# 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 loop_ _publ_author_name _publ_author_address 'Bernhard Keppler' ; Institut fuer Anorganische Chemie Universitaet Wien Waehringerstr. 42 A-1090 Vienna Austria ; 'Vladimir Arion' ; Institut fuer Anorganische Chemie, Universitaet Wien Waehringerstr. 42 A-1090 Vienna Austria ; 'Vesna M. Djinovic' ; Institut fuer Anorganische Chemie Universitaet Wien Waehringerstr. 42 A-1090 Vienna Austria ; 'Mathea S. Galanski' ; Institut fuer Anorganische Chemie Universitaet Wien Waehringerstr. 42 A-1090 Vienna Austria ; _publ_contact_author_name 'Bernhard Keppler' _publ_contact_author_email BERNHARD.KEPPLER@UNIVIE.AC.AT _publ_section_title ; Synthesis and structures of novel 1-methylcytosinato-bridged (ethylenediamine)platinum(II) and platinum(III) dinuclear complexes ; # Attachment 'CIF2.CIF' data_vedj016r _database_code_depnum_ccdc_archive 'CCDC 758045' #TrackingRef 'CIF2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(ethane-1,2-diamine-1kappa^2^N,N',2kappa^2^N,N')bis(miu-1-methylcytosinato-kappa^2^ N3,N4)diplatinum(II) dinitrate hydrate ; _chemical_name_common ; Bis(ethane-1,2-diamine-1kappa$2!N,N',2kappa$2!N,N')bis(miu-1- methylcytosinato-ka N3,N4)diplatinum(ii) dinitrate hydrate ; _chemical_melting_point ? _chemical_formula_moiety '2(C14 H28 N10 O2 Pt2), 4(N O3), H O, 4(H2 O), 2(O)' _chemical_formula_sum 'C28 H70 N24 O23 Pt4' _chemical_formula_weight 1891.44 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 25.8439(13) _cell_length_b 16.1026(11) _cell_length_c 18.3805(12) _cell_angle_alpha 90.00 _cell_angle_beta 132.070(6) _cell_angle_gamma 90.00 _cell_volume 5678.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 486 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 23.8 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3608 _exptl_absorpt_coefficient_mu 9.918 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3588 _exptl_absorpt_correction_T_max 0.4371 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 170968 _diffrn_reflns_av_R_equivalents 0.0812 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5572 _reflns_number_gt 4803 _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^)+(0.0307P)^2^+25.1076P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5572 _refine_ls_number_parameters 358 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_ref 0.0565 _refine_ls_wR_factor_gt 0.0529 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 Pt1A Pt 0.203929(9) 0.271459(10) 0.200733(12) 0.01468(6) Uani 1 1 d . . . O8A O 0.19848(18) 0.1455(2) 0.0775(2) 0.0238(7) Uani 1 1 d . . . N1A N 0.1668(2) 0.2154(2) -0.0534(3) 0.0209(8) Uani 1 1 d . . . N3A N 0.1958(2) 0.2858(2) 0.0828(3) 0.0169(8) Uani 1 1 d . . . N9A N 0.1901(2) 0.4303(2) 0.0817(3) 0.0175(8) Uani 1 1 d . . . H90A H 0.1752 0.4745 0.0442 0.021 Uiso 1 1 calc R . . C2A C 0.1879(2) 0.2125(3) 0.0385(3) 0.0184(10) Uani 1 1 d . . . C4A C 0.1843(2) 0.3612(3) 0.0396(3) 0.0161(9) Uani 1 1 d . . . C5A C 0.1655(2) 0.3615(3) -0.0541(3) 0.0214(10) Uani 1 1 d . . . H5A H 0.1593 0.4126 -0.0850 0.026 Uiso 1 1 calc R . . C6A C 0.1569(2) 0.2894(3) -0.0973(3) 0.0221(10) Uani 1 1 d . . . H6A H 0.1436 0.2898 -0.1596 0.026 Uiso 1 1 calc R . . C7A C 0.1519(3) 0.1359(3) -0.1034(4) 0.0318(12) Uani 1 1 d . . . H7A1 H 0.1395 0.1459 -0.1660 0.048 Uiso 1 1 calc R . . H7A2 H 0.1129 0.1084 -0.1154 0.048 Uiso 1 1 calc R . . H7A3 H 0.1932 0.1002 -0.0621 0.048 Uiso 1 1 calc R . . N10A N 0.3011(2) 0.2190(2) 0.2924(3) 0.0221(9) Uani 1 1 d . . . H10A H 0.3033 0.1779 0.2598 0.027 Uiso 1 1 calc R . . H10B H 0.3339 0.2586 0.3121 0.027 Uiso 1 1 calc R . . N11A N 0.2101(2) 0.2519(2) 0.3159(3) 0.0198(8) Uani 1 1 d . . . H11A H 0.1921 0.2969 0.3234 0.024 Uiso 1 1 calc R . . H11B H 0.1846 0.2058 0.3043 0.024 Uiso 1 1 calc R . . C10A C 0.3162(3) 0.1832(3) 0.3797(3) 0.0231(10) Uani 1 1 d . . . H10C H 0.3671 0.1794 0.4354 0.028 Uiso 1 1 calc R . . H10D H 0.2962 0.1267 0.3646 0.028 Uiso 1 1 calc R . . C11A C 0.2837(3) 0.2398(3) 0.4058(3) 0.0236(11) Uani 1 1 d . . . H11C H 0.2868 0.2140 0.4576 0.028 Uiso 1 1 calc R . . H11D H 0.3084 0.2938 0.4303 0.028 Uiso 1 1 calc R . . Pt1B Pt 0.227012(9) 0.454482(10) 0.217656(12) 0.01464(6) Uani 1 1 d . . . O8B O 0.14850(17) 0.57837(19) 0.2411(2) 0.0206(7) Uani 1 1 d . . . N1B N 0.0389(2) 0.5297(2) 0.1418(3) 0.0200(8) Uani 1 1 d . . . N3B N 0.12894(19) 0.4518(2) 0.1705(3) 0.0159(8) Uani 1 1 d . . . N9B N 0.10670(19) 0.3149(2) 0.1171(3) 0.0176(8) Uani 1 1 d . . . H90B H 0.0741 0.2803 0.0717 0.021 Uiso 1 1 calc R . . C2B C 0.1077(2) 0.5222(3) 0.1869(3) 0.0177(10) Uani 1 1 d . . . C4B C 0.0838(2) 0.3863(3) 0.1189(3) 0.0175(9) Uani 1 1 d . . . C5B C 0.0117(2) 0.3980(3) 0.0688(3) 0.0219(10) Uani 1 1 d . . . H5B H -0.0214 0.3560 0.0267 0.026 Uiso 1 1 calc R . . C6B C -0.0086(2) 0.4679(3) 0.0816(4) 0.0262(11) Uani 1 1 d . . . H6B H -0.0562 0.4754 0.0491 0.031 Uiso 1 1 calc R . . C7B C 0.0165(3) 0.6065(3) 0.1551(4) 0.0317(12) Uani 1 1 d . . . H7B1 H 0.0420 0.6142 0.2248 0.048 Uiso 1 1 calc R . . H7B2 H -0.0336 0.6038 0.1179 0.048 Uiso 1 1 calc R . . H7B3 H 0.0261 0.6533 0.1316 0.048 Uiso 1 1 calc R . . N10B N 0.2745(2) 0.4821(2) 0.3587(3) 0.0203(8) Uani 1 1 d . . . H10G H 0.2627 0.5350 0.3617 0.024 Uiso 1 1 calc R . . H10H H 0.2598 0.4458 0.3802 0.024 Uiso 1 1 calc R . . N11B N 0.3248(2) 0.4704(2) 0.2688(3) 0.0218(9) Uani 1 1 d . . . H11H H 0.3441 0.4197 0.2758 0.026 Uiso 1 1 calc R . . H11G H 0.3229 0.5016 0.2251 0.026 Uiso 1 1 calc R . . C10B C 0.3514(2) 0.4759(3) 0.4224(3) 0.0246(11) Uani 1 1 d . . . H10L H 0.3663 0.4171 0.4380 0.029 Uiso 1 1 calc R . . H10M H 0.3753 0.5064 0.4845 0.029 Uiso 1 1 calc R . . C11B C 0.3688(2) 0.5138(3) 0.3660(3) 0.0244(11) Uani 1 1 d . . . H11L H 0.3584 0.5740 0.3565 0.029 Uiso 1 1 calc R . . H11M H 0.4189 0.5062 0.4022 0.029 Uiso 1 1 calc R . . N13 N 0.4660(2) 0.3261(2) 0.4142(3) 0.0330(10) Uiso 1 1 d D . . O2 O 0.4084(7) 0.3165(7) 0.3287(10) 0.0351(12) Uiso 0.30 1 d PD A 1 O3 O 0.5097(9) 0.3730(7) 0.4205(15) 0.088(3) Uiso 0.30 1 d PD A 1 O4 O 0.4811(8) 0.2958(7) 0.4836(11) 0.0534(17) Uiso 0.30 1 d PD A 1 O2X O 0.4140(3) 0.3260(4) 0.3237(5) 0.0351(12) Uiso 0.70 1 d PD A 2 O3X O 0.5181(4) 0.3638(4) 0.4486(7) 0.088(3) Uiso 0.70 1 d PD A 2 O4X O 0.4607(3) 0.2856(4) 0.4671(5) 0.0534(17) Uiso 0.70 1 d PD A 2 N14 N 0.3382(4) 0.0985(3) 0.5976(4) 0.0471(15) Uani 1 1 d . . . O5 O 0.3784(3) 0.1317(3) 0.6806(3) 0.0767(19) Uani 1 1 d . . . O6 O 0.2739(3) 0.0972(3) 0.5508(4) 0.0565(13) Uani 1 1 d . . . O7 O 0.3603(3) 0.0706(2) 0.5606(3) 0.0489(12) Uani 1 1 d . . . O8 O 0.5265(8) 0.3467(7) 0.6559(9) 0.091(4) Uani 0.50 1 d P . . O9 O 0.4180(5) 0.6412(6) 0.1227(6) 0.052(2) Uani 0.50 1 d P . . O10 O 0.5000 0.2155(4) 0.7500 0.110(4) Uani 1 2 d S . . H10E H 0.4629 0.1899 0.7288 0.132 Uiso 0.50 1 d PR . . O11 O 0.4795(3) 0.5010(4) 0.2996(4) 0.0840(19) Uani 1 1 d . . . H11E H 0.4892 0.4606 0.3376 0.101 Uiso 1 1 d R . . H11F H 0.4771 0.5510 0.3137 0.101 Uiso 1 1 d R . . O12 O 0.3297(3) 0.5891(2) 0.1563(4) 0.0502(12) Uani 1 1 d . . . H12E H 0.2981 0.5912 0.0933 0.060 Uiso 1 1 d R . . H12F H 0.3701 0.6093 0.1834 0.060 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 Pt1A 0.01577(10) 0.01191(9) 0.01449(9) 0.00030(6) 0.00937(8) 0.00068(6) O8A 0.0302(19) 0.0159(17) 0.0231(17) 0.0012(14) 0.0170(16) 0.0037(14) N1A 0.026(2) 0.018(2) 0.0157(19) -0.0025(16) 0.0126(18) 0.0003(17) N3A 0.019(2) 0.0151(19) 0.0142(18) 0.0015(15) 0.0105(17) 0.0023(15) N9A 0.019(2) 0.0134(19) 0.021(2) 0.0037(15) 0.0132(18) 0.0018(15) C2A 0.017(2) 0.018(2) 0.020(2) -0.0027(19) 0.012(2) 0.0006(18) C4A 0.009(2) 0.020(2) 0.018(2) 0.0020(18) 0.0081(19) 0.0007(17) C5A 0.021(3) 0.020(3) 0.022(2) 0.0022(19) 0.015(2) 0.002(2) C6A 0.022(3) 0.027(3) 0.019(2) 0.004(2) 0.014(2) 0.004(2) C7A 0.046(3) 0.024(3) 0.028(3) -0.005(2) 0.026(3) 0.003(2) N10A 0.028(2) 0.017(2) 0.024(2) 0.0045(16) 0.018(2) 0.0056(17) N11A 0.024(2) 0.017(2) 0.020(2) 0.0002(16) 0.0152(19) 0.0006(16) C10A 0.026(3) 0.018(2) 0.021(2) 0.007(2) 0.014(2) 0.003(2) C11A 0.026(3) 0.021(3) 0.020(2) 0.004(2) 0.014(2) 0.003(2) Pt1B 0.01286(10) 0.01202(9) 0.01581(9) -0.00063(6) 0.00828(8) -0.00046(6) O8B 0.0215(18) 0.0152(17) 0.0239(17) -0.0030(13) 0.0148(16) -0.0017(14) N1B 0.016(2) 0.020(2) 0.022(2) -0.0013(16) 0.0126(19) 0.0029(16) N3B 0.016(2) 0.0133(19) 0.0175(19) 0.0008(15) 0.0110(17) 0.0008(15) N9B 0.0147(19) 0.018(2) 0.0176(19) -0.0030(16) 0.0097(17) -0.0035(16) C2B 0.020(2) 0.021(2) 0.014(2) 0.0029(18) 0.012(2) -0.0015(19) C4B 0.019(2) 0.017(2) 0.017(2) 0.0008(18) 0.012(2) 0.0005(18) C5B 0.015(2) 0.019(2) 0.024(2) -0.005(2) 0.010(2) -0.0049(19) C6B 0.010(2) 0.036(3) 0.024(3) -0.002(2) 0.008(2) 0.001(2) C7B 0.024(3) 0.032(3) 0.035(3) -0.002(2) 0.019(3) 0.006(2) N10B 0.020(2) 0.016(2) 0.022(2) -0.0003(16) 0.0127(19) -0.0027(16) N11B 0.017(2) 0.020(2) 0.025(2) -0.0003(17) 0.0129(19) -0.0003(16) C10B 0.017(3) 0.026(3) 0.019(2) 0.001(2) 0.007(2) 0.004(2) C11B 0.012(2) 0.026(3) 0.026(3) -0.004(2) 0.009(2) -0.005(2) N14 0.098(5) 0.029(3) 0.053(3) 0.019(2) 0.067(4) 0.030(3) O5 0.106(4) 0.093(4) 0.033(3) 0.016(3) 0.048(3) 0.061(3) O6 0.095(4) 0.049(3) 0.074(3) 0.019(3) 0.077(3) 0.018(3) O7 0.088(4) 0.031(2) 0.068(3) -0.012(2) 0.069(3) 0.000(2) O8 0.178(14) 0.048(7) 0.079(8) -0.011(6) 0.099(10) -0.004(7) O9 0.053(6) 0.058(6) 0.039(5) -0.003(4) 0.028(5) 0.004(5) O10 0.177(10) 0.038(4) 0.039(4) 0.000 0.041(6) 0.000 O11 0.109(5) 0.093(4) 0.096(4) -0.041(4) 0.088(4) -0.045(4) O12 0.069(3) 0.029(2) 0.088(4) 0.002(2) 0.067(3) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1A N9B 1.998(4) . ? Pt1A N11A 2.037(4) . ? Pt1A N10A 2.046(4) . ? Pt1A N3A 2.047(4) . ? Pt1A Pt1B 2.9816(3) . ? O8A C2A 1.221(5) . ? N1A C6A 1.364(6) . ? N1A C2A 1.385(6) . ? N1A C7A 1.468(6) . ? N3A C4A 1.369(6) . ? N3A C2A 1.370(6) . ? N9A C4A 1.307(6) . ? N9A Pt1B 2.027(4) . ? N9A H90A 0.8800 . ? C4A C5A 1.442(6) . ? C5A C6A 1.338(7) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? N10A C10A 1.490(6) . ? N10A H10A 0.9200 . ? N10A H10B 0.9200 . ? N11A C11A 1.474(6) . ? N11A H11A 0.9200 . ? N11A H11B 0.9200 . ? C10A C11A 1.518(7) . ? C10A H10C 0.9900 . ? C10A H10D 0.9900 . ? C11A H11C 0.9900 . ? C11A H11D 0.9900 . ? Pt1B N11B 2.039(4) . ? Pt1B N10B 2.039(4) . ? Pt1B N3B 2.058(4) . ? O8B C2B 1.231(5) . ? N1B C2B 1.372(6) . ? N1B C6B 1.379(6) . ? N1B C7B 1.454(6) . ? N3B C4B 1.374(6) . ? N3B C2B 1.379(6) . ? N9B C4B 1.304(6) . ? N9B H90B 0.8800 . ? C4B C5B 1.433(6) . ? C5B C6B 1.327(7) . ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? N10B C10B 1.486(6) . ? N10B H10G 0.9200 . ? N10B H10H 0.9200 . ? N11B C11B 1.501(6) . ? N11B H11H 0.9200 . ? N11B H11G 0.9200 . ? C10B C11B 1.507(7) . ? C10B H10L 0.9900 . ? C10B H10M 0.9900 . ? C11B H11L 0.9900 . ? C11B H11M 0.9900 . ? N13 O4 1.162(14) . ? N13 O3X 1.201(9) . ? N13 O4X 1.252(8) . ? N13 O2 1.255(15) . ? N13 O2X 1.256(8) . ? N13 O3 1.298(15) . ? N14 O7 1.230(6) . ? N14 O5 1.252(7) . ? N14 O6 1.259(7) . ? O10 H10E 0.8599 . ? O11 H11E 0.8594 . ? O11 H11F 0.8603 . ? O12 H12E 0.8607 . ? O12 H12F 0.8634 . ? 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 N9B Pt1A N11A 92.10(15) . . ? N9B Pt1A N10A 174.30(15) . . ? N11A Pt1A N10A 83.23(15) . . ? N9B Pt1A N3A 87.80(15) . . ? N11A Pt1A N3A 177.43(15) . . ? N10A Pt1A N3A 96.71(15) . . ? N9B Pt1A Pt1B 78.16(11) . . ? N11A Pt1A Pt1B 99.97(11) . . ? N10A Pt1A Pt1B 105.82(12) . . ? N3A Pt1A Pt1B 82.53(10) . . ? C6A N1A C2A 121.0(4) . . ? C6A N1A C7A 121.7(4) . . ? C2A N1A C7A 117.2(4) . . ? C4A N3A C2A 122.1(4) . . ? C4A N3A Pt1A 122.9(3) . . ? C2A N3A Pt1A 113.6(3) . . ? C4A N9A Pt1B 131.8(3) . . ? C4A N9A H90A 114.1 . . ? Pt1B N9A H90A 114.1 . . ? O8A C2A N3A 121.8(4) . . ? O8A C2A N1A 119.7(4) . . ? N3A C2A N1A 118.4(4) . . ? N9A C4A N3A 121.1(4) . . ? N9A C4A C5A 121.2(4) . . ? N3A C4A C5A 117.6(4) . . ? C6A C5A C4A 119.6(4) . . ? C6A C5A H5A 120.2 . . ? C4A C5A H5A 120.2 . . ? C5A C6A N1A 121.1(4) . . ? C5A C6A H6A 119.4 . . ? N1A C6A H6A 119.4 . . ? N1A C7A H7A1 109.5 . . ? N1A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? N1A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C10A N10A Pt1A 109.7(3) . . ? C10A N10A H10A 109.7 . . ? Pt1A N10A H10A 109.7 . . ? C10A N10A H10B 109.7 . . ? Pt1A N10A H10B 109.7 . . ? H10A N10A H10B 108.2 . . ? C11A N11A Pt1A 109.3(3) . . ? C11A N11A H11A 109.8 . . ? Pt1A N11A H11A 109.8 . . ? C11A N11A H11B 109.8 . . ? Pt1A N11A H11B 109.8 . . ? H11A N11A H11B 108.3 . . ? N10A C10A C11A 107.9(4) . . ? N10A C10A H10C 110.1 . . ? C11A C10A H10C 110.1 . . ? N10A C10A H10D 110.1 . . ? C11A C10A H10D 110.1 . . ? H10C C10A H10D 108.4 . . ? N11A C11A C10A 107.2(4) . . ? N11A C11A H11C 110.3 . . ? C10A C11A H11C 110.3 . . ? N11A C11A H11D 110.3 . . ? C10A C11A H11D 110.3 . . ? H11C C11A H11D 108.5 . . ? N9A Pt1B N11B 90.41(15) . . ? N9A Pt1B N10B 173.56(15) . . ? N11B Pt1B N10B 83.21(16) . . ? N9A Pt1B N3B 92.68(15) . . ? N11B Pt1B N3B 173.68(15) . . ? N10B Pt1B N3B 93.61(15) . . ? N9A Pt1B Pt1A 77.61(10) . . ? N11B Pt1B Pt1A 105.79(11) . . ? N10B Pt1B Pt1A 104.85(11) . . ? N3B Pt1B Pt1A 80.28(10) . . ? C2B N1B C6B 121.2(4) . . ? C2B N1B C7B 118.2(4) . . ? C6B N1B C7B 120.5(4) . . ? C4B N3B C2B 120.2(4) . . ? C4B N3B Pt1B 122.9(3) . . ? C2B N3B Pt1B 116.7(3) . . ? C4B N9B Pt1A 130.3(3) . . ? C4B N9B H90B 114.8 . . ? Pt1A N9B H90B 114.8 . . ? O8B C2B N1B 119.0(4) . . ? O8B C2B N3B 122.0(4) . . ? N1B C2B N3B 119.0(4) . . ? N9B C4B N3B 120.3(4) . . ? N9B C4B C5B 121.1(4) . . ? N3B C4B C5B 118.6(4) . . ? C6B C5B C4B 119.7(4) . . ? C6B C5B H5B 120.2 . . ? C4B C5B H5B 120.2 . . ? C5B C6B N1B 120.6(4) . . ? C5B C6B H6B 119.7 . . ? N1B C6B H6B 119.7 . . ? N1B C7B H7B1 109.5 . . ? N1B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? N1B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C10B N10B Pt1B 109.6(3) . . ? C10B N10B H10G 109.7 . . ? Pt1B N10B H10G 109.7 . . ? C10B N10B H10H 109.7 . . ? Pt1B N10B H10H 109.7 . . ? H10G N10B H10H 108.2 . . ? C11B N11B Pt1B 108.8(3) . . ? C11B N11B H11H 109.9 . . ? Pt1B N11B H11H 109.9 . . ? C11B N11B H11G 109.9 . . ? Pt1B N11B H11G 109.9 . . ? H11H N11B H11G 108.3 . . ? N10B C10B C11B 106.7(4) . . ? N10B C10B H10L 110.4 . . ? C11B C10B H10L 110.4 . . ? N10B C10B H10M 110.4 . . ? C11B C10B H10M 110.4 . . ? H10L C10B H10M 108.6 . . ? N11B C11B C10B 107.1(4) . . ? N11B C11B H11L 110.3 . . ? C10B C11B H11L 110.3 . . ? N11B C11B H11M 110.3 . . ? C10B C11B H11M 110.3 . . ? H11L C11B H11M 108.6 . . ? O4 N13 O3X 101.7(10) . . ? O3X N13 O4X 121.5(6) . . ? O4 N13 O2 124.6(12) . . ? O3X N13 O2 133.8(10) . . ? O4X N13 O2 104.7(10) . . ? O4 N13 O2X 136.6(10) . . ? O3X N13 O2X 121.7(6) . . ? O4X N13 O2X 116.8(6) . . ? O4 N13 O3 121.0(12) . . ? O4X N13 O3 140.9(10) . . ? O2 N13 O3 114.4(11) . . ? O2X N13 O3 102.4(11) . . ? O7 N14 O5 121.0(7) . . ? O7 N14 O6 120.3(6) . . ? O5 N14 O6 118.6(5) . . ? H11E O11 H11F 120.3 . . ? H12E O12 H12F 116.9 . . ? 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 N9B Pt1A N3A C4A 60.9(4) . . . . ? N10A Pt1A N3A C4A -122.6(3) . . . . ? Pt1B Pt1A N3A C4A -17.5(3) . . . . ? N9B Pt1A N3A C2A -105.8(3) . . . . ? N10A Pt1A N3A C2A 70.7(3) . . . . ? Pt1B Pt1A N3A C2A 175.8(3) . . . . ? C4A N3A C2A O8A 179.7(4) . . . . ? Pt1A N3A C2A O8A -13.4(6) . . . . ? C4A N3A C2A N1A -0.8(6) . . . . ? Pt1A N3A C2A N1A 166.0(3) . . . . ? C6A N1A C2A O8A -177.8(4) . . . . ? C7A N1A C2A O8A 5.5(7) . . . . ? C6A N1A C2A N3A 2.8(7) . . . . ? C7A N1A C2A N3A -173.9(4) . . . . ? Pt1B N9A C4A N3A 9.4(6) . . . . ? Pt1B N9A C4A C5A -170.7(3) . . . . ? C2A N3A C4A N9A 177.9(4) . . . . ? Pt1A N3A C4A N9A 12.2(6) . . . . ? C2A N3A C4A C5A -2.0(6) . . . . ? Pt1A N3A C4A C5A -167.6(3) . . . . ? N9A C4A C5A C6A -176.9(4) . . . . ? N3A C4A C5A C6A 3.0(6) . . . . ? C4A C5A C6A N1A -1.2(7) . . . . ? C2A N1A C6A C5A -1.8(7) . . . . ? C7A N1A C6A C5A 174.8(5) . . . . ? N11A Pt1A N10A C10A 10.1(3) . . . . ? N3A Pt1A N10A C10A -167.3(3) . . . . ? Pt1B Pt1A N10A C10A 108.6(3) . . . . ? N9B Pt1A N11A C11A -164.6(3) . . . . ? N10A Pt1A N11A C11A 18.7(3) . . . . ? Pt1B Pt1A N11A C11A -86.3(3) . . . . ? Pt1A N10A C10A C11A -36.1(4) . . . . ? Pt1A N11A C11A C10A -43.1(4) . . . . ? N10A C10A C11A N11A 52.0(5) . . . . ? C4A N9A Pt1B N11B 89.2(4) . . . . ? C4A N9A Pt1B N3B -96.4(4) . . . . ? C4A N9A Pt1B Pt1A -16.9(4) . . . . ? N9B Pt1A Pt1B N9A -75.68(15) . . . . ? N11A Pt1A Pt1B N9A -165.75(16) . . . . ? N10A Pt1A Pt1B N9A 108.54(15) . . . . ? N3A Pt1A Pt1B N9A 13.64(15) . . . . ? N9B Pt1A Pt1B N11B -162.55(16) . . . . ? N11A Pt1A Pt1B N11B 107.38(16) . . . . ? N10A Pt1A Pt1B N11B 21.66(16) . . . . ? N3A Pt1A Pt1B N11B -73.24(16) . . . . ? N9B Pt1A Pt1B N10B 110.44(15) . . . . ? N11A Pt1A Pt1B N10B 20.37(16) . . . . ? N10A Pt1A Pt1B N10B -65.34(16) . . . . ? N3A Pt1A Pt1B N10B -160.24(16) . . . . ? N9B Pt1A Pt1B N3B 19.26(15) . . . . ? N11A Pt1A Pt1B N3B -70.81(15) . . . . ? N10A Pt1A Pt1B N3B -156.52(15) . . . . ? N3A Pt1A Pt1B N3B 108.58(15) . . . . ? N9A Pt1B N3B C4B 53.0(3) . . . . ? N10B Pt1B N3B C4B -128.4(3) . . . . ? Pt1A Pt1B N3B C4B -23.9(3) . . . . ? N9A Pt1B N3B C2B -122.5(3) . . . . ? N10B Pt1B N3B C2B 56.1(3) . . . . ? Pt1A Pt1B N3B C2B 160.6(3) . . . . ? N11A Pt1A N9B C4B 75.3(4) . . . . ? N3A Pt1A N9B C4B -107.3(4) . . . . ? Pt1B Pt1A N9B C4B -24.5(4) . . . . ? C6B N1B C2B O8B -179.0(4) . . . . ? C7B N1B C2B O8B 3.9(6) . . . . ? C6B N1B C2B N3B 0.8(6) . . . . ? C7B N1B C2B N3B -176.3(4) . . . . ? C4B N3B C2B O8B 172.4(4) . . . . ? Pt1B N3B C2B O8B -11.9(5) . . . . ? C4B N3B C2B N1B -7.4(6) . . . . ? Pt1B N3B C2B N1B 168.3(3) . . . . ? Pt1A N9B C4B N3B 14.5(6) . . . . ? Pt1A N9B C4B C5B -164.6(3) . . . . ? C2B N3B C4B N9B -168.6(4) . . . . ? Pt1B N3B C4B N9B 16.0(6) . . . . ? C2B N3B C4B C5B 10.5(6) . . . . ? Pt1B N3B C4B C5B -164.9(3) . . . . ? N9B C4B C5B C6B 171.9(5) . . . . ? N3B C4B C5B C6B -7.2(7) . . . . ? C4B C5B C6B N1B 0.8(7) . . . . ? C2B N1B C6B C5B 2.5(7) . . . . ? C7B N1B C6B C5B 179.5(5) . . . . ? N11B Pt1B N10B C10B -14.7(3) . . . . ? N3B Pt1B N10B C10B 170.8(3) . . . . ? Pt1A Pt1B N10B C10B 89.9(3) . . . . ? N9A Pt1B N11B C11B 164.2(3) . . . . ? N10B Pt1B N11B C11B -15.0(3) . . . . ? Pt1A Pt1B N11B C11B -118.6(3) . . . . ? Pt1B N10B C10B C11B 41.2(4) . . . . ? Pt1B N11B C11B C10B 41.5(4) . . . . ? N10B C10B C11B N11B -54.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.586 _refine_diff_density_min -1.422 _refine_diff_density_rms 0.143 #===END data_vedj021a _database_code_depnum_ccdc_archive 'CCDC 758046' #TrackingRef 'CIF2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Chlorido(ethane-1,2-diamine)(1-methylcytosine)platinum(II) nitrate acetone solvate ; _chemical_name_common ; Chlorido(ethane-1,2-diamine)(1-methylcytosine)platinum(ii) nitrate acetone solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C7 H15 Cl N5 O Pt, 0.5(C6 H12 O2), N O3' _chemical_formula_sum 'C10 H21 Cl N6 O5 Pt' _chemical_formula_weight 535.