Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name J.Rourke _publ_contact_author_address ; Department of Chemistry University of Warwick Coventry CV4 7AL UNITED KINGDOM ; _publ_contact_author_email J.ROURKE@WARWICK.AC.UK _publ_section_title ; Carbene or Zwitterion? Competition in Organoplatinum Complexes. ; loop_ _publ_author_name 'J. Rourke' 'N. Alcock' 'Guy Clarkson' 'Christopher P. Newman' # Attachment 'cn1.cif' data_cn1 _database_code_depnum_ccdc_archive 'CCDC 294673' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H84 Cl2 N O4 P Pt' _chemical_formula_weight 1216.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9888(3) _cell_length_b 13.3067(4) _cell_length_c 21.2775(6) _cell_angle_alpha 75.4120(10) _cell_angle_beta 85.0940(10) _cell_angle_gamma 66.880(2) _cell_volume 3020.82(15) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2891 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _exptl_crystal_description plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 2.482 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5998 _exptl_absorpt_correction_T_max 0.9072 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique Set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(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 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 15439 _diffrn_reflns_av_R_equivalents 0.1747 _diffrn_reflns_av_sigmaI/netI 0.4251 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10273 _reflns_number_gt 3225 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0455P)^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 SHELXL _refine_ls_extinction_coef 0.0021(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10273 _refine_ls_number_parameters 632 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.2878 _refine_ls_R_factor_gt 0.0898 _refine_ls_wR_factor_ref 0.2043 _refine_ls_wR_factor_gt 0.1421 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.878 _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 0.81359(6) 0.44285(8) 0.23521(4) 0.0635(4) Uani 1 1 d . . . Cl1 Cl 0.8236(3) 0.5638(4) 0.2978(3) 0.0787(18) Uani 1 1 d . . . Cl2 Cl 1.0047(3) 0.4309(4) 0.1867(2) 0.0708(16) Uani 1 1 d . . . P10 P 0.8039(4) 0.3257(5) 0.1797(3) 0.0673(18) Uani 1 1 d . . . C11 C 0.9053(16) 0.1802(16) 0.2145(10) 0.076(6) Uani 1 1 d . . . C12 C 0.8936(18) 0.089(2) 0.2027(11) 0.104(8) Uani 1 1 d . . . H12D H 0.8258 0.1025 0.1769 0.125 Uiso 1 1 calc R . . C13 C 0.972(2) -0.023(2) 0.2248(14) 0.139(11) Uani 1 1 d . . . H13E H 0.9580 -0.0842 0.2160 0.166 Uiso 1 1 calc R . . C14 C 1.069(2) -0.039(2) 0.2600(15) 0.131(11) Uani 1 1 d . . . H14G H 1.1251 -0.1136 0.2767 0.158 Uiso 1 1 calc R . . C15 C 1.0895(17) 0.044(2) 0.2718(12) 0.109(9) Uani 1 1 d . . . H15A H 1.1604 0.0285 0.2956 0.131 Uiso 1 1 calc R . . C16 C 1.0081(17) 0.1582(18) 0.2499(9) 0.079(7) Uani 1 1 d . . . H16A H 1.0237 0.2177 0.2592 0.095 Uiso 1 1 calc R . . C21 C 0.8318(16) 0.356(2) 0.0940(11) 0.074(7) Uani 1 1 d . . . C22 C 0.8588(16) 0.279(2) 0.0570(12) 0.095(8) Uani 1 1 d . . . H22A H 0.8679 0.2049 0.0792 0.114 Uiso 1 1 calc R . . C23 C 0.873(2) 0.298(3) -0.0061(16) 0.114(10) Uani 1 1 d . . . H23A H 0.8849 0.2434 -0.0299 0.137 Uiso 1 1 calc R . . C24 C 0.8705(17) 0.410(3) -0.0368(13) 0.106(10) Uani 1 1 d . . . H24A H 0.8849 0.4289 -0.0821 0.128 Uiso 1 1 calc R . . C25 C 0.8480(18) 0.487(2) -0.0026(15) 0.099(8) Uani 1 1 d . . . H25A H 0.8443 0.5598 -0.0238 0.118 Uiso 1 1 calc R . . C26 C 0.8297(16) 0.460(2) 0.0651(14) 0.080(8) Uani 1 1 d . . . H26A H 0.8162 0.5136 0.0899 0.096 Uiso 1 1 calc R . . C31 C 0.6550(15) 0.3196(17) 0.1790(11) 0.058(6) Uani 1 1 d . . . C32 C 0.615(2) 0.2597(19) 0.2337(12) 0.090(8) Uani 1 1 d . . . H32A H 0.6728 0.2151 0.2678 0.107 Uiso 1 1 calc R . . C33 C 0.498(3) 0.259(2) 0.2433(12) 0.101(9) Uani 1 1 d . . . H33A H 