# Supplementary Material (ESI) for Chemical Science # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1475 loop_ _publ_author_name 'Waterman, Rory' 'Tilley, T.' _publ_contact_author_name 'Tilley, T.' _publ_contact_author_email tdtilley@berkeley.edu _publ_section_title ; Terminal Hafnium Phosphinidene Complexes and Phosphinidene Ligand Exchange ; # Attachment '- CpCpHfMe(PHPh).CIF' data_rw04m _database_code_depnum_ccdc_archive 'CCDC 815160' #TrackingRef '- CpCpHfMe(PHPh).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H28 Hf P' _chemical_formula_weight 501.90 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.4351(9) _cell_length_b 28.233(3) _cell_length_c 8.7547(9) _cell_angle_alpha 90.00 _cell_angle_beta 107.590(2) _cell_angle_gamma 90.00 _cell_volume 1987.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 148(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.110 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 5.330 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4402 _exptl_absorpt_correction_T_max 0.5558 _exptl_absorpt_process_details ? _exptl_special_details 'G. Sheldrick, Bruker Analytical X-ray Systems, Madison' _diffrn_ambient_temperature 148(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8965 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.25 _reflns_number_total 3377 _reflns_number_gt 2831 _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, 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^)+(0.0500P)^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 3377 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hf Hf 0.32865(3) 0.873433(8) 0.75562(3) 0.01966(11) Uani 1 1 d . . . P P 0.1383(2) 0.90368(6) 0.4745(2) 0.0315(4) Uani 1 1 d . . . C11 C 0.5613(7) 0.9198(2) 0.9418(7) 0.0231(13) Uani 1 1 d . . . C25 C 0.3899(10) 0.7859(2) 0.7859(8) 0.0423(18) Uani 1 1 d . . . H25A H 0.3491 0.7634 0.8539 0.051 Uiso 1 1 calc R . . C12 C 0.5053(7) 0.9459(2) 0.7992(7) 0.0231(13) Uani 1 1 d . . . C22 C 0.4274(8) 0.8223(2) 0.5664(8) 0.0363(16) Uani 1 1 d . . . H22A H 0.4157 0.8298 0.4519 0.044 Uiso 1 1 calc R . . C24 C 0.5417(9) 0.8119(2) 0.8347(8) 0.0427(18) Uani 1 1 d . . . H24A H 0.6282 0.8094 0.9415 0.051 Uiso 1 1 calc R . . C13 C 0.3432(7) 0.9622(2) 0.7864(7) 0.0238(13) Uani 1 1 d . . . C121 C 0.6032(8) 0.9594(2) 0.6895(8) 0.0356(16) Uani 1 1 d . . . H12A H 0.6639 0.9889 