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5962(5) _cell_length_b 8.4624(5) _cell_length_c 13.6279(10) _cell_angle_alpha 76.987(4) _cell_angle_beta 77.081(4) _cell_angle_gamma 86.098(4) _cell_volume 831.78(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1797 _cell_measurement_theta_min 3.14 _cell_measurement_theta_max 29.65 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 8.629 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3577 _exptl_absorpt_correction_T_max 0.6722 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42348 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 30.13 _reflns_number_total 4880 _reflns_number_gt 4498 _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^)+(0.0206P)^2^+0.3562P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4880 _refine_ls_number_parameters 226 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0211 _refine_ls_R_factor_gt 0.0174 _refine_ls_wR_factor_ref 0.0403 _refine_ls_wR_factor_gt 0.0391 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.965938(11) 0.210424(10) 0.076562(7) 0.01360(3) Uani 1 1 d . . . Cl1 Cl 1.22166(8) 0.35714(7) -0.00759(5) 0.01882(11) Uani 1 1 d . . . O8A O 1.1752(3) -0.0553(2) 0.20511(15) 0.0247(4) Uani 1 1 d . . . N1A N 1.1731(3) 0.0429(3) 0.34721(17) 0.0232(5) Uani 1 1 d . . . N3A N 1.0387(3) 0.1913(3) 0.21388(16) 0.0169(4) Uani 1 1 d . . . N9A N 0.9142(3) 0.4457(3) 0.22265(17) 0.0199(4) Uani 1 1 d . . . H9C H 0.8917 0.4552 0.1610 0.024 Uiso 1 1 calc R . . H9D H 0.8840 0.5250 0.2556 0.024 Uiso 1 1 calc R . . C2A C 1.1312(3) 0.0534(3) 0.2517(2) 0.0196(5) Uani 1 1 d . . . C4A C 0.9934(3) 0.3120(3) 0.26585(19) 0.0191(5) Uani 1 1 d . . . C5A C 1.0307(4) 0.2951(3) 0.3655(2) 0.0222(5) Uani 1 1 d . . . H5A H 0.9943 0.3764 0.4044 0.027 Uiso 1 1 calc R . . C6A C 1.1198(4) 0.1591(4) 0.4028(2) 0.0248(6) Uani 1 1 d . . . H6A H 1.1458 0.1444 0.4693 0.030 Uiso 1 1 calc R . . C7A C 1.2776(4) -0.1002(4) 0.3864(2) 0.0345(7) Uani 1 1 d . . . H7A H 1.3042 -0.0910 0.4520 0.052 Uiso 1 1 calc R . . H7B H 1.3910 -0.1074 0.3363 0.052 Uiso 1 1 calc R . . H7C H 1.2075 -0.1980 0.3971 0.052 Uiso 1 1 calc R . . N10A N 0.7319(3) 0.0898(3) 0.14555(17) 0.0190(4) Uani 1 1 d . . . H10A H 0.7575 -0.0110 0.1825 0.023 Uiso 1 1 calc R . . H10B H 0.6607 0.1464 0.1906 0.023 Uiso 1 1 calc R . . N11A N 0.8667(3) 0.2388(3) -0.05324(16) 0.0177(4) Uani 1 1 d . . . H11A H 0.8940 0.3398 -0.0946 0.021 Uiso 1 1 calc R . . H11B H 0.9168 0.1618 -0.0899 0.021 Uiso 1 1 calc R . . C10A C 0.6332(3) 0.0719(3) 0.0657(2) 0.0201(5) Uani 1 1 d . . . H10L H 0.5022 0.0612 0.0960 0.024 Uiso 1 1 calc R . . H10M H 0.6770 -0.0265 0.0391 0.024 Uiso 1 1 calc R . . C11A C 0.6665(3) 0.2200(3) -0.0204(2) 0.0193(5) Uani 1 1 d . . . H11L H 0.6156 0.2064 -0.0788 0.023 Uiso 1 1 calc R . . H11M H 0.6091 0.3170 0.0037 0.023 Uiso 1 1 calc R . . N2 N 0.1847(3) 0.2233(3) 0.65460(17) 0.0237(5) Uani 1 1 d . . . O1 O 0.2164(3) 0.2429(2) 0.73789(16) 0.0322(5) Uani 1 1 d . . . O2 O 0.1155(3) 0.3362(3) 0.59892(18) 0.0407(6) Uani 1 1 d . . . O3 O 0.2246(3) 0.0905(2) 0.62866(15) 0.0282(4) Uani 1 1 d . . . O5 O 0.5200(6) 0.2510(5) 0.3047(3) 0.0379(7) Uani 0.50 1 d PD A 1 C12 C 0.4745(5) 0.3907(8) 0.3168(4) 0.0276(9) Uani 0.50 1 d PD A 1 C13 C 0.4735(8) 0.4349(7) 0.4162(4) 0.0324(9) Uani 0.50 1 d PD A 1 H13A H 0.5299 0.3470 0.4597 0.049 Uiso 0.50 1 calc PR A 1 H13B H 0.3486 0.4523 0.4514 0.049 Uiso 0.50 1 calc PR A 1 H13C H 0.5413 0.5347 0.4033 0.049 Uiso 0.50 1 calc PR A 1 C14 C 0.4204(9) 0.5163(7) 0.2337(5) 0.0393(11) Uani 0.50 1 d PD A 1 H14A H 0.5139 0.5987 0.2069 0.059 Uiso 0.50 1 calc PR A 1 H14B H 0.3058 0.5674 0.2611 0.059 Uiso 0.50 1 calc PR A 1 H14C H 0.4057 0.4661 0.1779 0.059 Uiso 0.50 1 calc PR A 1 O5X O 0.4743(6) 0.3191(5) 0.2251(3) 0.0379(7) Uani 0.50 1 d PD B 2 C12X C 0.4674(5) 0.3834(7) 0.2997(5) 0.0276(9) Uani 0.50 1 d PD B 2 C13X C 0.5408(8) 0.2961(7) 0.3896(4) 0.0324(9) Uani 0.50 1 d PD B 2 H13D H 0.4414 0.2668 0.4498 0.049 Uiso 0.50 1 calc PR B 2 H13E H 0.6243 0.3662 0.4046 0.049 Uiso 0.50 1 calc PR B 2 H13F H 0.6052 0.1974 0.3739 0.049 Uiso 0.50 1 calc PR B 2 C14X C 0.3873(8) 0.5471(7) 0.3032(5) 0.0393(11) Uani 0.50 1 d PD B 2 H14D H 0.4822 0.6281 0.2759 0.059 Uiso 0.50 1 calc PR B 2 H14E H 0.3313 0.5517 0.3747 0.059 Uiso 0.50 1 calc PR B 2 H14F H 0.2955 0.5698 0.2613 0.059 Uiso 0.50 1 calc PR B 2 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 0.01081(4) 0.01567(5) 0.01438(5) -0.00230(3) -0.00321(3) -0.00216(3) Cl1 0.0123(3) 0.0233(3) 0.0193(3) -0.0004(2) -0.0035(2) -0.0037(2) O8A 0.0220(9) 0.0251(9) 0.0246(10) -0.0013(8) -0.0050(8) 0.0030(7) N1A 0.0178(11) 0.0296(12) 0.0197(11) 0.0037(9) -0.0072(9) -0.0040(9) N3A 0.0139(9) 0.0205(10) 0.0159(10) -0.0012(8) -0.0043(8) -0.0032(8) N9A 0.0217(11) 0.0194(10) 0.0212(11) -0.0077(8) -0.0063(9) -0.0020(8) C2A 0.0133(11) 0.0216(12) 0.0205(12) 0.0033(10) -0.0038(9) -0.0026(9) C4A 0.0144(11) 0.0245(12) 0.0180(12) -0.0024(10) -0.0030(9) -0.0065(9) C5A 0.0209(13) 0.0308(14) 0.0153(12) -0.0034(10) -0.0039(10) -0.0082(10) C6A 0.0198(13) 0.0385(15) 0.0147(12) 0.0001(11) -0.0038(10) -0.0108(11) C7A 0.0269(15) 0.0395(17) 0.0305(16) 0.0079(13) -0.0099(13) 0.0045(13) N10A 0.0152(10) 0.0206(10) 0.0206(11) -0.0025(8) -0.0027(8) -0.0062(8) N11A 0.0144(10) 0.0203(10) 0.0195(10) -0.0038(8) -0.0054(8) -0.0026(8) C10A 0.0137(11) 0.0217(12) 0.0268(14) -0.0078(10) -0.0045(10) -0.0047(9) C11A 0.0130(11) 0.0219(12) 0.0250(13) -0.0063(10) -0.0061(10) -0.0019(9) N2 0.0288(12) 0.0212(11) 0.0211(11) 0.0021(9) -0.0095(9) -0.0091(9) O1 0.0504(14) 0.0243(10) 0.0284(11) -0.0069(8) -0.0191(10) -0.0069(9) O2 0.0550(15) 0.0304(11) 0.0364(13) 0.0064(10) -0.0221(12) -0.0039(10) O3 0.0381(12) 0.0262(10) 0.0226(10) -0.0070(8) -0.0089(9) -0.0037(8) O5 0.0270(16) 0.046(2) 0.0374(18) -0.0135(15) 0.0062(14) -0.0050(14) C12 0.0156(13) 0.0283(15) 0.034(2) -0.0042(15) 0.0033(13) -0.0073(11) C13 0.030(2) 0.039(2) 0.028(2) -0.0032(18) -0.0083(18) -0.0036(18) C14 0.033(2) 0.039(2) 0.039(3) 0.000(2) -0.001(2) -0.0078(19) O5X 0.0270(16) 0.046(2) 0.0374(18) -0.0135(15) 0.0062(14) -0.0050(14) C12X 0.0156(13) 0.0283(15) 0.034(2) -0.0042(15) 0.0033(13) -0.0073(11) C13X 0.030(2) 0.039(2) 0.028(2) -0.0032(18) -0.0083(18) -0.0036(18) C14X 0.033(2) 0.039(2) 0.039(3) 0.000(2) -0.001(2) -0.0078(19) _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 N11A 2.033(2) . ? Pt1 N3A 2.036(2) . ? Pt1 N10A 2.038(2) . ? Pt1 Cl1 2.3067(6) . ? O8A C2A 1.220(3) . ? N1A C6A 1.360(4) . ? N1A C2A 1.389(3) . ? N1A C7A 1.467(4) . ? N3A C4A 1.353(3) . ? N3A C2A 1.379(3) . ? N9A C4A 1.325(3) . ? N9A H9C 0.8800 . ? N9A H9D 0.8800 . ? C4A C5A 1.423(3) . ? C5A C6A 1.351(4) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C7A H7A 0.9800 . ? C7A H7B 0.9800 . ? C7A H7C 0.9800 . ? N10A C10A 1.491(3) . ? N10A H10A 0.9200 . ? N10A H10B 0.9200 . ? N11A C11A 1.495(3) . ? N11A H11A 0.9200 . ? N11A H11B 0.9200 . ? C10A C11A 1.503(4) . ? C10A H10L 0.9900 . ? C10A H10M 0.9900 . ? C11A H11L 0.9900 . ? C11A H11M 0.9900 . ? N2 O2 1.244(3) . ? N2 O3 1.250(3) . ? N2 O1 1.260(3) . ? O5 C12 1.246(7) . ? C12 C14 1.479(7) . ? C12 C13 1.483(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O5X C12X 1.246(7) . ? C12X C14X 1.481(6) . ? C12X C13X 1.483(7) . ? C13X H13D 0.9800 . ? C13X H13E 0.9800 . ? C13X H13F 0.9800 . ? C14X H14D 0.9800 . ? C14X H14E 0.9800 . ? C14X H14F 0.9800 . ? 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 N11A Pt1 N3A 173.74(8) . . ? N11A Pt1 N10A 83.66(8) . . ? N3A Pt1 N10A 92.33(8) . . ? N11A Pt1 Cl1 93.68(6) . . ? N3A Pt1 Cl1 90.15(6) . . ? N10A Pt1 Cl1 176.69(6) . . ? C6A N1A C2A 122.0(2) . . ? C6A N1A C7A 120.9(2) . . ? C2A N1A C7A 117.1(2) . . ? C4A N3A C2A 122.0(2) . . ? C4A N3A Pt1 119.58(16) . . ? C2A N3A Pt1 118.46(17) . . ? C4A N9A H9C 120.0 . . ? C4A N9A H9D 120.0 . . ? H9C N9A H9D 120.0 . . ? O8A C2A N3A 122.7(2) . . ? O8A C2A N1A 120.7(2) . . ? N3A C2A N1A 116.6(2) . . ? N9A C4A N3A 119.1(2) . . ? N9A C4A C5A 120.6(2) . . ? N3A C4A C5A 120.3(2) . . ? C6A C5A C4A 117.5(3) . . ? C6A C5A H5A 121.3 . . ? C4A C5A H5A 121.3 . . ? C5A C6A N1A 121.5(2) . . ? C5A C6A H6A 119.3 . . ? N1A C6A H6A 119.3 . . ? N1A C7A H7A 109.5 . . ? N1A C7A H7B 109.5 . . ? H7A C7A H7B 109.5 . . ? N1A C7A H7C 109.5 . . ? H7A C7A H7C 109.5 . . ? H7B C7A H7C 109.5 . . ? C10A N10A Pt1 109.76(15) . . ? C10A N10A H10A 109.7 . . ? Pt1 N10A H10A 109.7 . . ? C10A N10A H10B 109.7 . . ? Pt1 N10A H10B 109.7 . . ? H10A N10A H10B 108.2 . . ? C11A N11A Pt1 107.49(15) . . ? C11A N11A H11A 110.2 . . ? Pt1 N11A H11A 110.2 . . ? C11A N11A H11B 110.2 . . ? Pt1 N11A H11B 110.2 . . ? H11A N11A H11B 108.5 . . ? N10A C10A C11A 108.17(19) . . ? N10A C10A H10L 110.1 . . ? C11A C10A H10L 110.1 . . ? N10A C10A H10M 110.1 . . ? C11A C10A H10M 110.1 . . ? H10L C10A H10M 108.4 . . ? N11A C11A C10A 106.8(2) . . ? N11A C11A H11L 110.4 . . ? C10A C11A H11L 110.4 . . ? N11A C11A H11M 110.4 . . ? C10A C11A H11M 110.4 . . ? H11L C11A H11M 108.6 . . ? O2 N2 O3 120.9(2) . . ? O2 N2 O1 119.7(2) . . ? O3 N2 O1 119.4(2) . . ? O5 C12 C14 121.5(5) . . ? O5 C12 C13 120.2(5) . . ? C14 C12 C13 118.3(5) . . ? O5X C12X C14X 122.4(6) . . ? O5X C12X C13X 120.2(5) . . ? C14X C12X C13X 117.3(5) . . ? C12X C13X H13D 109.5 . . ? C12X C13X H13E 109.5 . . ? H13D C13X H13E 109.5 . . ? C12X C13X H13F 109.5 . . ? H13D C13X H13F 109.5 . . ? H13E C13X H13F 109.5 . . ? C12X C14X H14D 109.5 . . ? C12X C14X H14E 109.5 . . ? H14D C14X H14E 109.5 . . ? C12X C14X H14F 109.5 . . ? H14D C14X H14F 109.5 . . ? H14E C14X H14F 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 N10A Pt1 N3A C4A -92.61(18) . . . . ? Cl1 Pt1 N3A C4A 85.20(18) . . . . ? N10A Pt1 N3A C2A 86.52(18) . . . . ? Cl1 Pt1 N3A C2A -95.67(17) . . . . ? C4A N3A C2A O8A -179.0(2) . . . . ? Pt1 N3A C2A O8A 1.9(3) . . . . ? C4A N3A C2A N1A 1.1(3) . . . . ? Pt1 N3A C2A N1A -177.97(16) . . . . ? C6A N1A C2A O8A -177.4(2) . . . . ? C7A N1A C2A O8A 2.4(4) . . . . ? C6A N1A C2A N3A 2.5(3) . . . . ? C7A N1A C2A N3A -177.7(2) . . . . ? C2A N3A C4A N9A 175.9(2) . . . . ? Pt1 N3A C4A N9A -5.0(3) . . . . ? C2A N3A C4A C5A -4.0(4) . . . . ? Pt1 N3A C4A C5A 175.12(18) . . . . ? N9A C4A C5A C6A -176.8(2) . . . . ? N3A C4A C5A C6A 3.2(4) . . . . ? C4A C5A C6A N1A 0.4(4) . . . . ? C2A N1A C6A C5A -3.3(4) . . . . ? C7A N1A C6A C5A 176.9(3) . . . . ? N11A Pt1 N10A C10A 6.62(16) . . . . ? N3A Pt1 N10A C10A -178.21(16) . . . . ? N10A Pt1 N11A C11A 22.09(15) . . . . ? Cl1 Pt1 N11A C11A -155.94(14) . . . . ? Pt1 N10A C10A C11A -34.1(2) . . . . ? Pt1 N11A C11A C10A -46.4(2) . . . . ? N10A C10A C11A N11A 53.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.13 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.152 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.115 #===END data_vedj036 _database_code_depnum_ccdc_archive 'CCDC 758047' #TrackingRef 'CIF2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Aqua-1kappaO)bis(ethane-1,2-diamine-1kappa^2^N,N',2kappa^2^N,N') (hydroxido-2kappaO)bis(miu-1-methylcytosinato-kappa^2^N3,N4) diplatinum(III)(Pt-Pt) triperchlorate monohydrate ; _chemical_name_common ; Aqua-1kappaO)bis(ethane-1,2-diamine- 1kappa$2!N,N',2kappa$2!N,N') (hydroxido-2kappaO)bis(miu-1- methylcytosinato-kappa$2!N3,N4) diplatinum(iii)(Pt-Pt) triperchlorate monohydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C14 H31 N10 O4 Pt2, 3(Cl O4), H2 O' _chemical_formula_sum 'C14 H33 Cl3 N10 O17 Pt2' _chemical_formula_weight 1110.