6360(5) 1.3171(6) 0.053(2) Uani 1 1 d . . . H14A H 0.3094 0.6164 1.2492 0.080 Uiso 1 1 calc R . . H14B H 0.2399 0.6300 1.3612 0.080 Uiso 1 1 calc R . . H14C H 0.4633 0.6068 1.3454 0.080 Uiso 1 1 calc R . . C15 C 0.2180(12) 1.0122(6) 1.2154(6) 0.047(2) Uani 1 1 d . . . C16 C 0.0803(16) 1.0750(7) 1.1831(9) 0.088(4) Uani 1 1 d . . . H16A H 0.1383 1.1067 1.1313 0.133 Uiso 1 1 calc R . . H16B H 0.0550 1.1074 1.2417 0.133 Uiso 1 1 calc R . . H16C H -0.0438 1.0527 1.1548 0.133 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0600(6) 0.0410(7) 0.0276(4) -0.0033(4) 0.0027(3) 0.0047(6) S1 0.0456(10) 0.0366(12) 0.0271(7) -0.0006(9) 0.0059(6) 0.0012(11) F1 0.097(5) 0.075(5) 0.135(5) -0.026(4) 0.052(4) 0.011(4) N1 0.061(5) 0.041(5) 0.032(3) -0.003(3) 0.009(3) 0.001(4) C1 0.042(4) 0.029(4) 0.029(3) -0.002(3) -0.003(3) -0.003(5) B1 0.033(5) 0.039(6) 0.026(4) 0.007(4) 0.002(3) -0.004(4) Cu2 0.0448(5) 0.0357(6) 0.0285(4) 0.0042(4) -0.0029(3) 0.0081(5) S2 0.0432(10) 0.0368(11) 0.0251(7) -0.0029(10) -0.0017(6) 0.0026(12) F2 0.097(6) 0.100(7) 0.154(6) 0.072(5) -0.041(5) -0.003(5) N2 0.049(5) 0.045(5) 0.043(3) -0.002(3) 0.002(3) 0.003(4) C2 0.071(6) 0.044(6) 0.037(4) -0.002(4) 0.000(4) 0.022(5) B2 0.064(8) 0.051(8) 0.040(5) -0.004(5) -0.005(5) -0.008(6) S3 0.0399(11) 0.0299(11) 0.0252(8) 0.0042(7) 0.0000(7) -0.0002(9) F3 0.106(5) 0.106(6) 0.065(3) -0.023(4) 0.011(3) -0.025(5) N3 0.043(4) 0.041(5) 0.047(3) 0.007(3) -0.007(3) 0.009(4) C3 0.050(5) 0.065(7) 0.041(4) -0.003(4) -0.002(3) 0.027(5) S4 0.0444(12) 0.0317(11) 0.0269(8) -0.0035(8) -0.0026(7) -0.0006(10) F4 0.089(5) 0.086(5) 0.116(5) 0.012(4) 0.053(4) -0.034(4) N4 0.041(4) 0.030(4) 0.051(3) 0.012(3) 0.003(3) 0.007(3) C4 0.055(6) 0.050(6) 0.041(4) -0.004(4) 0.011(3) 0.013(5) F5 0.068(4) 0.040(4) 0.208(7) -0.008(4) 0.012(4) -0.007(3) C5 0.031(4) 0.033(5) 0.031(3) 0.001(3) -0.002(3) 0.009(3) F6 0.250(12) 0.131(9) 0.259(11) 0.015(8) 0.218(10) 0.034(8) C6 0.040(5) 0.045(6) 0.034(4) 0.007(3) -0.011(3) 0.001(4) F7 0.059(3) 0.038(3) 0.066(3) -0.004(2) 0.008(2) 0.002(3) C7 0.032(4) 0.049(7) 0.053(4) -0.002(4) -0.002(3) -0.002(4) F8 0.210(10) 0.151(11) 0.309(13) -0.099(10) -0.212(11) 0.110(9) C8 0.031(4) 0.039(5) 0.036(3) 0.005(3) 0.008(3) 0.009(4) C9 0.047(6) 0.041(6) 0.045(4) -0.003(4) 0.006(4) 0.006(4) C10 0.045(5) 0.043(6) 0.075(5) -0.009(4) 0.018(4) -0.014(4) C11 0.042(5) 0.039(6) 0.047(4) -0.006(4) -0.011(4) -0.005(5) C12 0.050(6) 0.054(7) 0.093(7) 0.002(5) -0.001(5) 0.021(5) C13 0.042(5) 0.041(6) 0.039(4) -0.003(4) -0.009(3) -0.001(4) C14 0.042(5) 0.036(6) 0.080(6) 0.002(4) -0.009(4) -0.006(4) C15 0.034(5) 0.037(5) 0.070(5) 0.009(4) 0.006(4) -0.005(5) C16 0.055(7) 0.064(8) 0.147(10) 0.040(7) 0.012(6) 0.024(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 N2 1.974(8) . ? Cu1 N1 1.995(8) . ? Cu1 S1 2.2963(19) . ? Cu1 S4 2.317(2) 1_554 ? S1 C1 1.801(6) . ? S1 C4 1.811(9) . ? F1 B1 1.374(11) . ? N1 C9 1.117(11) . ? C1 S2 1.803(5) . ? B1 F3 1.341(10) . ? B1 F2 1.356(11) . ? B1 F4 1.375(10) . ? Cu2 N4 1.966(7) . ? Cu2 N3 1.991(8) . ? Cu2 S2 2.3059(19) . ? Cu2 S3 2.327(2) . ? S2 C2 1.802(9) . ? N2 C11 1.136(11) . ? C2 C3 1.537(10) . ? B2 F8 1.249(11) . ? B2 F6 1.295(12) . ? B2 F5 1.353(13) . ? B2 F7 1.389(12) . ? S3 C5 1.805(6) . ? S3 C8 1.815(7) . ? N3 C13 1.117(11) . ? C3 C4 1.515(10) . ? S4 C5 1.810(6) . ? S4 C6 1.826(8) . ? S4 Cu1 2.317(2) 1_556 ? N4 C15 1.133(10) . ? C6 C7 1.488(9) . ? C7 C8 1.531(9) . ? C9 C10 1.473(12) . ? C11 C12 1.457(13) . ? C13 C14 1.462(13) . ? C15 C16 1.449(13) . ? 