# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1393 data_global _publ_contact_author ; Prof. Maurizio Lanfranchi Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Universit\`a degli Studi di Parma Viale delle Scienze 78 I-43100 Parma Italy ; _publ_contact_letter ; Date November 10, 1998 Re: Paper submitted to J. Chem. Soc. Dalton Trans. we are sending you the CIF files of the structures inserted in the paper submitted to J. Chem. Soc. Dalton Trans. Yours Sincerely Maurizio Lanfranchi ; _publ_contact_author_phone '[int.code]521 905 424' _publ_contact_author_fax '[int.code]521 905 557' _publ_contact_author_email 'chimic4@ipruniv.cce.unipr.it' _publ_requested_journal 'Dalton Transaction' _publ_requested_coeditor_name 'Janet L Dean ' _publ_section_title ; Chirality in Mononuclear Square Planar Complexes ; _publ_author_name ; Marina Cingi Biagini Maura Ferrari Maurizio Lanfranchi Maria Angela Pellinghelli ; _publ_author_address ; Maurizio Lanfranchi Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Universit`a degli Studi di Parma Centro di Studio per la Strutturistica Diffrattometrica del CNR Viale delle Scienze 78 I-43100 Parma Italy ; data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H19 Cl3 N2 Pt' _chemical_formula_weight 516.75 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' 'Cl' 'Cl' 0.1484 0.1585 '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' '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 'P 1 21/n 1' 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 17.029(8) _cell_length_b 9.523(4) _cell_length_c 11.261(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.42(2) _cell_angle_gamma 90.00 _cell_volume 1783.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 9 _cell_measurement_theta_max 14 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.925 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 8.309 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4197 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Philips PW 1100 diffractometer' _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3292 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_av_sigmaI/netI 0.1139 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3134 _reflns_number_gt 1696 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR-92' _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 w=1/[\s^2^(Fo^2^)+(0.0599P)^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 3134 _refine_ls_number_parameters 185 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1102 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1031 _refine_ls_goodness_of_fit_ref 0.874 _refine_ls_restrained_S_all 0.878 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.53066(3) 0.18717(6) 0.31115(5) 0.0486(2) Uani 1 d . . . Cl1 Cl 0.4378(2) 0.2831(4) 0.4094(3) 0.0681(11) Uani 1 d . . . Cl2 Cl 0.4365(2) 0.1773(5) 0.1312(3) 0.0660(10) Uani 1 d . . . Cl3 Cl 0.6253(2) 0.0942(4) 0.2148(3) 0.0709(11) Uani 1 d . . . N11 N 0.6107(6) 0.1892(13) 0.4688(9) 0.049(3) Uani 1 d . . . C11 C 0.6667(9) 0.2928(17) 0.5038(12) 0.067(4) Uani 1 d D . . C21 C 0.7224(10) 0.285(2) 0.6118(15) 0.089(6) Uani 1 d . . . H21 H 0.7609 0.3553 0.6326 0.09(3) Uiso 1 calc R . . C31 C 0.7208(9) 0.173(2) 0.6895(16) 0.094(6) Uani 1 d . . . H31 H 