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2503(4) _cell_length_b 12.3786(4) _cell_length_c 13.0732(5) _cell_angle_alpha 67.701(2) _cell_angle_beta 70.504(2) _cell_angle_gamma 64.629(2) _cell_volume 1489.76(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 484 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 24.06 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 9.742 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2461 _exptl_absorpt_correction_T_max 0.3228 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60066 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 24.00 _reflns_number_total 4655 _reflns_number_gt 4154 _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^)+(0.0330P)^2^+13.4332P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4655 _refine_ls_number_parameters 417 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.041 _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 Pt1A Pt 0.13581(2) 0.69707(2) 0.37748(2) 0.01124(9) Uani 1 1 d D . . Pt1B Pt 0.21021(2) 0.81576(2) 0.17398(2) 0.01230(9) Uani 1 1 d . . . O1 O 0.0751(4) 0.5927(3) 0.56454(19) 0.0186(10) Uani 1 1 d D . . H10E H -0.0072 0.6377 0.5892 0.022 Uiso 1 1 d RD . . H10F H 0.0793 0.5202 0.5651 0.022 Uiso 1 1 d RD . . O2 O 0.2746(5) 0.9091(4) 0.2265(4) 0.0227(11) Uani 1 1 d . . . H20A H 0.2694 0.9812 0.2245 0.027 Uiso 1 1 d R . . N1A N -0.2848(5) 0.8231(5) 0.4050(4) 0.0141(12) Uani 1 1 d . . . C2A C -0.1557(6) 0.7423(6) 0.4057(5) 0.0126(14) Uani 1 1 d . . . N3A N -0.0540(5) 0.7895(5) 0.3446(4) 0.0112(11) Uani 1 1 d . . . C4A C -0.0793(6) 0.9054(6) 0.2694(5) 0.0118(14) Uani 1 1 d . . . C5A C -0.2155(7) 0.9891(6) 0.2756(5) 0.0152(14) Uani 1 1 d . . . H5A H -0.2357 1.0739 0.2323 0.018 Uiso 1 1 calc R . . C6A C -0.3131(7) 0.9461(6) 0.3429(5) 0.0152(14) Uani 1 1 d . . . H6A H -0.4038 1.0010 0.3484 0.018 Uiso 1 1 calc R . . C7A C -0.3929(7) 0.7758(7) 0.4774(6) 0.0232(16) Uani 1 1 d . . . H7A1 H -0.3806 0.7000 0.4615 0.035 Uiso 1 1 calc R . . H7A2 H -0.4797 0.8389 0.4622 0.035 Uiso 1 1 calc R . . H7A3 H -0.3908 0.7569 0.5568 0.035 Uiso 1 1 calc R . . O8A O -0.1322(4) 0.6318(4) 0.4618(4) 0.0147(10) Uani 1 1 d . . . N9A N 0.0223(5) 0.9359(5) 0.1978(5) 0.0143(12) Uani 1 1 d . . . H9A H 0.0069 1.0141 0.1576 0.017 Uiso 1 1 calc R . . N1B N 0.0985(5) 0.6523(5) -0.0013(5) 0.0159(12) Uani 1 1 d . . . C2B C 0.1138(6) 0.7385(6) 0.0306(6) 0.0142(14) Uani 1 1 d . . . N3B N 0.1515(5) 0.7028(5) 0.1318(4) 0.0130(12) Uani 1 1 d . . . C4B C 0.1593(6) 0.5860(6) 0.2053(5) 0.0123(14) Uani 1 1 d . . . C5B C 0.1635(7) 0.4942(6) 0.1621(6) 0.0186(15) Uani 1 1 d . . . H5B H 0.1885 0.4089 0.2039 0.022 Uiso 1 1 calc R . . C6B C 0.1316(7) 0.5308(6) 0.0619(6) 0.0172(15) Uani 1 1 d . . . H6B H 0.1319 0.4705 0.0335 0.021 Uiso 1 1 calc R . . C7B C 0.0553(8) 0.6922(7) -0.1076(6) 0.0213(16) Uani 1 1 d . . . H7B1 H 0.0658 0.6191 -0.1269 0.032 Uiso 1 1 calc R . . H7B2 H 0.1104 0.7380 -0.1677 0.032 Uiso 1 1 calc R . . H7B3 H -0.0393 0.7464 -0.0994 0.032 Uiso 1 1 calc R . . O8B O 0.0937(5) 0.8470(4) -0.0316(4) 0.0201(11) Uani 1 1 d . . . N9B N 0.1626(6) 0.5667(5) 0.3089(4) 0.0156(12) Uani 1 1 d . . . H9B H 0.1779 0.4899 0.3528 0.019 Uiso 1 1 calc R . . N10A N 0.1154(6) 0.8358(5) 0.4395(5) 0.0168(12) Uani 1 1 d . . . H10A H 0.1286 0.9027 0.3805 0.020 Uiso 1 1 calc R . . H10B H 0.0301 0.8620 0.4816 0.020 Uiso 1 1 calc R . . N11A N 0.3181(6) 0.6174(5) 0.4245(5) 0.0193(13) Uani 1 1 d . . . H11A H 0.3174 0.5503 0.4871 0.023 Uiso 1 1 calc R . . H11B H 0.3848 0.5896 0.3669 0.023 Uiso 1 1 calc R . . C10A C 0.2154(7) 0.7871(7) 0.5104(6) 0.0202(15) Uani 1 1 d . . . H10C H 0.1855 0.7344 0.5852 0.024 Uiso 1 1 calc R . . H10D H 0.2263 0.8568 0.5218 0.024 Uiso 1 1 calc R . . C11A C 0.3461(7) 0.7119(7) 0.4509(6) 0.0217(16) Uani 1 1 d . . . H11C H 0.4131 0.6694 0.4998 0.026 Uiso 1 1 calc R . . H11D H 0.3819 0.7663 0.3804 0.026 Uiso 1 1 calc R . . N10B N 0.4097(5) 0.7017(5) 0.1468(5) 0.0183(13) Uani 1 1 d . . . H10M H 0.4571 0.7152 0.1833 0.022 Uiso 1 1 calc R . . H10N H 0.4158 0.6196 0.1755 0.022 Uiso 1 1 calc R . . N11B N 0.2702(6) 0.9173(5) 0.0083(5) 0.0191(13) Uani 1 1 d . . . H11E H 0.2331 0.9093 -0.0403 0.023 Uiso 1 1 calc R . . H11F H 0.2402 1.0003 0.0044 0.023 Uiso 1 1 calc R . . C10B C 0.4681(7) 0.7290(7) 0.0232(6) 0.0218(16) Uani 1 1 d . . . H10K H 0.4379 0.6908 -0.0131 0.026 Uiso 1 1 calc R . . H10L H 0.5674 0.6947 0.0100 0.026 Uiso 1 1 calc R . . C11B C 0.4200(7) 0.8699(7) -0.0259(6) 0.0220(16) Uani 1 1 d . . . H11K H 0.4593 0.9073 0.0034 0.026 Uiso 1 1 calc R . . H11L H 0.4479 0.8920 -0.1093 0.026 Uiso 1 1 calc R . . Cl2 Cl 0.77431(17) 0.86745(15) 0.65986(14) 0.0198(4) Uani 1 1 d . . . O3 O 0.7432(6) 0.8374(5) 0.7803(4) 0.0333(13) Uani 1 1 d . . . O4 O 0.8126(5) 0.7564(4) 0.6249(4) 0.0233(11) Uani 1 1 d . . . O5 O 0.8869(5) 0.9097(5) 0.6165(5) 0.0325(13) Uani 1 1 d . . . O6 O 0.6613(5) 0.9605(5) 0.6140(5) 0.0346(13) Uani 1 1 d . . . Cl3 Cl 0.43770(17) 0.64624(15) 0.77609(14) 0.0209(4) Uani 1 1 d . . . O7 O 0.3951(6) 0.5800(5) 0.8886(4) 0.0350(13) Uani 1 1 d . . . O8 O 0.5559(5) 0.5625(5) 0.7224(5) 0.0354(14) Uani 1 1 d . . . O9 O 0.4682(6) 0.7483(5) 0.7745(5) 0.0374(14) Uani 1 1 d . . . O10 O 0.3358(6) 0.6942(6) 0.7127(5) 0.0441(16) Uani 1 1 d . . . Cl4 Cl 0.25683(18) 0.24831(17) 0.87147(15) 0.0256(4) Uani 1 1 d . . . O11 O 0.2790(7) 0.1619(6) 0.9804(5) 0.0466(16) Uani 1 1 d . . . O12 O 0.1628(6) 0.2307(7) 0.8357(6) 0.0515(18) Uani 1 1 d . . . O13 O 0.2089(6) 0.3743(5) 0.8795(5) 0.0392(14) Uani 1 1 d . . . O14 O 0.3840(6) 0.2275(6) 0.7922(5) 0.0413(15) Uani 1 1 d . . . O15 O 0.3814(6) 0.4701(6) 0.6481(5) 0.0417(15) Uani 1 1 d . . . H15A H 0.3681 0.5350 0.6660 0.050 Uiso 1 1 d R . . H15B H 0.3817 0.3975 0.6911 0.050 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 Pt1A 0.01088(15) 0.00923(14) 0.01199(15) -0.00064(10) -0.00436(10) -0.00252(11) Pt1B 0.01163(15) 0.00870(14) 0.01387(15) -0.00091(10) -0.00122(10) -0.00408(11) O1 0.020(3) 0.014(2) 0.020(3) -0.002(2) -0.007(2) -0.004(2) O2 0.023(3) 0.021(3) 0.032(3) -0.011(2) -0.004(2) -0.013(2) N1A 0.014(3) 0.012(3) 0.014(3) 0.000(2) -0.005(2) -0.005(2) C2A 0.013(4) 0.011(3) 0.014(3) -0.001(3) -0.005(3) -0.005(3) N3A 0.014(3) 0.011(3) 0.011(3) -0.005(2) -0.003(2) -0.005(2) C4A 0.018(4) 0.010(3) 0.008(3) -0.001(3) -0.007(3) -0.004(3) C5A 0.022(4) 0.009(3) 0.011(3) -0.001(3) -0.003(3) -0.004(3) C6A 0.014(4) 0.015(3) 0.010(3) -0.002(3) -0.004(3) 0.000(3) C7A 0.015(4) 0.021(4) 0.030(4) -0.005(3) 0.002(3) -0.010(3) O8A 0.015(2) 0.009(2) 0.017(2) 0.001(2) -0.005(2) -0.0040(19) N9A 0.016(3) 0.007(3) 0.014(3) 0.003(2) -0.002(2) -0.004(2) N1B 0.017(3) 0.013(3) 0.016(3) 0.000(2) -0.003(2) -0.007(2) C2B 0.012(3) 0.012(3) 0.016(4) 0.000(3) -0.003(3) -0.004(3) N3B 0.018(3) 0.009(3) 0.013(3) -0.001(2) -0.004(2) -0.006(2) C4B 0.008(3) 0.010(3) 0.018(4) -0.005(3) -0.003(3) -0.001(3) C5B 0.021(4) 0.008(3) 0.023(4) -0.003(3) 0.000(3) -0.006(3) C6B 0.019(4) 0.017(4) 0.018(4) -0.010(3) 0.003(3) -0.010(3) C7B 0.030(4) 0.025(4) 0.011(4) -0.003(3) -0.004(3) -0.014(3) O8B 0.027(3) 0.013(2) 0.018(3) 0.003(2) -0.008(2) -0.008(2) N9B 0.024(3) 0.016(3) 0.010(3) -0.007(2) 0.006(2) -0.015(3) N10A 0.017(3) 0.016(3) 0.018(3) -0.007(2) -0.003(2) -0.005(2) N11A 0.019(3) 0.019(3) 0.018(3) -0.003(3) -0.008(3) -0.004(3) C10A 0.022(4) 0.022(4) 0.024(4) -0.008(3) -0.012(3) -0.006(3) C11A 0.025(4) 0.023(4) 0.025(4) -0.007(3) -0.012(3) -0.010(3) N10B 0.012(3) 0.021(3) 0.022(3) -0.007(3) -0.002(2) -0.006(2) N11B 0.023(3) 0.017(3) 0.017(3) -0.004(2) -0.003(3) -0.009(3) C10B 0.022(4) 0.023(4) 0.018(4) -0.008(3) 0.001(3) -0.008(3) C11B 0.020(4) 0.029(4) 0.018(4) -0.006(3) 0.001(3) -0.013(3) Cl2 0.0208(9) 0.0163(8) 0.0192(9) -0.0050(7) -0.0028(7) -0.0046(7) O3 0.045(4) 0.031(3) 0.023(3) -0.012(2) 0.000(3) -0.015(3) O4 0.029(3) 0.016(3) 0.023(3) -0.009(2) -0.007(2) -0.003(2) O5 0.029(3) 0.029(3) 0.038(3) -0.015(3) 0.008(3) -0.015(2) O6 0.025(3) 0.022(3) 0.047(4) -0.007(3) -0.017(3) 0.004(2) Cl3 0.0190(9) 0.0194(9) 0.0185(9) -0.0049(7) -0.0050(7) -0.0010(7) O7 0.039(3) 0.044(3) 0.024(3) -0.008(3) -0.001(3) -0.022(3) O8 0.030(3) 0.020(3) 0.038(3) -0.009(2) 0.008(3) -0.002(2) O9 0.057(4) 0.027(3) 0.032(3) -0.007(3) -0.011(3) -0.017(3) O10 0.035(3) 0.054(4) 0.039(4) -0.018(3) -0.020(3) 0.001(3) Cl4 0.0253(10) 0.0268(10) 0.0286(10) -0.0139(8) -0.0011(8) -0.0106(8) O11 0.059(4) 0.034(3) 0.039(4) 0.001(3) -0.013(3) -0.016(3) O12 0.028(3) 0.083(5) 0.071(5) -0.060(4) -0.003(3) -0.016(3) O13 0.045(4) 0.025(3) 0.048(4) -0.018(3) -0.006(3) -0.008(3) O14 0.028(3) 0.058(4) 0.039(4) -0.024(3) 0.006(3) -0.017(3) O15 0.043(4) 0.039(3) 0.035(3) -0.002(3) -0.011(3) -0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1A N9B 2.001(5) . ? Pt1A N3A 2.050(5) . ? Pt1A N11A 2.050(5) . ? Pt1A N10A 2.062(5) . ? Pt1A O1 2.3152(16) . ? Pt1A Pt1B 2.5570(3) . ? Pt1B O2 1.996(5) . ? Pt1B N9A 1.999(5) . ? Pt1B N10B 2.071(5) . ? Pt1B N3B 2.077(5) . ? Pt1B N11B 2.101(6) . ? O1 H10E 0.8760 . ? O1 H10F 0.8744 . ? O2 H20A 0.8596 . ? N1A C2A 1.367(8) . ? N1A C6A 1.377(8) . ? N1A C7A 1.463(9) . ? C2A O8A 1.239(8) . ? C2A N3A 1.377(8) . ? N3A C4A 1.369(8) . ? C4A N9A 1.308(8) . ? C4A C5A 1.431(9) . ? C5A C6A 1.329(9) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? N9A H9A 0.8800 . ? N1B C6B 1.366(9) . ? N1B C2B 1.372(8) . ? N1B C7B 1.462(9) . ? C2B O8B 1.245(8) . ? C2B N3B 1.378(8) . ? N3B C4B 1.384(8) . ? C4B N9B 1.294(8) . ? C4B C5B 1.426(9) . ? C5B C6B 1.332(10) . ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? N9B H9B 0.8800 . ? N10A C10A 1.477(8) . ? N10A H10A 0.9200 . ? N10A H10B 0.9200 . ? N11A C11A 1.510(9) . ? N11A H11A 0.9200 . ? N11A H11B 0.9200 . ? C10A C11A 1.499(10) . ? C10A H10C 0.9900 . ? C10A H10D 0.9900 . ? C11A H11C 0.9900 . ? C11A H11D 0.9900 . ? N10B C10B 1.491(9) . ? N10B H10M 0.9200 . ? N10B H10N 0.9200 . ? N11B C11B 1.494(9) . ? N11B H11E 0.9200 . ? N11B H11F 0.9200 . ? C10B C11B 1.523(10) . ? C10B H10K 0.9900 . ? C10B H10L 0.9900 . ? C11B H11K 0.9900 . ? C11B H11L 0.9900 . ? Cl2 O6 1.425(5) . ? Cl2 O3 1.428(5) . ? Cl2 O5 1.436(5) . ? Cl2 O4 1.457(5) . ? Cl3 O7 1.420(6) . ? Cl3 O10 1.425(6) . ? Cl3 O9 1.436(6) . ? Cl3 O8 1.443(5) . ? Cl4 O12 1.410(6) . ? Cl4 O14 1.444(6) . ? Cl4 O11 1.445(6) . ? Cl4 O13 1.449(5) . ? O15 H15A 0.8604 . ? O15 H15B 0.8597 . ? 