# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'ProfD Tristram Chivers' _publ_contact_author_address ; Chemistry University of Calgary 2500 University Drive NW Calgary Alberta T2N 1N4 CANADA ; _publ_contact_author_email CHIVERS@UCALGARY.CA _publ_section_title ; Structure and Magnetic Properties of a Novel Copper Halide Framework {[tBuNH3]2[Cu3(\`i3-OH)( \`i2-H2O)Cl7]}n Synthesized via in situ Templation ; loop_ _publ_author_name 'T. Chivers' 'Zhiyong Fu.' 'L. Thompson' data_1 _database_code_depnum_ccdc_archive 'CCDC 261137' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H13.50 Cl3.50 Cu1.50 N O' _chemical_formula_weight 311.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 9.1349(18) _cell_length_b 26.780(5) _cell_length_c 8.5459(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2090.6(7) _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 block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.976 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 3.922 _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 6759 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1873 _reflns_number_gt 1415 _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^)+(0.0278P)^2^+3.4096P] 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 1873 _refine_ls_number_parameters 119 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0716 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.066 _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 0.72857(5) 0.68819(2) 0.46689(6) 0.02058(16) Uani 1 1 d . . . Cu2 Cu 0.43309(7) 0.7500 0.42973(8) 0.0182(2) Uani 1 2 d S . . Cl3 Cl 0.20088(14) 0.7500 0.51616(17) 0.0225(3) Uani 1 2 d S . . Cl4 Cl 0.52236(11) 0.68424(4) 0.61713(12) 0.0268(3) Uani 1 1 d . . . Cl1 Cl 0.81737(12) 0.61765(4) 0.57571(13) 0.0316(3) Uani 1 1 d . . . Cl2 Cl 0.88986(11) 0.68114(4) 0.26437(12) 0.0263(3) Uani 1 1 d . . . O2 O 0.8403(5) 0.7500 0.6165(5) 0.0259(10) Uani 1 2 d SD . . H2D H 0.814(7) 0.7500 0.714(3) 0.04(2) Uiso 1 2 d SD . . H2E H 0.935(2) 0.7500 0.619(7) 0.034(19) Uiso 1 2 d SD . . O1 O 0.6392(4) 0.7500 0.3732(5) 0.0195(9) Uani 1 2 d SD . . H1D H 0.666(8) 0.7500 0.277(3) 0.06(3) Uiso 1 2 d SD . . N1 N 0.1856(4) 0.62464(13) 0.5593(4) 0.0255(9) Uani 1 1 d . . . H1B H 0.2272 0.6462 0.4936 0.038 Uiso 1 1 calc R . . H1C H 0.2241 0.6284 0.6543 0.038 Uiso 1 1 calc R . . H1D' H 0.0897 0.6304 0.5634 0.038 Uiso 1 1 calc R . . C3 C 0.2124(4) 0.57179(15) 0.5026(5) 0.0211(10) Uani 1 1 d . . . C4 C 0.3767(5) 0.56388(19) 0.4973(5) 0.0346(12) Uani 1 1 d . . . H4A H 0.4165 0.5677 0.6006 0.052 Uiso 1 1 calc R . . H4B H 0.4201 0.5881 0.4287 0.052 Uiso 1 1 calc R . . H4C H 0.3974 0.5309 0.4593 0.052 Uiso 1 1 calc R . . C2 C 0.1394(5) 0.53675(16) 0.6172(5) 0.0293(11) Uani 1 1 d . . . H2A H 0.0358 0.5428 0.6179 0.044 Uiso 1 1 calc R . . H2B H 0.1783 0.5423 0.7200 0.044 Uiso 1 1 calc R . . H2C H 0.1576 0.5028 0.5864 0.044 Uiso 1 1 calc R . . C1 C 0.1429(5) 0.56775(17) 0.3403(5) 0.0296(11) Uani 1 1 d . . . H1A H 0.0414 0.5769 0.3465 0.044 Uiso 1 1 calc R . . H1B' H 0.1511 0.5340 0.3033 0.044 Uiso 1 1 calc R . . H1C' H 0.1925 0.5898 0.2694 0.044 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 0.0165(3) 0.0304(3) 0.0148(3) -0.0006(2) 0.0012(2) 0.0019(2) Cu2 0.0131(4) 0.0259(4) 0.0155(4) 0.000 0.0007(3) 