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 N1 112.3(3) . . ? N2 Cu1 S1 107.62(19) . . ? N1 Cu1 S1 115.3(2) . . ? N2 Cu1 S4 108.6(2) . 1_554 ? N1 Cu1 S4 106.93(17) . 1_554 ? S1 Cu1 S4 105.75(8) . 1_554 ? C1 S1 C4 98.7(4) . . ? C1 S1 Cu1 103.5(2) . . ? C4 S1 Cu1 109.5(3) . . ? C9 N1 Cu1 178.1(8) . . ? S1 C1 S2 111.0(4) . . ? F3 B1 F2 110.6(9) . . ? F3 B1 F4 112.4(6) . . ? F2 B1 F4 110.1(8) . . ? F3 B1 F1 110.4(7) . . ? F2 B1 F1 106.2(7) . . ? F4 B1 F1 106.9(9) . . ? N4 Cu2 N3 110.4(3) . . ? N4 Cu2 S2 111.39(18) . . ? N3 Cu2 S2 110.6(2) . . ? N4 Cu2 S3 112.7(2) . . ? N3 Cu2 S3 112.83(18) . . ? S2 Cu2 S3 98.46(7) . . ? C1 S2 C2 98.7(4) . . ? C1 S2 Cu2 108.6(2) . . ? C2 S2 Cu2 106.8(3) . . ? C11 N2 Cu1 172.3(7) . . ? C3 C2 S2 114.4(6) . . ? F8 B2 F6 114.4(12) . . ? F8 B2 F5 110.9(10) . . ? F6 B2 F5 106.2(9) . . ? F8 B2 F7 108.9(9) . . ? F6 B2 F7 107.1(9) . . ? F5 B2 F7 109.2(8) . . ? C5 S3 C8 98.6(3) . . ? C5 S3 Cu2 105.2(2) . . ? C8 S3 Cu2 103.3(2) . . ? C13 N3 Cu2 173.1(7) . . ? C4 C3 C2 112.7(7) . . ? C5 S4 C6 97.6(3) . . ? C5 S4 Cu1 103.7(2) . 1_556 ? C6 S4 Cu1 106.0(2) . 1_556 ? C15 N4 Cu2 171.5(7) . . ? C3 C4 S1 114.5(6) . . ? S3 C5 S4 111.5(4) . . ? C7 C6 S4 111.7(6) . . ? C6 C7 C8 115.1(6) . . ? C7 C8 S3 112.2(5) . . ? N1 C9 C10 177.6(10) . . ? N2 C11 C12 178.7(9) . . ? N3 C13 C14 177.1(9) . . ? N4 C15 C16 178.8(10) . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 0.526 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.073 data_c:\manusc~1\dithiane\jmk_ii~2\work\jmk_ii_ _database_code_depnum_ccdc_archive 'CCDC 212585' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H19 B Cu F4 N S4' _chemical_formula_weight 431.85 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' B B 0.0013 0.0007 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.6496(8) _cell_length_b 14.8560(17) _cell_length_c 17.325(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1711.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.792 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10744 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.12 _reflns_number_total 3766 _reflns_number_gt 3270 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1000P)^2^+0.0000P] 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 0.033(17) _refine_ls_number_reflns 3766 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1161 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 0.848 _refine_ls_restrained_S_all 0.848 _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 0.78603(8) 0.98779(3) 0.57455(3) 0.02061(14) Uani 1 1 d . . . S1 S 0.74156(16) 0.83606(6) 0.58003(6) 0.0254(2) Uani 1 1 d . . . F1 F 0.0729(9) 0.8610(4) 0.8678(3) 0.114(2) Uani 1 1 d . . . N1 N 0.8039(6) 