data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Esther Garcia Fernandez' "Dami\'an Fern\'andez-Anca" "M. I. Garc\'ia-Seijo" _publ_contact_author_name 'Esther Garcia Fernandez' _publ_contact_author_email MESTHER.GARCIA@USC.ES _publ_section_title ; Tripodal Polyphosphine Ligands as Inductors of Chelate Ring-Opening Processes in mononuclear Palladium(II) and Platinum(II) Compounds. The X-ray Crystal Structure of a Bromo and a Nitrate Derivative Containing Dangling Phosphorus. ; # Attachment 'PdBr.cif' data_PdBr _database_code_depnum_ccdc_archive 'CCDC 737980' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Pd(PP3)2]Br2.2CHCl3 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H84 Br2 Cl12 P8 Pd' _chemical_formula_weight 2080.93 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' Br Br -0.2901 2.4595 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.947(3) _cell_length_b 18.070(4) _cell_length_c 17.514(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.043(4) _cell_angle_gamma 90.00 _cell_volume 4719.0(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 971 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 25.98 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 1.561 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5401 _exptl_absorpt_correction_T_max 0.6349 _exptl_absorpt_process_details Sadabs _exptl_special_details ; [Pd(PP3)2]Br2.4CHCl3 ; _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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39885 _diffrn_reflns_av_R_equivalents 0.1652 _diffrn_reflns_av_sigmaI/netI 0.1598 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 26.43 _reflns_number_total 9662 _reflns_number_gt 4204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction 'BRUKER Shelxtl' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0670P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9662 _refine_ls_number_parameters 502 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1376 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1579 _refine_ls_wR_factor_gt 0.1359 _refine_ls_goodness_of_fit_ref 0.846 _refine_ls_restrained_S_all 0.846 _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 Cl1 Cl 0.35876(13) 0.30591(12) 0.31029(13) 0.0887(7) Uani 1 1 d . . . Cl3 Cl 0.17259(13) 0.32966(14) 0.26705(13) 0.0971(7) Uani 1 1 d . . . Cl4 Cl 0.81744(18) 0.32063(13) 0.70688(14) 0.1090(8) Uani 1 1 d . . . Cl6 Cl 0.97828(15) 0.38308(16) 0.78013(16) 0.1211(9) Uani 1 1 d . . . Cl5 Cl 0.87458(16) 0.46771(15) 0.67028(15) 0.1108(8) Uani 1 1 d . . . C101 C 0.8688(5) 0.4016(4) 0.7426(4) 0.067(2) Uani 1 1 d . . . C100 C 0.2661(4) 0.3652(4) 0.3216(4) 0.0613(19) Uani 1 1 d . . . Pd1 Pd 0.5000 0.0000 0.5000 0.02915(16) Uani 1 2 d S . . Br1 Br 0.32638(5) -0.00004(5) 0.69488(4) 0.0740(3) Uani 1 1 d . . . P2 P 0.40415(9) 0.03510(8) 0.39578(8) 0.0332(4) Uani 1 1 d . . . P1 P 0.55675(9) 0.11951(8) 0.48867(8) 0.0336(4) Uani 1 1 d . . . P3 P 0.45462(11) 0.28851(9) 0.64884(10) 0.0477(4) Uani 1 1 d . . . P4 P 0.83095(11) 0.19122(10) 0.43199(10) 0.0497(5) Uani 1 1 d . . . C31 C 0.8929(4) 0.1541(4) 0.5173(4) 0.0479(16) Uani 1 1 d . . . C5 C 0.6769(3) 0.1213(3) 0.4739(3) 0.0385(14) Uani 1 1 d . . . H5A H 0.7086 0.0950 0.5159 0.046 Uiso 1 1 calc R . . H5B H 0.6866 0.0946 0.4272 0.046 Uiso 1 1 calc R . . C1 C 0.5011(4) 0.1635(3) 0.4022(3) 0.0405(14) Uani 1 1 d . . . H1A H 0.4523 0.1947 0.4170 0.049 Uiso 1 1 calc R . . H1B H 0.5438 0.1947 0.3780 0.049 Uiso 1 1 calc R . . C3 C 0.5454(3) 0.1863(3) 0.5649(3) 0.0411(15) Uani 1 1 d . . . H3A H 0.5784 0.1677 0.6106 0.049 Uiso 1 1 calc R . . H3B H 0.5743 0.2318 0.5507 0.049 Uiso 1 1 calc R . . C17 C 0.2016(5) 0.1060(4) 0.5223(4) 0.062(2) Uani 1 1 d . . . H17 H 0.1844 0.0998 0.5719 0.074 Uiso 1 1 calc R . . C13 C 0.3037(3) 0.0804(3) 0.4256(3) 0.0378(14) Uani 1 1 d . . . C7 C 0.3666(4) -0.0335(3) 0.3260(3) 0.0389(14) Uani 1 1 d . . . C2 C 0.4647(4) 0.1053(3) 0.3458(3) 0.0395(14) Uani 1 1 d . . . H2A H 0.5138 0.0825 0.3211 0.047 Uiso 1 1 calc R . . H2B H 0.4248 0.1282 0.3066 0.047 Uiso 1 1 calc R . . C6 C 0.7182(3) 0.1989(3) 0.4685(4) 0.0450(15) Uani 1 1 d . . . H6A H 0.7227 0.2220 0.5186 0.054 Uiso 1 1 calc R . . H6B H 0.6802 0.2296 0.4343 0.054 Uiso 1 1 calc R . . C18 C 0.2807(4) 0.0727(3) 0.4998(4) 0.0435(15) Uani 1 1 d . . . H18 H 0.3171 0.0456 0.5348 0.052 Uiso 1 1 calc R . . C19 C 0.3395(4) 0.3237(3) 0.6365(3) 0.0438(15) Uani 1 1 d . . . C4 C 0.4505(4) 0.2055(3) 0.5858(3) 0.0430(15) Uani 1 1 d . . . H4A H 0.4251 0.1641 0.6121 0.052 Uiso 1 1 calc R . . H4B H 0.4127 0.2154 0.5397 0.052 Uiso 1 1 calc R . . C12 C 0.4287(4) -0.0658(3) 0.2798(4) 0.0512(17) Uani 1 1 d . . . H12 H 0.4878 -0.0493 0.2823 0.061 Uiso 1 1 calc R . . C32 C 0.9055(4) 0.0779(4) 0.5205(5) 0.0641(19) Uani 1 1 d . . . H32 H 0.8845 0.0485 0.4795 0.077 Uiso 1 1 calc R . . C42 C 0.8272(5) 0.3459(4) 0.4663(4) 0.0619(19) Uani 1 1 d . . . H42 H 0.7752 0.3373 0.4912 0.074 Uiso 1 1 calc R . . C36 C 0.9265(4) 0.1963(4) 0.5787(4) 0.064(2) Uani 1 1 d . . . H36 H 0.9190 0.2474 