# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jose Ruiz' _publ_contact_author_email JRUIZ@UM.ES _publ_section_title ; New Palladium(II) and Platinum(II) Complexes with the Model Nucleobase 9-Methylhypoxanthine: Crystal Structures and Theoretical Calculations ; loop_ _publ_author_name 'Jose Ruiz' 'Delia Bautista' 'Natalia Cutillas' 'Arturo Espinosa' 'Gregorio Lopez' 'Maria Dolores Villa' #===END data_md511s _database_code_depnum_ccdc_archive 'CCDC 742533' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H32 N5 O P Pt' _chemical_formula_weight 740.70 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4884(4) _cell_length_b 10.0705(5) _cell_length_c 17.4286(8) _cell_angle_alpha 103.460(2) _cell_angle_beta 94.548(2) _cell_angle_gamma 90.602(2) _cell_volume 1443.71(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8994 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 28.05 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 4.951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4845 _exptl_absorpt_correction_T_max 0.7899 _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 'Bruker SMART APEX' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16441 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.09 _reflns_number_total 6233 _reflns_number_gt 5965 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0305P)^2^+1.1565P] 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 'rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6233 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0628 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 0.699633(15) 0.490423(12) 0.295311(8) 0.01143(5) Uani 1 1 d . . . P1 P 0.55094(11) 0.36716(9) 0.19275(6) 0.01249(18) Uani 1 1 d . . . N1 N 0.6680(3) 0.3492(3) 0.36550(17) 0.0135(6) Uani 1 1 d . . . C2 C 0.5528(4) 0.3657(4) 0.4156(2) 0.0180(8) Uani 1 1 d . . . H2 H 0.4757 0.4304 0.4084 0.022 Uiso 1 1 calc R . . N3 N 0.5325(4) 0.3041(3) 0.4735(2) 0.0205(7) Uani 1 1 d . . . C4 C 0.6490(4) 0.2138(4) 0.4779(2) 0.0171(8) Uani 1 1 d . . . C5 C 0.7699(4) 0.1819(3) 0.4296(2) 0.0151(7) Uani 1 1 d . . . C6 C 0.7845(4) 0.2522(3) 0.3677(2) 0.0150(7) Uani 1 1 d . . . N7 N 0.8666(4) 0.0863(3) 0.4537(2) 0.0192(7) Uani 1 1 d . . . C8 C 0.8011(5) 0.0631(4) 0.5152(2) 0.0207(8) Uani 1 1 d . . . H8 H 0.8419 0.0010 0.5447 0.025 Uiso 1 1 calc R . . N9 N 0.6689(4) 0.1363(3) 0.53302(19) 0.0191(7) Uani 1 1 d . . . C10 C 0.5711(5) 0.1352(5) 0.5978(3) 0.0334(11) Uani 1 1 d . . . H10A H 0.4740 0.0806 0.5772 0.050 Uiso 1 1 calc R . . H10B H 0.5438 0.2289 0.6224 0.050 Uiso 1 1 calc R . . H10C H 0.6294 0.0952 0.6373 0.050 Uiso 1 1 calc R . . O1 O 0.8880(3) 0.2371(3) 0.32035(17) 0.0227(6) Uani 1 1 d . . . N10 N 0.8606(4) 0.6097(3) 0.38656(18) 0.0149(6) Uani 1 1 d . . . C11 C 0.7443(4) 0.6434(3) 0.2425(2) 0.0134(7) Uani 1 1 d . . . C12 C 0.7197(4) 0.6511(4) 0.1634(2) 0.0156(7) Uani 1 1 d . . . H12 H 0.6700 0.5755 0.1259 0.019 Uiso 1 1 calc R . . C13 C 0.7653(4) 0.7657(4) 0.1374(2) 0.0171(8) Uani 1 1 d . . . H13 H 0.7452 0.7671 0.0832 0.021 Uiso 1 1 calc R . . C14 C 0.8396(4) 0.8772(4) 0.1901(2) 0.0186(8) Uani 1 1 d . . . H14 H 