# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Gomez Quiroga, Adoracion' _publ_contact_author_email adoracion.gomez@uam.es _publ_section_title ; The Preparation and Characterization of trans-Platinum(IV) Complexes with Unusually High Cytotoxicity ; loop_ _publ_author_name 'A.Gomez Quiroga' L.Cubo T.Hambley 'P.Sanz Miguel' A.Carnero ; C.Navarro-Ranninger ; # Attachment '2iv-sanz.cif.txt' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_1 _database_code_depnum_ccdc_archive 'CCDC 778117' #TrackingRef '2iv-sanz.cif.txt' _audit_creation_date 2010-05-20T20:29:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C3 H14 Cl2 N2 O2 Pt, 3(H2 O)' _chemical_formula_sum 'C3 H20 Cl2 N2 O5 Pt' _chemical_formula_weight 430.2 #----------------------------------------------------------------------------# # 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 6.1970(3) _cell_length_b 8.1633(5) _cell_length_c 12.9784(7) _cell_angle_alpha 77.605(3) _cell_angle_beta 82.586(2) _cell_angle_gamma 74.228(2) _cell_volume 615.36(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12779 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 28.28 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prisms _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 2.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 11.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.134 _exptl_absorpt_correction_T_max 0.388 _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 0.029 _diffrn_reflns_av_unetI/netI 0.0263 _diffrn_reflns_number 12779 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 3024 _reflns_number_gt 2832 _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^)+(0.0151P)^2^+0.5724P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3024 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0195 _refine_ls_R_factor_gt 0.0166 _refine_ls_wR_factor_ref 0.0376 _refine_ls_wR_factor_gt 0.0365 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.118 _refine_diff_density_min -1.157 _refine_diff_density_rms 0.13 #----------------------------------------------------------------------------# # 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 0.026159(16) 0.459954(14) 0.708662(8) 0.01123(4) Uani 1 1 d . . . Cl1 Cl 0.24557(12) 0.64118(10) 0.61890(6) 0.01835(15) Uani 1 1 d . . . Cl2 Cl -0.20159(12) 0.29127(10) 0.80484(6) 0.01854(15) Uani 1 1 d . . . O1 O -0.1954(3) 0.5620(3) 0.59968(16) 0.0186(5) Uani 1 1 d . . . H11 H -0.3202 0.5424 0.624 0.028 Uiso 1 1 calc R . . O2 O 0.2539(3) 0.3604(3) 0.81784(15) 0.0145(4) Uani 1 1 d . . . H21 H 0.379 0.3774 0.7917 0.022 Uiso 1 1 calc R . . N11 N -0.1163(4) 0.6410(3) 0.80226(19) 0.0158(5) Uani 1 1 d . . . H11A H -0.1569 0.5835 0.8679 0.019 Uiso 1 1 calc R . . H11B H -0.0077 0.6934 0.8111 0.019 Uiso 1 1 calc R . . C12 C -0.3148(7) 0.7786(5) 0.7643(3) 0.0396(11) Uani 1 1 d . . . H12A H -0.2774 0.8383 0.6931 0.059 Uiso 1 1 calc R . . H12B H -0.3596 0.8618 0.8123 0.059 Uiso 1 1 calc R . . H12C H -0.4392 0.7267 0.7625 0.059 Uiso 1 1 calc R . . N1 N 0.1762(4) 0.2831(3) 0.61045(19) 0.0167(5) Uani 1 1 d . . . H1A H 0.1654 0.3469 0.5419 0.02 Uiso 1 1 calc . . . C2 C 0.4191(5) 0.2064(5) 0.6213(3) 0.0251(7) Uani 1 1 d . . . H2A