0.5771 0.077 Uiso 1 1 calc R . . C41 C 0.8609(5) 0.4173(4) 0.4641(4) 0.072(2) Uani 1 1 d . . . H41 H 0.8318 0.4558 0.4873 0.086 Uiso 1 1 calc R . . C25 C 0.5115(4) 0.3535(3) 0.5887(4) 0.0463(16) Uani 1 1 d . . . C37 C 0.8679(4) 0.2880(4) 0.4331(3) 0.0472(16) Uani 1 1 d . . . C15 C 0.1738(4) 0.1554(4) 0.3961(5) 0.068(2) Uani 1 1 d . . . H15 H 0.1381 0.1834 0.3613 0.082 Uiso 1 1 calc R . . C14 C 0.2508(4) 0.1214(4) 0.3735(4) 0.0541(17) Uani 1 1 d . . . H14 H 0.2668 0.1262 0.3234 0.065 Uiso 1 1 calc R . . C22 C 0.1668(6) 0.3810(5) 0.6299(5) 0.089(3) Uani 1 1 d . . . H22 H 0.1088 0.3999 0.6282 0.107 Uiso 1 1 calc R . . C30 C 0.5878(5) 0.3901(4) 0.6192(5) 0.072(2) Uani 1 1 d . . . H30 H 0.6067 0.3838 0.6705 0.086 Uiso 1 1 calc R . . C10 C 0.3145(5) -0.1489(4) 0.2276(4) 0.074(2) Uani 1 1 d . . . H10 H 0.2978 -0.1886 0.1959 0.089 Uiso 1 1 calc R . . C20 C 0.3240(5) 0.3971(4) 0.6527(4) 0.0630(19) Uani 1 1 d . . . H20 H 0.3722 0.4279 0.6667 0.076 Uiso 1 1 calc R . . C16 C 0.1503(5) 0.1474(4) 0.4709(6) 0.078(2) Uani 1 1 d . . . H16 H 0.0990 0.1706 0.4861 0.093 Uiso 1 1 calc R . . C26 C 0.4850(5) 0.3664(4) 0.5123(4) 0.0583(19) Uani 1 1 d . . . H26 H 0.4334 0.3439 0.4904 0.070 Uiso 1 1 calc R . . C33 C 0.9489(5) 0.0456(4) 0.5842(6) 0.081(2) Uani 1 1 d . . . H33 H 0.9565 -0.0055 0.5859 0.097 Uiso 1 1 calc R . . C38 C 0.9442(5) 0.3020(4) 0.3953(5) 0.079(2) Uani 1 1 d . . . H38 H 0.9729 0.2638 0.3712 0.095 Uiso 1 1 calc R . . C8 C 0.2789(4) -0.0599(3) 0.3208(4) 0.0507(17) Uani 1 1 d . . . H8 H 0.2368 -0.0388 0.3509 0.061 Uiso 1 1 calc R . . C11 C 0.4011(5) -0.1226(4) 0.2301(4) 0.072(2) Uani 1 1 d . . . H11 H 0.4416 -0.1431 0.1981 0.086 Uiso 1 1 calc R . . C29 C 0.6358(5) 0.4360(5) 0.5737(6) 0.093(3) Uani 1 1 d . . . H29 H 0.6871 0.4597 0.5946 0.111 Uiso 1 1 calc R . . C35 C 0.9710(5) 0.1644(5) 0.6420(5) 0.078(2) Uani 1 1 d . . . H35 H 0.9942 0.1936 0.6823 0.093 Uiso 1 1 calc R . . C40 C 0.9364(5) 0.4306(5) 0.4279(5) 0.083(3) Uani 1 1 d . . . H40 H 0.9597 0.4783 0.4263 0.100 Uiso 1 1 calc R . . C34 C 0.9809(5) 0.0878(5) 0.6448(5) 0.080(2) Uani 1 1 d . . . H34 H 1.0092 0.0655 0.6879 0.096 Uiso 1 1 calc R . . C24 C 0.2662(5) 0.2791(4) 0.6186(5) 0.074(2) Uani 1 1 d . . . H24 H 0.2744 0.2289 0.6097 0.089 Uiso 1 1 calc R . . C28 C 0.6093(6) 0.4465(5) 0.4997(6) 0.090(3) Uani 1 1 d . . . H28 H 0.6421 0.4773 0.4696 0.108 Uiso 1 1 calc R . . C23 C 0.1805(5) 0.3086(5) 0.6137(6) 0.095(3) Uani 1 1 d . . . H23 H 0.1319 0.2784 0.5992 0.114 Uiso 1 1 calc R . . C39 C 0.9780(5) 0.3739(5) 0.3938(6) 0.101(3) Uani 1 1 d . . . H39 H 1.0298 0.3832 0.3691 0.121 Uiso 1 1 calc R . . C9 C 0.2533(5) -0.1172(4) 0.2713(4) 0.070(2) Uani 1 1 d . . . H9 H 0.1943 -0.1340 0.2680 0.085 Uiso 1 1 calc R . . C27 C 0.5343(6) 0.4121(4) 0.4689(5) 0.075(2) Uani 1 1 d . . . H27 H 0.5162 0.4197 0.4176 0.090 Uiso 1 1 calc R . . Cl2 Cl 0.24316(14) 0.36899(13) 0.41819(11) 0.0882(7) Uani 1 1 d . . . C21 C 0.2380(6) 0.4255(4) 0.6486(4) 0.075(2) Uani 1 1 d . . . H21 H 0.2289 0.4754 0.6586 0.090 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 Cl1 0.0521(12) 0.0905(16) 0.1235(18) 0.0131(13) 0.0057(12) 0.0196(11) Cl3 0.0553(12) 0.131(2) 0.1025(16) -0.0115(15) -0.0142(11) 0.0030(13) Cl4 0.124(2) 0.0829(16) 0.1174(19) -0.0193(13) -0.0084(16) -0.0135(15) Cl6 0.0549(14) 0.148(2) 0.159(2) 0.0444(19) -0.0054(15) -0.0011(15) Cl5 0.0899(17) 0.1160(19) 0.127(2) 0.0439(16) 0.0153(15) 0.0026(15) C101 0.048(4) 0.075(5) 0.078(5) 0.015(4) -0.001(4) -0.002(4) C100 0.030(4) 0.076(5) 0.077(5) 0.004(4) 0.000(3) 0.007(4) Pd1 0.0160(3) 0.0308(3) 0.0401(3) 0.0023(3) -0.0012(2) -0.0015(3) Br1 0.0629(5) 0.0881(6) 0.0716(5) -0.0160(4) 0.0093(4) 0.0012(5) P2 0.0196(7) 0.0377(9) 0.0418(9) 0.0030(7) -0.0027(6) -0.0007(7) P1 0.0197(7) 0.0331(9) 0.0476(9) 0.0010(7) -0.0015(7) -0.0016(7) P3 0.0389(10) 0.0457(11) 0.0591(11) -0.0063(8) 0.0072(8) 0.0006(8) P4 0.0296(9) 0.0554(11) 0.0655(11) -0.0045(9) 0.0129(8) -0.0108(8) C31 0.025(3) 0.046(4) 0.074(5) -0.006(3) 0.007(3) -0.003(3) C5 0.018(3) 0.051(4) 0.046(3) -0.001(3) 0.005(3) -0.005(3) C1 0.031(3) 0.034(4) 0.055(4) 0.012(3) -0.001(3) -0.001(3) C3 0.029(3) 0.032(4) 0.062(4) -0.002(3) 0.000(3) -0.004(3) C17 0.050(4) 0.057(5) 0.082(5) -0.017(4) 0.030(4) -0.009(4) C13 0.022(3) 0.034(4) 0.056(4) -0.004(3) -0.001(3) -0.004(3) C7 0.031(3) 0.040(3) 0.045(4) 0.005(3) -0.007(3) -0.003(3) C2 0.029(3) 0.048(4) 0.041(3) 0.005(3) -0.002(3) -0.003(3) C6 0.019(3) 0.050(4) 0.066(4) 0.003(3) 0.000(3) -0.010(3) C18 0.026(3) 0.041(4) 0.063(4) -0.006(3) 0.006(3) -0.005(3) C19 0.043(4) 0.042(4) 0.048(4) -0.003(3) 0.015(3) 0.006(3) C4 0.028(3) 0.034(4) 0.068(4) -0.010(3) 0.014(3) -0.007(3) C12 0.040(4) 0.053(4) 0.061(4) -0.004(3) 0.008(3) -0.009(3) C32 0.036(4) 0.055(5) 0.101(6) -0.003(4) 0.006(4) -0.005(4) C42 0.046(4) 0.054(5) 0.088(5) -0.001(4) 0.025(4) -0.014(4) C36 0.046(4) 0.049(5) 0.097(6) 0.001(4) -0.008(4) 0.001(4) C41 0.061(5) 0.058(5) 0.097(6) -0.001(4) 0.014(4) -0.002(4) C25 0.036(4) 0.041(4) 0.063(4) -0.008(3) 0.007(3) 0.002(3) C37 0.025(3) 0.059(5) 0.057(4) 