0.8716 0.9548 0.1723 0.022 Uiso 1 1 calc R . . C15 C 0.8669(4) 0.8743(4) 0.2691(2) 0.0176(8) Uani 1 1 d . . . H15 H 0.9172 0.9505 0.3059 0.021 Uiso 1 1 calc R . . C16 C 0.8203(4) 0.7593(4) 0.2949(2) 0.0163(7) Uani 1 1 d . . . C17 C 0.8445(5) 0.7549(3) 0.3802(2) 0.0182(8) Uani 1 1 d . . . H17A H 0.7534 0.7955 0.4084 0.022 Uiso 1 1 calc R . . H17B H 0.9411 0.8089 0.4051 0.022 Uiso 1 1 calc R . . C18 C 1.0220(4) 0.5643(4) 0.3683(2) 0.0193(8) Uani 1 1 d . . . H18A H 1.0998 0.6183 0.4083 0.029 Uiso 1 1 calc R . . H18B H 1.0426 0.5772 0.3159 0.029 Uiso 1 1 calc R . . H18C H 1.0303 0.4674 0.3686 0.029 Uiso 1 1 calc R . . C19 C 0.8380(5) 0.6039(4) 0.4691(2) 0.0208(8) Uani 1 1 d . . . H19A H 0.8588 0.5116 0.4759 0.031 Uiso 1 1 calc R . . H19B H 0.7290 0.6267 0.4805 0.031 Uiso 1 1 calc R . . H19C H 0.9113 0.6695 0.5056 0.031 Uiso 1 1 calc R . . C21 C 0.6692(4) 0.2814(3) 0.1137(2) 0.0148(7) Uani 1 1 d . . . C22 C 0.8320(4) 0.3009(4) 0.1227(2) 0.0182(8) Uani 1 1 d . . . H22 H 0.8801 0.3638 0.1680 0.022 Uiso 1 1 calc R . . C23 C 0.9262(5) 0.2287(4) 0.0658(2) 0.0232(9) Uani 1 1 d . . . H23 H 1.0379 0.2419 0.0726 0.028 Uiso 1 1 calc R . . C24 C 0.8563(5) 0.1382(4) -0.0006(2) 0.0238(9) Uani 1 1 d . . . H24 H 0.9198 0.0904 -0.0399 0.029 Uiso 1 1 calc R . . C25 C 0.6936(5) 0.1170(4) -0.0098(2) 0.0254(9) Uani 1 1 d . . . H25 H 0.6460 0.0543 -0.0554 0.031 Uiso 1 1 calc R . . C26 C 0.5998(5) 0.1870(4) 0.0473(2) 0.0186(8) Uani 1 1 d . . . H26 H 0.4886 0.1708 0.0412 0.022 Uiso 1 1 calc R . . C31 C 0.3978(4) 0.4630(3) 0.1517(2) 0.0135(7) Uani 1 1 d . . . C32 C 0.3593(4) 0.4496(4) 0.0708(2) 0.0185(8) Uani 1 1 d . . . H32 H 0.4188 0.3922 0.0331 0.022 Uiso 1 1 calc R . . C33 C 0.2326(5) 0.5211(4) 0.0456(2) 0.0213(8) Uani 1 1 d . . . H33 H 0.2066 0.5127 -0.0094 0.026 Uiso 1 1 calc R . . C34 C 0.1454(5) 0.6036(4) 0.1002(2) 0.0221(8) Uani 1 1 d . . . H34 H 0.0575 0.6496 0.0826 0.026 Uiso 1 1 calc R . . C35 C 0.1851(5) 0.6199(4) 0.1803(2) 0.0192(8) Uani 1 1 d . . . H35 H 0.1257 0.6780 0.2177 0.023 Uiso 1 1 calc R . . C36 C 0.3119(4) 0.5510(4) 0.2059(2) 0.0183(8) Uani 1 1 d . . . H36 H 0.3406 0.5640 0.2610 0.022 Uiso 1 1 calc R . . C41 C 0.4386(4) 0.2237(3) 0.2112(2) 0.0136(7) Uani 1 1 d . . . C42 C 0.5191(4) 0.1037(4) 0.2153(2) 0.0155(7) Uani 1 1 d . . . H42 H 0.6296 0.0999 0.2101 0.019 Uiso 1 1 calc R . . C43 C 0.4375(5) -0.0088(4) 0.2268(2) 0.0177(8) Uani 1 1 d . . . H43 H 0.4916 -0.0905 0.2279 0.021 Uiso 1 1 calc R . . C44 C 0.2777(5) -0.0028(4) 0.2366(2) 0.0198(8) Uani 1 1 d . . . H44 H 0.2223 -0.0805 0.2442 0.024 Uiso 1 1 calc R . . C45 C 0.1977(5) 0.1162(4) 0.2354(3) 0.0236(9) Uani 1 1 d . . . H45 H 0.0883 0.1208 0.2435 0.028 Uiso 1 1 calc R . . C46 C 0.2783(5) 0.2287(4) 0.2224(2) 0.0201(8) Uani 1 1 d . . . H46 H 0.2233 0.3099 0.2211 0.024 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01068(8) 0.01139(7) 0.01227(8) 0.00332(5) -0.00043(5) 0.00057(5) P1 0.0114(4) 0.0118(4) 0.0146(5) 0.0040(4) 0.0003(3) 0.0007(3) N1 0.0128(15) 0.0151(14) 0.0118(15) 0.0019(12) -0.0001(12) 0.0017(12) C2 0.0154(19) 0.0183(17) 0.021(2) 0.0053(15) 0.0013(15) 0.0041(14) N3 0.0172(17) 0.0255(17) 0.0222(18) 