0.000 Cl3 0.0159(7) 0.0287(9) 0.0229(8) 0.000 0.0033(6) 0.000 Cl4 0.0212(5) 0.0366(7) 0.0227(6) -0.0034(5) 0.0070(4) -0.0047(5) Cl1 0.0310(6) 0.0376(7) 0.0262(6) 0.0048(5) 0.0024(5) 0.0074(5) Cl2 0.0232(6) 0.0320(6) 0.0238(6) -0.0014(5) 0.0082(5) 0.0032(5) O2 0.019(2) 0.039(3) 0.019(3) 0.000 -0.0022(19) 0.000 O1 0.016(2) 0.026(2) 0.017(2) 0.000 -0.0011(18) 0.000 N1 0.027(2) 0.027(2) 0.023(2) -0.0023(16) -0.0041(16) 0.0004(17) C3 0.026(2) 0.021(2) 0.016(2) -0.0004(18) 0.0008(18) 0.0017(19) C4 0.027(2) 0.042(3) 0.034(3) -0.003(2) 0.001(2) 0.006(2) C2 0.032(3) 0.031(3) 0.025(3) 0.000(2) -0.004(2) -0.001(2) C1 0.032(3) 0.037(3) 0.020(2) 0.001(2) 0.001(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 Cu1 O1 2.012(2) . ? Cu1 Cl1 2.2564(13) . ? Cu1 Cl2 2.2807(12) . ? Cu1 Cl4 2.2821(11) . ? Cu1 O2 2.327(3) . ? Cu2 O1 1.944(4) . ? Cu2 Cl3 2.2462(15) . ? Cu2 Cl2 2.5115(12) 6_556 ? Cu2 Cl2 2.5115(12) 4_465 ? Cu2 Cl4 2.5161(13) 7_575 ? Cu2 Cl4 2.5161(12) . ? Cl2 Cu2 2.5115(12) 6_656 ? O2 Cu1 2.327(3) 7_575 ? O1 Cu1 2.012(2) 7_575 ? N1 C3 1.516(5) . ? C3 C2 1.511(6) . ? C3 C4 1.517(6) . ? C3 C1 1.529(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 O1 Cu1 Cl1 177.11(11) . . ? O1 Cu1 Cl2 91.62(12) . . ? Cl1 Cu1 Cl2 90.64(4) . . ? O1 Cu1 Cl4 85.82(12) . . ? Cl1 Cu1 Cl4 91.49(4) . . ? Cl2 Cu1 Cl4 163.00(5) . . ? O1 Cu1 O2 79.12(12) . . ? Cl1 Cu1 O2 102.20(8) . . ? Cl2 Cu1 O2 101.09(12) . . ? Cl4 Cu1 O2 94.93(11) . . ? O1 Cu2 Cl3 175.18(13) . . ? O1 Cu2 Cl2 89.33(8) . 6_556 ? Cl3 Cu2 Cl2 93.94(4) . 6_556 ? O1 Cu2 Cl2 89.33(8) . 4_465 ? Cl3 Cu2 Cl2 93.94(4) . 4_465 ? Cl2 Cu2 Cl2 94.48(6) 6_556 4_465 ? O1 Cu2 Cl4 81.03(9) . 7_575 ? Cl3 Cu2 Cl4 95.55(4) . 7_575 ? Cl2 Cu2 Cl4 170.13(4) 6_556 7_575 ? Cl2 Cu2 Cl4 87.56(4) 4_465 7_575 ? O1 Cu2 Cl4 81.03(9) . . ? Cl3 Cu2 Cl4 95.55(4) . . ? Cl2 Cu2 Cl4 87.56(4) 6_556 . ? Cl2 Cu2 Cl4 170.13(4) 4_465 . ? Cl4 Cu2 Cl4 88.84(5) 7_575 . ? Cu1 Cl4 Cu2 82.93(4) . . ? Cu1 Cl2 Cu2 122.82(5) . 6_656 ? Cu1 O2 Cu1 90.67(15) . 7_575 ? Cu2 O1 Cu1 107.11(13) . 7_575 ? Cu2 O1 Cu1 107.11(13) . . ? Cu1 O1 Cu1 110.74(18) 7_575 . ? C2 C3 N1 107.5(3) . . ? C2 C3 C4 111.7(4) . . ? N1 C3 C4 107.4(3) . . ? C2 C3 C1 111.1(3) . . ? N1 C3 C1 106.8(3) . . ? C4 C3 C1 112.0(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.620 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.123 #=========================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 261138' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H12 Cl3 Cu N' _chemical_formula_weight 244.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/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 6.1048(12) _cell_length_b 16.946(3) _cell_length_c 9.1044(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.63(3) _cell_angle_gamma 90.00 _cell_volume 941.8(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 block _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 3.095 _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 3476 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 26.37 _reflns_number_total 1926 _reflns_number_gt 1379 _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^)+(0.0285P)^2^+2.8229P] 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 1926 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.0970 