0.7581 0.1679 0.7631 0.09(3) Uiso 1 calc R . . C41 C 0.6639(10) 0.068(2) 0.6577(14) 0.085(5) Uani 1 d . . . H41 H 0.6612 -0.0084 0.7081 0.09(3) Uiso 1 calc R . . C51 C 0.6111(8) 0.0836(18) 0.5465(13) 0.065(4) Uani 1 d . . . H51 H 0.5725 0.0140 0.5239 0.09(3) Uiso 1 calc R . . C61 C 0.6664(12) 0.4064(17) 0.4142(16) 0.107(7) Uani 1 d D . . H61A H 0.6812 0.3655 0.3432 0.35(9) Uiso 1 calc R . . H61B H 0.6116 0.4402 0.3889 0.35(9) Uiso 1 calc R . . C71 C 0.7193(11) 0.530(2) 0.4522(18) 0.131(8) Uani 1 d D . . H71A H 0.7131 0.5958 0.3862 0.35(9) Uiso 1 calc R . . H71B H 0.7743 0.4998 0.4741 0.35(9) Uiso 1 calc R . . H71C H 0.7047 0.5744 0.5209 0.35(9) Uiso 1 calc R . . N12 N 0.5661(9) 0.2544(14) 0.9483(12) 0.078(4) Uani 1 d . . . H12 H 0.5774 0.2128 1.0177 0.08(2) Uiso 1 calc R . . C12 C 0.6054(11) 0.3758(19) 0.9381(16) 0.092(6) Uani 1 d D . . C22 C 0.5830(10) 0.4328(19) 0.8202(15) 0.080(5) Uani 1 d . . . H22 H 0.6053 0.5185 0.8054 0.08(2) Uiso 1 calc R . . C32 C 0.5306(12) 0.3699(19) 0.7260(17) 0.086(5) Uani 1 d . . . H32 H 0.5193 0.4105 0.6490 0.08(2) Uiso 1 calc R . . C42 C 0.4947(9) 0.244(2) 0.7476(14) 0.076(5) Uani 1 d . . . H42 H 0.4599 0.1965 0.6856 0.08(2) Uiso 1 calc R . . C52 C 0.5121(10) 0.1936(18) 0.8616(16) 0.078(5) Uani 1 d . . . H52 H 0.4855 0.1139 0.8801 0.08(2) Uiso 1 calc R . . C62 C 0.6784(15) 0.420(2) 1.0400(18) 0.147(11) Uani 1 d D . . H62A H 0.6952 0.3463 1.0991 0.24(6) Uiso 1 calc R . . H62B H 0.7238 0.4511 1.0073 0.24(6) Uiso 1 calc R . . C72 C 0.6403(18) 0.537(3) 1.090(2) 0.250(19) Uani 1 d D . . H72A H 0.6784 0.5789 1.1561 0.24(6) Uiso 1 calc R . . H72B H 0.5951 0.5026 1.1201 0.24(6) Uiso 1 calc R . . H72C H 0.6224 0.6058 1.0283 0.24(6) Uiso 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 Pt 0.0505(3) 0.0471(3) 0.0475(3) 0.0047(3) 0.0088(2) -0.0061(3) Cl1 0.072(2) 0.078(3) 0.057(2) 0.003(2) 0.0197(18) 0.013(2) Cl2 0.060(2) 0.079(3) 0.057(2) 0.001(2) 0.0077(17) -0.004(2) Cl3 0.062(2) 0.086(3) 0.068(2) -0.001(2) 0.0237(19) -0.002(2) N11 0.039(6) 0.065(7) 0.047(6) 0.007(7) 0.018(5) -0.012(7) C11 0.068(10) 0.076(12) 0.055(9) -0.011(9) 0.008(8) -0.011(10) C21 0.066(11) 0.113(16) 0.076(12) 0.012(11) -0.010(9) -0.025(11) C31 0.049(9) 0.16(2) 0.065(11) -0.002(14) -0.002(8) 0.006(13) C41 0.074(11) 0.118(16) 0.058(10) 0.018(11) -0.002(9) 0.012(12) C51 0.053(9) 0.088(12) 0.057(9) -0.003(9) 0.014(8) -0.016(9) C61 0.139(17) 0.066(13) 0.102(14) 0.011(11) 0.000(12) -0.056(12) C71 0.117(17) 0.13(2) 0.15(2) 0.007(17) 0.039(15) -0.037(16) N12 0.123(12) 0.063(9) 0.047(8) 0.002(7) 0.014(8) -0.008(9) C12 0.126(16) 0.059(11) 0.081(13) 0.000(10) 0.001(12) -0.027(11) C22 0.097(12) 0.066(11) 0.078(12) 0.027(10) 0.020(10) 0.002(11) C32 0.106(15) 0.070(12) 0.077(13) 0.002(10) 0.009(11) 0.013(11) C42 0.072(11) 0.116(16) 0.042(9) -0.014(9) 0.017(8) -0.018(10) C52 0.099(12) 0.056(10) 0.080(12) -0.013(10) 0.021(10) -0.017(11) C62 0.25(3) 0.11(2) 0.094(17) -0.030(14) 0.065(19) -0.09(2) C72 0.27(4) 0.34(6) 0.11(2) 0.04(3) -0.01(3) -0.01(4) _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 Pt N11 1.992(10) . ? Pt Cl2 2.300(4) . ? Pt Cl3 2.305(4) . ? Pt Cl1 2.305(4) . ? N11 C51 1.332(17) . ? N11 C11 1.370(16) . ? C11 C21 1.373(19) . ? C11 C61 1.479(15) . ? C21 C31 1.39(2) . ? C21 H21 0.9300 . ? C31 C41 1.38(2) . ? C31 H31 0.9300 . ? C41 C51 1.383(18) . ? C41 H41 0.9300 . ? C51 H51 0.9300 . ? C61 C71 1.490(15) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? N12 C52 1.322(18) . ? N12 C12 1.353(19) . ? N12 H12 0.8600 . ? C12 C22 1.41(2) . ? C12 C62 1.559(17) . ? C22 C32 1.37(2) . ? C22 H22 0.9300 . ? C32 C42 1.39(2) . ? C32 H32 0.9300 . ? C42 C52 1.34(2) . ? C42 H42 0.9300 . ? C52 H52 0.9300 . ? C62 C72 1.460(18) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? 