0.0107(14) 0.0058(14) 0.0030(13) C4 0.0175(19) 0.0187(18) 0.0149(19) 0.0047(15) -0.0017(15) -0.0025(14) C5 0.0137(18) 0.0119(16) 0.0184(19) 0.0029(14) -0.0033(14) -0.0006(13) C6 0.0162(19) 0.0128(16) 0.0146(18) 0.0011(14) -0.0016(14) 0.0008(14) N7 0.0184(17) 0.0152(15) 0.0233(18) 0.0052(13) -0.0051(13) 0.0019(12) C8 0.022(2) 0.0171(18) 0.023(2) 0.0071(16) -0.0066(16) 0.0005(15) N9 0.0210(17) 0.0207(16) 0.0172(17) 0.0093(13) -0.0027(13) -0.0023(13) C10 0.031(3) 0.049(3) 0.029(2) 0.026(2) 0.005(2) 0.004(2) O1 0.0218(15) 0.0226(14) 0.0259(15) 0.0068(12) 0.0102(12) 0.0074(11) N10 0.0148(16) 0.0176(15) 0.0131(15) 0.0054(12) 0.0010(12) 0.0015(12) C11 0.0069(16) 0.0167(17) 0.0187(19) 0.0083(15) 0.0011(14) 0.0021(13) C12 0.0128(18) 0.0152(17) 0.0173(19) 0.0010(15) 0.0005(14) -0.0003(14) C13 0.0159(19) 0.0198(18) 0.0174(19) 0.0079(15) 0.0013(15) 0.0019(14) C14 0.0161(19) 0.0145(17) 0.027(2) 0.0073(16) 0.0052(16) 0.0015(14) C15 0.0146(18) 0.0121(16) 0.026(2) 0.0037(15) 0.0008(15) 0.0025(14) C16 0.0123(18) 0.0139(16) 0.022(2) 0.0041(15) 0.0005(15) 0.0015(13) C17 0.020(2) 0.0119(16) 0.020(2) 0.0003(15) -0.0041(15) -0.0014(14) C18 0.0133(19) 0.0246(19) 0.021(2) 0.0081(16) -0.0001(15) 0.0003(15) C19 0.018(2) 0.0221(19) 0.020(2) 0.0029(16) -0.0009(16) -0.0011(15) C21 0.0174(19) 0.0126(16) 0.0161(18) 0.0054(14) 0.0043(15) 0.0044(14) C22 0.0178(19) 0.0161(17) 0.020(2) 0.0043(15) -0.0001(15) 0.0023(14) C23 0.021(2) 0.027(2) 0.025(2) 0.0103(17) 0.0066(17) 0.0077(16) C24 0.033(2) 0.0183(18) 0.022(2) 0.0060(16) 0.0127(18) 0.0102(17) C25 0.037(3) 0.0193(19) 0.021(2) 0.0053(17) 0.0045(18) 0.0022(17) C26 0.020(2) 0.0145(17) 0.022(2) 0.0060(15) 0.0001(16) -0.0023(14) C31 0.0094(17) 0.0113(15) 0.0206(19) 0.0066(14) -0.0013(14) -0.0005(13) C32 0.0171(19) 0.0194(18) 0.020(2) 0.0066(16) 0.0025(16) 0.0017(15) C33 0.021(2) 0.030(2) 0.016(2) 0.0131(17) 0.0004(16) 0.0047(16) C34 0.0135(19) 0.026(2) 0.031(2) 0.0168(18) 0.0029(16) 0.0047(15) C35 0.019(2) 0.0152(17) 0.027(2) 0.0089(16) 0.0089(16) 0.0033(14) C36 0.021(2) 0.0177(17) 0.0174(19) 0.0070(15) 0.0027(16) 0.0010(15) C41 0.0146(18) 0.0138(16) 0.0115(17) 0.0017(14) -0.0007(14) -0.0033(13) C42 0.0121(18) 0.0166(17) 0.0180(19) 0.0051(15) 0.0002(14) 0.0006(14) C43 0.020(2) 0.0156(17) 0.0194(19) 0.0067(15) 0.0013(15) 0.0025(14) C44 0.019(2) 0.0181(18) 0.024(2) 0.0076(16) 0.0033(16) -0.0031(15) C45 0.016(2) 0.0212(19) 0.034(2) 0.0078(18) 0.0016(17) -0.0007(15) C46 0.0167(19) 0.0173(18) 0.025(2) 0.0028(16) 0.0000(16) 0.0023(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C11 2.017(3) . ? Pt1 N1 2.108(3) . ? Pt1 N10 2.138(3) . ? Pt1 P1 2.2148(9) . ? P1 C31 1.826(4) . ? P1 C41 1.826(4) . ? P1 C21 1.826(4) . ? N1 C2 1.349(5) . ? N1 C6 1.402(4) . ? C2 N3 1.321(5) . ? N3 C4 1.360(5) . ? C4 C5 1.372(5) . ? C4 N9 1.374(5) . ? C5 N7 1.388(4) . ? C5 C6 1.434(5) . ? C6 O1 1.239(4) . ? N7 C8 1.313(5) . ? C8 N9 1.366(5) . ? N9 C10 1.455(5) . ? N10 C19 1.481(5) . ? N10 C18 1.485(5) . ? N10 C17 1.499(4) . ? C11 C12 1.398(5) . ? C11 C16 1.416(5) . ? C12 C13 1.396(5) . ? C13 C14 1.384(5) . ? C14 C15 1.385(5) . ? C15 C16 1.401(5) . ? C16 C17 1.495(5) . ? C21 