# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2263 #====================================================================== data_a20a-b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H42 Cl2 Cu2 P2' _chemical_formula_sum 'C42 H42 Cl2 Cu2 P2' _chemical_formula_weight 806.68 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' 'P' 'P' 0.1023 0.0942 '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' 'Cu' 'Cu' 0.3201 1.2651 '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, -y, -z' _cell_length_a 9.7619(3) _cell_length_b 9.7619(3) _cell_length_c 9.7619(3) _cell_angle_alpha 90.02(3) _cell_angle_beta 90.02(3) _cell_angle_gamma 90.02(3) _cell_volume 930.26(5) _cell_formula_units_Z 1 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 1.402 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7295 _exptl_absorpt_correction_T_max 0.7295 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 3522 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.42 _reflns_number_total 2429 _reflns_number_gt 2305 _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^)+(0.1426P)^2^+6.0099P] 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_number_reflns 2429 _refine_ls_number_parameters 225 _refine_ls_number_restraints 162 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0894 _refine_ls_wR_factor_ref 0.2428 _refine_ls_wR_factor_gt 0.2397 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.010 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.0000 0.5000 0.0293(5) Uani 1 2 d SU . . Cu2 Cu 1.0000 -0.5000 0.0000 0.0353(6) Uani 1 2 d SU . . Cl2 Cl 1.1226(5) -0.3764(5) 0.1227(4) 0.0568(12) Uani 0.945(7) 1 d PU . . P1 P 0.3697(4) -0.1303(3) 0.3692(3) 0.0272(7) Uani 0.945(7) 1 d PU . . C1 C 0.3951(13) -0.3159(10) 0.3959(14) 0.028(3) Uani 0.945(7) 1 d PDU . . H1A H 0.3562 -0.3434 0.4842 0.034 Uiso 0.945(7) 1 calc PR . . H1B H 0.3486 -0.3676 0.3234 0.034 Uiso 0.945(7) 1 calc PR . . C11 C 0.5447(15) -0.3455(9) 0.3933(14) 0.033(3) Uani 0.945(7) 1 d PDU . . C12 C 0.6194(14) -0.3339(14) 0.5166(17) 0.042(4) Uani 0.945(7) 1 d PDU . . H12A H 0.5759 -0.3051 0.5975 0.050 Uiso 0.945(7) 1 calc PR . . C13 C 0.7664(17) -0.3674(15) 0.5164(17) 0.046(4) Uani 0.945(7) 1 d PDU . . H13A H 0.8184 -0.3639 0.5974 0.055 Uiso 0.945(7) 1 calc PR . . C14 C 0.8227(17) -0.4026(17) 0.399(2) 0.054(4) Uani 0.945(7) 1 d PDU . . H14A H 0.9167 -0.4234 0.3980 0.064 Uiso 0.945(7) 1 calc PR . . C15 C 0.7529(17) -0.4105(15) 0.279(2) 0.049(4) Uani 0.945(7) 1 d PDU . . H15A H 0.7989 -0.4331 0.1972 0.059 Uiso 0.945(7) 1 calc PR . . C16 C 0.611(2) -0.3845(17) 0.277(2) 0.061(5) Uani 0.945(7) 1 d PDU . . H16A H 0.5618 -0.3943 0.1953 0.073 Uiso 0.945(7) 1 calc PR . . C2 C 0.4018(16) -0.1061(11) 0.1832(11) 0.032(3) Uani 0.945(7) 1 d PDU . . H2A H 0.4927 -0.1411 0.1590 0.038 Uiso 0.945(7) 1 calc PR . . H2B H 0.3332 -0.1560 0.1295 0.038 Uiso 0.945(7) 1 calc PR . . C21 C 0.3931(15) 0.0474(14) 0.1526(9) 0.037(3) Uani 0.945(7) 1 d PDU . . C26 C 0.280(2) 0.1167(19) 0.1156(15) 0.054(4) Uani 0.945(7) 1 d PDU . . H26A H 0.1964 0.0691 0.1063 0.065 Uiso 0.945(7) 1 calc PR . . C25 C 0.2824(17) 0.2544(17) 0.0915(17) 0.052(4) Uani 0.945(7) 1 d PDU . . H25A H 0.1993 0.2969 0.0677 0.062 Uiso 0.945(7) 1 calc PR . . C24 C 0.385(2) 0.3275(16) 0.0983(18) 0.056(5) Uani 0.945(7) 1 d PDU . . H24A H 0.3797 0.4222 0.0818 0.067 Uiso 0.945(7) 1 calc PR . . C23 C 0.5176(17) 0.2629(19) 0.1328(17) 0.051(4) Uani 0.945(7) 1 d PDU . . H23A H 0.5987 0.3148 0.1351 0.061 Uiso 0.945(7) 1 calc PR . . C22 C 0.520(2) 0.1248(18) 0.1616(18) 0.059(5) Uani 0.945(7) 1 d PDU . . H22A H 0.6017 0.0813 0.1867 0.070 Uiso 0.945(7) 1 calc PR . . C3 C 0.1810(13) -0.1032(13) 0.4007(13) 0.032(3) Uani 0.945(7) 1 d PDU . . H3A H 0.1525 -0.0149 0.3625 0.038 Uiso 0.945(7) 1 calc PR . . H3B H 0.1282 -0.1756 0.3555 0.038 Uiso 0.945(7) 1 calc PR . . C31 C 0.1546(9) -0.1055(13) 0.5484(15) 0.034(3) Uani 0.945(7) 1 d PDU . . C36 C 0.1161(16) -0.2205(15) 0.6187(19) 0.048(4) Uani 0.945(7) 1 d PDU . . H36A H 0.1073 -0.3036 0.5708 0.057 Uiso 0.945(7) 1 calc PR . . C35 C 0.0913(15) -0.2184(18) 0.7494(17) 0.047(4) Uani 0.945(7) 1 d PDU . . H35A H 0.0626 -0.2994 0.7928 0.056 Uiso 0.945(7) 1 calc PR . . C34 C 0.105(2) -0.103(2) 0.8246(19) 0.062(5) Uani 0.945(7) 1 d PDU . . H34A H 0.0958 -0.1096 0.9202 0.075 Uiso 0.945(7) 1 calc PR . . C33 C 0.1336(17) 0.0227(16) 0.7677(18) 0.048(4) Uani 0.945(7) 1 d PDU . . H33A H 0.1323 0.1038 0.8195 0.058 Uiso 0.945(7) 1 calc PR . . C32 C 0.1648(15) 0.0219(13) 0.6245(15) 0.050(4) Uani 0.945(7) 1 d PDU . . H32A H 0.1916 0.1031 0.5802 0.059 Uiso 0.945(7) 1 calc PR . . Cl2' Cl 0.1244(15) -0.3775(13) 0.8660(15) 0.007(8) Uiso 0.055(7) 1 d PR . . P1' P 0.6276(15) 0.1243(13) 0.3682(15) 0.004(8) Uiso 0.055(7) 1 d PR . . 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 0.0280(15) 0.0270(11) 0.0330(13) 0.0006(9) -0.0057(11) -0.0018(10) Cu2 0.0349(17) 0.0334(13) 0.0377(15) 0.0018(10) -0.0023(12) -0.0003(12) Cl2 0.058(3) 0.062(3) 0.050(2) -0.009(2) -0.011(2) -0.016(2) P1 0.029(2) 0.0277(15) 0.0247(16) -0.0012(13) -0.0017(14) -0.0014(14) C1 0.025(7) 0.024(5) 0.035(6) 0.000(5) 0.013(5) 0.010(5) C11 0.037(8) 0.024(5) 0.038(7) 0.000(5) 0.000(6) -0.013(5) C12 0.021(7) 0.047(7) 0.057(9) 0.011(7) 0.006(6) -0.004(6) C13 0.047(9) 0.044(7) 0.048(9) 0.018(7) 0.008(7) 0.006(7) C14 0.030(8) 0.056(9) 0.075(12) 0.011(8) 0.008(8) 0.000(7) C15 0.037(9) 0.043(7) 0.067(10) -0.004(7) 0.013(8) 0.018(7) C16 0.067(12) 0.054(9) 0.061(11) 0.003(8) 0.002(9) 0.019(9) C2 0.054(9) 0.018(5) 0.022(5) 0.003(4) -0.009(6) 0.003(5) C21 0.036(8) 0.049(7) 0.024(6) -0.005(5) 0.007(5) 0.024(7) C26 0.067(12) 0.068(10) 0.028(7) 0.005(7) -0.004(7) 0.000(9) C25 0.044(9) 0.051(8) 0.060(10) 0.026(8) 0.006(8) 0.007(7) C24 0.070(13) 0.041(7) 0.057(10) 0.002(7) 0.031(9) 0.017(8) C23 0.030(8) 0.071(10) 0.052(9) 0.001(8) -0.001(7) -0.005(8) C22 0.054(10) 0.055(9) 0.067(11) 0.022(8) -0.004(8) -0.006(8) C3 0.033(7) 0.040(6) 0.023(6) 0.000(5) 0.009(5) 0.002(5) C31 0.012(6) 0.040(6) 0.050(8) 0.016(6) 0.012(5) 0.007(5) C36 0.037(9) 0.037(6) 0.069(10) 0.017(7) 0.016(8) 0.002(6) C35 0.030(8) 0.065(9) 0.045(8) 0.012(7) 0.016(7) -0.010(7) C34 0.077(14) 0.065(10) 0.045(9) 0.011(8) 0.004(9) 0.012(9) C33 0.046(10) 0.047(8) 0.052(9) -0.016(7) 0.000(8) -0.002(7) C32 0.055(10) 0.039(7) 0.054(9) 0.012(7) -0.010(8) -0.007(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 P1' 2.163(12) 2_656 ? Cu1 P1' 2.163(12) . ? Cu1 P1 2.205(3) . ? Cu1 P1 2.205(3) 2_656 ? Cu2 Cl2 2.079(4) . ? Cu2 Cl2 2.079(4) 2_745 ? Cu2 Cl2' 2.149(12) 1_654 ? Cu2 Cl2' 2.149(12) 2_646 ? P1 C3 1.887(13) . ? P1 C1 1.847(10) . ? P1 C2 1.858(12) . ? P1 P1' 2.564(15) 2_656 ? C1 C11 1.489(19) . ? C11 C16 1.36(2) . ? C11 C12 1.41(2) . ? C12 C13 1.47(2) . ? C13 C14 1.32(3) . ? C14 C15 1.36(3) . ? C15 C16 1.41(3) . ? C2 C21 1.531(17) . ? C21 C26 1.35(2) . ? C21 C22 1.45(2) . ? C26 C25 1.36(2) . ? C25 C24 1.23(3) . ? C24 C23 1.48(3) . ? C23 C22 1.38(2) . ? C22 P1' 2.28(2) . ? C3 C31 1.464(19) . ? C31 C36 1.368(17) . ? C31 C32 1.45(2) . ? C31 P1' 2.283(17) 2_656 ? C36 C35 1.30(2) . ? C35 C34 1.35(3) . ? C35 Cl2' 1.954(19) . ? C34 C33 1.38(3) . ? C33 C32 1.43(2) . ? Cl2' Cu2 2.149(12) 1_456 ? P1' C31 2.283(17) 2_656 ? P1' P1 2.564(15) 2_656 ? 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 P1' Cu1 P1' 180.0 2_656 . ? P1' Cu1 P1 71.9(4) 2_656 . ? P1' Cu1 P1 108.1(4) . . ? P1' Cu1 P1 108.1(4) 2_656 2_656 ? P1' Cu1 P1 71.9(4) . 2_656 ? P1 Cu1 P1 180.00(15) . 2_656 ? Cl2 Cu2 Cl2 180.00(19) . 2_745 ? Cl2 Cu2 Cl2' 72.7(4) . 1_654 ? Cl2 Cu2 Cl2' 107.3(4) 2_745 1_654 ? Cl2 Cu2 Cl2' 107.3(4) . 2_646 ? Cl2 Cu2 Cl2' 72.7(4) 2_745 2_646 ? Cl2' Cu2 Cl2' 180.0 1_654 2_646 ? C3 P1 C1 104.2(6) . . ? C3 P1 C2 107.8(6) . . ? C1 P1 C2 103.9(6) . . ? C3 P1 Cu1 112.8(4) . . ? C1 P1 Cu1 114.0(4) . . ? C2 P1 Cu1 113.3(4) . . ? C3 P1 P1' 81.0(5) . 2_656 ? C1 P1 P1' 83.1(5) . 2_656 ? C2 P1 P1' 166.5(5) . 2_656 ? Cu1 P1 P1' 53.3(3) . 2_656 ? C11 C1 P1 108.6(7) . . ? C16 C11 C12 119.1(15) . . ? C16 C11 C1 122.5(14) . . ? C12 C11 C1 118.4(13) . . ? C13 C12 C11 119.0(15) . . ? C14 C13 C12 117.7(16) . . ? C13 C14 C15 123.9(16) . . ? C14 C15 C16 119.4(17) . . ? C11 C16 C15 120.8(19) . . ? C21 C2 P1 107.9(6) . . ? C26 C21 C22 117.0(15) . . ? C26 C21 C2 126.1(16) . . ? C22 C21 C2 116.8(12) . . ? C21 C26 C25 121.7(18) . . ? C24 C25 C26 125.2(16) . . ? C25 C24 C23 118.5(15) . . ? C22 C23 C24 118.5(16) . . ? C23 C22 C21 119.1(15) . . ? C23 C22 P1' 100.9(13) . . ? C21 C22 P1' 116.6(10) . . ? C31 C3 P1 109.3(7) . . ? C36 C31 C32 117.7(14) . . ? C36 C31 C3 123.7(15) . . ? C32 C31 C3 118.6(11) . . ? C36 C31 P1' 90.6(9) . 2_656 ? C32 C31 P1' 79.8(9) . 2_656 ? C3 C31 P1' 100.8(7) . 2_656 ? C35 C36 C31 122.1(17) . . ? C36 C35 C34 121.9(15) . . ? C36 C35 Cl2' 122.0(15) . . ? C34 C35 Cl2' 109.1(13) . . ? C35 C34 C33 123.0(17) . . ? C32 C33 C34 115.6(15) . . ? C33 C32 C31 119.3(11) . . ? C35 Cl2' Cu2 134.7(9) . 