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 N11 Pt Cl2 177.9(3) . . ? N11 Pt Cl3 90.6(3) . . ? Cl2 Pt Cl3 89.73(14) . . ? N11 Pt Cl1 88.7(3) . . ? Cl2 Pt Cl1 91.07(14) . . ? Cl3 Pt Cl1 178.92(14) . . ? C51 N11 C11 116.7(11) . . ? C51 N11 Pt 119.0(9) . . ? C11 N11 Pt 124.3(9) . . ? N11 C11 C21 121.5(14) . . ? N11 C11 C61 115.5(12) . . ? C21 C11 C61 122.8(15) . . ? C11 C21 C31 119.7(16) . . ? C11 C21 H21 120.2 . . ? C31 C21 H21 120.2 . . ? C41 C31 C21 120.0(15) . . ? C41 C31 H31 120.0 . . ? C21 C31 H31 120.0 . . ? C51 C41 C31 116.1(17) . . ? C51 C41 H41 122.0 . . ? C31 C41 H41 122.0 . . ? N11 C51 C41 125.9(15) . . ? N11 C51 H51 117.0 . . ? C41 C51 H51 117.0 . . ? C71 C61 C11 118.0(15) . . ? C71 C61 H61A 107.8 . . ? C11 C61 H61A 107.8 . . ? C71 C61 H61B 107.8 . . ? C11 C61 H61B 107.8 . . ? H61A C61 H61B 107.1 . . ? C61 C71 H71A 109.5 . . ? C61 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C61 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C52 N12 C12 126.1(15) . . ? C52 N12 H12 116.9 . . ? C12 N12 H12 116.9 . . ? N12 C12 C22 111.8(15) . . ? N12 C12 C62 120.1(16) . . ? C22 C12 C62 126.9(18) . . ? C32 C22 C12 124.1(17) . . ? C32 C22 H22 117.9 . . ? C12 C22 H22 117.9 . . ? C42 C32 C22 118.6(17) . . ? C42 C32 H32 120.7 . . ? C22 C32 H32 120.7 . . ? C52 C42 C32 117.4(17) . . ? C52 C42 H42 121.3 . . ? C32 C42 H42 121.3 . . ? N12 C52 C42 121.7(17) . . ? N12 C52 H52 119.2 . . ? C42 C52 H52 119.2 . . ? C72 C62 C12 98(2) . . ? C72 C62 H62A 112.1 . . ? C12 C62 H62A 112.1 . . ? C72 C62 H62B 112.1 . . ? C12 C62 H62B 112.1 . . ? H62A C62 H62B 109.8 . . ? C62 C72 H72A 109.5 . . ? C62 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C62 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 1.130 _refine_diff_density_min -1.191 _refine_diff_density_rms 0.183 #=END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H18 Cl2 N2 Pd' _chemical_formula_weight 391.60 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' 'Pd' 'Pd' -0.9988 1.0072 '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 7.453(5) _cell_length_b 7.522(5) _cell_length_c 8.423(6) _cell_angle_alpha 97.36(2) _cell_angle_beta 114.85(2) _cell_angle_gamma 107.97(2) _cell_volume 389.0(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 17 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 196 _exptl_absorpt_coefficient_mu 1.524 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 AED diffractometer' _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1373 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.07 _reflns_number_total 1373 _reflns_number_gt 936 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR-92' _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 w=1/[\s^2^(Fo^2^)+(0.0725P)^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 0.080(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1373 