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 0.25219(10) 0.01386(4) 0.41369(7) 0.0173(2) Uani 1 1 d . . . Cl2 Cl 0.0328(2) -0.09734(7) 0.54286(15) 0.0201(3) Uani 1 1 d . . . Cl3 Cl 0.4401(2) 0.06267(7) 0.61680(15) 0.0224(3) Uani 1 1 d . . . Cl1 Cl 0.1806(2) 0.01045(8) 0.16729(15) 0.0253(3) Uani 1 1 d . . . N1 N 0.3178(7) -0.0850(2) 0.8623(5) 0.0223(11) Uani 1 1 d . . . H1D H 0.2468 -0.0618 0.9355 0.033 Uiso 1 1 calc R . . H1E H 0.2392 -0.0807 0.7798 0.033 Uiso 1 1 calc R . . H1F H 0.4470 -0.0616 0.8506 0.033 Uiso 1 1 calc R . . C4 C 0.1273(10) -0.2079(3) 0.9165(7) 0.0326(15) Uani 1 1 d . . . H4A H 0.0560 -0.1837 0.9985 0.049 Uiso 1 1 calc R . . H4B H 0.1413 -0.2635 0.9336 0.049 Uiso 1 1 calc R . . H4C H 0.0418 -0.1991 0.8289 0.049 Uiso 1 1 calc R . . C3 C 0.4754(10) -0.2078(3) 0.7688(7) 0.0322(15) Uani 1 1 d . . . H3A H 0.6166 -0.1834 0.7608 0.048 Uiso 1 1 calc R . . H3B H 0.3929 -0.1992 0.6798 0.048 Uiso 1 1 calc R . . H3C H 0.4936 -0.2635 0.7844 0.048 Uiso 1 1 calc R . . C2 C 0.3528(9) -0.1719(3) 0.8984(6) 0.0222(12) Uani 1 1 d . . . C1 C 0.4879(11) -0.1756(4) 1.0388(7) 0.0359(16) Uani 1 1 d . . . H1A H 0.4068 -0.1524 1.1176 0.054 Uiso 1 1 calc R . . H1B H 0.6221 -0.1470 1.0258 0.054 Uiso 1 1 calc R . . H1C H 0.5205 -0.2296 1.0618 0.054 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 0.0158(3) 0.0203(3) 0.0158(4) -0.0010(3) -0.0023(3) 0.0020(3) Cl2 0.0196(7) 0.0181(6) 0.0225(8) 0.0008(5) -0.0012(6) 0.0022(5) Cl3 0.0199(7) 0.0253(7) 0.0220(8) -0.0064(6) -0.0042(6) 0.0055(5) Cl1 0.0228(7) 0.0370(8) 0.0162(7) -0.0035(6) -0.0030(6) 0.0071(6) N1 0.020(3) 0.022(2) 0.025(3) 0.002(2) -0.001(2) 0.0034(19) C4 0.041(4) 0.027(3) 0.030(4) 0.005(3) 0.003(3) -0.003(3) C3 0.036(4) 0.032(3) 0.029(4) -0.001(3) -0.002(3) 0.007(3) C2 0.028(3) 0.020(3) 0.019(3) 0.001(2) -0.003(2) 0.005(2) C1 0.049(4) 0.032(3) 0.027(4) -0.004(3) -0.010(3) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 Cl2 2.2804(14) 3_556 ? Cu1 Cl1 2.2815(16) . ? Cu1 Cl3 2.3018(14) 3_656 ? Cu1 Cl3 2.3181(16) . ? Cu1 Cl2 2.6004(15) . ? Cl2 Cu1 2.2804(14) 3_556 ? Cl3 Cu1 2.3018(14) 3_656 ? N1 C2 1.524(6) . ? C4 C2 1.517(8) . ? C3 C2 1.531(8) . ? C2 C1 1.514(8) . ? 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 Cl2 Cu1 Cl1 92.75(6) 3_556 . ? Cl2 Cu1 Cl3 174.63(5) 3_556 3_656 ? Cl1 Cu1 Cl3 90.85(6) . 3_656 ? Cl2 Cu1 Cl3 90.69(5) 3_556 . ? Cl1 Cu1 Cl3 151.79(6) . . ? Cl3 Cu1 Cl3 84.26(5) 3_656 . ? Cl2 Cu1 Cl2 88.47(5) 3_556 . ? Cl1 Cu1 Cl2 109.41(5) . . ? Cl3 Cu1 Cl2 94.09(5) 3_656 . ? Cl3 Cu1 Cl2 98.66(5) . . ? Cu1 Cl2 Cu1 91.53(5) 3_556 . ? Cu1 Cl3 Cu1 95.74(5) 3_656 . ? C4 C2 C1 112.2(5) . . ? C4 C2 C3 112.1(5) . . ? C1 C2 C3 111.6(5) . . ? C4 C2 N1 106.7(4) . . ? C1 C2 N1 107.2(4) . . ? C3 C2 N1 106.7(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.549 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.131 data_3 _database_code_depnum_ccdc_archive 'CCDC 261139' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27.50 H66 Cl3 Cu N6 O2 P2' _chemical_formula_weight 744.69 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.241(2) _cell_length_b 13.790(3) _cell_length_c 16.238(3) _cell_angle_alpha 103.15(3) _cell_angle_beta 94.85(3) _cell_angle_gamma 103.03(3) _cell_volume 2153.