1.0118(3) 0.4595(2) 0.0310(8) Uani 1 1 d . . . C1 C 0.7898(7) 1.0089(3) 0.3946(3) 0.0295(9) Uani 1 1 d . . . B1 B 0.2043(10) 0.8409(4) 0.8112(3) 0.0368(12) Uani 1 1 d . . . S2 S 0.9320(2) 0.65447(8) 0.58407(8) 0.0426(3) Uani 1 1 d . . . F2 F 0.3950(7) 0.8434(4) 0.8360(4) 0.1048(18) Uani 1 1 d . . . C2 C 0.7746(9) 1.0038(3) 0.3102(3) 0.0392(11) Uani 1 1 d . . . H2A H 0.9008 1.0246 0.2870 0.059 Uiso 1 1 calc R . . H2B H 0.6637 1.0421 0.2926 0.059 Uiso 1 1 calc R . . H2C H 0.7491 0.9414 0.2947 0.059 Uiso 1 1 calc R . . S3 S 1.06075(15) 1.05942(7) 0.62665(6) 0.0195(2) Uani 1 1 d . . . F3 F 0.1835(9) 0.7520(3) 0.7908(3) 0.1031(18) Uani 1 1 d . . . C3 C 0.9759(7) 0.7745(3) 0.5856(3) 0.0311(10) Uani 1 1 d . . . H3A H 1.0627 0.7913 0.5415 0.037 Uiso 1 1 calc R . . H3B H 1.0472 0.7909 0.6338 0.037 Uiso 1 1 calc R . . S4 S 1.50840(14) 1.05991(6) 0.62469(6) 0.0200(2) Uani 1 1 d . . . F4 F 0.1869(8) 0.8972(3) 0.7496(2) 0.0919(16) Uani 1 1 d . . . C4 C 0.7852(9) 0.6444(3) 0.6723(3) 0.0411(12) Uani 1 1 d . . . H4A H 0.7499 0.5803 0.6800 0.049 Uiso 1 1 calc R . . H4B H 0.8702 0.6631 0.7164 0.049 Uiso 1 1 calc R . . C5 C 0.5963(9) 0.6987(3) 0.6734(3) 0.0425(14) Uani 1 1 d . . . H5A H 0.5183 0.6836 0.7203 0.051 Uiso 1 1 calc R . . H5B H 0.5135 0.6826 0.6279 0.051 Uiso 1 1 calc R . . C6 C 0.6373(7) 0.8009(3) 0.6722(3) 0.0324(11) Uani 1 1 d . . . H6A H 0.7328 0.8163 0.7140 0.039 Uiso 1 1 calc R . . H6B H 0.5103 0.8338 0.6819 0.039 Uiso 1 1 calc R . . C7 C 1.2829(6) 0.9995(2) 0.5957(2) 0.0198(7) Uani 1 1 d . . . H7A H 1.2810 0.9929 0.5388 0.024 Uiso 1 1 calc R . . H7B H 1.2837 0.9386 0.6188 0.024 Uiso 1 1 calc R . . C8 C 1.4743(6) 1.1609(3) 0.5664(3) 0.0238(9) Uani 1 1 d . . . H8A H 1.5907 1.2015 0.5741 0.029 Uiso 1 1 calc R . . H8B H 1.4703 1.1440 0.5112 0.029 Uiso 1 1 calc R . . C9 C 1.2813(6) 1.2110(2) 0.5871(2) 0.0233(8) Uani 1 1 d . . . H9A H 1.2820 1.2243 0.6431 0.028 Uiso 1 1 calc R . . H9B H 1.2790 1.2692 0.5592 0.028 Uiso 1 1 calc R . . C10 C 1.0919(6) 1.1592(3) 0.5677(3) 0.0246(9) Uani 1 1 d . . . H10A H 1.0962 1.1413 0.5127 0.029 Uiso 1 1 calc R . . H10B H 0.9740 1.1990 0.5750 0.029 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0153(2) 0.0202(2) 0.0263(2) 0.00138(19) -0.0001(2) 0.00011(18) S1 0.0272(5) 0.0196(5) 0.0293(5) 0.0014(4) -0.0037(5) -0.0006(4) F1 0.136(4) 0.114(4) 0.092(3) 0.051(3) 0.075(3) 0.061(3) N1 0.034(2) 0.035(2) 0.0248(19) 0.0042(15) 0.0017(16) 0.001(2) C1 0.030(2) 0.024(2) 0.035(2) 0.0013(17) 0.0021(19) -0.005(2) B1 0.032(3) 0.049(3) 0.029(2) 0.012(2) 0.006(2) 0.003(3) S2 0.0637(9) 0.0235(5) 0.0407(7) -0.0004(5) 0.0155(6) 0.0114(6) F2 0.064(3) 0.120(4) 0.130(4) 0.018(4) -0.037(3) -0.006(3) C2 0.051(3) 0.041(3) 0.025(2) 0.000(2) 0.001(2) 0.006(3) S3 0.0135(5) 0.0236(5) 0.0214(5) 0.0007(4) 0.0009(4) -0.0001(4) F3 0.149(5) 0.080(3) 0.080(3) -0.010(2) 0.018(3) -0.033(4) C3 0.032(2) 0.026(2) 0.035(2) 0.001(2) 0.008(2) 0.0079(18) S4 0.0125(5) 0.0232(5) 0.0242(5) 0.0018(4) -0.0007(4) 0.0005(4) F4 0.125(4) 0.098(3) 0.053(2) 0.041(2) 0.033(3) 0.051(3) C4 0.060(3) 0.024(2) 0.040(3) 0.008(2) 0.006(3) 0.007(2) C5 0.055(4) 0.029(3) 0.043(3) 