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.0000 0.0000 0.5000 0.0602(3) Uani 1 d S . . Cl Cl 0.0795(2) 0.29196(19) 0.69273(18) 0.0671(4) Uani 1 d . . . N N 0.1765(6) 0.1465(6) 0.3926(5) 0.0490(9) Uani 1 d . . . C1 C 0.0881(7) 0.1983(7) 0.2428(6) 0.0480(11) Uani 1 d . . . C2 C 0.2136(9) 0.2900(8) 0.1700(7) 0.0617(14) Uani 1 d . . . H2 H 0.1515 0.3241 0.0637 0.073(8) Uiso 1 calc R . . C3 C 0.4318(10) 0.3305(8) 0.2565(8) 0.0691(15) Uani 1 d . . . H3 H 0.5178 0.3927 0.2092 0.073(8) Uiso 1 calc R . . C4 C 0.5203(9) 0.2786(9) 0.4118(8) 0.0688(15) Uani 1 d . . . H4 H 0.6667 0.3045 0.4719 0.073(8) Uiso 1 calc R . . C5 C 0.3877(8) 0.1874(8) 0.4771(7) 0.0561(12) Uani 1 d . . . H5 H 0.4470 0.1529 0.5837 0.073(8) Uiso 1 calc R . . C6 C -0.1483(9) 0.1537(9) 0.1595(7) 0.0654(14) Uani 1 d . . . H6A H -0.1728 0.2163 0.2520 0.108(17) Uiso 1 calc R . . H6B H -0.2259 0.0135 0.1284 0.108(17) Uiso 1 calc R . . C7 C -0.2443(10) 0.2153(9) -0.0075(7) 0.0726(16) Uani 1 d . . . H7A H -0.3952 0.1806 -0.0486 0.099(12) Uiso 1 calc R . . H7B H -0.2270 0.1505 -0.1026 0.099(12) Uiso 1 calc R . . H7C H -0.1723 0.3545 0.0214 0.099(12) Uiso 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 Pd 0.0725(5) 0.0640(5) 0.0503(4) 0.0226(3) 0.0391(3) 0.0196(3) Cl 0.0856(10) 0.0569(8) 0.0607(8) 0.0129(6) 0.0490(7) 0.0140(7) N 0.057(3) 0.050(2) 0.045(2) 0.0160(18) 0.0315(19) 0.0164(19) C1 0.056(3) 0.050(3) 0.043(2) 0.017(2) 0.031(2) 0.016(2) C2 0.076(4) 0.059(3) 0.062(3) 0.027(3) 0.047(3) 0.019(3) C3 0.078(4) 0.066(4) 0.074(4) 0.020(3) 0.056(3) 0.015(3) C4 0.051(3) 0.075(4) 0.076(4) 0.011(3) 0.037(3) 0.014(3) C5 0.048(3) 0.068(3) 0.048(3) 0.016(2) 0.022(2) 0.019(2) C6 0.065(3) 0.079(4) 0.059(3) 0.033(3) 0.034(3) 0.026(3) C7 0.078(4) 0.085(4) 0.061(3) 0.033(3) 0.033(3) 0.036(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 Pd N 2.031(4) . ? Pd N 2.031(4) 2_556 ? Pd Cl 2.2988(19) 2_556 ? Pd Cl 2.2988(19) . ? N C1 1.328(6) . ? N C5 1.335(6) . ? C1 C2 1.385(6) . ? C1 C6 1.498(7) . ? C2 C3 1.382(8) . ? C2 H2 0.9300 . ? C3 C4 1.365(8) . ? C3 H3 0.9300 . ? C4 C5 1.373(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.494(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? 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 N Pd N 180.0 . 2_556 ? N Pd Cl 89.90(12) . 2_556 ? N Pd Cl 90.10(12) 2_556 2_556 ? N Pd Cl 90.10(12) . . ? N Pd Cl 89.90(12) 2_556 . ? Cl Pd Cl 180.0 2_556 . ? C1 N C5 120.4(4) . . ? C1 N Pd 122.3(3) . . ? C5 N Pd 117.4(3) . . ? N C1 C2 120.1(4) . . ? N C1 C6 117.2(4) . . ? C2 C1 C6 122.7(4) . . ? C1 C2 C3 119.5(5) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 119.5(5) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 118.4(5) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? N C5 C4 122.1(5) . . ? N C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C1 C6 C7 116.5(4) . . ? C1 C6 H6A 108.2 . . ? C7 C6 H6A 108.2 . . ? C1 C6 H6B 108.2 . . ? C7 C6 H6B 108.2 . . ? H6A C6 H6B 107.3 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.646 _refine_diff_density_min -0.952 _refine_diff_density_rms 0.101 #=END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Cl2 N2 Pd' _chemical_formula_weight 363.