1_456 ? Cu1 P1' C22 105.2(7) . . ? Cu1 P1' C31 106.2(6) . 2_656 ? C22 P1' C31 138.4(9) . 2_656 ? Cu1 P1' P1 54.8(3) . 2_656 ? C22 P1' P1 152.9(8) . 2_656 ? C31 P1' P1 68.7(5) 2_656 2_656 ? _diffrn_measured_fraction_theta_max 0.578 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.578 _refine_diff_density_max 0.665 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.134 #===END data_amb5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H42 Cu I P2' _chemical_formula_sum 'C42 H42 Cu I P2' _chemical_formula_weight 799.14 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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 mono9clinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.001(2) _cell_length_b 14.529(3) _cell_length_c 26.330(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.68(3) _cell_angle_gamma 90.00 _cell_volume 3813.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 15 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 1.494 _exptl_absorpt_correction_type 'empirical via \y scans' _exptl_absorpt_correction_T_min 0.5529 _exptl_absorpt_correction_T_max 0.6385 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'ENRAF-NONIUS CAD-4 ' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13921 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6717 _reflns_number_gt 4235 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS CAD4/PC' _computing_cell_refinement 'NONIUS CAD4/PC' _computing_data_reduction 'XCAD-4B (Harms, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XPMA (Zsolnai, 1994)' _computing_publication_material 'SHELXL-97 (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^)+(0.0652P)^2^+1.9007P] 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_number_reflns 6717 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1202 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.010 _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 I I 0.92326(4) 0.57907(2) 0.690164(12) 0.08391(16) Uani 1 1 d . . . Cu Cu 0.90678(5) 0.74829(4) 0.659791(18) 0.05104(15) Uani 1 1 d . . . P1 P 0.99808(10) 0.74971(8) 0.58492(4) 0.0498(2) Uani 1 1 d . . . P2 P 0.81776(10) 0.84545(7) 0.71348(4) 0.0471(2) Uani 1 1 d . . . C11 C 1.1820(4) 0.7648(3) 0.59337(19) 0.0660(12) Uani 1 1 d . . . H11A H 1.2164 0.7690 0.5605 0.079 Uiso 1 1 d R . . H11B H 1.2208 0.7112 0.6101 0.079 Uiso 1 1 d R . . C111 C 1.2250(4) 0.8486(3) 0.6240(2) 0.0672(13) Uani 1 1 d . . . C112 C 1.2256(5) 0.8468(4) 0.6765(2) 0.0823(16) Uani 1 1 d . . . H11C H 1.1943 0.7931 0.6931 0.099 Uiso 1 1 d R . . C113 C 1.2722(6) 0.9209(5) 0.7053(3) 0.105(2) Uani 1 1 d . . . H11D H 1.2697 0.9197 0.7416 0.126 Uiso 1 1 d R . . C114 C 1.3201(6) 0.9957(6) 0.6830(4) 0.115(3) Uani 1 1 d . . . H11E H 1.3579 1.0451 0.7038 0.138 Uiso 1 1 d R . . C115 C 1.3164(6) 1.0028(5) 0.6312(4) 0.110(2) Uani 1 1 d . . . H11F H 1.3456 1.0580 0.6153 0.132 Uiso 1 1 d R . . C116 C 1.2691(5) 0.9270(4) 0.6015(3) 0.0877(17) Uani 1 1 d . . . H11G H 1.2675 0.9303 0.5650 0.105 Uiso 1 1 d R . . C12 C 0.9790(5) 0.6382(3) 0.55213(17) 0.0670(12) Uani 1 1 d . . . H12A H 0.8925 0.6375 0.5334 0.080 Uiso 1 1 d R . . H12G H 0.9783 0.5910 0.5776 0.080 Uiso 1 1 d R . . C121 C 1.0808(5) 0.6118(3) 0.51600(16) 0.0616(11) Uani 1 1 d . . . C126 C 1.0662(6) 0.6306(4) 0.46538(18) 0.0839(16) Uani 1 1 d . . . H12B H 0.9881 0.6635 0.4517 0.101 Uiso 1 1 d R . . C125 C 1.1635(9) 0.6034(4) 0.4329(2) 0.109(2) Uani 1 1 d . . . H12C H 1.1529 0.6177 0.3972 0.130 Uiso 1 1 d R . . C124 C 1.2738(8) 0.5565(5) 0.4532(3) 0.117(2) Uani 1 1 d . . . H12D H 1.3419 0.5382 0.4316 0.141 Uiso 1 1 d R . . C123 C 1.2870(7) 0.5344(5) 0.5029(3) 0.121(2) Uani 1 1 d . . . H12E H 1.3628 0.4991 0.5164 0.145 Uiso 1 1 d R . . C122 C 1.1925(6) 0.5632(4) 0.5345(2) 0.0940(18) Uani 1 1 d . . . H12F H 1.2044 0.5489 0.5701 0.113 Uiso 1 1 d R . . C13 C 0.9498(4) 0.8348(3) 0.53496(16) 0.0601(11) Uani 1 1 d . . . H13A H 0.9911 0.8187 0.5045 0.072 Uiso 1 1 d R . . H13B H 0.9829 0.8943 0.5458 0.072 Uiso 1 1 d R . . C131 C 0.7994(5) 0.8401(3) 0.52319(16) 0.0626(12) Uani 1 1 d . . . C136 C 0.7363(6) 0.7916(5) 0.4843(2) 0.106(2) Uani 1 1 d . . . H13C H 0.7880 0.7536 0.4634 0.127 Uiso 1 1 d R . . C135 C 0.5956(7) 0.7958(6) 0.4741(3) 0.136(3) Uani 1 1 d . . . H13D H 0.5517 0.7595 0.4472 0.163 Uiso 1 1 d R . . C134 C 0.5230(6) 0.8498(6) 0.5028(3) 0.113(2) Uani 1 1 d . . . H13E H 0.4273 0.8526 0.4961 0.136 Uiso 1 1 d R . . C133 C 0.5847(6) 0.9008(5) 0.5408(2) 0.102(2) Uani 1 1 d . . . H13F H 0.5326 0.9407 0.5605 0.123 Uiso 1 1 d R . . C132 C 0.7224(5) 0.8962(4) 0.5509(2) 0.0767(14) Uani 1 1 d . . . H13G H 0.7649 0.9322 0.5782 0.092 Uiso 1 1 d R . . C21 C 0.8258(4) 0.8056(3) 0.77983(15) 0.0613(11) Uani 1 1 d . . . H21A H 0.7968 0.7426 0.7804 0.074 Uiso 1 1 d R . . H21B H 0.7644 0.8414 0.7979 0.074 Uiso 1 1 d R . . C211 C 0.9628(5) 0.8130(3) 0.80733(15) 0.0600(11) Uani 1 1 d . . . C212 C 0.9878(8) 0.8802(5) 0.8432(2) 0.106(2) Uani 1 1 d . . . H21C H 0.9179 0.9225 0.8502 0.127 Uiso 1 1 d R . . C213 C 1.1125(12) 0.8885(6) 0.8691(3) 0.148(4) Uani 1 1 d . . . H21D H 1.1272 0.9341 0.8953 0.177 Uiso 1 1 d R . . C214 C 1.2143(9) 0.8323(6) 0.8587(3) 0.122(3) Uani 1 1 d . . . H21E H 1.3030 0.8414 0.8747 0.147 Uiso 1 1 d R . . C215 C 1.1893(7) 0.7624(6) 0.8238(3) 0.117(2) Uani 1 1 d . . . H21F H 1.2584 0.7189 0.8177 0.140 Uiso 1 1 d R . . C216 C 1.0635(5) 0.7545(4) 0.7982(2) 0.0883(17) Uani 1 1 d . . . H21G H 1.0474 0.7069 0.7731 0.106 Uiso 1 1 d R . . C22 C 0.6359(4) 0.8599(3) 0.69907(19) 0.0620(11) Uani 1 1 d . . . H22A H 0.6203 0.8921 0.6673 0.074 Uiso 1 1 d R . . H22B H 0.6012 0.8972 0.7251 0.074 Uiso 1 1 d R . . C221 C 0.5607(4) 0.7704(3) 0.6954(2) 0.0652(12) Uani 1 1 d . . . C222 C 0.5011(5) 0.7356(4) 0.7372(2) 0.0843(16) Uani 1 1 d . . . H22C H 0.5112 0.7674 0.7692 0.101 Uiso 1 1 d R . . C223 C 0.4272(6) 0.6544(5) 0.7326(3) 0.102(2) Uani 1 1 d . . . H22D H 0.3835 0.6313 0.7612 0.122 Uiso 1 1 d R . . C224 C 0.4163(6) 0.6085(5) 0.6876(3) 0.106(2) Uani 1 1 d . . . H22E H 0.3655 0.5524 0.6849 0.127 Uiso 1 1 d R . . C225 C 0.4761(6) 0.6403(4) 0.6464(3) 0.101(2) Uani 1 1 d . . . H22F H 0.4670 0.6067 0.6149 0.121 Uiso 1 1 d R . . C226 C 0.5502(5) 0.7221(4) 0.6502(2) 0.0814(15) Uani 1 1 d . . . H22G H 0.5939 0.7443 0.6214 0.098 Uiso 1 1 d R . . C23 C 0.8746(4) 0.9652(3) 0.72194(15) 0.0521(10) Uani 1 1 d . . . H23A H 0.9681 0.9648 0.7335 0.062 Uiso 1 1 d R . . H23B H 0.8271 0.9929 0.7483 0.062 Uiso 1 1 d R . . C231 C 0.8564(4) 1.0244(3) 0.67523(15) 0.0496(9) Uani 1 1 d . . . C232 C 0.7390(4) 1.0741(3) 0.66400(17) 0.0585(11) Uani 1 1 d . . . H23C H 0.6671 1.0691 0.6859 0.070 Uiso 1 1 d R . . C233 C 0.7243(5) 1.1303(3) 0.62206(18) 0.0695(13) Uani 1 1 d . . . H23D H 0.6431 1.1650 0.6151 0.083 Uiso 1 1 d R . . C234 C 0.8261(6) 1.1376(4) 0.59029(19) 0.0770(14) Uani 1 1 d . . . H23E H 0.8149 1.1756 0.5604 0.092 Uiso 1 1 d R . . C235 C 0.9426(5) 1.0897(4) 0.6011(2) 0.0762(14) Uani 1 1 d . . . H23F H 1.0142 1.0962 0.5793 0.091 Uiso 1 1 d R . . C236 C 0.9587(4) 1.0332(3) 0.64253(18) 0.0629(12) Uani 1 1 d . . . H23G H 1.0408 0.9994 0.6493 0.075 Uiso 1 1 d 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 I 0.1259(4) 0.0612(2) 0.0654(2) 0.00606(15) 0.01197(19) 0.0051(2) Cu 0.0360(3) 0.0617(3) 0.0552(3) -0.0007(2) 0.0022(2) 0.0043(2) P1 0.0329(5) 0.0615(6) 0.0551(5) -0.0001(5) 0.0035(4) 0.0024(5) P2 0.0313(6) 0.0543(6) 0.0557(6) 0.0033(4) 0.0038(4) 0.0016(5) C11 0.028(2) 0.083(3) 0.087(3) -0.012(3) -0.001(2) 0.008(2) C111 0.020(2) 0.077(3) 0.104(4) -0.011(3) 0.002(2) 0.008(2) C112 0.047(3) 0.095(4) 0.101(4) -0.017(3) -0.021(3) 0.020(3) C113 0.059(4) 0.127(6) 0.122(5) -0.037(5) -0.035(4) 0.033(4) C114 0.034(3) 0.109(6) 0.196(9) -0.049(6) -0.022(4) 0.008(3) C115 0.041(4) 0.095(5) 0.197(8) -0.008(5) 0.024(4) -0.009(3) C116 0.034(3) 0.104(4) 0.127(5) -0.016(4) 0.021(3) -0.002(3) C12 0.067(3) 0.068(3) 0.067(3) -0.002(2) 0.014(2) -0.008(2) C121 0.063(3) 0.059(3) 0.063(3) -0.010(2) 0.009(2) -0.003(2) C126 0.107(5) 0.083(4) 0.062(3) -0.005(2) 0.011(3) 0.019(3) C125 0.168(8) 0.091(4) 0.072(3) -0.001(3) 0.040(4) 0.011(5) C124 0.112(6) 0.122(6) 0.127(6) 0.001(5) 0.056(5) 0.021(5) C123 0.099(6) 0.128(6) 0.134(6) -0.023(5) 0.013(5) 0.036(5) C122 0.089(4) 0.106(4) 0.085(4) -0.019(3) -0.003(3) 0.035(4) C13 0.041(3) 0.078(3) 0.061(2) 0.007(2) 0.005(2) 0.006(2) C131 0.049(3) 0.081(3) 0.057(2) 0.003(2) 0.000(2) 0.014(2) C136 0.070(4) 0.150(6) 0.092(4) -0.046(4) -0.021(3) 0.037(4) C135 0.075(5) 0.184(8) 0.139(6) -0.061(6) -0.050(4) 0.037(5) C134 0.047(4) 0.175(7) 0.114(5) -0.018(5) -0.016(3) 0.030(4) C133 0.055(4) 0.155(6) 0.094(4) -0.014(4) 0.000(3) 0.035(4) C132 0.049(3) 0.099(4) 0.082(3) -0.011(3) 0.001(2) 0.012(3) C21 0.056(3) 0.072(3) 0.058(2) 0.010(2) 0.014(2) 0.000(2) C211 0.065(3) 0.064(3) 0.051(2) 0.009(2) 0.003(2) -0.005(2) C212 0.132(6) 0.102(4) 0.076(4) -0.019(3) -0.029(4) 0.016(4) C213 0.218(11) 0.108(6) 0.104(5) -0.014(5) -0.069(7) -0.011(6) C214 0.115(6) 