0.003(3) 0.001(3) -0.002(3) C15 0.032(4) 0.052(5) 0.117(7) -0.003(4) -0.016(4) 0.012(3) C14 0.026(3) 0.067(5) 0.068(4) 0.008(4) -0.005(3) 0.007(3) C22 0.060(6) 0.098(8) 0.113(7) 0.017(6) 0.031(5) 0.035(6) C30 0.053(5) 0.063(5) 0.098(6) -0.014(4) -0.009(4) -0.015(4) C10 0.073(6) 0.071(5) 0.076(5) -0.025(4) -0.007(5) -0.023(5) C20 0.067(5) 0.056(5) 0.065(5) -0.003(4) -0.005(4) 0.011(4) C16 0.034(4) 0.062(5) 0.138(8) -0.021(5) 0.009(5) 0.009(4) C26 0.053(5) 0.056(5) 0.067(5) -0.003(4) 0.017(4) 0.000(4) C33 0.052(5) 0.048(5) 0.142(8) 0.016(5) 0.009(5) 0.012(4) C38 0.046(4) 0.060(5) 0.135(7) 0.002(5) 0.035(5) -0.014(4) C8 0.034(4) 0.058(5) 0.059(4) -0.001(3) -0.002(3) -0.002(3) C11 0.072(6) 0.083(6) 0.062(5) -0.017(4) 0.013(4) -0.007(5) C29 0.045(5) 0.065(6) 0.169(10) 0.013(6) 0.010(6) -0.022(4) C35 0.056(5) 0.084(7) 0.090(6) -0.006(5) -0.017(4) 0.005(5) C40 0.053(5) 0.062(6) 0.136(8) 0.018(5) 0.014(5) -0.021(5) C34 0.051(5) 0.079(7) 0.108(7) 0.015(5) -0.017(5) 0.009(5) C24 0.043(4) 0.053(5) 0.129(7) -0.004(4) 0.022(4) 0.002(4) C28 0.063(6) 0.068(6) 0.146(9) 0.034(6) 0.045(6) 0.011(5) C23 0.043(5) 0.083(7) 0.162(9) 0.007(6) 0.020(5) 0.002(5) C39 0.047(5) 0.082(7) 0.180(10) 0.016(6) 0.048(6) -0.015(5) C9 0.041(4) 0.084(6) 0.084(5) -0.020(5) -0.013(4) -0.023(4) C27 0.077(6) 0.068(6) 0.084(6) 0.010(4) 0.024(5) 0.015(5) Cl2 0.0727(14) 0.1153(18) 0.0767(13) 0.0074(12) 0.0059(11) -0.0047(13) C21 0.085(6) 0.056(5) 0.083(6) 0.004(4) 0.011(5) 0.034(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 Cl1 C100 1.773(7) . ? Cl3 C100 1.757(7) . ? Cl4 C101 1.748(7) . ? Cl6 C101 1.752(7) . ? Cl5 C101 1.747(7) . ? C100 Cl2 1.752(7) . ? Pd1 P2 2.3276(14) . ? Pd1 P2 2.3276(14) 3_656 ? Pd1 P1 2.3337(15) . ? Pd1 P1 2.3337(15) 3_656 ? P2 C7 1.802(6) . ? P2 C2 1.818(5) . ? P2 C13 1.819(6) . ? P1 C3 1.817(6) . ? P1 C5 1.832(5) . ? P1 C1 1.855(5) . ? P3 C25 1.827(6) . ? P3 C19 1.833(6) . ? P3 C4 1.861(5) . ? P4 C31 1.830(7) . ? P4 C37 1.833(7) . ? P4 C6 1.849(5) . ? C31 C36 1.383(8) . ? C31 C32 1.390(9) . ? C5 C6 1.538(7) . ? C1 C2 1.519(7) . ? C3 C4 1.529(7) . ? C17 C16 1.365(10) . ? C17 C18 1.408(8) . ? C13 C18 1.374(8) . ? C13 C14 1.380(8) . ? C7 C8 1.393(7) . ? C7 C12 1.401(8) . ? C19 C20 1.378(8) . ? C19 C24 1.378(8) . ? C12 C11 1.390(8) . ? C32 C33 1.380(10) . ? C42 C37 1.362(8) . ? C42 C41 1.387(9) . ? C36 C35 1.379(9) . ? C41 C40 1.354(9) . ? C25 C26 1.389(8) . ? C25 C30 1.392(8) . ? C37 C38 1.381(8) . ? C15 C16 1.387(10) . ? C15 C14 1.387(9) . ? C22 C21 1.357(10) . ? C22 C23 1.357(11) . ? C30 C29 1.385(10) . ? C10 C9 1.359(9) . ? C10 C11 1.377(9) . ? C20 C21 1.381(9) . ? C26 C27 1.372(9) . ? C33 C34 1.366(10) . ? C38 C39 1.396(10) . ? C8 C9 1.387(8) . ? C29 C28 1.341(11) . ? C35 C34 1.391(10) . ? C40 C39 1.357(10) . ? C24 C23 1.384(9) . ? C28 C27 1.360(11) . ? 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 Cl5 C101 Cl4 110.8(4) . . ? Cl5 C101 Cl6 108.1(4) . . ? Cl4 C101 Cl6 110.4(4) . . ? Cl2 C100 Cl3 109.7(4) . . ? Cl2 C100 Cl1 109.8(4) . . ? Cl3 C100 Cl1 108.5(4) . . ? P2 Pd1 P2 180.00(5) . 3_656 ? P2 Pd1 P1 83.60(5) . . ? P2 Pd1 P1 96.40(5) 3_656 . ? P2 Pd1 P1 96.40(5) . 3_656 ? P2 Pd1 P1 83.60(5) 3_656 3_656 ? P1 Pd1 P1 180.0 . 3_656 ? C7 P2 C2 107.2(3) . . ? C7 P2 C13 106.3(3) . . ? C2 P2 C13 105.9(3) . . ? C7 P2 Pd1 119.27(19) . . ? C2 P2 Pd1 105.55(18) . . ? C13 P2 Pd1 111.87(19) . . ? C3 P1 C5 103.6(3) . . ? C3 P1 C1 104.8(3) . . ? C5 P1 C1 105.4(3) . . ? C3 P1 Pd1 119.92(19) . . ? C5 P1 Pd1 113.21(19) . . ? C1 P1 Pd1 108.76(18) . . ? C25 P3 C19 100.3(3) . . ? C25 P3 C4 100.0(3) . . ? C19 P3 C4 102.6(3) . . ? C31 P4 C37 101.9(3) . . ? C31 P4 C6 99.6(3) . . ? C37 P4 C6 101.9(3) . . ? C36 C31 C32 118.4(7) . . ? C36 C31 P4 124.6(5) . . ? C32 C31 P4 117.1(5) . . ? C6 C5 P1 115.3(4) . . ? C2 C1 P1 110.7(4) . . ? C4 C3 P1 117.6(4) . . ? C16 C17 C18 119.5(7) . . ? C18 C13 C14 120.7(6) . . ? C18 C13 P2 119.5(4) . . ? C14 C13 P2 119.8(5) . . ? C8 C7 C12 118.6(6) . . ? C8 C7 P2 121.8(5) . . ? C12 C7 P2 119.4(4) . . ? C1 C2 P2 109.7(4) . . ? C5 C6 P4 109.4(4) . . ? C13 C18 C17 119.5(6) . . ? C20 C19 C24 117.8(6) . . ? C20 C19 P3 118.7(5) . . ? C24 C19 P3 123.2(5) . . ? C3 C4 P3 109.4(4) . . ? C11 C12 C7 119.4(6) . . ? C33 C32 C31 120.3(7) . . ? C37 C42 C41 121.9(6) . . ? C35 C36 C31 121.4(7) . . ? C40 C41 C42 119.7(7) . . ? C26 C25 C30 117.4(6) . . ? C26 C25 P3 123.4(5) . . ? C30 C25 P3 119.1(5) . . ? C42 C37 C38 118.2(6) . . ? C42 C37 P4 126.4(5) . . ? C38 C37 P4 115.4(5) . . ? C16 C15 C14 119.6(7) . . ? C13 C14 C15 119.8(7) . . ? C21 C22 C23 119.6(8) . . ? C29 C30 C25 120.5(8) . . ? C9 C10 C11 120.4(7) . . ? C19 C20 C21 121.1(7) . . ? C17 C16 C15 120.8(7) . . ? C27 C26 C25 120.5(7) . . ? C34 C33 C32 120.8(7) . . ? C37 C38 C39 119.4(7) . . ? C9 C8 C7 120.9(6) . . ? C10 C11 C12 120.7(7) . . ? C28 C29 C30 120.7(8) . . ? C36 C35 C34 119.3(7) . . ? C41 C40 C39 119.6(7) . . ? C33 C34 C35 119.8(8) . . ? C19 C24 C23 120.4(7) . . ? C29 C28 C27 119.9(8) . . ? C22 C23 C24 120.7(8) . . ? C40 C39 C38 121.2(7) . . ? C10 C9 C8 