0.4748 0.2147 0.2805 0.122 Uiso 1 1 calc R . . C34 C 0.419(2) 0.331(3) 0.1922(15) 0.105(9) Uani 1 1 d . . . H34A H 0.3359 0.3403 0.1965 0.126 Uiso 1 1 calc R . . C35 C 0.4517(15) 0.389(2) 0.1363(11) 0.084(8) Uani 1 1 d . . . H35A H 0.3944 0.4328 0.1020 0.101 Uiso 1 1 calc R . . C36 C 0.5731(14) 0.3816(16) 0.1303(9) 0.076(7) Uani 1 1 d . . . H36A H 0.5972 0.4210 0.0914 0.091 Uiso 1 1 calc R . . C101 C 0.8326(17) -0.204(2) 0.9149(11) 0.132(10) Uani 1 1 d . . . H10A H 0.8756 -0.2299 0.8772 0.198 Uiso 1 1 calc R . . H10B H 0.8634 -0.2637 0.9544 0.198 Uiso 1 1 calc R . . H10C H 0.8457 -0.1373 0.9184 0.198 Uiso 1 1 calc R . . C102 C 0.7036(19) -0.175(2) 0.9073(10) 0.139(11) Uani 1 1 d . . . H10D H 0.6571 -0.1390 0.9418 0.167 Uiso 1 1 calc R . . H10E H 0.6873 -0.2434 0.9091 0.167 Uiso 1 1 calc R . . C103 C 0.669(3) -0.092(3) 0.8387(15) 0.186(12) Uani 1 1 d DU . . H10F H 0.7238 -0.0509 0.8322 0.223 Uiso 1 1 calc R . . H10G H 0.6936 -0.1398 0.8072 0.223 Uiso 1 1 calc R . . C104 C 0.559(3) -0.013(3) 0.8177(19) 0.239(17) Uani 1 1 d DU . . H10H H 0.5361 0.0338 0.8499 0.287 Uiso 1 1 calc R . . H10I H 0.5053 -0.0552 0.8257 0.287 Uiso 1 1 calc R . . C105 C 0.517(2) 0.064(3) 0.7591(11) 0.140(11) Uani 1 1 d . . . H10J H 0.4355 0.0680 0.7507 0.168 Uiso 1 1 calc R . . H10K H 0.5707 0.0334 0.7246 0.168 Uiso 1 1 calc R . . C106 C 0.5089(19) 0.179(2) 0.7517(13) 0.095(8) Uani 1 1 d . . . H10L H 0.5889 0.1764 0.7623 0.114 Uiso 1 1 calc R . . H10M H 0.4497 0.2135 0.7831 0.114 Uiso 1 1 calc R . . C107 C 0.4720(16) 0.249(2) 0.6862(11) 0.096(8) Uani 1 1 d . . . H10N H 0.4618 0.3270 0.6840 0.115 Uiso 1 1 calc R . . H10O H 0.3940 0.2492 0.6737 0.115 Uiso 1 1 calc R . . O108 O 0.5684(11) 0.1996(12) 0.6423(8) 0.087(5) Uani 1 1 d . . . C109 C 0.5537(16) 0.2482(18) 0.5810(13) 0.071(6) Uani 1 1 d . . . C110 C 0.4505(14) 0.3478(17) 0.5530(11) 0.067(6) Uani 1 1 d . . . H11C H 0.3857 0.3812 0.5796 0.080 Uiso 1 1 calc R . . C111 C 0.4472(15) 0.3952(19) 0.4851(12) 0.074(7) Uani 1 1 d . . . C112 C 0.5452(15) 0.3613(16) 0.4452(12) 0.057(6) Uani 1 1 d . . . C113 C 0.6461(13) 0.2623(16) 0.4755(10) 0.064(6) Uani 1 1 d . . . H11D H 0.7131 0.2314 0.4495 0.077 Uiso 1 1 calc R . . C114 C 0.6503(15) 0.2101(16) 0.5402(11) 0.063(4) Uani 1 1 d . . . H11E H 0.7209 0.1465 0.5576 0.075 Uiso 1 1 calc R . . C115 C 0.5510(17) 0.4131(19) 0.3788(13) 0.075(7) Uani 1 1 d . . . N116 N 0.4448(12) 0.4710(13) 0.3445(9) 0.067(5) Uani 1 1 d . . . H11B H 0.3774 0.4739 0.3653 0.080 Uiso 1 1 calc R . . C117 C 0.4351(14) 0.5242(17) 0.2813(11) 0.062(6) Uani 1 1 d . . . C118 C 0.5431(15) 0.5177(17) 0.2478(9) 0.081(7) Uani 1 1 d . . . H11A H 0.5394 0.5561 0.2034 0.097 Uiso 1 1 calc R . . C119 C 0.6585(14) 0.4539(16) 0.2798(11) 0.063(4) Uani 1 1 d . . . C120 C 0.6531(15) 0.4085(14) 0.3465(10) 0.060(6) Uani 1 1 d . . . H12B H 0.7273 0.3717 0.3705 0.072 Uiso 1 1 calc R . . C121 C 0.3129(14) 0.598(2) 0.2470(11) 0.067(7) Uani 1 1 d . . . C122 C 0.2126(16) 0.567(2) 0.2661(12) 0.073(7) Uani 1 1 d . . . C123 C 0.1026(14) 0.6299(19) 0.2330(11) 0.067(7) Uani 1 1 d . . . H12A H 0.0325 0.6139 0.2463 0.081 Uiso 1 1 calc R . . C124 C 0.0986(16) 0.7173(19) 0.1796(10) 0.063(6) Uani 1 1 d . . . C125 C 0.1965(15) 0.7458(17) 0.1662(10) 0.075(7) Uani 1 1 d . . . H12C H 0.1871 0.8126 0.1339 0.090 Uiso 1 1 calc R . . C126 C 0.3021(17) 0.688(2) 0.1943(11) 0.079(7) Uani 1 1 d . . . H12E H 0.3700 0.7073 0.1794 0.094 Uiso 1 1 calc R . . O127 O -0.0074(9) 0.7818(10) 0.1436(5) 0.071(4) Uani 1 1 d . . . C128 C -0.1140(14) 0.7569(16) 0.1582(10) 0.090(7) Uani 1 1 d . . . H12H H -0.1488 0.7759 0.1995 0.108 Uiso 1 1 calc R . . H12I H -0.0938 0.6759 0.1624 0.108 Uiso 1 1 calc R . . C129 C -0.2011(14) 0.8247(19) 0.1046(8) 0.075(6) Uani 1 1 d . . . H12F H -0.1638 0.8043 0.0639 0.090 Uiso 1 1 calc R . . H12G H -0.2731 0.8045 0.1124 0.090 Uiso 1 1 calc R . . C130 