0.143(7) 0.098(5) 0.032(5) -0.053(5) -0.042(5) C215 0.074(4) 0.172(7) 0.101(5) 0.005(5) -0.017(4) 0.015(5) C216 0.066(4) 0.110(5) 0.085(3) -0.021(3) -0.017(3) 0.012(3) C22 0.036(2) 0.065(3) 0.085(3) 0.003(2) 0.005(2) 0.007(2) C221 0.026(2) 0.065(3) 0.102(4) 0.009(3) -0.009(2) 0.007(2) C222 0.048(3) 0.086(4) 0.120(4) 0.024(3) 0.014(3) 0.005(3) C223 0.054(4) 0.095(5) 0.157(6) 0.042(4) 0.016(4) 0.004(3) C224 0.064(4) 0.075(4) 0.175(8) 0.027(5) -0.015(5) -0.004(3) C225 0.072(4) 0.086(4) 0.138(6) -0.004(4) -0.031(4) -0.005(3) C226 0.047(3) 0.085(4) 0.110(4) 0.001(3) -0.013(3) 0.003(3) C23 0.043(2) 0.055(2) 0.058(2) -0.0009(18) 0.0038(18) 0.0024(19) C231 0.040(2) 0.049(2) 0.058(2) -0.0047(17) -0.0023(19) 0.0002(19) C232 0.044(3) 0.062(3) 0.070(3) -0.004(2) 0.009(2) 0.009(2) C233 0.063(3) 0.064(3) 0.080(3) 0.005(2) -0.003(3) 0.023(2) C234 0.086(4) 0.074(3) 0.071(3) 0.016(2) 0.005(3) 0.007(3) C235 0.062(3) 0.087(4) 0.081(3) 0.022(3) 0.016(3) -0.002(3) C236 0.033(2) 0.076(3) 0.079(3) 0.008(2) 0.004(2) 0.001(2) _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 I Cu 2.5865(8) . ? Cu P2 2.2336(12) . ? Cu P1 2.2391(13) . ? P1 C13 1.841(4) . ? P1 C12 1.839(5) . ? P1 C11 1.848(4) . ? P2 C21 1.836(4) . ? P2 C23 1.838(4) . ? P2 C22 1.839(4) . ? C11 C111 1.504(6) . ? C111 C116 1.374(8) . ? C111 C112 1.382(7) . ? C112 C113 1.376(8) . ? C113 C114 1.341(10) . ? C114 C115 1.367(10) . ? C115 C116 1.410(9) . ? C12 C121 1.499(6) . ? C121 C126 1.357(6) . ? C121 C122 1.376(7) . ? C126 C125 1.404(8) . ? C125 C124 1.367(10) . ? C124 C123 1.343(10) . ? C123 C122 1.373(9) . ? C13 C131 1.513(6) . ? C131 C136 1.356(7) . ? C131 C132 1.372(6) . ? C136 C135 1.413(8) . ? C135 C134 1.343(9) . ? C134 C133 1.352(9) . ? C133 C132 1.383(7) . ? C21 C211 1.500(6) . ? C211 C216 1.356(7) . ? C211 C212 1.368(7) . ? C212 C213 1.376(11) . ? C213 C214 1.351(12) . ? C214 C215 1.378(10) . ? C215 C216 1.383(8) . ? C22 C221 1.501(6) . ? C221 C226 1.378(7) . ? C221 C222 1.390(7) . ? C222 C223 1.391(8) . ? C223 C224 1.357(9) . ? C224 C225 1.361(9) . ? C225 C226 1.400(8) . ? C23 C231 1.499(6) . ? C231 C232 1.390(6) . ? C231 C236 1.396(6) . ? C232 C233 1.371(6) . ? C233 C234 1.374(7) . ? C234 C235 1.367(7) . ? C235 C236 1.364(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 P2 Cu P1 139.78(5) . . ? P2 Cu I 115.07(4) . . ? P1 Cu I 105.11(4) . . ? C13 P1 C12 104.2(2) . . ? C13 P1 C11 101.9(2) . . ? C12 P1 C11 103.0(2) . . ? C13 P1 Cu 122.24(14) . . ? C12 P1 Cu 111.79(15) . . ? C11 P1 Cu 111.63(16) . . ? C21 P2 C23 101.2(2) . . ? C21 P2 C22 101.4(2) . . ? C23 P2 C22 102.0(2) . . ? C21 P2 Cu 114.47(16) . . ? C23 P2 Cu 122.66(14) . . ? C22 P2 Cu 112.34(16) . . ? C111 C11 P1 113.5(3) . . ? C116 C111 C112 118.1(5) . . ? C116 C111 C11 121.9(5) . . ? C112 C111 C11 119.9(5) . . ? C113 C112 C111 120.7(6) . . ? C114 C113 C112 120.7(8) . . ? C113 C114 C115 121.0(7) . . ? C114 C115 C116 118.4(7) . . ? C111 C116 C115 120.9(7) . . ? C121 C12 P1 118.2(3) . . ? C126 C121 C122 118.0(5) . . ? C126 C121 C12 123.2(5) . . ? C122 C121 C12 118.7(5) . . ? C121 C126 C125 121.1(6) . . ? C124 C125 C126 118.7(6) . . ? C123 C124 C125 120.8(7) . . ? C124 C123 C122 119.9(7) . . ? C123 C122 C121 121.4(6) . . ? C131 C13 P1 112.2(3) . . ? C136 C131 C132 117.6(5) . . ? C136 C131 C13 121.5(4) . . ? C132 C131 C13 120.9(4) . . ? C131 C136 C135 121.1(6) . . ? C134 C135 C136 119.6(6) . . ? C135 C134 C133 120.1(6) . . ? C134 C133 C132 120.2(6) . . ? C131 C132 C133 121.4(5) . . ? C211 C21 P2 113.8(3) . . ? C216 C211 C212 118.3(5) . . ? C216 C211 C21 122.1(4) . . ? C212 C211 C21 119.6(5) . . ? C211 C212 C213 120.8(7) . . ? C214 C213 C212 120.9(7) . . ? C213 C214 C215 118.8(7) . . ? C214 C215 C216 119.7(7) . . ? C211 C216 C215 121.4(6) . . ? C221 C22 P2 113.3(3) . . ? C226 C221 C222 119.4(5) . . ? C226 C221 C22 120.0(5) . . ? C222 C221 C22 120.6(5) . . ? C221 C222 C223 120.0(6) . . ? C224 C223 C222 119.8(7) . . ? C223 C224 C225 121.3(7) . . ? C224 C225 C226 119.8(7) . . ? C221 C226 C225 119.8(6) . . ? C231 C23 P2 115.3(3) . . ? C232 C231 C236 118.1(4) . . ? C232 C231 C23 121.1(4) . . ? C236 C231 C23 120.8(4) . . ? C233 C232 C231 120.9(4) . . ? C232 C233 C234 120.0(4) . . ? C235 C234 C233 119.7(5) . . ? C236 C235 C234 121.1(5) . . ? C235 C236 C231 120.2(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.421 _refine_diff_density_min -1.194 _refine_diff_density_rms 0.080 #====END data_cup2br _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H42 Br Cu P2' _chemical_formula_sum 'C42 H42 Br Cu P2' _chemical_formula_weight 752.15 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' 'P' 'P' 0.1023 0.0942 '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' 'Br' 'Br' -0.2901 2.4595 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 22.7747(4) _cell_length_b 14.4082(2) _cell_length_c 23.4308(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.9860(10) _cell_angle_gamma 90.00 _cell_volume 7547.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.14 _cell_measurement_theta_max 27.52 _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 1.750 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4462 _exptl_absorpt_correction_T_max 0.5412 _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'Siemens SMART CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43932 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 27.52 _reflns_number_total 16605 _reflns_number_gt 11972 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XPMA (Zsolnai, 1994)' _computing_publication_material 'SHELXL-97 (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^)+(0.0275P)^2^+5.1594P] 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_number_reflns 16605 _refine_ls_number_parameters 829 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0938 _refine_ls_wR_factor_gt 0.0776 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.002 _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 Cu2 Cu 0.339384(14) 0.23570(2) 0.353012(13) 0.04842(8) Uani 1 1 d . . . Br2 Br 0.316260(17) 0.39430(2) 0.326605(15) 0.07494(11) Uani 1 1 d . . . P32 P 0.40524(3) 0.23788(5) 0.43787(3) 0.04704(15) Uani 1 1 d . . . P42 P 0.28696(3) 0.13403(5) 0.29110(3) 0.04523(15) Uani 1 1 d . . . C31 C 0.46454(13) 0.1504(2) 0.45409(12) 0.0556(7) Uani 1 1 d . . . H31A H 0.4915 0.1675 0.4898 0.067 Uiso 1 1 calc R . . H31B H 0.4467 0.0911 0.4606 0.067 Uiso 1 1 calc R . . C311 C 0.50021(13) 0.1392(2) 0.40634(13) 0.0588(7) Uani 1 1 d . . . C312 C 0.55737(15) 0.1747(3) 0.41213(17) 0.0820(10) Uani 1 1 d . . . H31C H 0.5746 0.2056 0.4461 0.098 Uiso 1 1 calc R . . C313 C 0.58937(19) 0.1646(4) 0.3677(2) 0.1103(15) Uani 1 1 d . . . H31D H 0.6277 0.1892 0.3718 0.132 Uiso 1 1 calc R . . C314 C 0.5647(2) 0.1187(4) 0.3182(2) 0.1146(17) Uani 1 1 d . . . H31E H 0.5862 0.1125 0.2884 0.138 Uiso 1 1 calc R . . C315 C 0.5086(2) 0.0817(3) 0.31178(18) 0.1027(13) Uani 1 1 d . . . H31F H 0.4922 0.0494 0.2782 0.123 Uiso 1 1 calc R . . C316 C 0.47639(17) 0.0928(2) 0.35594(15) 0.0773(9) Uani 1 1 d . . . H31G H 0.4380 0.0684 0.3514 0.093 Uiso 1 1 calc R . . C32 C 0.44560(14) 0.34973(19) 0.44902(12) 0.0601(7) Uani 1 1 d . . . H32A H 0.4750 0.3504 0.4240 0.072 Uiso 1 1 calc R . . H32G H 0.4171 0.3988 0.4357 0.072 Uiso 1 1 calc R . . C321 C 0.47747(14) 0.37412(19) 0.50983(13) 0.0613(8) Uani 1 1 d . . . C322 C 0.53775(16) 0.3604(2) 0.52808(16) 0.0790(10) Uani 1 1 d . . . H32B H 0.5600 0.3341 0.5028 0.095 Uiso 1 1 calc R . . C323 C 0.5661(2) 0.3854(3) 0.5841(2) 0.1029(14) Uani 1 1 d . . . H32C H 0.6070 0.3758 0.5959 0.124 Uiso 1 1 calc R . . C324 C 0.5341(3) 0.4238(3) 0.62161(18) 0.1040(15) Uani 1 1 d . . . H32D H 0.5531 0.4400 0.6590 0.125 Uiso 1 1 calc R . . C325 C 0.4749(2) 0.4384(3) 0.60433(17) 0.1002(13) Uani 1 1 d . . . H32E H 0.4530 0.4650 0.6299 0.120 Uiso 1 1 calc R . . C326 C 0.44649(18) 0.4141(2) 0.54898(15) 0.0799(10) Uani 1 1 d . . . H32F H 0.4056 0.4247 0.5377 0.096 Uiso 1 1 calc R . . C33 C 0.36940(13) 0.2297(2) 0.50185(12) 0.0581(7) Uani 1 1 d . . . H33A H 0.4004 0.2274 0.5365 0.070 Uiso 1 1 calc R . . H33B H 0.3462 0.2856 0.5040 0.070 Uiso 1 1 calc R . . C331 C 0.32905(13) 0.1469(2) 0.50179(11) 0.0525(6) Uani 1 1 d . . . C332 C 0.34566(15) 0.0708(2) 0.53734(13) 0.0688(8) Uani 1 1 d . . . H33G H 0.3835 0.0684 0.5607 0.083 Uiso 1 1 calc R . . C333 C 0.30562(19) -0.0021(2) 0.53811(16) 0.0835(11) Uani 1 1 d . . . H33F H 0.3168 -0.0528 0.5623 0.100 Uiso 1 1 calc R . . C334 C 0.24988(18) 0.0004(3) 0.50356(17) 0.0839(10) Uani 1 1 d . . . H33E H 0.2232 -0.0482 0.5045 0.101 Uiso 1 1 calc R . . C335 C 0.23362(15) 0.0744(3) 0.46783(16) 0.0768(9) Uani 1 1 d . . . H33D H 0.1960 0.0759 0.4440 0.092 Uiso 1 1 calc R . . C336 C 0.27254(13) 0.1469(2) 0.46693(13) 0.0635(8) Uani 1 1 d . . . H33C H 0.2608 0.1970 0.4424 0.076 Uiso 1 1 calc R . . C41 C 0.21120(12) 0.1743(2) 0.25850(11) 0.0561(7) Uani 1 1 d . . . H41A H 0.2141 0.2353 0.2417 0.067 Uiso 1 1 calc R . . H41B H 