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 N9B Pt1A N3A 90.1(2) . . ? N9B Pt1A N11A 96.7(2) . . ? N3A Pt1A N11A 172.8(2) . . ? N9B Pt1A N10A 176.6(2) . . ? N3A Pt1A N10A 90.7(2) . . ? N11A Pt1A N10A 82.6(2) . . ? N9B Pt1A O1 97.63(18) . . ? N3A Pt1A O1 97.22(18) . . ? N11A Pt1A O1 79.7(2) . . ? N10A Pt1A O1 85.59(19) . . ? N9B Pt1A Pt1B 84.52(15) . . ? N3A Pt1A Pt1B 84.69(14) . . ? N11A Pt1A Pt1B 98.12(17) . . ? N10A Pt1A Pt1B 92.23(16) . . ? O1 Pt1A Pt1B 177.11(11) . . ? O2 Pt1B N9A 91.0(2) . . ? O2 Pt1B N10B 85.4(2) . . ? N9A Pt1B N10B 175.9(2) . . ? O2 Pt1B N3B 174.2(2) . . ? N9A Pt1B N3B 92.3(2) . . ? N10B Pt1B N3B 91.4(2) . . ? O2 Pt1B N11B 87.4(2) . . ? N9A Pt1B N11B 95.7(2) . . ? N10B Pt1B N11B 82.1(2) . . ? N3B Pt1B N11B 97.0(2) . . ? O2 Pt1B Pt1A 91.25(14) . . ? N9A Pt1B Pt1A 83.54(15) . . ? N10B Pt1B Pt1A 98.59(16) . . ? N3B Pt1B Pt1A 84.37(14) . . ? N11B Pt1B Pt1A 178.48(15) . . ? Pt1A O1 H10E 106.6 . . ? Pt1A O1 H10F 106.7 . . ? H10E O1 H10F 111.5 . . ? Pt1B O2 H20A 145.8 . . ? C2A N1A C6A 121.8(5) . . ? C2A N1A C7A 117.4(5) . . ? C6A N1A C7A 120.7(5) . . ? O8A C2A N1A 120.8(6) . . ? O8A C2A N3A 121.9(6) . . ? N1A C2A N3A 117.3(5) . . ? C4A N3A C2A 121.3(5) . . ? C4A N3A Pt1A 117.6(4) . . ? C2A N3A Pt1A 120.7(4) . . ? N9A C4A N3A 118.6(6) . . ? N9A C4A C5A 123.1(6) . . ? N3A C4A C5A 118.3(6) . . ? C6A C5A C4A 118.7(6) . . ? C6A C5A H5A 120.6 . . ? C4A C5A H5A 120.6 . . ? C5A C6A N1A 121.0(6) . . ? C5A C6A H6A 119.5 . . ? N1A C6A H6A 119.5 . . ? N1A C7A H7A1 109.5 . . ? N1A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? N1A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C4A N9A Pt1B 124.1(4) . . ? C4A N9A H9A 118.0 . . ? Pt1B N9A H9A 118.0 . . ? C6B N1B C2B 120.2(6) . . ? C6B N1B C7B 121.3(6) . . ? C2B N1B C7B 118.4(5) . . ? O8B C2B N1B 120.1(6) . . ? O8B C2B N3B 121.0(6) . . ? N1B C2B N3B 119.0(5) . . ? C2B N3B C4B 120.1(5) . . ? C2B N3B Pt1B 121.6(4) . . ? C4B N3B Pt1B 118.2(4) . . ? N9B C4B N3B 117.9(6) . . ? N9B C4B C5B 124.0(6) . . ? N3B C4B C5B 118.0(6) . . ? C6B C5B C4B 118.5(6) . . ? C6B C5B H5B 120.7 . . ? C4B C5B H5B 120.7 . . ? C5B C6B N1B 122.0(6) . . ? C5B C6B H6B 119.0 . . ? N1B C6B H6B 119.0 . . ? N1B C7B H7B1 109.5 . . ? N1B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? N1B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C4B N9B Pt1A 125.4(5) . . ? C4B N9B H9B 117.3 . . ? Pt1A N9B H9B 117.3 . . ? C10A N10A Pt1A 109.1(4) . . ? C10A N10A H10A 109.9 . . ? Pt1A N10A H10A 109.9 . . ? C10A N10A H10B 109.9 . . ? Pt1A N10A H10B 109.9 . . ? H10A N10A H10B 108.3 . . ? C11A N11A Pt1A 109.7(4) . . ? C11A N11A H11A 109.7 . . ? Pt1A N11A H11A 109.7 . . ? C11A N11A H11B 109.7 . . ? Pt1A N11A H11B 109.7 . . ? H11A N11A H11B 108.2 . . ? N10A C10A C11A 107.8(5) . . ? N10A C10A H10C 110.1 . . ? C11A C10A H10C 110.1 . . ? N10A C10A H10D 110.1 . . ? C11A C10A H10D 110.1 . . ? H10C C10A H10D 108.5 . . ? C10A C11A N11A 107.1(5) . . ? C10A C11A H11C 110.3 . . ? N11A C11A H11C 110.3 . . ? C10A C11A H11D 110.3 . . ? N11A C11A H11D 110.3 . . ? H11C C11A H11D 108.6 . . ? C10B N10B Pt1B 109.5(4) . . ? C10B N10B H10M 109.8 . . ? Pt1B N10B H10M 109.8 . . ? C10B N10B H10N 109.8 . . ? Pt1B N10B H10N 109.8 . . ? H10M N10B H10N 108.2 . . ? C11B N11B Pt1B 109.7(4) . . ? C11B N11B H11E 109.7 . . ? Pt1B N11B H11E 109.7 . . ? C11B N11B H11F 109.7 . . ? Pt1B N11B H11F 109.7 . . ? H11E N11B H11F 108.2 . . ? N10B C10B C11B 107.6(6) . . ? N10B C10B H10K 110.2 . . ? C11B C10B H10K 110.2 . . ? N10B C10B H10L 110.2 . . ? C11B C10B H10L 110.2 . . ? H10K C10B H10L 108.5 . . ? N11B C11B C10B 107.5(6) . . ? N11B C11B H11K 110.2 . . ? C10B C11B H11K 110.2 . . ? N11B C11B H11L 110.2 . . ? C10B C11B H11L 110.2 . . ? H11K C11B H11L 108.5 . . ? O6 Cl2 O3 110.8(3) . . ? O6 Cl2 O5 110.2(3) . . ? O3 Cl2 O5 109.6(3) . . ? O6 Cl2 O4 109.0(3) . . ? O3 Cl2 O4 109.6(3) . . ? O5 Cl2 O4 107.6(3) . . ? O7 Cl3 O10 110.7(4) . . ? O7 Cl3 O9 110.9(3) . . ? O10 Cl3 O9 108.5(4) . . ? O7 Cl3 O8 109.1(3) . . ? O10 Cl3 O8 108.2(4) . . ? O9 Cl3 O8 109.4(4) . . ? O12 Cl4 O14 110.6(4) . . ? O12 Cl4 O11 110.2(4) . . ? O14 Cl4 O11 108.2(4) . . ? O12 Cl4 O13 110.4(4) . . ? O14 Cl4 O13 108.2(4) . . ? O11 Cl4 O13 109.1(4) . . ? H15A O15 H15B 129.4 . . ? 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 N9B Pt1A Pt1B O2 -154.4(2) . . . . ? N3A Pt1A Pt1B O2 114.9(2) . . . . ? N11A Pt1A Pt1B O2 -58.4(2) . . . . ? N10A Pt1A Pt1B O2 24.4(2) . . . . ? N9B Pt1A Pt1B N9A 114.7(2) . . . . ? N3A Pt1A Pt1B N9A 24.0(2) . . . . ? N11A Pt1A Pt1B N9A -149.3(2) . . . . ? N10A Pt1A Pt1B N9A -66.4(2) . . . . ? N9B Pt1A Pt1B N10B -68.9(2) . . . . ? N3A Pt1A Pt1B N10B -159.5(2) . . . . ? N11A Pt1A Pt1B N10B 27.2(2) . . . . ? N10A Pt1A Pt1B N10B 110.0(2) . . . . ? N9B Pt1A Pt1B N3B 21.8(2) . . . . ? N3A Pt1A Pt1B N3B -68.9(2) . . . . ? N11A Pt1A Pt1B N3B 117.8(2) . . . . ? N10A Pt1A Pt1B N3B -159.4(2) . . . . ? C6A N1A C2A O8A -179.7(6) . . . . ? C7A N1A C2A O8A 3.3(9) . . . . ? C6A N1A C2A N3A 2.1(9) . . . . ? C7A N1A C2A N3A -175.0(6) . . . . ? O8A C2A N3A C4A 169.6(6) . . . . ? N1A C2A N3A C4A -12.1(8) . . . . ? O8A C2A N3A Pt1A -17.9(8) . . . . ? N1A C2A N3A Pt1A 160.3(4) . . . . ? N9B Pt1A N3A C4A -115.3(5) . . . . ? N10A Pt1A N3A C4A 61.4(5) . . . . ? O1 Pt1A N3A C4A 147.0(4) . . . . ? Pt1B Pt1A N3A C4A -30.8(4) . . . . ? N9B Pt1A N3A C2A 72.0(5) . . . . ? N10A Pt1A N3A C2A -111.4(5) . . . . ? O1 Pt1A N3A C2A -25.7(5) . . . . ? Pt1B Pt1A N3A C2A 156.5(5) . . . . ? C2A N3A C4A N9A -166.5(6) . . . . ? Pt1A N3A C4A N9A 20.8(7) . . . . ? C2A N3A C4A C5A 15.6(8) . . . . ? Pt1A N3A C4A C5A -157.1(4) . . . . ? N9A C4A C5A C6A 173.3(6) . . . . ? N3A C4A C5A C6A -9.0(9) . . . . ? C4A C5A C6A N1A -0.7(9) . . . . ? C2A N1A C6A C5A 4.2(9) . . . . ? C7A N1A C6A C5A -178.8(6) . . . . ? N3A C4A N9A Pt1B 10.0(8) . . . . ? C5A C4A N9A Pt1B -172.2(5) . . . . ? O2 Pt1B N9A C4A -117.6(5) . . . . ? N3B Pt1B N9A C4A 57.7(5) . . . . ? N11B Pt1B N9A C4A 154.9(5) . . . . ? Pt1A Pt1B N9A C4A -26.4(5) . . . . ? C6B N1B C2B O8B 174.4(6) . . . . ? C7B N1B C2B O8B -1.5(9) . . . . ? C6B N1B C2B N3B -5.6(9) . . . . ? C7B N1B C2B N3B 178.5(6) . . . . ? O8B C2B N3B C4B 173.0(6) . . . . ? N1B C2B N3B C4B -7.0(9) . . . . ? O8B C2B N3B Pt1B -11.2(8) . . . . ? N1B C2B N3B Pt1B 168.8(4) . . . . ? N9A Pt1B N3B C2B 72.0(5) . . . . ? N10B Pt1B N3B C2B -106.2(5) . . . . ? N11B Pt1B N3B C2B -24.0(5) . . . . ? Pt1A Pt1B N3B C2B 155.3(5) . . . . ? N9A Pt1B N3B C4B -112.1(5) . . . . ? N10B Pt1B N3B C4B 69.7(5) . . . . ? N11B Pt1B N3B C4B 151.9(5) . . . . ? Pt1A Pt1B N3B C4B -28.8(4) . . . . ? C2B N3B C4B N9B -163.6(6) . . . . ? Pt1B N3B C4B N9B 20.5(7) . . . . ? C2B N3B C4B C5B 16.6(9) . . . . ? Pt1B N3B C4B C5B -159.3(5) . . . . ? N9B C4B C5B C6B 166.2(6) . . . . ? N3B C4B C5B C6B -14.0(9) . . . . ? C4B C5B C6B N1B 1.6(10) . . . . ? C2B N1B C6B C5B 8.3(10) . . . . ? C7B N1B C6B C5B -175.9(6) . . . . ? N3B C4B N9B Pt1A 7.6(8) . . . . ? C5B C4B N9B Pt1A -172.6(5) . . . . ? N3A Pt1A N9B C4B 61.1(5) . . . . ? N11A Pt1A N9B C4B -121.2(5) . . . . ? O1 Pt1A N9B C4B 158.4(5) . . . . ? Pt1B Pt1A N9B C4B -23.6(5) . . . . ? N3A Pt1A N10A C10A 160.7(5) . . . . ? N11A Pt1A N10A C10A -16.7(4) . . . . ? O1 Pt1A N10A C10A 63.5(4) . . . . ? Pt1B Pt1A N10A C10A -114.6(4) . . . . ? N9B Pt1A N11A C11A 164.3(4) . . . . ? N10A Pt1A N11A C11A -12.3(4) . . . . ? O1 Pt1A N11A C11A -99.1(4) . . . . ? Pt1B Pt1A N11A C11A 78.9(4) . . . . ? Pt1A N10A C10A C11A 42.8(6) . . . . ? N10A C10A C11A N11A -53.3(7) . . . . ? Pt1A N11A C11A C10A 38.6(6) . . . . ? O2 Pt1B N10B C10B -105.6(4) . . . . ? N3B Pt1B N10B C10B 79.3(4) . . . . ? N11B Pt1B N10B C10B -17.6(4) . . . . ? Pt1A Pt1B N10B C10B 163.8(4) . . . . ? O2 Pt1B N11B C11B 74.0(4) . . . . ? N9A Pt1B N11B C11B 164.8(4) . . . . ? N10B Pt1B N11B C11B -11.7(4) . . . . ? N3B Pt1B N11B C11B -102.2(4) . . . . ? Pt1B N10B C10B C11B 43.1(6) . . . . ? Pt1B N11B C11B C10B 38.0(6) . . . . ? N10B C10B C11B N11B -53.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 4.069 _refine_diff_density_min -1.825 _refine_diff_density_rms 0.156 #===END data_vedj041 _database_code_depnum_ccdc_archive 'CCDC 758048' #TrackingRef 'CIF2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Ethane-1,2-diamine)bis(1-methylcytosine)platinum(II)dinitrate dihydrate ; _chemical_name_common ;(Ethane-1,2-diamine)bis(1- methylcytosine)platinum(ii)dinitrate dihydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H22 N8 O2 Pt, 2(N O3), 2(O)' _chemical_formula_sum 'C12 H26 N10 O10 Pt' _chemical_formula_weight 665.52 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 10.7582(10) _cell_length_b 14.5690(17) _cell_length_c 14.0733(15) _cell_angle_alpha 90.00 _cell_angle_beta 101.110(6) _cell_angle_gamma 90.00 _cell_volume 2164.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 20.21 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.042 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 6.556 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5067 _exptl_absorpt_correction_T_max 0.5601 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59830 _diffrn_reflns_av_R_equivalents 0.0978 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 30.13 _reflns_number_total 6356 _reflns_number_gt 4787 _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^)+(0.0138P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6356 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0521 _refine_ls_wR_factor_gt 0.0492 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _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 0.889378(12) 0.593338(10) 0.170047(10) 0.01020(4) Uani 1 1 d . . . N1A N 0.6868(3) 0.3836(2) 0.2809(2) 0.0147(7) Uani 1 1 d . . . C2A C 0.7598(3) 0.4607(3) 0.2741(3) 0.0138(8) Uani 1 1 d . . . N3A N 0.7539(3) 0.4985(2) 0.1841(2) 0.0122(7) Uani 1 1 d . . . C4A C 0.6791(3) 0.4614(3) 0.1042(3) 0.0132(8) Uani 1 1 d . . . C5A C 0.6133(3) 0.3785(3) 0.1123(3) 0.0174(9) Uani 1 1 d . . . H5A H 0.5656 0.3493 0.0566 0.021 Uiso 1 1 calc R . . C6A C 0.6202(3) 0.3423(3) 0.2006(3) 0.0187(9) Uani 1 1 d . . . H6A H 0.5774 0.2863 0.2072 0.022 Uiso 1 1 calc R . . C7A C 0.6899(4) 0.3462(3) 0.3780(3) 0.0248(10) Uani 1 1 d . . . H7A1 H 0.6290 0.2957 0.3742 0.037 Uiso 1 1 calc R . . H7A2 H 0.6676 0.3945 0.4202 0.037 Uiso 1 1 calc R . . H7A3 H 0.7752 0.3233 0.4046 0.037 Uiso 1 1 calc R . . O8A O 0.8287(2) 0.49301(19) 0.34678(18) 0.0160(6) Uani 1 1 d . . . N9A N 0.6691(3) 0.5052(2) 0.0213(2) 0.0159(7) Uani 1 1 d . . . H9A1 H 0.7102 0.5570 0.0185 0.019 Uiso 1 1 calc R . . H9A2 H 0.6213 0.4826 -0.0313 0.019 Uiso 1 1 calc R . . N1B N 0.6548(3) 0.8249(2) 0.0910(2) 0.0150(7) Uani 1 1 d . . . C2B C 0.7205(3) 0.7438(3) 0.0878(3) 0.0129(8) Uani 1 1 d . . . N3B N 0.7724(2) 0.7032(2) 0.1742(2) 0.0093(7) Uani 1 1 d . . . C4B C 0.7549(3) 0.7387(3) 0.2594(3) 0.0112(8) Uani 1 1 d . . . C5B C 0.6900(3) 0.8226(3) 0.2610(3) 0.0140(8) Uani 1 1 d . . . H5B H 0.6805 0.8498 0.3205 0.017 Uiso 1 1 calc R . . C6B C 0.6419(3) 0.8629(3) 0.1763(3) 0.0168(9) Uani 1 1 d . . . H6B H 0.5978 0.9194 0.1762 0.020 Uiso 1 1 calc R . . C7B C 0.5998(4) 0.8687(3) -0.0010(3) 0.0240(10) Uani 1 1 d . . . H7B1 H 0.5373 0.9146 0.0098 0.036 Uiso 1 1 calc R . . H7B2 H 0.5583 0.8222 -0.0466 0.036 Uiso 1 1 calc R . . H7B3 H 0.6669 0.8987 -0.0278 0.036 Uiso 1 1 calc R . . O8B O 0.7305(2) 0.70987(19) 0.00887(18) 0.0162(6) Uani 1 1 d . . . N9B N 0.8037(3) 0.6961(2) 0.3410(2) 0.0138(7) Uani 1 1 d . . . H9B1 H 0.8471 0.6451 0.3395 0.017 Uiso 1 1 calc R . . H9B2 H 0.7929 0.7187 0.3968 0.017 Uiso 1 1 calc R . . N10 N 1.0326(3) 0.6768(2) 0.1477(2) 0.0136(7) Uani 1 1 d . . . H10A H 1.0144 0.6998 0.0856 0.016 Uiso 1 1 calc R . . H10B H 1.0403 0.7254 0.1901 0.016 Uiso 1 1 calc R . . N11 N 1.0208(3) 0.4932(2) 0.1730(2) 0.0176(8) Uani 1 1 d . . . H11A H 1.0521 0.4761 0.2360 0.021 Uiso 1 1 calc R . . H11B H 0.9842 0.4425 0.1399 0.021 Uiso 1 1 calc R . . C10 C 1.1544(3) 0.6244(3) 0.1622(3) 0.0172(9) Uani 1 1 d . . . H10E H 1.1950 0.6244 0.2316 0.021 Uiso 1 1 calc R . . H10F H 1.2133 0.6534 0.1251 0.021 Uiso 1 1 calc R . . C11 C 1.1255(3) 0.5273(3) 0.1276(3) 0.0175(9) Uani 1 1 d . . . H11E H 1.0998 0.5260 0.0562 0.021 Uiso 1 1 calc R . . H11F H 1.2013 0.4881 0.1466 0.021 Uiso 1 1 calc R . . N12 N 0.4701(3) 0.6014(2) 0.1989(2) 0.0166(7) Uani 1 1 d . . . O1 O 0.4947(3) 0.6351(2) 0.2821(2) 0.0374(9) Uani 1 1 d . . . O2 O 0.4411(2) 0.5184(2) 0.1873(2) 0.0215(7) Uani 1 1 d . . . O3 O 0.4737(2) 0.6503(2) 0.1268(2) 0.0258(7) Uani 1 1 d . . . N13 N 0.0838(3) 0.7750(3) 0.3824(2) 0.0184(8) Uani 1 1 d . . . O4 O 0.0585(3) 0.8258(2) 0.4469(2) 0.0313(8) Uani 1 1 d . . . O5 O 0.1079(3) 0.6920(2) 0.3995(2) 0.0323(8) Uani 1 1 d . . . O6 O 0.0853(2) 0.8078(2) 0.3003(2) 0.0215(7) Uani 1 1 d . . . O9 O 0.1726(4) 0.5046(3) 0.3798(3) 0.0353(11) Uiso 0.75 1 d P . . O9X O 0.3103(8) 0.5687(6) 0.4016(7) 0.009(2) Uiso 0.25 1 d P . . O10 O 0.0184(4) 0.3775(3) 0.4519(3) 0.0336(11) Uiso 0.75 1 d P . . O10X O 0.0979(10) 0.4392(8) 0.3698(8) 0.021(3) Uiso 0.25 1 d P . . 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 0.01105(6) 0.01009(7) 0.01032(7) 0.00009(8) 0.00423(4) -0.00012(7) N1A 0.0150(16) 0.0114(19) 0.0193(18) -0.0007(14) 0.0076(13) -0.0005(13) C2A 0.0132(19) 0.010(2) 0.020(2) 0.0037(17) 0.0069(16) -0.0001(15) N3A 0.0120(15) 0.0124(18) 0.0131(17) -0.0015(14) 0.0045(13) -0.0007(13) C4A 0.0079(17) 0.016(2) 0.016(2) -0.0022(17) 0.0025(15) 0.0041(15) C5A 0.0145(19) 0.012(2) 0.025(2) -0.0052(18) 0.0025(16) -0.0007(15) C6A 0.0130(19) 0.012(2) 0.033(3) -0.0061(19) 0.0106(17) -0.0007(16) C7A 0.034(2) 0.016(2) 0.029(3) 0.009(2) 0.017(2) -0.0014(19) O8A 0.0170(14) 0.0187(17) 0.0116(15) 0.0005(12) 0.0006(11) -0.0040(11) N9A 0.0132(15) 0.0176(19) 0.0166(18) -0.0045(15) 0.0022(13) -0.0022(14) N1B 0.0188(17) 0.0147(19) 0.0122(18) 0.0039(14) 0.0047(13) 0.0043(14) C2B 0.0117(18) 0.012(2) 0.016(2) 0.0025(17) 0.0054(15) -0.0023(15) N3B 0.0076(14) 0.0116(18) 0.0090(16) 0.0006(13) 0.0019(12) 0.0014(12) C4B 0.0091(17) 0.012(2) 0.013(2) -0.0008(16) 0.0023(14) -0.0027(15) C5B 0.0167(19) 0.013(2) 0.014(2) -0.0019(17) 0.0078(15) -0.0004(16) C6B 0.019(2) 0.012(2) 0.021(2) -0.0015(18) 0.0072(17) 0.0043(16) C7B 0.032(2) 0.020(2) 0.018(2) 0.0060(19) 0.0006(18) 0.0112(19) O8B 0.0271(15) 0.0156(16) 0.0069(14) -0.0022(12) 0.0057(11) 0.0036(12) N9B 0.0139(16) 0.0151(19) 0.0122(17) -0.0053(14) 0.0022(13) 0.0014(13) N10 0.0141(16) 0.0123(18) 0.0161(18) 0.0008(14) 0.0069(13) -0.0011(13) N11 0.0159(17) 0.016(2) 0.023(2) 0.0045(16) 0.0096(14) 0.0029(14) C10 0.0101(18) 0.023(2) 0.019(2) 0.0040(18) 0.0025(15) 0.0031(16) C11 0.0105(18) 0.021(2) 0.022(2) 0.0026(19) 0.0059(16) 0.0025(16) N12 0.0123(15) 0.018(2) 0.0180(18) -0.0040(17) 0.0001(12) 0.0028(15) O1 0.053(2) 0.035(2) 0.0174(18) -0.0145(15) -0.0103(15) 0.0048(17) O2 0.0207(14) 0.0136(16) 0.0297(18) -0.0038(14) 0.0034(12) -0.0022(12) O3 0.0278(16) 0.0242(18) 0.0266(18) 0.0115(15) 0.0085(13) 0.0023(13) N13 0.0170(17) 0.018(2) 0.020(2) -0.0037(17) 0.0023(14) -0.0016(15) O4 0.058(2) 0.0237(19) 0.0160(17) -0.0038(14) 0.0159(15) -0.0037(16) O5 0.0380(18) 0.0197(19) 0.038(2) 0.0097(15) 0.0053(15) 0.0136(14) O6 0.0306(16) 0.0204(17) 0.0154(16) -0.0018(13) 0.0091(12) -0.0090(13) _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 N11 2.027(3) . ? Pt1 N10 2.034(3) . ? Pt1 N3B 2.044(3) . ? Pt1 N3A 2.046(3) . ? N1A C6A 1.357(5) . ? N1A C2A 1.386(5) . ? N1A C7A 1.465(5) . ? C2A O8A 1.235(4) . ? C2A N3A 1.370(5) . ? N3A C4A 1.362(4) . ? C4A N9A 1.316(5) . ? C4A C5A 1.415(5) . ? C5A C6A 1.339(5) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? N9A H9A1 0.8800 . ? N9A H9A2 0.8800 . ? N1B C6B 1.353(5) . ? N1B C2B 1.382(5) . ? N1B C7B 1.462(5) . ? C2B O8B 1.239(4) . ? C2B N3B 1.371(4) . ? N3B C4B 1.353(5) . ? C4B N9B 1.322(4) . ? C4B C5B 1.409(5) . ? C5B C6B 1.340(5) . ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? N9B H9B1 0.8800 . ? N9B H9B2 0.8800 . ? N10 C10 1.497(4) . ? N10 H10A 0.9200 . ? N10 H10B 0.9200 . ? N11 C11 1.483(5) . ? N11 H11A 0.9200 . ? N11 H11B 0.9200 . ? C10 C11 1.509(5) . ? C10 H10E 0.9900 . ? C10 H10F 0.9900 . ? C11 H11E 0.9900 . ? C11 H11F 0.9900 . ? N12 O3 1.248(4) . ? N12 O1 1.249(4) . ? N12 O2 1.250(4) . ? N13 O4 1.242(4) . ? N13 O5 1.250(4) . ? N13 O6 1.253(4) . ? O9 O10X 1.237(11) . ? O9 O9X 1.728(10) . ? O10 O10X 1.804(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Pt1 N10 83.52(13) . . ? N11 Pt1 N3B 173.86(12) . . ? N10 Pt1 N3B 91.46(12) . . ? N11 Pt1 N3A 91.07(12) . . ? N10 Pt1 N3A 173.58(12) . . ? N3B Pt1 N3A 94.14(12) . . ? C6A N1A C2A 121.1(3) . . ? C6A N1A C7A 121.7(3) . . ? C2A N1A C7A 117.1(3) . . ? O8A C2A N3A 121.8(4) . . ? O8A C2A N1A 120.6(4) . . ? N3A C2A N1A 117.6(3) . . ? C4A N3A C2A 121.2(3) . . ? C4A N3A Pt1 120.5(3) . . ? C2A N3A Pt1 116.9(2) . . ? N9A C4A N3A 118.3(4) . . ? N9A C4A C5A 121.9(3) . . ? N3A C4A C5A 119.8(4) . . ? C6A C5A C4A 118.2(4) . . ? C6A C5A H5A 120.9 . . ? C4A C5A H5A 120.9 . . ? C5A C6A N1A 121.6(4) . . ? C5A C6A H6A 119.2 . . ? N1A C6A H6A 119.2 . . ? N1A C7A H7A1 109.5 . . ? N1A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? N1A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C4A N9A H9A1 120.0 . . ? C4A N9A H9A2 120.0 . . ? H9A1 N9A H9A2 120.0 . . ? C6B N1B C2B 121.3(3) . . ? C6B N1B C7B 120.9(3) . . ? C2B N1B C7B 117.8(3) . . ? O8B C2B N3B 122.1(4) . . ? O8B C2B N1B 120.3(3) . . ? N3B C2B N1B 117.6(3) . . ? C4B N3B C2B 121.3(3) . . ? C4B N3B Pt1 121.1(2) . . ? C2B N3B Pt1 117.4(2) . . ? N9B C4B N3B 119.3(3) . . ? N9B C4B C5B 120.6(4) . . ? N3B C4B C5B 120.0(3) . . ? C6B C5B C4B 118.3(4) . . ? C6B C5B H5B 120.9 . . ? C4B C5B H5B 120.9 . . ? C5B C6B N1B 121.5(4) . . ? C5B C6B H6B 119.3 . . ? N1B C6B H6B 119.3 . . ? N1B C7B H7B1 109.5 . . ? N1B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? N1B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C4B N9B H9B1 120.0 . . ? C4B N9B H9B2 120.0 . . ? H9B1 N9B H9B2 120.0 . . ? C10 N10 Pt1 110.1(2) . . ? C10 N10 H10A 109.6 . . ? Pt1 N10 H10A 109.6 . . ? C10 N10 H10B 109.6 . . ? Pt1 N10 H10B 109.6 . . ? H10A N10 H10B 108.2 . . ? C11 N11 Pt1 109.5(2) . . ? C11 N11 H11A 109.8 . . ? Pt1 N11 H11A 109.8 . . ? C11 N11 H11B 109.8 . . ? Pt1 N11 H11B 109.8 . . ? H11A N11 H11B 108.2 . . ? N10 C10 C11 108.2(3) . . ? N10 C10 H10E 110.1 . . ? C11 C10 H10E 110.1 . . ? N10 C10 H10F 110.1 . . ? C11 C10 H10F 110.1 . . ? H10E C10 H10F 108.4 . . ? N11 C11 C10 107.6(3) . . ? N11 C11 H11E 110.2 . . ? C10 C11 H11E 110.2 . . ? N11 C11 H11F 110.2 . . ? C10 C11 H11F 110.2 . . ? H11E C11 H11F 108.5 . . ? O3 N12 O1 120.2(4) . . ? O3 N12 O2 119.5(3) . . ? O1 N12 O2 120.4(4) . . ? O4 N13 O5 120.2(4) . . ? O4 N13 O6 119.3(4) . . ? O5 N13 O6 120.6(4) . . ? O10X O9 O9X 162.3(7) . . ? O9 O10X O10 133.5(8) . . ? 