C22 1.385(5) . ? C21 C26 1.399(5) . ? C22 C23 1.399(5) . ? C23 C24 1.382(6) . ? C24 C25 1.386(6) . ? C25 C26 1.390(6) . ? C31 C36 1.394(5) . ? C31 C32 1.396(5) . ? C32 C33 1.399(5) . ? C33 C34 1.379(6) . ? C34 C35 1.380(6) . ? C35 C36 1.386(5) . ? C41 C46 1.389(5) . ? C41 C42 1.408(5) . ? C42 C43 1.384(5) . ? C43 C44 1.381(5) . ? C44 C45 1.387(5) . ? C45 C46 1.390(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Pt1 N1 171.76(13) . . ? C11 Pt1 N10 81.76(13) . . ? N1 Pt1 N10 90.25(11) . . ? C11 Pt1 P1 94.94(11) . . ? N1 Pt1 P1 93.18(8) . . ? N10 Pt1 P1 174.42(8) . . ? C31 P1 C41 102.64(16) . . ? C31 P1 C21 109.15(17) . . ? C41 P1 C21 101.67(16) . . ? C31 P1 Pt1 114.18(12) . . ? C41 P1 Pt1 116.08(12) . . ? C21 P1 Pt1 112.02(13) . . ? C2 N1 C6 121.1(3) . . ? C2 N1 Pt1 120.4(2) . . ? C6 N1 Pt1 117.8(2) . . ? N3 C2 N1 128.8(3) . . ? C2 N3 C4 110.3(3) . . ? N3 C4 C5 127.8(3) . . ? N3 C4 N9 126.1(3) . . ? C5 C4 N9 106.1(3) . . ? C4 C5 N7 110.8(3) . . ? C4 C5 C6 119.0(3) . . ? N7 C5 C6 130.1(3) . . ? O1 C6 N1 120.1(3) . . ? O1 C6 C5 126.9(3) . . ? N1 C6 C5 113.0(3) . . ? C8 N7 C5 103.5(3) . . ? N7 C8 N9 114.0(3) . . ? C8 N9 C4 105.6(3) . . ? C8 N9 C10 127.4(3) . . ? C4 N9 C10 127.0(3) . . ? C19 N10 C18 108.7(3) . . ? C19 N10 C17 108.2(3) . . ? C18 N10 C17 109.3(3) . . ? C19 N10 Pt1 117.2(2) . . ? C18 N10 Pt1 107.0(2) . . ? C17 N10 Pt1 106.2(2) . . ? C12 C11 C16 115.7(3) . . ? C12 C11 Pt1 131.0(3) . . ? C16 C11 Pt1 113.3(3) . . ? C13 C12 C11 122.5(3) . . ? C14 C13 C12 120.4(4) . . ? C13 C14 C15 119.3(3) . . ? C14 C15 C16 120.1(3) . . ? C15 C16 C11 122.1(4) . . ? C15 C16 C17 121.2(3) . . ? C11 C16 C17 116.7(3) . . ? C16 C17 N10 109.5(3) . . ? C22 C21 C26 119.2(3) . . ? C22 C21 P1 119.5(3) . . ? C26 C21 P1 121.1(3) . . ? C21 C22 C23 120.6(4) . . ? C24 C23 C22 119.7(4) . . ? C23 C24 C25 120.1(4) . . ? C24 C25 C26 120.2(4) . . ? C25 C26 C21 120.1(4) . . ? C36 C31 C32 119.1(3) . . ? C36 C31 P1 116.6(3) . . ? C32 C31 P1 124.3(3) . . ? C31 C32 C33 119.6(4) . . ? C34 C33 C32 120.3(4) . . ? C33 C34 C35 120.4(4) . . ? C34 C35 C36 119.7(4) . . ? C35 C36 C31 120.8(4) . . ? C46 C41 C42 118.8(3) . . ? C46 C41 P1 122.9(3) . . ? C42 C41 P1 118.3(3) . . ? C43 C42 C41 120.1(3) . . ? C44 C43 C42 120.3(3) . . ? C43 C44 C45 120.3(3) . . ? C44 C45 C46 119.7(4) . . ? C41 C46 C45 120.7(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C19 H19B N3 0.98 2.47 3.447(5) 172.8 2_666 C45 H45 O1 0.95 2.39 3.230(5) 146.6 1_455 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.09 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.625 _refine_diff_density_min -1.565 _refine_diff_density_rms 0.129 #===END # Attachment 'new_md485b_md511s.cif' data_md485bs _database_code_depnum_ccdc_archive 'CCDC 742534' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H33 Cl N5 O5 P Pt' _chemical_formula_weight 841.15 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8061(4) _cell_length_b 9.5922(5) _cell_length_c 19.6841(11) _cell_angle_alpha 94.609(2) _cell_angle_beta 100.862(2) _cell_angle_gamma 102.408(2) _cell_volume 1582.07(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7735 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 28.12 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 4.620 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3285 _exptl_absorpt_correction_T_max 0.5072 _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 'Bruker SMART APEX' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17320 _diffrn_reflns_av_R_equivalents 0.0140 _diffrn_reflns_av_sigmaI/netI 0.0163 _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 -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6396 _reflns_number_gt 6301 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0200P)^2^+1.3715P] 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 'NH free,methyls rigid,others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6396 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0162 _refine_ls_R_factor_gt 0.0158 _refine_ls_wR_factor_ref 0.0394 _refine_ls_wR_factor_gt 0.0392 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.004 _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 0.165833(8) 0.267734(7) 0.728189(4) 0.01155(3) Uani 1 1 d . . . P1 P 0.10171(6) 0.37279(5) 0.82070(3) 0.01236(10) Uani 1 1 d . . . O1 O 0.39958(18) 0.56454(17) 0.66524(9) 0.0225(3) Uani 1 1 d . . . N1 N 0.2801(2) 0.68776(19) 0.58470(10) 0.0166(4) Uani 1 1 d . . . H01 H 0.368(4) 0.730(3) 0.5829(16) 0.031(8) Uiso 1 1 d . . . C2 C 0.1507(3) 0.7205(2) 0.54564(11) 0.0179(4) Uani 1 1 d . . . H2 H 0.1692 0.7930 0.5160 0.022 Uiso 1 1 calc R . . N3 N 0.0036(2) 0.66008(19) 0.54568(9) 0.0164(4) Uani 1 1 d . . . C4 C -0.0067(2) 0.5559(2) 0.58854(11) 0.0138(4) Uani 1 1 d . . . C5 C 0.1158(2) 0.5106(2) 0.62853(11) 0.0137(4) Uani 1 1 d . . . C6 C 0.2768(3) 0.5832(2) 0.63059(11) 0.0150(4) Uani 1 1 d . . . N7 N 0.0528(2) 0.39465(18) 0.66075(9) 0.0140(3) Uani 1 1 d . . . C8 C -0.1032(3) 0.3741(2) 0.64058(11) 0.0160(4) Uani 1 1 d . . . H8 H -0.1775 0.3007 0.6547 0.019 Uiso 1 1 calc R . . N9 N -0.1455(2) 0.46923(19) 0.59751(9) 0.0150(4) Uani 1 1 d . . . C10 C -0.3072(3) 0.4846(3) 0.56945(12) 0.0211(5) Uani 1 1 d . . . H10A H -0.3763 0.3898 0.5502 0.032 Uiso 1 1 calc R . . H10B H -0.3044 0.5473 0.5325 0.032 Uiso 1 1 calc R . . H10C H -0.3489 0.5271 0.6069 0.032 Uiso 1 1 calc R . . N10 N 0.2411(2) 0.16155(18) 0.64522(9) 0.0126(3) Uani 1 1 d . . . C11 C 0.2633(2) 0.1269(2) 0.78188(11) 0.0138(4) Uani 1 1 d . . . C12 C 0.3080(3) 0.1247(2) 0.85381(11) 0.0168(4) Uani 1 1 d . . . H12 H 0.2940 0.1997 0.8848 0.020 Uiso 1 1 calc R . . C13 C 0.3726(3) 0.0156(2) 0.88129(12) 0.0182(4) Uani 1 1 d . . . H13 H 0.3990 0.0158 0.9304 0.022 Uiso 1 1 calc R . . C14 C 0.3985(3) -0.0930(2) 0.83738(12) 0.0177(4) Uani 1 1 d . . . H14 H 0.4429 -0.1672 0.8561 0.021 Uiso 1 1 calc R . . C15 C 0.3588(3) -0.0924(2) 0.76584(12) 0.0173(4) Uani 1 1 d . . . H15 H 0.3790 -0.1649 0.7353 0.021 Uiso 1 1 calc R . . C16 C 0.2897(2) 0.0142(2) 0.73859(11) 0.0143(4) Uani 1 1 d . . . C17 C 0.2345(3) 0.0111(2) 0.66154(11) 0.0152(4) Uani 1 1 d . . . H17A H 0.3036 -0.0325 0.6364 0.018 Uiso 1 1 calc R . . H17B H 0.1242 -0.0478 0.6463 0.018 Uiso 1 1 calc R . . C18 C 0.4104(3) 0.2311(2) 0.64591(12) 0.0192(4) Uani 1 1 d . . . H18A H 0.4438 0.1848 0.6069 0.029 Uiso 1 1 calc R . . H18B H 0.4780 0.2207 0.6899 0.029 Uiso 1 1 calc R . . H18C H 0.4206 0.3335 0.6414 0.029 Uiso 1 1 calc R . . C19 C 0.1452(3) 0.1558(2) 0.57419(11) 0.0206(5) Uani 1 1 d . . . H19A H 0.1825 0.0965 0.5410 0.031 Uiso 1 1 calc R . . H19B H 0.1565 0.2534 0.5611 0.031 Uiso 1 1 calc R . . H19C H 0.0330 0.1137 0.5735 0.031 Uiso 1 1 calc R . . C21 C -0.0309(2) 0.4922(2) 0.79931(11) 0.0143(4) Uani 1 1 d . . . C22 C -0.1957(3) 0.4459(2) 0.79029(11) 0.0174(4) Uani 1 1 d . . . H22 H -0.2414 0.3541 0.8018 0.021 Uiso 1 1 calc R . . C23 C -0.2928(3) 0.5348(3) 0.76435(12) 0.0194(4) Uani 1 1 d . . . H23 H -0.4050 0.5025 0.7576 0.023 Uiso 1 1 calc R . . C24 C -0.2280(3) 0.6694(2) 0.74826(12) 0.0203(5) Uani 1 1 d . . . H24 H -0.2956 0.7289 0.7304 0.024 Uiso 1 1 calc R . . C25 C -0.0638(3) 0.7176(2) 0.75820(12) 0.0218(5) Uani 1 1 d . . . H25 H -0.0188 0.8107 0.7480 0.026 Uiso 1 1 calc R . . C26 C 0.0345(3) 0.6289(2) 0.78317(12) 0.0181(4) Uani 1 1 d . . . H26 H 0.1466 0.6613 0.7893 0.022 Uiso 1 1 calc R . . C31 C -0.0020(3) 0.2450(2) 0.86982(12) 0.0169(4) Uani 1 1 d . . . C32 C -0.1046(3) 0.1197(2) 0.83186(13) 0.0218(5) Uani 1 1 d . . . H32 H -0.1153 0.1031 0.7828 0.026 Uiso 1 1 calc R . . C33 C -0.1910(3) 0.0194(3) 0.86573(15) 0.0288(6) Uani 1 1 d . . . H33 H -0.2625 -0.0646 0.8396 0.035 Uiso 1 1 calc R . . C34 C -0.1732(3) 0.0416(3) 0.93741(15) 0.0298(6) Uani 1 1 d . . . H34 H -0.2322 -0.0274 0.9604 0.036 Uiso 1 1 calc R . . C35 C -0.0698(3) 0.1640(3) 0.97577(13) 0.0261(5) Uani 1 1 d . . . H35 H -0.0563 0.1779 1.0251 0.031 Uiso 1 1 calc R . . C36 C 0.0144(3) 0.2667(2) 0.94213(12) 0.0198(4) Uani 1 1 d . . . H36 H 0.0833 0.3518 0.9684 0.024 Uiso 1 1 calc R . . C41 C 0.2716(2) 0.4911(2) 0.88101(11) 0.0142(4) Uani 1 1 d . . . C42 C 0.4246(3) 0.4907(2) 0.87212(11) 0.0162(4) Uani 1 1 d . . . H42 H 0.4393 0.4263 0.8360 0.019 Uiso 1 1 calc R . . C43 C 0.5562(3) 0.5840(2) 0.91579(11) 0.0183(4) Uani 1 1 d . . . H43 H 0.6603 0.5840 0.9091 0.022 Uiso 1 1 calc R . . C44 C 0.5351(3) 0.6765(2) 0.96884(11) 0.0179(4) Uani 1 1 d . . . H44 H 0.6251 0.7391 0.9990 0.021 Uiso 1 1 calc R . . C45 C 0.3833(3) 0.6788(2) 0.97843(11) 0.0182(4) Uani 1 1 d . . . H45 H 0.3695 0.7425 1.0151 0.022 Uiso 1 1 calc R . . C46 C 0.2520(3) 0.5875(2) 0.93424(11) 0.0168(4) Uani 1 1 d . . . H46 H 0.1480 0.5903 0.9401 0.020 Uiso 1 1 calc R . . Cl1 Cl 0.68658(6) 0.93790(6) 0.59991(3) 0.02063(11) Uani 1 1 d . . . O2 O 0.5762(2) 0.8213(2) 0.55214(10) 0.0366(5) Uani 1 1 d . . . O3 O 0.8321(2) 0.8960(2) 0.62230(12) 0.0425(5) Uani 1 1 d . . . O4 O 0.7147(2) 1.06295(19) 0.56438(11) 0.0365(4) Uani 1 1 d . . . O5 O 0.6184(3) 0.9661(2) 0.65851(11) 0.0428(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01160(5) 0.01083(4) 0.01144(5) 0.00077(3) 0.00090(3) 0.00250(3) P1 0.0116(2) 0.0115(2) 0.0133(2) 0.00083(19) 0.0017(2) 0.00220(19) O1 0.0140(8) 0.0187(8) 0.0320(9) 0.0061(7) -0.0014(7) 0.0025(6) N1 0.0153(9) 0.0129(8) 0.0207(10) 0.0018(7) 0.0048(8) 0.0006(7) C2 0.0247(11) 0.0130(10) 0.0156(10) 0.0000(8) 0.0039(9) 0.0041(8) N3 0.0207(9) 0.0148(8) 0.0137(9) 0.0016(7) 0.0016(7) 0.0062(7) C4 0.0144(10) 0.0141(9) 0.0121(9) -0.0016(8) 0.0015(8) 0.0042(8) C5 0.0148(10) 0.0125(9) 0.0134(10) -0.0002(8) 0.0025(8) 0.0032(8) C6 0.0169(10) 0.0108(9) 0.0160(10) -0.0016(8) 0.0029(8) 0.0024(8) N7 0.0149(9) 0.0137(8) 0.0127(8) 0.0004(7) 0.0020(7) 0.0030(7) C8 0.0156(10) 0.0181(10) 0.0138(10) 0.0010(8) 0.0032(8) 0.0033(8) N9 0.0125(8) 0.0174(9) 0.0144(9) 0.0002(7) 0.0009(7) 0.0041(7) C10 0.0121(10) 0.0306(12) 0.0200(11) 0.0015(9) -0.0006(9) 0.0076(9) N10 0.0139(8) 0.0110(8) 0.0137(8) 0.0029(7) 0.0036(7) 0.0034(6) C11 0.0109(9) 0.0128(9) 0.0168(10) 0.0027(8) 0.0015(8) 0.0020(7) C12 0.0187(11) 0.0159(10) 0.0148(10) -0.0005(8) 0.0018(8) 0.0042(8) C13 0.0194(11) 0.0183(10) 0.0151(10) 0.0037(8) -0.0003(9) 0.0032(8) C14 0.0166(10) 0.0152(10) 0.0214(11) 0.0059(8) 0.0021(9) 0.0042(8) C15 0.0179(11) 0.0115(9) 0.0214(11) -0.0001(8) 0.0034(9) 0.0029(8) C16 0.0112(9) 0.0133(9) 0.0162(10) 0.0013(8) 0.0017(8) -0.0005(7) C17 0.0191(10) 0.0096(9) 0.0159(10) 0.0005(8) 0.0023(8) 0.0030(8) C18 0.0174(11) 0.0153(10) 0.0265(12) 0.0033(9) 0.0100(9) 0.0020(8) C19 0.0274(12) 0.0219(11) 0.0131(10) 0.0020(9) 0.0011(9) 0.0098(9) C21 0.0144(10) 0.0158(10) 0.0122(10) -0.0012(8) 0.0015(8) 0.0049(8) C22 0.0163(10) 0.0207(11) 0.0147(10) 0.0018(8) 0.0031(8) 0.0033(8) C23 0.0144(10) 0.0272(12) 0.0172(11) 0.0010(9) 0.0028(8) 0.0074(9) C24 0.0225(11) 0.0236(11) 0.0175(11) 0.0011(9) 0.0023(9) 0.0133(9) C25 0.0230(12) 0.0169(10) 0.0242(12) 0.0025(9) 0.0013(9) 0.0052(9) C26 0.0165(10) 0.0159(10) 0.0197(11) -0.0007(8) 0.0009(9) 0.0028(8) C31 0.0155(10) 0.0144(10) 0.0226(11) 0.0047(8) 0.0059(9) 0.0048(8) C32 0.0203(11) 0.0183(11) 0.0263(12) 0.0005(9) 0.0070(9) 0.0022(9) C33 0.0256(13) 0.0181(11) 0.0436(15) 0.0030(11) 0.0155(11) 0.0003(9) C34 0.0311(14) 0.0222(12) 0.0449(16) 0.0134(11) 0.0234(12) 0.0083(10) C35 0.0321(13) 0.0282(12) 0.0273(13) 0.0114(10) 0.0161(11) 0.0157(10) C36 0.0202(11) 0.0189(11) 0.0225(11) 0.0034(9) 0.0060(9) 0.0081(9) C41 0.0149(10) 0.0125(9) 0.0137(10) 0.0019(8) 0.0003(8) 0.0026(8) C42 0.0162(10) 0.0159(10) 0.0156(10) 0.0011(8) 0.0033(8) 0.0026(8) C43 0.0160(10) 0.0196(11) 0.0182(11) 0.0041(9) 0.0018(9) 0.0024(8) C44 0.0197(11) 0.0143(10) 0.0154(10) 0.0034(8) -0.0026(8) -0.0003(8) C45 0.0238(11) 0.0155(10) 0.0142(10) 0.0009(8) 0.0019(9) 0.0043(9) C46 0.0163(10) 0.0160(10) 0.0175(10) 0.0014(8) 0.0026(8) 0.0040(8) Cl1 0.0162(2) 0.0216(3) 0.0249(3) 0.0051(2) 0.0064(2) 0.0036(2) O2 0.0311(10) 0.0305(10) 0.0394(11) -0.0005(8) 0.0075(9) -0.0102(8) O3 0.0206(9) 0.0552(13) 0.0581(14) 0.0208(11) 0.0095(9) 0.0163(9) O4 0.0380(11) 0.0242(9) 0.0454(12) 0.0134(8) 0.0090(9) 0.0001(8) O5 0.0464(12) 0.0551(13) 0.0369(11) 0.0055(10) 0.0228(10) 0.0210(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 C11 2.016(2) . ? Pt1 N7 2.1253(18) . ? Pt1 N10 2.1390(17) . ? Pt1 P1 2.2333(5) . ? P1 C31 1.820(2) . ? P1 C21 1.822(2) . ? P1 C41 1.822(2) . ? O1 C6 1.221(3) . ? N1 C2 1.361(3) . ? N1 C6 1.402(3) . ? C2 N3 1.300(3) . ? N3 C4 1.358(3) . ? C4 N9 1.373(3) . ? C4 C5 1.382(3) . ? C5 N7 1.388(3) . ? C5 C6 1.431(3) . ? N7 C8 1.323(3) . ? C8 N9 1.357(3) . ? N9 C10 1.471(3) . ? N10 C19 