C -0.2416(14) 0.9465(17) 0.0952(9) 0.070(6) Uani 1 1 d . . . H13K H -0.1694 0.9662 0.0918 0.084 Uiso 1 1 calc R . . H13L H -0.2868 0.9682 0.1340 0.084 Uiso 1 1 calc R . . C131 C -0.3231(14) 1.016(2) 0.0344(10) 0.094(8) Uani 1 1 d . . . H13M H -0.2766 0.9964 -0.0045 0.113 Uiso 1 1 calc R . . H13N H -0.3933 0.9932 0.0369 0.113 Uiso 1 1 calc R . . C132 C -0.3705(18) 1.143(2) 0.0261(10) 0.099(8) Uani 1 1 d . . . H13O H -0.4166 1.1640 0.0649 0.119 Uiso 1 1 calc R . . H13P H -0.3017 1.1678 0.0212 0.119 Uiso 1 1 calc R . . C133 C -0.453(2) 1.2002(19) -0.0342(12) 0.124(9) Uani 1 1 d . . . H13Q H -0.4070 1.1757 -0.0723 0.148 Uiso 1 1 calc R . . H13R H -0.5225 1.1768 -0.0282 0.148 Uiso 1 1 calc R . . C134 C -0.494(2) 1.315(2) -0.0457(13) 0.170(13) Uani 1 1 d . . . H13S H -0.4310 1.3409 -0.0667 0.254 Uiso 1 1 calc R . . H13T H -0.5158 1.3380 -0.0045 0.254 Uiso 1 1 calc R . . H13U H -0.5664 1.3495 -0.0742 0.254 Uiso 1 1 calc R . . O135 O 0.2316(10) 0.4723(13) 0.3165(7) 0.074(5) Uani 1 1 d . B . C136 C 0.1312(14) 0.4345(18) 0.3307(9) 0.082(7) Uani 1 1 d U . . H13A H 0.0674 0.4829 0.3550 0.099 Uiso 1 1 calc R A 1 H13B H 0.0950 0.4367 0.2900 0.099 Uiso 1 1 calc R A 1 C137 C 0.184(2) 0.319(2) 0.3699(12) 0.119(9) Uiso 0.50 1 d P B 1 H37A H 0.1672 0.3311 0.4144 0.143 Uiso 0.50 1 calc PR B 1 H37B H 0.1240 0.2888 0.3624 0.143 Uiso 0.50 1 calc PR B 1 C38A C 0.289(6) 0.223(6) 0.380(3) 0.19(2) Uiso 0.50 1 d P B 1 H38A H 0.3544 0.2531 0.3730 0.224 Uiso 0.50 1 calc PR B 1 H38D H 0.2922 0.1922 0.3419 0.224 Uiso 0.50 1 calc PR B 1 C39A C 0.335(5) 0.126(6) 0.432(3) 0.18(3) Uiso 0.50 1 d P B 1 H39A H 0.2615 0.1117 0.4479 0.213 Uiso 0.50 1 calc PR B 1 H39D H 0.3808 0.0658 0.4091 0.213 Uiso 0.50 1 calc PR B 1 C40A C 0.404(3) 0.091(3) 0.4892(19) 0.083(12) Uiso 0.50 1 d P B 1 H40A H 0.3492 0.1221 0.5230 0.099 Uiso 0.50 1 calc PR B 1 H40B H 0.4651 0.1250 0.4813 0.099 Uiso 0.50 1 calc PR B 1 C41A C 0.468(6) -0.030(6) 0.516(3) 0.19(3) Uiso 0.50 1 d P B 1 H41A H 0.5231 -0.0659 0.4838 0.230 Uiso 0.50 1 calc PR B 1 H41B H 0.4092 -0.0673 0.5294 0.230 Uiso 0.50 1 calc PR B 1 C42A C 0.542(4) -0.041(5) 0.577(2) 0.145(19) Uiso 0.50 1 d P B 1 H42A H 0.5477 -0.1100 0.6098 0.218 Uiso 0.50 1 calc PR B 1 H42B H 0.5003 0.0242 0.5955 0.218 Uiso 0.50 1 calc PR B 1 H42C H 0.6234 -0.0454 0.5638 0.218 Uiso 0.50 1 calc PR B 1 C37A C 0.184(2) 0.319(2) 0.3699(12) 0.119(9) Uiso 0.50 1 d P B 2 H37C H 0.2162 0.3153 0.4121 0.143 Uiso 0.50 1 calc PR B 2 H37D H 0.2477 0.2691 0.3466 0.143 Uiso 0.50 1 calc PR B 2 C38B C 0.067(3) 0.293(3) 0.3781(16) 0.065(10) Uiso 0.50 1 d P B 2 H38B H 0.0041 0.3436 0.4014 0.078 Uiso 0.50 1 calc PR B 2 H38C H 0.0338 0.3004 0.3353 0.078 Uiso 0.50 1 calc PR B 2 C39B C 0.107(3) 0.177(3) 0.4158(19) 0.092(13) Uiso 0.50 1 d P B 2 H39B H 0.1499 0.1686 0.4555 0.111 Uiso 0.50 1 calc PR B 2 H39C H 0.1638 0.1266 0.3900 0.111 Uiso 0.50 1 calc PR B 2 C40B C -0.002(3) 0.141(4) 0.435(2) 0.106(14) Uiso 0.50 1 d P B 2 H40C H -0.0438 0.1765 0.4708 0.127 Uiso 0.50 1 calc PR B 2 H40D H -0.0590 0.1752 0.3975 0.127 Uiso 0.50 1 calc PR B 2 C41B C 0.017(4) 0.028(4) 0.454(2) 0.095(15) Uiso 0.50 1 d P B 2 H41C H 0.1029 -0.0135 0.4693 0.114 Uiso 0.50 1 calc PR B 2 H41G H 0.0090 0.0041 0.4151 0.114 Uiso 0.50 1 calc PR B 2 C42B C -0.055(3) -0.011(4) 0.503(2) 0.095(15) Uiso 0.50 1 d P B 2 H42D H -0.0030 -0.0805 0.5329 0.143 Uiso 0.50 1 calc PR B 2 H42E H -0.1156 -0.0256 0.4830 0.143 Uiso 0.50 1 calc PR B 2 H42F H -0.0961 0.0465 0.5279 0.143 Uiso 0.50 1 calc PR B 2 O143 O 0.3463(10) 0.4882(11) 0.4571(6) 0.087(5) Uani 1 1 d . . . C144 C 0.2374(16) 0.519(2) 0.4937(12) 0.131(11) Uani 1 1 d . . . H14H H 0.2500 0.5405 0.5331 0.157 Uiso 1 1 calc R . . H14I H 0.2077 0.4574 0.5066 0.157 Uiso 1 1 calc R . . C145 C 0.1429(16) 0.628(2) 0.4424(10) 0.103(8) Uani 1 1 d . D . H14J H 0.1599 0.6949 0.4425 0.124 Uiso 1 1 calc R . . H14K H 0.1600 0.6143 0.3983 0.124 Uiso 1 1 calc R . . C146 C 0.019(3) 0.653(3) 0.4541(18) 0.222(17) Uani 1 1 d . . . H14L H 0.0017 0.6592 0.4997 0.267 Uiso 1 1 calc R C 1 H14M H -0.0023 0.5916 0.4478 0.267 Uiso 1 1 calc R C 1 C147 C -0.065(2) 0.774(3) 0.4040(16) 0.189(15) Uani 0.67 1 d PD D 1 H14A H -0.0669 0.8368 0.4215 0.227 Uiso 0.67 1 calc PR D 1 H14B H -0.0243 0.7795 0.3615 0.227 Uiso 0.67 1 calc PR D 1 C148 C -0.184(4) 0.788(5) 0.394(3) 0.29(3) Uiso 0.67 1 d PD D 1 H14C H -0.2359 0.8040 0.4318 0.346 Uiso 0.67 1 calc PR D 1 H14D H -0.1886 0.7220 0.3820 0.346 Uiso 0.67 1 calc PR D 1 C149 C -0.211(4) 0.883(5) 0.340(2) 0.175(18) Uiso 0.67 1 d PD D 1 H14E H -0.2854 0.8939 0.3177 0.210 Uiso 0.67 1 calc PR D 1 H14F H -0.1439 0.8698 0.3093 0.210 Uiso 0.67 1 calc PR D 1 C150 C -0.232(4) 0.990(4) 0.362(3) 0.22(2) Uiso 0.67 1 d PD D 1 H15B H -0.2431 0.9768 0.4088 0.334 Uiso 0.67 1 calc PR D 1 H15C H -0.3038 1.0512 0.3396 0.334 Uiso 0.67 1 calc PR D 1 H15D H -0.1607 1.0098 0.3506 0.334 Uiso 0.67 1 calc PR D 1 C47A C -0.065(2) 0.774(3) 0.4040(16) 0.189(15) Uani 0.33 1 d P D 2 H14N H -0.0465 0.8375 0.4095 0.227 Uiso 0.33 1 calc PR D 2 H14O H -0.0533 0.7691 0.3581 0.227 Uiso 0.33 1 calc PR D 2 C48A C -0.190(12) 0.784(13) 0.426(8) 0.29(3) Uiso 0.33 1 d P D 2 H48A H -0.2017 0.7959 0.4709 0.346 Uiso 0.33 1 calc PR D 2 H48B H -0.2015 0.7143 0.4267 0.346 Uiso 0.33 1 calc PR D 2 C49A C -0.302(8) 0.907(8) 0.369(5) 0.175(18) Uiso 0.33 1 d P D 2 H49A H -0.2718 0.9179 0.3241 0.210 Uiso 0.33 1 calc PR D 2 H49B H -0.3819 0.9010 0.3693 0.210 Uiso 0.33 1 calc PR D 2 C50A C -0.305(9) 0.994(9) 0.401(5) 0.22(2) Uiso 0.33 1 d P D 2 H50A H -0.3589 1.0682 0.3765 0.334 Uiso 0.33 1 calc PR D 2 H50B H -0.2229 0.9930 0.4024 0.334 Uiso 0.33 1 calc PR D 2 H50C H -0.3346 0.9793 0.4453 0.334 Uiso 0.33 1 calc PR D 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 0.0314(4) 0.0786(7) 0.0908(7) -0.0473(5) -0.0084(3) -0.0135(3) Cl1 0.039(3) 0.094(5) 0.124(5) -0.078(4) 0.002(3) -0.016(3) Cl2 0.043(3) 0.084(4) 0.098(4) -0.053(3) -0.004(2) -0.018(2) P10 0.041(3) 0.088(5) 0.087(4) -0.054(4) -0.003(3) -0.020(3) C11 0.068(14) 0.040(15) 0.128(19) -0.048(14) 0.005(13) -0.013(11) C12 0.082(16) 0.067(19) 0.17(2) -0.078(18) 0.005(14) -0.009(14) C13 0.059(16) 0.10(2) 0.26(3) -0.11(2) -0.017(18) 0.000(15) C14 0.10(2) 0.06(2) 0.23(3) -0.04(2) -0.01(2) -0.017(16) C15 0.046(13) 0.11(3) 0.16(2) -0.05(2) -0.019(13) 0.000(16) C16 0.060(13) 0.075(18) 0.108(17) -0.064(14) -0.008(12) -0.005(12) C21 0.064(13) 0.09(2) 0.079(19) -0.049(17) -0.002(11) -0.025(13) C22 0.090(16) 0.15(3) 0.067(18) -0.061(19) 0.027(13) -0.058(15) C23 0.104(19) 0.14(3) 0.12(3) -0.08(2) 0.000(17) -0.038(19) C24 0.049(13) 0.19(3) 0.10(2) -0.08(3) 0.003(13) -0.038(18) C25 0.097(18) 0.11(2) 0.11(2) -0.03(2) -0.026(16) -0.052(16) C26 0.075(14) 0.09(2) 0.08(2) -0.044(18) -0.019(13) -0.022(14) C31 0.053(12) 0.063(16) 0.082(17) -0.045(13) 0.018(12) -0.033(11) C32 0.063(15) 0.11(2) 0.10(2) -0.046(18) -0.002(14) -0.027(14) C33 0.13(2) 0.10(2) 0.09(2) -0.028(17) -0.019(18) -0.046(18) C34 0.10(2) 0.14(3) 0.13(3) -0.11(2) 0.05(2) -0.069(19) C35 0.043(12) 0.17(2) 0.061(16) -0.023(16) 0.010(11) -0.064(14) C36 0.026(10) 0.105(17) 0.092(16) -0.003(13) -0.029(10) -0.025(10) C101 0.068(16) 0.16(3) 0.16(2) -0.09(2) 0.019(15) -0.009(15) C102 0.093(18) 0.19(3) 0.073(19) -0.020(19) 0.022(14) 0.003(17) C103 0.165(19) 0.22(2) 0.153(18) -0.064(16) -0.013(15) -0.034(15) C104 0.26(2) 0.22(2) 0.22(2) -0.075(18) 0.033(18) -0.061(17) C105 0.15(2) 0.17(3) 0.050(17) -0.02(2) 0.016(15) -0.02(2) C106 0.081(16) 0.061(19) 0.15(3) -0.041(19) 0.005(15) -0.028(14) C107 0.045(13) 0.11(2) 0.10(2) -0.020(18) -0.018(13) 0.000(13) O108 0.044(8) 0.095(13) 0.103(13) -0.025(11) 0.010(9) -0.008(8) C109 0.038(13) 0.070(18) 0.11(2) -0.031(16) 0.002(14) -0.019(12) C110 0.031(11) 