H 0.4416 0.1342 0.6917 0.038 Uiso 1 1 calc R . . H2B H 0.4964 0.2991 0.6119 0.038 Uiso 1 1 calc R . . H2C H 0.4804 0.135 0.5673 0.038 Uiso 1 1 calc R . . C3 C 0.0679(6) 0.1403(5) 0.6136(3) 0.0290(8) Uani 1 1 d . . . H3A H 0.1392 0.0759 0.5573 0.043 Uiso 1 1 calc R . . H3B H -0.0924 0.1889 0.6032 0.043 Uiso 1 1 calc R . . H3C H 0.0854 0.062 0.6824 0.043 Uiso 1 1 calc R . . O3 O 0.2933(4) 0.0595(3) 0.95828(18) 0.0254(5) Uani 1 1 d . . . H31 H 0.2638 0.1541 0.9073 0.038 Uiso 1 1 d R . . H32 H 0.4386 0.0389 0.9633 0.038 Uiso 1 1 d R . . O4 O 0.2823(4) 0.4988(3) 0.99063(18) 0.0273(5) Uani 1 1 d . . . H41 H 0.3062 0.4347 0.9396 0.041 Uiso 1 1 d R . . H42 H 0.3449 0.5849 0.9617 0.041 Uiso 1 1 d R . . O5 O 0.0833(4) 0.8373(3) 0.90676(19) 0.0306(6) Uani 1 1 d . . . H51 H 0.1817 0.7377 0.9292 0.046 Uiso 1 1 d R . . H52 H -0.0367 0.8746 0.9505 0.046 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 0.00972(6) 0.01419(7) 0.00925(6) -0.00226(4) -0.00202(4) -0.00150(4) Cl1 0.0163(3) 0.0192(4) 0.0180(4) 0.0000(3) 0.0001(3) -0.0053(3) Cl2 0.0150(3) 0.0211(4) 0.0201(4) -0.0021(3) -0.0022(3) -0.0065(3) O1 0.0125(10) 0.0279(13) 0.0134(10) -0.0024(9) -0.0022(8) -0.0023(9) O2 0.0098(9) 0.0196(12) 0.0127(10) -0.0004(8) -0.0040(7) -0.0021(8) N11 0.0137(12) 0.0163(14) 0.0155(13) -0.0046(10) -0.0015(9) 0.0009(10) C12 0.040(2) 0.035(2) 0.035(2) -0.0190(18) -0.0168(17) 0.0226(18) N1 0.0168(13) 0.0182(14) 0.0148(13) -0.0034(10) -0.0023(10) -0.0031(11) C2 0.0208(16) 0.0266(19) 0.0232(17) -0.0069(14) -0.0067(13) 0.0061(14) C3 0.0333(19) 0.028(2) 0.0289(19) -0.0097(15) -0.0028(15) -0.0097(16) O3 0.0248(12) 0.0217(13) 0.0293(13) 0.0029(10) -0.0094(9) -0.0078(10) O4 0.0314(13) 0.0343(15) 0.0231(12) -0.0127(11) 0.0025(10) -0.0163(11) O5 0.0377(14) 0.0293(14) 0.0289(13) -0.0101(11) -0.0006(11) -0.0127(12) #----------------------------------------------------------------------------# # 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 O1 1.988(2) . ? Pt1 O2 2.0146(19) . ? Pt1 N11 2.055(2) . ? Pt1 N1 2.081(2) . ? Pt1 Cl2 2.3044(8) . ? Pt1 Cl1 2.3107(7) . ? O1 H11 0.84 . ? O2 H21 0.84 . ? N11 C12 1.478(4) . ? N11 H11A 0.92 . ? N11 H11B 0.92 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? N1 C2 1.477(4) . ? N1 C3 1.486(4) . ? N1 H1A 0.93 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? O3 H31 0.8963 . ? O3 H32 0.8781 . ? O4 H41 0.9032 . ? O4 H42 0.8851 . ? O5 H51 0.89 . ? O5 H52 0.8998 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pt1 O2 178.85(9) . . ? O1 Pt1 N11 94.38(9) . . ? O2 Pt1 N11 85.38(9) . . ? O1 Pt1 N1 85.29(9) . . ? O2 Pt1 N1 94.90(9) . . ? N11 Pt1 N1 177.92(10) . . ? O1 Pt1 Cl2 91.27(7) . . ? O2 Pt1 Cl2 89.85(6) . . ? N11 Pt1 Cl2 88.02(8) . . ? N1 Pt1 Cl2 94.04(7) . . ? O1 Pt1 Cl1 89.14(7) . . ? O2 Pt1 Cl1 89.72(6) . . ? N11 Pt1 Cl1 88.49(8) . . ? N1 Pt1 Cl1 89.44(7) . . ? Cl2 Pt1 Cl1 176.51(3) . . ? Pt1 O1 H11 109.5 . . ? Pt1 O2 H21 109.5 . . ? C12 N11 Pt1 117.1(2) . . ? C12 N11 H11A 108 . . ? Pt1 N11 H11A 108 . . ? C12 N11 H11B 108 . . ? Pt1 N11 H11B 108 . . ? H11A N11 H11B 107.3 . . ? N11 C12 H12A 109.5 . . ? N11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C2 N1 C3 108.1(3) . . ? C2 N1 Pt1 114.47(19) . . ? C3 N1 Pt1 116.8(2) . . ? C2 N1 H1A 105.5 . . ? C3 N1 H1A 105.5 . . ? Pt1 N1 H1A 105.