0.1943 0.1325 0.2272 0.067 Uiso 1 1 calc R . . C411 C 0.16944(12) 0.1795(2) 0.30130(12) 0.0551(7) Uani 1 1 d . . . C412 C 0.17085(14) 0.2547(2) 0.33815(13) 0.0646(8) Uani 1 1 d . . . H41F H 0.1979 0.3027 0.3369 0.077 Uiso 1 1 calc R . . C413 C 0.13163(17) 0.2586(3) 0.37716(15) 0.0846(11) Uani 1 1 d . . . H41E H 0.1323 0.3095 0.4017 0.101 Uiso 1 1 calc R . . C414 C 0.09189(17) 0.1872(4) 0.37933(18) 0.0967(14) Uani 1 1 d . . . H41D H 0.0657 0.1899 0.4053 0.116 Uiso 1 1 calc R . . C145 C 0.09103(16) 0.1126(4) 0.34329(19) 0.0968(13) Uani 1 1 d . . . H14A H 0.0644 0.0642 0.3449 0.116 Uiso 1 1 calc R . . C416 C 0.12948(14) 0.1085(3) 0.30442(15) 0.0757(9) Uani 1 1 d . . . H41C H 0.1285 0.0573 0.2801 0.091 Uiso 1 1 calc R . . C42 C 0.31837(14) 0.11333(19) 0.22536(11) 0.0555(7) Uani 1 1 d . . . H42A H 0.3566 0.0822 0.2364 0.067 Uiso 1 1 calc R . . H42B H 0.2918 0.0721 0.1997 0.067 Uiso 1 1 calc R . . C421 C 0.32716(13) 0.20072(19) 0.19270(11) 0.0530(7) Uani 1 1 d . . . C422 C 0.38061(15) 0.2477(2) 0.20346(14) 0.0695(8) Uani 1 1 d . . . H42C H 0.4114 0.2263 0.2324 0.083 Uiso 1 1 calc R . . C423 C 0.3895(2) 0.3263(3) 0.17208(18) 0.0898(11) Uani 1 1 d . . . H42D H 0.4263 0.3566 0.1796 0.108 Uiso 1 1 calc R . . C424 C 0.3443(2) 0.3592(3) 0.13023(17) 0.0849(11) Uani 1 1 d . . . H42G H 0.3503 0.4119 0.1092 0.102 Uiso 1 1 calc R . . C425 C 0.29062(18) 0.3151(2) 0.11925(14) 0.0732(9) Uani 1 1 d . . . H42E H 0.2597 0.3383 0.0912 0.088 Uiso 1 1 calc R . . C426 C 0.28193(15) 0.2356(2) 0.14991(12) 0.0628(8) Uani 1 1 d . . . H42F H 0.2453 0.2052 0.1417 0.075 Uiso 1 1 calc R . . C43 C 0.27200(12) 0.01503(18) 0.31321(12) 0.0526(6) Uani 1 1 d . . . H43G H 0.2490 0.0183 0.3440 0.063 Uiso 1 1 calc R . . H43H H 0.2476 -0.0163 0.2804 0.063 Uiso 1 1 calc R . . C431 C 0.32698(13) -0.04209(18) 0.33411(12) 0.0533(7) Uani 1 1 d . . . C432 C 0.35340(16) -0.0925(2) 0.29567(14) 0.0700(9) Uani 1 1 d . . . H43A H 0.3368 -0.0914 0.2562 0.084 Uiso 1 1 calc R . . C433 C 0.40426(18) -0.1446(2) 0.31530(19) 0.0888(11) Uani 1 1 d . . . H43B H 0.4217 -0.1782 0.2890 0.107 Uiso 1 1 calc R . . C434 C 0.42916(19) -0.1468(3) 0.3740(2) 0.0962(13) Uani 1 1 d . . . H43C H 0.4637 -0.1811 0.3872 0.115 Uiso 1 1 calc R . . C435 C 0.40262(18) -0.0983(3) 0.41224(17) 0.0867(11) Uani 1 1 d . . . H43D H 0.4188 -0.1006 0.4518 0.104 Uiso 1 1 calc R . . C436 C 0.35226(15) -0.0462(2) 0.39285(13) 0.0647(8) Uani 1 1 d . . . H43E H 0.3349 -0.0131 0.4194 0.078 Uiso 1 1 calc R . . Cu1 Cu 0.796173(15) 0.35340(2) 0.352246(14) 0.05229(9) Uani 1 1 d . . . Br1 Br 0.755782(16) 0.19941(2) 0.336389(16) 0.07273(10) Uani 1 1 d . . . P11 P 0.86911(3) 0.32960(5) 0.42988(3) 0.04474(15) Uani 1 1 d . . . P12 P 0.76398(4) 0.46473(5) 0.28894(3) 0.05378(17) Uani 1 1 d . . . C11 C 0.83496(12) 0.2858(2) 0.48951(12) 0.0554(7) Uani 1 1 d . . . H11A H 0.8161 0.2265 0.4784 0.066 Uiso 1 1 calc R . . H11B H 0.8659 0.2761 0.5236 0.066 Uiso 1 1 calc R . . C111 C 0.78903(13) 0.3523(2) 0.50429(12) 0.0551(7) Uani 1 1 d . . . C112 C 0.73097(14) 0.3516(2) 0.47287(16) 0.0750(9) Uani 1 1 d . . . H11C H 0.7202 0.3104 0.4421 0.090 Uiso 1 1 calc R . . C113 C 0.68880(17) 0.4123(3) 0.4875(2) 0.0987(13) Uani 1 1 d . . . H11D H 0.6498 0.4119 0.4664 0.118 Uiso 1 1 calc R . . C114 C 0.7048(2) 0.4730(3) 0.5330(2) 0.0954(12) Uani 1 1 d . . . H11E H 0.6763 0.5130 0.5430 0.114 Uiso 1 1 calc R . . C115 C 0.76146(19) 0.4753(3) 0.56344(16) 0.0813(10) Uani 1 1 d . . . H11F H 0.7719 0.5171 0.5939 0.098 Uiso 1 1 calc R . . C116 C 0.80390(15) 0.4153(2) 0.54925(13) 0.0652(8) Uani 1 1 d . . . H11G H 0.8429 0.4174 0.5702 0.078 Uiso 1 1 calc R . . C12 C 0.91850(13) 0.23331(19) 0.41613(12) 0.0547(7) Uani 1 1 d . . . H12A H 0.8969 0.1954 0.3848 0.066 Uiso 1 1 calc R . . H12B H 0.9527 0.2596 0.4028 0.066 Uiso 1 1 calc R . . C121 C 0.94101(13) 0.17127(19) 0.46736(13) 0.0564(7) Uani 1 1 d . . . C122 C 0.91164(15) 0.0884(2) 0.47319(16) 0.0709(9) Uani 1 1 d . . . H12C H 0.8796 0.0704 0.4445 0.085 Uiso 1 1 calc R . . C123 C 0.92977(19) 0.0318(3) 0.5217(2) 0.0879(12) Uani 1 1 d . . . H12D H 0.9098 -0.0235 0.5254 0.105 Uiso 1 1 calc R . . C124 C 0.9768(2) 0.0580(3) 0.5635(2) 0.0964(14) Uani 1 1 d . . . H12E H 0.9892 0.0202 0.5957 0.116 Uiso 1 1 calc R . . C125 C 1.00577(17) 0.1392(3) 0.55854(17) 0.0889(11) Uani 1 1 d . . . H12F H 1.0375 0.1570 0.5876 0.107 Uiso 1 1 calc R . . C126 C 0.98848(14) 0.1954(2) 0.51060(15) 0.0698(8) Uani 1 1 d . . . H12G H 1.0091 0.2502 0.5074 0.084 Uiso 1 1 calc R . . C13 C 0.92084(12) 0.41834(19) 0.46767(11) 0.0513(6) Uani 1 1 d . . . H13A H 0.8979 0.4630 0.4853 0.062 Uiso 1 1 calc R . . H13B H 0.9487 0.3885 0.4987 0.062 Uiso 1 1 calc R . . C131 C 0.95603(12) 0.46963(18) 0.42948(11) 0.0491(6) Uani 1 1 d . . . C132 C 0.93500(14) 0.5524(2) 0.40375(13) 0.0610(7) Uani 1 1 d . . . H13C H 0.8986 0.5759 0.4098 0.073 Uiso 1 1 calc R . . C133 C 0.96727(18) 0.6010(2) 0.36903(15) 0.0770(9) Uani 1 1 d . . . H13D H 0.9527 0.6570 0.3523 0.092 Uiso 1 1 calc R . . C134 C 1.02058(18) 0.5670(3) 0.35918(15) 0.0794(10) Uani 1 1 d . . . H13E H 1.0422 0.5997 0.3359 0.095 Uiso 1 1 calc R . . C135 C 1.04190(15) 0.4846(3) 0.38377(15) 0.0741(9) Uani 1 1 d . . . H13F H 1.0777 0.4607 0.3766 0.089 Uiso 1 1 calc R . . C136 C 1.01043(13) 0.4365(2) 0.41930(13) 0.0602(7) Uani 1 1 d . . . H13G H 1.0259 0.3813 0.4366 0.072 Uiso 1 1 calc R . . C21 C 0.70692(16) 0.4340(2) 0.22453(13) 0.0728(9) Uani 1 1 d . . . H21A H 0.7104 0.4764 0.1932 0.087 Uiso 1 1 calc R . . H21B H 0.7152 0.3720 0.2120 0.087 Uiso 1 1 calc R . . C211 C 0.64435(16) 0.4367(2) 0.23461(14) 0.0707(9) Uani 1 1 d . . . C212 C 0.6080(2) 0.5133(3) 0.21786(19) 0.1104(16) Uani 1 1 d . . . H21G H 0.6226 0.5623 0.1988 0.133 Uiso 1 1 calc R . . C213 C 0.5510(3) 0.5180(4) 0.2289(3) 0.144(3) Uani 1 1 d . . . H21F H 0.5281 0.5709 0.2183 0.172 Uiso 1 1 calc R . . C214 C 0.5281(2) 0.4477(5) 0.2548(2) 0.128(2) Uani 1 1 d . . . H21E H 0.4890 0.4508 0.2609 0.154 Uiso 1 1 calc R . . C215 C 0.5627(2) 0.3708(4) 0.2723(2) 0.1111(14) Uani 1 1 d . . . H21D H 0.5473 0.3222 0.2910 0.133 Uiso 1 1 calc R . . C216 C 0.62073(17) 0.3659(3) 0.26204(17) 0.0847(10) Uani 1 1 d . . . H21C H 0.6439 0.3138 0.2740 0.102 Uiso 1 1 calc R . . C22 C 0.82687(14) 0.49963(19) 0.25489(13) 0.0627(8) Uani 1 1 d . . . H22A H 0.8121 0.5376 0.2210 0.075 Uiso 1 1 calc R . . H22B H 0.8547 0.5367 0.2821 0.075 Uiso 1 1 calc R . . C221 C 0.85891(15) 0.4164(2) 0.23696(12) 0.0611(8) Uani 1 1 d . . . C222 C 0.83845(19) 0.3711(3) 0.18468(14) 0.0844(11) Uani 1 1 d . . . H22C H 0.8051 0.3937 0.1593 0.101 Uiso 1 1 calc R . . C223 C 0.8671(2) 0.2928(3) 0.16989(19) 0.1051(14) Uani 1 1 d . . . H22D H 0.8521 0.2620 0.1353 0.126 Uiso 1 1 calc R . . C224 C 0.9173(3) 0.2605(3) 0.2057(2) 0.1140(17) Uani 1 1 d . . . H22E H 0.9371 0.2087 0.1950 0.137 Uiso 1 1 calc R . . C225 C 0.9386(2) 0.3044(3) 0.25745(18) 0.1014(13) Uani 1 1 d . . . H22F H 0.9725 0.2821 0.2821 0.122 Uiso 1 1 calc R . . C226 C 0.90932(17) 0.3820(2) 0.27277(15) 0.0781(10) Uani 1 1 d . . . H22G H 0.9239 0.4115 0.3079 0.094 Uiso 1 1 calc R . . C23 C 0.73233(14) 0.57389(19) 0.31021(13) 0.0624(8) Uani 1 1 d . . . H23A H 0.7242 0.6140 0.2764 0.075 Uiso 1 1 calc R . . H23G H 0.6943 0.5601 0.3212 0.075 Uiso 1 1 calc R . . C231 C 0.77008(13) 0.62698(19) 0.35915(13) 0.0574(7) Uani 1 1 d . . . C232 C 0.80341(15) 0.7019(2) 0.34740(14) 0.0694(8) Uani 1 1 d . . . H23F H 0.8051 0.7163 0.3091 0.083 Uiso 1 1 calc R . . C233 C 0.83428(17) 0.7558(2) 0.39184(17) 0.0828(10) Uani 1 1 d . . . H23E H 0.8561 0.8068 0.3832 0.099 Uiso 1 1 calc R . . C234 C 0.83301(18) 0.7345(3) 0.44860(18) 0.0893(12) Uani 1 1 d . . . H23D H 0.8536 0.7712 0.4785 0.107 Uiso 1 1 calc R . . C235 C 0.80148(19) 0.6596(3) 0.46089(16) 0.0903(11) Uani 1 1 d . . . H23C H 0.8012 0.6445 0.4994 0.108 Uiso 1 1 calc R . . C236 C 0.76976(16) 0.6053(2) 0.41672(14) 0.0741(9) Uani 1 1 d . . . H23B H 0.7482 0.5543 0.4257 0.089 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 Cu2 0.05240(18) 0.04848(18) 0.04285(16) -0.00199(14) 0.00526(13) 0.00224(14) Br2 0.0959(3) 0.04979(17) 0.0691(2) 0.00104(15) -0.00977(17) 0.01049(16) P32 0.0494(4) 0.0480(4) 0.0419(3) 0.0010(3) 0.0042(3) -0.0013(3) P42 0.0507(4) 0.0440(3) 0.0393(3) 0.0007(3) 0.0045(3) 0.0027(3) C31 0.0565(16) 0.0576(16) 0.0505(15) 0.0072(13) 0.0046(13) 0.0041(13) C311 0.0526(16) 0.0611(17) 0.0629(17) 0.0132(14) 0.0113(14) 0.0124(14) C312 0.057(2) 0.096(3) 0.093(3) 0.011(2) 0.0153(18) 0.0053(18) C313 0.068(3) 0.132(4) 0.140(4) 0.031(3) 0.044(3) 0.015(3) C314 0.112(4) 0.129(4) 0.122(4) 0.022(3) 0.073(3) 0.041(3) C315 0.121(4) 0.112(3) 0.083(3) -0.009(2) 0.040(3) 0.023(3) C316 0.079(2) 0.083(2) 0.073(2) -0.0065(18) 0.0235(18) 0.0036(19) C32 0.0671(19) 0.0515(16) 0.0579(16) 0.0070(13) 0.0027(14) -0.0078(14) C321 0.073(2) 0.0453(15) 0.0593(17) 0.0060(13) -0.0029(15) -0.0172(14) C322 0.070(2) 0.077(2) 0.085(2) 0.0013(19) 0.0018(18) -0.0189(18) C323 0.088(3) 0.091(3) 0.110(3) 0.006(3) -0.030(3) -0.024(2) C324 