Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Angeloni, Alessandro' 'Orpen, A.' _publ_contact_author_name 'Prof A Orpen' _publ_contact_author_address ; Prof A Orpen School of Chemistry University of Bristol Bristol BS8 1TS UNITED KINGDOM ; _publ_contact_author_email 'guy.orpen@bristol.ac.uk' #----------------------------------------------------------------- data_2bilbo _database_code_CSD 154209 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H22 Cl4 N2 Pt' _chemical_formula_weight 507.19 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' 'Pt' 'Pt' -1.7033 8.3905 '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 5.9922(11) _cell_length_b 10.766(3) _cell_length_c 11.601(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.545(12) _cell_angle_gamma 90.00 _cell_volume 744.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 94 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 484 _exptl_absorpt_coefficient_mu 10.117 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.231306 _exptl_absorpt_correction_T_max 0.347068 _exptl_absorpt_process_details ; G. M. Sheldrick. SADABS: A program for absorption correction with the Siemens SMART system; University of G\"ottingen: Germany, 1996. ; _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4671 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 27.52 _reflns_number_total 1700 _reflns_number_gt 1480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SMART (Siemens, 1995b)' _computing_data_reduction 'SMART (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _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^)+(0.0228P)^2^+1.0744P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0046(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1700 _refine_ls_number_parameters 80 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0216 _refine_ls_R_factor_gt 0.0176 _refine_ls_wR_factor_ref 0.0476 _refine_ls_wR_factor_gt 0.0461 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _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 Pt1 Pt 0.0000 0.5000 0.5000 0.01561(8) Uani 1 2 d S . . Cl1 Cl 0.12382(13) 0.64479(7) 0.63838(7) 0.02175(17) Uani 1 1 d . . . Cl2 Cl 0.28252(15) 0.36556(8) 0.56553(8) 0.0319(2) Uani 1 1 d . . . C3 C -0.1056(6) 0.4888(3) 0.9574(3) 0.0164(6) Uani 1 1 d . . . H3A H -0.2122 0.4393 0.9971 0.020 Uiso 1 1 calc R . . N1 N -0.3518(5) 0.5261(3) 0.7277(3) 0.0196(6) Uani 1 1 d . . . H1NA H -0.4725 0.5151 0.6762 0.024 Uiso 1 1 calc R . . H1NB H -0.2518 0.5725 0.6937 0.024 Uiso 1 1 calc R . . C1 C -0.2506(6) 0.4032(3) 0.7599(3) 0.0207(6) Uani 1 1 d . . . H1B H -0.2038 0.3632 0.6913 0.025 Uiso 1 1 calc R . . H1C H -0.3621 0.3507 0.7908 0.025 Uiso 1 1 calc R . . C4 C -0.2191(5) 0.6122(3) 0.9193(3) 0.0206(7) Uani 1 1 d . . . H4A H -0.2668 0.6543 0.9866 0.025 Uiso 1 1 calc R . . H4B H -0.1112 0.6651 0.8858 0.025 Uiso 1 1 calc R . . C5 C -0.4202(6) 0.5926(3) 0.8314(3) 0.0225(7) Uani 1 1 d . . . H5A H -0.5330 0.5445 0.8661 0.027 Uiso 1 1 calc R . . H5B H -0.4851 0.6724 0.8082 0.027 Uiso 1 1 calc R . . C2 C -0.0486(5) 0.4170(3) 0.8500(3) 0.0196(6) Uani 1 1 d . . . H2A H 0.0704 0.4600 0.8153 0.023 Uiso 1 1 calc R . . H2B H 0.0064 0.3352 0.8734 0.023 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 Pt1 0.01449(11) 0.01768(11) 0.01450(11) 0.00097(6) 0.00063(6) -0.00019(6) Cl1 0.0230(4) 0.0216(4) 0.0200(4) -0.0016(3) -0.0013(3) -0.0026(3) Cl2 