0.084(18) 0.087(18) -0.036(14) 0.006(11) -0.016(11) C111 0.037(12) 0.11(2) 0.11(2) -0.080(17) -0.009(13) -0.020(12) C112 0.039(12) 0.051(15) 0.090(18) -0.040(14) 0.017(12) -0.015(11) C113 0.021(9) 0.076(16) 0.098(17) -0.051(14) 0.020(10) -0.006(10) C114 0.044(8) 0.060(11) 0.094(12) -0.042(10) -0.007(8) -0.015(7) C115 0.034(12) 0.11(2) 0.10(2) -0.061(17) 0.007(14) -0.022(12) N116 0.028(9) 0.083(13) 0.100(15) -0.053(12) -0.003(9) -0.013(8) C117 0.032(11) 0.091(17) 0.083(17) -0.051(15) -0.010(12) -0.025(11) C118 0.044(12) 0.13(2) 0.083(15) -0.069(14) -0.023(11) -0.018(12) C119 0.044(8) 0.060(11) 0.094(12) -0.042(10) -0.007(8) -0.015(7) C120 0.051(12) 0.053(14) 0.072(16) -0.032(12) -0.017(11) -0.001(10) C121 0.025(10) 0.11(2) 0.092(18) -0.069(15) -0.014(11) -0.018(11) C122 0.037(14) 0.11(2) 0.10(2) -0.070(17) -0.006(13) -0.025(14) C123 0.022(10) 0.11(2) 0.087(18) -0.072(16) -0.012(11) -0.006(11) C124 0.048(13) 0.074(17) 0.059(16) -0.041(13) -0.011(12) 0.003(12) C125 0.015(9) 0.097(18) 0.127(19) -0.047(14) -0.003(11) -0.023(11) C126 0.050(14) 0.12(2) 0.086(19) -0.043(16) 0.014(12) -0.041(14) O127 0.039(7) 0.106(11) 0.070(9) -0.045(8) -0.011(6) -0.012(7) C128 0.029(11) 0.083(17) 0.16(2) -0.042(16) -0.028(12) -0.010(10) C129 0.037(11) 0.12(2) 0.064(14) -0.010(14) -0.022(10) -0.024(12) C130 0.035(10) 0.069(16) 0.086(16) 0.009(13) -0.036(10) -0.009(10) C131 0.036(11) 0.15(2) 0.105(18) -0.054(18) 0.001(11) -0.023(13) C132 0.084(16) 0.12(2) 0.100(19) 0.009(18) -0.050(14) -0.057(15) C133 0.16(2) 0.037(17) 0.15(3) -0.011(17) 0.004(19) -0.016(16) C134 0.19(3) 0.10(3) 0.16(3) -0.05(2) 0.04(2) 0.00(2) O135 0.042(8) 0.085(12) 0.106(13) -0.048(10) -0.017(8) -0.016(8) C136 0.027(10) 0.15(2) 0.083(15) -0.029(14) -0.017(9) -0.044(12) O143 0.029(7) 0.104(12) 0.119(11) -0.055(10) -0.005(7) 0.003(7) C144 0.031(12) 0.17(3) 0.21(3) -0.13(2) -0.001(15) -0.007(14) C145 0.031(11) 0.18(3) 0.111(19) -0.067(18) 0.019(12) -0.034(14) C146 0.18(3) 0.18(4) 0.31(5) -0.10(4) 0.10(3) -0.07(3) C147 0.068(18) 0.19(3) 0.24(4) -0.07(3) -0.03(2) 0.046(19) C47A 0.068(18) 0.19(3) 0.24(4) -0.07(3) -0.03(2) 0.046(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C119 1.983(18) . ? Pt1 P10 2.220(5) . ? Pt1 Cl1 2.374(4) . ? Pt1 Cl2 2.394(4) . ? P10 C21 1.80(2) . ? P10 C31 1.820(17) . ? P10 C11 1.832(19) . ? C11 C12 1.37(2) . ? C11 C16 1.39(2) . ? C12 C13 1.40(3) . ? C12 H12D 0.9500 . ? C13 C14 1.36(3) . ? C13 H13E 0.9500 . ? C14 C15 1.31(3) . ? C14 H14G 0.9500 . ? C15 C16 1.42(3) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C21 C26 1.35(3) . ? C21 C22 1.37(2) . ? C22 C23 1.31(3) . ? C22 H22A 0.9500 . ? C23 C24 1.46(3) . ? C23 H23A 0.9500 . ? C24 C25 1.33(3) . ? C24 H24A 0.9500 . ? C25 C26 1.41(3) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C31 C36 1.35(2) . ? C31 C32 1.40(3) . ? C32 C33 1.41(3) . ? C32 H32A 0.9500 . ? C33 C34 1.39(3) . ? C33 H33A 0.9500 . ? C34 C35 1.36(3) . ? C34 H34A 0.9500 . ? C35 C36 1.42(2) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C101 C102 1.45(2) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C102 C103 1.57(3) . ? C102 H10D 0.9900 . ? C102 H10E 0.9900 . ? C103 C104 1.342(18) . ? C103 H10F 0.9900 . ? C103 H10G 0.9900 . ? C104 C105 1.38(4) . ? C104 H10H 0.9900 . ? C104 H10I 0.9900 . ? C105 C106 1.46(3) . ? C105 H10J 0.9900 . ? C105 H10K 0.9900 . ? C106 C107 1.46(3) . ? C106 H10L 0.9900 . ? C106 H10M 0.9900 . ? C107 O108 1.47(2) . ? C107 H10N 0.9900 . ? C107 H10O 0.9900 . ? O108 C109 1.30(2) . ? C109 C114 1.39(2) . ? C109 C110 1.44(2) . ? C110 C111 1.42(2) . ? C110 H11C 0.9500 . ? C111 C112 1.38(2) . ? C111 O143 1.39(2) . ? C112 C115 1.42(2) . ? C112 C113 1.44(2) . ? C113 C114 1.37(2) . ? C113 H11D 0.9500 . ? C114 H11E 0.9500 . ? C115 C120 1.34(2) . ? C115 N116 1.36(2) . ? N116 C117 1.34(2) . ? N116 H11B 0.8800 . ? C117 C118 1.41(2) . ? C117 C121 