119.9(6) . . ? C28 C27 C26 121.0(8) . . ? C22 C21 C20 120.2(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pd1 P2 C7 -100(100) 3_656 . . . ? P1 Pd1 P2 C7 147.5(2) . . . . ? P1 Pd1 P2 C7 -32.5(2) 3_656 . . . ? P2 Pd1 P2 C2 140(100) 3_656 . . . ? P1 Pd1 P2 C2 27.0(2) . . . . ? P1 Pd1 P2 C2 -153.0(2) 3_656 . . . ? P2 Pd1 P2 C13 25(100) 3_656 . . . ? P1 Pd1 P2 C13 -87.6(2) . . . . ? P1 Pd1 P2 C13 92.4(2) 3_656 . . . ? P2 Pd1 P1 C3 115.2(2) . . . . ? P2 Pd1 P1 C3 -64.8(2) 3_656 . . . ? P1 Pd1 P1 C3 -78(100) 3_656 . . . ? P2 Pd1 P1 C5 -122.0(2) . . . . ? P2 Pd1 P1 C5 58.0(2) 3_656 . . . ? P1 Pd1 P1 C5 45(100) 3_656 . . . ? P2 Pd1 P1 C1 -5.2(2) . . . . ? P2 Pd1 P1 C1 174.8(2) 3_656 . . . ? P1 Pd1 P1 C1 162(100) 3_656 . . . ? C37 P4 C31 C36 22.5(6) . . . . ? C6 P4 C31 C36 -81.9(6) . . . . ? C37 P4 C31 C32 -158.4(5) . . . . ? C6 P4 C31 C32 97.1(5) . . . . ? C3 P1 C5 C6 -46.8(5) . . . . ? C1 P1 C5 C6 63.0(5) . . . . ? Pd1 P1 C5 C6 -178.3(4) . . . . ? C3 P1 C1 C2 -152.4(4) . . . . ? C5 P1 C1 C2 98.7(4) . . . . ? Pd1 P1 C1 C2 -23.0(4) . . . . ? C5 P1 C3 C4 173.2(4) . . . . ? C1 P1 C3 C4 62.9(5) . . . . ? Pd1 P1 C3 C4 -59.5(5) . . . . ? C7 P2 C13 C18 114.5(5) . . . . ? C2 P2 C13 C18 -131.8(5) . . . . ? Pd1 P2 C13 C18 -17.3(5) . . . . ? C7 P2 C13 C14 -64.8(5) . . . . ? C2 P2 C13 C14 49.0(5) . . . . ? Pd1 P2 C13 C14 163.5(4) . . . . ? C2 P2 C7 C8 -132.6(5) . . . . ? C13 P2 C7 C8 -19.8(6) . . . . ? Pd1 P2 C7 C8 107.7(5) . . . . ? C2 P2 C7 C12 52.6(5) . . . . ? C13 P2 C7 C12 165.4(5) . . . . ? Pd1 P2 C7 C12 -67.1(5) . . . . ? P1 C1 C2 P2 46.9(5) . . . . ? C7 P2 C2 C1 -178.0(4) . . . . ? C13 P2 C2 C1 68.9(4) . . . . ? Pd1 P2 C2 C1 -49.9(4) . . . . ? P1 C5 C6 P4 -167.1(3) . . . . ? C31 P4 C6 C5 -73.9(4) . . . . ? C37 P4 C6 C5 -178.3(4) . . . . ? C14 C13 C18 C17 1.0(8) . . . . ? P2 C13 C18 C17 -178.2(4) . . . . ? C16 C17 C18 C13 -2.0(9) . . . . ? C25 P3 C19 C20 -55.1(5) . . . . ? C4 P3 C19 C20 -157.9(5) . . . . ? C25 P3 C19 C24 131.1(6) . . . . ? C4 P3 C19 C24 28.3(6) . . . . ? P1 C3 C4 P3 -167.7(3) . . . . ? C25 P3 C4 C3 55.4(5) . . . . ? C19 P3 C4 C3 158.5(4) . . . . ? C8 C7 C12 C11 0.2(9) . . . . ? P2 C7 C12 C11 175.2(5) . . . . ? C36 C31 C32 C33 1.3(9) . . . . ? P4 C31 C32 C33 -177.8(5) . . . . ? C32 C31 C36 C35 -0.5(10) . . . . ? P4 C31 C36 C35 178.6(5) . . . . ? C37 C42 C41 C40 0.1(12) . . . . ? C19 P3 C25 C26 -54.8(6) . . . . ? C4 P3 C25 C26 50.1(6) . . . . ? C19 P3 C25 C30 128.1(5) . . . . ? C4 P3 C25 C30 -127.0(5) . . . . ? C41 C42 C37 C38 -1.0(11) . . . . ? C41 C42 C37 P4 179.8(5) . . . . ? C31 P4 C37 C42 -91.9(6) . . . . ? C6 P4 C37 C42 10.7(7) . . . . ? C31 P4 C37 C38 88.8(5) . . . . ? C6 P4 C37 C38 -168.6(5) . . . . ? C18 C13 C14 C15 0.2(9) . . . . ? P2 C13 C14 C15 179.5(5) . . . . ? C16 C15 C14 C13 -0.4(10) . . . . ? C26 C25 C30 C29 -1.6(10) . . . . ? P3 C25 C30 C29 175.7(6) . . . . ? C24 C19 C20 C21 -2.2(10) . . . . ? P3 C19 C20 C21 -176.3(5) . . . . ? C18 C17 C16 C15 1.8(11) . . . . ? C14 C15 C16 C17 -0.6(11) . . . . ? C30 C25 C26 C27 1.7(10) . . . . ? P3 C25 C26 C27 -175.5(5) . . . . ? C31 C32 C33 C34 -0.6(11) . . . . ? C42 C37 C38 C39 1.3(11) . . . . ? P4 C37 C38 C39 -179.3(7) . . . . ? C12 C7 C8 C9 0.5(9) . . . . ? P2 C7 C8 C9 -174.4(5) . . . . ? C9 C10 C11 C12 3.2(12) . . . . ? C7 C12 C11 C10 -2.0(10) . . . . ? C25 C30 C29 C28 0.7(13) . . . . ? C31 C36 C35 C34 -1.1(11) . . . . ? C42 C41 C40 C39 0.4(12) . . . . ? C32 C33 C34 C35 -1.1(12) . . . . ? C36 C35 C34 C33 1.9(12) . . . . ? C20 C19 C24 C23 3.0(11) . . . . ? P3 C19 C24 C23 176.8(6) . . . . ? C30 C29 C28 C27 0.2(13) . . . . ? C21 C22 C23 C24 2.2(14) . . . . ? C19 C24 C23 C22 -3.0(13) . . . . ? C41 C40 C39 C38 0.1(14) . . . . ? C37 C38 C39 C40 -0.9(14) . . . . ? C11 C10 C9 C8 -2.4(12) . . . . ? C7 C8 C9 C10 0.6(11) . . . . ? C29 C28 C27 C26 -0.1(13) . . . . ? C25 C26 C27 C28 -0.9(11) . . . . ? C23 C22 C21 C20 -1.4(13) . . . . ? C19 C20 C21 C22 1.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.653 _refine_diff_density_min -1.578 _refine_diff_density_rms 0.103 # Attachment 'PtNO3.cif' data_PtNO3 _database_code_depnum_ccdc_archive 'CCDC 737981' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Pt(PP3)2](NO3)2.2CHCl3 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H84 Cl6 N2 O6 P8 Pt' _chemical_formula_weight 1897.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 12.9530(18) _cell_length_b 13.2829(18) _cell_length_c 15.424(2) _cell_angle_alpha 103.192(2) _cell_angle_beta 105.354(2) _cell_angle_gamma 112.810(2) _cell_volume 2189.