0.140(4) 0.088(3) 0.070(2) -0.002(2) -0.017(3) -0.039(3) C325 0.127(4) 0.089(3) 0.081(3) -0.027(2) 0.013(3) -0.036(3) C326 0.089(3) 0.067(2) 0.079(2) -0.0175(18) 0.0046(19) -0.0078(18) C33 0.0634(18) 0.0606(17) 0.0508(15) -0.0110(13) 0.0121(13) -0.0058(14) C331 0.0578(16) 0.0586(16) 0.0437(14) -0.0048(12) 0.0162(12) 0.0008(13) C332 0.072(2) 0.079(2) 0.0535(17) 0.0056(16) 0.0072(15) 0.0001(17) C333 0.116(3) 0.067(2) 0.072(2) 0.0145(17) 0.028(2) 0.000(2) C334 0.083(3) 0.083(3) 0.093(3) -0.011(2) 0.033(2) -0.022(2) C335 0.0560(19) 0.090(3) 0.086(2) -0.011(2) 0.0169(17) -0.0032(18) C336 0.0570(18) 0.0666(19) 0.0668(18) -0.0026(15) 0.0115(15) 0.0063(15) C41 0.0547(16) 0.0654(17) 0.0447(14) 0.0078(13) 0.0008(12) 0.0087(14) C411 0.0445(15) 0.0671(18) 0.0494(15) 0.0119(14) -0.0016(12) 0.0069(13) C412 0.0616(18) 0.0678(19) 0.0644(18) 0.0131(16) 0.0120(15) 0.0155(15) C413 0.086(3) 0.101(3) 0.069(2) 0.013(2) 0.0201(19) 0.039(2) C414 0.058(2) 0.154(4) 0.083(3) 0.041(3) 0.025(2) 0.027(3) C145 0.051(2) 0.145(4) 0.091(3) 0.033(3) 0.005(2) -0.013(2) C416 0.0569(19) 0.093(3) 0.071(2) 0.0103(18) -0.0034(16) -0.0070(18) C42 0.0701(19) 0.0500(15) 0.0472(14) -0.0040(12) 0.0134(13) 0.0057(14) C421 0.0680(18) 0.0506(15) 0.0442(14) -0.0071(12) 0.0201(13) 0.0050(14) C422 0.072(2) 0.074(2) 0.0643(19) -0.0030(16) 0.0166(16) 0.0008(17) C423 0.097(3) 0.086(3) 0.091(3) -0.004(2) 0.031(2) -0.028(2) C424 0.119(3) 0.065(2) 0.081(2) 0.0079(19) 0.045(2) -0.002(2) C425 0.095(3) 0.072(2) 0.0585(18) 0.0132(16) 0.0301(18) 0.024(2) C426 0.072(2) 0.0677(19) 0.0521(16) -0.0011(14) 0.0202(14) 0.0025(16) C43 0.0578(16) 0.0475(15) 0.0498(15) 0.0020(12) 0.0035(12) -0.0045(12) C431 0.0624(17) 0.0385(13) 0.0557(15) 0.0016(12) 0.0025(13) -0.0019(12) C432 0.091(2) 0.0481(17) 0.0668(19) -0.0080(14) 0.0055(17) 0.0048(16) C433 0.102(3) 0.054(2) 0.111(3) -0.013(2) 0.023(2) 0.0201(19) C434 0.088(3) 0.070(2) 0.121(3) 0.013(2) -0.004(3) 0.026(2) C435 0.093(3) 0.077(2) 0.080(2) 0.017(2) -0.008(2) 0.014(2) C436 0.077(2) 0.0572(18) 0.0557(17) 0.0077(14) 0.0024(15) 0.0035(15) Cu1 0.0582(2) 0.04529(18) 0.05193(18) 0.00320(14) 0.00690(15) -0.00104(15) Br1 0.0763(2) 0.05168(17) 0.0857(2) -0.01047(16) 0.00380(17) -0.01327(15) P11 0.0474(4) 0.0423(3) 0.0459(3) 0.0029(3) 0.0125(3) -0.0009(3) P12 0.0641(5) 0.0432(4) 0.0502(4) 0.0006(3) 0.0013(3) -0.0026(3) C11 0.0554(16) 0.0542(16) 0.0611(16) 0.0108(13) 0.0224(13) 0.0037(13) C111 0.0569(17) 0.0552(16) 0.0591(16) 0.0107(13) 0.0261(14) 0.0046(13) C112 0.0573(19) 0.083(2) 0.089(2) -0.0095(19) 0.0238(17) 0.0013(17) C113 0.055(2) 0.125(4) 0.119(3) 0.000(3) 0.026(2) 0.016(2) C114 0.093(3) 0.097(3) 0.108(3) 0.003(3) 0.052(3) 0.028(2) C115 0.105(3) 0.075(2) 0.074(2) -0.0031(18) 0.041(2) 0.010(2) C116 0.072(2) 0.071(2) 0.0577(17) 0.0057(15) 0.0246(15) 0.0062(16) C12 0.0574(16) 0.0509(15) 0.0596(16) -0.0035(13) 0.0209(13) 0.0028(13) C121 0.0571(17) 0.0495(15) 0.0689(18) 0.0038(14) 0.0282(15) 0.0127(13) C122 0.069(2) 0.0563(18) 0.095(2) 0.0020(17) 0.0343(18) 0.0097(15) C123 0.089(3) 0.064(2) 0.127(3) 0.031(2) 0.063(3) 0.017(2) C124 0.088(3) 0.105(3) 0.107(3) 0.048(3) 0.047(3) 0.040(3) C125 0.074(2) 0.111(3) 0.081(2) 0.020(2) 0.0135(19) 0.027(2) C126 0.0591(19) 0.070(2) 0.080(2) 0.0100(17) 0.0135(16) 0.0105(16) C13 0.0536(16) 0.0532(15) 0.0470(14) -0.0036(12) 0.0094(12) -0.0027(12) C131 0.0502(15) 0.0488(15) 0.0467(14) -0.0049(12) 0.0051(12) -0.0072(12) C132 0.0644(18) 0.0546(17) 0.0636(18) -0.0016(14) 0.0110(14) -0.0036(14) C133 0.095(3) 0.0599(19) 0.073(2) 0.0104(16) 0.0087(19) -0.0115(19) C134 0.095(3) 0.079(2) 0.069(2) 0.0017(18) 0.0276(19) -0.029(2) C135 0.067(2) 0.080(2) 0.081(2) -0.0078(19) 0.0298(18) -0.0139(18) C136 0.0561(17) 0.0584(17) 0.0660(18) -0.0007(14) 0.0119(14) -0.0050(14) C21 0.088(2) 0.0656(19) 0.0567(18) -0.0038(15) -0.0078(16) -0.0146(17) C211 0.077(2) 0.0581(19) 0.0625(18) -0.0104(15) -0.0221(16) -0.0043(16) C212 0.105(3) 0.075(3) 0.121(3) 0.002(2) -0.056(3) 0.006(2) C213 0.096(4) 0.106(4) 0.188(6) -0.054(4) -0.078(4) 0.032(3) C214 0.069(3) 0.152(5) 0.147(5) -0.077(4) -0.023(3) 0.021(3) C215 0.087(3) 0.125(4) 0.118(4) -0.013(3) 0.013(3) -0.002(3) C216 0.072(2) 0.081(2) 0.096(3) -0.005(2) 0.002(2) 0.0071(19) C22 0.078(2) 0.0473(16) 0.0616(17) 0.0105(13) 0.0102(15) -0.0044(14) C221 0.084(2) 0.0544(17) 0.0480(15) 0.0071(13) 0.0202(15) -0.0067(15) C222 0.105(3) 0.099(3) 0.0526(18) -0.0012(19) 0.0230(18) -0.004(2) C223 0.153(4) 0.100(3) 0.074(3) -0.025(2) 0.052(3) -0.013(3) C224 0.182(5) 0.077(3) 0.101(3) -0.001(3) 0.072(4) 0.023(3) C225 0.129(4) 0.099(3) 0.082(3) 0.013(2) 0.035(3) 0.042(3) C226 0.098(3) 0.076(2) 0.0612(19) 0.0001(17) 0.0188(19) 0.014(2) C23 0.0640(18) 0.0493(16) 0.0673(18) -0.0026(14) -0.0041(15) 0.0056(14) C231 0.0619(18) 0.0448(15) 0.0622(17) -0.0046(13) 0.0035(14) 0.0082(13) C232 0.084(2) 0.0499(17) 0.0678(19) 0.0067(15) -0.0027(16) -0.0022(16) C233 0.089(3) 0.0527(19) 0.096(3) -0.0007(18) -0.007(2) -0.0085(17) C234 0.101(3) 0.069(2) 0.086(3) -0.028(2) -0.012(2) 0.004(2) C235 0.111(3) 0.098(3) 0.060(2) -0.018(2) 0.013(2) -0.001(2) C236 0.085(2) 0.070(2) 0.069(2) -0.0036(17) 0.0177(18) -0.0058(18) _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 Cu2 P42 2.2396(7) . ? Cu2 P32 2.2509(7) . ? Cu2 Br2 2.3995(4) . ? P32 C31 1.834(3) . ? P32 C33 1.842(3) . ? P32 C32 1.849(3) . ? P42 C43 1.841(3) . ? P42 C42 1.842(3) . ? P42 C41 1.842(3) . ? C31 C311 1.511(4) . ? C311 C316 1.376(4) . ? C311 C312 1.381(4) . ? C312 C313 1.388(6) . ? C313 C314 1.360(7) . ? C314 C315 1.366(6) . ? C315 C316 1.387(5) . ? C32 C321 1.512(4) . ? C321 C322 1.372(5) . ? C321 C326 1.385(5) . ? C322 C323 1.396(5) . ? C323 C324 1.360(6) . ? C324 C325 1.350(6) . ? C325 C326 1.380(5) . ? C33 C331 1.506(4) . ? C331 C332 1.384(4) . ? C331 C336 1.387(4) . ? C332 C333 1.394(5) . ? C333 C334 1.370(5) . ? C334 C335 1.363(5) . ? C335 C336 1.372(5) . ? C41 C411 1.510(4) . ? C411 C416 1.380(4) . ? C411 C412 1.383(4) . ? C412 C413 1.396(5) . ? C413 C414 1.377(6) . ? C414 C145 1.365(6) . ? C145 C416 1.380(5) . ? C42 C421 1.507(4) . ? C421 C422 1.373(4) . ? C421 C426 1.387(4) . ? C422 C423 1.387(5) . ? C423 C424 1.364(5) . ? C424 C425 1.359(5) . ? C425 C426 1.387(4) . ? C43 C431 1.500(4) . ? C431 C432 1.381(4) . ? C431 C436 1.388(4) . ? C432 C433 1.383(5) . ? C433 C434 1.384(5) . ? C434 C435 1.366(5) . ? C435 C436 1.374(5) . ? Cu1 P12 2.2127(8) . ? Cu1 P11 2.2436(7) . ? Cu1 Br1 2.4034(4) . ? P11 C11 1.836(3) . ? P11 C13 1.847(3) . ? P11 C12 1.853(3) . ? P12 C22 1.837(3) . ? P12 C23 1.838(3) . ? P12 C21 1.848(3) . ? C11 C111 1.507(4) . ? C111 C116 1.383(4) . ? C111 C112 1.386(4) . ? C112 C113 1.390(5) . ? C113 C114 1.374(6) . ? C114 C115 1.350(5) . ? C115 C116 1.383(4) . ? C12 C121 1.506(4) . ? C121 C126 1.378(4) . ? C121 C122 1.388(4) . ? C122 C123 1.396(5) . ? C123 C124 1.360(6) . ? C124 C125 1.359(6) . ? C125 C126 1.380(5) . ? C13 C131 1.504(4) . ? C131 C132 1.380(4) . ? C131 C136 1.390(4) . ? C132 C133 1.386(4) . ? C133 C134 1.370(5) . ? C134 C135 1.367(5) . ? C135 C136 1.384(4) . ? C21 C211 1.489(5) . ? C211 C216 1.369(5) . ? C211 C212 1.390(5) . ? C212 C213 1.373(7) . ? C213 C214 1.337(8) . ? C214 C215 1.377(7) . ? C215 C216 1.389(6) . ? C22 C221 1.505(4) . ? C221 C226 1.378(5) . ? C221 C222 1.388(4) . ? C222 C223 1.379(6) . ? C223 C224 1.365(6) . ? C224 C225 1.372(6) . ? C225 C226 1.384(5) . ? C23 C231 1.505(4) . ? C231 C232 1.377(4) . ? C231 C236 1.386(4) . ? C232 C233 1.379(4) . ? C233 C234 1.371(5) . ? C234 C235 1.358(5) . ? C235 C236 1.385(5) . ? 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 P42 Cu2 P32 139.86(3) . . ? P42 Cu2 Br2 113.09(2) . . ? P32 Cu2 Br2 106.92(2) . . ? C31 P32 C33 102.15(13) . . ? C31 P32 C32 104.08(14) . . ? C33 P32 C32 103.06(13) . . ? C31 P32 Cu2 120.93(9) . . ? C33 P32 Cu2 113.20(10) . . ? C32 P32 Cu2 111.51(9) . . ? C43 P42 C42 101.92(13) . . ? C43 P42 C41 101.59(13) . . ? C42 P42 C41 100.74(13) . . ? C43 P42 Cu2 122.09(9) . . ? C42 P42 Cu2 113.79(10) . . ? C41 P42 Cu2 113.85(10) . . ? C311 C31 P32 113.47(18) . . ? C316 C311 C312 118.3(3) . . ? C316 C311 C31 120.5(3) . . ? C312 C311 C31 121.2(3) . . ? C311 C312 C313 120.5(4) . . ? C314 C313 C312 120.1(4) . . ? C313 C314 C315 120.5(4) . . ? C314 C315 C316 119.3(4) . . ? C311 C316 C315 121.2(4) . . ? C321 C32 P32 118.17(19) . . ? C322 C321 C326 117.3(3) . . ? C322 C321 C32 122.2(3) . . ? C326 C321 C32 120.5(3) . . ? C321 C322 C323 120.8(4) . . ? C324 C323 C322 120.3(4) . . ? C325 C324 C323 119.8(4) . . ? C324 C325 C326 120.3(4) . . ? C325 C326 C321 121.5(4) . . ? C331 C33 P32 114.48(18) . . ? C332 C331 C336 118.1(3) . . ? C332 C331 C33 122.0(3) . . ? C336 C331 C33 119.9(3) . . ? C331 C332 C333 120.0(3) . . ? C334 C333 C332 120.5(3) . . ? C335 C334 C333 119.7(3) . . ? C334 C335 C336 120.3(3) . . ? C335 C336 C331 121.4(3) . . ? C411 C41 P42 113.51(18) . . ? C416 C411 C412 119.0(3) . . ? C416 C411 C41 120.2(3) . . ? C412 C411 