# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'B. Lippert' _publ_contact_author_email BERNHARD.LIPPERT@UNI-DORTMUND.DE _publ_section_title ; On the many roles of NH3 ligands in mono- and multinuclear complexes of platinum ; loop_ _publ_author_name 'B. Lippert' 'Edda C. Fusch' 'Lars Holland' 'Olga Krizanovic' 'Patrick Lax' 'Matthias Lutterbeck' ; M.Roitzsch ; 'Pablo J. Sanz Miguel' 'Markus Schurmann' 'Lu Yin.' # Attachment '1b_YL105_sanz.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 743520' _audit_creation_date 2008-11-15T18:11:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C10 H24 N10 O2 Pt2, N O3, Cl, 2(H2 O)' _chemical_formula_sum 'C10 H28 Cl N11 O7 Pt2' _chemical_formula_weight 840.06 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 9.6979(3) _cell_length_b 17.2903(5) _cell_length_c 15.1942(6) _cell_angle_alpha 90 _cell_angle_beta 114.677(3) _cell_angle_gamma 90 _cell_volume 2315.08(13) _cell_formula_units_Z 4 _cell_measurement_temperature 383(2) _cell_measurement_reflns_used 7285 _cell_measurement_theta_min 2.5892 _cell_measurement_theta_max 27.4999 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prisms _exptl_crystal_colour orange _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 2.41 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 12.242 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_absorpt_correction_T_min 0.043 _exptl_absorpt_correction_T_max 0.053 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 383(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_unetI/netI 0.0262 _diffrn_reflns_number 11662 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 27.58 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 _reflns_number_total 2634 _reflns_number_gt 2192 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0928P)^2^+5.3701P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2634 _refine_ls_number_parameters 142 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.122 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.821 _refine_diff_density_min -2.395 _refine_diff_density_rms 0.536 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 -0.03154(3) 0.049634(16) 0.337396(18) 0.02007(15) Uani 1 1 d . . . N1 N 0.3595(7) 0.1695(4) 0.5287(4) 0.0265(14) Uani 1 1 d . . . C1 C 0.4483(10) 0.1699(6) 0.6334(6) 0.038(2) Uani 1 1 d . . . H1A H 0.4445 0.1271 0.6554 0.056 Uiso 1 1 calc R . . H1B H 0.4128 0.2105 0.662 0.056 Uiso 1 1 d R . . H1C H 0.5541 0.178 0.6491 0.056 Uiso 1 1 d R . . C2 C 0.2326(9) 0.1232(4) 0.4901(5) 0.0219(15) Uani 1 1 d . . . O2 O 0.1859(7) 0.0911(3) 0.5444(4) 0.0285(13) Uani 1 1 d . . . N3 N 0.1599(7) 0.1158(3) 0.3919(4) 0.0176(12) Uani 1 1 d . . . C4 C 0.2143(8) 0.1539(4) 0.3327(5) 0.0189(14) Uani 1 1 d . . . N4 N 0.1539(7) 0.1397(4) 0.2388(4) 0.0225(13) Uani 1 1 d . . . H4A H 0.1696 0.1751 0.2043 0.027 Uiso 1 1 calc R . . C5 C 0.3362(9) 0.2069(5) 0.3754(6) 0.0255(16) Uani 1 1 d . . . H5A H 0.3662 0.238 0.3366 0.031 Uiso 1 1 calc R . . C6 C 0.4063(9) 0.2116(5) 0.4702(6) 0.0268(17) Uani 1 1 d . . . H6A H 0.4896 0.2443 0.498 0.032 Uiso 1 1 calc R . . N10 N -0.2258(9) -0.0153(4) 0.2816(5) 0.0358(18) Uani 1 1 d . . . H10A H -0.2758 -0.0011 0.2317 0.054 Uiso 1 1 calc R . . H10B H -0.2713 -0.0138 0.3219 0.054 Uiso 1 1 d R . . H10C H -0.2035 -0.0643 0.2742 0.054 Uiso 1 1 d R . . N11 N 0.0800(10) -0.0443(4) 0.4199(6) 0.0293(16) Uani 1 1 d . . . H11A H 0.1403 -0.0305 0.4671 0.044 Uiso 1 1 calc R . . H11B H 0.1153 -0.0744 0.3861 0.044 Uiso 1 1 d R . . H11C H 0.0155 -0.0714 0.4359 0.044 Uiso 1 1 d R . . N1N N 0.5316(18) 0.0256(11) 0.4583(9) 0.063(5) Uiso 0.5 1 d PD A -1 O11 O 0.5581(19) 0.0566(8) 0.3864(10) 0.059(4) Uiso 0.5 1 d PD A -1 O12 O 0.6192(19) 0.0433(10) 0.5489(9) 0.074(6) Uiso 0.5 1 d PD A -1 O13 O 0.4100(12) -0.0168(6) 0.4385(8) 0.028(3) Uiso 0.5 1 d PD A -1 Cl1 Cl 0 -0.1726(3) 0.25 0.182(5) Uani 1 2 d S . . O1W O 0.2821(11) 0.2173(8) 0.0973(8) 0.113(5) Uani 1 1 d . . . H1W H 0.3536 0.2536 0.1486 0.136 Uiso 1 1 d R . . H2W H 0.3348 0.1918 0.0557 0.136 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0271(2) 0.0207(2) 0.0128(2) 0.00015(9) 0.00874(14) -0.00300(11) N1 0.021(3) 0.037(4) 0.016(3) 0.000(3) 0.001(3) 0.001(3) C1 0.031(5) 0.058(6) 0.016(4) -0.001(4) 0.003(3) 0.008(4) C2 0.026(4) 0.022(3) 0.017(3) 0.003(3) 0.009(3) 0.007(3) O2 0.035(3) 0.029(3) 0.018(3) 0.003(2) 0.007(2) -0.006(2) N3 0.018(3) 0.021(3) 0.016(3) 0.001(2) 0.010(2) 0.005(2) C4 0.018(3) 0.020(3) 0.019(3) 0.002(3) 0.008(3) 0.006(3) N4 0.027(3) 0.025(3) 0.017(3) 0.002(2) 0.010(3) 0.004(3) C5 0.026(4) 0.028(4) 0.026(4) -0.001(3) 0.016(3) -0.005(3) C6 0.021(4) 0.033(4) 0.024(4) -0.004(3) 0.007(3) -0.003(3) N10 0.045(5) 0.042(4) 0.017(3) 0.005(3) 0.008(3) -0.018(4) N11 0.043(4) 0.023(4) 0.026(4) 0.003(3) 0.019(3) -0.001(3) Cl1 0.460(17) 0.036(2) 0.180(7) 0 0.262(10) 0 O1W 0.050(5) 0.200(13) 0.113(9) 0.091(9) 0.057(6) 0.036(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N4 2.006(6) 2 ? Pt1 N3 2.039(6) . ? Pt1 N10 2.048(7) . ? Pt1 N11 2.061(7) . ? Pt1 Pt1 2.9638(5) 2 ? N1 C6 1.365(11) . ? N1 C2 1.376(10) . ? N1 C1 1.459(9) . ? C1 H1A 0.82 . ? C1 H1B 0.9616 . ? C1 H1C 0.9617 . ? C2 O2 1.227(9) . ? C2 N3 1.364(9) . ? N3 C4 1.385(9) . ? C4 N4 1.320(9) . ? C4 C5 1.420(10) . ? N4 Pt1 2.006(6) 2 ? N4 H4A 0.86 . ? C5 C6 1.314(11) . ? C5 H5A 0.93 . ? C6 H6A 0.93 . ? N10 H10A 0.75 . ? N10 H10B 0.8925 . ? N10 H10C 0.8925 . ? N11 H11A 0.75 . ? N11 H11B 0.8931 . ? N11 H11C 0.8929 . ? N1N O12 1.316(9) . ? N1N O11 1.334(8) . ? N1N O13 1.312(8) . ? O1W H1W 1.0161 . ? O1W H2W 1.0614 . ? 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 N4 Pt1 N3 91.0(2) 2 . ? N4 Pt1 N10 88.1(3) 2 . ? N3 Pt1 N10 179.1(3) . . ? N4 Pt1 N11 175.1(3) 2 . ? N3 Pt1 N11 92.1(3) . . ? N10 Pt1 N11 88.8(3) . . ? N4 Pt1 Pt1 77.10(18) 2 2 ? N3 Pt1 Pt1 82.55(16) . 2 ? N10 Pt1 Pt1 97.3(2) . 2 ? N11 Pt1 Pt1 107.0(2) . 2 ? C6 N1 C2 120.9(6) . . ? C6 N1 C1 120.1(7) . . ? C2 N1 C1 118.9(7) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.6 . . ? H1A C1 H1B 113 . . ? N1 C1 H1C 110.7 . . ? H1A C1 H1C 104.8 . . ? H1B C1 H1C 109.1 . . ? O2 C2 N3 121.7(7) . . ? O2 C2 N1 119.5(7) . . ? N3 C2 N1 118.8(7) . . ? C2 N3 C4 120.2(6) . . ? C2 N3 Pt1 117.7(5) . . ? C4 N3 Pt1 122.1(5) . . ? N4 C4 N3 119.8(7) . . ? N4 C4 C5 121.6(7) . . ? N3 C4 C5 118.7(6) . . ? C4 N4 Pt1 131.1(5) . 2 ? C4 N4 H4A 114.5 . . ? Pt1 N4 H4A 114.5 2 . ? C6 C5 C4 119.5(7) . . ? C6 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C5 C6 N1 121.3(8) . . ? C5 C6 H6A 119.3 . . ? N1 C6 H6A 119.3 . . ? Pt1 N10 H10A 109.5 . . ? Pt1 N10 H10B 109.5 . . ? H10A N10 H10B 112.8 . . ? Pt1 N10 H10C 110 . . ? H10A N10 H10C 105.7 . . ? H10B N10 H10C 109.3 . . ? Pt1 N11 H11A 109.5 . . ? Pt1 N11 H11B 109.8 . . ? H11A N11 H11B 113.7 . . ? Pt1 N11 H11C 109.3 . . ? H11A N11 H11C 105.1 . . ? H11B N11 H11C 109.3 . . ? O12 N1N O11 120.2(9) . . ? O12 N1N O13 119.7(9) . . ? O11 N1N O13 119.9(9) . . ? H1W O1W H2W 111.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 C2 O2 -173.9(7) . . . . ? C1 N1 C2 O2 9.1(11) . . . . ? C6 N1 C2 N3 4.5(11) . . . . ? C1 N1 C2 N3 -172.4(7) . . . . ? O2 C2 N3 C4 178.9(7) . . . . ? N1 C2 N3 C4 0.5(10) . . . . ? O2 C2 N3 Pt1 0.4(9) . . . . ? N1 C2 N3 Pt1 -178.0(5) . . . . ? N4 Pt1 N3 C2 121.3(5) 2 . . . ? N11 Pt1 N3 C2 -54.9(5) . . . . ? Pt1 Pt1 N3 C2 -161.8(5) 2 . . . ? N4 Pt1 N3 C4 -57.2(6) 2 . . . ? N11 Pt1 N3 C4 126.6(6) . . . . ? Pt1 Pt1 N3 C4 19.7(5) 2 . . . ? C2 N3 C4 N4 172.5(7) . . . . ? Pt1 N3 C4 N4 -9.1(9) . . . . ? C2 N3 C4 C5 -6.7(10) . . . . ? Pt1 N3 C4 C5 171.7(5) . . . . ? N3 C4 N4 Pt1 -20.3(10) . . . 