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2372 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 26.21 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 962 _exptl_absorpt_coefficient_mu 1.983 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5970 _exptl_absorpt_correction_T_max 0.8903 _exptl_absorpt_process_details Sadabs _exptl_special_details ; [Pt(PP3)2](NO3)2.2CHCl3 ; _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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15829 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0944 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.39 _reflns_number_total 8696 _reflns_number_gt 6896 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction 'BRUKER Shelxtl' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0264P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8696 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0729 _refine_ls_wR_factor_gt 0.0674 _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 0.5000 0.0000 0.0000 0.02696(8) Uani 1 2 d S . . P1 P 0.66465(9) 0.11699(8) -0.02856(8) 0.0300(3) Uani 1 1 d . . . P2 P 0.39232(9) 0.05534(9) -0.10743(8) 0.0309(3) Uani 1 1 d . . . P3 P 0.70561(10) -0.09543(10) -0.26548(9) 0.0421(3) Uani 1 1 d . . . P4 P 1.02370(10) 0.44274(9) 0.15269(9) 0.0413(3) Uani 1 1 d . . . Cl2 Cl 0.2779(2) 0.2557(2) 0.62690(17) 0.1442(8) Uani 1 1 d . . . Cl3 Cl 0.2076(3) 0.2426(2) 0.78362(16) 0.1674(11) Uani 1 1 d . . . C7 C 0.2714(3) 0.0797(3) -0.0862(3) 0.0328(10) Uani 1 1 d . . . Cl1 Cl 0.0484(2) 0.2295(4) 0.6139(2) 0.264(2) Uani 1 1 d . . . C3 C 0.7295(3) 0.0410(3) -0.0900(3) 0.0344(10) Uani 1 1 d . . . H3A H 0.7842 0.0943 -0.1107 0.041 Uiso 1 1 calc R . . H3B H 0.7776 0.0208 -0.0442 0.041 Uiso 1 1 calc R . . C29 C 0.8192(8) 0.2201(6) -0.2970(6) 0.106(3) Uani 1 1 d . . . H29 H 0.8936 0.2869 -0.2768 0.128 Uiso 1 1 calc R . . C13 C 0.3280(3) -0.0438(3) -0.2317(3) 0.0362(10) Uani 1 1 d . . . C18 C 0.3151(3) -0.1560(4) -0.2541(3) 0.0429(11) Uani 1 1 d . . . H18 H 0.3390 -0.1814 -0.2047 0.051 Uiso 1 1 calc R . . C5 C 0.7948(3) 0.2411(3) 0.0764(3) 0.0353(10) Uani 1 1 d . . . H5A H 0.7707 0.2990 0.0998 0.042 Uiso 1 1 calc R . . H5B H 0.8167 0.2132 0.1277 0.042 Uiso 1 1 calc R . . C1 C 0.6125(3) 0.1832(4) -0.1108(3) 0.0401(11) Uani 1 1 d . . . H1A H 0.6782 0.2604 -0.0960 0.048 Uiso 1 1 calc R . . H1B H 0.5902 0.1347 -0.1770 0.048 Uiso 1 1 calc R . . C2 C 0.5033(3) 0.1949(3) -0.1012(3) 0.0373(10) Uani 1 1 d . . . H2A H 0.4674 0.2160 -0.1531 0.045 Uiso 1 1 calc R . . H2B H 0.5290 0.2563 -0.0399 0.045 Uiso 1 1 calc R . . C31 C 1.1524(4) 0.4654(3) 0.1165(4) 0.0419(11) Uani 1 1 d . . . C25 C 0.7051(4) 0.0232(4) -0.3072(3) 0.0473(12) Uani 1 1 d . . . C4 C 0.6358(3) -0.0715(3) -0.1784(3) 0.0379(10) Uani 1 1 d . . . H4A H 0.5647 -0.0639 -0.2085 0.045 Uiso 1 1 calc R . . H4B H 0.6100 -0.1382 -0.1583 0.045 Uiso 1 1 calc R . . C37 C 1.0577(4) 0.3939(4) 0.2528(3) 0.0409(11) Uani 1 1 d . . . C12 C 0.1499(4) -0.0037(4) -0.1426(3) 0.0422(11) Uani 1 1 d . . . H12 H 0.1301 -0.0697 -0.1940 0.051 Uiso 1 1 calc R . . C26 C 0.5995(5) 0.0232(4) -0.3571(3) 0.0615(14) Uani 1 1 d . . . H26 H 0.5245 -0.0430 -0.3778 0.074 Uiso 1 1 calc R . . C11 C 0.0593(4) 0.0129(4) -0.1212(4) 0.0577(14) Uani 1 1 d . . . H11 H -0.0218 -0.0430 -0.1580 0.069 Uiso 1 1 calc R . . C10 C 0.0874(4) 0.1101(4) -0.0470(4) 0.0612(15) Uani 1 1 d . . . H10 H 0.0254 0.1203 -0.0336 0.073 Uiso 1 1 calc R . . C34 C 1.3472(5) 0.5088(4) 0.0593(5) 0.0708(18) Uani 1 1 d . . . H34 H 1.4121 0.5217 0.0403 0.085 Uiso 1 1 calc R . . C9 C 0.2073(4) 0.1938(4) 0.0085(4) 0.0529(13) Uani 1 1 d . . . H9 H 0.2260 0.2606 0.0586 0.063 Uiso 1 1 calc R . . C8 C 0.2988(4) 0.1782(4) -0.0105(3) 0.0412(11) Uani 1 1 d . . . H8 H 0.3796 0.2340 0.0276 0.049 Uiso 1 1 calc R . . C32 C 1.1369(4) 0.4544(4) 0.0226(4) 0.0538(13) Uani 1 1 d . . . H32 H 1.0601 0.4315 -0.0222 0.065 Uiso 1 1 calc R . . C42 C 1.0985(4) 0.3121(4) 0.2526(4) 0.0567(14) Uani 1 1 d . . . H42 H 1.1136 0.2811 0.1998 0.068 Uiso 1 1 calc R . . C6 C 0.9065(3) 0.3003(3) 0.0544(3) 0.0389(11) Uani 1 1 d . . . H6A H 0.8815 0.3133 -0.0053 0.047 Uiso 1 1 calc R . . H6B H 0.9417 0.2483 0.0448 0.047 Uiso 1 1 calc R . . C36 C 1.2682(4) 0.5010(4) 0.1819(4) 0.0577(14) Uani 1 1 d . . . H36 H 1.2820 0.5113 0.2464 0.069 Uiso 1 1 calc R . . C24 C 0.5740(5) -0.2445(4) -0.4587(4) 0.0650(15) Uani 1 1 d . . . H24 H 0.6304 -0.1858 -0.4703 0.078 Uiso 1 1 calc R . . C30 C 0.8155(5) 0.1224(4) -0.2783(4) 0.0705(16) Uani 1 1 d . . . H30 H 0.8877 0.1232 -0.2460 0.085 Uiso 1 1 calc R . . C19 C 0.5809(4) -0.2269(4) -0.3657(3) 0.0441(11) Uani 1 1 d . . . C38 C 1.0367(4) 0.4389(5) 0.3321(4) 0.0684(15) Uani 1 1 d . . . H38 H 1.0091 0.4941 0.3336 0.082 Uiso 1 1 calc R . . C17 C 0.2671(4) -0.2305(4) -0.3496(4) 0.0624(14) Uani 1 1 d . . . H17 H 0.2573 -0.3064 -0.3643 0.075 Uiso 1 1 calc R . . C20 C 0.4987(5) -0.3175(4) -0.3516(4) 0.0708(16) Uani 1 1 d . . . H20 H 0.5027 -0.3103 -0.2893 0.085 Uiso 1 1 calc R . . C40 C 1.0961(5) 0.3209(7) 0.4065(5) 0.092(2) Uani 1 1 d . . . H40 H 1.1087 0.2961 0.4583 0.110 Uiso 1 1 calc R . . C23 C 0.4857(5) -0.3466(5) -0.5354(4) 0.0812(18) Uani 1 1 d . . . H23 H 0.4826 -0.3556 -0.5977 0.097 Uiso 1 1 calc R . . C22 C 0.4041(5) -0.4332(5) -0.5203(5) 0.0823(19) Uani 1 1 d . . . H22 H 0.3441 -0.5019 -0.5722 0.099 Uiso 1 1 calc R . . C33 C 1.2335(5) 0.4769(4) -0.0071(4) 0.0689(16) Uani 1 1 d . . . H33 H 1.2217 0.4704 -0.0707 0.083 Uiso 1 1 calc R . . C27 C 0.6048(7) 0.1208(6) -0.3762(4) 0.090(2) Uani 1 1 d . . . H27 H 0.5336 