C41 120.7(3) . . ? C411 C412 C413 119.9(3) . . ? C414 C413 C412 120.1(4) . . ? C145 C414 C413 119.8(4) . . ? C414 C145 C416 120.4(4) . . ? C145 C416 C411 120.7(4) . . ? C421 C42 P42 113.57(18) . . ? C422 C421 C426 117.7(3) . . ? C422 C421 C42 121.1(3) . . ? C426 C421 C42 121.2(3) . . ? C421 C422 C423 121.3(3) . . ? C424 C423 C422 119.9(4) . . ? C425 C424 C423 120.2(3) . . ? C424 C425 C426 120.0(3) . . ? C425 C426 C421 120.9(3) . . ? C431 C43 P42 114.51(19) . . ? C432 C431 C436 118.3(3) . . ? C432 C431 C43 121.0(3) . . ? C436 C431 C43 120.6(3) . . ? C431 C432 C433 120.6(3) . . ? C432 C433 C434 120.1(4) . . ? C435 C434 C433 119.4(4) . . ? C434 C435 C436 120.6(3) . . ? C435 C436 C431 120.9(3) . . ? P12 Cu1 P11 138.92(3) . . ? P12 Cu1 Br1 119.83(2) . . ? P11 Cu1 Br1 100.76(2) . . ? C11 P11 C13 101.37(13) . . ? C11 P11 C12 103.56(12) . . ? C13 P11 C12 104.40(13) . . ? C11 P11 Cu1 108.30(10) . . ? C13 P11 Cu1 126.09(9) . . ? C12 P11 Cu1 110.72(9) . . ? C22 P12 C23 105.19(14) . . ? C22 P12 C21 101.30(15) . . ? C23 P12 C21 100.11(15) . . ? C22 P12 Cu1 107.66(10) . . ? C23 P12 Cu1 122.39(10) . . ? C21 P12 Cu1 117.72(11) . . ? C111 C11 P11 111.70(19) . . ? C116 C111 C112 118.7(3) . . ? C116 C111 C11 120.8(3) . . ? C112 C111 C11 120.5(3) . . ? C111 C112 C113 119.9(4) . . ? C114 C113 C112 119.9(4) . . ? C115 C114 C113 120.7(4) . . ? C114 C115 C116 120.0(4) . . ? C115 C116 C111 120.8(3) . . ? C121 C12 P11 115.57(19) . . ? C126 C121 C122 118.0(3) . . ? C126 C121 C12 122.5(3) . . ? C122 C121 C12 119.5(3) . . ? C121 C122 C123 120.6(4) . . ? C124 C123 C122 119.6(4) . . ? C125 C124 C123 120.4(4) . . ? C124 C125 C126 120.5(4) . . ? C121 C126 C125 120.9(3) . . ? C131 C13 P11 114.75(18) . . ? C132 C131 C136 117.9(3) . . ? C132 C131 C13 120.3(3) . . ? C136 C131 C13 121.8(3) . . ? C131 C132 C133 121.0(3) . . ? C134 C133 C132 120.3(3) . . ? C135 C134 C133 119.7(3) . . ? C134 C135 C136 120.3(3) . . ? C135 C136 C131 120.8(3) . . ? C211 C21 P12 114.2(2) . . ? C216 C211 C212 117.2(4) . . ? C216 C211 C21 121.9(3) . . ? C212 C211 C21 120.8(4) . . ? C213 C212 C211 121.3(5) . . ? C214 C213 C212 120.9(5) . . ? C213 C214 C215 119.6(5) . . ? C214 C215 C216 119.9(5) . . ? C211 C216 C215 121.0(4) . . ? C221 C22 P12 111.26(19) . . ? C226 C221 C222 118.0(3) . . ? C226 C221 C22 120.6(3) . . ? C222 C221 C22 121.5(3) . . ? C223 C222 C221 120.7(4) . . ? C224 C223 C222 120.4(4) . . ? C223 C224 C225 120.0(4) . . ? C224 C225 C226 119.7(4) . . ? C221 C226 C225 121.3(4) . . ? C231 C23 P12 116.4(2) . . ? C232 C231 C236 118.4(3) . . ? C232 C231 C23 120.2(3) . . ? C236 C231 C23 121.3(3) . . ? C231 C232 C233 120.7(3) . . ? C234 C233 C232 120.3(3) . . ? C235 C234 C233 119.6(3) . . ? C234 C235 C236 120.8(4) . . ? C235 C236 C231 120.1(3) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.590 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.047 #====END data_cup2cl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H42 Cl Cu P2' _chemical_formula_sum 'C42 H42 Cl Cu P2' _chemical_formula_weight 707.69 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' 'P' 'P' 0.1023 0.0942 '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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monolcinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.4813(3) _cell_length_b 12.21130(10) _cell_length_c 25.1532(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.5710(10) _cell_angle_gamma 90.00 _cell_volume 7374.49(14) _cell_formula_units_Z 8 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 6837 _cell_measurement_theta_min 1.72 _cell_measurement_theta_max 27.44 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5924 _exptl_absorpt_correction_T_max 0.7354 _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'Siemens SMART CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21077 _diffrn_reflns_av_R_equivalents 0.0153 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.44 _reflns_number_total 7955 _reflns_number_gt 6837 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XPMA (Zsolnai, 1994)' _computing_publication_material 'SHELXL-97 (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^)+(0.0431P)^2^+5.4436P] 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_number_reflns 7955 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Cu Cu 0.176428(9) 0.335121(17) 0.130783(9) 0.04177(7) Uani 1 1 d . . . Cl Cl 0.19735(3) 0.15978(5) 0.15718(3) 0.07698(19) Uani 1 1 d . . . P1 P 0.124265(18) 0.32768(3) 0.039341(18) 0.03693(10) Uani 1 1 d . . . P2 P 0.216076(17) 0.46562(4) 0.193188(18) 0.03769(10) Uani 1 1 d . . . C11 C 0.08057(8) 0.20372(15) 0.02039(8) 0.0468(4) Uani 1 1 d . . . H11A H 0.0557 0.2120 -0.0182 0.056 Uiso 1 1 calc R . . H11G H 0.1047 0.1420 0.0210 0.056 Uiso 1 1 calc R . . C111 C 0.04559(7) 0.17493(15) 0.05667(8) 0.0448(4) Uani 1 1 d . . . C112 C 0.01879(10) 0.24980(19) 0.07953(11) 0.0694(6) Uani 1 1 d . . . H11B H 0.0222 0.3241 0.0732 0.083 Uiso 1 1 calc R . . C113 C -0.01327(11) 0.2171(2) 0.11194(13) 0.0786(7) Uani 1 1 d . . . H11C H -0.0308 0.2695 0.1270 0.094 Uiso 1 1 calc R . . C114 C -0.01919(11) 0.1090(2) 0.12171(12) 0.0787(7) Uani 1 1 d . . . H11D H -0.0408 0.0871 0.1431 0.094 Uiso 1 1 calc R . . C115 C 0.00702(17) 0.0335(2) 0.09974(18) 0.1170(14) Uani 1 1 d . . . H11E H 0.0035 -0.0405 0.1064 0.140 Uiso 1 1 calc R . . C116 C 0.03901(14) 0.0662(2) 0.06743(15) 0.0948(10) Uani 1 1 d . . . H11F H 0.0565 0.0132 0.0527 0.114 Uiso 1 1 calc R . . C12 C 0.07917(8) 0.44447(15) 0.00457(8) 0.0488(4) Uani 1 1 d . . . H12A H 0.0511 0.4539 0.0225 0.059 Uiso 1 1 calc R . . H12G H 0.1019 0.5101 0.0121 0.059 Uiso 1 1 calc R . . C121 C 0.04976(8) 0.43701(16) -0.05825(8) 0.0483(4) Uani 1 1 d . . . C122 C 0.00076(8) 0.3778(2) -0.08085(9) 0.0634(6) Uani 1 1 d . . . H12B H -0.0150 0.3440 -0.0567 0.076 Uiso 1 1 calc R . . C123 C -0.02516(9) 0.3679(3) -0.13889(10) 0.0775(7) Uani 1 1 d . . . H12C H -0.0574 0.3262 -0.1532 0.093 Uiso 1 1 calc R . . C124 C -0.00310(10) 0.4200(3) -0.17520(10) 0.0780(7) Uani 1 1 d . . . H12D H -0.0205 0.4140 -0.2140 0.094 Uiso 1 1 calc R . . C125 C 0.04486(11) 0.4810(2) -0.15383(10) 0.0712(6) Uani 1 1 d . . . H12E H 0.0595 0.5170 -0.1783 0.085 Uiso 1 1 calc R . . C126 C 0.07141(9) 0.48876(18) -0.09596(9) 0.0575(5) Uani 1 1 d . . . H12F H 0.1041 0.5291 -0.0820 0.069 Uiso 1 1 calc R . . C13 C 0.16902(7) 0.30295(15) -0.00402(8) 0.0441(4) Uani 1 1 d . . . H13A H 0.1819 0.2277 0.0016 0.053 Uiso 1 1 calc R . . H13B H 0.1465 0.3110 -0.0434 0.053 Uiso 1 1 calc R . . C131 C 0.21919(7) 0.37727(15) 0.00813(7) 0.0420(4) Uani 1 1 d . . . C132 C 0.22734(9) 0.44281(18) -0.03397(9) 0.0555(5) Uani 1 1 d . . . H13C H 0.2006 0.4436 -0.0698 0.067 Uiso 1 1 calc R . . C133 C 0.27495(10) 0.5068(2) -0.02290(10) 0.0660(6) Uani 1 1 d . . . H13D H 0.2799 0.5496 -0.0515 0.079 Uiso 1 1 calc R . . C134 C 0.31483(9) 0.50742(19) 0.02989(10) 0.0610(5) Uani 1 1 d . . . H13E H 0.3464 0.5511 0.0372 0.073 Uiso 1 1 calc R . . C135 C 0.30764(8) 0.44243(17) 0.07219(9) 0.0514(4) Uani 1 1 d . . . H13F H 0.3344 0.4425 0.1080 0.062 Uiso 1 1 calc R . . C136 C 0.26052(7) 0.37737(16) 0.06105(8) 0.0451(4) Uani 1 1 d . . . H13G H 0.2565 0.3330 0.0895 0.054 Uiso 1 1 calc R . . C21 C 0.27767(7) 0.41915(16) 0.25200(7) 0.0454(4) Uani 1 1 d . . . H21A H 0.2875 0.4755 0.2809 0.054 Uiso 1 1 calc R . . H21B H 0.2676 0.3540 0.2685 0.054 Uiso 1 1 calc R . . C211 C 0.32834(7) 0.39369(15) 0.23571(8) 0.0452(4) Uani 1 1 d . . . C212 C 0.37350(8) 0.4647(2) 0.25080(11) 0.0648(6) Uani 1 1 d . . . H21C H 0.3721 0.5289 0.2701 0.078 Uiso 1 1 calc R . . C213 C 0.42075(9) 0.4406(3) 0.23725(13) 0.0805(7) Uani 1 1 d . . . H21D H 0.4505 0.4893 0.2472 0.097 Uiso 1 1 calc R . . C214 C 0.42402(10) 0.3454(2) 0.20927(12) 0.0773(7) Uani 1 1 d . . . H21E H 0.4560 0.3294 0.2007 0.093 Uiso 1 1 calc R . . C215 C 0.37952(9) 0.2737(2) 0.19406(10) 0.0658(6) Uani 1 1 d . . . H21F H 0.3815 0.2093 0.1751 0.079 Uiso 1 1 calc R . . C216 C 0.33176(8) 0.29766(16) 0.20697(8) 0.0506(4) Uani 1 1 d . . . H21G H 0.3019 0.2492 0.1964 0.061 Uiso 1 1 calc R . . C22 C 0.17121(8) 0.51458(15) 0.23285(8) 0.0471(4) Uani 1 1 d . . . H22A H 0.1907 0.5713 0.2590 0.057 Uiso 1 1 calc R . . H22B H 0.1377 0.5467 0.2067 0.057 Uiso 1 1 calc R . . C221 C 0.15536(7) 0.42377(16) 0.26509(8) 0.0468(4) Uani 1 1 d . . . C222 C 0.18465(9) 0.4087(2) 0.32229(9) 0.0599(5) Uani 1 1 d . . . H22C H 0.2132 0.4568 0.3408 0.072 Uiso 1 1 calc R . . C223 C 0.17188(12) 0.3233(2) 0.35180(12) 0.0762(7) Uani 1 1 d . . . H22D H 0.1919 0.3141 0.3899 0.091 Uiso 1 1 calc R . . C224 C 0.12976(13) 0.2520(2) 0.32496(15) 0.0871(9) Uani 1 1 d . . . H22E H 0.1214 0.1942 0.3448 0.104 Uiso 1 1 calc R . . C225 C 0.09974(12) 0.2659(2) 0.26837(15) 0.0854(8) Uani 1 1 d . . . H22F H 0.0709 0.2180 0.2504 0.102 Uiso 1 1 calc R . . C226 C 0.11252(10) 0.35125(19) 0.23833(11) 0.0641(6) Uani 1 1 d . . . H22G H 0.0924 0.3600 0.2002 0.077 Uiso 1 1 calc R . . C23 C 0.24187(7) 0.59442(15) 