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' 0.1215 3.9337 '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 8.603(5) _cell_length_b 10.786(7) _cell_length_c 8.286(5) _cell_angle_alpha 91.17(2) _cell_angle_beta 116.37(2) _cell_angle_gamma 91.54(2) _cell_volume 688.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 21 _cell_measurement_theta_max 35 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 14.274 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5123 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1996 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 59.98 _reflns_number_total 1996 _reflns_number_gt 1660 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR-92' _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 w=1/[\s^2^(Fo^2^)+(0.1312P)^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 0.0011(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1996 _refine_ls_number_parameters 157 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1693 _refine_ls_wR_factor_gt 0.1577 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.26032(6) 0.22548(5) 0.13691(7) 0.0614(3) Uani 1 d . . . Cl1 Cl 0.2731(3) 0.1370(2) -0.1116(3) 0.0774(6) Uani 1 d . . . Cl2 Cl 0.2494(3) 0.3107(3) 0.3900(3) 0.0799(6) Uani 1 d . . . N11 N 0.0003(8) 0.2446(6) -0.0070(8) 0.0599(15) Uani 1 d . . . C11 C -0.0688(10) 0.3317(8) -0.1304(11) 0.0663(19) Uani 1 d . . . C21 C -0.2449(12) 0.3387(9) -0.2251(12) 0.076(2) Uani 1 d . . . H21 H -0.2911 0.3969 -0.3137 0.092 Uiso 1 calc R . . C31 C -0.3549(11) 0.2597(9) -0.1899(12) 0.076(2) Uani 1 d . . . H31 H -0.4746 0.2666 -0.2506 0.091 Uiso 1 calc R . . C41 C -0.2837(12) 0.1706(9) -0.0634(13) 0.078(2) Uani 1 d . . . H41 H -0.3543 0.1156 -0.0380 0.094 Uiso 1 calc R . . C51 C -0.1049(11) 0.1649(8) 0.0248(11) 0.070(2) Uani 1 d . . . H51 H -0.0560 0.1041 0.1088 0.084 Uiso 1 calc R . . C61 C 0.0531(11) 0.4170(8) -0.1640(12) 0.079(2) Uani 1 d . . . H61A H 0.1525 0.4383 -0.0519 0.118 Uiso 1 calc R . . H61B H -0.0049 0.4910 -0.2172 0.118 Uiso 1 calc R . . H61C H 0.0900 0.3762 -0.2445 0.118 Uiso 1 calc R . . N12 N 0.5196(8) 0.1983(6) 0.2819(9) 0.0655(16) Uani 1 d . . . C12 C 0.6405(12) 0.2848(10) 0.3002(12) 0.077(2) Uani 1 d . . . C22 C 0.8095(13) 0.2615(12) 0.3976(14) 0.091(3) Uani 1 d . . . H22 H 0.8930 0.3230 0.4120 0.109 Uiso 1 calc R . . C32 C 0.8617(13) 0.1502(13) 0.4758(14) 0.097(4) Uani 1 d . . . H32 H 0.9788 0.1345 0.5405 0.116 Uiso 1 calc R . . C42 C 0.7340(12) 0.0615(11) 0.4554(14) 0.090(3) Uani 1 d . . . H42 H 0.7630 -0.0151 0.5083 0.108 Uiso 1 calc R . . C52 C 0.5635(12) 0.0898(9) 0.3551(12) 0.078(2) Uani 1 d . . . H52 H 0.4766 0.0306 0.3385 0.094 Uiso 1 calc R . . C62 C 0.5823(13) 0.4087(10) 0.2172(16) 0.100(3) Uani 1 d . . . H62A H 0.5149 0.3968 0.0892 0.149 Uiso 1 calc R . . H62B H 0.6822 0.4619 0.2420 0.149 Uiso 1 calc R . . H62C H 0.5128 0.4461 0.2675 0.149 Uiso 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 Pd 0.0403(4) 0.0779(5) 0.0592(5) 0.0160(3) 0.0155(3) 0.0030(3) Cl1 0.0528(11) 0.1106(16) 0.0632(12) 0.0066(11) 0.0201(9) 0.0102(10) Cl2 0.0572(12) 0.1113(16) 0.0634(12) 0.0074(11) 0.0190(10) 0.0129(11) N11 0.040(3) 0.076(4) 0.058(4) 0.016(3) 0.016(3) 0.004(3) C11 0.057(5) 0.076(5) 0.061(5) 0.003(4) 0.023(4) 0.001(4) C21 0.060(5) 0.090(6) 0.063(5) 0.018(4) 0.012(4) 0.018(4) C31 0.044(4) 0.100(6) 0.071(5) 0.004(5) 