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 798 _exptl_absorpt_coefficient_mu 0.796 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 P4' _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 10118 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 23.25 _reflns_number_total 5976 _reflns_number_gt 4330 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1124P)^2^+13.8095P] 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 5976 _refine_ls_number_parameters 352 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.1230 _refine_ls_R_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.2580 _refine_ls_wR_factor_gt 0.2336 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.034 _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 0.39116(9) 1.01237(8) -0.07482(7) 0.0472(4) Uani 1 1 d . . . Cl1 Cl 0.4008(2) 1.13715(18) -0.13948(15) 0.0632(7) Uani 1 1 d . . . P1 P 0.1628(2) 0.67478(16) 0.01769(15) 0.0428(5) Uani 1 1 d . . . O1 O 0.1000(5) 0.5616(4) -0.0063(4) 0.0508(14) Uani 1 1 d . . . H1G H 0.0862 0.5403 -0.0585 0.076 Uiso 1 1 calc R . . N1 N 0.3065(8) 0.6986(5) -0.0168(6) 0.066(2) Uani 1 1 d . . . H1H H 0.3667 0.7496 0.0163 0.080 Uiso 1 1 calc R . . N2 N 0.1920(9) 0.7202(6) 0.1204(6) 0.074(2) Uani 1 1 d . . . H2E H 0.1802 0.7810 0.1378 0.089 Uiso 1 1 calc R . . N3 N 0.0724(7) 0.7428(6) -0.0144(7) 0.082(3) Uani 1 1 d . . . H3G H 0.1205 0.7936 -0.0297 0.098 Uiso 1 1 calc R . . N4 N 0.7247(11) 1.0177(8) 0.3428(7) 0.040(3) Uiso 0.60 1 d PD A 1 H1D' H 0.6620 0.9711 0.3073 0.048 Uiso 0.60 1 calc PR A 1 N4A N 0.771(2) 1.0689(17) 0.3375(14) 0.066(5) Uiso 0.40 1 d P A 2 H1Q H 0.7737 1.0799 0.2875 0.079 Uiso 0.40 1 calc PR A 2 N5 N 0.9751(9) 1.0527(9) 0.3095(6) 0.050(3) Uiso 0.70 1 d PD A 1 H5D H 0.9405 1.0894 0.2819 0.060 Uiso 0.70 1 calc PR A 1 N5A N 0.9816(17) 0.9979(19) 0.2980(15) 0.048(6) Uiso 0.30 1 d PD A 2 H5Q H 0.9540 0.9532 0.2497 0.057 Uiso 0.30 1 calc PR A 2 N6 N 0.8478(11) 0.8647(8) 0.3161(7) 0.054(3) Uiso 0.70 1 d P A 1 H8A H 0.8836 0.8506 0.2702 0.065 Uiso 0.70 1 calc PR A 1 N6A N 0.782(3) 0.890(2) 0.333(2) 0.077(8) Uiso 0.30 1 d P A 2 H8B H 0.7068 0.8897 0.3053 0.093 Uiso 0.30 1 calc PR A 2 C1 C 0.3534(8) 0.6481(6) -0.0958(6) 0.053(2) Uani 1 1 d . . . C2 C 0.4673(9) 0.7286(7) -0.1145(6) 0.059(2) Uani 1 1 d . . . H2A H 0.5384 0.7531 -0.0667 0.089 Uiso 1 1 calc R . . H2B H 0.4331 0.7851 -0.1241 0.089 Uiso 1 1 calc R . . H2C H 0.5021 0.6985 -0.1645 0.089 Uiso 1 1 calc R . . C3 C 0.2435(10) 0.6114(9) -0.1723(7) 0.084(3) Uani 1 1 d . . . H3H H 0.1704 0.5604 -0.1619 0.127 Uiso 1 1 calc R . . H3I H 0.2797 0.5820 -0.2219 0.127 Uiso 1 1 calc R . . H3J H 0.2107 0.6686 -0.1815 0.127 Uiso 1 1 calc R . . C4 C 0.4052(11) 0.5599(8) -0.0778(8) 0.075(3) Uani 1 1 d . . . H4A H 0.3322 0.5099 -0.0662 0.113 Uiso 1 1 calc R . . H4B H 0.4749 0.5851 -0.0292 0.113 Uiso 1 1 calc R . . H4C H 0.4416 0.5285 -0.1267 0.113 Uiso 1 1 calc R . . C5 C 0.2350(9) 0.6765(7) 0.1894(6) 0.057(2) Uani 1 1 d . . . C6 C 0.3390(10) 0.6161(9) 0.1677(8) 0.079(3) Uani 1 1 d . . . H6A H 0.3010 0.5588 0.1192 0.119 Uiso 1 1 calc R . . H6B H 0.3649 0.5912 0.2156 0.119 Uiso 1 1 calc R . . H6C H 0.4173 0.6598 0.1545 0.119 Uiso 1 1 calc R . . C7 C 0.1091(10) 0.6064(10) 0.2071(8) 0.091(4) Uani 1 1 d . . . H7A H 0.0731 0.5500 0.1577 0.137 Uiso 1 1 calc R . . H7B H 0.0425 0.6445 0.2200 0.137 Uiso 1 1 calc R . . H7C H 0.1322 