1.53(2) . ? C118 C119 1.43(2) . ? C118 H11A 0.9500 . ? C119 C120 1.40(2) . ? C120 H12B 0.9500 . ? C121 C126 1.39(2) . ? C121 C122 1.41(3) . ? C122 O135 1.39(2) . ? C122 C123 1.39(2) . ? C123 C124 1.39(2) . ? C123 H12A 0.9500 . ? C124 C125 1.36(2) . ? C124 O127 1.385(19) . ? C125 C126 1.30(2) . ? C125 H12C 0.9500 . ? C126 H12E 0.9500 . ? O127 C128 1.433(18) . ? C128 C129 1.47(2) . ? C128 H12H 0.9900 . ? C128 H12I 0.9900 . ? C129 C130 1.46(2) . ? C129 H12F 0.9900 . ? C129 H12G 0.9900 . ? C130 C131 1.54(2) . ? C130 H13K 0.9900 . ? C130 H13L 0.9900 . ? C131 C132 1.53(2) . ? C131 H13M 0.9900 . ? C131 H13N 0.9900 . ? C132 C133 1.53(3) . ? C132 H13O 0.9900 . ? C132 H13P 0.9900 . ? C133 C134 1.37(3) . ? C133 H13Q 0.9900 . ? C133 H13R 0.9900 . ? C134 H13S 0.9800 . ? C134 H13T 0.9800 . ? C134 H13U 0.9800 . ? O135 C136 1.460(19) . ? C136 C137 1.46(3) . ? C136 H13A 0.9900 . ? C136 H13B 0.9900 . ? C137 C38A 1.39(6) . ? C137 H37A 0.9900 . ? C137 H37B 0.9900 . ? C38A C39A 1.43(7) . ? C38A H38A 0.9900 . ? C38A H38D 0.9900 . ? C39A C40A 1.40(6) . ? C39A H39A 0.9900 . ? C39A H39D 0.9900 . ? C40A C41A 1.47(7) . ? C40A H40A 0.9900 . ? C40A H40B 0.9900 . ? C41A C42A 1.58(7) . ? C41A H41A 0.9900 . ? C41A H41B 0.9900 . ? C42A H42A 0.9800 . ? C42A H42B 0.9800 . ? C42A H42C 0.9800 . ? C38B C39B 1.45(5) . ? C38B H38B 0.9900 . ? C38B H38C 0.9900 . ? C39B C40B 1.54(5) . ? C39B H39B 0.9900 . ? C39B H39C 0.9900 . ? C40B C41B 1.39(5) . ? C40B H40C 0.9900 . ? C40B H40D 0.9900 . ? C41B C42B 1.42(4) . ? C41B H41C 0.9900 . ? C41B H41G 0.9900 . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 0.9800 . ? O143 C144 1.431(19) . ? C144 C145 1.64(3) . ? C144 H14H 0.9900 . ? C144 H14I 0.9900 . ? C145 C146 1.40(3) . ? C145 H14J 0.9900 . ? C145 H14K 0.9900 . ? C146 C147 1.67(4) . ? C146 H14L 0.9900 . ? C146 H14M 0.9900 . ? C147 C148 1.40(2) . ? C147 H14A 0.9900 . ? C147 H14B 0.9900 . ? C148 C149 1.43(2) . ? C148 H14C 0.9900 . ? C148 H14D 0.9900 . ? C149 C150 1.52(6) . ? C149 H14E 0.9900 . ? C149 H14F 0.9900 . ? C150 H15B 0.9800 . ? C150 H15C 0.9800 . ? C150 H15D 0.9800 . ? C48A C49A 1.87(14) . ? C48A H48A 0.9900 . ? C48A H48B 0.9900 . ? C49A C50A 1.48(11) . ? C49A H49A 0.9900 . ? C49A H49B 0.9900 . ? C50A H50A 0.9800 . ? C50A H50B 0.9800 . ? C50A H50C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C119 Pt1 P10 93.2(5) . . ? C119 Pt1 Cl1 85.8(5) . . ? P10 Pt1 Cl1 178.1(2) . . ? C119 Pt1 Cl2 176.8(6) . . ? P10 Pt1 Cl2 89.60(16) . . ? Cl1 Pt1 Cl2 91.38(15) . . ? C21 P10 C31 100.2(9) . . ? C21 P10 C11 107.5(10) . . ? C31 P10 C11 104.4(10) . . ? C21 P10 Pt1 117.6(9) . . ? C31 P10 Pt1 114.2(5) . . ? C11 P10 Pt1 111.7(7) . . ? C12 C11 C16 115.8(18) . . ? C12 C11 P10 123.7(17) . . ? C16 C11 P10 120.2(16) . . ? C11 C12 C13 126(2) . . ? C11 C12 H12D 116.9 . . ? C13 C12 H12D 116.9 . . ? C14 C13 C12 115(2) . . ? C14 C13 H13E 122.6 . . ? C12 C13 H13E 122.6 . . ? C15 C14 C13 123(3) . . ? C15 C14 H14G 118.5 . . ? C13 C14 H14G 118.5 . . ? C14 C15 C16 122(2) . . ? C14 C15 H15A 119.1 . . ? C16 C15 H15A 119.1 . . ? C11 C16 C15 118.5(19) . . ? C11 C16 H16A 120.8 . . ? C15 C16 H16A 120.8 . . ? C26 C21 C22 118(2) . . ? C26 C21 P10 118(2) . . ? C22 C21 P10 124(2) . . ? C23 C22 C21 126(3) . . ? C23 C22 H22A 116.8 . . ? C21 C22 H22A 116.8 . . ? C22 C23 C24 115(3) . . ? C22 C23 H23A 122.7 . . ? C24 C23 H23A 122.7 . . ? C25 C24 C23 121(3) . . ? C25 C24 H24A 119.5 . . ? C23 C24 H24A 119.5 . . ? C24 C25 C26 120(3) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C21 C26 C25 119(2) . . ? C21 C26 H26A 120.6 . . ? C25 C26 H26A 120.6 . . ? C36 C31 C32 116.6(17) . . ? C36 C31 P10 122.8(18) . . ? C32 C31 P10 120.2(17) . . ? C31 C32 C33 126(2) . . ? C31 C32 H32A 116.8 . . ? C33 C32 H32A 116.8 . . ? C34 C33 C32 112(3) . . ? C34 C33 H33A 123.9 . . ? C32 C33 H33A 123.9 . . ? C35 C34 C33 125(2) . . ? C35 C34 H34A 117.6 . . ? C33 C34 H34A 117.6 . . ? C34 C35 C36 119(2) . . ? C34 C35 H35A 120.6 . . ? C36 C35 H35A 120.6 . . ? C31 C36 C35 121.0(19) . . ? C31 C36 H36A 119.5 . . ? C35 C36 H36A 119.5 . . ? C102 C101 H10A 109.5 . . ? C102 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C102 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C101 C102 C103 105(2) . . ? C101 C102 H10D 110.8 . . ? C103 C102 H10D 110.8 . . ? C101 C102 H10E 110.8 . . ? C103 C102 H10E 110.8 . . ? H10D C102 H10E 108.9 . . ? C104 C103 C102 128(3) . . ? C104 C103 H10F 105.4 . . ? C102 C103 H10F 105.4 . . ? C104 C103 H10G 105.4 . . ? C102 C103 H10G 105.4 . . ? H10F C103 H10G 106.0 . . ? C103 C104 C105 133(4) . . ? C103 C104 H10H 103.9 . . ? C105 C104 H10H 103.9 . . ? C103 C104 H10I 103.9 . . ? C105 C104 H10I 103.9 . . ? H10H C104 H10I 105.4 . . ? C104 C105 C106 119(3) . . ? C104 C105 H10J 107.7 . . ? C106 C105 H10J 107.7 . . ? C104 C105 H10K 107.7 . . ? C106 C105 H10K 107.7 . . ? H10J C105 H10K 107.1 . . ? C105 C106 C107 113(2) . . ? C105 C106 H10L 109.0 . . ? C107 C106 H10L 109.0 . . ? C105 C106 H10M 109.0 . . ? C107 C106 H10M 109.0 . . ? H10L C106 H10M 107.8 . . ? C106 C107 O108 106.9(17) . . ? C106 C107 H10N 110.3 . . ? O108 C107 H10N 110.3 . . ? C106 C107 H10O 110.3 . . ? O108 C107 H10O 110.3 . . ? H10N C107 H10O 108.6 . . ? C109 O108 C107 117.4(16) . . ? O108 C109 C114 117.7(19) . . ? O108 C109 C110 124.6(19) . . ? C114 C109 C110 117(2) . . ? C111 C110 C109 119.1(18) . . ? C111 C110 H11C 120.4 . . ? C109 C110 H11C 120.4 . . ? C112 C111 O143 117(2) . . ? C112 C111 C110 123.4(19) . . ? O143 C111 C110 119.7(17) . . ? C111 C112 C115 126(2) . . ? C111 C112 C113 115(2) . . ? C115 C112 C113 119.6(17) . . ? C114 C113 C112 123.4(16) . . ? C114 C113 H11D 118.3 . . ? C112 C113 H11D 118.3 . . ? C113 C114 C109 121.6(19) . . ? C113 C114 H11E 119.2 . . ? C109 C114 H11E 119.2 . . ? C120 C115 N116 117(2) . . ? C120 C115 C112 125.2(19) . . ? N116 C115 C112 117.7(18) . . ? C117 N116 C115 124.9(18) . . ? C117 N116 H11B 117.5 . . ? C115 N116 H11B 117.5 . . ? N116 C117 C118 117.5(16) . . ? N116 C117 C121 122.7(18) . . ? C118 C117 C121 120(2) . . ? C117 C118 C119 120.8(19) . . ? C117 C118 H11A 119.6 . . ? C119 C118 H11A 119.6 . . ? C120 C119 C118 114.7(16) . . ? C120 C119 Pt1 122.5(14) . . ? C118 C119 Pt1 122.5(17) . . ? C115 C120 C119 124.8(18) . . ? C115 C120 H12B 117.6 . . ? C119 C120 H12B 117.6 . . ? C126 C121 C122 120.2(19) . . ? C126 C121 C117 121(2) . . ? C122 C121 C117 119(2) . . ? O135 C122 C123 124(2) . . ? O135 C122 C121 117.1(19) . . ? C123 C122 C121 119(3) . . ? C122 C123 C124 118(2) . . ? C122 C123 H12A 121.1 . . ? C124 C123 H12A 121.1 . . ? C125 C124 O127 119(2) . . ? C125 C124 C123 119.5(18) . . ? O127 C124 C123 120.9(19) . . ? C126 C125 C124 125(2) . . ? C126 C125 H12C 117.6 . . ? C124 C125 H12C 117.6 . . ? C125 C126 C121 117.9(19) . . ? C125 C126 H12E 121.0 . . ? C121 C126 H12E 121.0 . . ? C124 O127 C128 120.8(16) . . ? O127 C128 C129 107.4(17) . . ? O127 C128 H12H 110.2 . . ? C129 C128 H12H 110.2 . . ? O127 C128 H12I 110.2 . . ? C129 C128 H12I 110.2 . . ? H12H C128 H12I 108.5 . . ? C130 C129 C128 115.2(15) . . ? C130 C129 H12F 108.5 . . ? C128 C129 H12F 108.5 . . ? C130 C129 H12G 108.5 . . ? C128 C129 H12G 108.5 . . ? H12F C129 H12G 107.5 . . ? C129 C130 C131 114.1(16) . . ? C129 C130 H13K 108.7 . . ? C131 C130 H13K 108.7 . . ? C129 C130 H13L 108.7 . . ? C131 C130 H13L 108.7 . . ? H13K C130 H13L 107.6 . . ? C132 C131 C130 114.3(16) . . ? C132 C131 H13M 108.7 . . ? C130 C131 H13M 108.7 . . ? C132 C131 H13N 108.7 . . ? C130 C131 H13N 108.7 . . ? H13M C131 H13N 107.6 . . ? C133 C132 C131 108.5(18) . . ? C133 C132 H13O 110.0 . . ? C131 C132 H13O 110.0 . . ? C133 C132 H13P 110.0 . . ? C131 C132 H13P 110.0 . . ? H13O C132 H13P 108.4 . . ? C134 C133 C132 111(2) . . ? C134 C133 H13Q 109.4 . . ? C132 C133 H13Q 109.4 . . ? C134 C133 H13R 109.4 . . ? C132 C133 H13R 109.4 . . ? H13Q C133 H13R 108.0 . . ? C133 C134 H13S 109.5 . . ? C133 C134 H13T 109.5 . . ? H13S C134 H13T 109.5 . . ? C133 C134 H13U 109.5 . . ? H13S C134 H13U 109.5 . . ? H13T C134 H13U 109.5 . . ? C122 O135 C136 116.3(14) . . ? C137 C136 O135 105.7(16) . . ? C137 C136 H13A 110.6 . . ? O135 C136 H13A 110.6 . . ? C137 C136 H13B 110.6 . . ? O135 C136 H13B 110.6 . . ? H13A C136 H13B 108.7 . . ? C38A C137 C136 142(4) . . ? C38A C137 H37A 101.4 . . ? C136 C137 H37A 101.4 . . ? C38A C137 H37B 101.4 . . ? C136 C137 H37B 101.4 . . ? H37A C137 H37B 104.6 . . ? C137 C38A C39A 134(6) . . ? C137 C38A H38A 103.7 . . ? C39A C38A H38A 103.7 . . ? C137 C38A H38D 103.7 . . ? C39A C38A H38D 103.7 . . ? H38A C38A H38D 105.4 . . ? C40A C39A C38A 139(6) . . ? C40A C39A H39A 102.5 . . ? C38A C39A H39A 102.5 . . ? C40A C39A H39D 102.5 . . ? C38A C39A H39D 102.5 . . ? H39A C39A H39D 104.9 . . ? C39A C40A C41A 119(5) . . ? C39A C40A H40A 107.7 . . ? C41A C40A H40A 107.7 . . ? C39A C40A H40B 107.7 . . ? C41A C40A H40B 107.7 . . ? H40A C40A H40B 107.1 . . ? C40A C41A C42A 106(5) . . ? C40A C41A H41A 110.5 . . ? C42A C41A H41A 110.5 . . ? C40A C41A H41B 110.5 . . ? C42A C41A H41B 110.5 . . ? H41A C41A H41B 108.7 . . ? C39B C38B H38B 110.8 . . ? C39B C38B H38C 110.8 . . ? H38B C38B H38C 108.9 . . ? C38B C39B C40B 111(3) . . ? C38B C39B H39B 109.4 . . ? C40B C39B H39B 109.4 . . ? C38B C39B H39C 109.4 . . ? C40B C39B H39C 109.4 . . ? H39B C39B H39C 108.0 . . ? C41B C40B C39B 120(4) . . ? C41B C40B H40C 107.3 . . ? C39B C40B H40C 107.3 . . ? C41B C40B H40D 107.3 . . ? C39B C40B H40D 107.3 . . ? H40C C40B H40D 106.9 . . ? C40B C41B C42B 121(4) . . ? C40B C41B H41C 107.1 . . ? C42B C41B H41C 107.1 . . ? C40B C41B H41G 107.1 . . ? C42B C41B H41G 107.1 . . ? H41C C41B H41G 106.8 . . ? C41B C42B H42D 109.5 . . ? C41B C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C41B C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C111 O143 C144 119.1(18) . . ? O143 C144 C145 102.8(18) . . ? O143 C144 H14H 111.2 . . ? C145 C144 H14H 111.2 . . ? O143 C144 H14I 111.2 . . ? C145 C144 H14I 111.2 . . ? H14H C144 H14I 109.1 . . ? C146 C145 C144 116(2) . . ? C146 C145 H14J 108.2 . . ? C144 C145 H14J 108.2 . . ? C146 C145 H14K 108.2 . . ? C144 C145 H14K 108.2 . . ? H14J C145 H14K 107.4 . . ? C145 C146 C147 111(3) . . ? C145 C146 H14L 109.5 . . ? C147 C146 H14L 109.5 . . ? C145 C146 H14M 109.5 . . ? C147 C146 H14M 109.5 . . ? H14L C146 H14M 108.1 . . ? C148 C147 C146 115(3) . . ? C148 C147 H14A 108.4 . . ? C146 C147 H14A 108.4 . . ? C148 C147 H14B 108.4 . . ? C146 C147 H14B 108.4 . . ? H14A C147 H14B 107.5 . . ? C147 C148 C149 97(3) . . ? C147 C148 H14C 112.4 . . ? C149 C148 H14C 112.4 . . ? C147 C148 H14D 112.4 . . ? C149 C148 H14D 112.4 . . ? H14C C148 H14D 110.0 . . ? C148 C149 C150 112(4) . . ? C148 C149 H14E 109.2 . . ? C150 C149 H14E 109.2 . . ? C148 C149 H14F 109.2 . . ? C150 C149 H14F 109.2 . . ? H14E C149 H14F 107.9 . . ? C149 C150 H15B 109.5 . . ? C149 C150 H15C 109.5 . . ? H15B C150 H15C 109.5 . . ? C149 C150 H15D 109.5 . . ? H15B C150 H15D 109.5 . . ? H15C C150 H15D 109.5 . . ? C49A C48A H48A 110.0 . . ? C49A C48A H48B 110.0 . . ? H48A C48A H48B 108.4 . . ? C50A C49A C48A 97(8) . . ? C50A C49A H49A 112.4 . . ? C48A C49A H49A 112.4 . . ? C50A C49A H49B 112.4 . . ? C48A C49A H49B 112.4 . . ? H49A C49A H49B 110.0 . . ? C49A C50A H50A 109.5 . . ? C49A C50A H50B 109.5 . . ? H50A C50A H50B 109.5 . . ? C49A C50A H50C 109.5 . . ? H50A C50A H50C 109.5 . . ? H50B C50A H50C 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 N116 H11B O135 0.88 2.12 2.666(17) 119.8 . N116 H11B O143 0.88 2.00 2.60(2) 124.6 . _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.179 _refine_diff_density_min -1.136 _refine_diff_density_rms 0.132