0.1201 -0.4107 0.108 Uiso 1 1 calc R . . C100 C 0.1958(5) 0.2897(6) 0.6897(4) 0.0881(19) Uani 1 1 d . . . C14 C 0.2918(4) -0.0086(4) -0.3064(3) 0.0587(14) Uani 1 1 d . . . H14 H 0.2986 0.0662 -0.2923 0.070 Uiso 1 1 calc R . . C35 C 1.3629(5) 0.5211(4) 0.1517(5) 0.0735(17) Uani 1 1 d . . . H35 H 1.4397 0.5438 0.1963 0.088 Uiso 1 1 calc R . . C28 C 0.7144(9) 0.2186(6) -0.3449(5) 0.109(3) Uani 1 1 d . . . H28 H 0.7172 0.2851 -0.3565 0.131 Uiso 1 1 calc R . . C15 C 0.2459(5) -0.0819(6) -0.4014(4) 0.0801(18) Uani 1 1 d . . . H15 H 0.2230 -0.0566 -0.4512 0.096 Uiso 1 1 calc R . . C39 C 1.0562(6) 0.4028(7) 0.4094(5) 0.101(2) Uani 1 1 d . . . H39 H 1.0425 0.4339 0.4630 0.122 Uiso 1 1 calc R . . C21 C 0.4094(5) -0.4201(5) -0.4296(5) 0.0848(19) Uani 1 1 d . . . H21 H 0.3529 -0.4801 -0.4191 0.102 Uiso 1 1 calc R . . C16 C 0.2341(5) -0.1932(5) -0.4220(4) 0.0770(17) Uani 1 1 d . . . H16 H 0.2032 -0.2433 -0.4862 0.092 Uiso 1 1 calc R . . C41 C 1.1173(5) 0.2755(5) 0.3291(5) 0.0739(17) Uani 1 1 d . . . H41 H 1.1444 0.2199 0.3278 0.089 Uiso 1 1 calc R . . N01 N 0.3628(5) 0.6046(5) 0.8230(4) 0.0661(13) Uani 1 1 d . . . O1 O 0.4117(4) 0.7037(4) 0.8663(3) 0.0912(13) Uani 1 1 d . . . O2 O 0.2572(5) 0.5542(4) 0.7600(4) 0.144(2) Uani 1 1 d . . . O3 O 0.4067(5) 0.5437(5) 0.8320(5) 0.185(3) 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 0.01921(12) 0.02665(13) 0.02722(14) 0.00787(11) 0.00514(10) 0.00746(10) P1 0.0224(6) 0.0301(5) 0.0309(6) 0.0096(5) 0.0090(5) 0.0083(5) P2 0.0241(6) 0.0307(6) 0.0333(7) 0.0128(5) 0.0071(5) 0.0110(5) P3 0.0324(6) 0.0419(7) 0.0407(7) 0.0057(6) 0.0128(6) 0.0134(6) P4 0.0305(6) 0.0318(6) 0.0457(8) 0.0073(6) 0.0094(6) 0.0078(5) Cl2 0.171(2) 0.186(2) 0.158(2) 0.0978(19) 0.1091(18) 0.1150(19) Cl3 0.321(3) 0.188(2) 0.1261(18) 0.1176(18) 0.132(2) 0.184(3) C7 0.030(2) 0.032(2) 0.038(3) 0.018(2) 0.011(2) 0.0149(19) Cl1 0.0973(18) 0.465(6) 0.184(3) 0.159(4) 0.0530(19) 0.073(3) C3 0.025(2) 0.037(2) 0.030(2) 0.011(2) 0.0092(19) 0.0070(19) C29 0.141(7) 0.056(4) 0.116(7) 0.030(4) 0.083(6) 0.022(5) C13 0.027(2) 0.041(2) 0.034(3) 0.013(2) 0.007(2) 0.014(2) C18 0.030(2) 0.044(3) 0.040(3) 0.008(2) 0.008(2) 0.013(2) C5 0.022(2) 0.031(2) 0.036(3) 0.009(2) 0.006(2) 0.0032(18) C1 0.032(2) 0.042(2) 0.044(3) 0.023(2) 0.013(2) 0.013(2) C2 0.031(2) 0.034(2) 0.045(3) 0.019(2) 0.010(2) 0.0137(19) C31 0.031(2) 0.029(2) 0.052(3) 0.011(2) 0.014(2) 0.0048(19) C25 0.056(3) 0.042(3) 0.032(3) 0.006(2) 0.020(2) 0.015(2) C4 0.031(2) 0.037(2) 0.034(3) 0.009(2) 0.006(2) 0.012(2) C37 0.028(2) 0.038(2) 0.038(3) 0.008(2) 0.006(2) 0.007(2) C12 0.029(2) 0.045(3) 0.047(3) 0.016(2) 0.009(2) 0.017(2) C26 0.080(4) 0.057(3) 0.043(3) 0.018(3) 0.017(3) 0.032(3) C11 0.032(3) 0.056(3) 0.080(4) 0.026(3) 0.017(3) 0.020(2) C10 0.046(3) 0.066(3) 0.090(4) 0.030(3) 0.037(3) 0.037(3) C34 0.055(4) 0.043(3) 0.122(6) 0.031(4) 0.057(4) 0.016(3) C9 0.059(3) 0.041(3) 0.069(4) 0.017(3) 0.033(3) 0.030(3) C8 0.039(3) 0.038(2) 0.049(3) 0.020(2) 0.019(2) 0.018(2) C32 0.048(3) 0.044(3) 0.069(4) 0.027(3) 0.027(3) 0.016(2) C42 0.057(3) 0.045(3) 0.046(3) 0.010(3) 0.003(3) 0.018(3) C6 0.026(2) 0.038(2) 0.035(3) 0.009(2) 0.009(2) 0.0040(19) C36 0.034(3) 0.055(3) 0.060(4) 0.010(3) 0.010(3) 0.009(2) C24 0.058(3) 0.057(3) 0.050(4) 0.007(3) 0.020(3) 0.009(3) C30 0.074(4) 0.051(3) 0.067(4) 0.014(3) 0.035(3) 0.011(3) C19 0.040(3) 0.044(3) 0.042(3) 0.006(2) 0.016(2) 0.021(2) C38 0.060(4) 0.095(4) 0.057(4) 0.030(4) 0.027(3) 0.040(3) C17 0.053(3) 0.055(3) 0.058(4) 0.002(3) 0.017(3) 0.022(3) C20 0.068(4) 0.049(3) 0.062(4) 0.003(3) 0.026(3) 0.007(3) C40 0.068(4) 0.121(6) 0.076(5) 0.058(5) 0.018(4) 0.031(4) C23 0.084(4) 0.075(4) 0.044(4) -0.003(3) 0.014(3) 0.021(4) C22 0.072(4) 0.051(3) 0.073(5) -0.012(3) 0.015(4) 0.010(3) C33 0.079(4) 0.052(3) 0.088(5) 0.035(3) 0.052(4) 0.024(3) C27 0.145(7) 0.083(5) 0.056(4) 0.034(4) 0.036(4) 0.065(5) C100 0.085(4) 0.135(6) 0.080(5) 0.066(4) 0.047(4) 0.062(4) C14 0.067(3) 0.064(3) 0.038(3) 0.020(3) 0.011(3) 0.031(3) C35 0.033(3) 0.060(3) 0.096(5) 0.010(4) 0.020(3) 0.007(3) C28 0.203(10) 0.069(5) 0.094(6) 0.047(5) 0.087(7) 0.073(6) C15 0.083(4) 0.096(5) 0.042(4) 0.026(4) 0.007(3) 0.035(4) C39 0.089(5) 0.161(7) 0.066(5) 0.045(5) 0.043(4) 0.061(5) C21 0.068(4) 0.053(3) 0.084(5) 0.002(3) 0.026(4) -0.002(3) C16 0.073(4) 0.086(4) 0.035(3) 0.001(3) 0.009(3) 0.024(4) C41 0.059(4) 0.065(4) 0.073(4) 0.024(4) 0.004(3) 0.022(3) N01 0.057(3) 0.068(3) 0.097(4) 0.045(3) 0.037(3) 0.040(3) O1 0.083(3) 0.099(3) 0.088(3) 0.031(3) 0.023(3) 0.050(3) O2 0.105(4) 0.099(4) 0.160(5) 0.021(4) -0.013(4) 0.043(3) O3 0.108(4) 0.115(4) 0.312(9) 0.062(5) 0.033(5) 0.077(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 Pt1 P2 2.3149(10) . ? Pt1 P2 2.3149(10) 2_655 ? Pt1 P1 2.3234(10) . ? Pt1 P1 2.3234(10) 2_655 ? P1 C3 1.807(4) . ? P1 C5 1.834(4) . ? P1 C1 1.832(4) . ? P2 C13 1.803(4) . ? P2 C7 1.812(4) . ? P2 C2 1.815(4) . ? P3 C19 1.818(4) . ? P3 C25 1.835(5) . ? P3 C4 1.843(4) . ? P4 C37 1.822(4) . ? P4 C31 1.834(4) . ? P4 C6 1.851(4) . ? Cl2 C100 1.729(6) . ? Cl3 C100 