2 ? C5 C4 N4 Pt1 158.9(6) . . . 2 ? N4 C4 C5 C6 -170.9(8) . . . . ? N3 C4 C5 C6 8.3(11) . . . . ? C4 C5 C6 N1 -3.4(13) . . . . ? C2 N1 C6 C5 -3.0(12) . . . . ? C1 N1 C6 C5 173.9(8) . . . . ? # END of CIF # Attachment '1d_YL171_sanz.cif' data_1b _database_code_depnum_ccdc_archive 'CCDC 743521' _audit_creation_date 2009-07-05T16:21:05-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C10 H24 N10 O2 Pt2), Br4, 4(H2 O)' _chemical_formula_sum 'C20 H56 Br4 N20 O8 Pt4' _chemical_formula_weight 1804.85 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 9.8803(14) _cell_length_b 17.537(4) _cell_length_c 14.2272(15) _cell_angle_alpha 90 _cell_angle_beta 103.613(12) _cell_angle_gamma 90 _cell_volume 2395.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1809 _cell_measurement_theta_min 2.3251 _cell_measurement_theta_max 28.9805 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prisms _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 15.035 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.173 _exptl_absorpt_correction_T_max 0.222 _exptl_absorpt_process_details sadabs #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_unetI/netI 0.2184 _diffrn_reflns_number 6204 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 29.01 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.967 _diffrn_measured_fraction_theta_max 0.824 _reflns_number_total 2640 _reflns_number_gt 1316 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2640 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1187 _refine_ls_R_factor_gt 0.054 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.111 _refine_ls_goodness_of_fit_ref 0.841 _refine_ls_restrained_S_all 0.841 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.686 _refine_diff_density_min -2.288 _refine_diff_density_rms 0.323 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 -0.11602(6) 0.20311(4) 0.16205(4) 0.02157(18) Uani 1 1 d . . . O2 O -0.1177(11) 0.1542(6) -0.0448(7) 0.028(3) Uani 1 1 d . . . N1 N 0.0744(13) 0.0819(9) -0.0285(8) 0.032(4) Uani 1 1 d . . . N3 N 0.0169(12) 0.1358(7) 0.1084(8) 0.017(3) Uani 1 1 d . . . N4 N 0.1664(12) 0.1170(8) 0.2604(8) 0.025(3) Uani 1 1 d . . . H4A H 0.2209 0.0836 0.2939 0.03 Uiso 1 1 d R . . N10 N -0.2495(13) 0.2698(8) 0.2185(8) 0.033(4) Uani 1 1 d . . . H10A H -0.3232 0.2418 0.2222 0.04 Uiso 1 1 d R . . H10B H -0.2772 0.3097 0.18 0.04 Uiso 1 1 d R . . H10C H -0.2069 0.2861 0.2772 0.04 Uiso 1 1 d R . . N20 N -0.0865(12) 0.2928(9) 0.0760(7) 0.027(3) Uani 1 1 d . . . H20A H -0.0151 0.283 0.0496 0.033 Uiso 1 1 d R . . H20B H -0.0687 0.3348 0.1119 0.033 Uiso 1 1 d R . . H20C H -0.1632 0.2998 0.0294 0.033 Uiso 1 1 d R . . C1 C 0.0537(17) 0.0771(11) -0.1362(9) 0.034(5) Uani 1 1 d . . . H1A H -0.0459 0.0727 -0.1664 0.051 Uiso 1 1 calc R . . H1B H 0.1027 0.0322 -0.1526 0.051 Uiso 1 1 calc R . . H1C H 0.0909 0.1231 -0.16 0.051 Uiso 1 1 calc R . . C2 C -0.0153(16) 0.1263(9) 0.0083(10) 0.022(4) Uani 1 1 d . . . C4 C 0.1309(17) 0.1011(10) 0.1661(10) 0.029(4) Uani 1 1 d . . . C5 C 0.2125(16) 0.0504(9) 0.1272(9) 0.020(4) Uani 1 1 d . . . H5A H 0.286 0.0224 0.1674 0.024 Uiso 1 1 calc R . . C6 C 0.1825(15) 0.0430(11) 0.0306(10) 0.031(5) Uani 1 1 d . . . H6A H 0.2378 0.0099 0.0022 0.038 Uiso 1 1 calc R . . Br1 Br 0.0786(5) 0.4752(4) 0.1361(4) 0.101(2) Uani 0.5 1 d P . . Br3 Br 0 0.4217(6) 0.25 0.166(6) Uani 0.5 2 d SP . . Br2 Br 0.25 0.25 0 0.0547(17) Uani 0.5 2 d SP . . O1W O 0.4930(19) 0.1762(13) 0.1541(16) 0.153(10) Uani 1 1 d . . . H1W H 0.4212 0.1983 0.1643 0.23 Uiso 1 1 d R . . H2W H 0.4667 0.1345 0.1251 0.237 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0213(3) 0.0297(4) 0.0121(2) 0.0006(4) 0.00081(18) 0.0035(5) O2 0.038(7) 0.030(8) 0.014(5) 0.000(5) -0.001(5) 0.020(6) N1 0.031(8) 0.055(11) 0.010(6) 0.000(7) 0.004(6) 0.004(8) N3 0.011(6) 0.021(8) 0.018(6) -0.009(6) 0.001(5) -0.009(6) N4 0.022(7) 0.027(9) 0.027(7) 0.010(7) 0.006(6) 0.004(7) N10 0.023(7) 0.044(11) 0.027(7) 0.000(7) -0.003(6) 0.016(7) N20 0.038(7) 0.023(8) 0.018(6) -0.004(7) 0.001(5) -0.003(8) C1 0.047(11) 0.047(13) 0.012(8) -0.001(8) 0.015(7) 0.003(10) C2 0.035(9) 0.014(9) 0.015(7) -0.006(7) 0.002(7) 0.001(8) C4 0.045(10) 0.036(12) 0.006(7) -0.010(8) 0.009(7) -0.013(10) C5 0.031(9) 0.017(9) 0.015(7) 0.004(7) 0.011(7) -0.002(8) C6 0.011(8) 0.056(14) 0.027(9) 0.012(9) 0.004(7) -0.010(8) Br1 0.049(3) 0.173(7) 0.084(4) -0.075(4) 0.021(3) -0.021(4) Br3 0.202(12) 0.067(7) 0.157(9) 0 -0.104(9) 0 Br2 0.040(3) 0.029(4) 0.094(5) 0.020(3) 0.013(3) -0.009(3) O1W 0.066(12) 0.18(3) 0.21(2) -0.062(19) 0.016(14) -0.024(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N4 2.000(13) 2 ? Pt1 N10 2.062(12) . ? Pt1 N3 2.043(12) . ? Pt1 N20 2.057(13) . ? Pt1 Pt1 2.9695(13) 2 ? O2 C2 1.214(17) . ? N1 C6 1.375(19) . ? N1 C2 1.373(19) . ? N1 C1 1.500(16) . ? N3 C4 1.370(19) . ? N3 C2 1.394(17) . ? N4 C4 1.335(16) . ? N4 Pt1 2.000(13) 2 ? N4 H4A 0.8599 . ? N10 H10A 0.89 . ? N10 H10B 0.8899 . ? N10 H10C 0.89 . ? N20 H20A 0.89 . ? N20 H20B 0.89 . ? N20 H20C 0.89 . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C4 C5 1.40(2) . ? C5 C6 1.342(18) . ? C5 H5A 0.95 . ? C6 H6A 0.95 . ? Br1 Br3 2.169(7) . ? Br3 Br1 2.169(7) 2 ? O1W H1W 0.8504 . ? O1W H2W 0.8501 . ? 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 N4 Pt1 N10 87.1(5) 2 . ? N4 Pt1 N3 92.0(5) 2 . ? N10 Pt1 N3 178.9(5) . . ? N4 Pt1 N20 173.9(5) 2 . ? N10 Pt1 N20 89.5(5) . . ? N3 Pt1 N20 91.5(5) . . ? N4 Pt1 Pt1 77.2(3) 2 2 ? N10 Pt1 Pt1 96.3(3) . 2 ? N3 Pt1 Pt1 83.0(3) . 2 ? N20 Pt1 Pt1 108.2(3) . 2 ? C6 N1 C2 121.8(13) . . ? C6 N1 C1 119.7(13) . . ? C2 N1 C1 118.5(13) . . ? C4 N3 C2 121.1(13) . . ? C4 N3 Pt1 122.9(9) . . ? C2 N3 Pt1 116.0(10) . . ? C4 N4 Pt1 132.3(12) . 2 ? C4 N4 H4A 113.2 . . ? Pt1 N4 H4A 114.5 2 . ? Pt1 N10 H10A 108.5 . . ? Pt1 N10 H10B 109.8 . . ? H10A N10 H10B 109.5 . . ? Pt1 N10 H10C 110.1 . . ? H10A N10 H10C 109.5 . . ? H10B N10 H10C 109.5 . . ? Pt1 N20 H20A 109.8 . . ? Pt1 N20 H20B 109.1 . . ? H20A N20 H20B 109.5 . . ? Pt1 N20 H20C 109.4 . . ? H20A N20 H20C 109.5 . . ? H20B N20 H20C 109.5 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C2 N3 123.0(14) . . ? O2 C2 N1 120.6(13) . . ? N3 C2 N1 116.4(13) . . ? N3 C4 N4 119.5(15) . . ? N3 C4 C5 120.9(13) . . ? N4 C4 C5 119.5(15) . . ? C6 C5 C4 117.3(15) . . ? C6 C5 H5A 121.4 . . ? C4 C5 H5A 121.4 . . ? C5 C6 N1 122.0(16) . . ? C5 C6 H6A 119 . . ? N1 C6 H6A 119 . . ? Br1 Br3 Br1 128.7(6) 2 . ? H1W O1W H2W 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Pt1 N3 C4 -60.9(12) 2 . . . ? N20 Pt1 N3 C4 124.1(12) . . . . ? Pt1 Pt1 N3 C4 15.9(11) 2 . . . ? N4 Pt1 N3 C2 118.7(11) 2 . . . ? N20 Pt1 N3 C2 -56.3(11) . . . . ? Pt1 Pt1 N3 C2 -164.4(10) 2 . . . ? C4 N3 C2 O2 177.7(15) . . . . ? Pt1 N3 C2 O2 -2(2) . . . . ? C4 N3 C2 N1 -1(2) . . . . ? Pt1 N3 C2 N1 179.2(11) . . . . ? C6 N1 C2 O2 -172.9(16) . . . . ? C1 N1 C2 O2 8(2) . . . . ? C6 N1 C2 N3 6(2) . . . . ? C1 N1 C2 N3 -173.3(13) . . . . ? C2 N3 C4 N4 173.6(13) . . . . ? Pt1 N3 C4 N4 -7(2) . . . . ? C2 N3 C4 C5 -5(2) . . . . ? Pt1 N3 C4 C5 174.6(11) . . . . ? Pt1 N4 C4 N3 -18(2) 2 . . . ? Pt1 N4 C4 C5 160.7(12) 2 . . . ? N3 C4 C5 C6 6(2) . . . . ? N4 C4 C5 C6 -172.3(15) . . . . ? C4 C5 C6 N1 -1(2) . . . . ? C2 N1 C6 C5 -5(2) . . . . ? C1 N1 C6 C5 174.5(15) . . . . ? # END of CIF # Attachment '1e_YL187_sanz.cif' data_1c _database_code_depnum_ccdc_archive 'CCDC 743522' _audit_creation_date 2009-08-09T21:02:14-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C10 H24 N10 O2 Pt2), 2(O4 S), 10.5(H2 O)' _chemical_formula_sum 'C20 H69 N20 O22.50 Pt4 S2' _chemical_formula_weight 1794.43 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 11.8563(7) _cell_length_b 13.9280(8) _cell_length_c 16.1472(10) _cell_angle_alpha 73.828(5) _cell_angle_beta 89.480(5) _cell_angle_gamma 84.522(5) _cell_volume 2548.