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? H31 O3 H32 103.5 . . ? H41 O4 H42 103.5 . . ? H51 O5 H52 118.6 . . ? 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 O1 Pt1 N11 C12 -1.0(3) . . . . ? O2 Pt1 N11 C12 177.9(3) . . . . ? Cl2 Pt1 N11 C12 -92.1(3) . . . . ? Cl1 Pt1 N11 C12 88.1(3) . . . . ? O1 Pt1 N1 C2 154.1(2) . . . . ? O2 Pt1 N1 C2 -24.7(2) . . . . ? Cl2 Pt1 N1 C2 -114.9(2) . . . . ? Cl1 Pt1 N1 C2 64.9(2) . . . . ? O1 Pt1 N1 C3 -78.1(2) . . . . ? O2 Pt1 N1 C3 103.1(2) . . . . ? Cl2 Pt1 N1 C3 12.9(2) . . . . ? Cl1 Pt1 N1 C3 -167.2(2) . . . . ? # END of CIF # Attachment '3iv-sanz.cif.txt' data_3 _database_code_depnum_ccdc_archive 'CCDC 778118' #TrackingRef '3iv-sanz.cif.txt' _audit_creation_date 2010-05-20T20:07:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C4 H16 Cl2 N2 O2 Pt' _chemical_formula_sum 'C4 H16 Cl2 N2 O2 Pt' _chemical_formula_weight 390.18 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.4160(17) _cell_length_b 7.3210(15) _cell_length_c 18.708(5) _cell_angle_alpha 90 _cell_angle_beta 115.99(2) _cell_angle_gamma 90 _cell_volume 1036.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1296 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27.5 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description blocks _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 14.02 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.335 _exptl_absorpt_correction_T_max 0.496 _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 0.0511 _diffrn_reflns_av_unetI/netI 0.0841 _diffrn_reflns_number 2441 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 22.19 _diffrn_reflns_theta_full 22.19 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 1296 _reflns_number_gt 836 _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1296 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0644 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.693 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.187 #----------------------------------------------------------------------------# # 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 0.24344(9) 0.02343(5) 0.24555(4) 0.02194(19) Uani 1 1 d . . . Cl1 Cl 0.1914(5) -0.2647(4) 0.1892(2) 0.0353(10) Uani 1 1 d . . . Cl2 Cl 0.2953(5) 0.3112(4) 0.3014(2) 0.0342(10) Uani 1 1 d . . . O1 O -0.0049(11) 0.1003(11) 0.1730(5) 0.031(2) Uani 1 1 d . . . H1 H -0.0768 0.0328 0.1806 0.047 Uiso 1 1 calc R . . O2 O 0.4922(11) -0.0531(11) 0.3190(5) 0.031(2) Uani 1 1 d . . . H2 H 0.5641 0.0073 0.3085 0.047 Uiso 1 1 calc R . . N1 N 0.3369(13) 0.0986(13) 0.1641(6) 0.025(3) Uani 1 1 d . . . H1A H 0.3856 0.2133 0.1779 0.03 Uiso 1 1 calc R . . H1B H 0.4274 0.0201 0.1703 0.03 Uiso 1 1 calc R . . C2 C 0.2110(18) 0.1027(19) 0.0776(8) 0.035(4) Uani 1 1 d . . . H2A H 0.1156 0.0111 0.0681 0.042 Uiso 1 1 calc R . . C3 C 0.309(2) 0.046(2) 0.0302(8) 0.064(5) Uani 1 1 d . . . H3A H 0.2272 0.0457 -0.0265 0.096 Uiso 1 1 calc R . . H3B H 0.3569 -0.0776 0.0463 0.096 Uiso 1 1 calc R . . H3C H 0.4055 0.1313 0.0402 0.096 Uiso 1 1 calc R . . C4 C 0.1278(19) 0.2845(18) 0.0544(8) 0.050(5) Uani 1 1 d . . . H4A H 0.0662 0.3147 