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 C6A N1A C2A O8A -173.6(3) . . . . ? C7A N1A C2A O8A 3.4(5) . . . . ? C6A N1A C2A N3A 5.5(5) . . . . ? C7A N1A C2A N3A -177.5(3) . . . . ? O8A C2A N3A C4A 179.0(3) . . . . ? N1A C2A N3A C4A -0.1(5) . . . . ? O8A C2A N3A Pt1 12.3(5) . . . . ? N1A C2A N3A Pt1 -166.8(2) . . . . ? N11 Pt1 N3A C4A -91.4(3) . . . . ? N3B Pt1 N3A C4A 91.9(3) . . . . ? N11 Pt1 N3A C2A 75.4(3) . . . . ? N3B Pt1 N3A C2A -101.3(3) . . . . ? C2A N3A C4A N9A 174.3(3) . . . . ? Pt1 N3A C4A N9A -19.5(5) . . . . ? C2A N3A C4A C5A -4.9(5) . . . . ? Pt1 N3A C4A C5A 161.4(3) . . . . ? N9A C4A C5A C6A -174.5(4) . . . . ? N3A C4A C5A C6A 4.6(5) . . . . ? C4A C5A C6A N1A 0.7(6) . . . . ? C2A N1A C6A C5A -5.8(6) . . . . ? C7A N1A C6A C5A 177.3(4) . . . . ? C6B N1B C2B O8B 179.5(3) . . . . ? C7B N1B C2B O8B -0.7(5) . . . . ? C6B N1B C2B N3B 0.0(5) . . . . ? C7B N1B C2B N3B 179.8(3) . . . . ? O8B C2B N3B C4B -176.5(3) . . . . ? N1B C2B N3B C4B 3.0(5) . . . . ? O8B C2B N3B Pt1 8.6(5) . . . . ? N1B C2B N3B Pt1 -171.9(2) . . . . ? N10 Pt1 N3B C4B -99.0(3) . . . . ? N3A Pt1 N3B C4B 84.1(3) . . . . ? N10 Pt1 N3B C2B 75.9(3) . . . . ? N3A Pt1 N3B C2B -101.0(3) . . . . ? C2B N3B C4B N9B 178.2(3) . . . . ? Pt1 N3B C4B N9B -7.1(5) . . . . ? C2B N3B C4B C5B -4.5(5) . . . . ? Pt1 N3B C4B C5B 170.2(2) . . . . ? N9B C4B C5B C6B -179.8(3) . . . . ? N3B C4B C5B C6B 3.0(5) . . . . ? C4B C5B C6B N1B -0.1(6) . . . . ? C2B N1B C6B C5B -1.4(6) . . . . ? C7B N1B C6B C5B 178.8(4) . . . . ? N11 Pt1 N10 C10 -9.4(2) . . . . ? N3B Pt1 N10 C10 167.0(2) . . . . ? N10 Pt1 N11 C11 -18.2(2) . . . . ? N3A Pt1 N11 C11 158.4(3) . . . . ? Pt1 N10 C10 C11 34.7(4) . . . . ? Pt1 N11 C11 C10 41.8(3) . . . . ? N10 C10 C11 N11 -50.0(4) . . . . ? O9X O9 O10X O10 89(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.13 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.910 _refine_diff_density_min -1.141 _refine_diff_density_rms 0.163 #===END data_vedj047 _database_code_depnum_ccdc_archive 'CCDC 758049' #TrackingRef 'CIF2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(ethane-1,2-diamine-1kappa^2^N,N',2kappa^2^N,N')bis(miu-1-methylcytosinato- kappa^2^N3,N4)(disulfato-1kappaO,2kappaO)diplatinum(III)(Pt-Pt) hydrate ; _chemical_name_common ; Bis(ethane-1,2-diamine-1kappa$2!N,N',2kappa$2!N,N')bis(miu-1- methylcytosinato-kappa$2!N3,N4)(disulfato- 1kappaO,2kappaO)diplatinum(iii)(Pt-Pt) hydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C14 H28 N10 O10 Pt2 S2, 2(H2 O), 2(O0.80)' _chemical_formula_sum 'C14 H35.20 N10 O13.60 Pt2 S2' _chemical_formula_weight 1015.62 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 19.8579(6) _cell_length_b 12.0130(6) _cell_length_c 14.3117(6) _cell_angle_alpha 90.00 _cell_angle_beta 125.859(4) _cell_angle_gamma 90.00 _cell_volume 2767.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 489 _cell_measurement_theta_min 3.38 _cell_measurement_theta_max 27.57 _exptl_crystal_description stick _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 10.334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4247 _exptl_absorpt_correction_T_max 0.8200 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23112 _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2718 _reflns_number_gt 2191 _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^)+(0.0313P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2718 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0605 _refine_ls_wR_factor_gt 0.0572 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _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 Pt1A Pt 0.058173(13) 0.290819(19) 0.234354(19) 0.00843(8) Uani 1 1 d . . . S1A S 0.23633(9) 0.20164(14) 0.29653(13) 0.0144(3) Uani 1 1 d . . . O1A O 0.1522(2) 0.2583(3) 0.2089(4) 0.0119(9) Uani 1 1 d . . . O2A O 0.2823(3) 0.2088(4) 0.2473(4) 0.0242(11) Uani 1 1 d . . . O3A O 0.2196(2) 0.0838(3) 0.3076(4) 0.0185(10) Uani 1 1 d . . . O4A O 0.2771(2) 0.2562(4) 0.4077(4) 0.0173(10) Uani 1 1 d . . . N1A N -0.0663(3) 0.1200(5) -0.0858(4) 0.0172(12) Uani 1 1 d . . . C2A C -0.0255(3) 0.2054(5) -0.0060(5) 0.0129(12) Uani 1 1 d . . . N3A N -0.0254(3) 0.2018(4) 0.0902(4) 0.0112(10) Uani 1 1 d . . . C4A C -0.0773(3) 0.1297(5) 0.0959(5) 0.0116(12) Uani 1 1 d . . . C5A C -0.1117(3) 0.0390(5) 0.0179(5) 0.0142(13) Uani 1 1 d . . . H5 H -0.1385 -0.0202 0.0284 0.017 Uiso 1 1 calc R . . C6A C -0.1060(4) 0.0380(5) -0.0702(5) 0.0165(14) Uani 1 1 d . . . H6 H -0.1304 -0.0218 -0.1237 0.020 Uiso 1 1 calc R . . C7A C -0.0702(4) 0.1261(6) -0.1906(5) 0.0246(16) Uani 1 1 d . . . H7A H -0.1104 0.0714 -0.2465 0.037 Uiso 1 1 calc R . . H7B H -0.0152 0.1099 -0.1721 0.037 Uiso 1 1 calc R . . H7C H -0.0876 0.2010 -0.2235 0.037 Uiso 1 1 calc R . . O8A O 0.0081(3) 0.2814(4) -0.0226(4) 0.0188(10) Uani 1 1 d . . . N9A N -0.0895(3) 0.1501(4) 0.1739(4) 0.0108(11) Uani 1 1 d . . . H90 H -0.1215 0.1103 0.1712 0.013 Uiso 1 1 d R . . N10A N 0.0405(3) 0.4375(4) 0.1487(4) 0.0104(11) Uani 1 1 d . . . H10A H 0.0575 0.4289 0.1016 0.013 Uiso 1 1 calc R . . H10B H -0.0152 0.4550 0.1031 0.013 Uiso 1 1 calc R . . N11A N 0.1460(3) 0.3814(4) 0.3756(4) 0.0115(11) Uani 1 1 d . . . H11A H 0.1257 0.4030 0.4165 0.014 Uiso 1 1 calc R . . H11B H 0.1927 0.3388 0.4231 0.014 Uiso 1 1 calc R . . C10A C 0.0883(4) 0.5305(5) 0.2319(5) 0.0159(14) Uani 1 1 d . . . H10C H 0.0550 0.5653 0.2551 0.019 Uiso 1 1 calc R . . H10D H 0.1017 0.5881 0.1957 0.019 Uiso 1 1 calc R . . C11A C 0.1672(3) 0.4817(5) 0.3358(5) 0.0139(13) Uani 1 1 d . . . H11C H 0.2053 0.4604 0.3153 0.017 Uiso 1 1 calc R . . H11D H 0.1956 0.5376 0.3984 0.017 Uiso 1 1 calc R . . O5 O 0.3709(2) 0.9845(4) 0.4659(3) 0.0169(10) Uani 1 1 d . . . H5E H 0.3239 1.0158 0.4164 0.020 Uiso 1 1 d R . . H5F H 0.3620 0.9172 0.4763 0.020 Uiso 1 1 d R . . O6 O 0.3397(10) 0.762(2) 0.498(2) 0.022(4) Uani 0.50 1 d P . . O6X O 0.307(2) 0.763(4) 0.476(4) 0.056(12) Uani 0.30 1 d P . . 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 Pt1A 0.00501(12) 0.01083(12) 0.00653(12) -0.00007(11) 0.00175(9) 0.00012(10) S1A 0.0085(7) 0.0148(8) 0.0163(8) -0.0009(7) 0.0052(6) 0.0006(7) O1A 0.004(2) 0.018(2) 0.012(2) 0.0008(18) 0.0038(19) -0.0020(17) O2A 0.020(2) 0.025(3) 0.035(3) 0.004(2) 0.021(2) 0.005(2) O3A 0.009(2) 0.016(2) 0.024(3) -0.003(2) 0.005(2) 0.0000(18) O4A 0.010(2) 0.015(2) 0.014(2) -0.0044(18) 0.000(2) 0.0023(18) N1A 0.013(3) 0.021(3) 0.010(3) -0.003(2) 0.003(2) 0.002(2) C2A 0.008(3) 0.013(3) 0.010(3) 0.001(3) 0.001(3) 0.007(3) N3A 0.005(2) 0.016(3) 0.008(2) -0.003(2) 0.001(2) 0.000(2) C4A 0.006(3) 0.011(3) 0.011(3) 0.001(3) 0.001(2) 0.005(2) C5A 0.007(3) 0.013(3) 0.013(3) 0.001(3) 0.001(3) 0.000(2) C6A 0.014(3) 0.012(3) 0.018(3) -0.004(3) 0.006(3) 0.003(3) C7A 0.034(4) 0.023(4) 0.011(3) -0.005(3) 0.010(3) 0.002(3) O8A 0.014(2) 0.026(3) 0.009(2) 0.001(2) 0.0028(19) -0.001(2) N9A 0.006(2) 0.013(3) 0.008(3) -0.003(2) 0.002(2) -0.004(2) N10A 0.005(2) 0.014(3) 0.010(3) 0.003(2) 0.004(2) 0.000(2) N11A 0.008(2) 0.012(3) 0.009(3) 0.000(2) 0.002(2) 0.001(2) C10A 0.013(3) 0.019(4) 0.012(3) 0.001(3) 0.005(3) 0.002(3) C11A 0.009(3) 0.011(3) 0.016(3) 0.001(3) 0.003(3) 0.000(2) O5 0.012(2) 0.021(3) 0.013(2) 0.0001(19) 0.0041(19) 0.0032(19) O6 0.019(8) 0.022(7) 0.032(12) 0.012(7) 0.018(9) 0.008(7) O6X 0.08(3) 0.051(18) 0.021(19) 0.004(13) 0.02(3) 0.01(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1A N9A 2.002(5) 2 ? Pt1A N3A 2.035(5) . ? Pt1A N11A 2.045(5) . ? Pt1A N10A 2.056(5) . ? Pt1A O1A 2.138(4) . ? Pt1A Pt1A 2.5982(4) 2 ? S1A O2A 1.446(4) . ? S1A O4A 1.451(4) . ? S1A O3A 1.483(4) . ? S1A O1A 1.540(4) . ? N1A C6A 1.360(8) . ? N1A C2A 1.390(8) . ? N1A C7A 1.457(8) . ? C2A O8A 1.233(7) . ? C2A N3A 1.377(7) . ? N3A C4A 1.386(7) . ? C4A N9A 1.297(7) . ? C4A C5A 1.416(8) . ? C5A C6A 1.331(8) . ? C5A H5 0.9500 . ? C6A H6 0.9500 . ? C7A H7A 0.9800 . ? C7A H7B 0.9800 . ? C7A H7C 0.9800 . ? N9A Pt1A 2.002(5) 2 ? N9A H90 0.7782 . ? N10A C10A 1.497(7) . ? N10A H10A 0.9200 . ? N10A H10B 0.9200 . ? N11A C11A 1.495(7) . ? N11A H11A 0.9200 . ? N11A H11B 0.9200 . ? C10A C11A 1.510(8) . ? C10A H10C 0.9900 . ? C10A H10D 0.9900 . ? C11A H11C 0.9900 . ? C11A H11D 0.9900 . ? O5 H5E 0.8607 . ? O5 H5F 0.8597 . ? O6 O6X 0.52(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N9A Pt1A N3A 88.7(2) 2 . ? N9A Pt1A N11A 92.49(19) 2 . ? N3A Pt1A N11A 176.80(18) . . ? N9A Pt1A N10A 173.30(18) 2 . ? N3A Pt1A N10A 95.32(19) . . ? N11A Pt1A N10A 83.23(19) . . ? N9A Pt1A O1A 89.45(17) 2 . ? N3A Pt1A O1A 90.37(17) . . ? N11A Pt1A O1A 86.66(17) . . ? N10A Pt1A O1A 85.17(17) . . ? N9A Pt1A Pt1A 81.58(13) 2 2 ? N3A Pt1A Pt1A 83.99(13) . 2 ? N11A Pt1A Pt1A 99.13(13) . 2 ? N10A Pt1A Pt1A 104.14(13) . 2 ? O1A Pt1A Pt1A 169.49(11) . 2 ? O2A S1A O4A 113.6(3) . . ? O2A S1A O3A 110.7(3) . . ? O4A S1A O3A 109.3(3) . . ? O2A S1A O1A 105.7(2) . . ? O4A S1A O1A 109.6(2) . . ? O3A S1A O1A 107.8(2) . . ? S1A O1A Pt1A 125.5(2) . . ? C6A N1A C2A 121.0(5) . . ? C6A N1A C7A 121.3(5) . . ? C2A N1A C7A 117.5(5) . . ? O8A C2A N3A 122.1(6) . . ? O8A C2A N1A 120.6(5) . . ? N3A C2A N1A 117.2(6) . . ? C2A N3A C4A 120.9(5) . . ? C2A N3A Pt1A 121.3(4) . . ? C4A N3A Pt1A 117.5(4) . . ? N9A C4A N3A 116.9(5) . . ? N9A C4A C5A 125.2(6) . . ? N3A C4A C5A 117.9(5) . . ? C6A C5A C4A 118.9(6) . . ? C6A C5A H5 120.5 . . ? C4A C5A H5 120.5 . . ? C5A C6A N1A 121.9(6) . . ? C5A C6A H6 119.0 . . ? N1A C6A H6 119.0 . . ? N1A C7A H7A 109.5 . . ? N1A C7A H7B 109.5 . . ? H7A C7A H7B 109.5 . . ? N1A C7A H7C 109.5 . . ? H7A C7A H7C 109.5 . . ? H7B C7A H7C 109.5 . . ? C4A N9A Pt1A 125.5(4) . 2 ? C4A N9A H90 113.5 . . ? Pt1A N9A H90 118.9 2 . ? C10A N10A Pt1A 111.0(3) . . ? C10A N10A H10A 109.4 . . ? Pt1A N10A H10A 109.4 . . ? C10A N10A H10B 109.4 . . ? Pt1A N10A H10B 109.4 . . ? H10A N10A H10B 108.0 . . ? C11A N11A Pt1A 108.6(3) . . ? C11A N11A H11A 110.0 . . ? Pt1A N11A H11A 110.0 . . ? C11A N11A H11B 110.0 . . ? Pt1A N11A H11B 110.0 . . ? H11A N11A H11B 108.3 . . ? N10A C10A C11A 107.6(5) . . ? N10A C10A H10C 110.2 . . ? C11A C10A H10C 110.2 . . ? N10A C10A H10D 110.2 . . ? C11A C10A H10D 110.2 . . ? H10C C10A H10D 108.5 . . ? N11A C11A C10A 109.0(5) . . ? N11A C11A H11C 109.9 . . ? C10A C11A H11C 109.9 . . ? N11A C11A H11D 109.9 . . ? C10A C11A H11D 109.9 . . ? H11C C11A H11D 108.3 . . ? H5E O5 H5F 108.6 . . ? 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 O2A S1A O1A Pt1A -173.9(3) . . . . ? O4A S1A O1A Pt1A -51.1(4) . . . . ? O3A S1A O1A Pt1A 67.7(3) . . . . ? N9A Pt1A O1A S1A -34.1(3) 2 . . . ? N3A Pt1A O1A S1A -122.8(3) . . . . ? N11A Pt1A O1A S1A 58.4(3) . . . . ? N10A Pt1A O1A S1A 141.9(3) . . . . ? Pt1A Pt1A O1A S1A -65.4(7) 2 . . . ? C6A N1A C2A O8A -177.6(5) . . . . ? C7A N1A C2A O8A -2.0(8) . . . . ? C6A N1A C2A N3A 1.5(8) . . . . ? C7A N1A C2A N3A 177.0(5) . . . . ? O8A C2A N3A C4A 166.5(5) . . . . ? N1A C2A N3A C4A -12.6(8) . . . . ? O8A C2A N3A Pt1A -19.5(8) . . . . ? N1A C2A N3A Pt1A 161.5(4) . . . . ? N9A Pt1A N3A C2A -126.8(5) 2 . . . ? N10A Pt1A N3A C2A 47.8(5) . . . . ? O1A Pt1A N3A C2A -37.4(5) . . . . ? Pt1A Pt1A N3A C2A 151.5(4) 2 . . . ? N9A Pt1A N3A C4A 47.5(4) 2 . . . ? N10A Pt1A N3A C4A -137.9(4) . . . . ? O1A Pt1A N3A C4A 136.9(4) . . . . ? Pt1A Pt1A N3A C4A -34.2(4) 2 . . . ? C2A N3A C4A N9A -162.9(5) . . . . ? Pt1A N3A C4A N9A 22.8(7) . . . . ? C2A N3A C4A C5A 18.1(8) . . . . ? Pt1A N3A C4A C5A -156.2(4) . . . . ? N9A C4A C5A C6A 168.6(6) . . . . ? N3A C4A C5A C6A -12.5(8) . . . . ? C4A C5A C6A N1A 1.7(9) . . . . ? C2A N1A C6A C5A 3.9(9) . . . . ? C7A N1A C6A C5A -171.5(6) . . . . ? N3A C4A N9A Pt1A 12.4(7) . . . 