0.7273 0.053 Uiso 1 1 calc R . . H12B H 0.5275 0.9642 0.5810 0.053 Uiso 1 1 calc R . . H12C H 0.6823 0.9342 0.6880 0.053 Uiso 1 1 calc R . . C36 C -0.1303(8) 0.8384(2) 0.4290(7) 0.0320(15) Uani 1 1 d . . . H36A H -0.1615 0.8557 0.5086 0.038 Uiso 1 1 calc R . . C15 C 0.4346(7) 0.9174(2) 1.0150(7) 0.0224(13) Uani 1 1 d . . . C31 C 0.0095(7) 0.8527(2) 0.3864(6) 0.0246(13) Uani 1 1 d . . . C34 C -0.1838(8) 0.7746(2) 0.2392(7) 0.0380(17) Uani 1 1 d . . . H34A H -0.2486 0.7481 0.1897 0.046 Uiso 1 1 calc R . . C14 C 0.2975(7) 0.9448(2) 0.9190(7) 0.0241(13) Uani 1 1 d . . . C35 C -0.2244(8) 0.7996(2) 0.3572(8) 0.0348(16) Uani 1 1 d . . . H35A H -0.3175 0.7901 0.3898 0.042 Uiso 1 1 calc R . . C111 C 0.7365(7) 0.9014(2) 1.0173(7) 0.0304(14) Uani 1 1 d . . . H11A H 0.8044 0.9261 1.0849 0.046 Uiso 1 1 calc R . . H11B H 0.7853 0.8926 0.9328 0.046 Uiso 1 1 calc R . . H11C H 0.7330 0.8735 1.0828 0.046 Uiso 1 1 calc R . . C23 C 0.5638(9) 0.8334(3) 0.6974(9) 0.0444(18) Uani 1 1 d . . . H23A H 0.6680 0.8492 0.6917 0.053 Uiso 1 1 calc R . . C151 C 0.4433(8) 0.8939(2) 1.1720(7) 0.0339(15) Uani 1 1 d . . . H15A H 0.4879 0.9164 1.2600 0.051 Uiso 1 1 calc R . . H15B H 0.5162 0.8662 1.1874 0.051 Uiso 1 1 calc R . . H15C H 0.3316 0.8840 1.1707 0.051 Uiso 1 1 calc R . . C131 C 0.2492(8) 0.9996(2) 0.6697(8) 0.0331(15) Uani 1 1 d . . . H13A H 0.2817 1.0311 0.7153 0.050 Uiso 1 1 calc R . . H13B H 0.1294 0.9952 0.6499 0.050 Uiso 1 1 calc R . . H13C H 0.2757 0.9966 0.5686 0.050 Uiso 1 1 calc R . . C141 C 0.1428(7) 0.9572(2) 0.9624(8) 0.0334(15) Uani 1 1 d . . . H14A H 0.1614 0.9866 1.0250 0.050 Uiso 1 1 calc R . . H14B H 0.1166 0.9315 1.0260 0.050 Uiso 1 1 calc R . . H14C H 0.0499 0.9616 0.8643 0.050 Uiso 1 1 calc R . . C32 C 0.0468(8) 0.8267(2) 0.2660(8) 0.0317(14) Uani 1 1 d . . . H32A H 0.1400 0.8356 0.2328 0.038 Uiso 1 1 calc R . . C33 C -0.0487(8) 0.7884(2) 0.1939(7) 0.0349(16) Uani 1 1 d . . . H33A H -0.0205 0.7714 0.1120 0.042 Uiso 1 1 calc R . . C1 C 0.1260(10) 0.8454(3) 0.8459(9) 0.050(2) Uani 1 1 d . . . H1A H 0.1744 0.8322 0.9535 0.075 Uiso 1 1 calc R . . H1B H 0.0649 0.8206 0.7736 0.075 Uiso 1 1 calc R . . H1C H 0.0496 0.8712 0.8503 0.075 Uiso 1 1 calc R . . C21 C 0.3183(9) 0.7931(2) 0.6211(8) 0.0402(17) Uani 1 1 d . . . H21A H 0.2158 0.7772 0.5518 0.048 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 Hf 0.02143(16) 0.01997(16) 0.01761(16) 0.00003(10) 0.00597(10) 0.00055(10) P 0.0321(9) 0.0277(9) 0.0271(9) 0.0000(7) -0.0022(7) -0.0003(7) C11 0.020(3) 0.024(3) 0.021(3) -0.001(2) 0.000(2) -0.002(2) C25 0.065(5) 0.018(3) 0.042(4) 0.007(3) 0.014(4) 0.008(3) C12 0.018(3) 0.026(3) 0.024(3) -0.001(2) 0.004(2) -0.003(2) C22 0.042(4) 0.039(4) 0.031(4) -0.005(3) 0.016(3) 0.007(3) C24 0.054(5) 0.033(4) 0.030(4) -0.002(3) -0.004(3) 0.016(3) C13 0.025(3) 0.021(3) 0.022(3) -0.004(2) 0.001(3) -0.004(2) C121 0.034(4) 0.041(4) 0.032(4) 0.002(3) 0.011(3) -0.005(3) C36 0.032(4) 0.041(4) 0.019(3) 0.007(3) 0.002(3) 0.009(3) C15 0.021(3) 0.027(3) 0.018(3) -0.007(2) 0.002(2) -0.002(2) C31 0.029(3) 0.025(3) 0.014(3) 0.003(2) -0.003(3) 0.003(3) C34 0.045(5) 0.030(4) 0.033(4) 0.004(3) 0.003(3) -0.008(3) C14 0.024(3) 0.025(3) 0.025(3) -0.010(2) 0.009(3) -0.005(2) C35 0.028(4) 0.043(4) 0.032(4) 0.009(3) 0.007(3) -0.007(3) C111 0.019(3) 0.038(4) 0.031(3) -0.002(3) 0.002(3) 0.003(3) C23 0.041(4) 0.041(4) 0.053(5) -0.009(4) 0.017(4) 0.007(3) C151 0.032(4) 0.046(4) 0.023(3) 0.003(3) 0.007(3) -0.008(3) C131 0.035(4) 0.015(3) 0.043(4) 0.001(3) 0.003(3) 0.004(3) C141 0.027(4) 0.038(4) 0.035(4) -0.013(3) 0.009(3) 0.005(3) C32 0.027(3) 0.035(4) 0.034(4) 0.000(3) 0.009(3) -0.002(3) C33 0.037(4) 0.037(4) 0.026(4) -0.005(3) 0.002(3) -0.001(3) C1 0.055(5) 0.056(5) 0.047(5) -0.023(4) 0.028(4) -0.030(4) C21 0.054(5) 0.025(4) 0.036(4) -0.007(3) 0.006(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hf C1 2.234(7) . ? Hf C24 2.445(7) . ? Hf C23 2.466(7) . ? Hf C12 2.492(6) . ? Hf C15 2.504(5) . ? Hf C11 2.508(6) . ? Hf C13 2.519(6) . ? Hf C22 2.522(6) . ? Hf C25 2.523(6) . ? Hf C14 2.530(5) . ? Hf C21 2.543(6) . ? Hf P 2.6409(17) . ? P C31 1.829(6) . ? C11 C12 1.403(8) . ? C11 C15 1.404(8) . ? C11 C111 1.517(8) . ? C25 C21 1.400(9) . ? C25 C24 1.425(10) . ? C12 C13 1.414(8) . ? C12 C121 1.493(8) . ? C22 C23 1.393(10) . ? C22 C21 1.421(9) . ? C24 C23 1.409(10) . ? C13 C14 1.417(8) . ? C13 C131 1.516(8) . ? C36 C35 1.388(9) . ? C36 C31 1.400(8) . ? C15 C14 1.433(8) . ? C15 C151 1.508(8) . ? C31 C32 1.395(8) . ? C34 C33 1.371(8) . ? C34 C35 1.377(9) . ? C14 C141 1.506(7) . ? C32 C33 1.382(9) . ? 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 C1 Hf C24 102.9(3) . . ? C1 Hf C23 131.3(3) . . ? C24 Hf C23 33.3(2) . . ? C1 Hf C12 136.3(2) . . ? C24 Hf C12 100.7(2) . . ? C23 Hf C12 85.8(2) . . ? C1 Hf C15 87.5(2) . . ? C24 Hf C15 93.8(2) . . ? C23 Hf C15 109.0(2) . . ? C12 Hf C15 54.60(19) . . ? C1 Hf C11 119.2(2) . . ? C24 Hf C11 79.8(2) . . ? C23 Hf C11 81.5(2) . . ? C12 Hf C11 32.59(18) . . ? C15 Hf C11 32.54(18) . . ? C1 Hf C13 109.4(2) . . ? C24 Hf C13 132.0(2) . . ? C23 Hf C13 117.5(2) . . ? C12 Hf C13 32.78(18) . . ? C15 Hf C13 54.34(18) . . ? C11 Hf C13 53.69(18) . . ? C1 Hf C22 118.0(2) . . ? C24 Hf C22 54.4(2) . . ? C23 Hf C22 32.4(2) . . ? C12 Hf C22 105.7(2) . . ? C15 Hf C22 141.4(2) . . ? C11 Hf C22 112.1(2) . . ? C13 Hf C22 128.7(2) . . ? C1 Hf C25 76.7(3) . . ? C24 Hf C25 33.3(2) . . ? C23 Hf C25 54.6(2) . . ? C12 Hf C25 134.0(2) . . ? C15 Hf C25 112.7(2) . . ? C11 Hf C25 110.4(2) . . ? C13 Hf C25 164.1(2) . . ? C22 Hf C25 53.8(2) . . ? C1 Hf C14 82.0(2) . . ? C24 Hf C14 126.8(2) . . ? C23 Hf C14 135.1(2) . . ? C12 Hf C14 54.46(19) . . ? C15 Hf C14 33.07(19) . . ? C11 Hf C14 53.94(19) . . ? C13 Hf C14 32.58(18) . . ? C22 Hf C14 159.9(2) . . ? C25 Hf C14 140.7(2) . . ? C1 Hf C21 85.7(2) . . ? C24 Hf C21 54.3(2) . . ? C23 Hf C21 54.1(2) . . ? C12 Hf C21 137.6(2) . . ? C15 Hf C21 144.6(2) . . ? C11 Hf C21 132.6(2) . . ? C13 Hf C21 158.4(2) . . ? C22 Hf C21 32.6(2) . . ? C25 Hf C21 32.1(2) . . ? C14 Hf C21 167.5(2) . . ? C1 Hf P 97.4(2) . . ? C24 Hf P 132.96(16) . . ? C23 Hf P 104.83(18) . . ? C12 Hf P 92.53(14) . . ? C15 Hf P 129.37(14) . . ? C11 Hf P 124.94(13) . . ? C13 Hf P 76.96(13) . . ? C22 Hf P 78.56(16) . . ? C25 Hf P 117.52(17) . . ? C14 Hf P 97.54(14) . . ? C21 Hf P 86.02(16) . . ? C31 P Hf 104.77(19) . . ? C12 C11 C15 109.4(5) . . ? C12 C11 C111 126.1(5) . . ? C15 C11 C111 124.1(5) . . ? C12 C11 Hf 73.1(3) . . ? C15 C11 Hf 73.6(3) . . ? C111 C11 Hf 124.9(4) . . ? C21 C25 C24 107.6(6) . . ? C21 C25 Hf 74.8(4) . . ? C24 C25 Hf 70.3(4) . . ? C11 C12 C13 107.4(5) . . ? C11 C12 C121 127.1(5) . . ? C13 C12 C121 125.1(5) . . ? C11 C12 Hf 74.3(3) . . ? C13 C12 Hf 74.7(3) . . ? C121 C12 Hf 122.2(4) . . ? C23 C22 C21 108.1(6) . . ? C23 C22 Hf 71.6(4) . . ? C21 C22 Hf 74.5(4) . . ? C23 C24 C25 107.8(6) . . ? C23 C24 Hf 74.2(4) . . ? C25 C24 Hf 76.4(4) . . ? C12 C13 C14 108.6(5) . . ? C12 C13 C131 125.2(5) . . ? C14 C13 C131 125.2(5) . . ? C12 C13 Hf 72.6(3) . . ? C14 C13 Hf 74.1(3) . . ? C131 C13 Hf 128.5(4) . . ? C35 C36 C31 121.3(6) . . ? C11 C15 C14 107.3(5) . . ? C11 C15 C151 127.1(5) . . ? C14 C15 C151 125.5(5) . . ? C11 C15 Hf 73.9(3) . . ? C14 C15 Hf 74.5(3) . . ? C151 C15 Hf 120.9(4) . . ? C32 C31 C36 116.8(6) . . ? C32 C31 P 119.4(5) . . ? C36 C31 P 123.7(5) . . ? C33 C34 C35 119.2(6) . . ? C13 C14 C15 107.2(5) . . ? C13 C14 C141 126.7(6) . . ? C15 C14 C141 125.8(5) . . ? C13 C14 Hf 73.3(3) . . ? C15 C14 Hf 72.5(3) . . ? C141 C14 Hf 125.0(4) . . ? C34 C35 C36 120.4(6) . . ? C22 C23 C24 108.3(7) . . ? C22 C23 Hf 76.0(4) . . ? C24 C23 Hf 72.5(4) . . ? C33 C32 C31 121.5(6) . . ? C34 C33 C32 120.7(6) . . ? C25 C21 C22 108.1(7) . . ? C25 C21 Hf 73.2(4) . . ? C22 C21 Hf 72.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Hf P C31 -52.6(3) . . . . ? C24 Hf P C31 62.9(3) . . . . ? C23 Hf P C31 83.8(3) . . . . ? C12 Hf P C31 170.1(2) . . . . ? C15 Hf P C31 -145.4(3) . . . . ? C11 Hf P C31 173.8(3) . . . . ? C13 Hf P C31 -160.8(2) . . . . ? C22 Hf P C31 64.6(3) . . . . ? C25 Hf P C31 26.3(3) . . . . ? C14 Hf P C31 -135.4(2) . . . . ? C21 Hf P C31 32.6(3) . . . . ? C1 Hf C11 C12 -131.6(4) . . . . ? C24 Hf C11 C12 129.2(4) . . . . ? C23 Hf C11 C12 95.4(4) . . . . ? C15 Hf C11 C12 -116.9(5) . . . . ? C13 Hf C11 C12 -38.0(3) . . . . ? C22 Hf C11 C12 84.5(4) . . . . ? C25 Hf C11 C12 142.6(3) . . . . ? C14 Hf C11 C12 -78.7(4) . . . . ? C21 Hf C11 C12 115.0(4) . . . . ? P Hf C11 C12 -6.8(4) . . . . ? C1 Hf C11 C15 -14.7(4) . . . . ? C24 Hf C11 C15 -113.9(4) . . . . ? C23 Hf C11 C15 -147.7(4) . . . . ? C12 Hf C11 C15 116.9(5) . . . . ? C13 Hf C11 C15 78.9(4) . . . . ? C22 Hf C11 C15 -158.6(3) . . . . ? C25 Hf C11 C15 -100.5(4) . . . . ? C14 Hf C11 C15 38.2(3) . . . . ? C21 Hf C11 C15 -128.1(4) . . . . ? P Hf C11 C15 110.1(3) . . . . ? C1 Hf C11 C111 105.7(5) . . . . ? C24 Hf C11 C111 6.5(5) . . . . ? C23 Hf C11 C111 -27.2(5) . . . . ? C12 Hf C11 C111 -122.7(6) . . . . ? C15 Hf C11 C111 120.5(6) . . . . ? C13 Hf C11 C111 -160.7(6) . . . . ? C22 Hf C11 C111 -38.1(5) . . . . ? C25 Hf C11 C111 20.0(5) . . . . ? C14 Hf C11 C111 158.6(6) . . . . ? C21 Hf C11 C111 -7.6(6) . . . . ? P Hf C11 C111 -129.5(4) . . . . ? C1 Hf C25 C21 103.4(5) . . . . ? C24 Hf C25 C21 -115.4(6) . . . . ? C23 Hf C25 C21 -77.2(5) . . . . ? C12 Hf C25 C21 -113.0(5) . . . . ? C15 Hf C25 C21 -175.0(4) . . . . ? C11 Hf C25 C21 -140.1(4) . . . . ? C13 Hf C25 C21 -142.0(7) . . . . ? C22 Hf C25 C21 -37.0(4) . . . . ? C14 Hf C25 C21 162.5(4) . . . . ? P Hf C25 