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7505 _cell_measurement_theta_min 2.1533 _cell_measurement_theta_max 29.0528 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description blocks _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1706 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 11.116 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.292 _exptl_absorpt_correction_T_max 0.329 _exptl_absorpt_process_details sadabs #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_unetI/netI 0.1757 _diffrn_reflns_number 24381 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 29.02 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.836 _reflns_number_total 11340 _reflns_number_gt 6316 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0364P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 11340 _refine_ls_number_parameters 589 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.0975 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.876 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.2 _refine_diff_density_min -3.152 _refine_diff_density_rms 0.285 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.78409(4) 0.70332(3) 0.35947(4) 0.02038(14) Uani 1 1 d . . . Pt2 Pt 0.79291(4) 0.91358(3) 0.36356(3) 0.01503(12) Uani 1 1 d . . . Pt3 Pt 0.72808(4) 1.42724(3) 0.20909(3) 0.01467(12) Uani 1 1 d . . . Pt4 Pt 0.92786(4) 1.28114(3) 0.24259(3) 0.01446(12) Uani 1 1 d . . . N11 N 0.8628(8) 0.6128(6) 0.4699(7) 0.025(3) Uani 1 1 d . . . H11A H 0.8244 0.6221 0.5166 0.037 Uiso 1 1 calc R . . H11B H 0.9351 0.6286 0.4725 0.037 Uiso 1 1 calc R . . H11C H 0.8638 0.5474 0.4698 0.037 Uiso 1 1 calc R . . N12 N 0.6320(8) 0.6925(8) 0.4171(8) 0.037(3) Uani 1 1 d . . . H12A H 0.5893 0.7527 0.3993 0.055 Uiso 1 1 calc R . . H12B H 0.6424 0.6755 0.4753 0.055 Uiso 1 1 calc R . . H12C H 0.5959 0.6446 0.4026 0.055 Uiso 1 1 calc R . . N13 N 0.8946(8) 0.8733(7) 0.4713(7) 0.024(3) Uani 1 1 d . . . H13A H 0.9624 0.844 0.4594 0.036 Uiso 1 1 calc R . . H13B H 0.8608 0.829 0.5144 0.036 Uiso 1 1 calc R . . H13C H 0.9058 0.9288 0.4881 0.036 Uiso 1 1 calc R . . N14 N 0.6608(7) 0.9497(6) 0.4330(6) 0.018(2) Uani 1 1 d . . . H14A H 0.6734 1.0055 0.449 0.027 Uiso 1 1 calc R . . H14B H 0.6534 0.8978 0.4809 0.027 Uiso 1 1 calc R . . H14C H 0.5961 0.9621 0.4003 0.027 Uiso 1 1 calc R . . N15 N 0.6261(7) 1.3248(7) 0.2762(7) 0.026(3) Uani 1 1 d . . . H15A H 0.6402 1.2667 0.2611 0.039 Uiso 1 1 calc R . . H15B H 0.5523 1.3492 0.264 0.039 Uiso 1 1 calc R . . H15C H 0.64 1.3128 0.3337 0.039 Uiso 1 1 calc R . . N16 N 0.7290(8) 1.4844(7) 0.3121(7) 0.027(3) Uani 1 1 d . . . H16A H 0.7913 1.5183 0.3104 0.041 Uiso 1 1 calc R . . H16B H 0.7306 1.4334 0.3617 0.041 Uiso 1 1 calc R . . H16C H 0.6654 1.5271 0.3103 0.041 Uiso 1 1 calc R . . N17 N 0.8783(7) 1.1607(6) 0.3370(6) 0.015(2) Uani 1 1 d . . . H17A H 0.9349 1.1097 0.348 0.022 Uiso 1 1 calc R . . H17B H 0.815 1.1397 0.3188 0.022 Uiso 1 1 calc R . . H17C H 0.8629 1.1794 0.3859 0.022 Uiso 1 1 calc R . . N18 N 1.0005(7) 1.3332(6) 0.3352(7) 0.022(3) Uani 1 1 d . . . H18A H 1.0757 1.3118 0.3406 0.033 Uiso 1 1 calc R . . H18B H 0.9664 1.3093 0.3866 0.033 Uiso 1 1 calc R . . H18C H 0.9914 1.4015 0.3193 0.033 Uiso 1 1 calc R . . N1A N 1.1015(7) 0.6403(6) 0.2522(7) 0.019(3) Uani 1 1 d . . . C1A C 1.1753(9) 0.5512(9) 0.2552(9) 0.023(3) Uani 1 1 d . . . H1AA H 1.253 0.569 0.2436 0.035 Uiso 1 1 calc R . . H1AB H 1.1505 0.5205 0.2117 0.035 Uiso 1 1 calc R . . H1AC H 1.1727 0.5035 0.3126 0.035 Uiso 1 1 calc R . . C2A C 0.9975(10) 0.6314(8) 0.2929(9) 0.023(3) Uani 1 1 d . . . O2A O 0.9628(6) 0.5477(5) 0.3214(6) 0.023(2) Uani 1 1 d . . . N3A N 0.9354(7) 0.7177(6) 0.3021(6) 0.014(2) Uani 1 1 d . . . N4A N 0.9243(7) 0.8883(7) 0.2925(7) 0.020(3) Uani 1 1 d . . . H4A H 0.9557 0.9438 0.268 0.024 Uiso 1 1 calc R . . C4A C 0.9760(9) 0.8108(9) 0.2729(8) 0.018(3) Uani 1 1 d . . . C5A C 1.0763(10) 0.8177(10) 0.2227(8) 0.025(2) Uani 1 1 d . . . H5AA H 1.1 0.8814 0.1933 0.03 Uiso 1 1 calc R . . C6A C 1.1363(10) 0.7332(9) 0.2177(9) 0.025(3) Uani 1 1 d . . . H6AA H 1.2065 0.7383 0.1887 0.03 Uiso 1 1 calc R . . N1B N 0.5618(8) 1.0735(7) 0.1634(7) 0.023(3) Uani 1 1 d . . . C1B C 0.4952(9) 1.1738(9) 0.1432(9) 0.028(4) Uani 1 1 d . . . H1BA H 0.448 1.1834 0.0915 0.043 Uiso 1 1 calc R . . H1BB H 0.5471 1.2264 0.1329 0.043 Uiso 1 1 calc R . . H1BC H 0.4467 1.1775 0.1918 0.043 Uiso 1 1 calc R . . C2B C 0.6423(9) 1.0502(9) 0.2303(8) 0.018(3) Uani 1 1 d . . . O2B O 0.6625(6) 1.1128(5) 0.2650(6) 0.023(2) Uani 1 1 d . . . N3B N 0.6872(8) 0.9524(7) 0.2599(7) 0.022(3) Uani 1 1 d . . . C4B C 0.6624(8) 0.8785(8) 0.2200(9) 0.019(3) Uani 1 1 d . . . N4B N 0.7020(7) 0.7830(7) 0.2513(8) 0.025(3) Uani 1 1 d . . . H4B H 0.6892 0.7465 0.2164 0.03 Uiso 1 1 calc R . . C5B C 0.5912(10) 0.9111(9) 0.1432(9) 0.025(2) Uani 1 1 d . . . H5BA H 0.5793 0.8668 0.1095 0.03 Uiso 1 1 calc R . . C6B C 0.5419(10) 1.0070(9) 0.1208(9) 0.030(3) Uani 1 1 d . . . H6BA H 0.4909 1.0278 0.0727 0.036 Uiso 1 1 calc R . . N1C N 0.8619(8) 1.6902(7) 0.0589(7) 0.025(3) Uani 1 1 d . . . C1C C 0.8117(11) 1.7944(9) 0.0170(11) 0.042(4) Uani 1 1 d . . . H1CA H 0.8721 1.8363 -0.0082 0.063 Uiso 1 1 calc R . . H1CB H 0.7722 1.822 0.0602 0.063 Uiso 1 1 calc R . . H1CC H 0.7579 1.7937 -0.0284 0.063 Uiso 1 1 calc R . . C2C C 0.7917(11) 1.6242(9) 0.1096(8) 0.021(3) Uani 1 1 d . . . O2C O 0.6962(6) 1.6550(5) 0.1260(6) 0.022(2) Uani 1 1 d . . . N3C N 0.8343(7) 1.5247(6) 0.1435(6) 0.0116(15) Uani 1 1 d . . . C4C C 0.9439(10) 1.4929(9) 0.1238(8) 0.020(3) Uani 1 1 d . . . N4C N 0.9836(8) 1.3985(7) 0.1559(6) 0.0181(17) Uani 1 1 d . . . H4C H 1.0493 1.3838 0.1344 0.022 Uiso 1 1 calc R . . C5C C 1.0125(9) 1.5644(9) 0.0714(9) 0.022(3) Uani 1 1 d . . . H5CA H 1.0884 1.5452 0.0591 0.026 Uiso 1 1 calc R . . C6C C 0.9666(10) 1.6594(9) 0.0402(9) 0.023(3) Uani 1 1 d . . . H6CA H 1.0105 1.7068 0.0032 0.028 Uiso 1 1 calc R . . N1D N 0.8527(8) 1.1069(7) 0.0757(7) 0.019(2) Uani 1 1 d . . . C1D C 0.8861(11) 1.0028(9) 0.0727(10) 0.036(4) Uani 1 1 d . . . H1DA H 0.8462 0.9899 0.0246 0.053 Uiso 1 1 calc R . . H1DB H 0.8662 0.9556 0.1269 0.053 Uiso 1 1 calc R . . H1DC H 0.9681 0.994 0.0646 0.053 Uiso 1 1 calc R . . C2D C 0.8991(9) 1.1420(8) 0.1387(8) 0.016(3) Uani 1 1 d . . . O2D O 0.9765(6) 1.0881(5) 0.1855(5) 0.021(2) Uani 1 1 d . . . N3D N 0.8554(7) 1.2326(6) 0.1486(6) 0.0116(15) Uani 1 1 d . . . C4D C 0.7700(10) 1.2911(8) 0.0924(8) 0.022(3) Uani 1 1 d . . . N4D N 0.7227(7) 1.3721(7) 0.1073(7) 0.0181(17) Uani 1 1 d . . . H4D H 0.6797 1.4105 0.0643 0.022 Uiso 1 1 calc R . . C5D C 0.7358(10) 1.2544(10) 0.0216(9) 0.030(3) Uani 1 1 d . . . H5DA H 0.6838 1.2951 -0.0212 0.036 Uiso 1 1 calc R . . C6D C 0.7768(10) 1.1644(9) 0.0163(9) 0.027(3) Uani 1 1 d . . . H6DA H 0.7526 1.1403 -0.0295 0.033 Uiso 1 1 calc R . . S1 S 0.8140(3) 1.2963(2) 0.5247(2) 0.0212(7) Uani 1 1 d . . . O11 O 0.7625(15) 1.2912(13) 0.4449(13) 0.014(5) Uiso 0.449(17) 1 d P A 1 O12 O 0.9384(17) 1.3043(16) 0.5053(15) 0.042(7) Uiso 0.449(17) 1 d P A 1 O13 O 0.782(3) 1.386(3) 0.546(3) 0.114(14) Uiso 0.449(17) 1 d P A 1 O14 O 0.8154(17) 1.2077(16) 0.5973(16) 0.045(7) Uiso 0.449(17) 1 d P A 1 O15 O 0.7140(17) 1.3141(14) 0.4613(14) 0.045(6) Uiso 0.551(17) 1 d P A 2 O16 O 0.8830(12) 1.3783(11) 0.4959(11) 0.028(5) Uiso 0.551(17) 1 d P A 2 O17 O 0.7556(18) 1.2934(18) 0.6008(17) 