1.697(6) . ? C7 C8 1.387(5) . ? C7 C12 1.394(5) . ? Cl1 C100 1.692(6) . ? C3 C4 1.533(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C29 C28 1.353(9) . ? C29 C30 1.378(8) . ? C29 H29 0.9300 . ? C13 C14 1.377(6) . ? C13 C18 1.382(5) . ? C18 C17 1.381(6) . ? C18 H18 0.9300 . ? C5 C6 1.525(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C1 C2 1.521(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C31 C32 1.373(6) . ? C31 C36 1.387(6) . ? C25 C26 1.381(6) . ? C25 C30 1.383(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C37 C38 1.377(6) . ? C37 C42 1.380(6) . ? C12 C11 1.380(6) . ? C12 H12 0.9300 . ? C26 C27 1.374(7) . ? C26 H26 0.9300 . ? C11 C10 1.361(6) . ? C11 H11 0.9300 . ? C10 C9 1.379(6) . ? C10 H10 0.9300 . ? C34 C35 1.346(7) . ? C34 C33 1.384(7) . ? C34 H34 0.9300 . ? C9 C8 1.371(5) . ? C9 H9 0.9300 . ? C8 H8 0.9300 . ? C32 C33 1.393(6) . ? C32 H32 0.9300 . ? C42 C41 1.375(7) . ? C42 H42 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C36 C35 1.377(7) . ? C36 H36 0.9300 . ? C24 C23 1.376(7) . ? C24 C19 1.372(6) . ? C24 H24 0.9300 . ? C30 H30 0.9300 . ? C19 C20 1.370(6) . ? C38 C39 1.383(8) . ? C38 H38 0.9300 . ? C17 C16 1.356(7) . ? C17 H17 0.9300 . ? C20 C21 1.391(7) . ? C20 H20 0.9300 . ? C40 C41 1.355(8) . ? C40 C39 1.371(8) . ? C40 H40 0.9300 . ? C23 C22 1.343(7) . ? C23 H23 0.9300 . ? C22 C21 1.350(7) . ? C22 H22 0.9300 . ? C33 H33 0.9300 . ? C27 C28 1.362(9) . ? C27 H27 0.9300 . ? C14 C15 1.373(7) . ? C14 H14 0.9300 . ? C35 H35 0.9300 . ? C28 H28 0.9300 . ? C15 C16 1.377(7) . ? C15 H15 0.9300 . ? C39 H39 0.9300 . ? C21 H21 0.9300 . ? C16 H16 0.9300 . ? C41 H41 0.9300 . ? N01 O1 1.143(5) . ? N01 O3 1.168(5) . ? N01 O2 1.247(6) . ? 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 P2 Pt1 P2 180.00(5) . 2_655 ? P2 Pt1 P1 83.97(4) . . ? P2 Pt1 P1 96.03(4) 2_655 . ? P2 Pt1 P1 96.03(4) . 2_655 ? P2 Pt1 P1 83.97(4) 2_655 2_655 ? P1 Pt1 P1 180.00(5) . 2_655 ? C3 P1 C5 105.15(17) . . ? C3 P1 C1 103.90(19) . . ? C5 P1 C1 105.16(18) . . ? C3 P1 Pt1 115.93(13) . . ? C5 P1 Pt1 117.09(13) . . ? C1 P1 Pt1 108.34(13) . . ? C13 P2 C7 106.49(18) . . ? C13 P2 C2 105.9(2) . . ? C7 P2 C2 106.03(17) . . ? C13 P2 Pt1 113.21(13) . . ? C7 P2 Pt1 118.49(13) . . ? C2 P2 Pt1 105.79(13) . . ? C19 P3 C25 102.9(2) . . ? C19 P3 C4 102.63(19) . . ? C25 P3 C4 96.67(19) . . ? C37 P4 C31 103.2(2) . . ? C37 P4 C6 100.28(19) . . ? C31 P4 C6 99.24(19) . . ? C8 C7 C12 119.4(4) . . ? C8 C7 P2 120.3(3) . . ? C12 C7 P2 120.2(3) . . ? C4 C3 P1 114.6(3) . . ? C4 C3 H3A 108.6 . . ? P1 C3 H3A 108.6 . . ? C4 C3 H3B 108.6 . . ? P1 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C28 C29 C30 119.9(7) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C14 C13 C18 118.5(4) . . ? C14 C13 P2 120.5(3) . . ? C18 C13 P2 120.9(3) . . ? C13 C18 C17 120.4(4) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C6 C5 P1 113.5(3) . . ? C6 C5 H5A 108.9 . . ? P1 C5 H5A 108.9 . . ? C6 C5 H5B 108.9 . . ? P1 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C2 C1 P1 110.9(3) . . ? C2 C1 H1A 109.5 . . ? P1 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 108.0 . . ? C1 C2 P2 108.7(3) . . ? C1 C2 H2A 109.9 . . ? P2 C2 H2A 109.9 . . ? C1 C2 H2B 109.9 . . ? P2 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C32 C31 C36 117.9(4) . . ? C32 C31 P4 119.5(4) . . ? C36 C31 P4 122.5(4) . . ? C26 C25 C30 118.7(5) . . ? C26 C25 P3 123.1(4) . . ? C30 C25 P3 117.9(4) . . ? C3 C4 P3 109.0(3) . . ? C3 C4 H4A 109.9 . . ? P3 C4 H4A 109.9 . . ? C3 C4 H4B 109.9 . . ? P3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C38 C37 C42 118.4(5) . . ? C38 C37 P4 117.3(4) . . ? C42 C37 P4 124.3(4) . . ? C11 C12 C7 119.3(4) . . ? C11 C12 H12 120.4 . . ? C7 C12 H12 120.4 . . ? C27 C26 C25 120.2(6) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C10 C11 C12 120.8(4) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C10 C9 120.4(4) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C35 C34 C33 119.4(5) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C8 C9 C10 119.9(4) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C8 C7 120.3(4) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C31 C32 C33 121.6(5) . . ? C31 C32 H32 119.2 . . ? C33 C32 H32 119.2 . . ? C41 C42 C37 121.2(5) . . ? C41 C42 H42 119.4 . . ? C37 C42 H42 119.4 . . ? C5 C6 P4 112.4(3) . . ? C5 C6 H6A 109.1 . . ? P4 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? P4 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? C35 C36 C31 120.2(5) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C23 C24 C19 121.8(5) . . ? C23 C24 H24 119.1 . . ? C19 C24 H24 119.1 . . ? C29 C30 C25 120.4(6) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? C20 C19 C24 117.0(5) . . ? C20 C19 P3 122.3(4) . . ? C24 C19 P3 120.3(4) . . ? C37 C38 C39 120.6(6) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C16 C17 C18 120.1(5) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C20 C21 120.7(5) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C41 C40 C39 120.9(6) . . ? C41 