0.0269(4) 0.0256(4) 0.0398(5) -0.0046(4) -0.0139(4) 0.0068(4) C3 0.0191(16) 0.0158(15) 0.0138(15) 0.0000(11) -0.0006(12) -0.0024(11) N1 0.0180(14) 0.0235(14) 0.0167(14) 0.0007(11) -0.0015(10) -0.0001(11) C1 0.0240(16) 0.0193(15) 0.0182(15) -0.0018(12) -0.0011(12) -0.0018(13) C4 0.0202(16) 0.0206(16) 0.0204(16) -0.0036(12) -0.0018(12) 0.0032(12) C5 0.0201(16) 0.0270(17) 0.0200(16) -0.0017(13) 0.0008(12) 0.0027(13) C2 0.0213(16) 0.0177(15) 0.0190(16) -0.0020(12) -0.0014(12) 0.0015(12) _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 Pt1 Cl2 2.3000(9) . ? Pt1 Cl2 2.3001(9) 3_566 ? Pt1 Cl1 2.3081(9) 3_566 ? Pt1 Cl1 2.3081(9) . ? C3 C2 1.532(4) . ? C3 C4 1.538(4) . ? C3 C3 1.548(7) 3_567 ? N1 C1 1.488(4) . ? N1 C5 1.492(4) . ? C1 C2 1.528(4) . ? C4 C5 1.516(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Pt1 Cl2 180.0 . 3_566 ? Cl2 Pt1 Cl1 88.95(3) . 3_566 ? Cl2 Pt1 Cl1 91.05(3) 3_566 3_566 ? Cl2 Pt1 Cl1 91.05(3) . . ? Cl2 Pt1 Cl1 88.95(3) 3_566 . ? Cl1 Pt1 Cl1 180.00(4) 3_566 . ? C2 C3 C4 109.2(3) . . ? C2 C3 C3 111.4(3) . 3_567 ? C4 C3 C3 111.1(3) . 3_567 ? C1 N1 C5 111.2(3) . . ? N1 C1 C2 111.2(3) . . ? C5 C4 C3 112.0(3) . . ? N1 C5 C4 110.3(3) . . ? C1 C2 C3 112.4(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.661 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.111 data_3faramir _database_code_CSD 154210 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H12 Cl4 N2 Pt' _chemical_formula_weight 425.05 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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 12.0729(24) _cell_length_b 8.6976(28) _cell_length_c 10.1510(25) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1065.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 71 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 14.112 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.173285 _exptl_absorpt_correction_T_max 0.261711 _exptl_absorpt_process_details ; G. M. Sheldrick. SADABS: A program for absorption correction with the Siemens SMART system; University of G\"ottingen: Germany, 1996. ; _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3240 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 27.50 _reflns_number_total 646 _reflns_number_gt 533 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SMART (Siemens, 1995b)' _computing_data_reduction 'SMART (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _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^)+(0.0215P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00205(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 646 _refine_ls_number_parameters 30 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0206 _refine_ls_R_factor_gt 0.0160 _refine_ls_wR_factor_ref 0.0389 _refine_ls_wR_factor_gt 0.0384 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 Pt1 Pt 0.5000 1.0000 0.5000 0.01562(12) Uani 1 4 d S . . Cl1 Cl 0.63350(7) 0.94697(12) 0.65543(9) 0.0239(2) Uani 1 1 d . . . N1 N 0.5000 0.6149(5) 0.6000(4) 0.0200(9) Uani 1 2 d S . . H1A H 0.5000 0.5565 0.6732 0.024 Uiso 1 2 calc SR . . H2A H 0.5000 0.7141 0.6253 0.024 Uiso 1 2 calc SR . . C1 C 0.6025(3) 0.5832(5) 0.5234(3) 0.0234(8) Uani 1 1 d . . . H1B H 0.6670 0.6017 0.5783 0.028 Uiso 1 1 calc R . . H1C H 0.6063 0.6517 0.4482 0.028 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 Pt1 0.01436(14) 0.01838(16) 0.01413(15) -0.00138(11) 0.000 0.000 Cl1 0.0180(4) 0.0352(5) 0.0186(4) 0.0005(4) -0.0028(4) 0.0011(3) N1 0.023(2) 0.018(2) 0.019(2) -0.0024(18) 0.000 0.000 C1 0.0202(17) 0.028(2) 0.022(2) -0.0006(15) -0.0010(13) -0.0023(15) _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 Pt1 Cl1 2.3021(9) . ? Pt1 Cl1 2.3021(9) 12_655 ? Pt1 Cl1 2.3021(9) 9_676 ? Pt1 Cl1 2.3021(9) 4_576 ? N1 C1 1.488(4) 12_655 ? N1 C1 1.488(4) . ? C1 C1 1.523(8) 4_566 ? 