0.013(4) 0.008(4) C41 0.057(5) 0.093(6) 0.079(6) 0.005(5) 0.026(5) -0.007(4) C51 0.058(5) 0.086(5) 0.067(5) 0.011(4) 0.029(4) 0.001(4) C61 0.069(5) 0.079(5) 0.085(6) 0.015(4) 0.031(5) 0.003(4) N12 0.045(3) 0.081(4) 0.062(4) 0.018(3) 0.015(3) 0.002(3) C12 0.059(5) 0.102(6) 0.067(5) 0.010(5) 0.027(4) -0.002(5) C22 0.053(5) 0.132(9) 0.078(6) 0.002(6) 0.021(5) 0.003(5) C32 0.047(5) 0.158(11) 0.069(6) -0.012(7) 0.011(4) 0.027(6) C42 0.058(6) 0.119(8) 0.080(6) 0.015(5) 0.016(5) 0.034(5) C52 0.067(5) 0.085(6) 0.072(5) 0.012(4) 0.022(4) 0.014(4) C62 0.074(6) 0.100(7) 0.114(8) 0.025(6) 0.033(6) -0.016(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N11 2.033(6) . ? Pd N12 2.043(6) . ? Pd Cl1 2.300(3) . ? Pd Cl2 2.313(3) . ? N11 C51 1.344(10) . ? N11 C11 1.346(10) . ? C11 C21 1.367(12) . ? C11 C61 1.497(12) . ? C21 C31 1.385(14) . ? C21 H21 0.9300 . ? C31 C41 1.378(14) . ? C31 H31 0.9300 . ? C41 C51 1.383(12) . ? C41 H41 0.9300 . ? C51 H51 0.9300 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? N12 C52 1.315(11) . ? N12 C12 1.333(11) . ? C12 C22 1.347(15) . ? C12 C62 1.509(15) . ? C22 C32 1.366(17) . ? C22 H22 0.9300 . ? C32 C42 1.387(16) . ? C32 H32 0.9300 . ? C42 C52 1.374(12) . ? C42 H42 0.9300 . ? C52 H52 0.9300 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? 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 N11 Pd N12 177.5(2) . . ? N11 Pd Cl1 90.59(19) . . ? N12 Pd Cl1 88.7(2) . . ? N11 Pd Cl2 89.98(19) . . ? N12 Pd Cl2 90.6(2) . . ? Cl1 Pd Cl2 178.81(7) . . ? C51 N11 C11 119.6(7) . . ? C51 N11 Pd 117.2(5) . . ? C11 N11 Pd 123.2(5) . . ? N11 C11 C21 120.5(8) . . ? N11 C11 C61 117.8(7) . . ? C21 C11 C61 121.6(8) . . ? C11 C21 C31 120.5(8) . . ? C11 C21 H21 119.8 . . ? C31 C21 H21 119.8 . . ? C41 C31 C21 118.8(8) . . ? C41 C31 H31 120.6 . . ? C21 C31 H31 120.6 . . ? C51 C41 C31 118.5(9) . . ? C51 C41 H41 120.8 . . ? C31 C41 H41 120.8 . . ? N11 C51 C41 122.0(8) . . ? N11 C51 H51 119.0 . . ? C41 C51 H51 119.0 . . ? C11 C61 H61A 109.5 . . ? C11 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C11 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C52 N12 C12 120.8(8) . . ? C52 N12 Pd 116.9(6) . . ? C12 N12 Pd 122.3(6) . . ? N12 C12 C22 119.5(10) . . ? N12 C12 C62 118.4(8) . . ? C22 C12 C62 122.0(10) . . ? C32 C22 C12 121.9(12) . . ? C32 C22 H22 119.1 . . ? C12 C22 H22 119.1 . . ? C22 C32 C42 117.7(9) . . ? C22 C32 H32 121.1 . . ? C42 C32 H32 121.1 . . ? C52 C42 C32 118.2(10) . . ? C52 C42 H42 120.9 . . ? C32 C42 H42 120.9 . . ? N12 C52 C42 121.9(10) . . ? N12 C52 H52 119.1 . . ? C42 C52 H52 119.1 . . ? C12 C62 H62A 109.5 . . ? C12 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C12 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 59.98 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.203 _refine_diff_density_min -1.135 _refine_diff_density_rms 0.143 #=END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H18 I2 N2 Pt' _chemical_formula_weight 663.19 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' 'I' 'I' -0.4742 1.8119 '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 'P 1 21/a 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 10.693(6) _cell_length_b 13.656(7) _cell_length_c 11.749(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.41(2) _cell_angle_gamma 90.00 _cell_volume 1712.