2 ? C5A C4A N9A Pt1A -168.7(4) . . . 2 ? N3A Pt1A N10A C10A 174.4(4) . . . . ? N11A Pt1A N10A C10A -8.4(4) . . . . ? O1A Pt1A N10A C10A -95.6(4) . . . . ? Pt1A Pt1A N10A C10A 89.3(3) 2 . . . ? N9A Pt1A N11A C11A 156.3(4) 2 . . . ? N10A Pt1A N11A C11A -18.5(4) . . . . ? O1A Pt1A N11A C11A 67.0(3) . . . . ? Pt1A Pt1A N11A C11A -121.8(3) 2 . . . ? Pt1A N10A C10A C11A 33.2(5) . . . . ? Pt1A N11A C11A C10A 42.3(5) . . . . ? N10A C10A C11A N11A -49.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.558 _refine_diff_density_min -1.241 _refine_diff_density_rms 0.181 #===END #===END data_vedj022b _database_code_depnum_ccdc_archive 'CCDC 758050' #TrackingRef 'CIF1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Chlorido(N,N'-dimethylethane-1,2-diamine)(1-methylcytosine)platinum(II) nitrate monohydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H19 Cl N5 O Pt, 0.12(O8), N O3' _chemical_formula_sum 'C9 H21 Cl N6 O5 Pt' _chemical_formula_weight 523.86 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' Pt Pt -1.7033 8.3905 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 12.4934(4) _cell_length_b 12.7860(4) _cell_length_c 12.6634(4) _cell_angle_alpha 90.00 _cell_angle_beta 118.875(2) _cell_angle_gamma 90.00 _cell_volume 1771.37(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1354 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 29.23 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.964 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 8.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4190 _exptl_absorpt_correction_T_max 0.8548 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55502 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3470 _reflns_number_gt 3059 _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^)+(0.0346P)^2^+7.9850P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3470 _refine_ls_number_parameters 227 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.42549(2) 0.266577(16) 0.077033(18) 0.01871(9) Uani 1 1 d . . . Cl1 Cl 0.34347(15) 0.11604(11) -0.03280(13) 0.0299(3) Uani 1 1 d . . . O1 O 0.2033(4) 0.3776(3) -0.1151(3) 0.0297(10) Uani 1 1 d . . . N1 N 0.0641(5) 0.3686(4) -0.0500(5) 0.0312(12) Uani 1 1 d . . . N2 N 0.2596(4) 0.2955(4) 0.0637(4) 0.0208(10) Uani 1 1 d . . . N3 N 0.3073(4) 0.2020(4) 0.2375(4) 0.0247(11) Uani 1 1 d . . . H3A H 0.3801 0.1882 0.2459 0.030 Uiso 1 1 calc R . . H3B H 0.2870 0.1780 0.2906 0.030 Uiso 1 1 calc R . . N4 N 0.5933(5) 0.2474(4) 0.0891(5) 0.0245(11) Uani 1 1 d . . . H4 H 0.5846 0.2680 0.0150 0.029 Uiso 1 1 calc R . . N5 N 0.4987(4) 0.4025(4) 0.1708(4) 0.0202(10) Uani 1 1 d . . . H5 H 0.4435 0.4560 0.1303 0.024 Uiso 1 1 calc R . . C1 C 0.1788(5) 0.3484(5) -0.0377(5) 0.0268(13) Uani 1 1 d . . . C2 C 0.0324(6) 0.3343(6) 0.0331(6) 0.0374(16) Uani 1 1 d . . . H2 H -0.0475 0.3483 0.0208 0.045 Uiso 1 1 calc R . . C3 C 0.1108(6) 0.2815(5) 0.1314(6) 0.0335(15) Uani 1 1 d . . . H3 H 0.0887 0.2599 0.1901 0.040 Uiso 1 1 calc R . . C4 C 0.2286(6) 0.2586(5) 0.1453(5) 0.0255(13) Uani 1 1 d . . . C5 C -0.0233(6) 0.4238(7) -0.1599(6) 0.0449(19) Uani 1 1 d . . . H5A H 0.0134 0.4892 -0.1674 0.067 Uiso 1 1 calc R . . H5B H -0.0977 0.4394 -0.1553 0.067 Uiso 1 1 calc R . . H5C H -0.0438 0.3795 -0.2303 0.067 Uiso 1 1 calc R . . C6 C 0.6459(6) 0.1405(5) 0.1110(6) 0.0316(15) Uani 1 1 d . . . H6A H 0.5874 0.0926 0.0499 0.047 Uiso 1 1 calc R . . H6B H 0.6632 0.1168 0.1913 0.047 Uiso 1 1 calc R . . H6C H 0.7219 0.1413 0.1062 0.047 Uiso 1 1 calc R . . C7 C 0.6800(6) 0.3244(5) 0.1797(5) 0.0301(14) Uani 1 1 d . . . H7A H 0.7099 0.2974 0.2625 0.036 Uiso 1 1 calc R . . H7B H 0.7512 0.3358 0.1668 0.036 Uiso 1 1 calc R . . C8 C 0.6123(6) 0.4248(5) 0.1633(5) 0.0279(13) Uani 1 1 d . . . H8A H 0.6642 0.4752 0.2268 0.033 Uiso 1 1 calc R . . H8B H 0.5908 0.4557 0.0838 0.033 Uiso 1 1 calc R . . C9 C 0.5208(6) 0.4022(5) 0.2970(5) 0.0281(13) Uani 1 1 d . . . H9A H 0.4441 0.3874 0.2975 0.042 Uiso 1 1 calc R . . H9B H 0.5518 0.4707 0.3337 0.042 Uiso 1 1 calc R . . H9C H 0.5812 0.3482 0.3432 0.042 Uiso 1 1 calc R . . O2 O 0.7465(4) 0.2067(3) 0.4564(4) 0.0350(10) Uani 1 1 d . . . O3 O 0.7317(4) 0.0443(3) 0.4005(4) 0.0339(10) Uani 1 1 d . . . O4 O 0.5726(4) 0.1258(3) 0.3864(4) 0.0276(9) Uani 1 1 d . . . N6 N 0.6849(5) 0.1255(4) 0.4149(4) 0.0226(10) Uani 1 1 d . . . O6 O -0.0995(12) 0.0441(11) -0.0255(12) 0.014(3) Uani 0.25 1 d PU . . O7 O -0.0090(15) -0.0363(12) 0.0404(14) 0.026(4) Uani 0.25 1 d PU . . O8 O -0.0260(19) -0.0940(16) 0.1176(18) 0.044(5) Uani 0.25 1 d PU . . O5 O 0.0319(14) -0.1535(12) 0.1819(13) 0.020(3) Uani 0.25 1 d PU . . 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 0.02386(13) 0.01911(13) 0.01736(12) 0.00028(8) 0.01330(10) 0.00180(9) Cl1 0.0447(9) 0.0227(7) 0.0285(7) -0.0051(6) 0.0225(7) -0.0038(6) O1 0.032(3) 0.040(3) 0.021(2) 0.0034(18) 0.016(2) 0.0078(19) N1 0.024(3) 0.043(3) 0.027(3) 0.000(2) 0.013(2) 0.007(2) N2 0.024(3) 0.022(2) 0.016(2) -0.0031(19) 0.009(2) -0.002(2) N3 0.026(3) 0.030(3) 0.022(2) 0.003(2) 0.015(2) 0.000(2) N4 0.025(3) 0.029(3) 0.024(3) 0.005(2) 0.015(2) 0.007(2) N5 0.021(3) 0.020(2) 0.020(2) 0.0022(18) 0.010(2) 0.0045(19) C1 0.025(3) 0.034(3) 0.019(3) -0.005(2) 0.010(3) -0.002(3) C2 0.020(3) 0.061(5) 0.035(4) -0.002(3) 0.016(3) -0.001(3) C3 0.025(3) 0.052(4) 0.028(3) 0.001(3) 0.016(3) -0.001(3) C4 0.028(3) 0.028(3) 0.025(3) -0.006(2) 0.016(3) -0.006(2) C5 0.027(4) 0.072(5) 0.029(4) 0.011(3) 0.008(3) 0.015(3) C6 0.040(4) 0.033(4) 0.028(3) 0.009(3) 0.021(3) 0.017(3) C7 0.024(3) 0.045(4) 0.024(3) -0.004(3) 0.014(3) -0.004(3) C8 0.032(4) 0.029(3) 0.025(3) -0.001(2) 0.016(3) -0.006(3) C9 0.035(4) 0.032(3) 0.020(3) -0.003(2) 0.016(3) 0.000(3) O2 0.031(3) 0.029(2) 0.049(3) -0.006(2) 0.023(2) -0.005(2) O3 0.036(3) 0.025(2) 0.047(3) 0.0059(19) 0.025(2) 0.0093(19) O4 0.022(2) 0.036(2) 0.027(2) -0.0040(18) 0.0129(18) -0.0022(18) N6 0.030(3) 0.023(3) 0.021(2) 0.0035(19) 0.017(2) 0.001(2) O6 0.014(3) 0.014(3) 0.015(3) 0.0002(10) 0.0066(16) 0.0003(10) O7 0.026(4) 0.026(4) 0.026(4) -0.0006(10) 0.0124(19) -0.0002(10) O8 0.045(5) 0.044(5) 0.044(5) -0.0004(10) 0.021(2) -0.0003(10) O5 0.020(3) 0.020(3) 0.020(3) -0.0007(10) 0.0093(18) 0.0009(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N2 2.030(5) . ? Pt1 N4 2.042(5) . ? Pt1 N5 2.054(5) . ? Pt1 Cl1 2.3050(14) . ? O1 C1 1.219(7) . ? N1 C2 1.363(8) . ? N1 C1 1.389(8) . ? N1 C5 1.470(8) . ? N2 C4 1.352(7) . ? N2 C1 1.368(7) . ? N3 C4 1.321(8) . ? N3 H3A 0.8800 . ? N3 H3B 0.8800 . ? N4 C6 1.484(7) . ? N4 C7 1.502(8) . ? N4 H4 0.9300 . ? N5 C9 1.485(7) . ? N5 C8 1.495(7) . ? N5 H5 0.9300 . ? C2 C3 1.337(9) . ? C2 H2 0.9500 . ? C3 C4 1.427(9) . ? C3 H3 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.496(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? O2 N6 1.246(6) . ? O3 N6 1.247(6) . ? O4 N6 1.269(6) . ? O6 O7 1.46(2) . ? O6 O7 1.46(2) 3 ? O7 O8 1.32(2) . ? O7 O6 1.46(2) 3 ? O7 O7 1.48(3) 3 ? O8 O5 1.09(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 N2 Pt1 N4 176.37(19) . . ? N2 Pt1 N5 92.62(18) . . ? N4 Pt1 N5 84.48(19) . . ? N2 Pt1 Cl1 87.90(13) . . ? N4 Pt1 Cl1 94.94(14) . . ? N5 Pt1 Cl1 178.40(13) . . ? C2 N1 C1 121.5(5) . . ? C2 N1 C5 121.7(5) . . ? C1 N1 C5 116.7(5) . . ? C4 N2 C1 122.4(5) . . ? C4 N2 Pt1 122.0(4) . . ? C1 N2 Pt1 115.4(4) . . ? C4 N3 H3A 120.0 . . ? C4 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C6 N4 C7 111.7(5) . . ? C6 N4 Pt1 118.1(4) . . ? C7 N4 Pt1 108.3(3) . . ? C6 N4 H4 106.0 . . ? C7 N4 H4 106.0 . . ? Pt1 N4 H4 106.0 . . ? C9 N5 C8 112.3(5) . . ? C9 N5 Pt1 114.8(4) . . ? C8 N5 Pt1 107.2(3) . . ? C9 N5 H5 107.4 . . ? C8 N5 H5 107.4 . . ? Pt1 N5 H5 107.4 . . ? O1 C1 N2 123.2(5) . . ? O1 C1 N1 119.9(5) . . ? N2 C1 N1 116.8(5) . . ? C3 C2 N1 121.7(6) . . ? C3 C2 H2 119.1 . . ? N1 C2 H2 119.1 . . ? C2 C3 C4 117.8(6) . . ? C2 C3 H3 121.1 . . ? C4 C3 H3 121.1 . . ? N3 C4 N2 120.1(5) . . ? N3 C4 C3 120.3(5) . . ? N2 C4 C3 119.6(6) . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 H6A 109.5 . . ? N4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 N4 107.8(5) . . ? C8 C7 H7A 110.2 . . ? N4 C7 H7A 110.2 . . ? C8 C7 H7B 110.2 . . ? N4 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? N5 C8 C7 108.6(5) . . ? N5 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? N5 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? N5 C9 H9A 109.5 . . ? N5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 N6 O3 121.2(5) . . ? O2 N6 O4 119.3(5) . . ? O3 N6 O4 119.5(5) . . ? O7 O6 O7 60.9(12) . 3 ? O8 O7 O6 117.4(16) . . ? O8 O7 O6 123.3(16) . 3 ? O6 O7 O6 119.1(12) . 3 ? O8 O7 O7 175(2) . 3 ? O6 O7 O7 59.6(12) . 3 ? O6 O7 O7 59.5(12) 3 3 ? O5 O8 O7 131(2) . . ? 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 N5 Pt1 N2 C4 -92.8(4) . . . . ? Cl1 Pt1 N2 C4 88.7(4) . . . . ? N5 Pt1 N2 C1 91.6(4) . . . . ? Cl1 Pt1 N2 C1 -86.8(4) . . . . ? N5 Pt1 N4 C6 141.1(4) . . . . ? Cl1 Pt1 N4 C6 -40.4(4) . . . . ? N5 Pt1 N4 C7 12.9(4) . . . . ? N2 Pt1 N5 C9 72.2(4) . . . . ? N4 Pt1 N5 C9 -110.0(4) . . . . ? N2 Pt1 N5 C8 -162.2(4) . . . . ? N4 Pt1 N5 C8 15.6(4) . . . . ? C4 N2 C1 O1 -176.2(6) . . . . ? Pt1 N2 C1 O1 -0.7(8) . . . . ? C4 N2 C1 N1 4.0(8) . . . . ? Pt1 N2 C1 N1 179.5(4) . . . . ? C2 N1 C1 O1 178.0(6) . . . . ? C5 N1 C1 O1 1.2(9) . . . . ? C2 N1 C1 N2 -2.2(9) . . . . ? C5 N1 C1 N2 -179.0(6) . . . . ? C1 N1 C2 C3 1.4(10) . . . . ? C5 N1 C2 C3 178.0(7) . . . . ? N1 C2 C3 C4 -2.1(10) . . . . ? C1 N2 C4 N3 175.5(5) . . . . ? Pt1 N2 C4 N3 0.2(7) . . . . ? C1 N2 C4 C3 -4.8(8) . . . . ? Pt1 N2 C4 C3 179.9(4) . . . . ? C2 C3 C4 N3 -176.5(6) . . . . ? C2 C3 C4 N2 3.8(9) . . . . ? C6 N4 C7 C8 -170.9(5) . . . . ? Pt1 N4 C7 C8 -39.1(5) . . . . ? C9 N5 C8 C7 85.3(6) . . . . ? Pt1 N5 C8 C7 -41.7(5) . . . . ? N4 C7 C8 N5 54.0(6) . . . . ? O7 O6 O7 O8 175(2) 3 . . . ? O7 O6 O7 O6 0.000(2) 3 . . 3 ? O6 O7 O8 O5 -174(2) . . . . ? O6 O7 O8 O5 1(4) 3 . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.407 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.145 #===END