0.079(8) Uiso 0.551(17) 1 d P A 2 O18 O 0.8747(17) 1.2046(16) 0.5193(16) 0.068(7) Uiso 0.551(17) 1 d P A 2 S2 S 0.6736(2) 0.7388(3) 0.6461(2) 0.0275(8) Uani 1 1 d . . . O21 O 0.7802(13) 0.7124(11) 0.6050(12) 0.020(4) Uiso 0.498(12) 1 d P B 1 O22 O 0.6424(13) 0.6664(12) 0.7206(13) 0.029(5) Uiso 0.498(12) 1 d P B 1 O23 O 0.7056(13) 0.8394(12) 0.6740(12) 0.032(5) Uiso 0.498(12) 1 d P B 1 O24 O 0.5869(13) 0.7806(12) 0.5758(12) 0.027(5) Uiso 0.498(12) 1 d P B 1 O25 O 0.7331(15) 0.7318(13) 0.5693(13) 0.030(5) Uiso 0.502(12) 1 d P B 2 O26 O 0.6138(12) 0.6343(11) 0.6740(11) 0.020(4) Uiso 0.502(12) 1 d P B 2 O27 O 0.7523(13) 0.7298(12) 0.7143(12) 0.027(5) Uiso 0.502(12) 1 d P B 2 O28 O 0.5866(14) 0.8149(13) 0.6356(14) 0.038(5) Uiso 0.502(12) 1 d P B 2 O1W O 1.2422(7) 1.3681(6) 0.1164(6) 0.041(2) Uani 1 1 d . . . H11 H 1.1727 1.3665 0.1045 0.061 Uiso 1 1 d R . . H12 H 1.2455 1.3758 0.1668 0.061 Uiso 1 1 d R . . O2W O 0.6155(7) 1.1418(6) 0.4810(6) 0.045(3) Uani 1 1 d . . . H21 H 0.6616 1.1853 0.4615 0.067 Uiso 1 1 d R . . H22 H 0.5586 1.1553 0.4467 0.067 Uiso 1 1 d R . . O3W O 0.5686(9) 1.0207(8) 0.6422(9) 0.077(3) Uani 1 1 d . . . H31 H 0.6239 0.976 0.6595 0.116 Uiso 1 1 d R . . H32 H 0.5959 1.0757 0.618 0.116 Uiso 1 1 d R . . O4W O 0.8861(8) 0.9948(8) 0.5963(10) 0.085(3) Uani 1 1 d . . . H41 H 0.8763 0.9893 0.6497 0.127 Uiso 1 1 d R . . H42 H 0.8566 1.0524 0.568 0.127 Uiso 1 1 d R . . O5W O 1.4071(8) 1.5000(9) 0.0527(10) 0.085(3) Uani 1 1 d . . . H51 H 1.3682 1.5402 0.0109 0.127 Uiso 1 1 d R . . H52 H 1.3925 1.4408 0.055 0.127 Uiso 1 1 d R . . O6W O 0.7333(7) 2.0077(7) -0.1193(7) 0.045(3) Uani 1 1 d . . . H61 H 0.6858 2.0225 -0.0841 0.067 Uiso 1 1 d R . . H62 H 0.7811 2.0509 -0.1296 0.067 Uiso 1 1 d R . . O7W O 1.4736(8) 1.6144(9) 0.1504(9) 0.081(4) Uani 1 1 d . . . H71 H 1.4385 1.6707 0.1235 0.122 Uiso 1 1 d R . . H72 H 1.5436 1.6224 0.1508 0.122 Uiso 1 1 d R . . O8W O 0.8064(9) 0.8752(8) 0.7879(9) 0.085(3) Uani 1 1 d . . . H81 H 0.8704 0.8552 0.8134 0.127 Uiso 1 1 d R . . H82 H 0.774 0.8226 0.7884 0.127 Uiso 1 1 d R . . O9W O 0.6045(15) 1.1821(13) 0.7011(13) 0.041(2) Uani 0.5 1 d P . . H91 H 0.6757 1.1814 0.7062 0.061 Uiso 0.5 1 d PR . . H92 H 0.5882 1.1216 0.7168 0.061 Uiso 0.5 1 d PR . . O10W O 0.5911(14) 0.4872(13) 0.5343(13) 0.045(3) Uani 0.5 1 d P . . H101 H 0.549 0.4532 0.5717 0.067 Uiso 0.5 1 d PR . . H102 H 0.6352 0.4445 0.5161 0.067 Uiso 0.5 1 d PR . . O11W O 1.3872(9) 1.7917(8) 0.1501(9) 0.077(3) Uani 1 1 d . . . H111 H 1.3503 1.8505 0.1413 0.116 Uiso 1 1 d R . . H112 H 1.4255 1.7796 0.2055 0.116 Uiso 1 1 d R . . O12W O 0.5401(13) 0.5150(13) 0.6739(16) 0.053(7) Uani 0.5 1 d P . . H121 H 0.5929 0.4881 0.7107 0.079 Uiso 0.5 1 d PR . . H122 H 0.5707 0.5374 0.6254 0.079 Uiso 0.5 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0211(2) 0.0115(2) 0.0321(4) -0.0105(2) 0.0089(2) -0.00646(18) Pt2 0.0187(2) 0.0100(2) 0.0170(3) -0.0043(2) -0.0026(2) -0.00264(17) Pt3 0.0178(2) 0.0111(2) 0.0156(3) -0.0038(2) -0.0003(2) -0.00360(17) Pt4 0.0183(2) 0.0107(2) 0.0153(3) -0.0047(2) -0.0021(2) -0.00267(17) N11 0.033(6) 0.009(5) 0.036(8) -0.011(5) 0.015(6) -0.004(4) N12 0.025(6) 0.040(7) 0.053(9) -0.023(7) 0.004(6) -0.006(5) N13 0.036(6) 0.014(5) 0.019(7) 0.001(5) -0.002(5) -0.007(4) N14 0.026(5) 0.011(5) 0.016(6) -0.005(5) -0.002(5) 0.000(4) N15 0.030(6) 0.014(5) 0.040(8) -0.014(5) -0.019(6) -0.001(4) N16 0.036(6) 0.017(5) 0.028(7) -0.007(5) -0.009(6) 0.002(4) N17 0.019(5) 0.020(5) 0.012(6) -0.013(5) 0.006(5) -0.009(4) N18 0.024(5) 0.014(5) 0.024(7) 0.002(5) -0.020(5) -0.007(4) N1A 0.019(5) 0.009(5) 0.028(7) -0.005(5) -0.004(5) 0.002(4) C1A 0.014(6) 0.038(8) 0.023(8) -0.017(7) -0.001(6) -0.003(5) C2A 0.034(7) 0.012(6) 0.022(8) -0.001(6) -0.011(7) -0.006(5) O2A 0.032(5) 0.009(4) 0.036(6) -0.015(4) 0.005(4) -0.010(3) N3A 0.013(5) 0.014(5) 0.016(6) -0.006(5) -0.004(5) -0.001(4) N4A 0.023(5) 0.012(5) 0.030(7) -0.010(5) 0.005(5) -0.006(4) C4A 0.011(6) 0.026(7) 0.016(7) -0.005(6) -0.007(6) 0.003(5) C5A 0.028(5) 0.035(5) 0.019(6) -0.017(5) -0.001(5) -0.002(4) C6A 0.020(6) 0.039(8) 0.024(8) -0.019(7) 0.009(6) -0.010(6) N1B 0.022(5) 0.025(6) 0.026(7) -0.016(6) -0.006(5) -0.001(4) C1B 0.015(6) 0.034(7) 0.030(9) 0.003(7) -0.009(6) -0.009(5) C2B 0.014(6) 0.031(7) 0.010(7) -0.006(6) 0.004(6) -0.001(5) O2B 0.036(5) 0.006(4) 0.029(6) -0.008(4) -0.004(5) -0.005(3) N3B 0.038(6) 0.015(5) 0.015(6) -0.009(5) -0.003(5) 0.003(4) C4B 0.010(6) 0.019(6) 0.030(9) -0.012(6) 0.002(6) 0.000(5) N4B 0.022(5) 0.021(5) 0.044(8) -0.028(6) 0.001(6) -0.002(4) C5B 0.028(5) 0.035(5) 0.019(6) -0.017(5) -0.001(5) -0.002(4) C6B 0.034(7) 0.029(7) 0.025(9) -0.007(7) -0.016(7) 0.006(6) N1C 0.031(6) 0.012(5) 0.031(7) -0.002(5) -0.003(6) -0.007(4) C1C 0.046(9) 0.023(7) 0.052(12) -0.003(8) 0.013(8) -0.003(6) C2C 0.041(8) 0.018(6) 0.010(7) -0.007(6) -0.001(7) -0.019(6) O2C 0.027(5) 0.011(4) 0.026(6) -0.001(4) 0.011(4) -0.004(3) N3C 0.016(3) 0.007(3) 0.014(4) -0.006(3) 0.004(3) -0.006(3) C4C 0.036(7) 0.020(6) 0.008(7) -0.008(6) -0.005(6) -0.012(5) N4C 0.022(4) 0.022(4) 0.013(4) -0.008(4) 0.006(3) -0.003(3) C5C 0.020(6) 0.023(7) 0.024(8) -0.007(6) 0.003(6) -0.013(5) C6C 0.029(7) 0.025(7) 0.018(8) -0.005(6) 0.001(7) -0.014(6) N1D 0.022(5) 0.023(5) 0.020(6) -0.016(5) 0.000(5) -0.003(4) C1D 0.045(8) 0.028(7) 0.034(10) -0.016(7) -0.024(8) 0.019(6) C2D 0.027(7) 0.014(6) 0.006(7) -0.001(5) 0.002(6) -0.006(5) O2D 0.025(4) 0.018(4) 0.016(5) -0.001(4) 0.004(4) 0.000(3) N3D 0.016(3) 0.007(3) 0.014(4) -0.006(3) 0.004(3) -0.006(3) C4D 0.039(7) 0.014(6) 0.014(7) 0.001(6) 0.010(6) -0.016(5) N4D 0.022(4) 0.022(4) 0.013(4) -0.008(4) 0.006(3) -0.003(3) C5D 0.036(8) 0.042(8) 0.015(8) -0.014(7) -0.008(7) 0.005(6) C6D 0.040(8) 0.021(7) 0.029(9) -0.017(7) -0.017(7) -0.005(6) S1 0.0283(17) 0.0172(15) 0.0194(19) -0.0069(15) 0.0034(16) -0.0028(13) S2 0.0181(16) 0.043(2) 0.023(2) -0.0133(18) -0.0002(16) 0.0036(14) O1W 0.050(5) 0.043(5) 0.039(6) -0.028(5) 0.015(5) -0.012(4) O2W 0.039(5) 0.036(5) 0.039(6) 0.020(5) 0.012(5) 0.004(4) O3W 0.069(5) 0.059(5) 0.096(8) -0.013(6) -0.016(6) 0.003(4) O4W 0.053(4) 0.078(5) 0.145(8) -0.071(6) -0.011(5) 0.004(3) O5W 0.053(4) 0.078(5) 0.145(8) -0.071(6) -0.011(5) 0.004(3) O6W 0.033(5) 0.055(6) 0.051(8) -0.020(6) 0.006(5) -0.010(5) O7W 0.041(6) 0.128(11) 0.098(12) -0.062(10) 0.016(7) -0.039(7) O8W 0.053(4) 0.078(5) 0.145(8) -0.071(6) -0.011(5) 0.004(3) O9W 0.050(5) 0.043(5) 0.039(6) -0.028(5) 0.015(5) -0.012(4) O10W 0.039(5) 0.036(5) 0.039(6) 0.020(5) 0.012(5) 0.004(4) O11W 0.069(5) 0.059(5) 0.096(8) -0.013(6) -0.016(6) 0.003(4) O12W 0.027(10) 0.038(11) 0.09(2) -0.024(13) 0.006(12) 0.006(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N4B 1.994(10) . ? Pt1 N3A 2.013(9) . ? Pt1 N12 2.021(10) . ? Pt1 N11 2.048(10) . ? Pt1 Pt2 2.9593(6) . ? Pt2 N4A 1.989(10) . ? Pt2 N3B 2.017(10) . ? Pt2 N14 2.024(9) . ? Pt2 N13 2.039(9) . ? Pt3 N4D 2.003(10) . ? Pt3 N3C 2.013(8) . ? Pt3 N15 2.029(9) . ? Pt3 N16 2.035(11) . ? Pt3 Pt4 2.9213(6) . ? Pt4 N4C 1.996(9) . ? Pt4 N3D 2.050(9) . ? Pt4 N17 2.057(8) . ? Pt4 N18 2.062(9) . ? N11 H11A 0.91 . ? N11 H11B 0.91 . ? N11 H11C 0.91 . ? N12 H12A 0.91 . ? N12 H12B 0.91 . ? N12 H12C 0.91 . ? N13 H13A 0.91 . ? N13 H13B 0.91 . ? N13 H13C 0.91 . ? N14 H14A 0.91 . ? N14 H14B 0.91 . ? N14 H14C 0.91 . ? N15 H15A 0.91 . ? N15 H15B 0.91 . ? N15 H15C 0.91 . ? N16 H16A 0.91 . ? N16 H16B 0.91 . ? N16 H16C 0.91 . ? N17 H17A 0.91 . ? N17 H17B 0.91 . ? N17 H17C 0.91 . ? N18 H18A 0.91 . ? N18 H18B 0.91 . ? N18 H18C 0.91 . ? N1A C6A 1.361(14) . ? N1A C2A 1.392(15) . ? N1A C1A 1.438(14) . ? C1A H1AA 0.98 . ? C1A H1AB 0.98 . ? C1A