0.5803 0.2549 0.137 Uiso 1 1 calc R . . C8 C 0.2962(13) 0.7679(10) 0.2671(7) 0.092(4) Uani 1 1 d . . . H8C H 0.3755 0.8109 0.2542 0.137 Uiso 1 1 calc R . . H8D H 0.3205 0.7428 0.3153 0.137 Uiso 1 1 calc R . . H8E H 0.2309 0.8071 0.2804 0.137 Uiso 1 1 calc R . . C9 C -0.0728(8) 0.7410(7) -0.0245(6) 0.054(2) Uani 1 1 d . . . C10 C -0.1260(15) 0.6849(14) -0.1148(10) 0.135(6) Uani 1 1 d . . . H10A H -0.1164 0.6157 -0.1245 0.202 Uiso 1 1 calc R . . H10B H -0.0761 0.7192 -0.1520 0.202 Uiso 1 1 calc R . . H10C H -0.2200 0.6836 -0.1262 0.202 Uiso 1 1 calc R . . C11 C -0.0879(12) 0.8488(8) -0.0095(10) 0.100(5) Uani 1 1 d . . . H11A H -0.0534 0.8852 0.0488 0.151 Uiso 1 1 calc R . . H11B H -0.1819 0.8474 -0.0210 0.151 Uiso 1 1 calc R . . H11C H -0.0380 0.8829 -0.0468 0.151 Uiso 1 1 calc R . . C12 C -0.1473(14) 0.6847(11) 0.0312(11) 0.117(5) Uani 1 1 d . . . H12A H -0.1352 0.6161 0.0198 0.176 Uiso 1 1 calc R . . H12B H -0.2419 0.6818 0.0202 0.176 Uiso 1 1 calc R . . H12C H -0.1133 0.7196 0.0899 0.176 Uiso 1 1 calc R . . C14 C 1.1839(15) 1.0128(12) 0.3673(9) 0.065(4) Uiso 0.70 1 d PD A 1 H1A H 1.1839 1.0531 0.4239 0.098 Uiso 0.70 1 calc PR A 1 H1B H 1.2753 1.0129 0.3581 0.098 Uiso 0.70 1 calc PR A 1 H1C H 1.1326 0.9434 0.3609 0.098 Uiso 0.70 1 calc PR A 1 C14A C 1.219(3) 1.071(3) 0.3801(15) 0.059(8) Uiso 0.30 1 d PD A 2 H1D H 1.1696 1.0532 0.4246 0.089 Uiso 0.30 1 calc PR A 2 H1E H 1.2715 1.1411 0.3992 0.089 Uiso 0.30 1 calc PR A 2 H1F H 1.2775 1.0263 0.3663 0.089 Uiso 0.30 1 calc PR A 2 C15 C 1.1219(18) 0.9811(13) 0.2164(9) 0.086(5) Uiso 0.70 1 d PD A 1 H3A H 1.0770 0.9987 0.1697 0.129 Uiso 0.70 1 calc PR A 1 H3B H 1.0762 0.9131 0.2189 0.129 Uiso 0.70 1 calc PR A 1 H3C H 1.2141 0.9830 0.2082 0.129 Uiso 0.70 1 calc PR A 1 C15A C 1.175(3) 1.062(3) 0.2192(16) 0.070(9) Uiso 0.30 1 d PD A 2 H3D H 1.1112 1.0161 0.1723 0.105 Uiso 0.30 1 calc PR A 2 H3E H 1.2588 1.0422 0.2207 0.105 Uiso 0.30 1 calc PR A 2 H3F H 1.1907 1.1311 0.2119 0.105 Uiso 0.30 1 calc PR A 2 C16 C 1.1194(9) 1.0592(8) 0.3013(6) 0.073(3) Uiso 0.70 1 d PD A 1 C16A C 1.1194(9) 1.0592(8) 0.3013(6) 0.073(3) Uiso 0.30 1 d PD A 2 C21 C 0.8058(19) 1.2131(14) 0.3982(16) 0.092(6) Uiso 0.60 1 d PD A 1 H21A H 0.8794 1.2089 0.4369 0.137 Uiso 0.60 1 calc PR A 1 H21B H 0.7757 1.2733 0.4218 0.137 Uiso 0.60 1 calc PR A 1 H21C H 0.8358 1.2173 0.3444 0.137 Uiso 0.60 1 calc PR A 1 C21A C 0.778(4) 1.206(2) 0.453(2) 0.119(12) Uiso 0.40 1 d PD A 2 H21D H 0.8711 1.2126 0.4444 0.179 Uiso 0.40 1 calc PR A 2 H21E H 0.7677 1.1927 0.5083 0.179 Uiso 0.40 1 calc PR A 2 H21F H 0.7530 1.2680 0.4508 0.179 Uiso 0.40 1 calc PR A 2 C22 C 0.6547(15) 0.7960(15) 0.3830(11) 0.080(5) Uiso 0.70 1 d PD A 1 H22A H 0.6820 0.8532 0.4326 0.120 Uiso 0.70 1 calc PR A 1 H22B H 0.6114 0.7354 0.3996 0.120 Uiso 0.70 1 calc PR A 1 H22C H 0.5926 0.8105 0.3426 0.120 Uiso 0.70 1 calc PR A 1 C22A C 0.666(4) 0.742(4) 0.389(3) 0.093(13) Uiso 0.30 1 d PD A 2 H22D H 0.6498 0.8008 0.4276 0.139 Uiso 0.30 1 calc PR A 2 H22E H 0.6901 0.6965 0.4209 0.139 Uiso 0.30 1 calc PR A 2 H22F H 0.5861 0.7070 0.3489 0.139 Uiso 0.30 1 calc PR A 2 C23 C 0.645(3) 1.108(2) 0.4695(13) 0.118(9) Uiso 0.60 1 d PD A 1 H23A H 0.7174 1.0988 0.5055 0.176 Uiso 0.60 1 calc PR A 1 H23B H 0.5677 1.0505 0.4604 0.176 Uiso 0.60 1 calc PR A 1 H23C H 0.6204 1.1701 0.4964 