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C22 C23 C24 120.2(6) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C22 C21 119.8(6) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C34 C33 C32 119.1(6) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C26 C27 C28 120.0(7) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? Cl3 C100 Cl1 110.9(4) . . ? Cl3 C100 Cl2 110.6(3) . . ? Cl1 C100 Cl2 110.0(4) . . ? C13 C14 C15 121.2(5) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C34 C35 C36 121.8(5) . . ? C34 C35 H35 119.1 . . ? C36 C35 H35 119.1 . . ? C29 C28 C27 120.8(7) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C14 C15 C16 119.3(5) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C40 C39 C38 119.5(6) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C22 C21 C20 120.4(6) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C17 C16 C15 120.5(5) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C40 C41 C42 119.5(6) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? O1 N01 O3 124.0(6) . . ? O1 N01 O2 121.1(5) . . ? O3 N01 O2 114.9(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pt1 P1 C3 -114.05(15) . . . . ? P2 Pt1 P1 C3 65.95(15) 2_655 . . . ? P1 Pt1 P1 C3 163(100) 2_655 . . . ? P2 Pt1 P1 C5 120.84(15) . . . . ? P2 Pt1 P1 C5 -59.16(15) 2_655 . . . ? P1 Pt1 P1 C5 37(100) 2_655 . . . ? P2 Pt1 P1 C1 2.22(15) . . . . ? P2 Pt1 P1 C1 -177.78(15) 2_655 . . . ? P1 Pt1 P1 C1 -81(100) 2_655 . . . ? P2 Pt1 P2 C13 -122(85) 2_655 . . . ? P1 Pt1 P2 C13 90.43(15) . . . . ? P1 Pt1 P2 C13 -89.57(15) 2_655 . . . ? P2 Pt1 P2 C7 4(85) 2_655 . . . ? P1 Pt1 P2 C7 -143.83(15) . . . . ? P1 Pt1 P2 C7 36.17(15) 2_655 . . . ? P2 Pt1 P2 C2 123(85) 2_655 . . . ? P1 Pt1 P2 C2 -25.15(15) . . . . ? P1 Pt1 P2 C2 154.85(15) 2_655 . . . ? C13 P2 C7 C8 -159.0(3) . . . . ? C2 P2 C7 C8 -46.4(4) . . . . ? Pt1 P2 C7 C8 72.1(3) . . . . ? C13 P2 C7 C12 24.4(4) . . . . ? C2 P2 C7 C12 136.9(3) . . . . ? Pt1 P2 C7 C12 -104.5(3) . . . . ? C5 P1 C3 C4 176.8(3) . . . . ? C1 P1 C3 C4 -72.9(3) . . . . ? Pt1 P1 C3 C4 45.8(3) . . . . ? C7 P2 C13 C14 66.5(4) . . . . ? C2 P2 C13 C14 -46.1(4) . . . . ? Pt1 P2 C13 C14 -161.6(3) . . . . ? C7 P2 C13 C18 -114.2(3) . . . . ? C2 P2 C13 C18 133.2(3) . . . . ? Pt1 P2 C13 C18 17.7(4) . . . . ? C14 C13 C18 C17 0.1(6) . . . . ? P2 C13 C18 C17 -179.2(3) . . . . ? C3 P1 C5 C6 40.0(3) . . . . ? C1 P1 C5 C6 -69.4(3) . . . . ? Pt1 P1 C5 C6 170.3(2) . . . . ? C3 P1 C1 C2 150.6(3) . . . . ? C5 P1 C1 C2 -99.2(3) . . . . ? Pt1 P1 C1 C2 26.8(3) . . . . ? P1 C1 C2 P2 -48.9(3) . . . . ? C13 P2 C2 C1 -71.4(3) . . . . ? C7 P2 C2 C1 175.7(3) . . . . ? Pt1 P2 C2 C1 49.0(3) . . . . ? C37 P4 C31 C32 152.9(3) . . . . ? C6 P4 C31 C32 50.0(4) . . . . ? C37 P4 C31 C36 -31.4(4) . . . . ? C6 P4 C31 C36 -134.4(4) . . . . ? C19 P3 C25 C26 39.5(4) . . . . ? C4 P3 C25 C26 -65.1(4) . . . . ? C19 P3 C25 C30 -147.4(4) . . . . ? C4 P3 C25 C30 108.0(4) . . . . ? P1 C3 C4 P3 151.1(2) . . . . ? C19 P3 C4 C3 -177.7(3) . . . . ? C25 P3 C4 C3 -72.9(3) . . . . ? C31 P4 C37 C38 138.5(4) . . . . ? C6 P4 C37 C38 -119.4(4) . . . . ? C31 P4 C37 C42 -44.0(4) . . . . ? C6 P4 C37 C42 58.1(4) . . . . ? C8 C7 C12 C11 -0.7(6) . . . . ? P2 C7 C12 C11 175.9(3) . . . . ? C30 C25 C26 C27 -0.8(8) . . . . ? P3 C25 C26 C27 172.2(4) . . . . ? C7 C12 C11 C10 1.0(7) . . . . ? C12 C11 C10 C9 -0.2(8) . . . . ? C11 C10 C9 C8 -0.8(7) . . . . ? C10 C9 C8 C7 1.0(7) . . . . ? C12 C7 C8 C9 -0.3(6) . . . . ? P2 C7 C8 C9 -176.9(3) . . . . ? C36 C31 C32 C33 0.7(6) . . . . ? P4 C31 C32 C33 176.6(3) . . . . ? C38 C37 C42 C41 0.4(7) . . . . ? P4 C37 C42 C41 -177.1(4) . . . . ? P1 C5 C6 P4 167.8(2) . . . . ? C37 P4 C6 C5 60.7(3) . . . . ? C31 P4 C6 C5 166.0(3) . . . . ? C32 C31 C36 C35 -1.8(7) . . . . ? P4 C31 C36 C35 -177.5(4) . . . . ? C28 C29 C30 C25 -0.8(10) . . . . ? C26 C25 C30 C29 1.6(8) . . . . ? P3 C25 C30 C29 -171.8(5) . . . . ? C23 C24 C19 C20 2.4(8) . . . . ? C23 C24 C19 P3 175.4(4) . . . . ? C25 P3 C19 C20 -137.1(4) . . . . ? C4 P3 C19 C20 -37.2(4) . . . . ? C25 P3 C19 C24 50.2(4) . . . . ? C4 P3 C19 C24 150.1(4) . . . . ? C42 C37 C38 C39 0.0(7) . . . . ? P4 C37 C38 C39 177.7(4) . . . . ? C13 C18 C17 C16 1.1(7) . . . . ? C24 C19 C20 C21 -2.7(7) . . . . ? P3 C19 C20 C21 -175.7(4) . . . . ? C19 C24 C23 C22 -0.8(9) . . . . ? C24 C23 C22 C21 -0.5(9) . . . . ? C35 C34 C33 C32 -2.0(8) . . . . ? C31 C32 C33 C34 1.2(7) . . . . ? C25 C26 C27 C28 -0.9(9) . . . . ? C18 C13 C14 C15 -1.2(7) . . . . ? P2 C13 C14 C15 178.2(4) . . . . ? C33 C34 C35 C36 1.0(8) . . . . ? C31 C36 C35 C34 1.0(8) . . . . ? C30 C29 C28 C27 -1.0(11) . . . . ? C26 C27 C28 C29 1.8(11) . . . . ? C13 C14 C15 C16 1.1(9) . . . . ? C41 C40 C39 C38 0.5(10) . . . . ? C37 C38 C39 C40 -0.5(9) . . . . ? C23 C22 C21 C20 0.1(10) . . . . ? C19 C20 C21 C22 1.6(9) . . . . ? C18 C17 C16 C15 -1.3(9) . . . . ? C14 C15 C16 C17 0.2(9) . . . . ? C39 C40 C41 C42 0.0(9) . . . . ? C37 C42 C41 C40 -0.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.830 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.089