H1AC 0.98 . ? C2A O2A 1.236(12) . ? C2A N3A 1.392(14) . ? N3A C4A 1.381(13) . ? N4A C4A 1.305(14) . ? N4A H4A 0.88 . ? C4A C5A 1.429(16) . ? C5A C6A 1.337(16) . ? C5A H5AA 0.95 . ? C6A H6AA 0.95 . ? N1B C6B 1.336(15) . ? N1B C2B 1.394(14) . ? N1B C1B 1.491(15) . ? C1B H1BA 0.98 . ? C1B H1BB 0.98 . ? C1B H1BC 0.98 . ? C2B O2B 1.203(14) . ? C2B N3B 1.368(14) . ? N3B C4B 1.411(14) . ? C4B N4B 1.325(13) . ? C4B C5B 1.445(16) . ? N4B H4B 0.88 . ? C5B C6B 1.358(16) . ? C5B H5BA 0.95 . ? C6B H6BA 0.95 . ? N1C C6C 1.335(15) . ? N1C C2C 1.387(14) . ? N1C C1C 1.488(14) . ? C1C H1CA 0.98 . ? C1C H1CB 0.98 . ? C1C H1CC 0.98 . ? C2C O2C 1.225(14) . ? C2C N3C 1.387(14) . ? N3C C4C 1.395(15) . ? C4C N4C 1.313(14) . ? C4C C5C 1.429(15) . ? N4C H4C 0.88 . ? C5C C6C 1.341(16) . ? C5C H5CA 0.95 . ? C6C H6CA 0.95 . ? N1D C6D 1.350(14) . ? N1D C2D 1.384(14) . ? N1D C1D 1.480(14) . ? C1D H1DA 0.98 . ? C1D H1DB 0.98 . ? C1D H1DC 0.98 . ? C2D O2D 1.241(12) . ? C2D N3D 1.369(14) . ? N3D C4D 1.400(14) . ? C4D N4D 1.293(15) . ? C4D C5D 1.451(17) . ? N4D H4D 0.88 . ? C5D C6D 1.324(17) . ? C5D H5DA 0.95 . ? C6D H6DA 0.95 . ? S1 O17 1.40(3) . ? S1 O13 1.40(4) . ? S1 O18 1.43(2) . ? S1 O16 1.437(15) . ? S1 O14 1.44(2) . ? S1 O11 1.454(19) . ? S1 O12 1.51(2) . ? S1 O15 1.531(19) . ? S2 O28 1.382(18) . ? S2 O22 1.411(17) . ? S2 O27 1.421(16) . ? S2 O25 1.44(2) . ? S2 O21 1.485(17) . ? S2 O24 1.491(17) . ? S2 O26 1.629(15) . ? S2 O23 1.662(17) . ? O1W H11 0.8516 . ? O1W H12 0.852 . ? O2W H21 0.8484 . ? O2W H22 0.8492 . ? O3W H31 0.8502 . ? O3W H32 0.85 . ? O4W H41 0.8518 . ? O4W H42 0.8473 . ? O5W H51 0.8519 . ? O5W H52 0.8496 . ? O6W H61 0.8487 . ? O6W H62 0.8488 . ? O7W H71 0.853 . ? O7W H72 0.8486 . ? O8W H81 0.8503 . ? O8W H82 0.8566 . ? O9W H91 0.8482 . ? O9W H92 0.8503 . ? O10W H101 0.8479 . ? O10W H102 0.8643 . ? O11W H111 0.8661 . ? O11W H112 0.9717 . ? O12W H121 0.85 . ? O12W H122 0.8499 . ? 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 N4B Pt1 N3A 92.0(4) . . ? N4B Pt1 N12 87.6(4) . . ? N3A Pt1 N12 178.5(4) . . ? N4B Pt1 N11 175.9(4) . . ? N3A Pt1 N11 89.8(4) . . ? N12 Pt1 N11 90.7(4) . . ? N4B Pt1 Pt2 76.6(3) . . ? N3A Pt1 Pt2 85.5(3) . . ? N12 Pt1 Pt2 93.0(3) . . ? N11 Pt1 Pt2 107.2(3) . . ? N4A Pt2 N3B 91.7(4) . . ? N4A Pt2 N14 175.9(4) . . ? N3B Pt2 N14 87.7(4) . . ? N4A Pt2 N13 90.3(4) . . ? N3B Pt2 N13 177.8(4) . . ? N14 Pt2 N13 90.3(4) . . ? N4A Pt2 Pt1 75.7(3) . . ? N3B Pt2 Pt1 86.5(3) . . ? N14 Pt2 Pt1 108.2(2) . . ? N13 Pt2 Pt1 93.2(3) . . ? N4D Pt3 N3C 88.5(4) . . ? N4D Pt3 N15 91.0(4) . . ? N3C Pt3 N15 177.8(4) . . ? N4D Pt3 N16 178.4(4) . . ? N3C Pt3 N16 92.2(4) . . ? N15 Pt3 N16 88.3(4) . . ? N4D Pt3 Pt4 78.8(3) . . ? N3C Pt3 Pt4 85.1(2) . . ? N15 Pt3 Pt4 92.7(3) . . ? N16 Pt3 Pt4 102.7(3) . . ? N4C Pt4 N3D 92.1(4) . . ? N4C Pt4 N17 176.5(4) . . ? N3D Pt4 N17 91.1(3) . . ? N4C Pt4 N18 86.7(4) . . ? N3D Pt4 N18 178.7(3) . . ? N17 Pt4 N18 90.1(4) . . ? N4C Pt4 Pt3 77.5(3) . . ? N3D Pt4 Pt3 82.8(2) . . ? N17 Pt4 Pt3 104.4(2) . . ? N18 Pt4 Pt3 96.4(3) . . ? Pt1 N11 H11A 109.5 . . ? Pt1 N11 H11B 109.5 . . ? H11A N11 H11B 109.5 . . ? Pt1 N11 H11C 109.5 . . ? H11A N11 H11C 109.5 . . ? H11B N11 H11C 109.5 . . ? Pt1 N12 H12A 109.5 . . ? Pt1 N12 H12B 109.5 . . ? H12A N12 H12B 109.5 . . ? Pt1 N12 H12C 109.5 . . ? H12A N12 H12C 109.5 . . ? H12B N12 H12C 109.5 . . ? Pt2 N13 H13A 109.5 . . ? Pt2 N13 H13B 109.5 . . ? H13A N13 H13B 109.5 . . ? Pt2 N13 H13C 109.5 . . ? H13A N13 H13C 109.5 . . ? H13B N13 H13C 109.5 . . ? Pt2 N14 H14A 109.5 . . ? Pt2 N14 H14B 109.5 . . ? H14A N14 H14B 109.5 . . ? Pt2 N14 H14C 109.5 . . ? H14A N14 H14C 109.5 . . ? H14B N14 H14C 109.5 . . ? Pt3 N15 H15A 109.5 . . ? Pt3 N15 H15B 109.5 . . ? H15A N15 H15B 109.5 . . ? Pt3 N15 H15C 109.5 . . ? H15A N15 H15C 109.5 . . ? H15B N15 H15C 109.5 . . ? Pt3 N16 H16A 109.5 . . ? Pt3 N16 H16B 109.5 . . ? H16A N16 H16B 109.5 . . ? Pt3 N16 H16C 109.5 . . ? H16A N16 H16C 109.5 . . ? H16B N16 H16C 109.5 . . ? Pt4 N17 H17A 109.5 . . ? Pt4 N17 H17B 109.5 . . ? H17A N17 H17B 109.5 . . ? Pt4 N17 H17C 109.5 . . ? H17A N17 H17C 109.5 . . ? H17B N17 H17C 109.5 . . ? Pt4 N18 H18A 109.5 . . ? Pt4 N18 H18B 109.5 . . ? H18A N18 H18B 109.5 . . ? Pt4 N18 H18C 109.5 . . ? H18A N18 H18C 109.5 . . ? H18B N18 H18C 109.5 . . ? C6A N1A C2A 119.3(10) . . ? C6A N1A C1A 120.9(10) . . ? C2A N1A C1A 119.4(9) . . ? N1A C1A H1AA 109.5 . . ? N1A C1A H1AB 109.5 . . ? H1AA C1A H1AB 109.5 . . ? N1A C1A H1AC 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? O2A C2A N1A 119.9(11) . . ? O2A C2A N3A 121.3(11) . . ? N1A C2A N3A 118.8(9) . . ? C4A N3A C2A 121.2(10) . . ? C4A N3A Pt1 120.7(8) . . ? C2A N3A Pt1 118.1(7) . . ? C4A N4A Pt2 136.5(8) . . ? C4A N4A H4A 111.8 . . ? Pt2 N4A H4A 111.8 . . ? N4A C4A N3A 120.2(11) . . ? N4A C4A C5A 122.1(11) . . ? N3A C4A C5A 117.7(11) . . ? C6A C5A C4A 119.0(12) . . ? C6A C5A H5AA 120.5 . . ? C4A C5A H5AA 120.5 . . ? C5A C6A N1A 123.1(12) . . ? C5A C6A H6AA 118.5 . . ? N1A C6A H6AA 118.5 . . ? C6B N1B C2B 121.3(10) . . ? C6B N1B C1B 120.9(10) . . ? C2B N1B C1B 117.8(10) . . ? N1B C1B H1BA 109.5 . . ? N1B C1B H1BB 109.5 . . ? H1BA C1B H1BB 109.5 . . ? N1B C1B H1BC 109.5 . . ? H1BA C1B H1BC 109.5 . . ? H1BB C1B H1BC 109.5 . . ? O2B C2B N3B 122.0(11) . . ? O2B C2B N1B 120.1(11) . . ? N3B C2B N1B 117.6(11) . . ? C2B N3B C4B 122.0(10) . . ? C2B N3B Pt2 118.6(8) . . ? C4B N3B Pt2 119.3(7) . . ? N4B C4B N3B 121.8(11) . . ? N4B C4B C5B 120.9(12) . . ? N3B C4B C5B 117.3(10) . . ? C4B N4B Pt1 134.5(9) . . ? C4B N4B H4B 112.7 . . ? Pt1 N4B H4B 112.7 . . ? C6B C5B C4B 117.8(12) . . ? C6B C5B H5BA 121.1 . . ? C4B C5B H5BA 121.1 . . ? N1B C6B C5B 123.0(12) . . ? N1B C6B H6BA 118.5 . . ? C5B C6B H6BA 118.5 . . ? C6C N1C C2C 121.6(10) . . ? C6C N1C C1C 120.5(10) . . ? C2C N1C C1C 117.5(11) . . ? N1C C1C H1CA 109.5 . . ? N1C C1C H1CB 109.5 . . ? H1CA C1C H1CB 109.5 . . ? N1C C1C H1CC 109.5 . . ? H1CA C1C H1CC 109.5 . . ? H1CB C1C H1CC 109.5 . . ? O2C C2C N3C 121.7(10) . . ? O2C C2C N1C 119.9(11) . . ? N3C C2C N1C 118.3(11) . . ? C2C N3C C4C 119.8(9) . . ? C2C N3C Pt3 117.9(7) . . ? C4C N3C Pt3 121.8(7) . . ? N4C C4C N3C 119.5(10) . . ? N4C C4C C5C 121.1(12) . . ? N3C C4C C5C 119.4(10) . . ? C4C N4C Pt4 134.2(9) . . ? C4C N4C H4C 112.9 . . ? Pt4 N4C H4C 112.9 . . ? C6C C5C C4C 118.1(12) . . ? C6C C5C H5CA 120.9 . . ? C4C C5C H5CA 120.9 . . ? N1C C6C C5C 122.7(11) . . ? N1C C6C H6CA 118.6 . . ? C5C C6C H6CA 118.6 . . ? C6D N1D C2D 122.2(10) . . ? C6D N1D C1D 118.2(10) . . ? C2D N1D C1D 119.6(10) . . ? N1D C1D H1DA 109.5 . . ? N1D C1D H1DB 109.5 . . ? H1DA C1D H1DB 109.5 . . ? N1D C1D H1DC 109.5 . . ? H1DA C1D H1DC 109.5 . . ? H1DB C1D H1DC 109.5 . . ? O2D C2D N3D 122.9(11) . . ? O2D C2D N1D 118.3(11) . . ? N3D C2D N1D 118.8(10) . . ? C2D N3D C4D 120.3(10) . . ? C2D N3D Pt4 117.1(7) . . ? C4D N3D Pt4 122.5(8) . . ? N4D C4D N3D 119.3(11) . . ? N4D C4D C5D 123.3(11) . . ? N3D C4D C5D 117.3(11) . . ? C4D N4D Pt3 132.5(9) . . ? C4D N4D H4D 113.7 . . ? Pt3 N4D H4D 113.7 . . ? C6D C5D C4D 120.4(12) . . ? C6D C5D H5DA 119.8 . . ? C4D C5D H5DA 119.8 . . ? C5D C6D N1D 120.3(12) . . ? C5D C6D H6DA 119.8 . . ? N1D C6D H6DA 119.8 . . ? O17 S1 O13 60.2(16) . . ? O17 S1 O18 116.8(13) . . ? O13 S1 O18 162.7(16) . . ? O17 S1 O16 115.3(12) . . ? O13 S1 O16 61.5(15) . . ? O18 S1 O16 110.4(11) . . ? O17 S1 O14 56.4(12) . . ? O13 S1 O14 113.4(19) . . ? O18 S1 O14 60.4(12) . . ? O16 S1 O14 136.1(10) . . ? O17 S1 O11 124.7(12) . . ? O13 S1 O11 114.1(16) . . ? O18 S1 O11 82.1(12) . . ? O16 S1 O11 102.7(10) . . ? O14 S1 O11 116.8(11) . . ? O17 S1 O12 130.3(13) . . ? O13 S1 O12 