0.176 Uiso 0.60 1 calc PR A 1 C23A C 0.604(3) 1.062(2) 0.4424(19) 0.079(9) Uiso 0.40 1 d PD A 2 H23D H 0.6593 1.0704 0.4956 0.119 Uiso 0.40 1 calc PR A 2 H23E H 0.5719 0.9900 0.4144 0.119 Uiso 0.40 1 calc PR A 2 H23F H 0.5285 1.0910 0.4530 0.119 Uiso 0.40 1 calc PR A 2 C24 C 1.196(2) 1.1650(13) 0.3006(15) 0.111(6) Uiso 0.70 1 d PD A 1 H24A H 1.1943 1.2123 0.3537 0.167 Uiso 0.70 1 calc PR A 1 H24B H 1.1545 1.1855 0.2543 0.167 Uiso 0.70 1 calc PR A 1 H24C H 1.2879 1.1650 0.2933 0.167 Uiso 0.70 1 calc PR A 1 C24A C 1.116(8) 1.173(2) 0.336(5) 0.18(3) Uiso 0.30 1 d PD A 2 H24D H 1.2061 1.2139 0.3592 0.263 Uiso 0.30 1 calc PR A 2 H24E H 1.0587 1.1776 0.3795 0.263 Uiso 0.30 1 calc PR A 2 H24F H 1.0815 1.1977 0.2900 0.263 Uiso 0.30 1 calc PR A 2 C25 C 0.8780(19) 0.7525(15) 0.4071(11) 0.088(5) Uiso 0.70 1 d PD A 1 H25A H 0.9063 0.8098 0.4566 0.132 Uiso 0.70 1 calc PR A 1 H25B H 0.9559 0.7393 0.3821 0.132 Uiso 0.70 1 calc PR A 1 H25C H 0.8316 0.6928 0.4236 0.132 Uiso 0.70 1 calc PR A 1 C25A C 0.921(3) 0.788(3) 0.390(2) 0.075(11) Uiso 0.30 1 d PD A 2 H25D H 0.9199 0.8090 0.4499 0.113 Uiso 0.30 1 calc PR A 2 H25E H 0.9882 0.8382 0.3730 0.113 Uiso 0.30 1 calc PR A 2 H25F H 0.9438 0.7226 0.3758 0.113 Uiso 0.30 1 calc PR A 2 C27 C 0.5693(17) 1.1186(17) 0.3232(11) 0.069(5) Uiso 0.60 1 d PD A 1 H27A H 0.5029 1.0539 0.3114 0.103 Uiso 0.60 1 calc PR A 1 H27B H 0.5997 1.1296 0.2710 0.103 Uiso 0.60 1 calc PR A 1 H27C H 0.5298 1.1731 0.3485 0.103 Uiso 0.60 1 calc PR A 1 C27A C 0.602(3) 1.161(3) 0.3272(18) 0.076(9) Uiso 0.40 1 d PD A 2 H27D H 0.5182 1.1109 0.3030 0.114 Uiso 0.40 1 calc PR A 2 H27E H 0.6502 1.1783 0.2822 0.114 Uiso 0.40 1 calc PR A 2 H27F H 0.5829 1.2221 0.3609 0.114 Uiso 0.40 1 calc PR A 2 C28 C 0.7819(9) 0.7778(7) 0.3413(6) 0.062(2) Uiso 0.70 1 d PD A 1 C28A C 0.7819(9) 0.7778(7) 0.3413(6) 0.062(2) Uiso 0.30 1 d PD A 2 C29 C 0.6890(9) 1.1172(7) 0.3848(6) 0.064(3) Uiso 0.60 1 d PD A 1 C29A C 0.6890(9) 1.1172(7) 0.3848(6) 0.064(3) Uiso 0.40 1 d PD A 2 C31 C 0.732(2) 0.6806(13) 0.2695(12) 0.088(6) Uiso 0.70 1 d PD A 1 H31A H 0.8050 0.6682 0.2389 0.133 Uiso 0.70 1 calc PR A 1 H31B H 0.6604 0.6885 0.2313 0.133 Uiso 0.70 1 calc PR A 1 H31C H 0.6980 0.6234 0.2929 0.133 Uiso 0.70 1 calc PR A 1 C31A C 0.760(4) 0.706(3) 0.2506(16) 0.062(10) Uiso 0.30 1 d PD A 2 H31D H 0.8201 0.6615 0.2483 0.093 Uiso 0.30 1 calc PR A 2 H31E H 0.7785 0.7467 0.2101 0.093 Uiso 0.30 1 calc PR A 2 H31F H 0.6680 0.6655 0.2369 0.093 Uiso 0.30 1 calc PR A 2 C101 C 0.925(3) 0.503(2) 0.423(2) 0.153(13) Uiso 0.50 1 d PD . 1 H10G H 0.8731 0.5056 0.3737 0.184 Uiso 0.50 1 calc PR . 1 C102 C 0.897(3) 0.541(2) 0.5040(16) 0.148(13) Uiso 0.50 1 d PD B 1 H10H H 0.8236 0.5712 0.5072 0.178 Uiso 0.50 1 calc PR B 1 C103 C 0.965(3) 0.540(2) 0.5810(16) 0.134(11) Uiso 0.50 1 d PD . 1 C104 C 0.928(5) 0.588(4) 0.6609(19) 0.14(2) Uiso 0.25 1 d PD C 1 H10I H 0.9876 0.5815 0.7073 0.210 Uiso 0.25 1 calc PR C 1 H10J H 0.8365 0.5549 0.6644 0.210 Uiso 0.25 1 calc PR C 1 H10K H 0.9359 0.6596 0.6645 0.210 Uiso 0.25 1 calc PR C 1 C201 C 0.561(3) 1.537(2) -0.3652(12) 0.125(10) Uiso 0.50 1 d PD . 2 C202 C 0.481(4) 1.589(2) -0.4032(14) 0.16(3) Uiso 0.25 1 d PD . 2 C203 C 0.440(3) 1.5675(18) -0.4910(15) 0.141(12) Uiso 0.50 1 d PD . 2 C204 C 0.484(4) 1.490(3) -0.5417(12) 0.118(19) Uiso 0.25 1 d PD . 