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 18 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 11.788 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6179 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 AED diffractometer' _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5212 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 30.04 _reflns_number_total 5001 _reflns_number_gt 3091 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR-92' _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 w=1/[\s^2^(Fo^2^)+(0.0817P)^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 5001 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.52561(3) 0.54157(2) 0.23964(3) 0.03914(11) Uani 1 d . . . I1 I 0.49551(6) 0.71470(4) 0.15207(5) 0.05582(17) Uani 1 d . . . I2 I 0.74623(6) 0.58591(5) 0.32552(6) 0.06054(19) Uani 1 d . . . N11 N 0.3505(6) 0.5021(5) 0.1728(6) 0.0431(15) Uani 1 d . . . C11 C 0.2424(8) 0.5286(7) 0.2166(8) 0.048(2) Uani 1 d . . . C21 C 0.1301(9) 0.4975(8) 0.1654(10) 0.060(2) Uani 1 d . . . H21 H 0.0553 0.5162 0.1956 0.12(5) Uiso 1 calc R . . C31 C 0.1277(9) 0.4390(8) 0.0700(9) 0.060(3) Uani 1 d . . . H31 H 0.0518 0.4188 0.0350 0.07(3) Uiso 1 calc R . . C41 C 0.2376(9) 0.4112(7) 0.0273(9) 0.058(2) Uani 1 d . . . H41 H 0.2387 0.3708 -0.0364 0.08(4) Uiso 1 calc R . . C51 C 0.3462(9) 0.4443(7) 0.0809(8) 0.049(2) Uani 1 d . . . H51 H 0.4216 0.4255 0.0517 0.10(5) Uiso 1 calc R . . C61 C 0.2481(10) 0.5946(9) 0.3182(9) 0.063(3) Uani 1 d . . . H61A H 0.2496 0.6618 0.2915 0.08(4) Uiso 1 calc R . . H61B H 0.3267 0.5827 0.3616 0.05(2) Uiso 1 calc R . . C71 C 0.1437(13) 0.5849(10) 0.3976(10) 0.080(4) Uani 1 d . . . H71A H 0.1566 0.6304 0.4595 0.12(3) Uiso 1 calc R . . H71B H 0.1425 0.5194 0.4272 0.12(3) Uiso 1 calc R . . H71C H 0.0652 0.5987 0.3568 0.12(3) Uiso 1 calc R . . N12 N 0.5472(7) 0.4030(5) 0.3102(6) 0.0440(15) Uani 1 d . . . C12 C 0.6197(7) 0.3329(7) 0.2677(7) 0.0453(18) Uani 1 d . . . C22 C 0.6355(11) 0.2442(8) 0.3233(9) 0.066(3) Uani 1 d . . . H22 H 0.6845 0.1953 0.2933 0.08(3) Uiso 1 calc R . . C32 C 0.5784(13) 0.2290(10) 0.4231(10) 0.080(3) Uani 1 d . . . H32 H 0.5914 0.1707 0.4630 0.11(5) Uiso 1 calc R . . C42 C 0.5022(14) 0.2996(9) 0.4642(10) 0.076(3) Uani 1 d . . . H42 H 0.4596 0.2895 0.5299 0.16(8) Uiso 1 calc R . . C52 C 0.4911(9) 0.3852(7) 0.4051(7) 0.052(2) Uani 1 d . . . H52 H 0.4410 0.4341 0.4333 0.04(2) Uiso 1 calc R . . C62 C 0.6786(9) 0.3493(8) 0.1561(8) 0.056(2) Uani 1 d . . . H62A H 0.6381 0.3068 0.0989 0.03(2) Uiso 1 calc R . . H62B H 0.6632 0.4165 0.1321 0.06(3) Uiso 1 calc R . . C72 C 0.8175(12) 0.3305(12) 0.1607(13) 0.092(4) Uani 1 d . . . H72A H 0.8488 0.3427 0.0871 0.16(4) Uiso 1 calc R . . H72B H 0.8336 0.2636 0.1821 0.16(4) Uiso 1 calc R . . H72C H 0.8588 0.3732 0.2160 0.16(4) Uiso 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 Pt 0.04008(17) 0.03855(17) 0.03880(16) -0.00270(13) 0.00238(11) -0.00046(13) I1 0.0705(4) 0.0410(3) 0.0556(3) 0.0020(3) 0.0006(3) 0.0039(3) I2 0.0512(3) 0.0635(4) 0.0653(4) -0.0017(3) -0.0099(3) -0.0111(3) N11 0.048(4) 0.035(3) 0.046(4) -0.003(3) 0.002(3) 0.001(3) C11 0.045(4) 0.047(5) 0.053(5) -0.007(4) 0.006(4) 0.010(4) C21 0.040(4) 0.059(6) 0.080(7) -0.006(5) -0.004(4) -0.002(5) C31 0.051(5) 0.073(7) 