102.2(16) . . ? O18 S1 O12 65.9(11) . . ? O16 S1 O12 45.4(9) . . ? O14 S1 O12 103.1(12) . . ? O11 S1 O12 105.0(12) . . ? O17 S1 O15 99.9(13) . . ? O13 S1 O15 92.2(16) . . ? O18 S1 O15 105.0(12) . . ? O16 S1 O15 108.0(9) . . ? O14 S1 O15 115.9(11) . . ? O12 S1 O15 128.5(12) . . ? O28 S2 O22 103.0(11) . . ? O28 S2 O27 115.9(11) . . ? O22 S2 O27 70.3(9) . . ? O28 S2 O25 116.5(12) . . ? O22 S2 O25 133.1(10) . . ? O27 S2 O25 110.0(10) . . ? O28 S2 O21 140.9(11) . . ? O22 S2 O21 116.2(9) . . ? O27 S2 O21 80.1(10) . . ? O28 S2 O24 48.7(10) . . ? O22 S2 O24 117.9(9) . . ? O27 S2 O24 162.5(10) . . ? O25 S2 O24 76.4(10) . . ? O21 S2 O24 107.2(10) . . ? O28 S2 O26 105.9(9) . . ? O27 S2 O26 104.2(9) . . ? O25 S2 O26 102.5(10) . . ? O21 S2 O26 103.8(8) . . ? O24 S2 O26 89.7(8) . . ? O28 S2 O23 64.8(9) . . ? O22 S2 O23 108.7(10) . . ? O27 S2 O23 59.1(8) . . ? O25 S2 O23 110.3(9) . . ? O21 S2 O23 101.3(9) . . ? O24 S2 O23 103.5(9) . . ? O26 S2 O23 146.6(10) . . ? H11 O1W H12 107.3 . . ? H21 O2W H22 107.9 . . ? H31 O3W H32 107.7 . . ? H41 O4W H42 107.8 . . ? H51 O5W H52 107.6 . . ? H61 O6W H62 107.9 . . ? H71 O7W H72 107.6 . . ? H81 O8W H82 107 . . ? H91 O9W H92 107.8 . . ? H101 O10W H102 106.5 . . ? H111 O11W H112 104.8 . . ? H121 O12W H122 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4B Pt1 Pt2 N4A -85.0(4) . . . . ? N3A Pt1 Pt2 N4A 8.1(4) . . . . ? N12 Pt1 Pt2 N4A -171.9(4) . . . . ? N11 Pt1 Pt2 N4A 96.4(4) . . . . ? N4B Pt1 Pt2 N3B 7.6(4) . . . . ? N3A Pt1 Pt2 N3B 100.7(4) . . . . ? N12 Pt1 Pt2 N3B -79.2(5) . . . . ? N11 Pt1 Pt2 N3B -170.9(4) . . . . ? N4B Pt1 Pt2 N14 94.1(4) . . . . ? N3A Pt1 Pt2 N14 -172.8(4) . . . . ? N12 Pt1 Pt2 N14 7.2(4) . . . . ? N11 Pt1 Pt2 N14 -84.5(4) . . . . ? N4B Pt1 Pt2 N13 -174.6(4) . . . . ? N3A Pt1 Pt2 N13 -81.5(4) . . . . ? N12 Pt1 Pt2 N13 98.6(5) . . . . ? N11 Pt1 Pt2 N13 6.9(4) . . . . ? N4D Pt3 Pt4 N4C 80.1(4) . . . . ? N3C Pt3 Pt4 N4C -9.3(4) . . . . ? N15 Pt3 Pt4 N4C 170.7(4) . . . . ? N16 Pt3 Pt4 N4C -100.5(4) . . . . ? N4D Pt3 Pt4 N3D -13.6(4) . . . . ? N3C Pt3 Pt4 N3D -103.1(4) . . . . ? N15 Pt3 Pt4 N3D 76.9(4) . . . . ? N16 Pt3 Pt4 N3D 165.7(4) . . . . ? N4D Pt3 Pt4 N17 -102.9(4) . . . . ? N3C Pt3 Pt4 N17 167.6(4) . . . . ? N15 Pt3 Pt4 N17 -12.4(4) . . . . ? N16 Pt3 Pt4 N17 76.4(4) . . . . ? N4D Pt3 Pt4 N18 165.3(4) . . . . ? N3C Pt3 Pt4 N18 75.8(4) . . . . ? N15 Pt3 Pt4 N18 -104.2(4) . . . . ? N16 Pt3 Pt4 N18 -15.3(4) . . . . ? C6A N1A C2A O2A 177.0(12) . . . . ? C1A N1A C2A O2A -9.5(18) . . . . ? C6A N1A C2A N3A -4.1(17) . . . . ? C1A N1A C2A N3A 169.4(10) . . . . ? O2A C2A N3A C4A 177.8(11) . . . . ? N1A C2A N3A C4A -1.1(17) . . . . ? O2A C2A N3A Pt1 -2.1(16) . . . . ? N1A C2A N3A Pt1 179.0(8) . . . . ? N4B Pt1 N3A C4A 65.2(9) . . . . ? N11 Pt1 N3A C4A -118.5(9) . . . . ? Pt2 Pt1 N3A C4A -11.2(8) . . . . ? N4B Pt1 N3A C2A -114.9(9) . . . . ? N11 Pt1 N3A C2A 61.4(9) . . . . ? Pt2 Pt1 N3A C2A 168.7(8) . . . . ? N3B Pt2 N4A C4A -94.9(12) . . . . ? N13 Pt2 N4A C4A 84.4(12) . . . . ? Pt1 Pt2 N4A C4A -8.9(11) . . . . ? Pt2 N4A C4A N3A 3.2(18) . . . . ? Pt2 N4A C4A C5A -175.6(9) . . . . ? C2A N3A C4A N4A -170.5(10) . . . . ? Pt1 N3A C4A N4A 9.3(15) . . . . ? C2A N3A C4A C5A 8.3(16) . . . . ? Pt1 N3A C4A C5A -171.8(8) . . . . ? N4A C4A C5A C6A 168.2(12) . . . . ? N3A C4A C5A C6A -10.6(17) . . . . ? C4A C5A C6A N1A 5.8(19) . . . . ? C2A N1A C6A C5A 1.7(19) . . . . ? C1A N1A C6A C5A -171.7(12) . . . . ? C6B N1B C2B O2B 176.6(11) . . . . ? C1B N1B C2B O2B -5.9(16) . . . . ? C6B N1B C2B N3B -10.1(17) . . . . ? C1B N1B C2B N3B 167.5(11) . . . . ? O2B C2B N3B C4B 179.1(11) . . . . ? N1B C2B N3B C4B 5.9(17) . . . . ? O2B C2B N3B Pt2 -1.3(16) . . . . ? N1B C2B N3B Pt2 -174.5(8) . . . . ? N4A Pt2 N3B C2B -111.9(9) . . . . ? N14 Pt2 N3B C2B 64.1(9) . . . . ? Pt1 Pt2 N3B C2B 172.5(9) . . . . ? N4A Pt2 N3B C4B 67.8(9) . . . . ? N14 Pt2 N3B C4B -116.2(9) . . . . ? Pt1 Pt2 N3B C4B -7.8(8) . . . . ? C2B N3B C4B N4B -176.9(11) . . . . ? Pt2 N3B C4B N4B 3.5(15) . . . . ? C2B N3B C4B C5B 3.0(16) . . . . ? Pt2 N3B C4B C5B -176.7(8) . . . . ? N3B C4B N4B Pt1 8.7(18) . . . . ? C5B C4B N4B Pt1 -171.1(9) . . . . ? N3A Pt1 N4B C4B -96.1(12) . . . . ? N12 Pt1 N4B C4B 82.6(12) . . . . ? Pt2 Pt1 N4B C4B -11.1(11) . . . . ? N4B C4B C5B C6B 171.8(12) . . . . ? N3B C4B C5B C6B -8.0(17) . . . . ? C2B N1B C6B C5B 5(2) . . . . ? C1B N1B C6B C5B -172.4(12) . . . . ? C4B C5B C6B N1B 4(2) . . . . ? C6C N1C C2C O2C 179.6(12) . . . . ? C1C N1C C2C O2C -7.7(18) . . . . ? C6C N1C C2C N3C 2.2(18) . . . . ? C1C N1C C2C N3C 174.9(12) . . . . ? O2C C2C N3C C4C -179.5(11) . . . . ? N1C C2C N3C C4C -2.1(17) . . . . ? O2C C2C N3C Pt3 7.4(16) . . . . ? N1C C2C N3C Pt3 -175.2(8) . . . . ? N4D Pt3 N3C C2C 105.3(9) . . . . ? N16 Pt3 N3C C2C -73.3(9) . . . . ? Pt4 Pt3 N3C C2C -175.9(9) . . . . ? N4D Pt3 N3C C4C -67.7(9) . . . . ? N16 Pt3 N3C C4C 113.7(9) . . . . ? Pt4 Pt3 N3C C4C 11.2(8) . . . . ? C2C N3C C4C N4C -179.8(11) . . . . ? Pt3 N3C C4C N4C -7.0(15) . . . . ? C2C N3C C4C C5C 2.4(17) . . . . ? Pt3 N3C C4C C5C 175.2(9) . . . . ? N3C C4C N4C Pt4 -7.8(18) . . . . ? C5C C4C N4C Pt4 170.0(9) . . . . ? N3D Pt4 N4C C4C 94.5(12) . . . . ? N18 Pt4 N4C C4C -84.9(12) . . . . ? Pt3 Pt4 N4C C4C 12.3(11) . . . . ? N4C C4C C5C C6C 179.6(12) . . . . ? N3C C4C C5C C6C -2.7(18) . . . . ? C2C N1C C6C C5C -3(2) . . . . ? C1C N1C C6C C5C -175.1(13) . . . . ? C4C C5C C6C N1C 3(2) . . . . ? C6D N1D C2D O2D -173.0(11) . . . . ? C1D N1D C2D O2D 7.3(16) . . . . ? C6D N1D C2D N3D 9.1(16) . . . . ? C1D N1D C2D N3D -170.5(11) . . . . ? O2D C2D N3D C4D 178.4(10) . . . . ? N1D C2D N3D C4D -3.8(15) . . . . ? O2D C2D N3D Pt4 2.5(14) . . . . ? N1D C2D N3D Pt4 -179.8(7) . . . . ? N4C Pt4 N3D C2D 115.3(8) . . . . ? N17 Pt4 N3D C2D -63.2(8) . . . . ? Pt3 Pt4 N3D C2D -167.6(8) . . . . ? N4C Pt4 N3D C4D -60.5(9) . . . . ? N17 Pt4 N3D C4D 120.9(9) . . . . ? Pt3 Pt4 N3D C4D 16.5(8) . . . . ? C2D N3D C4D N4D 173.8(10) . . . . ? Pt4 N3D C4D N4D -10.4(14) . . . . ? C2D N3D C4D C5D -3.6(15) . . . . ? Pt4 N3D C4D C5D 172.2(8) . . . . ? N3D C4D N4D Pt3 -11.1(16) . . . . ? C5D C4D N4D Pt3 166.1(9) . . . . ? N3C Pt3 N4D C4D 103.4(10) . . . . ? N15 Pt3 N4D C4D -74.5(11) . . . . ? Pt4 Pt3 N4D C4D 18.1(10) . . . . ? N4D C4D C5D C6D -170.9(12) . . . . ? N3D C4D C5D C6D 6.4(18) . . . . ? C4D C5D C6D N1D -1(2) . . . . ? C2D N1D C6D C5D -6.4(19) . . . . ? C1D N1D C6D C5D 173.2(13) . . . . ? # END of CIF # Attachment '4_NIC314_schurmann.CIF' data_314a _database_code_depnum_ccdc_archive 'CCDC 743523' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H14 Cl N3 O3 Pt' _chemical_formula_weight 478.80 _chemical_melting_point ? _chemical_compound_source ? 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 ? _symmetry_space_group_name_H-M ? 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 13.305(4) _cell_length_b 6.900(3) _cell_length_c 16.059(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.12(3) _cell_angle_gamma 90.00 _cell_volume 1409.