2 C206 C 0.602(5) 1.460(3) -0.4209(17) 0.15(3) Uiso 0.25 1 d PD . 2 Cl2 Cl 0.61997(19) 1.02611(17) -0.05445(14) 0.0504(6) Uani 1 1 d . . . P2 P 0.8700(2) 0.9915(2) 0.35898(15) 0.0539(6) Uani 1 1 d . . . O2 O 0.9161(6) 1.0152(5) 0.4530(4) 0.0675(18) Uani 1 1 d . A . H2D H 0.9313 1.0774 0.4738 0.101 Uiso 1 1 calc R . . Cl3 Cl 0.1967(2) 0.90672(18) -0.14044(16) 0.0596(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 0.0358(6) 0.0503(7) 0.0533(7) 0.0194(5) 0.0027(4) 0.0018(4) Cl1 0.0599(14) 0.0578(14) 0.0650(15) 0.0263(11) -0.0077(11) -0.0034(11) P1 0.0305(10) 0.0369(11) 0.0586(14) 0.0120(10) 0.0075(9) 0.0032(8) O1 0.049(3) 0.041(3) 0.059(4) 0.010(3) 0.015(3) 0.004(3) N1 0.054(5) 0.041(4) 0.096(6) 0.006(4) 0.033(4) -0.002(3) N2 0.091(6) 0.047(5) 0.078(6) 0.012(4) -0.002(5) 0.012(4) N3 0.037(4) 0.046(5) 0.159(9) 0.037(5) -0.005(5) 0.001(3) C1 0.043(5) 0.042(5) 0.074(6) 0.012(4) 0.019(4) 0.006(4) C2 0.043(5) 0.060(6) 0.069(6) 0.013(5) 0.017(4) 0.003(4) C3 0.053(6) 0.094(8) 0.089(8) 0.018(7) -0.007(6) -0.006(6) C4 0.068(7) 0.069(7) 0.095(8) 0.031(6) 0.016(6) 0.020(5) C5 0.044(5) 0.067(6) 0.056(6) 0.014(5) 0.003(4) 0.006(4) C6 0.053(6) 0.080(7) 0.106(9) 0.021(6) 0.003(6) 0.025(5) C7 0.051(6) 0.124(10) 0.100(9) 0.036(8) 0.020(6) 0.013(6) C8 0.090(8) 0.101(9) 0.069(8) 0.008(6) 0.000(6) 0.013(7) C9 0.038(5) 0.054(5) 0.076(6) 0.022(5) 0.020(4) 0.012(4) C10 0.095(10) 0.175(16) 0.104(11) 0.003(11) -0.032(9) 0.022(10) C11 0.077(8) 0.069(7) 0.175(14) 0.043(8) 0.067(9) 0.029(6) C12 0.090(9) 0.107(10) 0.202(16) 0.096(11) 0.069(10) 0.042(8) Cl2 0.0368(10) 0.0605(13) 0.0537(13) 0.0224(10) 0.0082(9) 0.0034(9) P2 0.0368(12) 0.0757(17) 0.0427(13) 0.0027(11) -0.0052(9) 0.0179(11) O2 0.056(4) 0.094(5) 0.048(4) 0.001(3) -0.003(3) 0.029(4) Cl3 0.0351(11) 0.0700(15) 0.0709(15) 0.0319(12) -0.0046(10) -0.0017(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 Cu1 Cl1 2.199(3) . ? Cu1 Cl3 2.202(2) . ? Cu1 Cl2 2.285(2) 2_675 ? Cu1 Cl2 2.297(2) . ? P1 O1 1.494(6) . ? P1 N3 1.595(8) . ? P1 N1 1.610(7) . ? P1 N2 1.619(9) . ? N1 C1 1.487(11) . ? N2 C5 1.468(13) . ? N3 C9 1.475(11) . ? N4 C29 1.524(10) . ? N4 P2 1.624(10) . ? N4A P2 1.70(2) . ? N5 C16 1.479(12) . ? N5 P2 1.601(10) . ? N5A P2 1.57(2) . ? N6 C28 1.401(14) . ? N6 P2 1.683(11) . ? N6A P2 1.43(3) . ? C1 C4 1.507(13) . ? C1 C3 1.511(14) . ? C1 C2 1.522(11) . ? C5 C6 1.511(13) . ? C5 C7 1.519(14) . ? C5 C8 1.537(14) . ? C9 C12 1.474(15) . ? C9 C10 1.484(16) . ? C9 C11 1.496(13) . ? C14 C16 1.542(13) . ? C15 C16 1.550(14) . ? C16 C24 1.495(15) . ? C21 C29 1.529(15) . ? C22 C28 1.561(14) . ? C23 C29 1.506(17) . ? C25 C28 1.542(14) . ? C27 C29 1.521(15) . ? C28 C31 1.516(14) . ? C101 C103 1.387(7) 2_766 ? C101 C102 1.388(7) . ? C102 C103 1.387(7) . ? C103 C101 1.387(7) 2_766 ? C103 C104 1.438(17) . ? C201 C202 1.396(10) . ? C201 C206 1.397(10) . ? C201 C204 1.479(18) 2_684 ? C202 C204 1.38(3) 2_684 ? C202 C203 1.396(10) . ? C203 C204 1.382(10) 2_684 ? C203 C204 1.387(10) . ? C203 C206 1.397(10) 2_684 ? C204 C204 1.31(4) 2_684 ? C204 C202 1.38(3) 2_684 ? C204 C203 1.382(10) 2_684 ? C204 C206 1.42(3) 2_684 ? C204 C201 1.479(18) 2_684 ? C206 C203 1.397(10) 2_684 ? C206 C204 1.42(3) 2_684 ? Cl2 Cu1 2.285(2) 2_675 ? P2 O2 1.498(7) . ? 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 Cl1 Cu1 Cl3 100.46(10) . . ? Cl1 Cu1 Cl2 143.68(10) . 