0.009(2) 0.019(3) -0.008(2) C6 0.028(2) 0.028(2) 0.042(3) 0.007(2) 0.011(2) 0.0040(18) C7 0.0144(17) 0.0187(17) 0.0264(18) -0.0008(14) 0.0005(15) -0.0012(15) C8 0.021(2) 0.021(2) 0.029(2) 0.0053(19) 0.0021(18) -0.0032(16) C9 0.0193(19) 0.0180(18) 0.033(2) 0.0037(15) -0.0001(19) -0.0002(16) C10 0.017(2) 0.026(2) 0.031(2) 0.001(2) -0.0061(17) 0.0040(16) _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 N1 2.027(4) . ? Cu1 S1 2.2753(11) . ? Cu1 S3 2.2988(11) . ? Cu1 S4 2.3044(11) 1_455 ? S1 C3 1.810(5) . ? S1 C6 1.818(5) . ? F1 B1 1.346(7) . ? N1 C1 1.130(6) . ? C1 C2 1.467(6) . ? B1 F2 1.339(7) . ? B1 F4 1.361(6) . ? B1 F3 1.375(8) . ? S2 C3 1.807(4) . ? S2 C4 1.820(5) . ? S3 C7 1.806(4) . ? S3 C10 1.812(4) . ? S4 C7 1.818(4) . ? S4 C8 1.823(4) . ? S4 Cu1 2.3044(11) 1_655 ? C4 C5 1.493(7) . ? C5 C6 1.542(7) . ? C8 C9 1.526(6) . ? C9 C10 1.514(6) . ? 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 N1 Cu1 S1 102.86(11) . . ? N1 Cu1 S3 104.95(12) . . ? S1 Cu1 S3 123.06(4) . . ? N1 Cu1 S4 109.62(12) . 1_455 ? S1 Cu1 S4 109.92(4) . 1_455 ? S3 Cu1 S4 105.87(4) . 1_455 ? C3 S1 C6 97.8(2) . . ? C3 S1 Cu1 113.03(15) . . ? C6 S1 Cu1 111.76(16) . . ? C1 N1 Cu1 165.3(4) . . ? N1 C1 C2 178.9(5) . . ? F2 B1 F1 112.1(6) . . ? F2 B1 F4 108.3(6) . . ? F1 B1 F4 112.3(5) . . ? F2 B1 F3 101.8(6) . . ? F1 B1 F3 109.6(6) . . ? F4 B1 F3 112.3(5) . . ? C3 S2 C4 99.0(2) . . ? C7 S3 C10 98.16(19) . . ? C7 S3 Cu1 107.77(13) . . ? C10 S3 Cu1 104.36(14) . . ? S2 C3 S1 111.0(3) . . ? C7 S4 C8 98.64(18) . . ? C7 S4 Cu1 109.10(13) . 1_655 ? C8 S4 Cu1 105.88(14) . 1_655 ? C5 C4 S2 114.6(4) . . ? C4 C5 C6 112.5(4) . . ? C5 C6 S1 111.2(4) . . ? S3 C7 S4 110.46(19) . . ? C9 C8 S4 112.1(3) . . ? C10 C9 C8 113.5(3) . . ? C9 C10 S3 112.7(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.683 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.089 data_u:\keller~1\jackie\dithiane\as64j\work\as64j _database_code_depnum_ccdc_archive 'CCDC 212586' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cu3 C19 H35 N3 S6 Cl2 B3 F12' _chemical_formula_weight 1019.81 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' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.1164(17) _cell_length_b 16.379(2) _cell_length_c 19.486(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3867.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5343 _cell_measurement_theta_min 2.4325 _cell_measurement_theta_max 22.3645 _exptl_crystal_description columns _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 2.175 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.618386 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; Data were collected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker SMART CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24178 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0829 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.12 _reflns_number_total 8402 _reflns_number_gt 5814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart (Bruker 1998)' _computing_cell_refinement 'Smart (Bruker 1998)' _computing_data_reduction 'Saint (Bruker 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; The included dichloromethane solvent molecule is disordered over two positions. C1A, C1lA, Cl2A, and C1B, Cl1B, Cl2B were split into parts and refined to site occupancies of 0.68 and 0.32. All dichloromethane atoms were refined with isotropic thermal parameters. One of the BF4 anions (B3 and F9-F12) was refined with geometric restraints, and F10 and F11 were refined with isotropic thermal parameters. 