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.257 _exptl_crystal_density_method ? _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 10.158 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3076 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2498 _reflns_number_observed 1732 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0898P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2492 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_obs 0.0526 _refine_ls_wR_factor_all 0.1407 _refine_ls_wR_factor_obs 0.1235 _refine_ls_goodness_of_fit_all 0.937 _refine_ls_goodness_of_fit_obs 1.087 _refine_ls_restrained_S_all 1.017 _refine_ls_restrained_S_obs 1.087 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.21285(3) 0.13123(7) 0.19046(3) 0.0246(2) Uani 1 d . . Cl1 Cl 0.0324(3) 0.1306(6) 0.1306(2) 0.0425(8) Uani 1 d . . O1 O 0.5201(8) 0.1447(18) 0.2064(10) 0.070(4) Uani 1 d . . O2 O 0.6705(8) -0.1405(18) 0.2861(7) 0.049(3) Uani 1 d . . O3 O 0.6279(9) 0.4959(18) 0.1959(9) 0.058(3) Uani 1 d . . N1 N 0.2489(9) 0.1341(21) 0.0754(8) 0.041(3) Uani 1 d . . N2 N 0.2202(10) 0.1250(20) 0.3171(8) 0.044(3) Uani 1 d . . N3 N 0.3627(8) 0.1294(15) 0.2399(7) 0.027(2) Uani 1 d . . C1 C 0.4214(10) 0.1388(23) 0.1870(11) 0.041(4) Uani 1 d . . C2 C 0.4057(11) 0.1307(23) 0.3335(11) 0.049(4) Uani 1 d . . H2A H 0.4473(11) 0.2500(23) 0.3528(11) 0.122(63) Uiso 1 calc R . H2B H 0.4523(11) 0.0173(23) 0.3530(11) 0.122(63) Uiso 1 calc R . C11 C 0.3570(12) 0.1385(25) 0.0925(11) 0.045(4) Uani 1 d . . C12 C 0.3972(17) 0.1435(30) 0.0213(15) 0.072(6) Uani 1 d . . H12 H 0.4712(17) 0.1468(30) 0.0312(15) 0.125(36) Uiso 1 calc R . C13 C 0.3339(22) 0.1437(36) -0.0598(15) 0.086(8) Uani 1 d . . H13 H 0.3618(22) 0.1516(36) -0.1078(15) 0.125(36) Uiso 1 calc R . C14 C 0.2296(20) 0.1327(32) -0.0729(11) 0.072(6) Uani 1 d . . H14 H 0.1838(20) 0.1292(32) -0.1308(11) 0.125(36) Uiso 1 calc R . C15 C 0.1876(13) 0.1262(26) -0.0037(8) 0.045(4) Uani 1 d . . H15 H 0.1137(13) 0.1159(26) -0.0144(8) 0.125(36) Uiso 1 calc R . C21 C 0.3168(15) 0.1228(22) 0.3708(9) 0.050(4) Uani 1 d . . C22 C 0.3303(16) 0.1306(22) 0.4627(11) 0.056(5) Uani 1 d . . H22 H 0.3991(16) 0.1379(22) 0.5022(11) 0.125(36) Uiso 1 calc R . C23 C 0.2463(28) 0.1277(29) 0.4938(11) 0.095(10) Uani 1 d . . H23 H 0.2560(28) 0.1277(29) 0.5548(11) 0.125(36) Uiso 1 calc R . C24 C 0.1503(25) 0.1248(33) 0.4383(14) 0.087(8) Uani 1 d . . H24 H 0.0917(25) 0.1246(33) 0.4607(14) 0.125(36) Uiso 1 calc R . C25 C 0.1319(15) 0.1221(31) 0.3488(10) 0.059(5) Uani 1 d . . H25 H 0.0624(15) 0.1185(31) 0.3102(10) 0.125(36) 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 Pt1 0.0233(3) 0.0227(3) 0.0273(3) -0.0009(3) 0.0066(2) -0.0008(3) Cl1 0.028(2) 0.040(2) 0.054(2) -0.003(2) 0.0044(15) -0.001(2) O1 0.029(6) 0.042(7) 0.140(12) 0.028(8) 0.027(7) 0.004(6) O2 0.037(5) 0.061(8) 0.051(6) 0.009(6) 0.014(5) 0.006(6) O3 0.044(6) 0.056(8) 0.079(9) 0.004(7) 0.023(6) -0.002(6) N1 0.041(6) 0.049(8) 0.039(6) -0.012(7) 0.023(5) -0.002(7) N2 0.050(7) 0.038(7) 0.035(6) 0.004(7) 0.000(6) -0.009(7) N3 0.029(5) 0.003(4) 0.047(6) -0.005(5) 0.007(5) -0.004(5) C1 0.028(7) 0.022(7) 0.075(10) 0.013(8) 0.017(7) 0.001(7) C2 0.028(7) 0.025(7) 0.071(11) 0.010(9) -0.022(7) -0.004(7) C11 0.045(8) 0.036(8) 0.068(10) 0.004(9) 0.039(8) -0.010(8) C12 0.088(14) 0.057(12) 0.104(17) 0.017(13) 0.079(14) 0.003(12) C13 0.140(22) 0.080(16) 0.077(14) -0.002(14) 0.093(16) 0.008(17) C14 0.126(19) 0.068(13) 0.030(8) -0.009(10) 0.035(10) -0.010(15) C15 0.061(10) 0.043(9) 0.026(7) -0.015(8) 0.007(7) -0.016(9) C21 0.088(12) 0.018(7) 0.031(7) -0.007(7) -0.002(8) -0.006(9) C22 0.101(14) 0.008(6) 0.038(8) 0.001(8) -0.011(9) -0.022(9) C23 0.225(32) 0.028(9) 0.022(8) 0.002(9) 0.021(14) -0.027(18) C24 0.185(27) 0.040(10) 0.056(12) -0.001(11) 0.067(16) 0.000(16) C25 0.077(12) 0.071(12) 0.040(8) -0.003(11) 0.035(8) -0.004(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 N3 1.917(10) . ? Pt1 N2 2.008(12) . ? Pt1 N1 2.042(11) . ? Pt1 Cl1 2.308(3) . ? Pt1 Pt1 3.9274(14) 2 ? Pt1 Pt1 3.9274(14) 2_545 ? O1 C1 1.26(2) . ? O1 O2 2.83(2) . ? O1 O3 2.85(2) . ? N1 C15 1.29(2) . ? N1 C11 1.38(2) . ? N2 C21 1.32(2) . ? N2 C25 1.41(2) . ? N3 C1 1.31(2) . ? N3 C2 1.44(2) . ? C1 C11 1.51(2) . ? C2 C21 1.48(2) . ? C11 C12 1.40(2) . ? C12 C13 1.33(3) . ? C13 C14 1.34(3) . ? C14 C15 1.38(2) . ? C21 C22 1.43(2) . ? C22 C23 1.35(3) . ? C23 C24 1.33(4) . ? C24 C25 1.38(2) . ? 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 N3 Pt1 N2 81.1(5) . . ? N3 Pt1 N1 83.2(5) . . ? N2 Pt1 N1 164.3(5) . . ? N3 Pt1 Cl1 179.5(3) . . ? N2 Pt1 Cl1 99.0(4) . . ? N1 Pt1 Cl1 96.6(4) . . ? N3 Pt1 Pt1 73.9(3) . 2 ? N2 Pt1 Pt1 66.1(4) . 2 ? N1 Pt1 Pt1 109.9(4) . 2 ? Cl1 Pt1 Pt1 106.65(11) . 2 ? N3 Pt1 Pt1 73.2(3) . 2_545 ? N2 Pt1 Pt1 63.8(4) . 2_545 ? N1 Pt1 Pt1 110.9(4) . 2_545 ? Cl1 Pt1 Pt1 106.44(11) . 2_545 ? Pt1 Pt1 Pt1 122.91(4) 2 2_545 ? C1 O1 O2 129.6(10) . . ? C1 O1 O3 121.4(10) . . ? O2 O1 O3 108.5(5) . . ? C15 N1 C11 121.0(13) . . ? C15 N1 Pt1 129.8(11) . . ? C11 N1 Pt1 109.2(10) . . ? C21 N2 C25 121.2(14) . . ? C21 N2 Pt1 114.1(11) . . ? C25 N2 Pt1 124.6(10) . . ? C1 N3 C2 123.0(12) . . ? C1 N3 Pt1 118.4(10) . . ? C2 N3 Pt1 118.5(9) . . ? O1 C1 N3 128.2(16) . . ? O1 C1 C11 119.5(14) . . ? N3 C1 C11 112.4(11) . . ? N3 C2 C21 107.7(11) . . ? N1 C11 C12 117.7(17) . . ? N1 C11 C1 116.7(12) . . ? C12 C11 C1 125.6(16) . . ? C13 C12 C11 121.2(19) . . ? C12 C13 C14 118.8(15) . . ? C13 C14 C15 121.3(18) . . ? N1 C15 C14 120.0(17) . . ? N2 C21 C22 118.3(18) . . ? N2 C21 C2 118.5(13) . . ? C22 C21 C2 123.0(16) . . ? C23 C22 C21 120.9(18) . . ? C24 C23 C22 119.3(17) . . ? C23 C24 C25 122.6(24) . . ? C24 C25 N2 117.5(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Pt1 N1 C15 175.9(18) . . . . ? N2 Pt1 N1 C15 173.8(18) . . . . ? Cl1 Pt1 N1 C15 -3.6(17) . . . . ? Pt1 Pt1 N1 C15 -114.0(16) 2 . . . ? Pt1 Pt1 N1 C15 106.9(16) 2_545 . . . ? N3 Pt1 N1 C11 -1.6(11) . . . . ? N2 Pt1 N1 C11 -3.7(28) . . . . ? Cl1 Pt1 N1 C11 178.9(11) . . . . ? Pt1 Pt1 N1 C11 68.5(12) 2 . . . ? Pt1 Pt1 N1 C11 -70.6(12) 2_545 . . . ? N3 Pt1 N2 C21 0.0(11) . . . . ? N1 Pt1 N2 C21 2.1(28) . . . . ? Cl1 Pt1 N2 C21 179.5(11) . . . . ? Pt1 Pt1 N2 C21 -76.2(11) 2 . . . ? Pt1 Pt1 N2 C21 75.6(11) 2_545 . . . ? N3 Pt1 N2 C25 -179.7(16) . . . . ? N1 Pt1 N2 C25 -177.6(18) . . . . ? Cl1 Pt1 N2 C25 -0.2(15) . . . . ? Pt1 Pt1 N2 C25 104.1(15) 2 . . . ? Pt1 Pt1 N2 C25 -104.2(15) 2_545 . . . ? N2 Pt1 N3 C1 -177.8(12) . . . . ? N1 Pt1 N3 C1 2.8(11) . . . . ? Cl1 Pt1 N3 C1 75.6(401) . . . . ? Pt1 Pt1 N3 C1 -110.2(11) 2 . . . ? Pt1 Pt1 N3 C1 117.1(11) 2_545 . . . ? N2 Pt1 N3 C2 -1.8(10) . . . . ? N1 Pt1 N3 C2 178.8(12) . . . . ? Cl1 Pt1 N3 C2 -108.5(396) . . . . ? Pt1 Pt1 N3 C2 65.8(10) 2 . . . ? Pt1 Pt1 N3 C2 -66.9(10) 2_545 . . . ? O2 O1 C1 N3 66.2(24) . . . . ? O3 O1 C1 N3 -104.2(17) . . . . ? O2 O1 C1 C11 -112.6(16) . . . . ? O3 O1 C1 C11 77.0(19) . . . . ? C2 N3 C1 O1 2.1(25) . . . . ? Pt1 N3 C1 O1 177.9(13) . . . . ? C2 N3 C1 C11 -179.0(14) . . . . ? Pt1 N3 C1 C11 -3.2(18) . . . . ? C1 N3 C2 C21 178.7(14) . . . . ? Pt1 N3 C2 C21 2.9(16) . . . . ? C15 N1 C11 C12 3.0(27) . . . . ? Pt1 N1 C11 C12 -179.2(14) . . . . ? C15 N1 C11 C1 -177.4(16) . . . . ? Pt1 N1 C11 C1 0.4(19) . . . . ? O1 C1 C11 N1 -179.3(15) . . . . ? N3 C1 C11 N1 1.8(22) . . . . ? O1 C1 C11 C12 0.3(28) . . . . ? N3 C1 C11 C12 -178.7(17) . . . . ? N1 C11 C12 C13 -0.1(32) . . . . ? C1 C11 C12 C13 -179.7(21) . . . . ? C11 C12 C13 C14 -2.1(39) . . . . ? C12 C13 C14 C15 1.7(38) . . . . ? C11 N1 C15 C14 -3.6(29) . . . . ? Pt1 N1 C15 C14 179.2(14) . . . . ? C13 C14 C15 N1 1.2(34) . . . . ? C25 N2 C21 C22 -4.1(24) . . . . ? Pt1 N2 C21 C22 176.2(11) . . . . ? C25 N2 C21 C2 -178.6(16) . . . . ? Pt1 N2 C21 C2 1.7(19) . . . . ? N3 C2 C21 N2 -2.9(20) . . . . ? N3 C2 C21 C22 -177.1(14) . . . . ? N2 C21 C22 C23 4.2(25) . . . . ? C2 C21 C22 C23 178.4(17) . . . . ? C21 C22 C23 C24 -2.5(31) . . . . ? C22 C23 C24 C25 0.9(37) . . . . ? C23 C24 C25 N2 -0.8(36) . . . . ? C21 N2 C25 C24 2.5(29) . . . . ? Pt1 N2 C25 C24 -177.8(16) . . . . ? _refine_diff_density_max 4.759 _refine_diff_density_min -5.071 _refine_diff_density_rms 0.308 # Attachment '5_C3264_schurmann.CIF' data_c3264 _database_code_depnum_ccdc_archive 'CCDC 743524' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H8 Cl N3 O2 Pt' _chemical_formula_weight 456.75 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' 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.1698(5) _cell_length_b 7.4365(3) _cell_length_c 22.5026(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2371.18(17) _cell_formula_units_Z 8 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 23532 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 12.060 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.141 _exptl_absorpt_correction_T_max 0.379 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _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 none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23532 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2717 _reflns_number_gt 1865 _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^)+(0.0181P)^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 2717 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0460 _refine_ls_wR_factor_gt 0.0447 _refine_ls_goodness_of_fit_ref 0.894 _refine_ls_restrained_S_all 0.894 _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 0.724723(11) 0.09196(2) 0.622223(7) 0.01833(7) Uani 1 1 d . . . Cl1 Cl 0.88878(7) 0.09416(16) 0.62102(5) 0.0237(2) Uani 1 1 d . . . O1 O 0.4607(2) -0.0270(5) 0.67977(14) 0.0282(8) Uani 1 1 d . . . O2 O 0.4548(2) 0.1572(5) 0.56610(14) 0.0337(9) Uani 1 1 d . . . N1 N 0.7097(3) -0.0196(5) 0.70304(15) 0.0182(9) Uani 1 1 d . . . N2 N 0.7022(3) 0.2076(6) 0.54279(15) 0.0196(9) Uani 1 1 d . . . N3 N 0.5869(2) 0.0821(5) 0.62296(15) 0.0194(8) Uani 1 1 d . . . C1 C 0.5442(3) 0.0001(6) 0.6716(2) 0.0229(11) Uani 1 1 d . . . C2 C 0.5396(3) 0.1501(7) 0.5740(2) 0.0241(12) Uani 1 1 d . . . C11 C 0.6171(3) -0.0494(6) 0.71714(19) 0.0203(11) Uani 1 1 d . . . C12 C 0.5926(3) -0.1228(6) 0.7707(2) 0.0256(12) Uani 1 1 d . . . H12A H 0.5293 -0.1414 0.7798 0.031 Uiso 1 1 calc R . . C13 C 0.6615(3) -0.1693(7) 0.8113(2) 0.0266(12) Uani 1 1 d . . . H13A H 0.6456 -0.2213 0.8476 0.032 Uiso 1 1 calc R . . C14 C 0.7542(3) -0.1367(6) 0.7968(2) 0.0258(12) Uani 1 1 d . . . H14A H 0.8019 -0.1649 0.8236 0.031 Uiso 1 1 calc R . . C15 C 0.7765(3) -0.0626(6) 0.74256(19) 0.0223(11) Uani 1 1 d . . . H15A H 0.8395 -0.0418 0.7332 0.027 Uiso 1 1 calc R . . C21 C 0.6083(3) 0.2185(7) 0.52920(19) 0.0228(11) Uani 1 1 d . . . C22 C 0.5776(3) 0.2943(7) 0.4772(2) 0.0281(12) Uani 1 1 d . . . H22A H 0.5134 0.2994 0.4687 0.034 Uiso 1 1 calc R . . C23 C 0.6427(3) 0.3635(7) 0.4372(2) 0.0297(13) Uani 1 1 d . . . H23A H 0.6231 0.4148 0.4015 0.036 Uiso 1 1 calc R . . C24 C 0.7370(3) 0.3541(6) 0.4517(2) 0.0266(12) Uani 1 1 d . . . H24A H 0.7821 0.4018 0.4262 0.032 Uiso 1 1 calc R . . C25 C 0.7649(3) 0.2734(7) 0.50460(19) 0.0221(11) Uani 1 1 d . . . H25A H 0.8289 0.2652 0.5135 0.027 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 0.01340(10) 0.02418(11) 0.01743(10) -0.00202(8) 0.00056(8) -0.00037(8) Cl1 0.0132(5) 0.0322(6) 0.0257(6) -0.0002(6) 0.0014(5) -0.0010(5) O1 0.0123(18) 0.041(2) 0.0310(19) 0.0052(16) 0.0048(15) -0.0007(16) O2 0.0153(19) 0.059(3) 0.0269(19) 0.0053(17) -0.0033(15) 0.0020(18) N1 0.017(2) 0.019(2) 0.0188(19) -0.0025(16) -0.0006(16) -0.0007(17) N2 0.017(2) 0.024(2) 0.0184(19) -0.0071(17) 0.0046(16) 0.0004(18) N3 0.019(2) 0.024(2) 0.0159(19) 0.002(2) -0.0001(16) 0.0005(16) C1 0.019(3) 0.023(3) 0.026(3) -0.002(2) 0.003(2) 0.001(2) C2 0.022(3) 0.028(3) 0.022(3) -0.004(2) -0.001(2) 0.002(2) C11 0.019(3) 0.021(3) 0.022(2) -0.003(2) 0.004(2) -0.001(2) C12 0.021(3) 0.030(3) 0.026(3) 0.000(2) 0.006(2) -0.002(2) C13 0.031(3) 0.030(3) 0.019(3) 0.002(2) 0.004(2) -0.002(3) C14 0.026(3) 0.028(3) 0.024(2) -0.001(2) -0.006(2) -0.002(2) C15 0.018(3) 0.026(3) 0.023(2) -0.004(2) 0.000(2) -0.001(2) C21 0.022(3) 0.025(3) 0.021(3) -0.005(2) -0.001(2) 0.001(2) C22 0.022(3) 0.038(3) 0.024(3) -0.002(2) -0.003(2) 0.002(3) C23 0.032(3) 0.036(4) 0.020(3) 0.001(2) -0.001(2) 0.004(2) C24 0.028(3) 0.028(3) 0.025(2) -0.002(2) 0.010(2) -0.002(2) C25 0.019(3) 0.024(3) 0.024(2) -0.005(2) -0.002(2) 0.002(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 Pt1 N3 1.954(3) . ? Pt1 N2 2.009(4) . ? Pt1 N1 2.010(4) . ? Pt1 Cl1 2.3249(10) . ? O1 C1 1.214(5) . ? O2 C2 1.216(5) . ? N1 C15 1.337(5) . ? N1 C11 1.368(5) . ? N2 C25 1.329(6) . ? N2 C21 1.367(5) . ? N3 C2 1.385(6) . ? N3 C1 1.391(6) . ? C1 C11 1.502(6) . ? C2 C21 1.492(6) . ? C11 C12 1.368(6) . ? C12 C13 1.382(6) . ? C13 C14 1.376(6) . ? C14 C15 1.375(6) . ? C21 C22 1.370(6) . ? C22 C23 1.387(7) . ? C23 C24 1.379(6) . ? C24 C25 1.390(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 N3 Pt1 N2 82.24(14) . . ? N3 Pt1 N1 82.61(14) . . ? N2 Pt1 N1 164.76(15) . . ? N3 Pt1 Cl1 178.25(11) . . ? N2 Pt1 Cl1 98.36(11) . . ? N1 Pt1 Cl1 96.84(11) . . ? C15 N1 C11 119.1(4) . . ? C15 N1 Pt1 128.7(3) . . ? C11 N1 Pt1 112.2(3) . . ? C25 N2 C21 118.9(4) . . ? C25 N2 Pt1 128.8(3) . . ? C21 N2 Pt1 112.3(3) . . ? C2 N3 C1 125.1(4) . . ? C2 N3 Pt1 117.6(3) . . ? C1 N3 Pt1 117.3(3) . . ? O1 C1 N3 128.0(4) . . ? O1 C1 C11 121.7(4) . . ? N3 C1 C11 110.2(4) . . ? O2 C2 N3 127.7(4) . . ? O2 C2 C21 122.1(4) . . ? N3 C2 C21 110.2(4) . . ? C12 C11 N1 120.8(4) . . ? C12 C11 C1 121.6(4) . . ? N1 C11 C1 117.5(4) . . ? C11 C12 C13 120.2(5) . . ? C14 C13 C12 118.2(4) . . ? C15 C14 C13 120.0(4) . . ? N1 C15 C14 121.6(4) . . ? N2 C21 C22 121.6(4) . . ? N2 C21 C2 117.6(4) . . ? C22 C21 C2 120.7(4) . . ? C21 C22 C23 119.8(5) . . ? C24 C23 C22 118.1(4) . . ? C23 C24 C25 120.1(5) . . ? N2 C25 C24 121.5(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Pt1 N1 C15 -177.4(4) . . . . ? N2 Pt1 N1 C15 -171.3(5) . . . . ? Cl1 Pt1 N1 C15 4.2(4) . . . . ? N3 Pt1 N1 C11 1.4(3) . . . . ? N2 Pt1 N1 C11 7.5(8) . . . . ? Cl1 Pt1 N1 C11 -176.9(3) . . . . ? N3 Pt1 N2 C25 178.0(4) . . . . ? N1 Pt1 N2 C25 171.8(5) . . . . ? Cl1 Pt1 N2 C25 -3.7(4) . . . . ? N3 Pt1 N2 C21 -1.0(3) . . . . ? N1 Pt1 N2 C21 -7.1(8) . . . . ? Cl1 Pt1 N2 C21 177.4(3) . . . . ? N2 Pt1 N3 C2 0.3(3) . . . . ? N1 Pt1 N3 C2 178.7(4) . . . . ? Cl1 Pt1 N3 C2 -110(3) . . . . ? N2 Pt1 N3 C1 177.6(3) . . . . ? N1 Pt1 N3 C1 -4.0(3) . . . . ? Cl1 Pt1 N3 C1 67(3) . . . . ? C2 N3 C1 O1 0.3(8) . . . . ? Pt1 N3 C1 O1 -176.7(4) . . . . ? C2 N3 C1 C11 -177.5(4) . . . . ? Pt1 N3 C1 C11 5.5(5) . . . . ? C1 N3 C2 O2 3.4(8) . . . . ? Pt1 N3 C2 O2 -179.6(4) . . . . ? C1 N3 C2 C21 -176.7(4) . . . . ? Pt1 N3 C2 C21 0.3(5) . . . . ? C15 N1 C11 C12 -0.3(7) . . . . ? Pt1 N1 C11 C12 -179.3(4) . . . . ? C15 N1 C11 C1 -179.8(4) . . . . ? Pt1 N1 C11 C1 1.2(5) . . . . ? O1 C1 C11 C12 -1.8(7) . . . . ? N3 C1 C11 C12 176.2(4) . . . . ? O1 C1 C11 N1 177.7(4) . . . . ? N3 C1 C11 N1 -4.3(6) . . . . ? N1 C11 C12 C13 -0.5(7) . . . . ? C1 C11 C12 C13 179.0(4) . . . . ? C11 C12 C13 C14 1.2(7) . . . . ? C12 C13 C14 C15 -1.1(7) . . . . ? C11 N1 C15 C14 0.4(7) . . . . ? Pt1 N1 C15 C14 179.1(3) . . . . ? C13 C14 C15 N1 0.3(7) . . . . ? C25 N2 C21 C22 0.4(7) . . . . ? Pt1 N2 C21 C22 179.4(4) . . . . ? C25 N2 C21 C2 -177.6(4) . . . . ? Pt1 N2 C21 C2 1.4(5) . . . . ? O2 C2 C21 N2 178.8(5) . . . . ? N3 C2 C21 N2 -1.2(6) . . . . ? O2 C2 C21 C22 0.7(8) . . . . ? N3 C2 C21 C22 -179.2(5) . . . . ? N2 C21 C22 C23 -0.5(8) . . . . ? C2 C21 C22 C23 177.4(5) . . . . ? C21 C22 C23 C24 -0.4(8) . . . . ? C22 C23 C24 C25 1.4(7) . . . . ? C21 N2 C25 C24 0.6(7) . . . . ? Pt1 N2 C25 C24 -178.2(3) . . . . ? C23 C24 C25 N2 -1.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.283 _refine_diff_density_min -1.673 _refine_diff_density_rms 0.162