2_675 ? Cl3 Cu1 Cl2 96.87(9) . 2_675 ? Cl1 Cu1 Cl2 96.61(9) . . ? Cl3 Cu1 Cl2 142.57(10) . . ? Cl2 Cu1 Cl2 88.38(8) 2_675 . ? O1 P1 N3 115.3(4) . . ? O1 P1 N1 110.2(4) . . ? N3 P1 N1 108.8(5) . . ? O1 P1 N2 111.2(4) . . ? N3 P1 N2 104.1(5) . . ? N1 P1 N2 106.9(5) . . ? C1 N1 P1 131.3(6) . . ? C5 N2 P1 131.6(7) . . ? C9 N3 P1 136.3(7) . . ? C29 N4 P2 126.0(8) . . ? C16 N5 P2 133.3(9) . . ? C28 N6 P2 131.9(9) . . ? N1 C1 C4 107.7(8) . . ? N1 C1 C3 112.7(8) . . ? C4 C1 C3 111.1(8) . . ? N1 C1 C2 106.8(7) . . ? C4 C1 C2 110.6(8) . . ? C3 C1 C2 108.0(8) . . ? N2 C5 C6 113.4(9) . . ? N2 C5 C7 107.1(8) . . ? C6 C5 C7 109.5(9) . . ? N2 C5 C8 106.3(8) . . ? C6 C5 C8 109.3(9) . . ? C7 C5 C8 111.2(9) . . ? C12 C9 N3 112.1(9) . . ? C12 C9 C10 108.4(12) . . ? N3 C9 C10 105.4(9) . . ? C12 C9 C11 111.9(9) . . ? N3 C9 C11 109.5(8) . . ? C10 C9 C11 109.4(11) . . ? N5 C16 C24 112.4(12) . . ? N5 C16 C14 110.7(9) . . ? C24 C16 C14 114.6(12) . . ? N5 C16 C15 106.5(10) . . ? C24 C16 C15 110.4(13) . . ? C14 C16 C15 101.3(11) . . ? N6 C28 C31 114.8(12) . . ? N6 C28 C25 110.4(11) . . ? C31 C28 C25 106.1(12) . . ? N6 C28 C22 111.2(10) . . ? C31 C28 C22 105.9(12) . . ? C25 C28 C22 108.1(12) . . ? C23 C29 C27 109.9(15) . . ? C23 C29 N4 108.4(13) . . ? C27 C29 N4 103.0(10) . . ? C23 C29 C21 109.7(15) . . ? C27 C29 C21 112.1(13) . . ? N4 C29 C21 113.5(11) . . ? C103 C101 C102 116(3) 2_766 . ? C103 C102 C101 127(3) . . ? C102 C103 C101 117(2) . 2_766 ? C102 C103 C104 120.8(17) . . ? C101 C103 C104 121.9(18) 2_766 . ? C202 C201 C206 116.1(15) . . ? C202 C201 C204 57.2(12) . 2_684 ? C206 C201 C204 58.9(13) . 2_684 ? C204 C202 C201 64.4(11) 2_684 . ? C204 C202 C203 59.8(8) 2_684 . ? C201 C202 C203 124.2(15) . . ? C204 C203 C204 56.7(17) 2_684 . ? C204 C203 C202 59.5(13) 2_684 . ? C204 C203 C202 116.1(15) . . ? C204 C203 C206 117.7(16) 2_684 2_684 ? C204 C203 C206 61.2(13) . 2_684 ? C202 C203 C206 176.6(19) . 2_684 ? C204 C204 C202 122.6(13) 2_684 2_684 ? C204 C204 C203 61.9(10) 2_684 2_684 ? C202 C204 C203 60.8(8) 2_684 2_684 ? C204 C204 C203 61.5(10) 2_684 . ? C202 C204 C203 175(2) 2_684 . ? C203 C204 C203 123.3(17) 2_684 . ? C204 C204 C206 121.0(14) 2_684 2_684 ? C202 C204 C206 116.0(13) 2_684 2_684 ? C203 C204 C206 175(4) 2_684 2_684 ? C203 C204 C206 59.8(8) . 2_684 ? C204 C204 C201 176(6) 2_684 2_684 ? C202 C204 C201 58.4(8) 2_684 2_684 ? C203 C204 C201 119.1(14) 2_684 2_684 ? C203 C204 C201 117.4(14) . 2_684 ? C206 C204 C201 57.7(8) 2_684 2_684 ? C203 C206 C201 122.5(15) 2_684 . ? C203 C206 C204 59.1(8) 2_684 2_684 ? C201 C206 C204 63.4(10) . 2_684 ? Cu1 Cl2 Cu1 91.62(8) 2_675 . ? N6A P2 O2 107.7(13) . . ? N6A P2 N5A 108.2(16) . . ? O2 P2 N5A 117.9(8) . . ? N6A P2 N5 131.1(13) . . ? O2 P2 N5 113.4(5) . . ? N5A P2 N5 27.5(8) . . ? N6A P2 N4 79.5(15) . . ? O2 P2 N4 109.6(4) . . ? N5A P2 N4 125.5(10) . . ? N5 P2 N4 109.1(6) . . ? N6A P2 N6 30.9(13) . . ? O2 P2 N6 109.1(5) . . ? N5A P2 N6 81.4(10) . . ? N5 P2 N6 108.0(6) . . ? N4 P2 N6 107.5(6) . . ? N6A P2 N4A 104.7(16) . . ? O2 P2 N4A 110.8(8) . . ? N5A P2 N4A 106.8(12) . . ? N5 P2 N4A 84.6(9) . . ? N4 P2 N4A 27.3(7) . . ? N6 P2 N4A 128.4(8) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.179 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.105