0.054(5) 0.002(5) -0.014(4) -0.008(5) C41 0.056(5) 0.053(6) 0.064(6) -0.004(5) -0.001(5) -0.008(4) C51 0.044(4) 0.050(5) 0.054(5) -0.006(4) 0.003(4) -0.002(4) C61 0.055(5) 0.066(7) 0.069(6) -0.011(5) 0.019(5) 0.012(5) C71 0.092(9) 0.086(9) 0.064(7) 0.004(6) 0.023(6) 0.023(7) N12 0.045(4) 0.051(4) 0.036(3) -0.010(3) 0.000(3) -0.001(3) C12 0.041(4) 0.047(5) 0.047(4) -0.005(4) 0.001(3) 0.009(4) C22 0.086(7) 0.049(5) 0.062(6) 0.005(5) -0.001(5) 0.017(5) C32 0.108(10) 0.067(7) 0.064(7) 0.018(6) 0.000(6) 0.005(7) C42 0.114(10) 0.058(7) 0.055(6) 0.005(5) 0.014(6) -0.015(7) C52 0.062(5) 0.050(5) 0.046(4) 0.000(4) 0.018(4) -0.004(4) C62 0.064(6) 0.057(6) 0.049(5) -0.004(4) 0.017(4) 0.011(5) C72 0.069(7) 0.092(10) 0.119(11) -0.020(8) 0.042(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 Pt N11 2.059(7) . ? Pt N12 2.074(8) . ? Pt I2 2.5820(14) . ? Pt I1 2.5909(13) . ? N11 C51 1.337(11) . ? N11 C11 1.342(11) . ? C11 C21 1.378(13) . ? C11 C61 1.494(13) . ? C21 C31 1.376(15) . ? C21 H21 0.9300 . ? C31 C41 1.358(15) . ? C31 H31 0.9300 . ? C41 C51 1.365(13) . ? C41 H41 0.9300 . ? C51 H51 0.9300 . ? C61 C71 1.503(15) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? N12 C52 1.319(11) . ? N12 C12 1.346(11) . ? C12 C22 1.382(13) . ? C12 C62 1.506(12) . ? C22 C32 1.370(16) . ? C22 H22 0.9300 . ? C32 C42 1.369(18) . ? C32 H32 0.9300 . ? C42 C52 1.361(14) . ? C42 H42 0.9300 . ? C52 H52 0.9300 . ? C62 C72 1.506(16) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? 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 N11 Pt N12 89.5(3) . . ? N11 Pt I2 178.3(2) . . ? N12 Pt I2 88.87(19) . . ? N11 Pt I1 89.9(2) . . ? N12 Pt I1 179.2(2) . . ? I2 Pt I1 91.73(3) . . ? C51 N11 C11 118.7(8) . . ? C51 N11 Pt 116.7(6) . . ? C11 N11 Pt 124.6(6) . . ? N11 C11 C21 119.8(9) . . ? N11 C11 C61 118.3(8) . . ? C21 C11 C61 121.9(8) . . ? C11 C21 C31 120.5(9) . . ? C11 C21 H21 119.7 . . ? C31 C21 H21 119.7 . . ? C41 C31 C21 119.3(9) . . ? C41 C31 H31 120.4 . . ? C21 C31 H31 120.4 . . ? C31 C41 C51 117.9(10) . . ? C31 C41 H41 121.0 . . ? C51 C41 H41 121.0 . . ? N11 C51 C41 123.7(9) . . ? N11 C51 H51 118.2 . . ? C41 C51 H51 118.2 . . ? C11 C61 C71 116.5(10) . . ? C11 C61 H61A 108.2 . . ? C71 C61 H61A 108.2 . . ? C11 C61 H61B 108.2 . . ? C71 C61 H61B 108.2 . . ? H61A C61 H61B 107.3 . . ? C61 C71 H71A 109.5 . . ? C61 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C61 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C52 N12 C12 118.9(8) . . ? C52 N12 Pt 117.4(6) . . ? C12 N12 Pt 123.6(6) . . ? N12 C12 C22 120.3(8) . . ? N12 C12 C62 119.8(8) . . ? C22 C12 C62 119.8(8) . . ? C12 C22 C32 119.3(10) . . ? C12 C22 H22 120.4 . . ? C32 C22 H22 120.4 . . ? C42 C32 C22 120.0(11) . . ? C42 C32 H32 120.0 . . ? C22 C32 H32 120.0 . . ? C32 C42 C52 117.4(11) . . ? C32 C42 H42 121.3 . . ? C52 C42 H42 121.3 . . ? N12 C52 C42 124.0(10) . . ? N12 C52 H52 118.0 . . ? C42 C52 H52 118.0 . . ? C72 C62 C12 114.0(9) . . ? C72 C62 H62A 108.8 . . ? C12 C62 H62A 108.8 . . ? C72 C62 H62B 108.8 . . ? C12 C62 H62B 108.8 . . ? H62A C62 H62B 107.7 . . ? C62 C72 H72A 109.5 . . ? C62 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C62 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 2.487 _refine_diff_density_min -2.176 _refine_diff_density_rms 0.238 #=END