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^)+(0.0856P)^2^+3.6477P] 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 -0.02(2) _refine_ls_number_reflns 8402 _refine_ls_number_parameters 424 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0974 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1621 _refine_ls_wR_factor_gt 0.1420 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.016 _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 0.30431(8) 0.01502(6) 0.74780(5) 0.0323(2) Uani 1 1 d . . . Cu2 Cu 0.43706(8) -0.17397(5) 0.81718(4) 0.0332(2) Uani 1 1 d . . . Cu3 Cu 0.55780(8) -0.29794(5) 0.67038(4) 0.0323(2) Uani 1 1 d . . . Cl1A Cl 0.3484(7) -0.4969(6) 1.0713(4) 0.157(3) Uiso 0.680(7) 1 d PD A 2 Cl2A Cl 0.5223(10) -0.3779(8) 1.0459(6) 0.202(5) Uiso 0.680(7) 1 d PD A 2 Cl1B Cl 0.5122(12) -0.4216(9) 1.0071(6) 0.107(4) Uiso 0.320(7) 1 d PD A 1 Cl2B Cl 0.5511(8) -0.3450(6) 1.1385(4) 0.074(3) Uiso 0.320(7) 1 d PD A 1 S1 S 0.39960(16) -0.03995(11) 0.83882(9) 0.0298(4) Uani 1 1 d . . . S2 S 0.51127(19) 0.10710(12) 0.90527(9) 0.0356(5) Uani 1 1 d . . . S3 S 0.41917(16) -0.20966(11) 0.70390(8) 0.0288(4) Uani 1 1 d . . . S4 S 0.31752(18) -0.05303(11) 0.64545(9) 0.0341(5) Uani 1 1 d . . . S5 S 0.59862(19) -0.21969(13) 0.86987(10) 0.0405(5) Uani 1 1 d . . . S6 S 0.65779(16) -0.34673(11) 0.76166(9) 0.0309(4) Uani 1 1 d . . . F1 F 0.3692(8) -0.0712(4) 1.1080(4) 0.116(3) Uani 1 1 d . . . F2 F 0.4863(7) -0.1726(6) 1.1218(4) 0.116(3) Uani 1 1 d . . . F3 F 0.3486(9) -0.1776(6) 1.0478(5) 0.142(4) Uani 1 1 d . . . F4 F 0.4905(5) -0.0988(4) 1.0234(3) 0.0736(18) Uani 1 1 d . . . F5 F 0.6075(9) 0.0926(4) 0.7327(3) 0.110(3) Uani 1 1 d . . . F6 F 0.6204(7) -0.0440(4) 0.7250(3) 0.080(2) Uani 1 1 d . . . F7 F 0.5817(7) 0.0320(4) 0.6326(3) 0.086(2) Uani 1 1 d . . . F8 F 0.7494(7) 0.0353(9) 0.6722(5) 0.168(5) Uani 1 1 d . . . F9 F 0.5888(5) -0.2130(6) 0.4390(4) 0.105(3) Uani 1 1 d D . . F10 F 0.4548(9) -0.2813(6) 0.3913(5) 0.163(4) Uiso 1 1 d D . . F11 F 0.4367(9) -0.1590(6) 0.3906(5) 0.158(4) Uiso 1 1 d D . . F12 F 0.4214(7) -0.2205(5) 0.4913(3) 0.119(3) Uani 1 1 d D . . N1 N 0.1455(6) 0.0162(5) 0.7730(3) 0.0434(17) Uani 1 1 d . . . N2 N 0.3343(6) -0.2431(4) 0.8703(4) 0.0436(18) Uani 1 1 d . . . N3 N 0.6584(6) -0.2280(4) 0.6149(3) 0.0422(17) Uani 1 1 d . . . C1 C 0.0550(9) 0.0351(6) 0.7743(5) 0.051(2) Uani 1 1 d . . . C2 C -0.0611(9) 0.0599(11) 0.7718(9) 0.117(6) Uani 1 1 d . . . H2A H -0.0693 0.1064 0.7406 0.175 Uiso 1 1 calc R . . H2B H -0.0856 0.0757 0.8179 0.175 Uiso 1 1 calc R . . H2C H -0.1061 0.0142 0.7554 0.175 Uiso 1 1 calc R . . C3 C 0.2868(8) -0.2822(6) 0.9064(4) 0.043(2) Uani 1 1 d . . . C4 C 0.2290(11) -0.3375(9) 0.9533(6) 0.087(4) Uani 1 1 d . . . H4A H 0.1790 -0.3727 0.9271 0.131 Uiso 1 1 calc R . . H4B H 0.1863 -0.3055 0.9865 0.131 Uiso 1 1 calc R . . H4C H 0.2829 -0.3713 0.9777 0.131 Uiso 1 1 calc R . . C5 C 0.7080(9) -0.1818(6) 0.5847(5) 0.052(2) Uani 1 1 d . . . C6 C 0.7691(12) -0.1234(8) 0.5471(7) 0.099(5) Uani 1 1 d . . . H6A H 0.7542 -0.1301 0.4980 0.148 Uiso 1 1 calc R . . H6B H 0.8481 -0.1312 0.5558 0.148 Uiso 1 1 calc R . . H6C H 0.7474 -0.0684 0.5616 0.148 Uiso 1 1 calc R . . C7 C 0.5257(7) 0.0054(5) 0.8725(4) 0.0362(18) Uani 1 1 d . . . H7A H 0.5540 -0.0300 0.9098 0.043 Uiso 1 1 calc R . . H7B H 0.5817 0.0059 0.8356 0.043 Uiso 1 1 calc R . . C8 C 0.4040(9) 0.0910(5) 0.9689(4) 0.050(3) Uani 1 1 d . . . H8A H 0.4326 0.0540 1.0049 0.060 Uiso 1 1 calc R . . H8B H 0.3865 0.1439 0.9909 0.060 Uiso 1 1 calc R . . C9 C 0.2992(8) 0.0552(6) 0.9401(4) 0.045(2) Uani 1 1 d . . . H9A H 0.2736 0.0900 0.9017 0.054 Uiso 1 1 calc R . . H9B H 0.2416 0.0565 0.9761 0.054 Uiso 1 1 calc R . . C10 C 0.3114(7) -0.0319(5) 0.9144(4) 0.0393(19) Uani 1 1 d . . . H10A H 0.2374 -0.0538 0.9032 0.047 Uiso 1 1 calc R . . H10B H 0.3428 -0.0659 0.9516 0.047 Uiso 1 1 calc R . . C11 C 0.4242(8) -0.1288(5) 0.6411(4) 0.040(2) Uani 1 1 d . . . H11A H 0.4962 -0.1007 0.6455 0.048 Uiso 1 1 calc R . . H11B H 0.4219 -0.1539 0.5949 0.048 Uiso 1 1 calc R . . C12 C 0.1960(7) -0.1196(5) 0.6416(4) 0.040(2) Uani 1 1 d . . . H12A H 0.1290 -0.0854 0.6456 0.048 Uiso 1 1 calc R . . H12B H 0.1941 -0.1463 0.5960 0.048 Uiso 1 1 calc R . . C13 C 0.1918(7) -0.1847(5) 0.6960(4) 0.0399(19) Uani 1 1 d . . . H13A H 0.1185 -0.2113 0.6946 0.048 Uiso 1 1 calc R . . H13B H 0.2000 -0.1586 0.7416 0.048 Uiso 1 1 calc R . . C14 C 0.2821(7) -0.2508(5) 0.6879(4) 0.0379(19) Uani 1 1 d . . . H14A H 0.2791 -0.2735 0.6409 0.046 Uiso 1 1 calc R . . H14B H 0.2674 -0.2959 0.7205 0.046 Uiso 1 1 calc R . . C15 C 0.6153(7) -0.3267(5) 0.8499(4) 0.0340(18) Uani 1 1 d . . . H15A H 0.5445 -0.3550 0.8586 0.041 Uiso 1 1 calc R . . H15B H 0.6710 -0.3502 0.8814 0.041 Uiso 1 1 calc R . . C16 C 0.7867(7) -0.2916(5) 0.7589(5) 0.043(2) Uani 1 1 d . . . H16A H 0.8376 -0.3148 0.7935 0.051 Uiso 1 1 calc R . . H16B H 0.8207 -0.2989 0.7131 0.051 Uiso 1 1 calc R . . C17 C 0.7714(8) -0.1987(5) 0.7732(5) 0.046(2) Uani 1 1 d . . . H17A H 0.8421 -0.1704 0.7643 0.055 Uiso 1 1 calc R . . H17B H 0.7160 -0.1767 0.7407 0.055 Uiso 1 1 calc R . . C18 C 0.7347(8) -0.1801(6) 0.8457(5) 0.053(2) Uani 1 1 d . . . H18A H 0.7342 -0.1201 0.8518 0.064 Uiso 1 1 calc R . . H18B H 0.7901 -0.2027 0.8778 0.064 Uiso 1 1 calc R . . C1A C 0.4768(16) -0.4809(12) 1.0301(12) 0.115(8) Uiso 0.680(7) 1 d PD A 2 H1A1 H 0.4689 -0.4900 0.9801 0.138 Uiso 0.680(7) 1 calc PR A 2 H1A2 H 0.5321 -0.5200 1.0479 0.138 Uiso 0.680(7) 1 calc PR A 2 C1B C 0.562(4) -0.3342(18) 1.0489(10) 0.092(13) Uiso 0.320(7) 1 d PD A 1 H1B1 H 0.5191 -0.2860 1.0338 0.111 Uiso 0.320(7) 1 calc PR A 1 H1B2 H 0.6402 -0.3253 1.0362 0.111 Uiso 0.320(7) 1 calc PR A 1 B1 B 0.4282(12) -0.1257(7) 1.0744(6) 0.059(3) Uani 1 1 d . . . B2 B 0.6467(10) 0.0280(8) 0.6940(6) 0.058(3) Uani 1 1 d . . . B3 B 0.4788(9) -0.2090(7) 0.4357(5) 0.058(3) Uani 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 0.0388(5) 0.0274(4) 0.0308(5) -0.0029(4) -0.0020(4) -0.0005(4) Cu2 0.0437(6) 0.0284(5) 0.0276(4) 0.0002(4) -0.0020(4) -0.0009(4) Cu3 0.0422(6) 0.0275(5) 0.0272(4) 0.0024(3) -0.0004(4) 0.0040(4) S1 0.0407(11) 0.0271(9) 0.0217(8) -0.0008(7) -0.0022(7) -0.0021(8) S2 0.0513(13) 0.0304(10) 0.0250(9) -0.0005(7) -0.0044(8) -0.0069(9) S3 0.0392(11) 0.0232(9) 0.0239(8) -0.0007(7) -0.0034(7) 0.0020(8) S4 0.0526(13) 0.0240(9) 0.0259(9) -0.0014(7) -0.0092(9) 0.0055(9) S5 0.0497(13) 0.0374(11) 0.0344(10) -0.0045(9) -0.0113(9) 0.0072(10) S6 0.0401(11) 0.0234(9) 0.0294(9) 0.0036(7) -0.0032(8) 0.0002(8) F1 0.144(7) 0.066(5) 0.137(7) -0.004(5) 0.063(6) 0.039(5) F2 0.109(6) 0.158(8) 0.079(5) 0.072(5) 0.031(4) 0.052(6) F3 0.185(10) 0.132(8) 0.111(7) -0.015(6) 0.045(7) -0.072(8) F4 0.068(4) 0.082(5) 0.070(4) 0.036(3) 0.019(3) 0.008(3) F5 0.214(10) 0.053(4) 0.064(4) -0.014(3) 0.023(5) -0.016(5) F6 0.142(6) 0.046(3) 0.053(3) 0.006(3) -0.005(4) 0.017(4) F7 0.131(6) 0.067(4) 0.060(4) 0.006(3) -0.022(4) -0.012(4) F8 0.063(5) 0.326(17) 0.116(7) 0.045(9) 0.015(5) -0.020(7) F9 0.058(4) 0.147(7) 0.110(6) -0.038(5) -0.018(4) 0.017(5) F12 0.163(8) 0.143(7) 0.052(4) -0.038(4) 0.036(5) -0.069(7) N1 0.039(4) 0.046(4) 0.045(4) 0.001(3) 0.000(3) -0.001(4) N2 0.061(5) 0.035(4) 0.035(4) -0.002(3) 0.011(4) -0.001(4) N3 0.054(5) 0.037(4) 0.036(4) -0.005(3) 0.007(3) 0.010(4) C1 0.042(6) 0.058(6) 0.053(5) 0.004(4) -0.004(4) -0.005(5) C2 0.033(7) 0.163(15) 0.155(14) 0.022(12) 0.018(8) 0.017(8) C3 0.048(5) 0.053(5) 0.027(4) -0.001(4) -0.001(4) 0.006(5) C4 0.092(10) 0.107(11) 0.063(7) 0.038(7) 0.031(7) -0.013(8) C5 0.062(6) 0.032(5) 0.063(6) -0.001(4) 0.015(5) 0.006(5) C6 0.115(12) 0.071(9) 0.111(11) 0.023(8) 0.057(10) 0.000(8) C7 0.051(5) 0.028(4) 0.030(4) -0.001(3) -0.001(3) -0.001(4) C8 0.102(8) 0.035(5) 0.014(3) -0.004(3) 0.008(4) -0.011(5) C9 0.050(6) 0.050(5) 0.036(4) -0.010(4) 0.016(4) -0.008(5) C10 0.044(5) 0.045(5) 0.030(4) -0.002(3) 0.009(4) -0.007(4) C11 0.068(6) 0.026(4) 0.025(4) 0.005(3) 0.002(4) 0.011(4) C12 0.031(4) 0.041(5) 0.049(5) -0.014(4) -0.012(4) -0.007(4) C13 0.044(5) 0.035(4) 0.041(4) -0.003(3) -0.002(4) 0.001(4) C14 0.051(5) 0.027(4) 0.036(4) -0.001(3) -0.007(4) -0.002(4) C15 0.045(5) 0.027(4) 0.030(4) 0.002(3) -0.014(3) 0.003(4) C16 0.050(5) 0.028(4) 0.051(5) -0.001(4) -0.005(4) 0.007(4) C17 0.050(6) 0.031(5) 0.057(5) 0.000(4) -0.009(4) -0.012(4) C18 0.057(6) 0.034(5) 0.068(6) -0.005(4) -0.027(5) -0.005(4) B1 0.072(9) 0.046(6) 0.060(7) 0.018(5) 0.014(7) 0.021(7) B2 0.056(7) 0.061(8) 0.057(7) -0.007(6) 0.011(6) -0.008(6) B3 0.067(8) 0.068(8) 0.041(6) 0.012(6) -0.011(5) 0.011(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 N1 1.985(8) . ? Cu1 S4 2.290(2) . ? Cu1 S1 2.300(2) . ? Cu1 S6 2.318(2) 4_656 ? Cu2 N2 1.976(7) . ? Cu2 S1 2.281(2) . ? Cu2 S3 2.2937(19) . ? Cu2 S5 2.334(2) . ? Cu3 N3 1.991(8) . ? Cu3 S6 2.296(2) . ? Cu3 S2 2.301(2) 4_646 ? Cu3 S3 2.311(2) . ? Cl1A C1A 1.770(16) . ? Cl2A C1A 1.801(16) . ? Cl1B C1B 1.753(19) . ? Cl2B C1B 1.760(19) . ? S1 