0.0869 0.075 Uiso 1 1 calc R . . H4B H 0.0429 0.283 -0.0019 0.075 Uiso 1 1 calc R . . H4C H 0.2191 0.3763 0.063 0.075 Uiso 1 1 calc R . . N11 N 0.1519(13) -0.0561(12) 0.3273(6) 0.022(3) Uani 1 1 d . . . H11A H 0.0612 0.021 0.3222 0.027 Uiso 1 1 calc R . . H11B H 0.1048 -0.1715 0.3138 0.027 Uiso 1 1 calc R . . C12 C 0.2809(19) -0.059(2) 0.4116(8) 0.051(5) Uani 1 1 d . . . H12A H 0.2225 -0.0995 0.4441 0.076 Uiso 1 1 calc R . . H12B H 0.3287 0.0643 0.4281 0.076 Uiso 1 1 calc R . . H12C H 0.3773 -0.1429 0.4188 0.076 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 0.0213(3) 0.0158(3) 0.0301(3) 0.0004(4) 0.0126(2) 0.0006(4) Cl1 0.039(3) 0.023(2) 0.049(3) -0.0057(17) 0.024(2) -0.0046(18) Cl2 0.037(3) 0.0196(19) 0.052(3) -0.0073(17) 0.025(2) -0.0054(17) O1 0.022(6) 0.031(5) 0.035(6) 0.011(4) 0.007(5) 0.010(5) O2 0.018(5) 0.034(6) 0.041(6) 0.016(5) 0.012(5) 0.014(5) N1 0.028(8) 0.014(6) 0.033(8) 0.002(5) 0.015(6) -0.001(5) C2 0.024(9) 0.045(10) 0.019(9) 0.001(7) -0.006(8) -0.008(8) C3 0.061(12) 0.106(15) 0.026(10) -0.015(10) 0.020(9) 0.008(11) C4 0.051(12) 0.050(10) 0.039(11) 0.022(8) 0.011(9) -0.003(9) N11 0.028(7) 0.013(6) 0.034(7) 0.003(5) 0.020(6) 0.003(5) C12 0.035(10) 0.085(13) 0.025(10) 0.004(9) 0.006(8) -0.008(9) #----------------------------------------------------------------------------# # 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 O1 2.011(8) . ? Pt1 O2 2.016(8) . ? Pt1 N1 2.071(9) . ? Pt1 N11 2.075(9) . ? Pt1 Cl2 2.307(3) . ? Pt1 Cl1 2.312(3) . ? O1 H1 0.84 . ? O2 H2 0.84 . ? N1 C2 1.498(14) . ? N1 H1A 0.92 . ? N1 H1B 0.92 . ? C2 C4 1.478(18) . ? C2 C3 1.508(19) . ? C2 H2A 1 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? N11 C12 1.471(14) . ? N11 H11A 0.92 . ? N11 H11B 0.92 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pt1 O2 179.6(3) . . ? O1 Pt1 N1 92.7(4) . . ? O2 Pt1 N1 87.7(4) . . ? O1 Pt1 N11 88.0(4) . . ? O2 Pt1 N11 91.7(3) . . ? N1 Pt1 N11 179.0(4) . . ? O1 Pt1 Cl2 89.1(3) . . ? O2 Pt1 Cl2 90.7(2) . . ? N1 Pt1 Cl2 91.9(3) . . ? N11 Pt1 Cl2 88.9(3) . . ? O1 Pt1 Cl1 90.8(3) . . ? O2 Pt1 Cl1 89.4(2) . . ? N1 Pt1 Cl1 88.0(3) . . ? N11 Pt1 Cl1 91.3(3) . . ? Cl2 Pt1 Cl1 179.84(13) . . ? Pt1 O1 H1 109.5 . . ? Pt1 O2 H2 109.5 . . ? C2 N1 Pt1 118.9(8) . . ? C2 N1 H1A 107.6 . . ? Pt1 N1 H1A 107.6 . . ? C2 N1 H1B 107.6 . . ? Pt1 N1 H1B 107.6 . . ? H1A N1 H1B 107 . . ? C4 C2 N1 110.8(12) . . ? C4 C2 C3 112.8(12) . . ? N1 C2 C3 108.7(11) . . ? C4 C2 H2A 108.1 . . ? N1 C2 H2A 108.1 . . ? C3 C2 H2A 108.1 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C12 N11 Pt1 117.1(8) . . ? C12 N11 H11A 108 . . ? Pt1 N11 H11A 108 . . ? C12 N11 H11B 108 . . ? Pt1 N11 H11B 108 . . ? H11A N11 H11B 107.3 . . ? N11 C12 H12A 109.5 . . ? N11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? 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 O1 Pt1 N1 C2 -25.1(9) . . . . ? O2 Pt1 N1 C2 155.1(9) . . . . ? Cl2 Pt1 N1 C2 -114.3(9) . . . . ? Cl1 Pt1 N1 C2 65.7(9) . . . . ? Pt1 N1 C2 C4 90.0(12) . . . . ? Pt1 N1 C2 C3 -145.6(10) . . . . ? O1 Pt1 N11 C12 -154.7(9) . . . . ? O2 Pt1 N11 C12 25.1(9) . . . . ? Cl2 Pt1 N11 C12 -65.5(9) . . . . ? Cl1 Pt1 N11 C12 114.5(9) . . . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF