# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Zhong-Ning Chen' _publ_contact_author_email CZN@FJIRSM.AC.CN _publ_section_title ; Luminescence vapochromic properties of a platinum(II) complex with 5,5'-bis(trimethylsilylethynyl)-2,2'-bipyridine ; loop_ _publ_author_name 'Zhong-Ning Chen.' 'Jun Ni.' 'Hui-Min Wen.' 'Li-Yi Zhang.' # Attachment 'CCDC 710899.cif' data_1.Acetone _database_code_depnum_ccdc_archive 'CCDC 710899' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H44 N6 O Pt Si2' _chemical_formula_weight 960.15 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' Pt Pt -1.7033 8.3905 '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' Si Si 0.0817 0.0704 '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' H H 0.0000 0.0000 '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 7.097(3) _cell_length_b 15.148(6) _cell_length_c 21.774(9) _cell_angle_alpha 71.790(10) _cell_angle_beta 86.630(10) _cell_angle_gamma 83.210(10) _cell_volume 2207.4(16) _cell_formula_units_Z 2 _cell_measurement_temperature 113.1(1) _cell_measurement_reflns_used 5411 _cell_measurement_theta_min 3.0330 _cell_measurement_theta_max 27.4603 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0700 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 3.274 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.794 _exptl_absorpt_correction_T_min 0.711 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113.1(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Saturn70 _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13544 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0875 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7575 _reflns_number_gt 6510 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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. Constraints on the pyridine ring,TMS group and solvent are given below in SHELX format. simu 0.005 c18 c19 c20 c18' c19' c20' delu 0.005 c18 c19 c20 c18' c19' c20' dfix 1.83 0.01 si2 c18 si2 c19 si2 c20 si2 c18' si2 c19' si2 c20' sadi 0.5 c18 c19 c19 c20 c18 c20 c18' c19' c19' c20' c20' c18' rem dfix 1.39 0.01 c40 c41 c41 c42 c42 c43 c43 c44 c44 n6 n6 c40 rem dfix 2.4 0.1 c40 c42 c41 c43 c42 c44 c43 n6 c44 c40 c41 n6 simu 0.01 c40 c41 c42 c43 c44 n6 delu 0.01 c40 c41 c42 c43 c44 n6 isor 0.01 c40 c41 c42 c43 c44 n6 ; _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^)+(0.0721P)^2^+3.6024P] 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 SHELXL _refine_ls_extinction_coef 0.0204(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7575 _refine_ls_number_parameters 531 _refine_ls_number_restraints 129 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1618 _refine_ls_wR_factor_gt 0.1421 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.167 _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 0.24747(5) 0.56050(2) 0.422154(16) 0.0341(2) Uani 1 1 d . . . Si1 Si 0.3303(5) 0.4428(2) 0.81324(15) 0.0578(8) Uani 1 1 d . . . Si2 Si 0.2065(6) 0.3314(4) 0.1157(2) 0.0884(14) Uani 1 1 d D . . N1 N 0.2510(10) 0.4551(5) 0.5080(4) 0.0315(16) Uani 1 1 d . . . C1 C 0.2721(12) 0.4640(7) 0.5674(4) 0.037(2) Uani 1 1 d . . . H1A H 0.2916 0.5223 0.5701 0.044 Uiso 1 1 calc R . . C2 C 0.2658(14) 0.3896(7) 0.6245(4) 0.043(2) Uani 1 1 d . . . C3 C 0.2401(15) 0.3030(7) 0.6203(5) 0.045(2) Uani 1 1 d . . . H3A H 0.2332 0.2525 0.6577 0.054 Uiso 1 1 calc R . . C4 C 0.2244(14) 0.2912(6) 0.5597(4) 0.038(2) Uani 1 1 d . . . H4A H 0.2139 0.2325 0.5559 0.046 Uiso 1 1 calc R . . C5 C 0.2248(13) 0.3694(6) 0.5053(4) 0.036(2) Uani 1 1 d . . . C11 C 0.2812(15) 0.4057(7) 0.6861(5) 0.045(2) Uani 1 1 d . . . C12 C 0.2993(15) 0.4232(8) 0.7354(5) 0.052(3) Uani 1 1 d . . . C13 C 0.3252(18) 0.5700(8) 0.7977(6) 0.061(3) Uani 1 1 d . . . H13A H 0.4303 0.5926 0.7696 0.092 Uiso 1 1 calc R . . H13B H 0.3342 0.5828 0.8378 0.092 Uiso 1 1 calc R . . H13C H 0.2085 0.6008 0.7774 0.092 Uiso 1 1 calc R . . C14 C 0.562(2) 0.3818(11) 0.8455(7) 0.088(5) Uani 1 1 d . . . H14A H 0.6618 0.4072 0.8160 0.132 Uiso 1 1 calc R . . H14B H 0.5644 0.3164 0.8507 0.132 Uiso 1 1 calc R . . H14C H 0.5796 0.3901 0.8867 0.132 Uiso 1 1 calc R . . C15 C 0.128(3) 0.3973(11) 0.8678(6) 0.101(6) Uani 1 1 d . . . H15A H 0.0107 0.4309 0.8493 0.151 Uiso 1 1 calc R . . H15B H 0.1415 0.4054 0.9092 0.151 Uiso 1 1 calc R . . H15C H 0.1263 0.3320 0.8729 0.151 Uiso 1 1 calc R . . C16 C 0.1994(14) 0.3690(7) 0.2452(5) 0.040(2) Uani 1 1 d . . . C17 C 0.2024(17) 0.3605(8) 0.1923(5) 0.052(3) Uani 1 1 d . A . C18 C -0.034(5) 0.343(5) 0.087(4) 0.104(19) Uani 0.514(19) 1 d PDU A 1 H18A H -0.0715 0.4073 0.0631 0.156 Uiso 0.514(19) 1 calc PR A 1 H18B H -0.1202 0.3227 0.1226 0.156 Uiso 0.514(19) 1 calc PR A 1 H18C H -0.0379 0.3054 0.0585 0.156 Uiso 0.514(19) 1 calc PR A 1 C19 C 0.383(6) 0.236(3) 0.112(2) 0.150(11) Uani 0.514(19) 1 d PDU A 1 H19A H 0.4951 0.2603 0.0894 0.226 Uiso 0.514(19) 1 calc PR A 1 H19B H 0.3322 0.1993 0.0885 0.226 Uiso 0.514(19) 1 calc PR A 1 H19C H 0.4136 0.1965 0.1545 0.226 Uiso 0.514(19) 1 calc PR A 1 C20 C 0.310(6) 0.431(2) 0.0577(13) 0.152(11) Uani 0.514(19) 1 d PDU A 1 H20A H 0.2459 0.4883 0.0619 0.228 Uiso 0.514(19) 1 calc PR A 1 H20B H 0.2971 0.4291 0.0145 0.228 Uiso 0.514(19) 1 calc PR A 1 H20C H 0.4426 0.4278 0.0663 0.228 Uiso 0.514(19) 1 calc PR A 1 C18' C -0.005(7) 0.381(6) 0.068(4) 0.11(2) Uani 0.486(19) 1 d PDU A 2 H18D H -0.0016 0.4467 0.0483 0.163 Uiso 0.486(19) 1 calc PR A 2 H18E H -0.1162 0.3691 0.0949 0.163 Uiso 0.486(19) 1 calc PR A 2 H18F H -0.0082 0.3517 0.0342 0.163 Uiso 0.486(19) 1 calc PR A 2 C19' C 0.206(8) 0.2035(9) 0.1454(14) 0.144(11) Uani 0.486(19) 1 d PDU A 2 H19D H 0.1037 0.1875 0.1763 0.215 Uiso 0.486(19) 1 calc PR A 2 H19E H 0.3245 0.1756 0.1657 0.215 Uiso 0.486(19) 1 calc PR A 2 H19F H 0.1901 0.1807 0.1098 0.215 Uiso 0.486(19) 1 calc PR A 2 C20' C 0.445(3) 0.335(4) 0.0790(19) 0.149(10) Uani 0.486(19) 1 d PDU A 2 H20D H 0.4670 0.3987 0.0571 0.224 Uiso 0.486(19) 1 calc PR A 2 H20E H 0.4569 0.3003 0.0486 0.224 Uiso 0.486(19) 1 calc PR A 2 H20F H 0.5373 0.3078 0.1121 0.224 Uiso 0.486(19) 1 calc PR A 2 C21 C 0.2776(13) 0.6575(6) 0.4620(5) 0.038(2) Uani 1 1 d . . . C22 C 0.3050(13) 0.7071(6) 0.4937(5) 0.039(2) Uani 1 1 d . . . N2 N 0.2195(11) 0.4464(5) 0.3902(3) 0.0347(17) Uani 1 1 d . A . C6 C 0.2081(13) 0.3635(6) 0.4389(4) 0.035(2) Uani 1 1 d . . . C7 C 0.1861(13) 0.2835(7) 0.4246(4) 0.039(2) Uani 1 1 d . A . H7A H 0.1744 0.2281 0.4579 0.047 Uiso 1 1 calc R . . C8 C 0.1813(14) 0.2842(7) 0.3617(5) 0.041(2) Uani 1 1 d . . . H8A H 0.1684 0.2295 0.3522 0.050 Uiso 1 1 calc R A . C9 C 0.1957(14) 0.3672(6) 0.3122(4) 0.038(2) Uani 1 1 d . A . C10 C 0.2115(13) 0.4478(6) 0.3289(4) 0.037(2) Uani 1 1 d . . . H10A H 0.2166 0.5043 0.2962 0.044 Uiso 1 1 calc R A . N3 N 0.3154(13) 0.7633(6) 0.6480(4) 0.044(2) Uani 1 1 d . . . C23 C 0.3327(13) 0.7603(7) 0.5369(4) 0.038(2) Uani 1 1 d . . . C24 C 0.3973(14) 0.8469(7) 0.5170(5) 0.042(2) Uani 1 1 d . . . H24A H 0.4290 0.8743 0.4737 0.051 Uiso 1 1 calc R . . C25 C 0.4154(15) 0.8933(6) 0.5614(4) 0.042(2) Uani 1 1 d . . . H25A H 0.4555 0.9528 0.5479 0.050 Uiso 1 1 calc R . . C26 C 0.3732(13) 0.8504(7) 0.6264(4) 0.038(2) Uani 1 1 d . . . C27 C 0.2977(14) 0.7214(7) 0.6032(5) 0.041(2) Uani 1 1 d . . . H27A H 0.2590 0.6616 0.6172 0.049 Uiso 1 1 calc R . . N4 N 0.4505(12) 0.9820(6) 0.6567(4) 0.051(2) Uani 1 1 d . . . C28 C 0.3762(15) 0.8997(8) 0.6756(5) 0.047(3) Uani 1 1 d . . . C29 C 0.3033(19) 0.8617(9) 0.7368(6) 0.064(3) Uani 1 1 d . . . H29A H 0.2579 0.8034 0.7494 0.077 Uiso 1 1 calc R . . C30 C 0.300(2) 0.9153(11) 0.7803(6) 0.079(4) Uani 1 1 d . . . H30A H 0.2479 0.8926 0.8217 0.095 Uiso 1 1 calc R . . C31 C 0.3710(18) 0.9975(11) 0.7626(7) 0.071(4) Uani 1 1 d . . . H31A H 0.3701 1.0323 0.7910 0.085 Uiso 1 1 calc R . . C32 C 0.4458(17) 1.0292(9) 0.7007(6) 0.060(3) Uani 1 1 d . . . H32A H 0.4960 1.0863 0.6882 0.072 Uiso 1 1 calc R . . C33 C 0.2255(14) 0.6566(6) 0.3371(5) 0.038(2) Uani 1 1 d . . . C34 C 0.1961(16) 0.7145(7) 0.2867(5) 0.046(2) Uani 1 1 d . . . N5 N -0.0979(18) 0.8726(8) 0.1530(5) 0.074(3) Uani 1 1 d . . . C35 C 0.1410(18) 0.7895(7) 0.2294(5) 0.052(3) Uani 1 1 d . . . C36 C 0.264(2) 0.8599(8) 0.1989(6) 0.066(3) Uani 1 1 d . . . H36A H 0.3863 0.8545 0.2135 0.080 Uiso 1 1 calc R . . C37 C 0.201(3) 0.9337(9) 0.1495(6) 0.079(4) Uani 1 1 d . . . H37A H 0.2801 0.9798 0.1293 0.094 Uiso 1 1 calc R . . C38 C 0.016(3) 0.9404(8) 0.1284(5) 0.079(5) Uani 1 1 d . . . C39 C -0.0354(18) 0.7994(8) 0.2041(5) 0.056(3) Uani 1 1 d . . . H39A H -0.1161 0.7537 0.2229 0.067 Uiso 1 1 calc R . . N6 N 0.0435(14) 1.0825(9) 0.0467(6) 0.119(3) Uani 1 1 d GU . . C40 C -0.078(2) 1.0157(7) 0.0779(5) 0.112(4) Uani 1 1 d GU . . C41 C -0.2664(18) 1.0284(8) 0.0601(6) 0.116(4) Uani 1 1 d GU . . H41A H -0.3476 0.9837 0.0809 0.139 Uiso 1 1 calc R . . C42 C -0.3338(14) 1.1078(10) 0.0112(6) 0.125(4) Uani 1 1 d GU . . H42A H -0.4600 1.1163 -0.0006 0.150 Uiso 1 1 calc R . . C43 C -0.212(2) 1.1746(7) -0.0199(5) 0.116(4) Uani 1 1 d GU . . H43A H -0.2576 1.2277 -0.0526 0.139 Uiso 1 1 calc R . . C44 C -0.0239(19) 1.1619(8) -0.0021(6) 0.125(4) Uani 1 1 d GU . . H44A H 0.0573 1.2066 -0.0230 0.150 Uiso 1 1 calc R . . O01 O -0.0965(11) 0.9077(5) 0.4529(4) 0.0543(18) Uani 1 1 d . . . C01 C 0.0792(14) 1.0371(7) 0.4033(6) 0.051(3) Uani 1 1 d . . . H01A H 0.0374 1.0548 0.4410 0.076 Uiso 1 1 calc R . . H01B H 0.0325 1.0850 0.3653 0.076 Uiso 1 1 calc R . . H01C H 0.2154 1.0293 0.4013 0.076 Uiso 1 1 calc R . . C02 C 0.0043(15) 0.9464(7) 0.4071(5) 0.045(2) Uani 1 1 d . . . C03 C 0.0551(17) 0.9062(7) 0.3528(6) 0.055(3) Uani 1 1 d . . . H03A H -0.0001 0.8485 0.3614 0.083 Uiso 1 1 calc R . . H03B H 0.1906 0.8947 0.3491 0.083 Uiso 1 1 calc R . . H03C H 0.0072 0.9495 0.3131 0.083 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 0.0420(3) 0.0309(2) 0.0316(3) -0.01258(16) -0.00276(15) -0.00346(15) Si1 0.079(2) 0.062(2) 0.0367(16) -0.0222(15) -0.0063(15) -0.0033(17) Si2 0.079(3) 0.152(4) 0.067(2) -0.080(3) 0.002(2) -0.013(3) N1 0.022(4) 0.039(4) 0.038(4) -0.020(3) -0.002(3) 0.000(3) C1 0.037(5) 0.044(5) 0.034(5) -0.016(4) 0.001(4) -0.010(4) C2 0.041(6) 0.060(6) 0.028(5) -0.020(5) -0.008(4) 0.011(5) C3 0.054(6) 0.047(6) 0.031(5) -0.011(4) -0.001(4) -0.002(5) C4 0.047(6) 0.039(5) 0.031(5) -0.015(4) -0.004(4) 0.001(4) C5 0.041(5) 0.036(5) 0.033(5) -0.012(4) -0.005(4) -0.007(4) C11 0.053(6) 0.050(6) 0.036(5) -0.019(5) -0.003(5) -0.005(5) C12 0.051(7) 0.071(7) 0.040(6) -0.024(6) 0.000(5) -0.007(5) C13 0.065(8) 0.072(8) 0.054(7) -0.027(6) 0.000(6) -0.018(6) C14 0.106(12) 0.094(11) 0.055(8) -0.017(8) -0.032(8) 0.021(9) C15 0.173(17) 0.093(11) 0.048(7) -0.032(8) 0.036(9) -0.051(11) C16 0.047(6) 0.042(5) 0.034(5) -0.011(4) -0.004(4) -0.014(4) C17 0.072(8) 0.051(6) 0.037(6) -0.020(5) -0.003(5) -0.004(5) C18 0.14(2) 0.12(5) 0.06(4) -0.06(3) -0.05(2) 0.05(2) C19 0.22(3) 0.16(2) 0.106(17) -0.100(19) -0.009(16) 0.01(2) C20 0.21(3) 0.18(2) 0.091(18) -0.08(2) -0.012(18) -0.01(2) C18' 0.14(2) 0.13(5) 0.06(4) -0.06(3) -0.05(2) 0.05(2) C19' 0.22(3) 0.15(2) 0.108(19) -0.112(19) -0.011(17) 0.01(2) C20' 0.22(3) 0.17(2) 0.096(17) -0.095(19) -0.009(16) 0.00(2) C21 0.034(5) 0.036(5) 0.038(5) -0.004(4) 0.000(4) 0.002(4) C22 0.040(5) 0.029(4) 0.052(6) -0.019(4) 0.000(4) -0.004(4) N2 0.043(5) 0.036(4) 0.027(4) -0.013(3) -0.003(3) -0.004(3) C6 0.044(5) 0.031(4) 0.031(5) -0.012(4) 0.000(4) -0.001(4) C7 0.043(5) 0.039(5) 0.036(5) -0.011(4) 0.002(4) -0.011(4) C8 0.046(6) 0.040(5) 0.048(6) -0.026(5) 0.002(5) -0.009(4) C9 0.045(6) 0.037(5) 0.033(5) -0.014(4) -0.009(4) 0.000(4) C10 0.046(6) 0.037(5) 0.030(5) -0.013(4) -0.007(4) -0.003(4) N3 0.062(6) 0.042(5) 0.030(4) -0.017(4) -0.004(4) 0.001(4) C23 0.038(5) 0.047(5) 0.034(5) -0.023(4) 0.000(4) 0.006(4) C24 0.055(6) 0.039(5) 0.039(5) -0.020(4) -0.002(5) -0.005(4) C25 0.066(7) 0.028(4) 0.031(5) -0.009(4) 0.005(4) -0.009(4) C26 0.037(5) 0.042(5) 0.036(5) -0.018(4) -0.005(4) 0.005(4) C27 0.046(6) 0.036(5) 0.044(5) -0.017(4) 0.003(4) -0.008(4) N4 0.047(5) 0.057(5) 0.061(6) -0.038(5) -0.004(4) 0.000(4) C28 0.051(6) 0.056(6) 0.039(5) -0.026(5) -0.009(5) 0.005(5) C29 0.090(9) 0.058(7) 0.052(7) -0.026(6) 0.007(6) -0.016(6) C30 0.101(11) 0.100(11) 0.049(7) -0.047(8) 0.002(7) 0.000(9) C31 0.064(8) 0.099(10) 0.077(9) -0.069(9) -0.002(7) -0.004(7) C32 0.059(7) 0.065(7) 0.076(8) -0.048(7) -0.003(6) -0.007(6) C33 0.043(6) 0.036(5) 0.041(5) -0.024(5) 0.008(4) 0.006(4) C34 0.072(7) 0.034(5) 0.033(5) -0.014(5) 0.004(5) -0.004(5) N5 0.121(10) 0.059(7) 0.038(5) -0.016(5) -0.009(6) 0.021(7) C35 0.092(9) 0.042(6) 0.028(5) -0.019(5) -0.003(5) -0.001(5) C36 0.112(11) 0.043(6) 0.046(6) -0.007(5) -0.003(7) -0.033(7) C37 0.146(14) 0.047(7) 0.040(7) -0.003(6) -0.009(8) -0.020(8) C38 0.168(16) 0.032(6) 0.025(5) -0.008(5) 0.010(8) 0.025(8) C39 0.083(9) 0.049(6) 0.038(6) -0.022(5) -0.003(6) 0.003(6) N6 0.171(6) 0.107(6) 0.092(6) -0.053(5) -0.015(5) 0.004(5) C40 0.156(7) 0.107(6) 0.088(6) -0.058(5) -0.005(5) 0.003(5) C41 0.155(6) 0.112(6) 0.089(6) -0.055(5) -0.003(6) 0.022(5) C42 0.162(6) 0.121(6) 0.099(6) -0.054(5) -0.007(6) 0.016(5) C43 0.161(7) 0.107(6) 0.097(6) -0.064(5) -0.006(5) 0.015(5) C44 0.171(7) 0.113(6) 0.101(6) -0.053(5) -0.009(6) 0.003(6) O01 0.072(5) 0.042(4) 0.051(4) -0.016(4) 0.002(4) -0.015(4) C01 0.039(6) 0.051(6) 0.067(7) -0.023(6) -0.003(5) -0.006(5) C02 0.044(6) 0.039(5) 0.054(6) -0.015(5) -0.008(5) -0.003(4) C03 0.071(8) 0.044(6) 0.058(7) -0.024(5) 0.001(6) -0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C21 1.962(10) . ? Pt1 C33 1.966(10) . ? Pt1 N1 2.043(8) . ? Pt1 N2 2.087(7) . ? Si1 C12 1.839(11) . ? Si1 C13 1.846(12) . ? Si1 C14 1.849(13) . ? Si1 C15 1.865(15) . ? Si2 C19 1.822(10) . ? Si2 C18' 1.827(10) . ? Si2 C18 1.829(10) . ? Si2 C20' 1.830(10) . ? Si2 C20 1.839(10) . ? Si2 C19' 1.840(10) . ? Si2 C17 1.852(11) . ? N1 C5 1.354(11) . ? N1 C1 1.360(11) . ? C1 C2 1.396(14) . ? C2 C3 1.378(14) . ? C2 C11 1.448(13) . ? C3 C4 1.399(13) . ? C4 C5 1.389(13) . ? C5 C6 1.489(12) . ? C11 C12 1.200(13) . ? C16 C17 1.197(13) . ? C16 C9 1.448(13) . ? C21 C22 1.205(13) . ? C22 C23 1.451(13) . ? N2 C10 1.333(11) . ? N2 C6 1.374(11) . ? C6 C7 1.371(12) . ? C7 C8 1.369(13) . ? C8 C9 1.387(14) . ? C9 C10 1.397(12) . ? N3 C27 1.339(12) . ? N3 C26 1.359(13) . ? C23 C24 1.372(14) . ? C23 C27 1.398(13) . ? C24 C25 1.380(12) . ? C25 C26 1.392(13) . ? C26 C28 1.488(13) . ? N4 C28 1.346(14) . ? N4 C32 1.358(13) . ? C28 C29 1.373(16) . ? C29 C30 1.426(16) . ? C30 C31 1.33(2) . ? C31 C32 1.379(19) . ? C33 C34 1.183(13) . ? C34 C35 1.439(14) . ? N5 C38 1.341(19) . ? N5 C39 1.354(14) . ? C35 C39 1.370(16) . ? C35 C36 1.430(17) . ? C36 C37 1.338(17) . ? C37 C38 1.40(2) . ? C38 C40 1.442(14) . ? N6 C40 1.3900 . ? N6 C44 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? O01 C02 1.225(13) . ? C01 C02 1.508(14) . ? C02 C03 1.500(14) . ? 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 C21 Pt1 C33 89.7(4) . . ? C21 Pt1 N1 94.3(3) . . ? C33 Pt1 N1 174.7(3) . . ? C21 Pt1 N2 173.5(3) . . ? C33 Pt1 N2 96.8(3) . . ? N1 Pt1 N2 79.2(3) . . ? C12 Si1 C13 107.5(6) . . ? C12 Si1 C14 108.2(6) . . ? C13 Si1 C14 110.8(7) . . ? C12 Si1 C15 107.6(6) . . ? C13 Si1 C15 110.2(6) . . ? C14 Si1 C15 112.3(8) . . ? C19 Si2 C18' 129(4) . . ? C19 Si2 C18 122(3) . . ? C18' Si2 C18 20(4) . . ? C19 Si2 C20' 50(2) . . ? C18' Si2 C20' 122(3) . . ? C18 Si2 C20' 136(3) . . ? C19 Si2 C20 101(2) . . ? C18' Si2 C20 83(3) . . ? C18 Si2 C20 103(2) . . ? C20' Si2 C20 52(2) . . ? C19 Si2 C19' 47(2) . . ? C18' Si2 C19' 108(3) . . ? C18 Si2 C19' 90(3) . . ? C20' Si2 C19' 98(2) . . ? C20 Si2 C19' 146.3(19) . . ? C19 Si2 C17 114.6(12) . . ? C18' Si2 C17 114(4) . . ? C18 Si2 C17 110(3) . . ? C20' Si2 C17 110.5(12) . . ? C20 Si2 C17 102.6(11) . . ? C19' Si2 C17 101.7(10) . . ? C5 N1 C1 117.4(8) . . ? C5 N1 Pt1 116.6(6) . . ? C1 N1 Pt1 125.9(6) . . ? N1 C1 C2 123.0(9) . . ? C3 C2 C1 118.4(8) . . ? C3 C2 C11 122.0(9) . . ? C1 C2 C11 119.6(9) . . ? C2 C3 C4 119.8(9) . . ? C5 C4 C3 118.3(9) . . ? N1 C5 C4 122.9(8) . . ? N1 C5 C6 114.9(8) . . ? C4 C5 C6 122.1(8) . . ? C12 C11 C2 176.4(12) . . ? C11 C12 Si1 176.7(11) . . ? C17 C16 C9 173.1(11) . . ? C16 C17 Si2 172.8(10) . . ? C22 C21 Pt1 171.1(8) . . ? C21 C22 C23 174.8(11) . . ? C10 N2 C6 119.2(8) . . ? C10 N2 Pt1 126.3(6) . . ? C6 N2 Pt1 114.5(5) . . ? C7 C6 N2 120.4(8) . . ? C7 C6 C5 124.9(8) . . ? N2 C6 C5 114.7(7) . . ? C8 C7 C6 120.5(9) . . ? C7 C8 C9 119.5(8) . . ? C8 C9 C10 118.1(8) . . ? C8 C9 C16 120.5(8) . . ? C10 C9 C16 121.4(9) . . ? N2 C10 C9 122.2(9) . . ? C27 N3 C26 116.4(8) . . ? C24 C23 C27 116.8(8) . . ? C24 C23 C22 123.9(9) . . ? C27 C23 C22 119.2(9) . . ? C23 C24 C25 119.9(9) . . ? C24 C25 C26 119.5(9) . . ? N3 C26 C25 122.0(8) . . ? N3 C26 C28 116.0(9) . . ? C25 C26 C28 121.8(9) . . ? N3 C27 C23 125.2(9) . . ? C28 N4 C32 117.0(10) . . ? N4 C28 C29 122.9(9) . . ? N4 C28 C26 116.9(9) . . ? C29 C28 C26 120.2(10) . . ? C28 C29 C30 117.2(12) . . ? C31 C30 C29 121.0(13) . . ? C30 C31 C32 117.8(11) . . ? N4 C32 C31 124.0(12) . . ? C34 C33 Pt1 174.4(9) . . ? C33 C34 C35 173.0(11) . . ? C38 N5 C39 117.7(13) . . ? C39 C35 C36 117.4(11) . . ? C39 C35 C34 121.3(11) . . ? C36 C35 C34 121.2(11) . . ? C37 C36 C35 119.8(14) . . ? C36 C37 C38 119.1(14) . . ? N5 C38 C37 122.5(11) . . ? N5 C38 C40 110.4(16) . . ? C37 C38 C40 127.1(15) . . ? N5 C39 C35 123.2(12) . . ? C40 N6 C44 120.0 . . ? C41 C40 N6 120.0 . . ? C41 C40 C38 128.2(13) . . ? N6 C40 C38 111.8(13) . . ? C40 C41 C42 120.0 . . ? C43 C42 C41 120.0 . . ? C42 C43 C44 120.0 . . ? C43 C44 N6 120.0 . . ? O01 C02 C03 121.4(9) . . ? O01 C02 C01 120.7(10) . . ? C03 C02 C01 117.9(10) . . ? 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 C7 H7A O01 0.93 2.44 3.366(12) 171.8 2_566 C4 H4A O01 0.93 2.44 3.342(11) 164.8 2_566 C31 H31A N5 0.93 2.73 3.458(14) 135.9 2_576 C01 H01A O01 0.96 2.61 3.497(13) 152.9 2_576 C01 H01C N4 0.96 2.64 3.531(13) 154.9 2_676 C13 H13A Cg1 0.96 2.81 3.579 137.7 2_666 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.393 _refine_diff_density_min -1.262 _refine_diff_density_rms 0.176 # Attachment 'CCDC 710900.cif' data_1.CHCl3 _database_code_depnum_ccdc_archive 'CCDC 710900' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45.50 H40.5 Cl4.50 N6 O0.50 Pt Si2' _chemical_formula_weight 1090.89 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' O O 0.0106 0.0060 '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' _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 25.299(11) _cell_length_b 32.774(13) _cell_length_c 13.478(6) _cell_angle_alpha 90.00 _cell_angle_beta 112.987(8) _cell_angle_gamma 90.00 _cell_volume 10288(8) _cell_formula_units_Z 8 _cell_measurement_temperature 113.1500 _cell_measurement_reflns_used 10834 _cell_measurement_theta_min 3.0396 _cell_measurement_theta_max 27.4333 _exptl_crystal_description Prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.0500 _exptl_crystal_size_min 0.0200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4342 _exptl_absorpt_coefficient_mu 3.045 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.942 _exptl_absorpt_correction_T_min 0.541 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113.1(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Saturn70 _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32100 _diffrn_reflns_av_R_equivalents 0.0843 _diffrn_reflns_av_sigmaI/netI 0.0948 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8887 _reflns_number_gt 6875 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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. The solvent molecule with C02 atom are modelled using anisotropic temperature factors The CH3 group with C18, C19, C20 atoms are disordered and are modelled using anisotropic temperature factors The large non-solvent C Ueq(max)/Ueq(min) ... 4.21 Ratio, large non-solvent H Ueq(max)/Ueq(min) ... 5.22 ratio and large non-solvent N Ueq(max)/Ueq(min)...3.82 Ratio are caused by disorderd atoms of structure and poor quality of the crystal. Constraints of the structure are given below in SHELX format. dfix 1.35 0.01 n4 c40 c40 c41 c41 c42 c42 c43 c43 c44 c44 n4 dfix 1.83 0.008 si2 c18 si2 c19 si2 c20 si2 c18' si2 c19' si2 c20' dfix 1.83 0.008 si1 c1 si1 c2 si1 c3 sadi 0.05 c18 c19 c19 c20 c20 c18 c18' c19' c19' c20' c20' c18' simu c18 c19 c20 c18' c19' c20' SI2 delu c18 c19 c20 c18' c19' c20' SI2 dfix 1.76 0.01 c02 cl4 c02 cl5 c02 cl6 dfix 1.76 0.01 c02' cl4' c02' cl5' c02' cl6' dang 2.9 0.01 cl4 cl5 cl5 cl6 cl6 cl4 dang 2.9 0.01 cl4' cl5' cl5' cl6' cl6' cl4' simu 0.01 c02 cl4 cl5 cl6 c02' cl4' cl5' cl6' delu c02 cl4 cl5 cl6 c02' cl4' cl5' cl6' simu 0.01 n4 c40 c41 c42 c43 c44 simu 0.01 c4 c5 c6 c7 c8 c9 c10 N1 dfix 1.20 0.01 c4 c5 isor o01 isor 0.01 c19 c20 c19' c20' eqiv $1 1-x,y,-1.5-z eqiv $2 x,y,1+z dang 3.2 0.01 CL6 CL6_$1 dang 3.18 0.01 C44 CL5'_$2 ; _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^)+(0.0812P)^2^+42.2224P] 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 SHELXL _refine_ls_extinction_coef 0.00069(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8887 _refine_ls_number_parameters 624 _refine_ls_number_restraints 231 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1806 _refine_ls_wR_factor_gt 0.1636 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.006 _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 0.476640(14) 0.452191(10) 0.61981(3) 0.04037(18) Uani 1 1 d . . . Si1 Si 0.39355(14) 0.69340(8) 0.6210(3) 0.0635(8) Uani 1 1 d D . . Si2 Si 0.75310(17) 0.28667(14) 0.7696(4) 0.1201(17) Uani 1 1 d DU . . C1 C 0.3177(4) 0.6783(4) 0.5747(12) 0.094(4) Uani 1 1 d D . . H1A H 0.3136 0.6573 0.6209 0.141 Uiso 1 1 calc R . . H1B H 0.3047 0.6682 0.5022 0.141 Uiso 1 1 calc R . . H1C H 0.2950 0.7015 0.5768 0.141 Uiso 1 1 calc R . . C2 C 0.4213(6) 0.7092(3) 0.7632(6) 0.082(4) Uani 1 1 d D . . H2A H 0.4003 0.7325 0.7708 0.123 Uiso 1 1 calc R . . H2B H 0.4612 0.7161 0.7865 0.123 Uiso 1 1 calc R . . H2C H 0.4170 0.6872 0.8064 0.123 Uiso 1 1 calc R . . C3 C 0.4046(6) 0.7345(3) 0.5382(10) 0.086(4) Uani 1 1 d D . . H3A H 0.4445 0.7419 0.5658 0.129 Uiso 1 1 calc R . . H3B H 0.3822 0.7579 0.5405 0.129 Uiso 1 1 calc R . . H3C H 0.3928 0.7253 0.4651 0.129 Uiso 1 1 calc R . . C4 C 0.4364(5) 0.6486(3) 0.6142(8) 0.060(2) Uani 1 1 d DU . . C5 C 0.4658(4) 0.6192(3) 0.6162(7) 0.051(2) Uani 1 1 d DU . . C6 C 0.4762(4) 0.5460(2) 0.6175(6) 0.0390(19) Uani 1 1 d U . . H6A H 0.4374 0.5440 0.6047 0.047 Uiso 1 1 calc R . . C7 C 0.4999(4) 0.5838(3) 0.6262(7) 0.0420(17) Uani 1 1 d U . . C8 C 0.5604(4) 0.5866(3) 0.6544(7) 0.0444(18) Uani 1 1 d U . . H8A H 0.5805 0.6111 0.6693 0.053 Uiso 1 1 calc R . . C9 C 0.5852(4) 0.5506(2) 0.6574(6) 0.0382(17) Uani 1 1 d U . . H9A H 0.6234 0.5519 0.6655 0.046 Uiso 1 1 calc R . . C10 C 0.5646(4) 0.5133(2) 0.6509(6) 0.0404(17) Uani 1 1 d U . . C11 C 0.5956(4) 0.4751(3) 0.6591(6) 0.042(2) Uani 1 1 d . . . C12 C 0.6513(4) 0.4713(3) 0.6694(7) 0.050(2) Uani 1 1 d . . . H12A H 0.6720 0.4946 0.6682 0.060 Uiso 1 1 calc R . . C13 C 0.6766(4) 0.4351(3) 0.6810(8) 0.053(2) Uani 1 1 d . . . H13A H 0.7145 0.4331 0.6881 0.064 Uiso 1 1 calc R . . C14 C 0.6455(4) 0.3998(3) 0.6825(7) 0.051(2) Uani 1 1 d . A . C15 C 0.5879(4) 0.4036(3) 0.6649(7) 0.048(2) Uani 1 1 d . . . H15A H 0.5663 0.3803 0.6623 0.057 Uiso 1 1 calc R . . C16 C 0.6733(4) 0.3599(3) 0.7023(8) 0.057(3) Uani 1 1 d . . . C17 C 0.7024(5) 0.3291(3) 0.7254(10) 0.075(3) Uani 1 1 d . A . C21 C 0.3990(4) 0.4699(3) 0.5895(7) 0.044(2) Uani 1 1 d . . . C22 C 0.3539(4) 0.4861(3) 0.5747(7) 0.050(2) Uani 1 1 d . . . C23 C 0.2519(4) 0.4902(3) 0.5616(9) 0.067(3) Uani 1 1 d . . . H23A H 0.2490 0.4619 0.5606 0.080 Uiso 1 1 calc R . . C24 C 0.3025(4) 0.5082(3) 0.5656(7) 0.051(2) Uani 1 1 d . . . C25 C 0.3025(4) 0.5522(3) 0.5645(8) 0.054(2) Uani 1 1 d . . . H25A H 0.3352 0.5656 0.5660 0.065 Uiso 1 1 calc R . . C26 C 0.2589(4) 0.5740(3) 0.5615(7) 0.044(2) Uani 1 1 d . . . H26A H 0.2615 0.6023 0.5622 0.052 Uiso 1 1 calc R . . C27 C 0.2099(4) 0.5563(3) 0.5575(8) 0.051(2) Uani 1 1 d . . . C28 C 0.1627(4) 0.5825(3) 0.5539(9) 0.063(3) Uani 1 1 d . . . C29 C 0.1137(4) 0.5644(3) 0.5473(10) 0.067(3) Uani 1 1 d . . . H29A H 0.1102 0.5362 0.5429 0.081 Uiso 1 1 calc R . . C30 C 0.1218(5) 0.6477(3) 0.5560(11) 0.081(4) Uani 1 1 d . . . H30A H 0.1243 0.6761 0.5585 0.098 Uiso 1 1 calc R . . C31 C 0.0720(5) 0.6295(4) 0.5516(11) 0.082(4) Uani 1 1 d . . . H31A H 0.0411 0.6449 0.5518 0.099 Uiso 1 1 calc R . . C32 C 0.0698(5) 0.5877(4) 0.5470(12) 0.095(4) Uani 1 1 d . . . H32A H 0.0364 0.5748 0.5435 0.113 Uiso 1 1 calc R . . C33 C 0.4544(4) 0.3948(3) 0.6105(7) 0.047(2) Uani 1 1 d . . . C34 C 0.4467(4) 0.3580(3) 0.6071(7) 0.047(2) Uani 1 1 d . . . C35 C 0.4031(5) 0.2960(3) 0.6430(9) 0.063(3) Uani 1 1 d . . . H35A H 0.3799 0.3133 0.6634 0.076 Uiso 1 1 calc R . . C36 C 0.4414(4) 0.3141(3) 0.6088(7) 0.051(2) Uani 1 1 d . . . C37 C 0.4759(5) 0.2880(3) 0.5827(11) 0.073(3) Uani 1 1 d . . . H37A H 0.5043 0.2986 0.5626 0.088 Uiso 1 1 calc R . . C38 C 0.4697(5) 0.2464(3) 0.5853(11) 0.079(4) Uani 1 1 d . . . H38A H 0.4920 0.2289 0.5636 0.095 Uiso 1 1 calc R . . C39 C 0.4296(4) 0.2316(3) 0.6211(9) 0.061(3) Uani 1 1 d . . . C40 C 0.4211(6) 0.1869(3) 0.6303(16) 0.119(4) Uani 1 1 d DU . . C41 C 0.3819(6) 0.1714(3) 0.6656(15) 0.116(4) Uani 1 1 d DU . . H41A H 0.3601 0.1893 0.6878 0.139 Uiso 1 1 calc R . . C42 C 0.3732(7) 0.1304(3) 0.6699(17) 0.130(4) Uani 1 1 d DU . . H42A H 0.3476 0.1202 0.6981 0.156 Uiso 1 1 calc R . . C43 C 0.4031(8) 0.1051(5) 0.6315(19) 0.154(5) Uani 1 1 d DU . . H43A H 0.3985 0.0770 0.6320 0.184 Uiso 1 1 calc R . . C44 C 0.4398(8) 0.1219(4) 0.5922(18) 0.158(5) Uani 1 1 d DU . . H44A H 0.4594 0.1043 0.5644 0.189 Uiso 1 1 calc R . . N1 N 0.5070(3) 0.5109(2) 0.6268(5) 0.0383(15) Uani 1 1 d U . . N2 N 0.5627(3) 0.4409(2) 0.6514(5) 0.0447(17) Uani 1 1 d . . . N3 N 0.3955(4) 0.2562(3) 0.6500(8) 0.065(2) Uani 1 1 d . . . N4 N 0.4500(7) 0.1620(3) 0.5905(15) 0.145(4) Uani 1 1 d DU . . N5 N 0.2051(4) 0.5139(3) 0.5592(8) 0.083(3) Uani 1 1 d . . . N6 N 0.1685(5) 0.6253(3) 0.5567(10) 0.096(3) Uani 1 1 d . . . C01 C 0.3079(5) 0.3935(3) 0.4306(8) 0.063(3) Uani 1 1 d . . . H01A H 0.3453 0.4064 0.4686 0.076 Uiso 1 1 calc R . . Cl01 Cl 0.31724(15) 0.35179(10) 0.3574(3) 0.0885(10) Uani 1 1 d . . . Cl02 Cl 0.26115(12) 0.42976(10) 0.3446(2) 0.0734(8) Uani 1 1 d . . . Cl03 Cl 0.28161(14) 0.37637(10) 0.5275(2) 0.0784(8) Uani 1 1 d . . . O01 O -0.0252(10) 0.6756(9) -0.715(3) 0.23(2) Uani 0.50 1 d PU . . C18 C 0.7231(17) 0.2400(7) 0.695(2) 0.094(8) Uani 0.497(19) 1 d PDU A 1 H18A H 0.7175 0.2436 0.6205 0.142 Uiso 0.497(19) 1 calc PR A 1 H18B H 0.6869 0.2342 0.6992 0.142 Uiso 0.497(19) 1 calc PR A 1 H18C H 0.7491 0.2178 0.7249 0.142 Uiso 0.497(19) 1 calc PR A 1 C19 C 0.7578(13) 0.2746(9) 0.9069(12) 0.117(7) Uani 0.497(19) 1 d PDU A 1 H19A H 0.7840 0.2524 0.9359 0.175 Uiso 0.497(19) 1 calc PR A 1 H19B H 0.7205 0.2670 0.9038 0.175 Uiso 0.497(19) 1 calc PR A 1 H19C H 0.7712 0.2981 0.9523 0.175 Uiso 0.497(19) 1 calc PR A 1 C20 C 0.8261(8) 0.2987(13) 0.784(3) 0.160(10) Uani 0.497(19) 1 d PDU A 1 H20A H 0.8264 0.3052 0.7151 0.240 Uiso 0.497(19) 1 calc PR A 1 H20B H 0.8505 0.2756 0.8141 0.240 Uiso 0.497(19) 1 calc PR A 1 H20C H 0.8400 0.3217 0.8318 0.240 Uiso 0.497(19) 1 calc PR A 1 C18' C 0.7142(17) 0.2385(8) 0.743(3) 0.125(11) Uani 0.503(19) 1 d PDU A 2 H18D H 0.7020 0.2318 0.6677 0.188 Uiso 0.503(19) 1 calc PR A 2 H18E H 0.6812 0.2409 0.7608 0.188 Uiso 0.503(19) 1 calc PR A 2 H18F H 0.7388 0.2173 0.7855 0.188 Uiso 0.503(19) 1 calc PR A 2 C19' C 0.8066(11) 0.2965(10) 0.9041(13) 0.122(8) Uani 0.503(19) 1 d PDU A 2 H19D H 0.8398 0.3090 0.8987 0.183 Uiso 0.503(19) 1 calc PR A 2 H19E H 0.8175 0.2713 0.9429 0.183 Uiso 0.503(19) 1 calc PR A 2 H19F H 0.7908 0.3146 0.9416 0.183 Uiso 0.503(19) 1 calc PR A 2 C20' C 0.7917(15) 0.2895(12) 0.679(2) 0.155(10) Uani 0.503(19) 1 d PDU A 2 H20D H 0.7646 0.2934 0.6058 0.233 Uiso 0.503(19) 1 calc PR A 2 H20E H 0.8124 0.2646 0.6830 0.233 Uiso 0.503(19) 1 calc PR A 2 H20F H 0.8181 0.3120 0.6993 0.233 Uiso 0.503(19) 1 calc PR A 2 C02 C 0.404(2) 0.0539(15) -0.694(4) 0.333(15) Uani 0.25 1 d PDU B 1 H02A H 0.4043 0.0599 -0.6228 0.400 Uiso 0.25 1 calc PR B 1 Cl4 Cl 0.339(2) 0.029(3) -0.769(5) 0.40(2) Uani 0.25 1 d PDU B 1 Cl5 Cl 0.409(3) 0.1006(14) -0.755(4) 0.45(4) Uani 0.25 1 d PDU B 1 Cl6 Cl 0.463(3) 0.0224(13) -0.676(5) 0.335(14) Uani 0.25 1 d PDU B 1 C02' C 0.403(2) 0.0368(13) -0.715(3) 0.330(15) Uani 0.25 1 d PDU C 2 H02B H 0.4105 0.0581 -0.7590 0.396 Uiso 0.25 1 calc PR C 2 Cl4' Cl 0.340(3) 0.011(3) -0.798(5) 0.40(2) Uani 0.25 1 d PDU C 2 Cl5' Cl 0.3940(16) 0.0609(9) -0.606(3) 0.310(14) Uani 0.25 1 d PDU C 2 Cl6' Cl 0.462(2) 0.0035(11) -0.671(6) 0.314(14) Uani 0.25 1 d PDU C 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 0.0492(3) 0.0390(3) 0.0344(3) -0.00175(13) 0.01805(18) 0.00111(14) Si1 0.085(2) 0.0411(15) 0.0719(19) 0.0020(14) 0.0381(17) 0.0104(14) Si2 0.081(2) 0.089(3) 0.151(4) -0.033(3) 0.003(2) 0.047(2) C1 0.099(9) 0.084(9) 0.115(11) -0.024(8) 0.059(9) -0.005(8) C2 0.126(10) 0.052(7) 0.084(8) -0.008(6) 0.059(8) 0.007(7) C3 0.109(10) 0.049(7) 0.109(10) 0.016(6) 0.052(8) 0.021(7) C4 0.080(6) 0.049(5) 0.053(5) 0.003(4) 0.030(5) 0.000(5) C5 0.069(5) 0.055(5) 0.035(4) 0.003(4) 0.026(4) 0.009(4) C6 0.050(4) 0.042(4) 0.029(4) -0.001(3) 0.021(3) 0.003(3) C7 0.058(4) 0.033(4) 0.040(4) -0.003(3) 0.024(3) 0.001(3) C8 0.062(4) 0.029(4) 0.047(4) -0.004(3) 0.026(4) -0.010(3) C9 0.077(5) 0.028(3) 0.029(4) 0.003(3) 0.042(4) 0.012(3) C10 0.063(4) 0.028(4) 0.034(4) -0.001(3) 0.024(4) -0.001(3) C11 0.057(5) 0.042(5) 0.028(4) 0.004(4) 0.016(4) 0.001(4) C12 0.057(5) 0.052(6) 0.045(5) 0.010(4) 0.023(5) -0.004(5) C13 0.051(5) 0.056(6) 0.056(6) -0.004(5) 0.022(5) 0.000(5) C14 0.057(5) 0.057(6) 0.044(5) -0.005(4) 0.024(4) 0.014(5) C15 0.056(5) 0.049(5) 0.045(5) 0.010(4) 0.027(4) 0.012(4) C16 0.042(5) 0.074(7) 0.059(6) -0.003(5) 0.024(5) 0.010(5) C17 0.065(6) 0.059(7) 0.087(8) -0.012(6) 0.015(6) 0.016(6) C21 0.062(6) 0.033(4) 0.037(5) -0.007(4) 0.018(4) 0.001(4) C22 0.058(5) 0.048(5) 0.045(5) -0.005(4) 0.023(4) -0.008(5) C23 0.057(6) 0.057(6) 0.089(8) -0.008(6) 0.033(6) 0.003(5) C24 0.054(5) 0.053(6) 0.045(5) -0.005(4) 0.017(4) -0.003(4) C25 0.056(5) 0.059(6) 0.052(6) 0.002(4) 0.024(5) -0.002(5) C26 0.053(5) 0.030(4) 0.051(5) 0.001(4) 0.024(4) 0.007(4) C27 0.040(5) 0.063(6) 0.046(5) 0.016(5) 0.010(4) 0.007(4) C28 0.062(6) 0.054(6) 0.073(7) -0.008(5) 0.026(5) 0.007(5) C29 0.050(5) 0.032(5) 0.123(10) -0.005(6) 0.038(6) -0.001(4) C30 0.089(8) 0.041(6) 0.115(10) 0.002(6) 0.041(8) 0.017(6) C31 0.069(7) 0.065(8) 0.108(10) 0.005(7) 0.030(7) 0.017(6) C32 0.063(7) 0.082(9) 0.134(12) -0.001(8) 0.034(8) 0.006(7) C33 0.049(5) 0.062(6) 0.034(5) 0.001(4) 0.021(4) 0.004(5) C34 0.051(5) 0.039(5) 0.049(5) 0.001(4) 0.018(4) 0.003(4) C35 0.066(6) 0.051(6) 0.074(7) -0.003(5) 0.029(6) -0.001(5) C36 0.052(5) 0.044(5) 0.048(5) 0.009(4) 0.009(4) 0.004(4) C37 0.088(8) 0.045(6) 0.111(9) -0.008(6) 0.065(7) -0.004(5) C38 0.110(9) 0.038(6) 0.125(10) -0.010(6) 0.085(8) 0.011(6) C39 0.063(6) 0.047(6) 0.078(7) 0.007(5) 0.034(6) -0.008(5) C40 0.117(7) 0.040(5) 0.245(11) 0.037(6) 0.120(7) 0.011(5) C41 0.109(7) 0.044(5) 0.233(11) 0.048(6) 0.108(7) 0.011(5) C42 0.119(7) 0.056(6) 0.254(11) 0.039(7) 0.113(8) 0.004(6) C43 0.151(8) 0.061(7) 0.285(12) 0.032(8) 0.124(8) 0.001(6) C44 0.160(8) 0.066(7) 0.293(11) 0.024(8) 0.139(8) 0.007(7) N1 0.043(3) 0.046(4) 0.027(3) 0.003(3) 0.016(3) 0.014(3) N2 0.060(4) 0.047(4) 0.030(4) 0.003(3) 0.020(3) 0.004(4) N3 0.064(5) 0.058(5) 0.086(6) 0.003(5) 0.042(5) 0.003(4) N4 0.151(7) 0.060(6) 0.277(11) 0.025(7) 0.141(7) 0.009(6) N5 0.072(6) 0.081(7) 0.085(7) -0.008(6) 0.017(5) 0.010(5) N6 0.094(7) 0.073(7) 0.122(9) 0.005(7) 0.044(7) 0.010(6) C01 0.070(6) 0.057(6) 0.054(6) -0.002(5) 0.017(5) -0.007(5) Cl01 0.104(2) 0.080(2) 0.083(2) -0.0346(17) 0.0374(18) -0.0268(18) Cl02 0.0663(15) 0.083(2) 0.0581(16) 0.0116(14) 0.0107(13) -0.0184(15) Cl03 0.090(2) 0.079(2) 0.0730(19) 0.0170(15) 0.0400(16) 0.0011(16) O01 0.12(2) 0.16(2) 0.29(4) 0.09(3) -0.05(2) 0.009(16) C18 0.137(19) 0.051(11) 0.090(17) 0.018(11) 0.038(18) 0.054(10) C19 0.102(12) 0.098(12) 0.135(9) -0.034(8) 0.029(9) 0.021(9) C20 0.146(10) 0.160(14) 0.172(14) 0.002(10) 0.060(10) 0.003(9) C18' 0.13(2) 0.078(15) 0.13(3) 0.010(19) 0.006(18) 0.043(11) C19' 0.111(11) 0.114(12) 0.129(8) 0.000(9) 0.034(7) 0.010(9) C20' 0.155(14) 0.148(15) 0.149(11) -0.011(10) 0.044(10) 0.019(9) C02 0.33(2) 0.18(2) 0.55(4) -0.09(2) 0.23(3) -0.05(2) Cl4 0.30(2) 0.79(7) 0.10(3) 0.02(3) 0.08(2) -0.13(3) Cl5 0.78(10) 0.23(4) 0.25(5) -0.02(3) 0.09(6) 0.04(3) Cl6 0.314(19) 0.19(3) 0.55(4) -0.04(3) 0.22(2) -0.05(2) C02' 0.32(2) 0.18(2) 0.55(4) -0.08(3) 0.23(3) -0.04(2) Cl4' 0.33(2) 0.78(7) 0.10(3) 0.02(2) 0.09(2) -0.14(3) Cl5' 0.33(3) 0.133(19) 0.53(4) -0.08(2) 0.24(3) -0.100(19) Cl6' 0.29(2) 0.16(3) 0.55(4) -0.03(3) 0.23(2) -0.06(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C21 1.932(10) . ? Pt1 C33 1.953(10) . ? Pt1 N1 2.059(7) . ? Pt1 N2 2.081(8) . ? Pt1 Pt1 3.2363(15) 2_656 ? Si1 C1 1.840(7) . ? Si1 C3 1.840(7) . ? Si1 C2 1.839(7) . ? Si1 C4 1.848(10) . ? Si2 C19' 1.819(8) . ? Si2 C18' 1.821(8) . ? Si2 C20 1.822(8) . ? Si2 C18 1.826(8) . ? Si2 C17 1.828(11) . ? Si2 C20' 1.845(8) . ? Si2 C19 1.851(8) . ? C4 C5 1.210(8) . ? C5 C7 1.423(12) . ? C6 C7 1.362(11) . ? C6 N1 1.369(10) . ? C7 C8 1.428(12) . ? C8 C9 1.330(11) . ? C9 C10 1.317(11) . ? C10 N1 1.366(11) . ? C10 C11 1.458(12) . ? C11 C12 1.368(13) . ? C11 N2 1.376(11) . ? C12 C13 1.328(13) . ? C13 C14 1.404(14) . ? C14 C15 1.388(12) . ? C14 C16 1.458(14) . ? C15 N2 1.359(11) . ? C16 C17 1.214(14) . ? C21 C22 1.204(12) . ? C22 C24 1.452(13) . ? C23 C24 1.391(13) . ? C23 N5 1.404(13) . ? C24 C25 1.441(13) . ? C25 C26 1.302(12) . ? C26 C27 1.350(12) . ? C27 N5 1.396(14) . ? C27 C28 1.458(14) . ? C28 C29 1.343(14) . ? C28 N6 1.412(14) . ? C29 C32 1.346(15) . ? C30 C31 1.374(17) . ? C30 N6 1.388(15) . ? C31 C32 1.373(17) . ? C33 C34 1.221(13) . ? C34 C36 1.444(13) . ? C35 N3 1.328(13) . ? C35 C36 1.362(14) . ? C36 C37 1.363(14) . ? C37 C38 1.374(14) . ? C38 C39 1.372(14) . ? C39 N3 1.344(13) . ? C39 C40 1.493(14) . ? C40 N4 1.340(9) . ? C40 C41 1.357(9) . ? C41 C42 1.365(9) . ? C42 C43 1.355(9) . ? C43 C44 1.351(9) . ? C44 N4 1.342(9) . ? C01 Cl01 1.755(11) . ? C01 Cl02 1.756(11) . ? C01 Cl03 1.772(11) . ? C02 Cl5 1.759(10) . ? C02 Cl4 1.760(10) . ? C02 Cl6 1.760(10) . ? C02' Cl5' 1.758(10) . ? C02' Cl4' 1.758(10) . ? C02' Cl6' 1.759(10) . ? 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 C21 Pt1 C33 91.8(4) . . ? C21 Pt1 N1 93.4(3) . . ? C33 Pt1 N1 174.4(3) . . ? C21 Pt1 N2 172.7(3) . . ? C33 Pt1 N2 95.4(3) . . ? N1 Pt1 N2 79.3(3) . . ? C21 Pt1 Pt1 98.1(2) . 2_656 ? C33 Pt1 Pt1 92.5(2) . 2_656 ? N1 Pt1 Pt1 88.78(17) . 2_656 ? N2 Pt1 Pt1 82.42(19) . 2_656 ? C1 Si1 C3 112.1(7) . . ? C1 Si1 C2 110.7(6) . . ? C3 Si1 C2 109.8(6) . . ? C1 Si1 C4 108.9(6) . . ? C3 Si1 C4 108.7(5) . . ? C2 Si1 C4 106.4(5) . . ? C19' Si2 C18' 119.1(14) . . ? C19' Si2 C20 61.6(15) . . ? C18' Si2 C20 131(2) . . ? C19' Si2 C18 133.4(17) . . ? C18' Si2 C18 24.2(14) . . ? C20 Si2 C18 115.3(15) . . ? C19' Si2 C17 110.1(11) . . ? C18' Si2 C17 109.9(15) . . ? C20 Si2 C17 115.1(15) . . ? C18 Si2 C17 111.7(14) . . ? C19' Si2 C20' 105.8(13) . . ? C18' Si2 C20' 107.3(14) . . ? C20 Si2 C20' 44.3(14) . . ? C18 Si2 C20' 83.6(15) . . ? C17 Si2 C20' 103.4(14) . . ? C19' Si2 C19 46.3(12) . . ? C18' Si2 C19 80.3(14) . . ? C20 Si2 C19 105.7(13) . . ? C18 Si2 C19 102.9(12) . . ? C17 Si2 C19 104.6(10) . . ? C20' Si2 C19 146.3(15) . . ? C5 C4 Si1 176.2(9) . . ? C4 C5 C7 175.6(10) . . ? C7 C6 N1 122.8(8) . . ? C6 C7 C5 120.2(8) . . ? C6 C7 C8 118.2(8) . . ? C5 C7 C8 121.4(8) . . ? C9 C8 C7 113.2(8) . . ? C10 C9 C8 130.7(9) . . ? C9 C10 N1 115.3(8) . . ? C9 C10 C11 127.3(8) . . ? N1 C10 C11 117.3(7) . . ? C12 C11 N2 120.2(8) . . ? C12 C11 C10 126.0(8) . . ? N2 C11 C10 113.7(8) . . ? C13 C12 C11 121.5(9) . . ? C12 C13 C14 119.5(9) . . ? C15 C14 C13 118.6(9) . . ? C15 C14 C16 120.7(9) . . ? C13 C14 C16 120.6(8) . . ? N2 C15 C14 120.7(9) . . ? C17 C16 C14 172.3(11) . . ? C16 C17 Si2 173.4(10) . . ? C22 C21 Pt1 171.1(8) . . ? C21 C22 C24 174.4(10) . . ? C24 C23 N5 121.4(10) . . ? C23 C24 C25 115.3(9) . . ? C23 C24 C22 124.8(9) . . ? C25 C24 C22 119.8(9) . . ? C26 C25 C24 123.1(9) . . ? C25 C26 C27 121.1(9) . . ? C26 C27 N5 120.9(9) . . ? C26 C27 C28 118.3(9) . . ? N5 C27 C28 120.8(9) . . ? C29 C28 N6 121.6(10) . . ? C29 C28 C27 117.8(9) . . ? N6 C28 C27 120.6(10) . . ? C28 C29 C32 119.3(10) . . ? C31 C30 N6 122.3(11) . . ? C32 C31 C30 117.1(11) . . ? C29 C32 C31 123.1(12) . . ? C34 C33 Pt1 172.9(8) . . ? C33 C34 C36 176.2(10) . . ? N3 C35 C36 126.4(10) . . ? C35 C36 C37 115.2(9) . . ? C35 C36 C34 121.4(9) . . ? C37 C36 C34 123.3(9) . . ? C36 C37 C38 121.8(11) . . ? C37 C38 C39 117.8(10) . . ? N3 C39 C38 122.5(9) . . ? N3 C39 C40 115.8(9) . . ? C38 C39 C40 121.7(10) . . ? N4 C40 C41 120.0(12) . . ? N4 C40 C39 116.5(10) . . ? C41 C40 C39 123.1(10) . . ? C40 C41 C42 122.4(12) . . ? C43 C42 C41 117.5(14) . . ? C44 C43 C42 118.3(15) . . ? N4 C44 C43 124.8(15) . . ? C10 N1 C6 119.3(7) . . ? C10 N1 Pt1 114.2(5) . . ? C6 N1 Pt1 126.3(6) . . ? C15 N2 C11 119.0(8) . . ? C15 N2 Pt1 125.9(6) . . ? C11 N2 Pt1 115.1(6) . . ? C35 N3 C39 116.2(9) . . ? C40 N4 C44 116.9(13) . . ? C27 N5 C23 118.1(10) . . ? C30 N6 C28 116.5(11) . . ? Cl01 C01 Cl02 111.1(6) . . ? Cl01 C01 Cl03 109.8(6) . . ? Cl02 C01 Cl03 110.6(6) . . ? Cl5 C02 Cl4 111.1(9) . . ? Cl5 C02 Cl6 111.4(9) . . ? Cl4 C02 Cl6 111.0(9) . . ? Cl5' C02' Cl4' 111.1(9) . . ? Cl5' C02' Cl6' 111.4(9) . . ? Cl4' C02' Cl6' 111.2(9) . . ? 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 C31 H31A N4 0.93 2.62 3.495(18) 157.0 3_455 C19 H19C Cl03 0.96 2.94 3.68(3) 134.5 2_656 C01 H01A Cg1 0.98 2.74 3.471 131.8 1_555 C01 H01A Cg2 0.98 2.78 3.513 128.8 1_555 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.456 _refine_diff_density_min -2.180 _refine_diff_density_rms 0.142 # Attachment 'CCDC 710901.CIF' data_1.CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 710901' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H40 Cl2 N6 Pt Si2' _chemical_formula_weight 987.00 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' H H 0.0000 0.0000 '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 10.871(2) _cell_length_b 13.0950(10) _cell_length_c 16.6330(10) _cell_angle_alpha 110.080(10) _cell_angle_beta 95.310(10) _cell_angle_gamma 98.440(10) _cell_volume 2173.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6221 _cell_measurement_theta_min 2.4898 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 3.445 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.712 _exptl_absorpt_correction_T_min 0.558 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type Saturn70 _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16765 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9783 _reflns_number_gt 8682 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0380P)^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 9783 _refine_ls_number_parameters 511 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.003 _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 0.253843(11) 0.987686(9) 1.001098(7) 0.03741(5) Uani 1 1 d . . . Si1 Si 0.85369(10) 1.23827(8) 1.37341(6) 0.0500(2) Uani 1 1 d . . . Si2 Si -0.29397(10) 1.01844(9) 0.65054(7) 0.0538(3) Uani 1 1 d . . . N1 N 0.3828(3) 1.1323(2) 1.06635(16) 0.0357(6) Uani 1 1 d . . . N2 N 0.1777(3) 1.0969(2) 0.95668(16) 0.0379(6) Uani 1 1 d . . . N3 N 0.6809(3) 0.8468(2) 1.23382(18) 0.0490(7) Uani 1 1 d . . . N4 N 0.7453(3) 0.5958(2) 1.25626(19) 0.0542(7) Uani 1 1 d . . . N5 N -0.2739(3) 0.6969(2) 0.74068(19) 0.0501(7) Uani 1 1 d . . . N6 N -0.4164(3) 0.4073(3) 0.6355(3) 0.0711(10) Uani 1 1 d . . . C1 C 0.4840(3) 1.1432(3) 1.12259(19) 0.0426(7) Uani 1 1 d . . . H1 H 0.5024 1.0803 1.1313 0.051 Uiso 1 1 calc R . . C2 C 0.5636(3) 1.2447(3) 1.1689(2) 0.0414(7) Uani 1 1 d . . . C3 C 0.5362(3) 1.3378(3) 1.1532(2) 0.0457(8) Uani 1 1 d . . . H3 H 0.5871 1.4070 1.1828 0.055 Uiso 1 1 calc R . . C4 C 0.4336(3) 1.3265(3) 1.0941(2) 0.0451(8) Uani 1 1 d . . . H4 H 0.4161 1.3881 1.0827 0.054 Uiso 1 1 calc R . . C5 C 0.3557(3) 1.2235(2) 1.05081(19) 0.0373(7) Uani 1 1 d . . . C6 C 0.2435(3) 1.2036(2) 0.98820(19) 0.0373(7) Uani 1 1 d . . . C7 C 0.2043(3) 1.2828(3) 0.9598(2) 0.0441(8) Uani 1 1 d . . . H7 H 0.2487 1.3554 0.9830 0.053 Uiso 1 1 calc R . . C8 C 0.1005(3) 1.2552(3) 0.8976(2) 0.0436(8) Uani 1 1 d . . . H8 H 0.0759 1.3085 0.8777 0.052 Uiso 1 1 calc R . . C9 C 0.0321(3) 1.1468(3) 0.8643(2) 0.0419(7) Uani 1 1 d . . . C10 C 0.0742(3) 1.0713(3) 0.8978(2) 0.0429(7) Uani 1 1 d . . . H10 H 0.0279 0.9995 0.8781 0.052 Uiso 1 1 calc R . . C11 C 0.6638(3) 1.2482(3) 1.2325(2) 0.0456(8) Uani 1 1 d . . . C12 C 0.7429(4) 1.2470(3) 1.2867(2) 0.0505(8) Uani 1 1 d . . . C13 C 0.9858(4) 1.3569(4) 1.4068(3) 0.0812(14) Uani 1 1 d . . . H13A H 1.0271 1.3555 1.3579 0.122 Uiso 1 1 calc R . . H13B H 1.0446 1.3525 1.4516 0.122 Uiso 1 1 calc R . . H13C H 0.9546 1.4246 1.4281 0.122 Uiso 1 1 calc R . . C14 C 0.7653(5) 1.2425(6) 1.4628(3) 0.124(3) Uani 1 1 d . . . H14A H 0.7515 1.3164 1.4908 0.186 Uiso 1 1 calc R . . H14B H 0.8125 1.2208 1.5039 0.186 Uiso 1 1 calc R . . H14C H 0.6858 1.1926 1.4406 0.186 Uiso 1 1 calc R . . C15 C 0.9122(6) 1.1079(4) 1.3314(5) 0.125(3) Uani 1 1 d . . . H15A H 0.8474 1.0470 1.3269 0.188 Uiso 1 1 calc R . . H15B H 0.9846 1.1103 1.3702 0.188 Uiso 1 1 calc R . . H15C H 0.9350 1.0984 1.2753 0.188 Uiso 1 1 calc R . . C16 C -0.0751(4) 1.1101(3) 0.7980(2) 0.0463(8) Uani 1 1 d . . . C17 C -0.1612(4) 1.0763(3) 0.7401(2) 0.0535(9) Uani 1 1 d . . . C18 C -0.3733(5) 1.1317(4) 0.6446(3) 0.0864(15) Uani 1 1 d . . . H18A H -0.3983 1.1680 0.6996 0.130 Uiso 1 1 calc R . . H18B H -0.4463 1.1017 0.6007 0.130 Uiso 1 1 calc R . . H18C H -0.3165 1.1841 0.6305 0.130 Uiso 1 1 calc R . . C19 C -0.2282(5) 0.9569(4) 0.5481(3) 0.0873(15) Uani 1 1 d . . . H19A H -0.1684 1.0131 0.5402 0.131 Uiso 1 1 calc R . . H19B H -0.2952 0.9280 0.4998 0.131 Uiso 1 1 calc R . . H19C H -0.1872 0.8982 0.5518 0.131 Uiso 1 1 calc R . . C20 C -0.4020(5) 0.9117(5) 0.6740(4) 0.0925(17) Uani 1 1 d . . . H20A H -0.3599 0.8520 0.6736 0.139 Uiso 1 1 calc R . . H20B H -0.4756 0.8837 0.6306 0.139 Uiso 1 1 calc R . . H20C H -0.4262 0.9442 0.7299 0.139 Uiso 1 1 calc R . . C21 C 0.5989(4) 0.8798(3) 1.1885(2) 0.0495(9) Uani 1 1 d . . . H21 H 0.6128 0.9545 1.1960 0.059 Uiso 1 1 calc R . . C22 C 0.4934(3) 0.8115(3) 1.1305(2) 0.0439(8) Uani 1 1 d . . . C23 C 0.4773(4) 0.6996(3) 1.1202(3) 0.0583(10) Uani 1 1 d . . . H23 H 0.4098 0.6490 1.0819 0.070 Uiso 1 1 calc R . . C24 C 0.5615(3) 0.6651(3) 1.1670(3) 0.0576(10) Uani 1 1 d . . . H24 H 0.5506 0.5907 1.1604 0.069 Uiso 1 1 calc R . . C25 C 0.6620(3) 0.7391(3) 1.2236(2) 0.0405(7) Uani 1 1 d . . . C26 C 0.7584(3) 0.7044(3) 1.2712(2) 0.0416(7) Uani 1 1 d . . . C27 C 0.8605(4) 0.7794(3) 1.3257(3) 0.0660(11) Uani 1 1 d . . . H27 H 0.8678 0.8546 1.3357 0.079 Uiso 1 1 calc R . . C28 C 0.9514(4) 0.7420(4) 1.3649(3) 0.0843(15) Uani 1 1 d . . . H28 H 1.0207 0.7916 1.4020 0.101 Uiso 1 1 calc R . . C29 C 0.9392(4) 0.6305(4) 1.3490(3) 0.0684(12) Uani 1 1 d . . . H29 H 1.0004 0.6029 1.3738 0.082 Uiso 1 1 calc R . . C30 C 0.8345(4) 0.5618(3) 1.2957(3) 0.0627(10) Uani 1 1 d . . . H30 H 0.8246 0.4866 1.2862 0.075 Uiso 1 1 calc R . . C31 C 0.4096(3) 0.8552(3) 1.0844(2) 0.0462(8) Uani 1 1 d . . . C32 C 0.3431(3) 0.8987(2) 1.0494(2) 0.0407(7) Uani 1 1 d . . . C33 C -0.1710(3) 0.7595(3) 0.7954(2) 0.0492(8) Uani 1 1 d . . . H33 H -0.1624 0.8359 0.8117 0.059 Uiso 1 1 calc R . . C34 C -0.0756(3) 0.7194(3) 0.8300(2) 0.0416(7) Uani 1 1 d . . . C35 C -0.0914(4) 0.6049(3) 0.8036(2) 0.0535(9) Uani 1 1 d . . . H35 H -0.0302 0.5728 0.8235 0.064 Uiso 1 1 calc R . . C36 C -0.1973(3) 0.5392(3) 0.7483(2) 0.0507(9) Uani 1 1 d . . . H36 H -0.2083 0.4626 0.7314 0.061 Uiso 1 1 calc R . . C37 C -0.2874(3) 0.5861(3) 0.7177(2) 0.0418(7) Uani 1 1 d . . . C38 C -0.4038(3) 0.5176(3) 0.6591(2) 0.0467(8) Uani 1 1 d . . . C39 C -0.4955(4) 0.5653(3) 0.6312(2) 0.0563(9) Uani 1 1 d . . . H39 H -0.4850 0.6419 0.6486 0.068 Uiso 1 1 calc R . . C40 C -0.6028(4) 0.4988(4) 0.5775(3) 0.0712(12) Uani 1 1 d . . . H40 H -0.6657 0.5296 0.5580 0.085 Uiso 1 1 calc R . . C41 C -0.6150(4) 0.3860(4) 0.5534(3) 0.0739(13) Uani 1 1 d . . . H41 H -0.6863 0.3388 0.5170 0.089 Uiso 1 1 calc R . . C42 C -0.5218(4) 0.3450(4) 0.5834(3) 0.0822(14) Uani 1 1 d . . . H42 H -0.5313 0.2685 0.5668 0.099 Uiso 1 1 calc R . . C43 C 0.0319(3) 0.7932(3) 0.8887(2) 0.0432(7) Uani 1 1 d . . . C44 C 0.1212(3) 0.8625(2) 0.9347(2) 0.0387(7) Uani 1 1 d . . . C45 C 0.8572(4) 0.3604(3) 0.9868(3) 0.0623(10) Uani 1 1 d . . . H45A H 0.8091 0.2853 0.9652 0.075 Uiso 1 1 calc R . . H45B H 0.9432 0.3583 1.0065 0.075 Uiso 1 1 calc R . . Cl1 Cl 0.79371(11) 0.44238(9) 1.07303(7) 0.0723(3) Uani 1 1 d . . . Cl2 Cl 0.85445(12) 0.41355(11) 0.90245(9) 0.0863(4) 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 0.04338(8) 0.03276(7) 0.03563(7) 0.01421(5) -0.00207(5) 0.00649(5) Si1 0.0463(6) 0.0518(5) 0.0507(6) 0.0204(4) -0.0093(4) 0.0123(5) Si2 0.0468(6) 0.0588(6) 0.0545(6) 0.0242(5) -0.0100(5) 0.0082(5) N1 0.0400(15) 0.0329(12) 0.0325(13) 0.0124(10) -0.0022(11) 0.0057(11) N2 0.0437(16) 0.0354(13) 0.0324(13) 0.0121(10) -0.0008(11) 0.0051(11) N3 0.0508(18) 0.0375(14) 0.0535(17) 0.0134(12) -0.0076(14) 0.0096(13) N4 0.0567(19) 0.0440(16) 0.0582(18) 0.0181(13) -0.0114(15) 0.0125(14) N5 0.0475(18) 0.0405(15) 0.0597(18) 0.0177(13) -0.0005(14) 0.0066(13) N6 0.060(2) 0.0455(18) 0.091(3) 0.0125(17) -0.0169(19) 0.0050(16) C1 0.051(2) 0.0399(16) 0.0359(16) 0.0137(13) -0.0031(15) 0.0106(15) C2 0.0448(19) 0.0414(16) 0.0347(16) 0.0131(13) -0.0026(14) 0.0045(14) C3 0.050(2) 0.0397(17) 0.0423(18) 0.0152(14) -0.0048(16) -0.0005(15) C4 0.054(2) 0.0353(16) 0.0437(18) 0.0170(13) -0.0051(15) 0.0032(15) C5 0.0469(19) 0.0321(14) 0.0334(15) 0.0131(12) 0.0025(14) 0.0083(13) C6 0.0450(19) 0.0324(14) 0.0335(15) 0.0117(12) 0.0013(13) 0.0082(13) C7 0.055(2) 0.0331(15) 0.0424(17) 0.0144(13) -0.0033(15) 0.0092(14) C8 0.050(2) 0.0395(16) 0.0452(18) 0.0196(14) 0.0007(15) 0.0134(15) C9 0.0434(19) 0.0473(18) 0.0376(17) 0.0189(14) -0.0008(14) 0.0125(15) C10 0.0448(19) 0.0397(16) 0.0437(18) 0.0175(14) -0.0048(15) 0.0077(14) C11 0.047(2) 0.0422(17) 0.0422(18) 0.0120(14) -0.0036(16) 0.0074(15) C12 0.051(2) 0.0500(19) 0.0456(19) 0.0136(15) -0.0049(17) 0.0114(17) C13 0.085(3) 0.078(3) 0.061(3) 0.021(2) -0.020(2) -0.011(3) C14 0.070(3) 0.243(8) 0.095(4) 0.111(5) 0.006(3) 0.022(4) C15 0.116(5) 0.064(3) 0.166(6) 0.013(3) -0.045(4) 0.038(3) C16 0.048(2) 0.0454(18) 0.0492(19) 0.0233(15) -0.0015(17) 0.0115(16) C17 0.052(2) 0.053(2) 0.056(2) 0.0239(17) -0.0072(18) 0.0100(17) C18 0.083(3) 0.109(4) 0.092(4) 0.061(3) 0.003(3) 0.040(3) C19 0.084(4) 0.092(4) 0.067(3) 0.009(2) -0.003(3) 0.015(3) C20 0.075(4) 0.090(4) 0.109(4) 0.048(3) -0.011(3) -0.010(3) C21 0.052(2) 0.0362(16) 0.059(2) 0.0171(15) -0.0035(18) 0.0119(15) C22 0.047(2) 0.0413(17) 0.0485(19) 0.0218(14) 0.0005(16) 0.0136(15) C23 0.050(2) 0.0412(18) 0.078(3) 0.0253(17) -0.0186(19) 0.0011(16) C24 0.056(2) 0.0377(17) 0.080(3) 0.0316(17) -0.013(2) 0.0009(16) C25 0.0428(19) 0.0402(16) 0.0408(17) 0.0176(13) 0.0016(14) 0.0108(14) C26 0.0457(19) 0.0421(17) 0.0384(16) 0.0169(13) -0.0003(14) 0.0108(15) C27 0.068(3) 0.047(2) 0.075(3) 0.0255(19) -0.026(2) 0.0021(19) C28 0.075(3) 0.067(3) 0.095(3) 0.031(2) -0.046(3) -0.002(2) C29 0.060(3) 0.070(3) 0.074(3) 0.032(2) -0.021(2) 0.016(2) C30 0.071(3) 0.049(2) 0.068(3) 0.0243(18) -0.013(2) 0.018(2) C31 0.053(2) 0.0421(17) 0.0471(19) 0.0207(14) -0.0024(16) 0.0146(16) C32 0.0450(19) 0.0303(14) 0.0431(17) 0.0119(13) 0.0004(15) 0.0032(14) C33 0.048(2) 0.0384(17) 0.059(2) 0.0177(15) 0.0017(18) 0.0059(15) C34 0.045(2) 0.0394(16) 0.0392(17) 0.0156(13) 0.0021(15) 0.0037(14) C35 0.058(2) 0.0407(18) 0.059(2) 0.0203(16) -0.0109(18) 0.0064(16) C36 0.055(2) 0.0330(16) 0.057(2) 0.0144(14) -0.0112(17) 0.0041(15) C37 0.0449(19) 0.0384(16) 0.0411(17) 0.0135(13) 0.0062(15) 0.0075(14) C38 0.045(2) 0.0443(18) 0.0470(19) 0.0126(14) 0.0048(16) 0.0067(15) C39 0.055(2) 0.050(2) 0.057(2) 0.0117(16) -0.0013(18) 0.0127(18) C40 0.058(3) 0.074(3) 0.072(3) 0.019(2) -0.009(2) 0.014(2) C41 0.052(3) 0.070(3) 0.075(3) 0.007(2) -0.011(2) -0.005(2) C42 0.069(3) 0.047(2) 0.104(4) 0.008(2) -0.021(3) 0.001(2) C43 0.048(2) 0.0385(16) 0.0421(18) 0.0168(13) 0.0024(15) 0.0037(15) C44 0.0441(19) 0.0338(15) 0.0391(16) 0.0149(13) 0.0015(14) 0.0094(14) C45 0.067(3) 0.054(2) 0.072(3) 0.0295(19) 0.012(2) 0.0144(19) Cl1 0.0704(7) 0.0714(7) 0.0753(7) 0.0243(5) 0.0118(6) 0.0190(5) Cl2 0.0820(8) 0.1065(9) 0.0972(9) 0.0664(8) 0.0212(7) 0.0230(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C44 1.937(3) . ? Pt1 C32 1.943(3) . ? Pt1 N2 2.058(3) . ? Pt1 N1 2.063(3) . ? Si1 C14 1.833(5) . ? Si1 C12 1.837(4) . ? Si1 C15 1.841(5) . ? Si1 C13 1.841(4) . ? Si2 C17 1.839(4) . ? Si2 C18 1.847(5) . ? Si2 C20 1.861(5) . ? Si2 C19 1.875(4) . ? N1 C1 1.333(4) . ? N1 C5 1.372(4) . ? N2 C10 1.341(4) . ? N2 C6 1.369(4) . ? N3 C21 1.327(4) . ? N3 C25 1.344(4) . ? N4 C30 1.333(5) . ? N4 C26 1.340(4) . ? N5 C33 1.335(4) . ? N5 C37 1.349(4) . ? N6 C42 1.336(5) . ? N6 C38 1.343(5) . ? C1 C2 1.394(4) . ? C1 H1 0.9300 . ? C2 C3 1.398(5) . ? C2 C11 1.430(5) . ? C3 C4 1.372(5) . ? C3 H3 0.9300 . ? C4 C5 1.394(4) . ? C4 H4 0.9300 . ? C5 C6 1.458(4) . ? C6 C7 1.381(4) . ? C7 C8 1.371(5) . ? C7 H7 0.9300 . ? C8 C9 1.396(5) . ? C8 H8 0.9300 . ? C9 C10 1.400(4) . ? C9 C16 1.429(5) . ? C10 H10 0.9300 . ? C11 C12 1.193(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.191(5) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.395(5) . ? C21 H21 0.9300 . ? C22 C23 1.397(5) . ? C22 C31 1.439(5) . ? C23 C24 1.372(5) . ? C23 H23 0.9300 . ? C24 C25 1.375(5) . ? C24 H24 0.9300 . ? C25 C26 1.471(4) . ? C26 C27 1.379(5) . ? C27 C28 1.374(6) . ? C27 H27 0.9300 . ? C28 C29 1.375(6) . ? C28 H28 0.9300 . ? C29 C30 1.362(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.207(5) . ? C33 C34 1.393(5) . ? C33 H33 0.9300 . ? C34 C35 1.388(4) . ? C34 C43 1.436(5) . ? C35 C36 1.372(5) . ? C35 H35 0.9300 . ? C36 C37 1.376(5) . ? C36 H36 0.9300 . ? C37 C38 1.481(5) . ? C38 C39 1.375(5) . ? C39 C40 1.376(5) . ? C39 H39 0.9300 . ? C40 C41 1.374(6) . ? C40 H40 0.9300 . ? C41 C42 1.347(6) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.216(5) . ? C45 Cl1 1.741(4) . ? C45 Cl2 1.767(4) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? 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 C44 Pt1 C32 92.65(13) . . ? C44 Pt1 N2 94.14(12) . . ? C32 Pt1 N2 173.15(11) . . ? C44 Pt1 N1 173.16(11) . . ? C32 Pt1 N1 94.18(12) . . ? N2 Pt1 N1 79.04(10) . . ? C14 Si1 C12 106.4(2) . . ? C14 Si1 C15 111.8(4) . . ? C12 Si1 C15 108.6(2) . . ? C14 Si1 C13 111.1(3) . . ? C12 Si1 C13 109.0(2) . . ? C15 Si1 C13 109.9(3) . . ? C17 Si2 C18 108.7(2) . . ? C17 Si2 C20 107.4(2) . . ? C18 Si2 C20 111.3(3) . . ? C17 Si2 C19 107.6(2) . . ? C18 Si2 C19 110.1(2) . . ? C20 Si2 C19 111.7(3) . . ? C1 N1 C5 119.5(3) . . ? C1 N1 Pt1 125.6(2) . . ? C5 N1 Pt1 114.8(2) . . ? C10 N2 C6 118.3(3) . . ? C10 N2 Pt1 125.8(2) . . ? C6 N2 Pt1 115.8(2) . . ? C21 N3 C25 118.0(3) . . ? C30 N4 C26 118.0(3) . . ? C33 N5 C37 117.6(3) . . ? C42 N6 C38 117.4(4) . . ? N1 C1 C2 123.0(3) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 117.6(3) . . ? C1 C2 C11 118.2(3) . . ? C3 C2 C11 124.1(3) . . ? C4 C3 C2 119.6(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 120.4(3) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? N1 C5 C4 119.8(3) . . ? N1 C5 C6 115.7(3) . . ? C4 C5 C6 124.5(3) . . ? N2 C6 C7 120.8(3) . . ? N2 C6 C5 114.5(3) . . ? C7 C6 C5 124.7(3) . . ? C8 C7 C6 120.6(3) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 119.7(3) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C8 C9 C10 117.0(3) . . ? C8 C9 C16 123.5(3) . . ? C10 C9 C16 119.5(3) . . ? N2 C10 C9 123.6(3) . . ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? C12 C11 C2 176.3(4) . . ? C11 C12 Si1 175.0(4) . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C9 176.8(4) . . ? C16 C17 Si2 177.7(3) . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 125.3(3) . . ? N3 C21 H21 117.3 . . ? C22 C21 H21 117.3 . . ? C21 C22 C23 115.4(3) . . ? C21 C22 C31 121.2(3) . . ? C23 C22 C31 123.4(3) . . ? C24 C23 C22 119.6(3) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 120.8(3) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? N3 C25 C24 120.9(3) . . ? N3 C25 C26 116.5(3) . . ? C24 C25 C26 122.5(3) . . ? N4 C26 C27 121.5(3) . . ? N4 C26 C25 116.9(3) . . ? C27 C26 C25 121.6(3) . . ? C28 C27 C26 119.3(4) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C27 C28 C29 119.5(4) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C30 C29 C28 117.7(4) . . ? C30 C29 H29 121.1 . . ? C28 C29 H29 121.1 . . ? N4 C30 C29 124.0(4) . . ? N4 C30 H30 118.0 . . ? C29 C30 H30 118.0 . . ? C32 C31 C22 175.8(4) . . ? C31 C32 Pt1 171.9(3) . . ? N5 C33 C34 125.1(3) . . ? N5 C33 H33 117.4 . . ? C34 C33 H33 117.4 . . ? C35 C34 C33 115.8(3) . . ? C35 C34 C43 123.0(3) . . ? C33 C34 C43 121.3(3) . . ? C36 C35 C34 120.0(3) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 120.3(3) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? N5 C37 C36 121.2(3) . . ? N5 C37 C38 117.1(3) . . ? C36 C37 C38 121.7(3) . . ? N6 C38 C39 121.7(3) . . ? N6 C38 C37 117.0(3) . . ? C39 C38 C37 121.4(3) . . ? C38 C39 C40 119.6(4) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C41 C40 C39 118.5(4) . . ? C41 C40 H40 120.8 . . ? C39 C40 H40 120.8 . . ? C42 C41 C40 118.8(4) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? N6 C42 C41 124.1(4) . . ? N6 C42 H42 117.9 . . ? C41 C42 H42 117.9 . . ? C44 C43 C34 174.0(4) . . ? C43 C44 Pt1 171.6(3) . . ? Cl1 C45 Cl2 110.6(2) . . ? Cl1 C45 H45A 109.5 . . ? Cl2 C45 H45A 109.5 . . ? Cl1 C45 H45B 109.5 . . ? Cl2 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? 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 C3 H3 N4 0.93 2.62 3.546(5) 174.8 1_565 C23 H23 Cl2 0.93 2.93 3.625(4) 132.6 2_667 C45 H45A Cg1 0.97 2.58 3.502 158.8 2_667 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.455 _refine_diff_density_min -1.306 _refine_diff_density_rms 0.086 # Attachment 'CCDC-710902.cif' data_1.Ethyl_Acetate _database_code_depnum_ccdc_archive 'CCDC 710902' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H42 N6 O Pt Si2' _chemical_formula_weight 946.13 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/n' _symmetry_space_group_name_Hall '-P 2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 21.954(15) _cell_length_b 7.210(4) _cell_length_c 28.56(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.360(10) _cell_angle_gamma 90.00 _cell_volume 4380(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8341 _cell_measurement_theta_min 3.0151 _cell_measurement_theta_max 27.3910 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.0500 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 3.299 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.852 _exptl_absorpt_correction_T_min 0.818 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31762 _diffrn_reflns_av_R_equivalents 0.1064 _diffrn_reflns_av_sigmaI/netI 0.1151 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.40 _reflns_number_total 9799 _reflns_number_gt 6955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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. The unassigned maximum residual density (3.00 e \%A^-3^) is at 1.36 \%A from C3, the minimum density (-1.60 e \%A^-3^) at 1.32\%A from Pt1. The solvate are disordered and are modelled using anisotropic temperature factors. Constraints on the solvent are given below in SHELX format. flat O1 > c04 dfix 1.5 0.008 c01 c02 dfix 1.20 0.008 c02 o1 dfix 1.35 0.008 C02 o2 dfix 1.41 0.008 o2 c03 dfix 1.51 0.008 c03 c04 dang 2.3 0.01 o2 c04 simu 0.01 o1 > c04 delu O1 > C04 ; _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^)+(0.0418P)^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 9799 _refine_ls_number_parameters 538 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.1028 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1579 _refine_ls_wR_factor_gt 0.1386 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 0.453028(13) 0.29516(5) 0.501327(11) 0.03732(12) Uani 1 1 d . . . Si1 Si 0.43033(12) 0.5280(4) 0.79214(10) 0.0554(7) Uani 1 1 d . . . Si2 Si 0.73167(11) 0.0441(4) 0.35655(9) 0.0521(7) Uani 1 1 d . . . N1 N 0.5461(3) 0.2164(9) 0.5068(3) 0.0401(16) Uani 1 1 d . . . N2 N 0.4895(3) 0.3073(9) 0.5750(3) 0.0371(16) Uani 1 1 d . . . N3 N 0.3337(4) 0.2444(16) 0.2561(3) 0.085(3) Uani 1 1 d . . . N4 N 0.4093(4) 0.0602(13) 0.1639(3) 0.079(3) Uani 1 1 d . . . N5 N 0.1510(4) 0.6155(14) 0.4582(3) 0.072(2) Uani 1 1 d . . . N6 N 0.0498(4) 0.6761(13) 0.5466(4) 0.076(3) Uani 1 1 d . . . C1 C 0.6841(4) 0.0690(14) 0.4012(3) 0.052(2) Uani 1 1 d . . . C2 C 0.6577(4) 0.0925(13) 0.4338(3) 0.047(2) Uani 1 1 d . . . C3 C 0.6336(4) 0.1248(11) 0.4738(3) 0.0359(18) Uani 1 1 d . . . C4 C 0.6702(3) 0.1177(12) 0.5221(3) 0.044(2) Uani 1 1 d . . . H4 H 0.7125 0.0856 0.5277 0.053 Uiso 1 1 calc R . . C5 C 0.6457(4) 0.1569(13) 0.5616(3) 0.048(2) Uani 1 1 d . . . H5 H 0.6702 0.1474 0.5932 0.058 Uiso 1 1 calc R . . C6 C 0.5827(4) 0.2109(12) 0.5516(3) 0.0403(19) Uani 1 1 d . . . C7 C 0.5698(4) 0.1769(11) 0.4684(3) 0.041(2) Uani 1 1 d . . . H7 H 0.5434 0.1842 0.4375 0.049 Uiso 1 1 calc R . . C8 C 0.5525(3) 0.2625(11) 0.5913(3) 0.0398(19) Uani 1 1 d . . . C9 C 0.5838(4) 0.2686(13) 0.6396(3) 0.051(2) Uani 1 1 d . . . H9 H 0.6262 0.2377 0.6490 0.061 Uiso 1 1 calc R . . C10 C 0.5529(4) 0.3201(14) 0.6739(3) 0.057(3) Uani 1 1 d . . . H10 H 0.5733 0.3207 0.7066 0.069 Uiso 1 1 calc R . . C11 C 0.4882(4) 0.3726(13) 0.6577(3) 0.043(2) Uani 1 1 d . . . C12 C 0.4591(4) 0.3640(12) 0.6090(3) 0.043(2) Uani 1 1 d . . . H12 H 0.4170 0.3981 0.5988 0.052 Uiso 1 1 calc R . . C13 C 0.4575(4) 0.4325(14) 0.6954(3) 0.053(2) Uani 1 1 d . . . C14 C 0.4405(4) 0.4778(14) 0.7312(3) 0.050(2) Uani 1 1 d . . . C15 C 0.4267(3) 0.2701(11) 0.4315(3) 0.0365(18) Uani 1 1 d . . . C16 C 0.4168(4) 0.2506(13) 0.3873(3) 0.049(2) Uani 1 1 d . . . C17 C 0.4047(4) 0.2221(14) 0.3364(3) 0.052(2) Uani 1 1 d . . . C18 C 0.3465(4) 0.2696(17) 0.3051(4) 0.072(3) Uani 1 1 d . . . H18 H 0.3155 0.3203 0.3183 0.086 Uiso 1 1 calc R . . C19 C 0.4503(5) 0.1508(15) 0.3140(4) 0.064(3) Uani 1 1 d . . . H19 H 0.4899 0.1190 0.3327 0.077 Uiso 1 1 calc R . . C20 C 0.3786(4) 0.1730(14) 0.2364(3) 0.055(3) Uani 1 1 d . . . C21 C 0.3615(5) 0.1415(13) 0.1826(3) 0.052(2) Uani 1 1 d . . . C23 C 0.4363(4) 0.1279(14) 0.2646(3) 0.051(2) Uani 1 1 d . . . H23 H 0.4668 0.0811 0.2503 0.061 Uiso 1 1 calc R . . C25 C 0.3037(4) 0.1918(14) 0.1552(3) 0.055(2) Uani 1 1 d . . . H25 H 0.2743 0.2464 0.1693 0.066 Uiso 1 1 calc R . . C26 C 0.2903(6) 0.1607(16) 0.1072(4) 0.071(3) Uani 1 1 d . . . H26 H 0.2508 0.1930 0.0884 0.085 Uiso 1 1 calc R . . C28 C 0.2123(3) 0.5510(13) 0.4585(3) 0.048(2) Uani 1 1 d . . . H28 H 0.2256 0.5509 0.4300 0.057 Uiso 1 1 calc R . . C32 C 0.2292(4) 0.4967(13) 0.5438(3) 0.047(2) Uani 1 1 d . . . H32 H 0.2550 0.4551 0.5728 0.057 Uiso 1 1 calc R . . C33 C 0.1718(3) 0.5625(11) 0.5439(3) 0.0386(19) Uani 1 1 d . . . H33 H 0.1587 0.5679 0.5724 0.046 Uiso 1 1 calc R . . C34 C 0.1339(4) 0.6198(12) 0.5022(3) 0.044(2) Uani 1 1 d . . . C35 C 0.0690(4) 0.6867(11) 0.5018(3) 0.044(2) Uani 1 1 d . . . C36 C 0.0329(3) 0.7494(11) 0.4609(3) 0.0363(18) Uani 1 1 d . . . H36 H 0.0479 0.7553 0.4332 0.044 Uiso 1 1 calc R . . C37 C -0.0260(4) 0.8048(13) 0.4598(4) 0.058(3) Uani 1 1 d . . . H37 H -0.0510 0.8512 0.4310 0.069 Uiso 1 1 calc R . . C39 C -0.0129(4) 0.7317(12) 0.5428(4) 0.055(3) Uani 1 1 d . . . H39 H -0.0291 0.7255 0.5699 0.065 Uiso 1 1 calc R . . C60 C 0.3614(5) 0.3959(18) 0.8023(4) 0.087(4) Uani 1 1 d . . . H60A H 0.3236 0.4391 0.7802 0.131 Uiso 1 1 calc R . . H60B H 0.3583 0.4146 0.8349 0.131 Uiso 1 1 calc R . . H60C H 0.3668 0.2662 0.7969 0.131 Uiso 1 1 calc R . . C61 C 0.4168(5) 0.7817(16) 0.7981(4) 0.079(4) Uani 1 1 d . . . H61A H 0.4510 0.8501 0.7910 0.119 Uiso 1 1 calc R . . H61B H 0.4144 0.8086 0.8305 0.119 Uiso 1 1 calc R . . H61C H 0.3781 0.8170 0.7758 0.119 Uiso 1 1 calc R . . C62 C 0.5055(5) 0.4512(17) 0.8350(4) 0.081(3) Uani 1 1 d . . . H62A H 0.5148 0.3262 0.8275 0.122 Uiso 1 1 calc R . . H62B H 0.5010 0.4566 0.8675 0.122 Uiso 1 1 calc R . . H62C H 0.5391 0.5314 0.8318 0.122 Uiso 1 1 calc R . . C63 C 0.8130(4) -0.0241(15) 0.3901(4) 0.064(3) Uani 1 1 d . . . H63A H 0.8110 -0.1324 0.4093 0.095 Uiso 1 1 calc R . . H63B H 0.8320 0.0758 0.4109 0.095 Uiso 1 1 calc R . . H63C H 0.8377 -0.0507 0.3675 0.095 Uiso 1 1 calc R . . C64 C 0.7320(5) 0.2751(15) 0.3261(4) 0.069(3) Uani 1 1 d . . . H64A H 0.7504 0.2617 0.2991 0.104 Uiso 1 1 calc R . . H64B H 0.7561 0.3622 0.3487 0.104 Uiso 1 1 calc R . . H64C H 0.6896 0.3193 0.3149 0.104 Uiso 1 1 calc R . . C65 C 0.6953(5) -0.1411(17) 0.3131(4) 0.083(4) Uani 1 1 d . . . H65A H 0.6985 -0.2579 0.3296 0.125 Uiso 1 1 calc R . . H65B H 0.7170 -0.1487 0.2877 0.125 Uiso 1 1 calc R . . H65C H 0.6519 -0.1122 0.2994 0.125 Uiso 1 1 calc R . . C106 C -0.0508(4) 0.7955(12) 0.4995(4) 0.052(3) Uani 1 1 d . . . H106 H -0.0921 0.8313 0.4974 0.063 Uiso 1 1 calc R . . C107 C 0.3925(5) 0.0332(16) 0.1137(4) 0.070(3) Uani 1 1 d . . . H107 H 0.4218 -0.0192 0.0990 0.084 Uiso 1 1 calc R . . C108 C 0.3337(6) 0.0818(16) 0.0852(4) 0.074(3) Uani 1 1 d . . . H108 H 0.3236 0.0619 0.0520 0.089 Uiso 1 1 calc R . . C150 C 0.2527(3) 0.4875(13) 0.5016(3) 0.044(2) Uani 1 1 d . . . C151 C 0.3147(4) 0.4182(12) 0.5031(3) 0.0418(19) Uani 1 1 d . . . C152 C 0.3671(4) 0.3693(13) 0.5012(3) 0.047(2) Uani 1 1 d . . . O1 O 0.2384(8) 0.714(3) 0.1723(8) 0.124(4) Uani 0.50 1 d PDU A -1 O2 O 0.2890(10) 0.723(2) 0.2476(9) 0.120(4) Uani 0.50 1 d PDU A -1 C01 C 0.3503(11) 0.662(4) 0.1903(11) 0.118(5) Uani 0.50 1 d PDU A -1 H01A H 0.3446 0.6404 0.1563 0.177 Uiso 0.50 1 calc PR A -1 H01B H 0.3693 0.5545 0.2080 0.177 Uiso 0.50 1 calc PR A -1 H01C H 0.3770 0.7674 0.1999 0.177 Uiso 0.50 1 calc PR A -1 C02 C 0.2881(9) 0.697(3) 0.2007(9) 0.119(4) Uani 0.50 1 d PDU A -1 C03 C 0.2266(10) 0.764(3) 0.2503(11) 0.122(4) Uani 0.50 1 d PDU A -1 H03A H 0.1977 0.6675 0.2352 0.146 Uiso 0.50 1 calc PR A -1 H03C H 0.2125 0.8818 0.2348 0.146 Uiso 0.50 1 calc PR A -1 C04 C 0.2318(13) 0.773(4) 0.3038(11) 0.123(5) Uani 0.50 1 d PDU A -1 H04D H 0.1912 0.8003 0.3092 0.185 Uiso 0.50 1 calc PR A -1 H04A H 0.2609 0.8693 0.3179 0.185 Uiso 0.50 1 calc PR A -1 H04B H 0.2465 0.6564 0.3183 0.185 Uiso 0.50 1 calc PR A -1 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 0.03258(17) 0.0358(2) 0.0463(2) -0.00091(15) 0.01502(14) 0.00123(14) Si1 0.0533(14) 0.064(2) 0.0546(15) -0.0060(14) 0.0233(13) 0.0000(14) Si2 0.0454(13) 0.0607(19) 0.0560(15) -0.0040(13) 0.0235(12) 0.0011(13) N1 0.039(4) 0.033(4) 0.053(4) -0.001(3) 0.019(3) -0.003(3) N2 0.031(3) 0.028(4) 0.059(4) 0.008(3) 0.023(3) 0.000(3) N3 0.057(5) 0.139(10) 0.060(6) -0.011(6) 0.014(5) -0.003(6) N4 0.097(7) 0.074(7) 0.083(6) -0.014(5) 0.055(6) -0.019(6) N5 0.056(5) 0.077(7) 0.081(6) 0.001(5) 0.014(5) -0.001(5) N6 0.064(5) 0.064(7) 0.113(8) -0.004(5) 0.046(6) 0.002(5) C1 0.045(4) 0.055(6) 0.062(6) -0.001(5) 0.021(4) -0.002(4) C2 0.037(4) 0.053(6) 0.054(5) -0.002(4) 0.017(4) 0.001(4) C3 0.048(4) 0.018(4) 0.050(5) -0.001(3) 0.029(4) 0.004(3) C4 0.028(4) 0.044(5) 0.058(5) 0.004(4) 0.007(4) 0.004(4) C5 0.045(4) 0.054(6) 0.050(5) 0.009(4) 0.021(4) 0.012(4) C6 0.032(4) 0.043(5) 0.051(5) 0.002(4) 0.021(4) 0.005(4) C7 0.044(4) 0.036(5) 0.050(5) -0.003(4) 0.026(4) -0.003(4) C8 0.030(4) 0.035(5) 0.053(5) 0.004(4) 0.008(4) 0.002(3) C9 0.035(4) 0.068(7) 0.054(5) -0.006(5) 0.019(4) 0.001(4) C10 0.050(5) 0.080(8) 0.041(5) 0.003(5) 0.012(4) -0.003(5) C11 0.039(4) 0.041(5) 0.053(5) -0.007(4) 0.021(4) -0.008(4) C12 0.039(4) 0.039(5) 0.057(5) 0.001(4) 0.022(4) 0.001(4) C13 0.042(4) 0.063(7) 0.059(6) 0.008(5) 0.020(4) -0.004(4) C14 0.044(4) 0.069(7) 0.044(5) -0.006(4) 0.021(4) -0.003(5) C15 0.031(4) 0.028(4) 0.050(5) 0.000(4) 0.010(4) -0.003(3) C16 0.044(5) 0.054(6) 0.049(5) -0.004(4) 0.012(4) -0.003(4) C17 0.043(5) 0.062(7) 0.055(6) -0.006(5) 0.019(4) -0.003(5) C18 0.043(5) 0.123(11) 0.052(6) -0.020(6) 0.017(5) 0.012(6) C19 0.059(6) 0.068(8) 0.072(7) -0.006(6) 0.030(5) 0.000(5) C20 0.056(5) 0.065(7) 0.048(5) -0.015(5) 0.019(5) -0.018(5) C21 0.070(6) 0.042(6) 0.048(5) -0.014(4) 0.022(5) -0.020(5) C23 0.056(5) 0.059(6) 0.049(5) -0.008(5) 0.032(5) -0.006(5) C25 0.054(5) 0.063(7) 0.048(5) 0.002(5) 0.014(5) 0.002(5) C26 0.087(8) 0.078(9) 0.047(6) -0.016(5) 0.015(6) -0.018(7) C28 0.035(4) 0.053(6) 0.060(5) 0.005(4) 0.020(4) 0.012(4) C32 0.041(4) 0.048(6) 0.049(5) 0.006(4) 0.005(4) 0.005(4) C33 0.032(4) 0.040(5) 0.046(4) 0.010(4) 0.015(3) 0.010(4) C34 0.038(4) 0.030(5) 0.068(6) -0.002(4) 0.020(4) 0.005(4) C35 0.036(4) 0.030(5) 0.075(6) -0.002(4) 0.027(4) -0.002(4) C36 0.030(4) 0.036(5) 0.044(4) 0.003(4) 0.009(3) 0.005(3) C37 0.043(5) 0.051(6) 0.077(7) 0.009(5) 0.010(5) 0.004(4) C39 0.055(5) 0.033(5) 0.088(7) -0.008(5) 0.042(6) 0.001(4) C60 0.100(8) 0.100(10) 0.085(8) -0.029(7) 0.067(7) -0.044(8) C61 0.071(7) 0.089(10) 0.085(8) -0.029(7) 0.036(7) 0.005(6) C62 0.095(8) 0.082(9) 0.069(7) -0.003(6) 0.024(7) 0.010(7) C63 0.047(5) 0.069(8) 0.077(7) -0.007(6) 0.019(5) 0.009(5) C64 0.069(7) 0.075(8) 0.073(7) 0.005(6) 0.036(6) 0.004(6) C65 0.071(7) 0.085(9) 0.095(9) -0.036(7) 0.022(7) -0.032(7) C106 0.034(4) 0.033(5) 0.096(8) -0.001(5) 0.026(5) 0.000(4) C107 0.084(7) 0.076(8) 0.062(6) -0.018(6) 0.041(6) -0.027(7) C108 0.110(9) 0.067(8) 0.053(6) -0.014(6) 0.034(7) -0.026(7) C150 0.028(3) 0.055(6) 0.048(5) -0.010(4) 0.008(3) 0.004(4) C151 0.048(4) 0.030(5) 0.050(5) -0.001(4) 0.017(4) 0.001(4) C152 0.044(4) 0.041(5) 0.058(5) 0.005(4) 0.018(4) -0.001(4) O1 0.089(8) 0.136(10) 0.144(9) 0.041(10) 0.022(8) 0.013(8) O2 0.088(8) 0.131(9) 0.140(9) 0.034(10) 0.028(8) 0.037(7) C01 0.092(8) 0.127(11) 0.135(10) 0.037(11) 0.030(8) 0.026(9) C02 0.088(8) 0.129(9) 0.139(9) 0.038(10) 0.027(8) 0.031(7) C03 0.089(8) 0.132(9) 0.142(9) 0.033(10) 0.026(8) 0.041(8) C04 0.091(10) 0.133(11) 0.143(9) 0.024(11) 0.025(9) 0.057(9) _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 C15 1.942(9) . ? Pt1 C152 1.959(8) . ? Pt1 N2 2.058(7) . ? Pt1 N1 2.089(6) . ? Si1 C14 1.845(8) . ? Si1 C61 1.868(11) . ? Si1 C60 1.871(10) . ? Si1 C62 1.878(11) . ? Si2 C1 1.846(8) . ? Si2 C65 1.863(10) . ? Si2 C63 1.871(9) . ? Si2 C64 1.879(11) . ? N1 C6 1.333(10) . ? N1 C7 1.355(9) . ? N2 C12 1.371(9) . ? N2 C8 1.384(9) . ? N3 C20 1.351(12) . ? N3 C18 1.370(13) . ? N4 C107 1.401(13) . ? N4 C21 1.418(12) . ? N5 C34 1.399(11) . ? N5 C28 1.422(10) . ? N6 C39 1.412(11) . ? N6 C35 1.444(12) . ? C1 C2 1.224(11) . ? C2 C3 1.392(10) . ? C3 C4 1.416(11) . ? C3 C7 1.421(10) . ? C4 C5 1.395(11) . ? C4 H4 0.9300 . ? C5 C6 1.398(10) . ? C5 H5 0.9300 . ? C6 C8 1.493(11) . ? C7 H7 0.9300 . ? C8 C9 1.381(12) . ? C9 C10 1.376(11) . ? C9 H9 0.9300 . ? C10 C11 1.430(12) . ? C10 H10 0.9300 . ? C11 C12 1.380(11) . ? C11 C13 1.471(11) . ? C12 H12 0.9300 . ? C13 C14 1.218(11) . ? C15 C16 1.236(11) . ? C16 C17 1.426(12) . ? C17 C18 1.408(13) . ? C17 C19 1.411(12) . ? C18 H18 0.9300 . ? C19 C23 1.376(12) . ? C19 H19 0.9300 . ? C20 C23 1.361(13) . ? C20 C21 1.507(12) . ? C21 C25 1.363(13) . ? C23 H23 0.9300 . ? C25 C26 1.346(12) . ? C25 H25 0.9300 . ? C26 C108 1.387(14) . ? C26 H26 0.9300 . ? C28 C150 1.404(11) . ? C28 H28 0.9300 . ? C32 C33 1.348(10) . ? C32 C150 1.424(11) . ? C32 H32 0.9300 . ? C33 C34 1.337(11) . ? C33 H33 0.9300 . ? C34 C35 1.501(10) . ? C35 C36 1.317(11) . ? C36 C37 1.346(11) . ? C36 H36 0.9300 . ? C37 C106 1.376(12) . ? C37 H37 0.9300 . ? C39 C106 1.386(13) . ? C39 H39 0.9300 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C106 H106 0.9300 . ? C107 C108 1.391(15) . ? C107 H107 0.9300 . ? C108 H108 0.9300 . ? C150 C151 1.440(10) . ? C151 C152 1.219(10) . ? O1 C02 1.193(8) . ? O2 C02 1.348(8) . ? O2 C03 1.421(8) . ? C01 C02 1.489(8) . ? C01 H01A 0.9600 . ? C01 H01B 0.9600 . ? C01 H01C 0.9600 . ? C03 C04 1.506(8) . ? C03 H03A 0.9700 . ? C03 H03C 0.9700 . ? C04 H04D 0.9600 . ? C04 H04A 0.9600 . ? C04 H04B 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 Pt1 C152 89.0(3) . . ? C15 Pt1 N2 173.9(3) . . ? C152 Pt1 N2 96.9(3) . . ? C15 Pt1 N1 95.0(3) . . ? C152 Pt1 N1 175.9(3) . . ? N2 Pt1 N1 79.0(3) . . ? C14 Si1 C61 109.7(5) . . ? C14 Si1 C60 109.7(4) . . ? C61 Si1 C60 109.4(5) . . ? C14 Si1 C62 105.3(4) . . ? C61 Si1 C62 111.3(5) . . ? C60 Si1 C62 111.3(6) . . ? C1 Si2 C65 108.0(5) . . ? C1 Si2 C63 107.6(4) . . ? C65 Si2 C63 110.5(5) . . ? C1 Si2 C64 107.5(5) . . ? C65 Si2 C64 112.1(6) . . ? C63 Si2 C64 110.9(5) . . ? C6 N1 C7 120.7(7) . . ? C6 N1 Pt1 115.1(5) . . ? C7 N1 Pt1 124.1(6) . . ? C12 N2 C8 116.9(7) . . ? C12 N2 Pt1 127.0(5) . . ? C8 N2 Pt1 115.9(5) . . ? C20 N3 C18 119.2(9) . . ? C107 N4 C21 114.3(10) . . ? C34 N5 C28 117.8(8) . . ? C39 N6 C35 114.2(9) . . ? C2 C1 Si2 173.7(8) . . ? C1 C2 C3 174.2(9) . . ? C2 C3 C4 123.6(7) . . ? C2 C3 C7 121.4(8) . . ? C4 C3 C7 114.9(7) . . ? C5 C4 C3 122.8(7) . . ? C5 C4 H4 118.6 . . ? C3 C4 H4 118.6 . . ? C4 C5 C6 116.9(8) . . ? C4 C5 H5 121.5 . . ? C6 C5 H5 121.5 . . ? N1 C6 C5 122.3(7) . . ? N1 C6 C8 116.5(6) . . ? C5 C6 C8 121.2(8) . . ? N1 C7 C3 122.3(8) . . ? N1 C7 H7 118.8 . . ? C3 C7 H7 118.8 . . ? C9 C8 N2 122.5(8) . . ? C9 C8 C6 124.1(7) . . ? N2 C8 C6 113.4(7) . . ? C10 C9 C8 120.7(8) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 117.7(8) . . ? C9 C10 H10 121.1 . . ? C11 C10 H10 121.1 . . ? C12 C11 C10 119.3(7) . . ? C12 C11 C13 124.7(7) . . ? C10 C11 C13 116.0(8) . . ? N2 C12 C11 122.8(7) . . ? N2 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? C14 C13 C11 170.6(9) . . ? C13 C14 Si1 168.3(8) . . ? C16 C15 Pt1 173.1(7) . . ? C15 C16 C17 178.1(10) . . ? C18 C17 C19 115.7(9) . . ? C18 C17 C16 121.4(8) . . ? C19 C17 C16 122.8(9) . . ? N3 C18 C17 122.7(9) . . ? N3 C18 H18 118.6 . . ? C17 C18 H18 118.6 . . ? C23 C19 C17 120.4(10) . . ? C23 C19 H19 119.8 . . ? C17 C19 H19 119.8 . . ? N3 C20 C23 121.0(9) . . ? N3 C20 C21 117.2(9) . . ? C23 C20 C21 121.8(9) . . ? C25 C21 N4 124.3(9) . . ? C25 C21 C20 120.4(9) . . ? N4 C21 C20 115.2(9) . . ? C20 C23 C19 120.9(8) . . ? C20 C23 H23 119.5 . . ? C19 C23 H23 119.5 . . ? C26 C25 C21 118.5(10) . . ? C26 C25 H25 120.8 . . ? C21 C25 H25 120.8 . . ? C25 C26 C108 121.9(11) . . ? C25 C26 H26 119.1 . . ? C108 C26 H26 119.1 . . ? C150 C28 N5 120.2(8) . . ? C150 C28 H28 119.9 . . ? N5 C28 H28 119.9 . . ? C33 C32 C150 123.5(8) . . ? C33 C32 H32 118.2 . . ? C150 C32 H32 118.2 . . ? C34 C33 C32 118.9(8) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C33 C34 N5 123.1(7) . . ? C33 C34 C35 119.2(8) . . ? N5 C34 C35 117.7(8) . . ? C36 C35 N6 124.0(8) . . ? C36 C35 C34 118.6(8) . . ? N6 C35 C34 117.4(8) . . ? C35 C36 C37 119.1(8) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C36 C37 C106 122.6(9) . . ? C36 C37 H37 118.7 . . ? C106 C37 H37 118.7 . . ? C106 C39 N6 121.3(9) . . ? C106 C39 H39 119.3 . . ? N6 C39 H39 119.3 . . ? Si1 C60 H60A 109.5 . . ? Si1 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? Si1 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? Si1 C61 H61A 109.5 . . ? Si1 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? Si1 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? Si1 C62 H62A 109.5 . . ? Si1 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? Si1 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? Si2 C63 H63A 109.5 . . ? Si2 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? Si2 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? Si2 C64 H64A 109.5 . . ? Si2 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? Si2 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? Si2 C65 H65A 109.5 . . ? Si2 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? Si2 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C37 C106 C39 118.7(8) . . ? C37 C106 H106 120.7 . . ? C39 C106 H106 120.7 . . ? C108 C107 N4 122.3(10) . . ? C108 C107 H107 118.9 . . ? N4 C107 H107 118.9 . . ? C26 C108 C107 118.7(10) . . ? C26 C108 H108 120.6 . . ? C107 C108 H108 120.6 . . ? C28 C150 C32 116.4(7) . . ? C28 C150 C151 121.7(7) . . ? C32 C150 C151 121.9(8) . . ? C152 C151 C150 174.6(9) . . ? C151 C152 Pt1 177.3(8) . . ? C02 O2 C03 107.8(18) . . ? C02 C01 H01A 109.5 . . ? C02 C01 H01B 109.5 . . ? H01A C01 H01B 109.5 . . ? C02 C01 H01C 109.5 . . ? H01A C01 H01C 109.5 . . ? H01B C01 H01C 109.5 . . ? O1 C02 O2 116(2) . . ? O1 C02 C01 128(2) . . ? O2 C02 C01 116(2) . . ? O2 C03 C04 103.5(8) . . ? O2 C03 H03A 111.1 . . ? C04 C03 H03A 111.1 . . ? O2 C03 H03C 111.1 . . ? C04 C03 H03C 111.1 . . ? H03A C03 H03C 109.0 . . ? C03 C04 H04D 109.5 . . ? C03 C04 H04A 109.5 . . ? H04D C04 H04A 109.5 . . ? C03 C04 H04B 109.5 . . ? H04D C04 H04B 109.5 . . ? H04A C04 H04B 109.5 . . ? 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 C5 H5 O1 0.93 2.58 3.44(3) 152.8 4_666 C9 H9 O1 0.93 2.41 3.29(3) 157.8 4_666 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 3.006 _refine_diff_density_min -1.605 _refine_diff_density_rms 0.154 # Attachment 'CCDC 710903.cif' data_1.Hexane _database_code_depnum_ccdc_archive 'CCDC 710903' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H90 N12 Pt2 Si4' _chemical_formula_weight 1890.32 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' H H 0.0000 0.0000 '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 15.104(4) _cell_length_b 15.307(4) _cell_length_c 20.785(6) _cell_angle_alpha 90.500(10) _cell_angle_beta 100.190(10) _cell_angle_gamma 110.160(10) _cell_volume 4427(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9869 _cell_measurement_theta_min 3.0839 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.6000 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1900 _exptl_absorpt_coefficient_mu 3.262 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.622 _exptl_absorpt_correction_T_min 0.559 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Saturn70 _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27972 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14881 _reflns_number_gt 12150 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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. The resolution of the collected data is approximately 0.95 \"O depending on the quality of the crystal. This crystal is difficult to grow and we have collected the structure for namy times and all of them are data completeness Constraints on the solvent are given below in SHELX format. dfix 1.21 0.008 c36 c37 dfix 1.53 0.01 C300 C301 C301 C302 C304 C305 C305 C306 dang 2.55 0.01 C304 C306 dfix 1.53 0.01 C304 C304_$1 dang 2.5 0.01 C304 C305_$1 eqiv $1 1-x, -y, 2-z simu c304 c305 c306 delu c304 c305 c306 isor c304 c305 c306 ; _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^)+(0.0470P)^2^+0.9522P] 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 14881 _refine_ls_number_parameters 1023 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.007 _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 C201 C 0.5220(8) 1.2671(8) -0.2785(6) 0.163(5) Uani 1 1 d . . . H201 H 0.5588 1.2917 -0.3099 0.195 Uiso 1 1 calc R . . C155 C 0.5577(8) 1.2941(7) -0.2127(6) 0.152(4) Uani 1 1 d . . . H155 H 0.6198 1.3366 -0.1995 0.182 Uiso 1 1 calc R . . N16 N 0.5015(6) 1.2581(6) -0.1656(4) 0.137(3) Uani 1 1 d . . . C154 C 0.4333(8) 1.2046(9) -0.2959(4) 0.182(6) Uani 1 1 d . . . H154 H 0.4091 1.1844 -0.3399 0.218 Uiso 1 1 calc R . . C153 C 0.3782(6) 1.1704(7) -0.2517(4) 0.135(4) Uani 1 1 d . . . H153 H 0.3160 1.1284 -0.2658 0.162 Uiso 1 1 calc R . . C152 C 0.4104(5) 1.1951(6) -0.1882(4) 0.090(2) Uani 1 1 d . . . C127 C 0.3532(5) 1.1548(5) -0.1378(3) 0.0757(17) Uani 1 1 d . . . N20 N 0.2673(4) 1.0853(4) -0.1587(3) 0.0906(18) Uani 1 1 d . . . C200 C 0.3850(4) 1.1818(4) -0.0747(3) 0.0726(17) Uani 1 1 d . . . H200 H 0.4432 1.2306 -0.0613 0.087 Uiso 1 1 calc R . . C128 C 0.2160(4) 1.0418(5) -0.1132(3) 0.0792(19) Uani 1 1 d . . . H128 H 0.1572 0.9943 -0.1275 0.095 Uiso 1 1 calc R . . C125 C 0.3344(5) 1.1397(5) -0.0304(3) 0.0790(18) Uani 1 1 d . . . H125 H 0.3581 1.1609 0.0135 0.095 Uiso 1 1 calc R . . C47 C 0.2475(4) 1.0654(4) -0.0467(3) 0.0634(15) Uani 1 1 d . . . C46 C 0.1946(4) 1.0156(4) -0.0002(3) 0.0601(14) Uani 1 1 d . . . C45 C 0.1465(5) 0.9713(4) 0.0368(3) 0.0672(16) Uani 1 1 d . . . Pt1 Pt 0.055703(15) 0.891656(15) 0.086919(9) 0.05420(8) Uani 1 1 d . . . C23 C 0.5639(4) 0.2904(4) 1.0743(3) 0.0693(16) Uani 1 1 d . . . H23 H 0.5077 0.2406 1.0581 0.083 Uiso 1 1 calc R . . C26 C 0.5119(5) 0.2825(5) 1.1795(3) 0.0760(17) Uani 1 1 d . . . Pt2 Pt 0.932848(15) 0.585508(15) 0.943469(9) 0.05408(8) Uani 1 1 d . . . Si2 Si -0.10963(15) 0.78540(14) 0.43552(8) 0.0796(5) Uani 1 1 d . . . Si1 Si 1.25745(14) 0.83088(17) 0.65420(10) 0.0928(6) Uani 1 1 d . . . N7 N -0.0534(3) 0.8071(3) 0.1298(2) 0.0553(11) Uani 1 1 d . . . C19 C 0.8282(4) 0.5044(5) 0.9819(3) 0.0638(15) Uani 1 1 d . . . N6 N -0.0542(3) 0.8388(3) 0.00569(19) 0.0546(11) Uani 1 1 d . . . N1 N 1.0249(3) 0.6320(3) 1.0343(2) 0.0592(12) Uani 1 1 d . . . N2 N 1.0556(3) 0.6778(3) 0.9157(2) 0.0572(11) Uani 1 1 d . . . C36 C 0.1537(4) 0.9195(5) 0.1681(3) 0.0679(16) Uani 1 1 d D . . C11 C 0.8095(4) 0.5387(4) 0.7998(3) 0.0629(15) Uani 1 1 d . . . C10 C 0.8527(4) 0.5528(4) 0.8542(3) 0.0654(15) Uani 1 1 d . . . C33 C -0.0525(4) 0.7998(4) 0.1937(2) 0.0620(15) Uani 1 1 d . . . H33 H 0.0038 0.8334 0.2228 0.074 Uiso 1 1 calc R . . C27 C -0.0468(4) 0.8602(4) -0.0562(2) 0.0542(14) Uani 1 1 d . . . H27 H 0.0081 0.9072 -0.0636 0.065 Uiso 1 1 calc R . . C7 C 1.0671(4) 0.6943(4) 0.8528(3) 0.0635(15) Uani 1 1 d . . . H7 H 1.0177 0.6627 0.8181 0.076 Uiso 1 1 calc R . . C15 C 0.6837(4) 0.5295(5) 0.6019(3) 0.0672(16) Uani 1 1 d . . . C12 C 0.7630(4) 0.5321(4) 0.7324(3) 0.0617(15) Uani 1 1 d . . . C21 C 0.7111(4) 0.4076(4) 1.0568(3) 0.0647(15) Uani 1 1 d . . . C20 C 0.7738(4) 0.4585(4) 1.0141(3) 0.0668(15) Uani 1 1 d . . . C1 C 1.0031(5) 0.6020(4) 1.0917(3) 0.0654(15) Uani 1 1 d . . . H1 H 0.9423 0.5587 1.0921 0.078 Uiso 1 1 calc R . . C25 C 0.7306(4) 0.4322(5) 1.1233(3) 0.0774(19) Uani 1 1 d . . . H25 H 0.7883 0.4791 1.1414 0.093 Uiso 1 1 calc R . . C34 C -0.1237(5) 0.7516(5) 0.2896(3) 0.0744(17) Uani 1 1 d . . . N4 N 0.6966(4) 0.6031(4) 0.6424(3) 0.0902(17) Uani 1 1 d . . . C37 C 0.2072(4) 0.9190(5) 0.2180(3) 0.0720(16) Uani 1 1 d D . . C22 C 0.6267(5) 0.3332(5) 1.0334(4) 0.087(2) Uani 1 1 d . . . H22 H 0.6121 0.3117 0.9895 0.104 Uiso 1 1 calc R . . C38 C 0.2675(4) 0.9069(4) 0.2762(3) 0.0696(16) Uani 1 1 d . . . C14 C 0.7055(4) 0.4530(4) 0.6237(3) 0.0687(15) Uani 1 1 d . . . H14 H 0.6945 0.4020 0.5949 0.082 Uiso 1 1 calc R . . C43 C 0.4500(4) 0.8633(5) 0.4417(3) 0.0690(16) Uani 1 1 d . . . N8 N 0.2945(5) 0.8202(5) 0.3684(3) 0.104(2) Uani 1 1 d . . . C35 C -0.1179(5) 0.7611(5) 0.3472(3) 0.0765(18) Uani 1 1 d . . . C16 C 0.7356(5) 0.6026(5) 0.7061(3) 0.0838(19) Uani 1 1 d . . . H16 H 0.7444 0.6539 0.7341 0.101 Uiso 1 1 calc R . . C32 C -0.1293(5) 0.7457(4) 0.2191(3) 0.0658(16) Uani 1 1 d . . . C2 C 1.1116(4) 0.6951(4) 1.0316(3) 0.0605(14) Uani 1 1 d . . . C28 C -0.1340(4) 0.7732(4) 0.0168(2) 0.0548(13) Uani 1 1 d . . . C29 C -0.1358(4) 0.7567(4) 0.0873(2) 0.0542(13) Uani 1 1 d . . . C3 C 1.1277(4) 0.7219(4) 0.9665(3) 0.0616(14) Uani 1 1 d . . . C17 C 0.6468(4) 0.5351(5) 0.5319(3) 0.0801(19) Uani 1 1 d . . . C41 C 0.4191(4) 0.9520(4) 0.3487(3) 0.0725(17) Uani 1 1 d . . . H41 H 0.4820 0.9933 0.3611 0.087 Uiso 1 1 calc R . . C13 C 0.7443(4) 0.4540(4) 0.6895(3) 0.0705(16) Uani 1 1 d . . . H13 H 0.7579 0.4025 0.7053 0.085 Uiso 1 1 calc R . . C31 C -0.2124(5) 0.6929(5) 0.1758(3) 0.0783(19) Uani 1 1 d . . . H31 H -0.2660 0.6545 0.1910 0.094 Uiso 1 1 calc R . . N5 N 0.6501(4) 0.4711(5) 0.4892(3) 0.106(2) Uani 1 1 d . . . N9 N 0.5418(5) 0.9272(5) 0.4581(3) 0.115(2) Uani 1 1 d . . . N3 N 0.6690(4) 0.3908(4) 1.1629(3) 0.0959(18) Uani 1 1 d . . . C30 C -0.2130(4) 0.6992(4) 0.1096(3) 0.0702(16) Uani 1 1 d . . . H30 H -0.2674 0.6633 0.0796 0.084 Uiso 1 1 calc R . . C24 C 0.5853(4) 0.3216(4) 1.1369(3) 0.0706(16) Uani 1 1 d . . . C42 C 0.3861(4) 0.8797(4) 0.3842(3) 0.0692(16) Uani 1 1 d . . . C6 C 1.1527(5) 0.7586(5) 0.8402(3) 0.0723(17) Uani 1 1 d . . . C40 C 0.3626(5) 0.9655(5) 0.2956(3) 0.0845(19) Uani 1 1 d . . . H40 H 0.3875 1.0154 0.2709 0.101 Uiso 1 1 calc R . . C44 C 0.4182(5) 0.7916(5) 0.4755(3) 0.093(2) Uani 1 1 d . . . H44 H 0.3553 0.7501 0.4637 0.112 Uiso 1 1 calc R . . C18 C 0.6113(5) 0.6028(6) 0.5125(3) 0.096(2) Uani 1 1 d . . . H18 H 0.6101 0.6467 0.5432 0.116 Uiso 1 1 calc R . . C39 C 0.2357(5) 0.8358(5) 0.3149(3) 0.090(2) Uani 1 1 d . . . H39 H 0.1718 0.7963 0.3046 0.108 Uiso 1 1 calc R . . C8 C 1.1700(5) 0.7743(5) 0.7745(3) 0.0795(18) Uani 1 1 d . . . C4 C 1.2107(5) 0.7870(5) 0.9555(3) 0.0796(18) Uani 1 1 d . . . H4 H 1.2585 0.8193 0.9908 0.096 Uiso 1 1 calc R . . C9 C 1.1960(5) 0.7940(5) 0.7240(3) 0.090(2) Uani 1 1 d . . . C5 C 1.2241(5) 0.8052(5) 0.8928(3) 0.0836(19) Uani 1 1 d . . . H5 H 1.2813 0.8489 0.8857 0.100 Uiso 1 1 calc R . . Si5 Si -0.06633(13) 0.89713(14) -0.30825(7) 0.0708(5) Uani 1 1 d . . . C117 C -0.1183(4) 0.8146(4) -0.1092(2) 0.0582(15) Uani 1 1 d . . . C118 C -0.1997(4) 0.7448(4) -0.0971(2) 0.0637(15) Uani 1 1 d . . . H118 H -0.2484 0.7120 -0.1317 0.076 Uiso 1 1 calc R . . C119 C -0.2082(4) 0.7243(4) -0.0334(2) 0.0611(14) Uani 1 1 d . . . H119 H -0.2629 0.6784 -0.0246 0.073 Uiso 1 1 calc R . . C106 C 1.1573(5) 0.6977(5) 1.1485(3) 0.0752(18) Uani 1 1 d . . . H106 H 1.2024 0.7209 1.1870 0.090 Uiso 1 1 calc R . . C105 C 1.0674(5) 0.6329(4) 1.1503(3) 0.0659(15) Uani 1 1 d . . . C116 C -0.1055(4) 0.8392(4) -0.1745(2) 0.0645(15) Uani 1 1 d . . . N10 N 0.4350(5) 0.2050(5) 1.1532(4) 0.108(2) Uani 1 1 d . . . C114 C 0.5213(5) 0.3262(5) 1.2386(3) 0.089(2) Uani 1 1 d . . . H114 H 0.5749 0.3789 1.2546 0.106 Uiso 1 1 calc R . . C107 C 1.1791(5) 0.7274(5) 1.0889(3) 0.0746(17) Uani 1 1 d . . . H107 H 1.2398 0.7697 1.0873 0.090 Uiso 1 1 calc R . . C115 C -0.0918(5) 0.8607(5) -0.2271(3) 0.0766(18) Uani 1 1 d . . . C103 C 1.0393(5) 0.6001(5) 1.2112(3) 0.0727(17) Uani 1 1 d . . . C120 C -0.1329(5) 0.6760(5) 0.4757(3) 0.090(2) Uani 1 1 d . . . H12A H -0.1937 0.6316 0.4543 0.135 Uiso 1 1 calc R . . H12B H -0.1345 0.6873 0.5209 0.135 Uiso 1 1 calc R . . H12C H -0.0829 0.6517 0.4729 0.135 Uiso 1 1 calc R . . C104 C 1.0174(5) 0.5721(5) 1.2604(3) 0.0782(18) Uani 1 1 d . . . C108 C 0.6189(7) 0.4790(7) 0.4243(4) 0.134(4) Uani 1 1 d . . . H108 H 0.6233 0.4364 0.3939 0.161 Uiso 1 1 calc R . . C133 C 0.8575(5) 0.5022(5) 1.3346(4) 0.106(2) Uani 1 1 d . . . H13A H 0.8410 0.5554 1.3210 0.159 Uiso 1 1 calc R . . H13B H 0.8415 0.4872 1.3768 0.159 Uiso 1 1 calc R . . H13C H 0.8223 0.4499 1.3033 0.159 Uiso 1 1 calc R . . C112 C 0.3727(6) 0.2150(7) 1.2507(5) 0.120(3) Uani 1 1 d . . . H112 H 0.3247 0.1925 1.2752 0.144 Uiso 1 1 calc R . . C122 C 0.6011(5) 0.9110(7) 0.5114(4) 0.109(3) Uani 1 1 d . . . H122 H 0.6646 0.9514 0.5227 0.131 Uiso 1 1 calc R . . C113 C 0.4520(6) 0.2922(7) 1.2735(4) 0.112(3) Uani 1 1 d . . . H113 H 0.4579 0.3217 1.3141 0.134 Uiso 1 1 calc R . . C111 C 0.3654(5) 0.1727(6) 1.1926(5) 0.106(3) Uani 1 1 d . . . H111 H 0.3119 0.1196 1.1776 0.128 Uiso 1 1 calc R . . C110 C 0.5765(6) 0.6060(7) 0.4457(4) 0.125(4) Uani 1 1 d . . . H110 H 0.5495 0.6505 0.4320 0.151 Uiso 1 1 calc R . . C109 C 0.5823(7) 0.5441(9) 0.4011(4) 0.149(5) Uani 1 1 d . . . H109 H 0.5619 0.5463 0.3564 0.179 Uiso 1 1 calc R . . C130 C -0.1601(7) 0.9385(8) -0.3496(4) 0.172(5) Uani 1 1 d . . . H13D H -0.2175 0.8860 -0.3656 0.258 Uiso 1 1 calc R . . H13E H -0.1388 0.9732 -0.3856 0.258 Uiso 1 1 calc R . . H13F H -0.1731 0.9780 -0.3192 0.258 Uiso 1 1 calc R . . C123 C 0.5696(7) 0.8385(7) 0.5474(4) 0.122(3) Uani 1 1 d . . . H123 H 0.6096 0.8299 0.5843 0.146 Uiso 1 1 calc R . . C132 C 1.0184(5) 0.4221(5) 1.3531(4) 0.115(3) Uani 1 1 d . . . H13G H 0.9762 0.3728 1.3214 0.173 Uiso 1 1 calc R . . H13H H 1.0111 0.4034 1.3964 0.173 Uiso 1 1 calc R . . H13I H 1.0837 0.4348 1.3485 0.173 Uiso 1 1 calc R . . C129 C -0.0616(7) 0.7980(6) -0.3544(4) 0.135(3) Uani 1 1 d . . . H12D H -0.1250 0.7523 -0.3665 0.203 Uiso 1 1 calc R . . H12E H -0.0204 0.7710 -0.3279 0.203 Uiso 1 1 calc R . . H12F H -0.0367 0.8185 -0.3933 0.203 Uiso 1 1 calc R . . C121 C -0.2000(7) 0.8369(7) 0.4444(4) 0.143(4) Uani 1 1 d . . . H12G H -0.1848 0.8958 0.4252 0.215 Uiso 1 1 calc R . . H12H H -0.2004 0.8461 0.4901 0.215 Uiso 1 1 calc R . . H12I H -0.2622 0.7957 0.4225 0.215 Uiso 1 1 calc R . . C124 C 0.4788(8) 0.7781(7) 0.5289(5) 0.140(4) Uani 1 1 d . . . H124 H 0.4568 0.7265 0.5527 0.168 Uiso 1 1 calc R . . C101 C 1.2492(8) 0.9410(7) 0.6308(5) 0.177(5) Uani 1 1 d . . . H10A H 1.2822 0.9877 0.6664 0.266 Uiso 1 1 calc R . . H10B H 1.1829 0.9354 0.6204 0.266 Uiso 1 1 calc R . . H10C H 1.2780 0.9587 0.5931 0.266 Uiso 1 1 calc R . . C102 C 1.3793(7) 0.8376(11) 0.6811(6) 0.252(8) Uani 1 1 d . . . H10D H 1.4055 0.8279 0.6440 0.378 Uiso 1 1 calc R . . H10E H 1.3809 0.7905 0.7110 0.378 Uiso 1 1 calc R . . H10F H 1.4167 0.8981 0.7029 0.378 Uiso 1 1 calc R . . C100 C 1.1984(9) 0.7462(8) 0.5820(5) 0.211(6) Uani 1 1 d . . . H10G H 1.2314 0.7666 0.5464 0.317 Uiso 1 1 calc R . . H10H H 1.1327 0.7422 0.5693 0.317 Uiso 1 1 calc R . . H10I H 1.2004 0.6860 0.5929 0.317 Uiso 1 1 calc R . . C151 C 0.0134(6) 0.8699(6) 0.4664(4) 0.138(4) Uani 1 1 d . . . H15A H 0.0587 0.8383 0.4693 0.208 Uiso 1 1 calc R . . H15B H 0.0164 0.8967 0.5091 0.208 Uiso 1 1 calc R . . H15C H 0.0286 0.9185 0.4369 0.208 Uiso 1 1 calc R . . C150 C 0.0524(6) 0.9889(6) -0.2942(4) 0.131(3) Uani 1 1 d . . . H15D H 0.0650 1.0150 -0.3349 0.196 Uiso 1 1 calc R . . H15E H 0.1004 0.9629 -0.2769 0.196 Uiso 1 1 calc R . . H15F H 0.0541 1.0369 -0.2635 0.196 Uiso 1 1 calc R . . Si4 Si 0.98750(14) 0.52958(14) 1.33970(9) 0.0769(5) Uani 1 1 d . . . C131 C 1.0616(5) 0.6247(6) 1.4035(4) 0.118(3) Uani 1 1 d . . . H13J H 1.1284 0.6340 1.4061 0.178 Uiso 1 1 calc R . . H13K H 1.0442 0.6080 1.4452 0.178 Uiso 1 1 calc R . . H13L H 1.0506 0.6813 1.3924 0.178 Uiso 1 1 calc R . . C300 C 0.5347(10) 0.5248(11) 0.9805(7) 0.201(7) Uani 1 1 d D . . H30C H 0.5971 0.5212 0.9984 0.241 Uiso 1 1 calc R . . H30D H 0.5409 0.5900 0.9809 0.241 Uiso 1 1 calc R . . C301 C 0.4997(12) 0.4797(10) 0.9098(8) 0.243(10) Uani 1 1 d D . . H30A H 0.4384 0.4864 0.8930 0.291 Uiso 1 1 calc R . . H30B H 0.4879 0.4134 0.9116 0.291 Uiso 1 1 calc R . . C302 C 0.5652(10) 0.5165(11) 0.8596(10) 0.275(10) Uani 1 1 d D . . H30E H 0.6175 0.4935 0.8674 0.412 Uiso 1 1 calc R . . H30F H 0.5900 0.5834 0.8639 0.412 Uiso 1 1 calc R . . H30G H 0.5288 0.4953 0.8160 0.412 Uiso 1 1 calc R . . C304 C 0.4851(12) -0.0125(13) 0.9633(2) 0.338(13) Uani 1 1 d DU . . H30H H 0.4223 -0.0083 0.9481 0.406 Uiso 1 1 calc R . . H30I H 0.4804 -0.0763 0.9541 0.406 Uiso 1 1 calc R . . C305 C 0.5577(14) 0.0530(15) 0.9264(6) 0.356(14) Uani 1 1 d DU . . H30J H 0.5596 0.1164 0.9337 0.428 Uiso 1 1 calc R . . H30K H 0.6212 0.0517 0.9437 0.428 Uiso 1 1 calc R . . C306 C 0.5323(17) 0.0255(13) 0.8537(5) 0.378(14) Uani 1 1 d DU . . H30L H 0.4654 -0.0122 0.8419 0.567 Uiso 1 1 calc R . . H30M H 0.5704 -0.0095 0.8430 0.567 Uiso 1 1 calc R . . H30N H 0.5449 0.0806 0.8299 0.567 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 C201 0.145(10) 0.173(11) 0.121(8) 0.037(8) 0.058(7) -0.023(8) C155 0.130(8) 0.143(9) 0.148(10) 0.023(8) 0.051(8) -0.008(7) N16 0.131(6) 0.131(7) 0.127(6) 0.018(5) 0.046(5) 0.008(5) C154 0.153(9) 0.235(13) 0.082(6) 0.020(7) 0.043(6) -0.038(9) C153 0.116(6) 0.167(9) 0.059(5) 0.011(5) 0.024(4) -0.034(6) C152 0.083(5) 0.095(6) 0.080(5) 0.012(4) 0.023(4) 0.012(4) C127 0.074(4) 0.076(5) 0.071(4) 0.010(4) 0.017(3) 0.018(4) N20 0.085(4) 0.101(5) 0.070(4) 0.009(3) 0.019(3) 0.010(3) C200 0.058(4) 0.067(4) 0.073(4) 0.003(3) 0.009(3) -0.002(3) C128 0.061(4) 0.094(5) 0.062(4) 0.003(4) 0.010(3) 0.002(3) C125 0.070(4) 0.089(5) 0.065(4) 0.000(4) -0.001(3) 0.020(4) C47 0.067(4) 0.065(4) 0.060(4) 0.013(3) 0.015(3) 0.024(3) C46 0.068(4) 0.063(4) 0.050(3) 0.010(3) 0.012(3) 0.024(3) C45 0.100(5) 0.069(4) 0.045(3) 0.005(3) 0.005(3) 0.048(4) Pt1 0.06827(15) 0.06535(17) 0.03416(11) 0.00246(10) 0.00618(9) 0.03182(12) C23 0.050(3) 0.056(4) 0.080(4) 0.010(3) 0.005(3) -0.005(3) C26 0.064(4) 0.072(5) 0.085(5) 0.021(4) 0.009(3) 0.018(3) Pt2 0.06233(15) 0.05758(16) 0.04736(13) 0.00380(10) 0.00777(10) 0.02872(12) Si2 0.1098(14) 0.0819(13) 0.0377(8) 0.0078(8) 0.0211(8) 0.0183(11) Si1 0.0780(13) 0.1167(17) 0.0860(14) 0.0409(13) 0.0315(10) 0.0283(12) N7 0.071(3) 0.066(3) 0.036(2) 0.005(2) 0.010(2) 0.032(2) C19 0.061(3) 0.078(4) 0.062(4) 0.007(3) 0.012(3) 0.037(3) N6 0.062(3) 0.068(3) 0.039(2) 0.003(2) 0.006(2) 0.031(2) N1 0.070(3) 0.067(3) 0.046(3) 0.005(2) 0.003(2) 0.034(3) N2 0.071(3) 0.050(3) 0.052(3) 0.002(2) 0.009(2) 0.024(2) C36 0.062(4) 0.086(5) 0.056(3) 0.005(3) 0.007(3) 0.028(3) C11 0.062(3) 0.075(4) 0.050(3) 0.002(3) 0.005(3) 0.024(3) C10 0.068(4) 0.081(4) 0.054(3) 0.008(3) 0.011(3) 0.035(3) C33 0.081(4) 0.071(4) 0.038(3) 0.005(3) 0.008(3) 0.035(3) C27 0.075(4) 0.062(4) 0.033(3) 0.008(2) 0.013(2) 0.033(3) C7 0.071(4) 0.072(4) 0.050(3) 0.015(3) 0.012(3) 0.027(3) C15 0.055(3) 0.080(4) 0.048(3) 0.011(3) -0.001(2) 0.005(3) C12 0.044(3) 0.074(4) 0.056(3) -0.001(3) 0.006(2) 0.009(3) C21 0.056(3) 0.060(4) 0.075(4) 0.007(3) 0.005(3) 0.020(3) C20 0.065(4) 0.071(4) 0.068(4) 0.008(3) 0.009(3) 0.030(3) C1 0.081(4) 0.063(4) 0.057(3) 0.007(3) 0.005(3) 0.035(3) C25 0.054(3) 0.089(5) 0.072(4) 0.003(4) 0.015(3) 0.002(3) C34 0.095(5) 0.083(5) 0.048(3) 0.021(3) 0.022(3) 0.031(4) N4 0.102(4) 0.092(4) 0.072(4) 0.011(3) -0.002(3) 0.036(3) C37 0.078(4) 0.087(5) 0.048(3) 0.008(3) 0.000(3) 0.030(3) C22 0.079(5) 0.076(5) 0.090(5) -0.003(4) -0.006(4) 0.018(4) C38 0.081(4) 0.068(4) 0.047(3) -0.003(3) -0.004(3) 0.019(3) C14 0.074(4) 0.067(4) 0.057(3) -0.007(3) 0.005(3) 0.018(3) C43 0.069(4) 0.085(5) 0.049(3) 0.001(3) -0.004(3) 0.030(4) N8 0.101(5) 0.113(5) 0.067(4) 0.024(3) -0.010(3) 0.011(4) C35 0.098(5) 0.090(5) 0.039(3) 0.009(3) 0.015(3) 0.028(4) C16 0.108(5) 0.079(5) 0.062(4) -0.002(3) -0.002(4) 0.039(4) C32 0.090(4) 0.076(4) 0.039(3) 0.015(3) 0.017(3) 0.036(4) C2 0.073(4) 0.056(4) 0.054(3) -0.002(3) 0.008(3) 0.026(3) C28 0.067(3) 0.069(4) 0.038(3) 0.002(3) 0.009(2) 0.035(3) C29 0.071(4) 0.061(4) 0.036(3) 0.009(2) 0.010(2) 0.029(3) C3 0.075(4) 0.060(4) 0.050(3) 0.002(3) 0.004(3) 0.028(3) C17 0.066(4) 0.094(5) 0.055(4) 0.008(4) 0.005(3) -0.001(4) C41 0.054(3) 0.073(4) 0.065(4) 0.022(3) -0.007(3) 0.000(3) C13 0.070(4) 0.068(4) 0.063(4) 0.002(3) -0.001(3) 0.018(3) C31 0.095(5) 0.085(5) 0.052(3) 0.020(3) 0.023(3) 0.024(4) N5 0.096(4) 0.122(5) 0.060(4) 0.005(4) 0.007(3) -0.008(4) N9 0.086(4) 0.170(7) 0.085(4) 0.027(4) 0.000(3) 0.047(5) N3 0.081(4) 0.103(5) 0.084(4) 0.002(4) 0.020(3) 0.007(3) C30 0.082(4) 0.076(4) 0.044(3) 0.005(3) 0.005(3) 0.020(3) C24 0.056(4) 0.064(4) 0.085(5) 0.019(3) 0.007(3) 0.015(3) C42 0.067(4) 0.076(4) 0.052(3) 0.005(3) -0.001(3) 0.015(3) C6 0.067(4) 0.079(5) 0.072(4) 0.015(4) 0.015(3) 0.027(3) C40 0.079(4) 0.080(5) 0.073(4) 0.020(4) -0.003(3) 0.010(4) C44 0.084(5) 0.095(5) 0.080(5) 0.032(4) -0.010(4) 0.017(4) C18 0.070(4) 0.129(7) 0.070(4) 0.030(4) 0.006(3) 0.012(4) C39 0.083(5) 0.095(5) 0.061(4) 0.019(4) -0.010(3) 0.003(4) C8 0.068(4) 0.087(5) 0.072(4) 0.024(4) 0.013(3) 0.014(4) C4 0.075(4) 0.077(5) 0.069(4) 0.009(3) 0.002(3) 0.010(3) C9 0.074(4) 0.111(6) 0.075(4) 0.031(4) 0.017(3) 0.018(4) C5 0.077(4) 0.075(5) 0.085(5) 0.021(4) 0.018(4) 0.008(4) Si5 0.0858(12) 0.0924(13) 0.0378(8) 0.0110(8) 0.0177(8) 0.0328(10) C117 0.083(4) 0.072(4) 0.031(3) 0.002(3) 0.007(3) 0.043(3) C118 0.079(4) 0.081(4) 0.036(3) -0.001(3) 0.003(3) 0.038(3) C119 0.070(4) 0.068(4) 0.046(3) 0.002(3) 0.013(3) 0.024(3) C106 0.099(5) 0.080(5) 0.052(3) -0.006(3) -0.001(3) 0.046(4) C105 0.086(4) 0.070(4) 0.055(3) 0.009(3) 0.014(3) 0.043(4) C116 0.086(4) 0.072(4) 0.036(3) -0.004(3) 0.006(3) 0.033(3) N10 0.087(4) 0.097(5) 0.134(6) 0.031(4) 0.015(4) 0.029(4) C114 0.077(4) 0.104(6) 0.068(4) 0.018(4) 0.018(3) 0.007(4) C107 0.077(4) 0.081(5) 0.057(4) -0.004(3) 0.001(3) 0.022(3) C115 0.089(4) 0.102(5) 0.039(3) 0.005(3) 0.011(3) 0.035(4) C103 0.083(4) 0.080(5) 0.057(4) 0.002(3) 0.001(3) 0.037(4) C120 0.117(6) 0.090(5) 0.052(4) 0.012(3) 0.031(4) 0.016(4) C104 0.095(5) 0.088(5) 0.055(4) 0.007(3) 0.009(3) 0.040(4) C108 0.133(8) 0.155(9) 0.049(5) 0.004(5) 0.006(4) -0.025(7) C133 0.092(5) 0.111(6) 0.112(6) 0.004(5) 0.026(5) 0.028(5) C112 0.087(6) 0.147(9) 0.138(8) 0.067(7) 0.047(6) 0.041(6) C122 0.077(5) 0.169(9) 0.078(5) 0.023(5) -0.004(4) 0.048(5) C113 0.087(6) 0.156(9) 0.091(5) 0.032(5) 0.036(4) 0.031(6) C111 0.067(5) 0.098(6) 0.147(8) 0.047(6) 0.017(5) 0.020(4) C110 0.086(5) 0.168(10) 0.086(6) 0.054(6) -0.005(4) 0.008(6) C109 0.125(8) 0.198(13) 0.057(5) 0.040(7) -0.001(5) -0.019(8) C130 0.150(8) 0.346(16) 0.093(6) 0.102(8) 0.054(6) 0.161(10) C123 0.113(7) 0.165(9) 0.080(5) 0.029(6) -0.013(5) 0.054(7) C132 0.103(6) 0.102(6) 0.140(7) 0.037(5) 0.031(5) 0.029(5) C129 0.190(9) 0.132(8) 0.083(6) -0.009(5) 0.058(6) 0.042(7) C121 0.223(11) 0.149(8) 0.106(7) 0.029(6) 0.066(7) 0.108(8) C124 0.153(9) 0.133(8) 0.119(8) 0.059(6) -0.011(7) 0.050(7) C101 0.239(13) 0.140(9) 0.199(11) 0.086(8) 0.132(10) 0.078(9) C102 0.109(8) 0.48(2) 0.223(13) 0.211(15) 0.081(8) 0.140(12) C100 0.278(15) 0.177(11) 0.107(8) -0.033(8) 0.089(9) -0.034(10) C151 0.159(8) 0.111(7) 0.080(5) 0.013(5) 0.005(5) -0.026(6) C150 0.150(8) 0.115(7) 0.116(7) 0.014(6) 0.046(6) 0.022(6) Si4 0.0837(12) 0.0804(13) 0.0605(10) 0.0037(9) 0.0155(9) 0.0202(10) C131 0.100(6) 0.141(8) 0.085(5) -0.018(5) 0.018(4) 0.006(5) C300 0.217(17) 0.205(17) 0.28(2) 0.110(14) 0.111(14) 0.166(15) C301 0.30(2) 0.195(16) 0.36(3) 0.137(18) 0.17(2) 0.187(17) C302 0.175(14) 0.196(16) 0.49(3) 0.121(19) 0.099(18) 0.091(12) C304 0.31(2) 0.25(2) 0.50(3) -0.05(3) -0.05(3) 0.227(18) C305 0.35(3) 0.36(3) 0.41(3) -0.03(2) -0.06(2) 0.248(19) C306 0.49(3) 0.29(2) 0.43(3) -0.11(2) -0.05(3) 0.29(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 C201 C154 1.334(12) . ? C201 C155 1.382(13) . ? C201 H201 0.9300 . ? C155 N16 1.401(11) . ? C155 H155 0.9300 . ? N16 C152 1.375(10) . ? C154 C153 1.337(10) . ? C154 H154 0.9300 . ? C153 C152 1.327(10) . ? C153 H153 0.9300 . ? C152 C127 1.478(9) . ? C127 C200 1.324(8) . ? C127 N20 1.358(8) . ? N20 C128 1.361(7) . ? C200 C125 1.331(8) . ? C200 H200 0.9300 . ? C128 C47 1.382(8) . ? C128 H128 0.9300 . ? C125 C47 1.392(8) . ? C125 H125 0.9300 . ? C47 C46 1.421(8) . ? C46 C45 1.203(8) . ? C45 Pt1 1.956(7) . ? Pt1 C36 1.971(5) . ? Pt1 N7 2.063(5) . ? Pt1 N6 2.079(4) . ? C23 C24 1.327(8) . ? C23 C22 1.385(9) . ? C23 H23 0.9300 . ? C26 C114 1.353(9) . ? C26 N10 1.368(9) . ? C26 C24 1.507(9) . ? Pt2 C19 1.947(6) . ? Pt2 C10 1.983(6) . ? Pt2 N2 2.087(5) . ? Pt2 N1 2.091(5) . ? Si2 C121 1.829(8) . ? Si2 C120 1.829(6) . ? Si2 C35 1.843(6) . ? Si2 C151 1.856(8) . ? Si1 C102 1.792(9) . ? Si1 C101 1.798(9) . ? Si1 C9 1.847(7) . ? Si1 C100 1.850(10) . ? N7 C33 1.331(6) . ? N7 C29 1.365(7) . ? C19 C20 1.193(8) . ? N6 C28 1.335(7) . ? N6 C27 1.345(6) . ? N1 C1 1.336(7) . ? N1 C2 1.344(7) . ? N2 C3 1.352(7) . ? N2 C7 1.364(7) . ? C36 C37 1.199(6) . ? C11 C10 1.178(7) . ? C11 C12 1.438(7) . ? C33 C32 1.369(8) . ? C33 H33 0.9300 . ? C27 C117 1.384(8) . ? C27 H27 0.9300 . ? C7 C6 1.399(8) . ? C7 H7 0.9300 . ? C15 N4 1.337(8) . ? C15 C14 1.380(8) . ? C15 C17 1.478(8) . ? C12 C16 1.369(8) . ? C12 C13 1.399(8) . ? C21 C25 1.381(8) . ? C21 C22 1.389(9) . ? C21 C20 1.447(8) . ? C1 C105 1.382(8) . ? C1 H1 0.9300 . ? C25 N3 1.349(7) . ? C25 H25 0.9300 . ? C34 C35 1.190(7) . ? C34 C32 1.452(7) . ? N4 C16 1.352(8) . ? C37 C38 1.435(7) . ? C22 H22 0.9300 . ? C38 C39 1.362(8) . ? C38 C40 1.390(8) . ? C14 C13 1.387(7) . ? C14 H14 0.9300 . ? C43 C44 1.305(8) . ? C43 N9 1.374(8) . ? C43 C42 1.479(7) . ? N8 C42 1.348(8) . ? N8 C39 1.374(8) . ? C16 H16 0.9300 . ? C32 C31 1.388(9) . ? C2 C107 1.384(8) . ? C2 C3 1.454(7) . ? C28 C119 1.379(7) . ? C28 C29 1.492(6) . ? C29 C30 1.357(8) . ? C3 C4 1.364(8) . ? C17 N5 1.336(9) . ? C17 C18 1.355(10) . ? C41 C42 1.334(8) . ? C41 C40 1.336(8) . ? C41 H41 0.9300 . ? C13 H13 0.9300 . ? C31 C30 1.379(7) . ? C31 H31 0.9300 . ? N5 C108 1.370(9) . ? N9 C122 1.378(8) . ? N3 C24 1.356(8) . ? C30 H30 0.9300 . ? C6 C5 1.381(9) . ? C6 C8 1.442(8) . ? C40 H40 0.9300 . ? C44 C124 1.373(10) . ? C44 H44 0.9300 . ? C18 C110 1.404(10) . ? C18 H18 0.9300 . ? C39 H39 0.9300 . ? C8 C9 1.190(8) . ? C4 C5 1.370(8) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? Si5 C129 1.817(8) . ? Si5 C130 1.828(8) . ? Si5 C150 1.829(8) . ? Si5 C115 1.845(6) . ? C117 C118 1.387(8) . ? C117 C116 1.440(7) . ? C118 C119 1.381(7) . ? C118 H118 0.9300 . ? C119 H119 0.9300 . ? C106 C107 1.377(8) . ? C106 C105 1.386(9) . ? C106 H106 0.9300 . ? C105 C103 1.445(8) . ? C116 C115 1.177(7) . ? N10 C111 1.405(10) . ? C114 C113 1.340(9) . ? C114 H114 0.9300 . ? C107 H107 0.9300 . ? C103 C104 1.170(8) . ? C120 H12A 0.9600 . ? C120 H12B 0.9600 . ? C120 H12C 0.9600 . ? C104 Si4 1.850(7) . ? C108 C109 1.351(14) . ? C108 H108 0.9300 . ? C133 Si4 1.844(7) . ? C133 H13A 0.9600 . ? C133 H13B 0.9600 . ? C133 H13C 0.9600 . ? C112 C111 1.334(11) . ? C112 C113 1.366(12) . ? C112 H112 0.9300 . ? C122 C123 1.339(11) . ? C122 H122 0.9300 . ? C113 H113 0.9300 . ? C111 H111 0.9300 . ? C110 C109 1.354(14) . ? C110 H110 0.9300 . ? C109 H109 0.9300 . ? C130 H13D 0.9600 . ? C130 H13E 0.9600 . ? C130 H13F 0.9600 . ? C123 C124 1.348(11) . ? C123 H123 0.9300 . ? C132 Si4 1.870(7) . ? C132 H13G 0.9600 . ? C132 H13H 0.9600 . ? C132 H13I 0.9600 . ? C129 H12D 0.9600 . ? C129 H12E 0.9600 . ? C129 H12F 0.9600 . ? C121 H12G 0.9600 . ? C121 H12H 0.9600 . ? C121 H12I 0.9600 . ? C124 H124 0.9300 . ? C101 H10A 0.9600 . ? C101 H10B 0.9600 . ? C101 H10C 0.9600 . ? C102 H10D 0.9600 . ? C102 H10E 0.9600 . ? C102 H10F 0.9600 . ? C100 H10G 0.9600 . ? C100 H10H 0.9600 . ? C100 H10I 0.9600 . ? C151 H15A 0.9600 . ? C151 H15B 0.9600 . ? C151 H15C 0.9600 . ? C150 H15D 0.9600 . ? C150 H15E 0.9600 . ? C150 H15F 0.9600 . ? Si4 C131 1.858(7) . ? C131 H13J 0.9600 . ? C131 H13K 0.9600 . ? C131 H13L 0.9600 . ? C300 C300 1.45(3) 2_667 ? C300 C301 1.540(10) . ? C300 H30C 0.9700 . ? C300 H30D 0.9700 . ? C301 C302 1.542(9) . ? C301 H30A 0.9700 . ? C301 H30B 0.9700 . ? C302 H30E 0.9600 . ? C302 H30F 0.9600 . ? C302 H30G 0.9600 . ? C304 C304 1.516(10) 2_657 ? C304 C305 1.533(10) . ? C304 H30H 0.9700 . ? C304 H30I 0.9700 . ? C305 C306 1.512(9) . ? C305 H30J 0.9700 . ? C305 H30K 0.9700 . ? C306 H30L 0.9600 . ? C306 H30M 0.9600 . ? C306 H30N 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C154 C201 C155 118.2(9) . . ? C154 C201 H201 120.9 . . ? C155 C201 H201 120.9 . . ? C201 C155 N16 120.8(9) . . ? C201 C155 H155 119.6 . . ? N16 C155 H155 119.6 . . ? C152 N16 C155 116.9(8) . . ? C201 C154 C153 121.7(10) . . ? C201 C154 H154 119.1 . . ? C153 C154 H154 119.1 . . ? C152 C153 C154 121.4(8) . . ? C152 C153 H153 119.3 . . ? C154 C153 H153 119.3 . . ? C153 C152 N16 120.9(7) . . ? C153 C152 C127 122.7(7) . . ? N16 C152 C127 116.4(7) . . ? C200 C127 N20 120.7(6) . . ? C200 C127 C152 122.2(6) . . ? N20 C127 C152 117.0(6) . . ? C127 N20 C128 118.6(6) . . ? C127 C200 C125 120.5(6) . . ? C127 C200 H200 119.7 . . ? C125 C200 H200 119.7 . . ? N20 C128 C47 122.8(6) . . ? N20 C128 H128 118.6 . . ? C47 C128 H128 118.6 . . ? C200 C125 C47 123.0(6) . . ? C200 C125 H125 118.5 . . ? C47 C125 H125 118.5 . . ? C128 C47 C125 114.3(5) . . ? C128 C47 C46 121.5(6) . . ? C125 C47 C46 124.3(6) . . ? C45 C46 C47 177.1(7) . . ? C46 C45 Pt1 172.5(6) . . ? C45 Pt1 C36 92.7(2) . . ? C45 Pt1 N7 172.8(2) . . ? C36 Pt1 N7 94.4(2) . . ? C45 Pt1 N6 94.4(2) . . ? C36 Pt1 N6 170.2(2) . . ? N7 Pt1 N6 78.78(17) . . ? C24 C23 C22 119.0(6) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C114 C26 N10 123.5(6) . . ? C114 C26 C24 120.5(6) . . ? N10 C26 C24 115.9(7) . . ? C19 Pt2 C10 91.5(2) . . ? C19 Pt2 N2 172.0(2) . . ? C10 Pt2 N2 96.5(2) . . ? C19 Pt2 N1 93.5(2) . . ? C10 Pt2 N1 174.5(2) . . ? N2 Pt2 N1 78.55(18) . . ? C121 Si2 C120 110.4(4) . . ? C121 Si2 C35 107.7(4) . . ? C120 Si2 C35 109.1(3) . . ? C121 Si2 C151 110.8(5) . . ? C120 Si2 C151 112.3(4) . . ? C35 Si2 C151 106.3(3) . . ? C102 Si1 C101 112.4(6) . . ? C102 Si1 C9 106.5(4) . . ? C101 Si1 C9 109.3(4) . . ? C102 Si1 C100 110.8(7) . . ? C101 Si1 C100 107.0(6) . . ? C9 Si1 C100 110.8(4) . . ? C33 N7 C29 117.7(5) . . ? C33 N7 Pt1 126.9(4) . . ? C29 N7 Pt1 115.3(3) . . ? C20 C19 Pt2 170.1(6) . . ? C28 N6 C27 119.3(5) . . ? C28 N6 Pt1 115.7(3) . . ? C27 N6 Pt1 124.7(4) . . ? C1 N1 C2 120.7(5) . . ? C1 N1 Pt2 124.5(4) . . ? C2 N1 Pt2 114.8(4) . . ? C3 N2 C7 120.3(5) . . ? C3 N2 Pt2 114.2(4) . . ? C7 N2 Pt2 125.5(4) . . ? C37 C36 Pt1 168.0(6) . . ? C10 C11 C12 173.6(7) . . ? C11 C10 Pt2 175.4(6) . . ? N7 C33 C32 124.0(6) . . ? N7 C33 H33 118.0 . . ? C32 C33 H33 118.0 . . ? N6 C27 C117 122.1(6) . . ? N6 C27 H27 119.0 . . ? C117 C27 H27 119.0 . . ? N2 C7 C6 120.4(6) . . ? N2 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? N4 C15 C14 122.2(5) . . ? N4 C15 C17 116.4(6) . . ? C14 C15 C17 121.4(6) . . ? C16 C12 C13 116.0(6) . . ? C16 C12 C11 121.8(6) . . ? C13 C12 C11 122.2(6) . . ? C25 C21 C22 116.1(6) . . ? C25 C21 C20 121.6(6) . . ? C22 C21 C20 122.3(6) . . ? C19 C20 C21 176.1(7) . . ? N1 C1 C105 122.4(6) . . ? N1 C1 H1 118.8 . . ? C105 C1 H1 118.8 . . ? N3 C25 C21 122.5(6) . . ? N3 C25 H25 118.8 . . ? C21 C25 H25 118.8 . . ? C35 C34 C32 176.7(7) . . ? C15 N4 C16 117.9(6) . . ? C36 C37 C38 173.4(7) . . ? C23 C22 C21 121.3(7) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C39 C38 C40 115.9(6) . . ? C39 C38 C37 121.9(6) . . ? C40 C38 C37 122.1(6) . . ? C15 C14 C13 118.6(6) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C44 C43 N9 122.3(6) . . ? C44 C43 C42 120.2(6) . . ? N9 C43 C42 117.4(6) . . ? C42 N8 C39 118.3(6) . . ? C34 C35 Si2 175.3(6) . . ? N4 C16 C12 124.7(6) . . ? N4 C16 H16 117.6 . . ? C12 C16 H16 117.6 . . ? C33 C32 C31 118.3(5) . . ? C33 C32 C34 119.0(6) . . ? C31 C32 C34 122.5(6) . . ? N1 C2 C107 119.1(5) . . ? N1 C2 C3 115.9(5) . . ? C107 C2 C3 125.0(6) . . ? N6 C28 C119 122.1(5) . . ? N6 C28 C29 114.9(5) . . ? C119 C28 C29 123.0(5) . . ? C30 C29 N7 120.9(5) . . ? C30 C29 C28 124.2(5) . . ? N7 C29 C28 114.8(5) . . ? N2 C3 C4 120.4(5) . . ? N2 C3 C2 116.5(5) . . ? C4 C3 C2 123.1(6) . . ? N5 C17 C18 122.0(7) . . ? N5 C17 C15 117.2(7) . . ? C18 C17 C15 120.8(7) . . ? C42 C41 C40 120.6(6) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C14 C13 C12 120.5(6) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C30 C31 C32 117.9(6) . . ? C30 C31 H31 121.1 . . ? C32 C31 H31 121.1 . . ? C17 N5 C108 116.7(8) . . ? C43 N9 C122 117.0(7) . . ? C25 N3 C24 119.0(6) . . ? C29 C30 C31 121.2(6) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C23 C24 N3 122.1(6) . . ? C23 C24 C26 118.9(6) . . ? N3 C24 C26 118.9(6) . . ? C41 C42 N8 121.1(6) . . ? C41 C42 C43 120.3(6) . . ? N8 C42 C43 118.7(6) . . ? C5 C6 C7 118.3(6) . . ? C5 C6 C8 119.5(6) . . ? C7 C6 C8 122.2(6) . . ? C41 C40 C38 121.7(6) . . ? C41 C40 H40 119.2 . . ? C38 C40 H40 119.2 . . ? C43 C44 C124 119.1(7) . . ? C43 C44 H44 120.4 . . ? C124 C44 H44 120.4 . . ? C17 C18 C110 119.4(9) . . ? C17 C18 H18 120.3 . . ? C110 C18 H18 120.3 . . ? C38 C39 N8 122.5(6) . . ? C38 C39 H39 118.8 . . ? N8 C39 H39 118.8 . . ? C9 C8 C6 171.5(8) . . ? C3 C4 C5 120.5(6) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C8 C9 Si1 170.2(7) . . ? C4 C5 C6 120.1(6) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C129 Si5 C130 111.7(5) . . ? C129 Si5 C150 108.6(4) . . ? C130 Si5 C150 112.0(5) . . ? C129 Si5 C115 108.4(3) . . ? C130 Si5 C115 109.0(3) . . ? C150 Si5 C115 107.0(4) . . ? C27 C117 C118 118.0(5) . . ? C27 C117 C116 119.6(6) . . ? C118 C117 C116 122.4(5) . . ? C119 C118 C117 119.9(5) . . ? C119 C118 H118 120.0 . . ? C117 C118 H118 120.0 . . ? C28 C119 C118 118.6(5) . . ? C28 C119 H119 120.7 . . ? C118 C119 H119 120.7 . . ? C107 C106 C105 119.1(6) . . ? C107 C106 H106 120.4 . . ? C105 C106 H106 120.4 . . ? C1 C105 C106 117.8(6) . . ? C1 C105 C103 120.2(6) . . ? C106 C105 C103 122.0(6) . . ? C115 C116 C117 177.7(7) . . ? C26 N10 C111 114.7(7) . . ? C113 C114 C26 118.7(7) . . ? C113 C114 H114 120.7 . . ? C26 C114 H114 120.7 . . ? C106 C107 C2 120.8(6) . . ? C106 C107 H107 119.6 . . ? C2 C107 H107 119.6 . . ? C116 C115 Si5 178.1(7) . . ? C104 C103 C105 178.5(7) . . ? Si2 C120 H12A 109.5 . . ? Si2 C120 H12B 109.5 . . ? H12A C120 H12B 109.5 . . ? Si2 C120 H12C 109.5 . . ? H12A C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? C103 C104 Si4 177.9(7) . . ? C109 C108 N5 124.8(10) . . ? C109 C108 H108 117.6 . . ? N5 C108 H108 117.6 . . ? Si4 C133 H13A 109.5 . . ? Si4 C133 H13B 109.5 . . ? H13A C133 H13B 109.5 . . ? Si4 C133 H13C 109.5 . . ? H13A C133 H13C 109.5 . . ? H13B C133 H13C 109.5 . . ? C111 C112 C113 118.7(8) . . ? C111 C112 H112 120.6 . . ? C113 C112 H112 120.6 . . ? C123 C122 N9 121.5(8) . . ? C123 C122 H122 119.2 . . ? N9 C122 H122 119.2 . . ? C114 C113 C112 121.5(9) . . ? C114 C113 H113 119.2 . . ? C112 C113 H113 119.2 . . ? C112 C111 N10 122.8(8) . . ? C112 C111 H111 118.6 . . ? N10 C111 H111 118.6 . . ? C109 C110 C18 119.8(10) . . ? C109 C110 H110 120.1 . . ? C18 C110 H110 120.1 . . ? C108 C109 C110 117.2(9) . . ? C108 C109 H109 121.4 . . ? C110 C109 H109 121.4 . . ? Si5 C130 H13D 109.5 . . ? Si5 C130 H13E 109.5 . . ? H13D C130 H13E 109.5 . . ? Si5 C130 H13F 109.5 . . ? H13D C130 H13F 109.5 . . ? H13E C130 H13F 109.5 . . ? C122 C123 C124 118.7(8) . . ? C122 C123 H123 120.6 . . ? C124 C123 H123 120.6 . . ? Si4 C132 H13G 109.5 . . ? Si4 C132 H13H 109.5 . . ? H13G C132 H13H 109.5 . . ? Si4 C132 H13I 109.5 . . ? H13G C132 H13I 109.5 . . ? H13H C132 H13I 109.5 . . ? Si5 C129 H12D 109.5 . . ? Si5 C129 H12E 109.5 . . ? H12D C129 H12E 109.5 . . ? Si5 C129 H12F 109.5 . . ? H12D C129 H12F 109.5 . . ? H12E C129 H12F 109.5 . . ? Si2 C121 H12G 109.5 . . ? Si2 C121 H12H 109.5 . . ? H12G C121 H12H 109.5 . . ? Si2 C121 H12I 109.5 . . ? H12G C121 H12I 109.5 . . ? H12H C121 H12I 109.5 . . ? C123 C124 C44 121.2(9) . . ? C123 C124 H124 119.4 . . ? C44 C124 H124 119.4 . . ? Si1 C101 H10A 109.5 . . ? Si1 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? Si1 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? Si1 C102 H10D 109.5 . . ? Si1 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? Si1 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? Si1 C100 H10G 109.5 . . ? Si1 C100 H10H 109.5 . . ? H10G C100 H10H 109.5 . . ? Si1 C100 H10I 109.5 . . ? H10G C100 H10I 109.5 . . ? H10H C100 H10I 109.5 . . ? Si2 C151 H15A 109.5 . . ? Si2 C151 H15B 109.5 . . ? H15A C151 H15B 109.5 . . ? Si2 C151 H15C 109.5 . . ? H15A C151 H15C 109.5 . . ? H15B C151 H15C 109.5 . . ? Si5 C150 H15D 109.5 . . ? Si5 C150 H15E 109.5 . . ? H15D C150 H15E 109.5 . . ? Si5 C150 H15F 109.5 . . ? H15D C150 H15F 109.5 . . ? H15E C150 H15F 109.5 . . ? C133 Si4 C104 107.9(3) . . ? C133 Si4 C131 112.5(4) . . ? C104 Si4 C131 106.5(4) . . ? C133 Si4 C132 110.3(4) . . ? C104 Si4 C132 108.2(3) . . ? C131 Si4 C132 111.1(4) . . ? Si4 C131 H13J 109.5 . . ? Si4 C131 H13K 109.5 . . ? H13J C131 H13K 109.5 . . ? Si4 C131 H13L 109.5 . . ? H13J C131 H13L 109.5 . . ? H13K C131 H13L 109.5 . . ? C300 C300 C301 108.4(18) 2_667 . ? C300 C300 H30C 110.0 2_667 . ? C301 C300 H30C 110.0 . . ? C300 C300 H30D 110.0 2_667 . ? C301 C300 H30D 110.0 . . ? H30C C300 H30D 108.4 . . ? C300 C301 C302 118.1(16) . . ? C300 C301 H30A 107.8 . . ? C302 C301 H30A 107.8 . . ? C300 C301 H30B 107.8 . . ? C302 C301 H30B 107.8 . . ? H30A C301 H30B 107.1 . . ? C301 C302 H30E 109.5 . . ? C301 C302 H30F 109.5 . . ? H30E C302 H30F 109.5 . . ? C301 C302 H30G 109.5 . . ? H30E C302 H30G 109.5 . . ? H30F C302 H30G 109.5 . . ? C304 C304 C305 111.2(10) 2_657 . ? C304 C304 H30H 109.4 2_657 . ? C305 C304 H30H 109.4 . . ? C304 C304 H30I 109.4 2_657 . ? C305 C304 H30I 109.4 . . ? H30H C304 H30I 108.0 . . ? C306 C305 C304 111.8(10) . . ? C306 C305 H30J 109.3 . . ? C304 C305 H30J 109.3 . . ? C306 C305 H30K 109.3 . . ? C304 C305 H30K 109.3 . . ? H30J C305 H30K 107.9 . . ? C305 C306 H30L 109.5 . . ? C305 C306 H30M 109.5 . . ? H30L C306 H30M 109.5 . . ? C305 C306 H30N 109.5 . . ? H30L C306 H30N 109.5 . . ? H30M C306 H30N 109.5 . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.499 _refine_diff_density_min -1.128 _refine_diff_density_rms 0.084 # Attachment 'CCDC 710904.cif' data_1.THF _database_code_depnum_ccdc_archive 'CCDC 710904' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H46 N6 O Pt Si2' _chemical_formula_weight 974.18 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' Si Si 0.0817 0.0704 '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 28.870(3) _cell_length_b 23.5279(12) _cell_length_c 13.5575(9) _cell_angle_alpha 90.00 _cell_angle_beta 99.285(5) _cell_angle_gamma 90.00 _cell_volume 9088.4(11) _cell_formula_units_Z 8 _cell_measurement_temperature 113.1(1) _cell_measurement_reflns_used 9524 _cell_measurement_theta_min 3.0448 _cell_measurement_theta_max 27.4758 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.8000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.0800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3920 _exptl_absorpt_coefficient_mu 3.182 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.1790 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113.1(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Saturn70 _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28346 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7886 _reflns_number_gt 6627 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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. The bipyridine groups containing N4 and N6 are severe disorder. Constraints of the structure are given below in SHELX format. flat c40 c41 c42 c43 c44 n6 dfix 1.38 0.01 c40 c41 c41 c42 c42 c43 c43 c44 c44 n6 n6 c40 dfix 2.4 0.01 c40 c42 c41 c43 c42 c44 c43 n6 c44 c40 n6 c41 flat c40' c41' c42' c43' c44' n6' dfix 1.38 0.01 c40' c41' c41' c42' c42' c43' c43' c44' c44' n6' n6' c40' dfix 2.4 0.01 c40' c42' c41' c43' c42' c44' c43' n6' c44' c40' n6' c41' flat c35' c36' c37' c38' c39' n5' dfix 1.38 0.01 c35' c36' c36' c37' c37' c38' c38' n5' n5' c39' c39' c35' dfix 2.35 0.01 c35' c37' c36' c38' c37' n5' c38' c39' n5' c35' c39' c36' dfix 1.38 0.01 n4' c29' c29' c30' c30' c31' c31' c32' c32' c28' c28' n4' dfix 1.38 0.01 n4 c29 c29 c30 c30 c31 c31 c32 c32 c28 c28 n4 dfix 1.38 0.01 c23 c24 c24 n3 n3 c25 c25 c26 c26 c27 c27 c23 dfix 1.38 0.01 c23 c24' c24' n3' n3' c25' c25' c26' c26' c27' c27' c23 simu 0.01 n3 > n4 simu 0.01 n3' > n4' simu 0.01 c35 > n6 simu 0.01 c35' > n6' dfix 1.20 0.01 c33 c34 dfix 1.42 0.01 o01 c01 o01 c04 dfix 1.52 0.01 c01 c02 c02 c03 c03 c04 dfix 2.35 0.01 o01 c02 o01 c03 c02 c04 c01 c03 dfix 2.3 0.01 c01 c04 simu c01 c02 c03 c04 o01 ; _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^)+(0.0632P)^2^+44.6382P] 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 SHELXL _refine_ls_extinction_coef 0.00048(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7886 _refine_ls_number_parameters 727 _refine_ls_number_restraints 390 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1422 _refine_ls_wR_factor_gt 0.1321 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.151 _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 0.014979(9) 0.428598(10) 0.140658(18) 0.04063(16) Uani 1 1 d . . . Si1 Si 0.08866(8) 0.75640(9) 0.22495(19) 0.0628(6) Uani 1 1 d . . . Si2 Si -0.18853(10) 0.17733(11) 0.0462(2) 0.0794(8) Uani 1 1 d . . . N1 N -0.01178(18) 0.5094(2) 0.1174(4) 0.0407(13) Uani 1 1 d . . . N2 N -0.0553(2) 0.4112(2) 0.0924(4) 0.0427(13) Uani 1 1 d . . . C1 C 0.0136(2) 0.5574(3) 0.1370(4) 0.0416(16) Uani 1 1 d . . . H1A H 0.0455 0.5548 0.1613 0.050 Uiso 1 1 calc R . . C2 C -0.0073(2) 0.6109(3) 0.1213(5) 0.0447(16) Uani 1 1 d . . . C3 C -0.0550(2) 0.6147(3) 0.0854(5) 0.0427(15) Uani 1 1 d . . . H3A H -0.0693 0.6501 0.0748 0.051 Uiso 1 1 calc R . . C4 C -0.0812(2) 0.5655(3) 0.0657(5) 0.0429(16) Uani 1 1 d . . . H4A H -0.1133 0.5672 0.0423 0.051 Uiso 1 1 calc R . . C5 C -0.0587(2) 0.5141(3) 0.0817(4) 0.0403(15) Uani 1 1 d . . . C6 C -0.0819(2) 0.4566(3) 0.0632(5) 0.0436(16) Uani 1 1 d . . . C7 C -0.1293(3) 0.4518(3) 0.0225(5) 0.056(2) Uani 1 1 d . . . H7A H -0.1470 0.4840 0.0018 0.068 Uiso 1 1 calc R . . C8 C -0.1496(3) 0.3982(3) 0.0135(6) 0.060(2) Uani 1 1 d . . . H8A H -0.1808 0.3937 -0.0157 0.072 Uiso 1 1 calc R . . C9 C -0.1225(3) 0.3508(3) 0.0488(5) 0.0515(17) Uani 1 1 d . . . C10 C -0.0748(2) 0.3591(3) 0.0862(5) 0.0455(16) Uani 1 1 d . . . H10A H -0.0562 0.3278 0.1072 0.055 Uiso 1 1 calc R . . C11 C 0.0221(2) 0.6611(3) 0.1451(5) 0.0418(15) Uani 1 1 d . . . C12 C 0.0492(2) 0.6982(3) 0.1730(6) 0.0517(18) Uani 1 1 d . . . C13 C 0.0826(4) 0.8149(4) 0.1317(9) 0.093(3) Uani 1 1 d . . . H13A H 0.0921 0.8016 0.0711 0.140 Uiso 1 1 calc R . . H13B H 0.1021 0.8462 0.1578 0.140 Uiso 1 1 calc R . . H13C H 0.0504 0.8270 0.1180 0.140 Uiso 1 1 calc R . . C14 C 0.1491(3) 0.7273(4) 0.2458(8) 0.078(3) Uani 1 1 d . . . H14A H 0.1573 0.7155 0.1831 0.117 Uiso 1 1 calc R . . H14B H 0.1507 0.6954 0.2902 0.117 Uiso 1 1 calc R . . H14C H 0.1706 0.7561 0.2749 0.117 Uiso 1 1 calc R . . C15 C 0.0711(4) 0.7805(4) 0.3433(7) 0.086(3) Uani 1 1 d . . . H15A H 0.0913 0.8108 0.3710 0.130 Uiso 1 1 calc R . . H15B H 0.0737 0.7494 0.3897 0.130 Uiso 1 1 calc R . . H15C H 0.0392 0.7936 0.3307 0.130 Uiso 1 1 calc R . . C16 C -0.1428(3) 0.2950(3) 0.0481(6) 0.059(2) Uani 1 1 d . . . C17 C -0.1606(3) 0.2491(4) 0.0469(6) 0.067(2) Uani 1 1 d . . . C18 C -0.2306(5) 0.1788(5) 0.1376(10) 0.130(5) Uani 1 1 d . . . H18A H -0.2546 0.2065 0.1167 0.195 Uiso 1 1 calc R . . H18B H -0.2141 0.1887 0.2025 0.195 Uiso 1 1 calc R . . H18C H -0.2447 0.1420 0.1404 0.195 Uiso 1 1 calc R . . C19 C -0.1427(4) 0.1241(5) 0.0805(11) 0.127(5) Uani 1 1 d . . . H19A H -0.1567 0.0871 0.0801 0.191 Uiso 1 1 calc R . . H19B H -0.1260 0.1323 0.1461 0.191 Uiso 1 1 calc RD . . H19C H -0.1213 0.1250 0.0332 0.191 Uiso 1 1 calc R . . C20 C -0.2206(4) 0.1643(4) -0.0815(8) 0.090(3) Uani 1 1 d . . . H20A H -0.1988 0.1636 -0.1279 0.135 Uiso 1 1 calc R . . H20B H -0.2431 0.1941 -0.0996 0.135 Uiso 1 1 calc R . . H20C H -0.2365 0.1284 -0.0832 0.135 Uiso 1 1 calc RD . . C21 C 0.0797(3) 0.4535(3) 0.1835(5) 0.0445(16) Uani 1 1 d . . . C22 C 0.1178(2) 0.4736(3) 0.2123(5) 0.0455(16) Uani 1 1 d . A . C23 C 0.1621(2) 0.4974(3) 0.2566(6) 0.0549(19) Uani 1 1 d D . . C24 C 0.1737(8) 0.5546(5) 0.261(3) 0.054(9) Uani 0.50 1 d PD A 1 H24A H 0.1499 0.5810 0.2417 0.065 Uiso 0.50 1 calc PR A 1 N3 N 0.2188(5) 0.5747(7) 0.2911(16) 0.076(4) Uani 0.50 1 d PDU A 1 C25 C 0.2541(5) 0.5364(5) 0.3213(16) 0.072(3) Uani 0.50 1 d PDU A 1 C26 C 0.2460(5) 0.4791(5) 0.3192(16) 0.069(4) Uani 0.50 1 d PDU A 1 H26A H 0.2692 0.4530 0.3431 0.083 Uiso 0.50 1 calc PR A 1 C27 C 0.2013(4) 0.4629(7) 0.2794(19) 0.075(6) Uani 0.50 1 d PDU A 1 H27A H 0.1967 0.4243 0.2662 0.090 Uiso 0.50 1 calc PR A 1 C28 C 0.3029(6) 0.5520(6) 0.3651(18) 0.088(4) Uani 0.50 1 d PDU A 1 C29 C 0.3825(7) 0.5331(8) 0.437(2) 0.120(5) Uani 0.50 1 d PDU A 1 H29A H 0.4068 0.5074 0.4546 0.144 Uiso 0.50 1 calc PR A 1 C30 C 0.3912(7) 0.5905(8) 0.447(2) 0.113(5) Uani 0.50 1 d PDU A 1 H30A H 0.4206 0.6041 0.4749 0.135 Uiso 0.50 1 calc PR A 1 C31 C 0.3546(5) 0.6268(8) 0.4147(17) 0.095(4) Uani 0.50 1 d PDU A 1 H31A H 0.3605 0.6656 0.4187 0.114 Uiso 0.50 1 calc PR A 1 C32 C 0.3096(5) 0.6096(6) 0.3766(16) 0.080(4) Uani 0.50 1 d PDU A 1 H32A H 0.2853 0.6355 0.3597 0.096 Uiso 0.50 1 calc PR A 1 N4 N 0.3379(5) 0.5134(7) 0.3996(18) 0.113(4) Uani 0.50 1 d PDU A 1 C24' C 0.1664(13) 0.5555(5) 0.272(4) 0.088(15) Uani 0.50 1 d PD A 2 H24B H 0.1438 0.5799 0.2391 0.106 Uiso 0.50 1 calc PR A 2 N3' N 0.2042(7) 0.5774(8) 0.3368(17) 0.095(5) Uani 0.50 1 d PDU A 2 C25' C 0.2348(7) 0.5408(5) 0.3946(17) 0.082(4) Uani 0.50 1 d PDU A 2 C26' C 0.2285(5) 0.4839(4) 0.3843(13) 0.060(3) Uani 0.50 1 d PDU A 2 H26B H 0.2493 0.4594 0.4229 0.072 Uiso 0.50 1 calc PR A 2 C28' C 0.2734(8) 0.5555(7) 0.4746(18) 0.103(4) Uani 0.50 1 d PDU A 2 C27' C 0.1921(6) 0.4618(6) 0.3180(13) 0.062(5) Uani 0.50 1 d PDU A 2 H27B H 0.1876 0.4226 0.3142 0.075 Uiso 0.50 1 calc PR A 2 C29' C 0.3305(9) 0.5376(8) 0.6205(19) 0.134(5) Uani 0.50 1 d PDU A 2 H29B H 0.3444 0.5137 0.6713 0.161 Uiso 0.50 1 calc PR A 2 C30' C 0.3426(10) 0.5942(8) 0.6175(19) 0.135(6) Uani 0.50 1 d PDU A 2 H30B H 0.3640 0.6096 0.6692 0.162 Uiso 0.50 1 calc PR A 2 C31' C 0.3232(8) 0.6279(7) 0.5389(18) 0.127(5) Uani 0.50 1 d PDU A 2 H31B H 0.3364 0.6635 0.5321 0.152 Uiso 0.50 1 calc PR A 2 C32' C 0.2853(7) 0.6118(7) 0.4696(18) 0.110(5) Uani 0.50 1 d PDU A 2 H32B H 0.2692 0.6369 0.4232 0.132 Uiso 0.50 1 calc PR A 2 N4' N 0.2968(8) 0.5183(8) 0.5444(16) 0.131(5) Uani 0.50 1 d PDU A 2 C33 C 0.0337(3) 0.3491(3) 0.1516(6) 0.0549(18) Uani 1 1 d D B . C34 C 0.0399(4) 0.2986(3) 0.1519(7) 0.077(3) Uani 1 1 d D . . C35 C 0.0353(9) 0.2387(8) 0.164(2) 0.114(6) Uani 0.50 1 d PU B 1 C36 C 0.0527(9) 0.2032(7) 0.2487(19) 0.117(5) Uani 0.50 1 d PU B 1 H36A H 0.0696 0.2215 0.3039 0.140 Uiso 0.50 1 calc PR B 1 C37 C 0.0473(5) 0.1484(7) 0.2567(18) 0.118(5) Uani 0.50 1 d PU B 1 H37A H 0.0623 0.1289 0.3126 0.141 Uiso 0.50 1 calc PR B 1 C38 C 0.0213(9) 0.1223(8) 0.187(2) 0.125(5) Uani 0.50 1 d PU B 1 N5 N -0.0021(8) 0.1483(7) 0.1023(17) 0.125(5) Uani 0.50 1 d PU B 1 C39 C 0.0066(9) 0.2080(8) 0.092(2) 0.117(6) Uani 0.50 1 d PU B 1 H39A H -0.0078 0.2267 0.0350 0.140 Uiso 0.50 1 calc PR B 1 C40 C 0.0166(9) 0.0591(6) 0.2064(17) 0.157(6) Uani 0.50 1 d PDU . 1 C41 C -0.0088(10) 0.0254(7) 0.1338(13) 0.176(7) Uani 0.50 1 d PDU . 1 H41A H -0.0239 0.0421 0.0722 0.211 Uiso 0.50 1 d PR . 1 C42 C -0.0146(10) -0.0321(7) 0.1530(10) 0.188(7) Uani 0.50 1 d PDU . 1 H42A H -0.0314 -0.0562 0.1023 0.226 Uiso 0.50 1 d PR . 1 C43 C 0.0000 -0.0527(6) 0.2500 0.189(7) Uani 1 2 d SDU . 1 H43A H -0.0117 -0.0877 0.2728 0.226 Uiso 0.50 1 d PR . 1 C44 C 0.0346(10) -0.0225(7) 0.3114(17) 0.177(7) Uani 0.50 1 d PDU . 1 H44A H 0.0568 -0.0416 0.3608 0.212 Uiso 0.50 1 d PR . 1 N6 N 0.0378(9) 0.0355(6) 0.2961(17) 0.168(6) Uani 0.50 1 d PDU . 1 C35' C 0.0501(9) 0.2381(8) 0.143(2) 0.169(8) Uani 0.50 1 d PDU B 2 C36' C 0.0928(8) 0.2199(6) 0.1903(18) 0.171(7) Uani 0.50 1 d PDU B 2 H36B H 0.1116 0.2446 0.2329 0.205 Uiso 0.50 1 calc PRD B 2 C37' C 0.1084(8) 0.1665(7) 0.176(2) 0.165(7) Uani 0.50 1 d PDU B 2 H37B H 0.1385 0.1556 0.2054 0.198 Uiso 0.50 1 calc PR B 2 C38' C 0.0793(10) 0.1292(6) 0.120(2) 0.170(6) Uani 0.50 1 d PDU B 2 C39' C 0.0229(10) 0.2021(11) 0.079(3) 0.171(8) Uani 0.50 1 d PDU B 2 H39B H -0.0054 0.2146 0.0431 0.205 Uiso 0.50 1 calc PR B 2 N5' N 0.0374(10) 0.1476(8) 0.069(2) 0.179(7) Uani 0.50 1 d PDU B 2 C40' C 0.1016(11) 0.0741(7) 0.124(2) 0.180(6) Uani 0.50 1 d PDU B 2 C41' C 0.0712(10) 0.0343(10) 0.076(2) 0.185(7) Uani 0.50 1 d PDU B 2 H41B H 0.0423 0.0453 0.0400 0.222 Uiso 0.50 1 calc PR B 2 C42' C 0.0841(11) -0.0228(8) 0.080(2) 0.192(7) Uani 0.50 1 d PDU B 2 H42B H 0.0635 -0.0503 0.0499 0.230 Uiso 0.50 1 calc PR B 2 C43' C 0.1278(11) -0.0384(7) 0.131(3) 0.194(8) Uani 0.50 1 d PDU B 2 H43B H 0.1377 -0.0760 0.1285 0.233 Uiso 0.50 1 calc PR B 2 C44' C 0.1570(10) 0.0014(9) 0.184(3) 0.190(7) Uani 0.50 1 d PDU B 2 H44B H 0.1849 -0.0098 0.2235 0.228 Uiso 0.50 1 calc PR B 2 N6' N 0.1441(10) 0.0582(8) 0.179(2) 0.187(7) Uani 0.50 1 d PDU B 2 C01 C 0.1959(6) 0.7187(6) 0.5071(8) 0.201(8) Uani 1 1 d DU . . H01A H 0.1847 0.7540 0.4747 0.242 Uiso 1 1 calc RD . . H01B H 0.2197 0.7030 0.4722 0.242 Uiso 1 1 calc R . . C02 C 0.2162(7) 0.7297(9) 0.6142(10) 0.211(8) Uani 1 1 d DU . . H02A H 0.2494 0.7205 0.6267 0.253 Uiso 1 1 calc R . . H02B H 0.2123 0.7692 0.6312 0.253 Uiso 1 1 calc R . . C03 C 0.1899(6) 0.6923(7) 0.6729(7) 0.243(10) Uani 1 1 d DU . . H03A H 0.1708 0.7146 0.7113 0.291 Uiso 1 1 calc R . . H03B H 0.2112 0.6689 0.7185 0.291 Uiso 1 1 calc R . . C04 C 0.1595(7) 0.6561(8) 0.5978(9) 0.213(9) Uani 1 1 d DU . . H04A H 0.1720 0.6178 0.5987 0.256 Uiso 1 1 calc R . . H04C H 0.1280 0.6541 0.6138 0.256 Uiso 1 1 calc R . . O01 O 0.1584(4) 0.6800(5) 0.5040(7) 0.165(4) Uani 1 1 d DU . . 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 0.0429(2) 0.0439(2) 0.0350(2) -0.00432(10) 0.00599(13) -0.00556(10) Si1 0.0599(13) 0.0469(11) 0.0785(16) -0.0056(11) 0.0020(11) -0.0156(10) Si2 0.0867(18) 0.0595(14) 0.0881(18) 0.0022(13) 0.0021(15) -0.0342(13) N1 0.043(3) 0.050(3) 0.027(3) -0.002(2) -0.001(2) -0.008(3) N2 0.052(3) 0.046(3) 0.032(3) -0.005(2) 0.014(3) -0.008(3) C1 0.045(4) 0.047(4) 0.033(4) -0.005(3) 0.007(3) -0.008(3) C2 0.050(4) 0.047(4) 0.039(4) 0.004(3) 0.013(3) -0.006(3) C3 0.055(4) 0.036(3) 0.037(3) 0.003(3) 0.006(3) 0.002(3) C4 0.030(3) 0.051(4) 0.046(4) 0.002(3) 0.001(3) -0.001(3) C5 0.043(4) 0.058(4) 0.021(3) -0.008(3) 0.004(3) -0.010(3) C6 0.047(4) 0.053(4) 0.028(3) -0.004(3) -0.001(3) -0.025(3) C7 0.059(5) 0.055(4) 0.047(4) 0.008(4) -0.015(4) -0.016(4) C8 0.054(5) 0.070(5) 0.051(4) 0.001(4) -0.008(4) -0.022(4) C9 0.054(4) 0.052(4) 0.047(4) 0.001(3) 0.004(3) -0.019(3) C10 0.052(4) 0.045(4) 0.039(3) -0.001(3) 0.005(3) -0.011(3) C11 0.049(4) 0.033(3) 0.043(4) -0.002(3) 0.009(3) -0.010(3) C12 0.031(3) 0.052(4) 0.067(5) 0.006(4) -0.006(3) 0.007(3) C13 0.092(7) 0.056(5) 0.126(9) 0.004(6) -0.002(7) -0.026(5) C14 0.055(5) 0.085(6) 0.092(7) -0.010(5) 0.005(5) -0.017(5) C15 0.107(8) 0.068(6) 0.083(7) -0.025(5) 0.013(6) -0.010(5) C16 0.063(5) 0.056(4) 0.053(4) 0.002(4) -0.002(4) -0.017(4) C17 0.071(5) 0.063(5) 0.063(5) -0.001(4) -0.003(4) -0.024(4) C18 0.154(12) 0.108(9) 0.135(11) -0.004(8) 0.045(10) -0.079(9) C19 0.138(11) 0.071(7) 0.153(12) 0.024(7) -0.036(9) -0.037(7) C20 0.092(7) 0.074(6) 0.100(7) -0.018(5) 0.002(6) -0.034(5) C21 0.056(4) 0.046(4) 0.032(3) -0.005(3) 0.009(3) 0.003(3) C22 0.037(4) 0.049(4) 0.049(4) -0.006(3) 0.002(3) -0.004(3) C23 0.051(4) 0.052(4) 0.056(4) -0.002(4) -0.009(4) -0.008(3) C24 0.059(17) 0.051(15) 0.047(13) 0.013(12) -0.009(12) -0.009(11) N3 0.056(8) 0.069(8) 0.095(10) 0.006(8) -0.010(8) -0.011(6) C25 0.050(6) 0.054(6) 0.101(8) -0.005(6) -0.020(6) -0.006(5) C26 0.046(7) 0.041(6) 0.107(9) -0.010(7) -0.029(7) 0.006(5) C27 0.056(9) 0.046(8) 0.115(12) -0.006(8) -0.013(9) -0.002(7) C28 0.062(6) 0.072(6) 0.118(8) -0.001(7) -0.024(6) -0.013(6) C29 0.084(8) 0.105(9) 0.154(11) -0.011(9) -0.033(8) -0.018(8) C30 0.082(8) 0.102(9) 0.139(10) -0.006(9) -0.027(8) -0.024(8) C31 0.071(8) 0.081(8) 0.121(10) 0.000(8) -0.023(8) -0.025(7) C32 0.055(7) 0.063(7) 0.108(9) 0.003(7) -0.025(7) -0.018(6) N4 0.076(7) 0.098(8) 0.151(10) -0.006(8) -0.029(8) -0.018(7) C24' 0.054(14) 0.08(2) 0.11(3) -0.03(2) -0.022(19) 0.013(14) N3' 0.076(10) 0.080(9) 0.119(11) -0.009(9) -0.019(9) 0.002(8) C25' 0.065(7) 0.061(6) 0.109(8) -0.016(7) -0.021(7) -0.006(6) C26' 0.046(7) 0.044(6) 0.080(8) -0.010(6) -0.021(6) -0.005(5) C28' 0.085(8) 0.074(7) 0.130(9) -0.023(7) -0.040(7) -0.006(6) C27' 0.055(8) 0.049(8) 0.070(10) -0.008(7) -0.026(7) -0.008(7) C29' 0.122(10) 0.099(9) 0.154(11) -0.035(9) -0.060(9) -0.011(8) C30' 0.122(10) 0.096(9) 0.160(12) -0.038(9) -0.058(9) -0.018(8) C31' 0.110(10) 0.087(9) 0.160(11) -0.032(9) -0.048(9) -0.023(8) C32' 0.094(9) 0.072(8) 0.145(10) -0.026(8) -0.043(8) -0.014(7) N4' 0.120(9) 0.099(8) 0.150(10) -0.026(8) -0.052(8) -0.002(8) C33 0.051(4) 0.053(4) 0.058(5) -0.011(4) 0.001(3) -0.012(4) C34 0.086(7) 0.058(5) 0.074(6) -0.025(4) -0.021(5) 0.014(5) C35 0.130(10) 0.042(7) 0.128(10) -0.028(7) -0.103(9) 0.031(7) C36 0.139(10) 0.042(6) 0.134(10) -0.009(7) -0.086(9) 0.014(7) C37 0.142(10) 0.037(6) 0.138(10) 0.000(7) -0.089(9) 0.015(7) C38 0.138(9) 0.043(6) 0.157(9) 0.004(6) -0.091(8) 0.027(6) N5 0.123(9) 0.057(6) 0.155(10) -0.021(7) -0.098(8) 0.032(7) C39 0.131(10) 0.039(6) 0.141(10) -0.035(7) -0.096(9) 0.029(7) C40 0.169(11) 0.064(7) 0.203(12) -0.002(7) -0.075(9) 0.023(7) C41 0.181(13) 0.080(9) 0.232(14) -0.004(9) -0.075(11) 0.017(9) C42 0.193(14) 0.091(9) 0.246(15) -0.002(8) -0.073(12) 0.008(8) C43 0.198(14) 0.091(8) 0.244(15) 0.000 -0.066(12) 0.000 C44 0.194(14) 0.073(9) 0.232(14) 0.009(8) -0.060(12) -0.001(8) N6 0.190(13) 0.065(7) 0.217(13) 0.015(8) -0.062(11) 0.007(8) C35' 0.27(2) 0.055(9) 0.179(15) -0.042(10) 0.032(14) 0.032(11) C36' 0.273(19) 0.054(8) 0.183(14) -0.034(9) 0.031(14) 0.037(10) C37' 0.270(19) 0.046(7) 0.181(14) -0.034(9) 0.044(13) 0.040(10) C38' 0.275(18) 0.053(7) 0.191(13) -0.021(8) 0.065(12) 0.025(9) C39' 0.274(19) 0.060(9) 0.182(14) -0.039(10) 0.045(14) 0.019(11) N5' 0.280(19) 0.072(8) 0.192(14) -0.030(9) 0.058(13) 0.014(10) C40' 0.279(18) 0.067(8) 0.209(14) -0.009(9) 0.088(13) 0.022(9) C41' 0.281(19) 0.071(9) 0.221(15) -0.003(10) 0.097(14) 0.015(11) C42' 0.29(2) 0.081(10) 0.229(16) 0.001(11) 0.099(15) 0.014(12) C43' 0.29(2) 0.082(10) 0.232(16) 0.000(11) 0.098(15) 0.014(12) C44' 0.28(2) 0.081(10) 0.227(16) 0.001(11) 0.099(14) 0.020(11) N6' 0.284(19) 0.076(8) 0.220(15) -0.004(10) 0.096(14) 0.024(11) C01 0.196(16) 0.264(19) 0.133(13) -0.017(13) -0.007(12) -0.115(15) C02 0.207(17) 0.29(2) 0.114(12) -0.001(14) -0.028(12) -0.103(16) C03 0.32(2) 0.229(18) 0.144(14) 0.038(13) -0.062(15) -0.187(16) C04 0.227(17) 0.266(18) 0.121(12) 0.038(13) -0.050(12) -0.159(15) O01 0.140(8) 0.227(12) 0.123(7) -0.007(8) 0.005(6) -0.098(8) _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 C33 1.946(7) . ? Pt1 C21 1.955(7) . ? Pt1 N1 2.058(5) . ? Pt1 N2 2.069(6) . ? Pt1 Pt1 3.2196(5) 2 ? Si1 C12 1.847(8) . ? Si1 C15 1.848(10) . ? Si1 C14 1.853(9) . ? Si1 C13 1.858(10) . ? Si2 C19 1.826(12) . ? Si2 C20 1.852(10) . ? Si2 C17 1.870(8) . ? Si2 C18 1.870(13) . ? N1 C1 1.348(9) . ? N1 C5 1.366(8) . ? N2 C6 1.339(9) . ? N2 C10 1.346(8) . ? C1 C2 1.397(10) . ? C2 C3 1.388(10) . ? C2 C11 1.460(9) . ? C3 C4 1.386(9) . ? C4 C5 1.374(9) . ? C5 C6 1.512(9) . ? C6 C7 1.397(10) . ? C7 C8 1.388(11) . ? C8 C9 1.400(11) . ? C9 C10 1.401(10) . ? C9 C16 1.438(10) . ? C11 C12 1.192(9) . ? C16 C17 1.196(10) . ? C21 C22 1.203(9) . ? C22 C23 1.435(9) . ? C23 C27' 1.384(9) . ? C23 C24' 1.386(10) . ? C23 C24 1.387(9) . ? C23 C27 1.388(9) . ? C24 N3 1.383(10) . ? N3 C25 1.372(10) . ? C25 C26 1.368(9) . ? C25 C28 1.48(2) . ? C26 C27 1.370(10) . ? C28 C32 1.374(10) . ? C28 N4 1.384(10) . ? C29 C30 1.375(10) . ? C29 N4 1.382(10) . ? C30 C31 1.375(10) . ? C31 C32 1.376(10) . ? C24' N3' 1.382(10) . ? N3' C25' 1.383(10) . ? C25' C26' 1.357(9) . ? C25' C28' 1.47(2) . ? C26' C27' 1.369(9) . ? C28' C32' 1.374(10) . ? C28' N4' 1.382(10) . ? C29' N4' 1.376(10) . ? C29' C30' 1.378(10) . ? C30' C31' 1.374(10) . ? C31' C32' 1.374(10) . ? C33 C34 1.201(8) . ? C34 C35 1.43(2) . ? C34 C35' 1.463(17) . ? C35 C39 1.37(2) . ? C35 C36 1.45(3) . ? C36 C37 1.30(2) . ? C37 C38 1.27(2) . ? C38 N5 1.38(3) . ? C38 C40 1.52(2) . ? N5 C39 1.44(3) . ? C40 C41 1.379(9) . ? C40 N6 1.385(9) . ? C40 C40 1.64(6) 2 ? C40 N6 1.66(4) 2 ? C41 N6 1.38(4) 2 ? C41 C42 1.394(9) . ? C41 C44 1.60(4) 2 ? C42 C44 0.84(4) 2 ? C42 C43 1.401(9) . ? C42 N6 1.90(3) 2 ? C43 C44 1.389(9) 2 ? C43 C44 1.389(9) . ? C43 C42 1.401(9) 2 ? C44 C42 0.84(4) 2 ? C44 N6 1.386(9) . ? C44 C41 1.60(4) 2 ? N6 C41 1.38(4) 2 ? N6 C40 1.66(4) 2 ? N6 C42 1.90(3) 2 ? C35' C36' 1.362(9) . ? C35' C39' 1.365(9) . ? C36' C37' 1.358(8) . ? C37' C38' 1.364(9) . ? C38' N5' 1.361(9) . ? C38' C40' 1.44(2) . ? C39' N5' 1.362(9) . ? C40' C41' 1.374(9) . ? C40' N6' 1.381(9) . ? C41' C42' 1.393(9) . ? C42' C43' 1.382(9) . ? C43' C44' 1.385(9) . ? C44' N6' 1.386(9) . ? C01 O01 1.409(8) . ? C01 C02 1.498(8) . ? C02 C03 1.477(9) . ? C03 C04 1.498(8) . ? C04 O01 1.386(8) . ? 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 C33 Pt1 C21 91.4(3) . . ? C33 Pt1 N1 173.1(2) . . ? C21 Pt1 N1 94.9(2) . . ? C33 Pt1 N2 94.6(3) . . ? C21 Pt1 N2 174.0(2) . . ? N1 Pt1 N2 79.0(2) . . ? C33 Pt1 Pt1 92.4(2) . 2 ? C21 Pt1 Pt1 96.43(19) . 2 ? N1 Pt1 Pt1 89.50(14) . 2 ? N2 Pt1 Pt1 84.04(14) . 2 ? C12 Si1 C15 108.7(4) . . ? C12 Si1 C14 107.0(4) . . ? C15 Si1 C14 111.3(5) . . ? C12 Si1 C13 107.8(4) . . ? C15 Si1 C13 110.8(5) . . ? C14 Si1 C13 111.1(5) . . ? C19 Si2 C20 110.9(6) . . ? C19 Si2 C17 108.9(5) . . ? C20 Si2 C17 107.7(4) . . ? C19 Si2 C18 111.4(7) . . ? C20 Si2 C18 110.0(6) . . ? C17 Si2 C18 107.8(5) . . ? C1 N1 C5 118.6(6) . . ? C1 N1 Pt1 124.4(4) . . ? C5 N1 Pt1 117.0(4) . . ? C6 N2 C10 119.6(6) . . ? C6 N2 Pt1 114.9(4) . . ? C10 N2 Pt1 125.4(5) . . ? N1 C1 C2 121.1(6) . . ? C3 C2 C1 119.4(6) . . ? C3 C2 C11 122.2(6) . . ? C1 C2 C11 118.4(6) . . ? C4 C3 C2 119.6(6) . . ? C5 C4 C3 118.4(6) . . ? N1 C5 C4 123.0(6) . . ? N1 C5 C6 112.0(6) . . ? C4 C5 C6 125.1(6) . . ? N2 C6 C7 122.1(6) . . ? N2 C6 C5 116.6(6) . . ? C7 C6 C5 121.2(7) . . ? C8 C7 C6 118.7(8) . . ? C7 C8 C9 119.3(7) . . ? C8 C9 C10 118.3(6) . . ? C8 C9 C16 121.3(7) . . ? C10 C9 C16 120.3(7) . . ? N2 C10 C9 121.7(7) . . ? C12 C11 C2 172.1(7) . . ? C11 C12 Si1 175.3(7) . . ? C17 C16 C9 178.6(9) . . ? C16 C17 Si2 179.5(9) . . ? C22 C21 Pt1 173.8(6) . . ? C21 C22 C23 174.3(8) . . ? C27' C23 C24' 118.2(14) . . ? C27' C23 C24 116.1(12) . . ? C24' C23 C24 12(4) . . ? C27' C23 C27 26.0(14) . . ? C24' C23 C27 119.5(15) . . ? C24 C23 C27 112.0(13) . . ? C27' C23 C22 116.5(9) . . ? C24' C23 C22 120.1(13) . . ? C24 C23 C22 126.1(10) . . ? C27 C23 C22 120.4(9) . . ? N3 C24 C23 123.7(17) . . ? C25 N3 C24 118.8(17) . . ? C26 C25 N3 121.7(14) . . ? C26 C25 C28 113.6(12) . . ? N3 C25 C28 124.6(12) . . ? C25 C26 C27 115.5(14) . . ? C26 C27 C23 127.4(15) . . ? C32 C28 N4 121.7(15) . . ? C32 C28 C25 113.4(12) . . ? N4 C28 C25 124.6(12) . . ? C30 C29 N4 120.7(19) . . ? C31 C30 C29 117.3(19) . . ? C30 C31 C32 124.5(18) . . ? C28 C32 C31 116.1(15) . . ? C29 N4 C28 119.3(17) . . ? N3' C24' C23 120(2) . . ? C24' N3' C25' 120(2) . . ? C26' C25' N3' 119.5(15) . . ? C26' C25' C28' 112.5(13) . . ? N3' C25' C28' 127.8(13) . . ? C25' C26' C27' 121.2(13) . . ? C32' C28' N4' 123.1(17) . . ? C32' C28' C25' 110.9(14) . . ? N4' C28' C25' 125.9(14) . . ? C26' C27' C23 120.3(13) . . ? N4' C29' C30' 116.7(19) . . ? C31' C30' C29' 120.5(19) . . ? C30' C31' C32' 123(2) . . ? C28' C32' C31' 114.2(17) . . ? C29' N4' C28' 120.8(18) . . ? C34 C33 Pt1 171.9(7) . . ? C33 C34 C35 163.9(17) . . ? C33 C34 C35' 173.7(17) . . ? C35 C34 C35' 22(2) . . ? C39 C35 C34 119.7(17) . . ? C39 C35 C36 110.6(19) . . ? C34 C35 C36 129.3(15) . . ? C37 C36 C35 127.3(18) . . ? C38 C37 C36 118.7(19) . . ? C37 C38 N5 124.0(18) . . ? C37 C38 C40 113.8(18) . . ? N5 C38 C40 122.2(19) . . ? C38 N5 C39 116.3(16) . . ? C35 C39 N5 123(2) . . ? C41 C40 N6 120.3(7) . . ? C41 C40 C38 119.3(16) . . ? N6 C40 C38 120.3(16) . . ? C41 C40 C40 102.0(18) . 2 ? N6 C40 C40 66.0(18) . 2 ? C38 C40 C40 101.8(16) . 2 ? C41 C40 N6 53.2(14) . 2 ? N6 C40 N6 99.5(15) . 2 ? C38 C40 N6 115.7(17) . 2 ? C40 C40 N6 49.6(14) 2 2 ? C40 C41 N6 73.9(18) . 2 ? C40 C41 C42 119.4(8) . . ? N6 C41 C42 86.3(13) 2 . ? C40 C41 C44 108.0(10) . 2 ? N6 C41 C44 54.8(11) 2 2 ? C42 C41 C44 31.7(14) . 2 ? C44 C42 C41 88(2) 2 . ? C44 C42 C43 71.7(13) 2 . ? C41 C42 C43 118.9(8) . . ? C44 C42 N6 41.5(18) 2 2 ? C41 C42 N6 46.6(12) . 2 ? C43 C42 N6 91.0(13) . 2 ? C44 C43 C44 118.6(16) 2 . ? C44 C43 C42 117.7(9) 2 2 ? C44 C43 C42 35.1(19) . 2 ? C44 C43 C42 35.1(19) 2 . ? C44 C43 C42 117.7(9) . . ? C42 C43 C42 139.7(14) 2 . ? C42 C44 N6 115(3) 2 . ? C42 C44 C43 73.2(13) 2 . ? N6 C44 C43 118.1(9) . . ? C42 C44 C41 61(2) 2 2 ? N6 C44 C41 54.7(17) . 2 ? C43 C44 C41 107(2) . 2 ? C41 N6 C40 116(2) 2 . ? C41 N6 C44 70.5(19) 2 . ? C40 N6 C44 119.7(8) . . ? C41 N6 C40 52.9(14) 2 2 ? C40 N6 C40 64(2) . 2 ? C44 N6 C40 104.3(18) . 2 ? C41 N6 C42 47.1(9) 2 2 ? C40 N6 C42 121.6(11) . 2 ? C44 N6 C42 23.7(17) . 2 ? C40 N6 C42 84.2(14) 2 2 ? C36' C35' C39' 119.2(8) . . ? C36' C35' C34 116.4(15) . . ? C39' C35' C34 123.6(16) . . ? C37' C36' C35' 121.3(8) . . ? C36' C37' C38' 119.1(8) . . ? N5' C38' C37' 119.7(8) . . ? N5' C38' C40' 131.2(19) . . ? C37' C38' C40' 109.1(19) . . ? N5' C39' C35' 119.5(8) . . ? C38' N5' C39' 120.9(8) . . ? C41' C40' N6' 121.1(8) . . ? C41' C40' C38' 110(2) . . ? N6' C40' C38' 128(2) . . ? C40' C41' C42' 119.3(8) . . ? C43' C42' C41' 119.7(8) . . ? C42' C43' C44' 120.5(8) . . ? C43' C44' N6' 119.3(8) . . ? C40' N6' C44' 119.8(8) . . ? O01 C01 C02 108.7(5) . . ? C03 C02 C01 105.3(5) . . ? C02 C03 C04 105.5(6) . . ? O01 C04 C03 108.5(6) . . ? C04 O01 C01 109.3(6) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.632 _refine_diff_density_min -1.527 _refine_diff_density_rms 0.128 # Attachment 'CCDC 710905.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 710905' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H24 N6 O Pt' _chemical_formula_weight 775.72 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' Pt Pt -1.7033 8.3905 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall -P2n2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.479(5) _cell_length_b 11.794(3) _cell_length_c 12.660(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3057.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5307 _cell_measurement_theta_min 2.5595 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.2600 _exptl_crystal_size_mid 0.0300 _exptl_crystal_size_min 0.0200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 4.631 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.918 _exptl_absorpt_correction_T_min 0.8451 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _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 Confocal _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 22593 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3511 _reflns_number_gt 2667 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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. DFIX command applied to O-H distances. The unassigned maximum residual density (2.04 e \%A^-3^) is at 1.82 \%A from C8, it should not to be another O atom for short distances to C8 atom. ; _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^)+(0.0595P)^2^+0.9074P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3511 _refine_ls_number_parameters 213 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _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 O1 O 1.0000 0.3467(7) 0.2500 0.077(2) Uani 1 2 d SD . . H1 H 0.958(3) 0.312(9) 0.267(6) 0.16(5) Uiso 1 1 d D . . C8 C 0.0371(3) 0.0610(3) 0.3430(4) 0.0425(11) Uani 1 1 d . . . C9 C 0.0631(2) 0.1210(4) 0.4066(4) 0.0469(11) Uani 1 1 d . . . Pt1 Pt 0.0000 -0.053033(19) 0.2500 0.03674(12) Uani 1 2 d S . . N1 N -0.0326(2) -0.1880(3) 0.1615(3) 0.0386(8) Uani 1 1 d . . . N2 N 0.1315(2) 0.3576(3) 0.5680(3) 0.0514(10) Uani 1 1 d . . . C13 C 0.1534(2) 0.1828(4) 0.6543(4) 0.0460(11) Uani 1 1 d . . . H13 H 0.1716 0.1444 0.7113 0.055 Uiso 1 1 calc R . . C12 C 0.1229(2) 0.1237(4) 0.5747(4) 0.0477(12) Uani 1 1 d . . . H12 H 0.1203 0.0450 0.5781 0.057 Uiso 1 1 calc R . . C14 C 0.1567(2) 0.2999(4) 0.6490(4) 0.0444(11) Uani 1 1 d . . . C4 C -0.0845(2) -0.2728(4) 0.0122(4) 0.0454(11) Uani 1 1 d . . . C1 C -0.0182(2) -0.2928(4) 0.1992(4) 0.0413(10) Uani 1 1 d . . . N3 N 0.2117(2) 0.3067(4) 0.8162(3) 0.0553(11) Uani 1 1 d . . . C18 C 0.2408(3) 0.4813(6) 0.9019(5) 0.0696(17) Uani 1 1 d . . . H18 H 0.2591 0.5178 0.9599 0.084 Uiso 1 1 calc R . . C11 C 0.0961(2) 0.1808(4) 0.4895(4) 0.0406(10) Uani 1 1 d . . . C19 C 0.2379(3) 0.3650(6) 0.8963(4) 0.0647(15) Uani 1 1 d . . . H19 H 0.2553 0.3239 0.9523 0.078 Uiso 1 1 calc R . . C2 C -0.0359(2) -0.3896(4) 0.1447(4) 0.0461(11) Uani 1 1 d . . . H2 H -0.0256 -0.4608 0.1715 0.055 Uiso 1 1 calc R . . C10 C 0.1022(3) 0.2981(4) 0.4914(4) 0.0514(12) Uani 1 1 d . . . H10 H 0.0846 0.3385 0.4351 0.062 Uiso 1 1 calc R . . C15 C 0.1870(2) 0.3657(5) 0.7359(4) 0.0450(12) Uani 1 1 d . . . C5 C -0.0644(2) -0.1792(4) 0.0709(4) 0.0440(11) Uani 1 1 d . . . H5 H -0.0739 -0.1071 0.0453 0.053 Uiso 1 1 calc R . . C16 C 0.1886(4) 0.4837(6) 0.7339(5) 0.0629(17) Uani 1 1 d . . . H16 H 0.1718 0.5235 0.6767 0.076 Uiso 1 1 calc R . . C3 C -0.0690(3) -0.3796(4) 0.0506(4) 0.0504(12) Uani 1 1 d . . . H3 H -0.0809 -0.4441 0.0129 0.060 Uiso 1 1 calc R . . C17 C 0.2160(3) 0.5409(5) 0.8193(6) 0.0732(19) Uani 1 1 d . . . H17 H 0.2172 0.6197 0.8198 0.088 Uiso 1 1 calc R . . C6 C -0.1196(3) -0.2513(4) -0.0852(4) 0.0575(14) Uani 1 1 d . . . C7 C -0.1479(4) -0.2256(6) -0.1601(5) 0.087(2) Uani 1 1 d . . . H7 H -0.1707 -0.2049 -0.2206 0.104 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 O1 0.099(6) 0.063(4) 0.070(5) 0.000 -0.010(3) 0.000 C8 0.060(3) 0.029(2) 0.039(3) 0.0056(18) -0.004(2) 0.000(2) C9 0.055(3) 0.036(2) 0.049(3) -0.003(2) 0.002(2) 0.000(2) Pt1 0.04527(19) 0.03138(16) 0.03356(17) 0.000 -0.00431(10) 0.000 N1 0.046(2) 0.034(2) 0.036(2) 0.0015(15) -0.0050(17) 0.0000(17) N2 0.063(3) 0.038(2) 0.054(3) -0.0004(19) -0.011(2) -0.0013(18) C13 0.049(3) 0.044(3) 0.045(3) 0.001(2) -0.005(2) 0.001(2) C12 0.058(3) 0.037(2) 0.048(3) -0.003(2) -0.002(2) 0.002(2) C14 0.046(3) 0.043(2) 0.044(3) -0.001(2) 0.004(2) -0.004(2) C4 0.054(3) 0.043(3) 0.040(3) 0.001(2) -0.002(2) 0.001(2) C1 0.051(3) 0.037(2) 0.036(3) -0.005(2) -0.003(2) -0.003(2) N3 0.059(3) 0.055(3) 0.052(3) -0.009(2) -0.006(2) 0.007(2) C18 0.068(4) 0.075(4) 0.066(4) -0.028(3) -0.014(3) -0.004(3) C11 0.046(3) 0.038(3) 0.038(3) -0.006(2) 0.005(2) -0.0030(19) C19 0.061(4) 0.081(4) 0.051(3) -0.013(3) -0.012(3) 0.005(3) C2 0.049(3) 0.037(2) 0.052(3) 0.003(2) 0.001(2) -0.004(2) C10 0.064(3) 0.046(3) 0.044(3) -0.003(2) -0.013(2) 0.003(2) C15 0.036(3) 0.049(3) 0.050(3) -0.008(2) 0.002(2) -0.004(2) C5 0.052(3) 0.039(2) 0.041(3) -0.0009(19) -0.008(2) -0.002(2) C16 0.073(4) 0.050(3) 0.066(4) -0.001(3) -0.005(3) -0.016(3) C3 0.059(3) 0.041(3) 0.051(3) -0.005(2) -0.005(2) -0.004(2) C17 0.091(5) 0.050(3) 0.078(5) -0.016(3) -0.008(4) -0.021(3) C6 0.069(4) 0.048(3) 0.056(3) -0.010(3) -0.019(3) -0.003(3) C7 0.102(5) 0.087(5) 0.071(4) -0.004(4) -0.039(4) 0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 H1 0.98(3) . ? C8 C9 1.196(6) . ? C8 Pt1 1.943(5) . ? C9 C11 1.433(6) . ? Pt1 C8 1.943(5) 3 ? Pt1 N1 2.057(3) . ? Pt1 N1 2.057(3) 3 ? N1 C5 1.324(5) . ? N1 C1 1.358(6) . ? N2 C10 1.339(6) . ? N2 C14 1.335(6) . ? C13 C12 1.375(6) . ? C13 C14 1.384(6) . ? C13 H13 0.9300 . ? C12 C11 1.386(6) . ? C12 H12 0.9300 . ? C14 C15 1.482(6) . ? C4 C3 1.388(6) . ? C4 C5 1.393(6) . ? C4 C6 1.450(7) . ? C1 C2 1.382(6) . ? C1 C1 1.488(10) 3 ? N3 C15 1.331(7) . ? N3 C19 1.338(6) . ? C18 C17 1.360(9) . ? C18 C19 1.375(8) . ? C18 H18 0.9300 . ? C11 C10 1.390(6) . ? C19 H19 0.9300 . ? C2 C3 1.376(6) . ? C2 H2 0.9300 . ? C10 H10 0.9300 . ? C15 C16 1.393(8) . ? C5 H5 0.9300 . ? C16 C17 1.391(8) . ? C16 H16 0.9300 . ? C3 H3 0.9300 . ? C17 H17 0.9300 . ? C6 C7 1.152(8) . ? C7 H7 0.9300 . ? 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 C9 C8 Pt1 172.4(4) . . ? C8 C9 C11 173.2(5) . . ? C8 Pt1 C8 92.4(3) . 3 ? C8 Pt1 N1 173.00(16) . . ? C8 Pt1 N1 94.52(16) 3 . ? C8 Pt1 N1 94.52(16) . 3 ? C8 Pt1 N1 173.00(16) 3 3 ? N1 Pt1 N1 78.65(19) . 3 ? C5 N1 C1 118.9(4) . . ? C5 N1 Pt1 124.8(3) . . ? C1 N1 Pt1 116.3(3) . . ? C10 N2 C14 117.5(4) . . ? C12 C13 C14 119.5(5) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C12 C11 120.3(4) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? N2 C14 C13 121.8(4) . . ? N2 C14 C15 117.7(4) . . ? C13 C14 C15 120.5(5) . . ? C3 C4 C5 117.7(4) . . ? C3 C4 C6 124.8(4) . . ? C5 C4 C6 117.5(4) . . ? N1 C1 C2 121.4(4) . . ? N1 C1 C1 114.4(2) . 3 ? C2 C1 C1 124.3(3) . 3 ? C15 N3 C19 117.6(5) . . ? C17 C18 C19 117.4(5) . . ? C17 C18 H18 121.3 . . ? C19 C18 H18 121.3 . . ? C12 C11 C10 115.7(4) . . ? C12 C11 C9 121.2(4) . . ? C10 C11 C9 123.0(5) . . ? N3 C19 C18 124.7(6) . . ? N3 C19 H19 117.6 . . ? C18 C19 H19 117.6 . . ? C3 C2 C1 119.4(4) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? N2 C10 C11 125.1(5) . . ? N2 C10 H10 117.4 . . ? C11 C10 H10 117.4 . . ? N3 C15 C16 121.8(5) . . ? N3 C15 C14 116.9(5) . . ? C16 C15 C14 121.3(5) . . ? N1 C5 C4 123.1(4) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C17 C16 C15 118.7(6) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C2 C3 C4 119.6(4) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C18 C17 C16 119.8(6) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C7 C6 C4 174.7(6) . . ? C6 C7 H7 180.0 . . ? 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 C7 H7 N3 0.93 2.70 3.509(9) 146.1(5) 4_556 C17 H17 N3 0.93 2.64 3.466(8) 148.0(4) 8_665 C2 H2 O1 0.93 2.53 3.461(9) 178.0(3) 1_445 O1 H1 Cg1 0.99 2.51 3.521 158.7 6_656 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.035 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.089