0.17201(8) 0.0466(4) Uani 1 1 d . . . H23A H 0.2559 0.6409 0.2050 0.056 Uiso 1 1 calc R . . H23B H 0.2730 0.5770 0.1595 0.056 Uiso 1 1 calc R . . C231 C 0.19979(7) 0.65874(13) 0.12604(8) 0.0427(4) Uani 1 1 d . . . C232 C 0.16274(8) 0.73026(16) 0.13867(9) 0.0529(4) Uani 1 1 d . . . H23C H 0.1634 0.7365 0.1757 0.063 Uiso 1 1 calc R . . C233 C 0.12510(9) 0.7920(2) 0.09688(11) 0.0671(6) Uani 1 1 d . . . H23D H 0.1011 0.8397 0.1063 0.081 Uiso 1 1 calc R . . C234 C 0.12279(10) 0.7835(2) 0.04172(11) 0.0687(6) Uani 1 1 d . . . H23E H 0.0972 0.8245 0.0137 0.082 Uiso 1 1 calc R . . C235 C 0.15889(12) 0.7135(2) 0.02834(10) 0.0703(6) Uani 1 1 d . . . H23F H 0.1577 0.7075 -0.0089 0.084 Uiso 1 1 calc R . . C236 C 0.19717(10) 0.65160(16) 0.07011(9) 0.0579(5) Uani 1 1 d . . . H23G H 0.2213 0.6048 0.0604 0.069 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 Cu 0.04563(13) 0.04253(12) 0.03782(12) -0.00121(8) 0.01485(9) -0.00050(9) Cl 0.0742(4) 0.0480(3) 0.0899(4) 0.0203(3) 0.0026(3) -0.0004(3) P1 0.0386(2) 0.0370(2) 0.0368(2) -0.00084(16) 0.01482(17) 0.00312(16) P2 0.0371(2) 0.0380(2) 0.0383(2) -0.00053(16) 0.01299(17) 0.00249(16) C11 0.0490(10) 0.0429(9) 0.0496(10) -0.0077(8) 0.0179(8) -0.0036(8) C111 0.0377(8) 0.0458(10) 0.0481(10) 0.0008(8) 0.0105(7) -0.0005(7) C112 0.0827(16) 0.0503(12) 0.0941(17) 0.0030(11) 0.0548(14) 0.0016(11) C113 0.0841(17) 0.0736(16) 0.0993(19) 0.0022(14) 0.0589(16) 0.0059(13) C114 0.0738(15) 0.0853(18) 0.0911(18) 0.0194(15) 0.0463(14) -0.0032(13) C115 0.158(3) 0.0586(16) 0.183(4) 0.026(2) 0.123(3) 0.0043(18) C116 0.128(2) 0.0490(13) 0.145(3) 0.0164(15) 0.095(2) 0.0137(15) C12 0.0551(10) 0.0436(9) 0.0507(10) 0.0041(8) 0.0216(9) 0.0109(8) C121 0.0454(9) 0.0528(10) 0.0489(10) 0.0116(8) 0.0186(8) 0.0154(8) C122 0.0415(10) 0.0938(17) 0.0561(12) 0.0206(12) 0.0180(9) 0.0060(10) C123 0.0447(11) 0.118(2) 0.0620(14) 0.0147(14) 0.0077(10) -0.0016(13) C124 0.0629(14) 0.117(2) 0.0505(12) 0.0185(13) 0.0140(11) 0.0155(14) C125 0.0744(15) 0.0887(17) 0.0582(13) 0.0250(12) 0.0325(12) 0.0127(13) C126 0.0563(11) 0.0564(12) 0.0626(12) 0.0135(10) 0.0235(10) 0.0055(9) C13 0.0450(9) 0.0476(9) 0.0440(9) -0.0055(7) 0.0206(8) 0.0032(7) C131 0.0433(9) 0.0443(9) 0.0439(9) -0.0013(7) 0.0219(7) 0.0064(7) C132 0.0527(11) 0.0690(13) 0.0461(10) 0.0091(9) 0.0184(9) 0.0001(10) C133 0.0685(13) 0.0720(14) 0.0628(13) 0.0168(11) 0.0292(11) -0.0053(11) C134 0.0574(12) 0.0603(12) 0.0687(14) 0.0016(10) 0.0259(11) -0.0076(10) C135 0.0465(10) 0.0579(11) 0.0499(10) -0.0030(9) 0.0164(8) 0.0024(8) C136 0.0472(9) 0.0496(10) 0.0437(9) 0.0021(8) 0.0222(8) 0.0055(8) C21 0.0426(9) 0.0518(10) 0.0408(9) 0.0044(8) 0.0125(7) 0.0068(8) C211 0.0382(8) 0.0491(10) 0.0457(9) 0.0083(8) 0.0107(7) 0.0076(7) C212 0.0447(11) 0.0647(13) 0.0794(15) -0.0074(11) 0.0135(10) -0.0012(9) C213 0.0420(11) 0.0918(19) 0.105(2) -0.0025(16) 0.0217(12) -0.0066(12) C214 0.0444(12) 0.109(2) 0.0822(17) 0.0087(15) 0.0254(12) 0.0193(12) C215 0.0614(13) 0.0712(14) 0.0652(13) 0.0025(11) 0.0216(11) 0.0239(11) C216 0.0484(10) 0.0485(10) 0.0533(11) 0.0060(8) 0.0150(8) 0.0074(8) C22 0.0466(9) 0.0462(10) 0.0527(10) -0.0048(8) 0.0222(8) 0.0056(8) C221 0.0442(9) 0.0511(10) 0.0521(10) -0.0064(8) 0.0255(8) 0.0044(8) C222 0.0600(12) 0.0748(14) 0.0524(11) -0.0043(10) 0.0287(10) 0.0020(11) C223 0.0816(17) 0.0926(19) 0.0703(15) 0.0180(14) 0.0465(14) 0.0209(15) C224 0.099(2) 0.0750(17) 0.117(2) 0.0239(17) 0.076(2) 0.0145(16) C225 0.0752(17) 0.0711(16) 0.125(3) -0.0119(17) 0.0531(18) -0.0187(13) C226 0.0582(12) 0.0680(14) 0.0709(14) -0.0116(11) 0.0280(11) -0.0074(10) C23 0.0417(9) 0.0445(9) 0.0526(10) 0.0022(8) 0.0146(8) -0.0029(7) C231 0.0443(9) 0.0343(8) 0.0491(10) -0.0008(7) 0.0152(8) -0.0064(7) C232 0.0565(11) 0.0473(10) 0.0570(11) -0.0019(9) 0.0219(9) -0.0001(9) C233 0.0573(12) 0.0567(12) 0.0909(17) 0.0171(12) 0.0296(12) 0.0113(10) C234 0.0635(13) 0.0591(13) 0.0723(15) 0.0240(11) 0.0080(11) -0.0024(11) C235 0.1034(19) 0.0559(13) 0.0484(11) 0.0079(10) 0.0213(12) -0.0095(13) C236 0.0823(15) 0.0422(10) 0.0565(12) 0.0013(8) 0.0328(11) 0.0022(10) _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 Cu P2 2.2275(5) . ? Cu P1 2.2399(5) . ? Cu Cl 2.2521(6) . ? P1 C11 1.8446(18) . ? P1 C13 1.8477(17) . ? P1 C12 1.8564(18) . ? P2 C23 1.8505(18) . ? P2 C21 1.8489(17) . ? P2 C22 1.8502(17) . ? C11 C111 1.515(3) . ? C111 C116 1.377(3) . ? C111 C112 1.377(3) . ? C112 C113 1.392(3) . ? C113 C114 1.360(4) . ? C114 C115 1.359(4) . ? C115 C116 1.389(4) . ? C12 C121 1.508(3) . ? C121 C122 1.389(3) . ? C121 C126 1.398(3) . ? C122 C123 1.391(3) . ? C123 C124 1.378(3) . ? C124 C125 1.377(4) . ? C125 C126 1.388(3) . ? C13 C131 1.513(3) . ? C131 C136 1.394(3) . ? C131 C132 1.397(3) . ? C132 C133 1.390(3) . ? C133 C134 1.376(3) . ? C134 C135 1.388(3) . ? C135 C136 1.388(3) . ? C21 C211 1.512(2) . ? C211 C212 1.388(3) . ? C211 C216 1.396(3) . ? C212 C213 1.388(3) . ? C213 C214 1.376(4) . ? C214 C215 1.381(4) . ? C215 C216 1.392(3) . ? C22 C221 1.507(3) . ? C221 C226 1.392(3) . ? C221 C222 1.393(3) . ? C222 C223 1.381(3) . ? C223 C224 1.371(4) . ? C224 C225 1.382(4) . ? C225 C226 1.388(4) . ? C23 C231 1.508(3) . ? C231 C236 1.388(3) . ? C231 C232 1.399(3) . ? C232 C233 1.385(3) . ? C233 C234 1.373(4) . ? C234 C235 1.378(4) . ? C235 C236 1.393(3) . ? 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 P2 Cu P1 136.528(18) . . ? P2 Cu Cl 117.76(2) . . ? P1 Cu Cl 105.34(2) . . ? C11 P1 C13 98.73(8) . . ? C11 P1 C12 106.49(9) . . ? C13 P1 C12 104.74(9) . . ? C11 P1 Cu 113.44(6) . . ? C13 P1 Cu 109.97(6) . . ? C12 P1 Cu 120.89(6) . . ? C23 P2 C21 101.71(8) . . ? C23 P2 C22 102.93(9) . . ? C21 P2 C22 100.37(9) . . ? C23 P2 Cu 121.75(6) . . ? C21 P2 Cu 114.04(6) . . ? C22 P2 Cu 113.25(6) . . ? C111 C11 P1 117.44(13) . . ? C116 C111 C112 116.6(2) . . ? C116 C111 C11 118.50(19) . . ? C112 C111 C11 124.85(17) . . ? C111 C112 C113 121.6(2) . . ? C114 C113 C112 120.4(2) . . ? C115 C114 C113 119.0(2) . . ? C114 C115 C116 120.5(3) . . ? C111 C116 C115 121.7(2) . . ? C121 C12 P1 117.34(13) . . ? C122 C121 C126 117.56(19) . . ? C122 C121 C12 121.56(17) . . ? C126 C121 C12 120.87(19) . . ? C121 C122 C123 121.3(2) . . ? C124 C123 C122 120.0(2) . . ? C123 C124 C125 119.8(2) . . ? C124 C125 C126 120.3(2) . . ? C125 C126 C121 121.1(2) . . ? C131 C13 P1 115.43(12) . . ? C136 C131 C132 117.82(17) . . ? C136 C131 C13 120.71(16) . . ? C132 C131 C13 121.37(17) . . ? C133 C132 C131 120.76(19) . . ? C134 C133 C132 120.6(2) . . ? C133 C134 C135 119.5(2) . . ? C134 C135 C136 120.01(19) . . ? C135 C136 C131 121.29(17) . . ? C211 C21 P2 114.80(13) . . ? C212 C211 C216 118.45(18) . . ? C212 C211 C21 120.16(18) . . ? C216 C211 C21 121.36(17) . . ? C211 C212 C213 120.5(2) . . ? C214 C213 C212 120.7(2) . . ? C213 C214 C215 119.5(2) . . ? C214 C215 C216 120.2(2) . . ? C215 C216 C211 120.6(2) . . ? C221 C22 P2 112.21(12) . . ? C226 C221 C222 118.5(2) . . ? C226 C221 C22 121.08(19) . . ? C222 C221 C22 120.37(18) . . ? C223 C222 C221 120.9(2) . . ? C224 C223 C222 120.1(3) . . ? C223 C224 C225 120.0(2) . . ? C224 C225 C226 120.2(3) . . ? C221 C226 C225 120.2(2) . . ? C231 C23 P2 115.70(12) . . ? C236 C231 C232 117.53(18) . . ? C236 C231 C23 121.66(17) . . ? C232 C231 C23 120.79(18) . . ? C233 C232 C231 121.1(2) . . ? C234 C233 C232 120.7(2) . . ? C233 C234 C235 119.2(2) . . ? C234 C235 C236 120.6(2) . . ? C231 C236 C235 120.9(2) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.289 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.040 #====END data_gf61 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H33 Cl Cu P' _chemical_formula_sum 'C33 H33 Cl Cu P' _chemical_formula_weight 559.55 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' 'P' 'P' 0.1023 0.0942 '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' '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 P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.902(3) _cell_length_b 10.432(4) _cell_length_c 14.326(5) _cell_angle_alpha 94.710(5) _cell_angle_beta 97.485(4) _cell_angle_gamma 95.759(5) _cell_volume 1453.