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 Pt1 Cl1 88.87(4) . 12_655 ? Cl1 Pt1 Cl1 180.0 . 9_676 ? Cl1 Pt1 Cl1 91.13(4) 12_655 9_676 ? Cl1 Pt1 Cl1 91.13(4) . 4_576 ? Cl1 Pt1 Cl1 180.0 12_655 4_576 ? Cl1 Pt1 Cl1 88.87(4) 9_676 4_576 ? C1 N1 C1 112.6(4) 12_655 . ? N1 C1 C1 109.8(3) . 4_566 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.183 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.132 data_4gollum _database_code_CSD 154211 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H16 Cl4 N2 O6 Pt' _chemical_formula_weight 621.16 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' 'Pt' 'Pt' -1.7033 8.3905 '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 6.9551(13) _cell_length_b 8.5188(12) _cell_length_c 8.9795(10) _cell_angle_alpha 86.462(13) _cell_angle_beta 73.017(9) _cell_angle_gamma 66.472(10) _cell_volume 465.61(11) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 91 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 296 _exptl_absorpt_coefficient_mu 8.139 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.802653 _exptl_absorpt_correction_T_max 0.962304 _exptl_absorpt_process_details ; G. M. Sheldrick. SADABS: A program for absorption correction with the Siemens SMART system; University of G\"ottingen: Germany, 1996. ; _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4892 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2114 _reflns_number_gt 2107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SMART (Siemens, 1995b)' _computing_data_reduction 'SMART (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _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^)+(0.0205P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2114 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0190 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0426 _refine_ls_wR_factor_gt 0.0426 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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 Pt1 Pt 1.0000 0.5000 0.5000 0.01824(6) Uani 1 2 d S . . Cl1 Cl 1.29408(13) 0.24101(10) 0.48409(9) 0.02635(18) Uani 1 1 d . . . Cl2 Cl 1.11921(14) 0.61909(10) 0.65991(10) 0.02765(18) Uani 1 1 d . . . N1 N 0.5531(5) 1.3205(4) 0.7034(3) 0.0259(6) Uani 1 1 d . . . H1A H 0.4383 1.3613 0.6716 0.031 Uiso 1 1 calc R . . O1 O 1.1722(5) 1.2181(4) 0.9116(3) 0.0436(7) Uani 1 1 d . . . O2 O 1.2118(5) 0.9548(4) 0.8460(4) 0.0422(7) Uani 1 1 d . . . C4 C 0.7748(6) 1.3637(4) 0.8354(4) 0.0247(7) Uani 1 1 d . . . H4A H 0.8052 1.4362 0.8897 0.030 Uiso 1 1 calc R . . C6 C 1.1125(6) 1.1216(5) 0.8612(4) 0.0287(8) Uani 1 1 d . . . C3 C 0.9107(5) 1.1911(4) 0.8073(4) 0.0230(7) Uani 1 1 d . . . C2 C 0.8642(6) 1.0854(5) 0.7249(4) 0.0279(8) Uani 1 1 d . . . H2A H 0.9549 0.9693 0.7052 0.034 Uiso 1 1 calc R . . C5 C 0.5938(6) 1.4260(4) 0.7812(4) 0.0266(8) Uani 1 1 d . . . H5A H 0.5002 1.5415 0.7989 0.032 Uiso 1 1 calc R . . C1 C 0.6828(6) 1.1541(5) 0.6727(4) 0.0288(8) Uani 1 1 d . . . H1B H 0.6502 1.0851 0.6162 0.035 