C7 1.821(8) . ? S1 C10 1.825(8) . ? S2 C7 1.793(8) . ? S2 C8 1.816(9) . ? S2 Cu3 2.301(2) 4_656 ? S3 C11 1.805(7) . ? S3 C14 1.819(8) . ? S4 C11 1.793(8) . ? S4 C12 1.833(8) . ? S5 C15 1.806(8) . ? S5 C18 1.834(10) . ? S6 C16 1.804(9) . ? S6 C15 1.825(8) . ? S6 Cu1 2.318(2) 4_646 ? F1 B1 1.318(13) . ? F2 B1 1.394(13) . ? F3 B1 1.386(16) . ? F4 B1 1.323(13) . ? F5 B2 1.384(13) . ? F6 B2 1.364(14) . ? F7 B2 1.433(14) . ? F8 B2 1.320(14) . ? F9 B3 1.335(11) . ? F10 B3 1.495(12) . ? F11 B3 1.306(11) . ? F12 B3 1.301(11) . ? N1 C1 1.140(11) . ? N2 C3 1.111(11) . ? N3 C5 1.132(11) . ? C1 C2 1.466(15) . ? C3 C4 1.465(13) . ? C5 C6 1.413(15) . ? C8 C9 1.506(13) . ? C9 C10 1.519(11) . ? C12 C13 1.504(11) . ? C13 C14 1.547(11) . ? C16 C17 1.557(11) . ? C17 C18 1.512(13) . ? 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 N1 Cu1 S4 106.7(2) . . ? N1 Cu1 S1 107.4(2) . . ? S4 Cu1 S1 116.48(8) . . ? N1 Cu1 S6 101.7(2) . 4_656 ? S4 Cu1 S6 113.10(8) . 4_656 ? S1 Cu1 S6 110.14(7) . 4_656 ? N2 Cu2 S1 109.2(2) . . ? N2 Cu2 S3 107.4(2) . . ? S1 Cu2 S3 113.86(7) . . ? N2 Cu2 S5 96.6(2) . . ? S1 Cu2 S5 113.23(8) . . ? S3 Cu2 S5 114.89(8) . . ? N3 Cu3 S6 107.3(2) . . ? N3 Cu3 S2 105.3(2) . 4_646 ? S6 Cu3 S2 116.94(8) . 4_646 ? N3 Cu3 S3 103.8(2) . . ? S6 Cu3 S3 112.49(7) . . ? S2 Cu3 S3 109.87(8) 4_646 . ? C7 S1 C10 99.8(4) . . ? C7 S1 Cu2 107.0(3) . . ? C10 S1 Cu2 109.6(3) . . ? C7 S1 Cu1 122.7(3) . . ? C10 S1 Cu1 107.5(3) . . ? Cu2 S1 Cu1 109.52(8) . . ? C7 S2 C8 100.2(4) . . ? C7 S2 Cu3 115.8(3) . 4_656 ? C8 S2 Cu3 106.0(3) . 4_656 ? C11 S3 C14 100.8(4) . . ? C11 S3 Cu2 117.5(3) . . ? C14 S3 Cu2 110.2(3) . . ? C11 S3 Cu3 104.1(3) . . ? C14 S3 Cu3 112.5(3) . . ? Cu2 S3 Cu3 111.28(8) . . ? C11 S4 C12 99.5(4) . . ? C11 S4 Cu1 115.4(3) . . ? C12 S4 Cu1 105.6(3) . . ? C15 S5 C18 100.8(4) . . ? C15 S5 Cu2 108.1(3) . . ? C18 S5 Cu2 121.8(3) . . ? C16 S6 C15 100.5(4) . . ? C16 S6 Cu3 105.0(3) . . ? C15 S6 Cu3 121.2(3) . . ? C16 S6 Cu1 108.4(3) . 4_646 ? C15 S6 Cu1 107.9(3) . 4_646 ? Cu3 S6 Cu1 112.52(8) . 4_646 ? C1 N1 Cu1 160.2(8) . . ? C3 N2 Cu2 171.1(8) . . ? C5 N3 Cu3 172.7(7) . . ? N1 C1 C2 176.7(11) . . ? N2 C3 C4 176.6(11) . . ? N3 C5 C6 179.4(12) . . ? S2 C7 S1 115.2(4) . . ? C9 C8 S2 113.9(5) . . ? C8 C9 C10 113.9(8) . . ? C9 C10 S1 113.0(6) . . ? S4 C11 S3 116.8(5) . . ? C13 C12 S4 114.8(6) . . ? C12 C13 C14 113.6(7) . . ? C13 C14 S3 111.6(5) . . ? S5 C15 S6 114.2(4) . . ? C17 C16 S6 112.4(6) . . ? C18 C17 C16 113.5(8) . . ? C17 C18 S5 115.7(6) . . ? Cl1A C1A Cl2A 109.3(11) . . ? Cl1B C1B Cl2B 110.7(14) . . ? F1 B1 F4 117.2(9) . . ? F1 B1 F3 102.9(11) . . ? F4 B1 F3 108.8(10) . . ? F1 B1 F2 108.5(10) . . ? F4 B1 F2 113.1(10) . . ? F3 B1 F2 105.1(10) . . ? F8 B2 F6 116.2(12) . . ? F8 B2 F5 115.4(12) . . ? F6 B2 F5 109.8(9) . . ? F8 B2 F7 104.2(10) . . ? F6 B2 F7 106.4(9) . . ? F5 B2 F7 103.4(10) . . ? F12 B3 F11 116.2(10) . . ? F12 B3 F9 119.1(9) . . ? F11 B3 F9 116.9(10) . . ? F12 B3 F10 105.3(9) . . ? F11 B3 F10 91.7(8) . . ? F9 B3 F10 100.6(9) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.237 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.123