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 3444 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 25 _exptl_crystal_description colorless _exptl_crystal_colour plate _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 0.918 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7703 _exptl_absorpt_correction_T_max 0.9642 _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 'Siemens SMART CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17080 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5107 _reflns_number_gt 3444 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XPMA (Zsolnai, 1994)' _computing_publication_material 'SHELXL-97 (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^)+(0.0536P)^2^+0.9581P] 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_number_reflns 5107 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.002 _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 Cu Cu 0.50713(5) 0.92865(5) 0.90320(3) 0.03155(17) Uani 1 1 d . . . Cl Cl 0.36440(12) 1.07489(11) 0.95122(7) 0.0437(3) Uani 1 1 d . . . P P 0.50673(10) 0.81791(9) 0.76693(7) 0.0253(2) Uani 1 1 d . . . C1 C 0.3479(4) 0.7045(4) 0.7314(3) 0.0311(9) Uani 1 1 d . . . H1A H 0.2677 0.7540 0.7232 0.037 Uiso 1 1 calc R . . H1B H 0.3530 0.6549 0.6703 0.037 Uiso 1 1 calc R . . C11 C 0.3311(4) 0.6123(4) 0.8065(3) 0.0281(9) Uani 1 1 d . . . C12 C 0.2910(5) 0.6538(4) 0.8919(3) 0.0446(11) Uani 1 1 d . . . H12A H 0.2661 0.7390 0.9019 0.054 Uiso 1 1 calc R . . C13 C 0.2870(6) 0.5705(6) 0.9640(3) 0.0669(16) Uani 1 1 d . . . H13A H 0.2597 0.5992 1.0226 0.080 Uiso 1 1 calc R . . C14 C 0.3229(6) 0.4467(5) 0.9492(4) 0.0683(16) Uani 1 1 d . . . H14A H 0.3214 0.3908 0.9983 0.082 Uiso 1 1 calc R . . C15 C 0.3607(5) 0.4037(5) 0.8646(4) 0.0550(13) Uani 1 1 d . . . H15A H 0.3838 0.3179 0.8546 0.066 Uiso 1 1 calc R . . C16 C 0.3649(4) 0.4858(4) 0.7934(3) 0.0398(10) Uani 1 1 d . . . H16A H 0.3913 0.4556 0.7348 0.048 Uiso 1 1 calc R . . C2 C 0.6410(4) 0.7081(4) 0.7633(3) 0.0307(9) Uani 1 1 d . . . H2A H 0.6321 0.6474 0.8124 0.037 Uiso 1 1 calc R . . H2B H 0.6259 0.6564 0.7011 0.037 Uiso 1 1 calc R . . C21 C 0.7854(4) 0.7770(3) 0.7791(3) 0.0282(9) Uani 1 1 d . . . C26 C 0.8510(4) 0.8091(4) 0.7026(3) 0.0348(10) Uani 1 1 d . . . H26A H 0.8051 0.7867 0.6401 0.042 Uiso 1 1 calc R . . C25 C 0.9826(5) 0.8733(4) 0.7168(3) 0.0419(11) Uani 1 1 d . . . H25A H 1.0256 0.8953 0.6639 0.050 Uiso 1 1 calc R . . C24 C 1.0522(4) 0.9056(4) 0.8075(3) 0.0419(11) Uani 1 1 d . . . H24A H 1.1425 0.9495 0.8170 0.050 Uiso 1 1 calc R . . C23 C 0.9879(4) 0.8729(4) 0.8844(3) 0.0414(11) Uani 1 1 d . . . H23A H 1.0352 0.8936 0.9467 0.050 Uiso 1 1 calc R . . C22 C 0.8554(4) 0.8101(4) 0.8709(3) 0.0350(10) Uani 1 1 d . . . H22A H 0.8120 0.7896 0.9240 0.042 Uiso 1 1 calc R . . C3 C 0.5241(4) 0.9033(4) 0.6595(3) 0.0318(9) Uani 1 1 d . . . H3A H 0.6049 0.9694 0.6734 0.038 Uiso 1 1 calc R . . H3B H 0.5414 0.8402 0.6082 0.038 Uiso 1 1 calc R . . C31 C 0.3992(4) 0.9692(4) 0.6247(3) 0.0284(9) Uani 1 1 d . . . C32 C 0.3526(4) 1.0665(4) 0.6814(3) 0.0343(10) Uani 1 1 d . . . H32A H 0.3978 1.0908 0.7439 0.041 Uiso 1 1 calc R . . C33 C 0.2404(4) 1.1280(4) 0.6468(3) 0.0408(11) Uani 1 1 d . . . H33A H 0.2093 1.1942 0.6854 0.049 Uiso 1 1 calc R . . C34 C 0.1744(5) 1.0915(4) 0.5553(3) 0.0454(12) Uani 1 1 d . . . H34A H 0.0984 1.1337 0.5313 0.054 Uiso 1 1 calc R . . C35 C 0.2183(5) 0.9948(4) 0.4992(3) 0.0442(11) Uani 1 1 d . . . H35A H 0.1721 0.9694 0.4371 0.053 Uiso 1 1 calc R . . C36 C 0.3298(4) 0.9352(4) 0.5339(3) 0.0382(10) Uani 1 1 d . . . H36A H 0.3601 0.8691 0.4947 0.046 Uiso 1 1 calc R . . C1A C 0.1636(7) 0.8283(5) 0.1737(6) 0.115(3) Uani 1 1 d . . . H1AA H 0.1699 0.9172 0.1630 0.138 Uiso 1 1 calc R . . C2A C 0.0405(6) 0.7559(5) 0.1577(4) 0.0680(16) Uani 1 1 d . . . H2AA H -0.0399 0.7936 0.1362 0.082 Uiso 1 1 calc R . . C3A C 0.0324(6) 0.6255(5) 0.1731(4) 0.0659(15) Uani 1 1 d . . . H3AA H -0.0533 0.5731 0.1613 0.079 Uiso 1 1 calc R . . C4A C 0.1493(8) 0.5737(6) 0.2053(4) 0.0745(19) Uani 1 1 d . . . H4AA H 0.1444 0.4851 0.2170 0.089 Uiso 1 1 calc R . . C5A C 0.2701(7) 0.6465(7) 0.2206(4) 0.077(2) Uani 1 1 d . . . H5AA H 0.3506 0.6092 0.2424 0.092 Uiso 1 1 calc R . . C6A C 0.2790(6) 0.7745(7) 0.2050(6) 0.123(3) Uani 1 1 d . . . H6AA H 0.3654 0.8259 0.2160 0.147 Uiso 1 1 calc R . . C1B C 0.0520(4) 0.6278(4) 0.5309(3) 0.0410(11) Uani 1 1 d . . . H1BA H 0.0875 0.7149 0.5517 0.049 Uiso 1 1 calc R . . C2B C 0.0316(4) 0.5385(4) 0.5967(3) 0.0434(11) Uani 1 1 d . . . H2BA H 0.0530 0.5643 0.6626 0.052 Uiso 1 1 calc R . . C3B C -0.0204(4) 0.4114(4) 0.5648(3) 0.0426(11) Uani 1 1 d . . . H3BA H -0.0344 0.3505 0.6094 0.051 Uiso 1 1 calc R . . C1C C 0.6346(5) 0.5478(4) 0.4964(3) 0.0432(12) Uani 1 1 d . . . H1CA H 0.7271 0.5803 0.4942 0.052 Uiso 1 1 calc R . . C2C C 0.5292(5) 0.6142(4) 0.4587(3) 0.0446(12) Uani 1 1 d . . . H2CA H 0.5487 0.6920 0.4304 0.053 Uiso 1 1 calc R . . C3C C 0.3945(5) 0.5653(4) 0.4631(3) 0.0444(11) Uani 1 1 d . . . H3CA H 0.3216 0.6104 0.4378 0.053 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 Cu 0.0374(3) 0.0316(3) 0.0245(3) -0.0020(2) 0.0043(2) 0.0021(2) Cl 0.0485(7) 0.0531(7) 0.0304(6) -0.0024(5) -0.0019(5) 0.0255(6) P 0.0266(6) 0.0263(5) 0.0228(5) 0.0013(4) 0.0031(4) 0.0032(4) C1 0.028(2) 0.037(2) 0.029(2) 0.0021(17) 0.0038(18) 0.0045(18) C11 0.021(2) 0.030(2) 0.031(2) 0.0016(17) 0.0011(17) -0.0039(17) C12 0.052(3) 0.041(3) 0.042(3) 0.001(2) 0.015(2) -0.002(2) C13 0.083(4) 0.076(4) 0.041(3) 0.007(3) 0.022(3) -0.016(3) C14 0.076(4) 0.060(4) 0.064(4) 0.030(3) -0.005(3) -0.016(3) C15 0.053(3) 0.045(3) 0.068(4) 0.020(3) 0.002(3) 0.004(2) C16 0.037(3) 0.035(2) 0.046(3) 0.002(2) 0.004(2) 0.001(2) C2 0.036(3) 0.027(2) 0.030(2) 0.0041(17) 0.0069(18) 0.0068(18) C21 0.026(2) 0.0225(19) 0.038(2) 0.0058(16) 0.0063(18) 0.0083(17) C26 0.034(3) 0.038(2) 0.034(2) 0.0042(19) 0.0050(19) 0.009(2) C25 0.039(3) 0.044(3) 0.047(3) 0.009(2) 0.018(2) 0.008(2) C24 0.025(2) 0.042(3) 0.058(3) 0.001(2) 0.006(2) 0.005(2) C23 0.034(3) 0.048(3) 0.040(3) -0.003(2) -0.005(2) 0.009(2) C22 0.036(3) 0.039(2) 0.032(2) 0.0073(18) 0.0071(19) 0.007(2) C3 0.033(2) 0.036(2) 0.028(2) 0.0072(17) 0.0069(18) 0.0040(19) C31 0.026(2) 0.031(2) 0.030(2) 0.0139(17) 0.0055(18) 0.0005(17) C32 0.036(3) 0.035(2) 0.032(2) 0.0065(18) 0.0035(19) 0.002(2) C33 0.038(3) 0.038(2) 0.051(3) 0.011(2) 0.014(2) 0.010(2) C34 0.028(3) 0.054(3) 0.058(3) 0.028(2) 0.004(2) 0.007(2) C35 0.039(3) 0.053(3) 0.039(3) 0.013(2) 0.001(2) 0.001(2) C36 0.040(3) 0.038(2) 0.037(2) 0.0075(19) 0.006(2) 0.002(2) C1A 0.063(5) 0.034(3) 0.238(9) 0.003(4) -0.005(5) 0.005(3) C2A 0.046(4) 0.067(4) 0.092(4) 0.023(3) -0.008(3) 0.020(3) C3A 0.055(4) 0.063(4) 0.080(4) 0.012(3) 0.014(3) -0.003(3) C4A 0.092(5) 0.065(4) 0.092(4) 0.044(3) 0.062(4) 0.042(4) C5A 0.074(5) 0.112(5) 0.050(3) -0.005(3) -0.002(3) 0.063(4) C6A 0.046(4) 0.075(5) 0.219(9) -0.069(5) -0.039(5) 0.016(3) C1B 0.027(3) 0.041(3) 0.054(3) -0.002(2) 0.007(2) -0.001(2) C2B 0.025(3) 0.059(3) 0.043(3) -0.008(2) 0.001(2) 0.000(2) C3B 0.030(3) 0.050(3) 0.050(3) 0.008(2) 0.008(2) 0.009(2) C1C 0.029(3) 0.055(3) 0.043(3) -0.014(2) 0.015(2) -0.006(2) C2C 0.052(3) 0.042(3) 0.042(3) -0.001(2) 0.021(2) 0.001(2) C3C 0.038(3) 0.057(3) 0.039(3) -0.004(2) 0.009(2) 0.018(2) _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 Cu P 2.1846(12) . ? Cu Cl 2.3022(13) 2_677 ? Cu Cl 2.3049(12) . ? Cl Cu 2.3022(13) 2_677 ? P C2 1.843(4) . ? P C1 1.857(4) . ? P C3 1.859(4) . ? C1 C11 1.515(5) . ? C11 C12 1.384(5) . ? C11 C16 1.398(5) . ? C12 C13 1.405(6) . ? C13 C14 1.380(8) . ? C14 C15 1.369(7) . ? C15 C16 1.386(6) . ? C2 C21 1.514(5) . ? C21 C26 1.392(5) . ? C21 C22 1.403(5) . ? C26 C25 1.387(6) . ? C25 C24 1.388(6) . ? C24 C23 1.391(6) . ? C23 C22 1.389(6) . ? C3 C31 1.522(5) . ? C31 C36 1.390(5) . ? C31 C32 1.400(5) . ? C32 C33 1.394(5) . ? C33 C34 1.391(6) . ? C34 C35 1.378(6) . ? C35 C36 1.378(6) . ? C1A C2A 1.351(8) . ? C1A C6A 1.362(8) . ? C2A C3A 1.391(7) . ? C3A C4A 1.369(7) . ? C4A C5A 1.333(8) . ? C5A C6A 1.368(9) . ? C1B C3B 1.384(6) 2_566 ? C1B C2B 1.398(6) . ? C2B C3B 1.391(6) . ? C3B C1B 1.384(6) 2_566 ? C1C C3C 1.378(6) 2_666 ? C1C C2C 1.386(6) . ? C2C C3C 1.391(6) . ? C3C C1C 1.378(6) 2_666 ? 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 P Cu Cl 132.07(4) . 2_677 ? P Cu Cl 131.14(4) . . ? Cl Cu Cl 96.59(4) 2_677 . ? Cu Cl Cu 83.41(4) 2_677 . ? C2 P C1 101.95(18) . . ? C2 P C3 101.53(17) . . ? C1 P C3 103.36(18) . . ? C2 P Cu 115.31(13) . . ? C1 P Cu 112.37(13) . . ? C3 P Cu 120.06(13) . . ? C11 C1 P 109.9(3) . . ? C12 C11 C16 118.6(4) . . ? C12 C11 C1 120.8(3) . . ? C16 C11 C1 120.4(4) . . ? C11 C12 C13 120.2(4) . . ? C14 C13 C12 119.8(5) . . ? C15 C14 C13 120.6(5) . . ? C14 C15 C16 119.8(5) . . ? C15 C16 C11 121.0(4) . . ? C21 C2 P 113.9(3) . . ? C26 C21 C22 118.7(4) . . ? C26 C21 C2 120.5(4) . . ? C22 C21 C2 120.8(4) . . ? C25 C26 C21 120.7(4) . . ? C26 C25 C24 120.7(4) . . ? C25 C24 C23 119.0(4) . . ? C22 C23 C24 120.7(4) . . ? C23 C22 C21 120.3(4) . . ? C31 C3 P 114.0(3) . . ? C36 C31 C32 118.2(4) . . ? C36 C31 C3 120.2(4) . . ? C32 C31 C3 121.6(4) . . ? C33 C32 C31 120.5(4) . . ? C34 C33 C32 119.5(4) . . ? C35 C34 C33 120.6(4) . . ? C36 C35 C34 119.5(4) . . ? C35 C36 C31 121.8(4) . . ? C2A C1A C6A 120.4(6) . . ? C1A C2A C3A 119.4(5) . . ? C4A C3A C2A 119.3(5) . . ? C5A C4A C3A 120.5(5) . . ? C4A C5A C6A 120.6(5) . . ? C1A C6A C5A 119.8(6) . . ? C3B C1B C2B 119.7(4) 2_566 . ? C3B C2B C1B 119.3(4) . . ? C1B C3B C2B 121.0(4) 2_566 . ? C3C C1C C2C 120.2(4) 2_666 . ? C1C C2C C3C 118.9(4) . . ? C1C C3C C2C 120.9(4) 2_666 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 0.50 _diffrn_measured_fraction_theta_full 0.000 _refine_diff_density_max 0.324 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.071 #=====END