Uiso 1 1 calc R . . O3 O 1.5919(4) 0.7974(4) 0.8922(4) 0.0322(6) Uani 1 1 d . . . H3 H 1.675(8) 0.769(6) 0.815(6) 0.047(15) Uiso 1 1 d . . . H33 H 1.647(10) 0.814(8) 0.957(7) 0.09(2) Uiso 1 1 d . . . H2 H 1.326(15) 0.931(11) 0.893(10) 0.17(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01664(10) 0.01890(10) 0.01900(10) 0.00186(6) -0.00716(7) -0.00564(7) Cl1 0.0246(4) 0.0226(4) 0.0299(4) -0.0013(3) -0.0138(3) -0.0030(3) Cl2 0.0262(4) 0.0234(4) 0.0346(5) -0.0026(3) -0.0169(4) -0.0051(3) N1 0.0192(14) 0.0298(16) 0.0308(16) 0.0062(13) -0.0124(12) -0.0089(13) O1 0.0483(18) 0.0581(19) 0.0473(17) 0.0171(14) -0.0320(14) -0.0337(16) O2 0.0289(15) 0.0407(17) 0.0582(19) 0.0169(14) -0.0230(14) -0.0098(13) C4 0.0285(18) 0.0275(18) 0.0227(17) 0.0030(14) -0.0094(14) -0.0148(15) C6 0.0258(19) 0.038(2) 0.0284(18) 0.0111(16) -0.0126(15) -0.0167(17) C3 0.0199(17) 0.0284(18) 0.0232(16) 0.0073(14) -0.0085(13) -0.0113(14) C2 0.0262(19) 0.0227(18) 0.0348(19) 0.0047(15) -0.0131(15) -0.0071(15) C5 0.0244(18) 0.0218(17) 0.0314(19) 0.0043(14) -0.0069(15) -0.0082(15) C1 0.0290(19) 0.0265(19) 0.036(2) 0.0009(15) -0.0153(16) -0.0121(16) O3 0.0242(14) 0.0401(16) 0.0275(15) -0.0020(12) -0.0083(13) -0.0068(12) _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 Pt1 Cl2 2.3077(8) . ? Pt1 Cl2 2.3077(8) 2_766 ? Pt1 Cl1 2.3102(8) 2_766 ? Pt1 Cl1 2.3102(8) . ? N1 C5 1.331(5) . ? N1 C1 1.335(4) . ? O1 C6 1.216(5) . ? O2 C6 1.304(5) . ? C4 C5 1.377(5) . ? C4 C3 1.384(5) . ? C6 C3 1.501(5) . ? C3 C2 1.385(5) . ? C2 C1 1.369(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 Cl2 Pt1 Cl2 179.999(1) . 2_766 ? Cl2 Pt1 Cl1 89.67(3) . 2_766 ? Cl2 Pt1 Cl1 90.33(3) 2_766 2_766 ? Cl2 Pt1 Cl1 90.33(3) . . ? Cl2 Pt1 Cl1 89.67(3) 2_766 . ? Cl1 Pt1 Cl1 179.999(2) 2_766 . ? C5 N1 C1 122.8(3) . . ? C5 C4 C3 118.7(3) . . ? O1 C6 O2 125.6(4) . . ? O1 C6 C3 120.6(3) . . ? O2 C6 C3 113.8(3) . . ? C4 C3 C2 119.9(3) . . ? C4 C3 C6 119.5(3) . . ? C2 C3 C6 120.6(3) . . ? C1 C2 C3 119.1(3) . . ? N1 C5 C4 119.8(3) . . ? N1 C1 C2 119.7(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.099 _refine_diff_density_min -0.827 _refine_diff_density_rms 0.116 data_5elrond _database_code_CSD 154212 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Cl4 N4 O2 Pt' _chemical_formula_weight 583.16 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' 'Pt' 'Pt' -1.7033 8.3905 '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 6.8888(13) _cell_length_b 7.7068(18) _cell_length_c 8.2032(15) _cell_angle_alpha 88.779(15) _cell_angle_beta 72.911(19) _cell_angle_gamma 89.466(19) _cell_volume 416.19(15) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 77 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 276 _exptl_absorpt_coefficient_mu 9.083 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.147804 _exptl_absorpt_correction_T_max 0.261655 _exptl_absorpt_process_details ; G. M. Sheldrick. SADABS: A program for absorption correction with the Siemens SMART system; University of G\"ottingen: Germany, 1996. ; _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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4377 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.51 _reflns_number_total 1900 _reflns_number_gt 1900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SMART (Siemens, 1995b)' _computing_data_reduction 'SMART (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _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^)+(0.0338P)^2^+0.3338P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0040(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1900 _refine_ls_number_parameters 107 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0179 _refine_ls_R_factor_gt 0.0179 _refine_ls_wR_factor_ref 0.0472 _refine_ls_wR_factor_gt 0.0472 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 Pt1 Pt 0.5000 0.5000 1.5000 0.02086(8) Uani 1 2 d S . . Cl1 Cl 0.69930(12) 0.68231(11) 1.60281(10) 0.03044(16) Uani 1 1 d . . . Cl2 Cl 0.23011(12) 0.54199(11) 1.74071(10) 0.03100(17) Uani 1 1 d . . . O1 O 0.7981(4) 0.9707(4) 1.1885(4) 0.0418(6) Uani 1 1 d . . . N1 N 0.1172(4) 0.7231(4) 1.2999(4) 0.0310(6) Uani 1 1 d . . . H1A H -0.0063 0.6898 1.3437 0.037 Uiso 1 1 calc R . . N2 N 0.8274(5) 0.8448(5) 0.9370(4) 0.0373(7) Uani 1 1 d . . . H2A H 0.9518 0.8763 0.8940 0.045 Uiso 1 1 calc R . . H2B H 0.7687 0.7858 0.8773 0.045 Uiso 1 1 calc R . . C3 C 0.5078(5) 0.8269(4) 1.1607(4) 0.0248(6) Uani 1 1 d . . . C2 C 0.4121(5) 0.7318(5) 1.0660(4) 0.0308(7) Uani 1 1 d . . . H2C H 0.4802 0.7032 0.9541 0.037 Uiso 1 1 calc R . . C4 C 0.4011(6) 0.8702(5) 1.3258(4) 0.0311(7) Uani 1 1 d . . . H4A H 0.4628 0.9362 1.3902 0.037 Uiso 1 1 calc R . . C6 C 0.7267(5) 0.8871(5) 1.0946(5) 0.0307(7) Uani 1 1 d . . . C5 C 0.2043(6) 0.8158(5) 1.3945(4) 0.0322(7) Uani 1 1 d . . . H5A H 0.1324 0.8433 1.5058 0.039 Uiso 1 1 calc R . . C1 C 0.2146(6) 0.6798(5) 1.1396(5) 0.0349(7) Uani 1 1 d . . . H1B H 0.1489 0.6146 1.0778 0.042 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 Pt1 0.01863(10) 0.02325(10) 0.01985(10) -0.00171(5) -0.00420(6) -0.00091(5) Cl1 0.0260(4) 0.0378(4) 0.0257(3) -0.0068(3) -0.0042(3) -0.0074(3) Cl2 0.0233(4) 0.0401(4) 0.0257(4) -0.0084(3) -0.0006(3) -0.0046(3) O1 0.0341(14) 0.0465(16) 0.0477(15) -0.0011(12) -0.0163(12) -0.0139(11) N1 0.0224(13) 0.0381(15) 0.0297(14) 0.0030(11) -0.0036(11) -0.0025(11) N2 0.0227(14) 0.0531(19) 0.0353(15) 0.0052(13) -0.0070(11) -0.0123(12) C3 0.0222(14) 0.0255(14) 0.0268(15) 0.0009(11) -0.0077(11) -0.0009(11) C2 0.0291(16) 0.0380(18) 0.0237(14) -0.0051(12) -0.0051(12) -0.0039(13) C4 0.0344(17) 0.0322(17) 0.0299(16) -0.0049(13) -0.0141(13) -0.0003(13) C6 0.0217(15) 0.0311(16) 0.0405(18) 0.0073(13) -0.0116(13) -0.0046(12) C5 0.0317(17) 0.0385(18) 0.0234(14) -0.0023(12) -0.0036(12) 0.0039(13) C1 0.0304(17) 0.0421(19) 0.0325(17) -0.0064(14) -0.0089(14) -0.0075(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 Cl2 2.3062(7) 2_668 ? Pt1 Cl2 2.3063(7) . ? Pt1 Cl1 2.3103(8) . ? Pt1 Cl1 2.3103(8) 2_668 ? O1 C6 1.225(5) . ? N1 C5 1.333(5) . ? N1 C1 1.336(5) . ? N2 C6 1.321(5) . ? C3 C2 1.382(5) . ? C3 C4 1.385(5) . ? C3 C6 1.518(4) . ? C2 C1 1.375(5) . ? C4 C5 1.372(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 Cl2 Pt1 Cl2 180.00(4) 2_668 . ? Cl2 Pt1 Cl1 89.44(3) 2_668 . ? Cl2 Pt1 Cl1 90.56(3) . . ? Cl2 Pt1 Cl1 90.56(3) 2_668 2_668 ? Cl2 Pt1 Cl1 89.44(3) . 2_668 ? Cl1 Pt1 Cl1 179.999(2) . 2_668 ? C5 N1 C1 122.5(3) . . ? C2 C3 C4 119.1(3) . . ? C2 C3 C6 123.7(3) . . ? C4 C3 C6 117.2(3) . . ? C1 C2 C3 119.1(3) . . ? C5 C4 C3 120.0(3) . . ? O1 C6 N2 124.4(3) . . ? O1 C6 C3 118.8(3) . . ? N2 C6 C3 116.7(3) . . ? N1 C5 C4 119.3(3) . . ? N1 C1 C2 120.0(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.005 _refine_diff_density_min -1.029 _refine_diff_density_rms 0.115