1.481(3) . ? N10 C18 1.494(3) . ? N10 C17 1.494(3) . ? C11 C12 1.400(3) . ? C11 C16 1.409(3) . ? C12 C13 1.393(3) . ? C13 C14 1.384(3) . ? C14 C15 1.386(3) . ? C15 C16 1.391(3) . ? C16 C17 1.499(3) . ? C21 C22 1.396(3) . ? C21 C26 1.402(3) . ? C22 C23 1.392(3) . ? C23 C24 1.382(3) . ? C24 C25 1.391(3) . ? C25 C26 1.392(3) . ? C31 C36 1.397(3) . ? C31 C32 1.398(3) . ? C32 C33 1.388(3) . ? C33 C34 1.384(4) . ? C34 C35 1.384(4) . ? C35 C36 1.390(3) . ? C41 C42 1.391(3) . ? C41 C46 1.402(3) . ? C42 C43 1.392(3) . ? C43 C44 1.382(3) . ? C44 C45 1.389(3) . ? C45 C46 1.387(3) . ? Cl1 O3 1.4265(19) . ? Cl1 O5 1.430(2) . ? Cl1 O4 1.4359(18) . ? Cl1 O2 1.4490(19) . ? 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 C11 Pt1 N7 172.66(7) . . ? C11 Pt1 N10 81.46(8) . . ? N7 Pt1 N10 92.67(7) . . ? C11 Pt1 P1 94.34(6) . . ? N7 Pt1 P1 91.64(5) . . ? N10 Pt1 P1 175.46(5) . . ? C31 P1 C21 104.24(10) . . ? C31 P1 C41 108.15(10) . . ? C21 P1 C41 102.56(10) . . ? C31 P1 Pt1 113.30(7) . . ? C21 P1 Pt1 114.09(7) . . ? C41 P1 Pt1 113.53(7) . . ? C2 N1 C6 125.74(19) . . ? N3 C2 N1 125.1(2) . . ? C2 N3 C4 111.70(18) . . ? N3 C4 N9 125.41(19) . . ? N3 C4 C5 128.1(2) . . ? N9 C4 C5 106.38(18) . . ? C4 C5 N7 109.40(18) . . ? C4 C5 C6 119.32(19) . . ? N7 C5 C6 131.27(19) . . ? O1 C6 N1 121.1(2) . . ? O1 C6 C5 129.0(2) . . ? N1 C6 C5 109.89(18) . . ? C8 N7 C5 104.97(17) . . ? C8 N7 Pt1 123.97(14) . . ? C5 N7 Pt1 131.05(14) . . ? N7 C8 N9 112.62(19) . . ? C8 N9 C4 106.61(17) . . ? C8 N9 C10 127.29(19) . . ? C4 N9 C10 125.98(18) . . ? C19 N10 C18 108.64(17) . . ? C19 N10 C17 108.65(16) . . ? C18 N10 C17 107.75(16) . . ? C19 N10 Pt1 116.12(13) . . ? C18 N10 Pt1 109.44(13) . . ? C17 N10 Pt1 105.93(12) . . ? C12 C11 C16 116.37(19) . . ? C12 C11 Pt1 130.45(16) . . ? C16 C11 Pt1 113.18(15) . . ? C13 C12 C11 122.0(2) . . ? C14 C13 C12 120.3(2) . . ? C13 C14 C15 119.3(2) . . ? C14 C15 C16 120.2(2) . . ? C15 C16 C11 121.8(2) . . ? C15 C16 C17 121.28(19) . . ? C11 C16 C17 116.86(18) . . ? N10 C17 C16 109.03(16) . . ? C22 C21 C26 119.3(2) . . ? C22 C21 P1 122.17(16) . . ? C26 C21 P1 118.00(16) . . ? C23 C22 C21 119.7(2) . . ? C24 C23 C22 120.8(2) . . ? C23 C24 C25 119.9(2) . . ? C24 C25 C26 119.8(2) . . ? C25 C26 C21 120.4(2) . . ? C36 C31 C32 119.2(2) . . ? C36 C31 P1 123.70(17) . . ? C32 C31 P1 117.08(17) . . ? C33 C32 C31 120.2(2) . . ? C34 C33 C32 120.1(2) . . ? C33 C34 C35 120.3(2) . . ? C34 C35 C36 120.0(2) . . ? C35 C36 C31 120.2(2) . . ? C42 C41 C46 119.05(19) . . ? C42 C41 P1 119.28(16) . . ? C46 C41 P1 121.60(16) . . ? C41 C42 C43 120.5(2) . . ? C44 C43 C42 119.8(2) . . ? C43 C44 C45 120.6(2) . . ? C46 C45 C44 119.6(2) . . ? C45 C46 C41 120.4(2) . . ? O3 Cl1 O5 109.99(13) . . ? O3 Cl1 O4 109.94(12) . . ? O5 Cl1 O4 110.52(13) . . ? O3 Cl1 O2 108.91(13) . . ? O5 Cl1 O2 108.63(13) . . ? O4 Cl1 O2 108.81(12) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H01 O2 0.80(3) 2.08(3) 2.859(3) 166(3) . C2 H2 O4 0.95 2.41 3.323(3) 160.8 2_676 C17 H17B O3 0.99 2.46 3.394(3) 157.9 1_445 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.873 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.076