C21 11.9(5) . . . . ? C1 Hf C25 C24 -141.1(5) . . . . ? C23 Hf C25 C24 38.3(4) . . . . ? C12 Hf C25 C24 2.4(5) . . . . ? C15 Hf C25 C24 -59.6(4) . . . . ? C11 Hf C25 C24 -24.6(5) . . . . ? C13 Hf C25 C24 -26.5(10) . . . . ? C22 Hf C25 C24 78.5(4) . . . . ? C14 Hf C25 C24 -82.1(5) . . . . ? C21 Hf C25 C24 115.4(6) . . . . ? P Hf C25 C24 127.3(4) . . . . ? C15 C11 C12 C13 2.8(7) . . . . ? C111 C11 C12 C13 -170.9(6) . . . . ? Hf C11 C12 C13 67.9(4) . . . . ? C15 C11 C12 C121 176.1(6) . . . . ? C111 C11 C12 C121 2.5(10) . . . . ? Hf C11 C12 C121 -118.8(6) . . . . ? C15 C11 C12 Hf -65.1(4) . . . . ? C111 C11 C12 Hf 121.2(6) . . . . ? C1 Hf C12 C11 70.9(5) . . . . ? C24 Hf C12 C11 -50.9(4) . . . . ? C23 Hf C12 C11 -80.9(4) . . . . ? C15 Hf C12 C11 36.1(3) . . . . ? C13 Hf C12 C11 113.5(5) . . . . ? C22 Hf C12 C11 -106.7(4) . . . . ? C25 Hf C12 C11 -52.3(4) . . . . ? C14 Hf C12 C11 77.0(4) . . . . ? C21 Hf C12 C11 -98.7(4) . . . . ? P Hf C12 C11 174.4(3) . . . . ? C1 Hf C12 C13 -42.6(5) . . . . ? C24 Hf C12 C13 -164.4(3) . . . . ? C23 Hf C12 C13 165.6(4) . . . . ? C15 Hf C12 C13 -77.4(4) . . . . ? C11 Hf C12 C13 -113.5(5) . . . . ? C22 Hf C12 C13 139.8(3) . . . . ? C25 Hf C12 C13 -165.8(3) . . . . ? C14 Hf C12 C13 -36.5(3) . . . . ? C21 Hf C12 C13 147.8(3) . . . . ? P Hf C12 C13 60.9(3) . . . . ? C1 Hf C12 C121 -164.7(5) . . . . ? C24 Hf C12 C121 73.4(5) . . . . ? C23 Hf C12 C121 43.5(5) . . . . ? C15 Hf C12 C121 160.4(6) . . . . ? C11 Hf C12 C121 124.3(6) . . . . ? C13 Hf C12 C121 -122.2(6) . . . . ? C22 Hf C12 C121 17.6(5) . . . . ? C25 Hf C12 C121 72.1(6) . . . . ? C14 Hf C12 C121 -158.7(6) . . . . ? C21 Hf C12 C121 25.6(6) . . . . ? P Hf C12 C121 -61.2(5) . . . . ? C1 Hf C22 C23 -123.9(5) . . . . ? C24 Hf C22 C23 -37.9(4) . . . . ? C12 Hf C22 C23 54.3(5) . . . . ? C15 Hf C22 C23 2.1(6) . . . . ? C11 Hf C22 C23 20.4(5) . . . . ? C13 Hf C22 C23 80.9(5) . . . . ? C25 Hf C22 C23 -79.2(5) . . . . ? C14 Hf C22 C23 63.1(8) . . . . ? C21 Hf C22 C23 -115.6(6) . . . . ? P Hf C22 C23 143.7(4) . . . . ? C1 Hf C22 C21 -8.3(5) . . . . ? C24 Hf C22 C21 77.8(4) . . . . ? C23 Hf C22 C21 115.6(6) . . . . ? C12 Hf C22 C21 169.9(4) . . . . ? C15 Hf C22 C21 117.7(4) . . . . ? C11 Hf C22 C21 136.1(4) . . . . ? C13 Hf C22 C21 -163.5(4) . . . . ? C25 Hf C22 C21 36.4(4) . . . . ? C14 Hf C22 C21 178.7(5) . . . . ? P Hf C22 C21 -100.7(4) . . . . ? C21 C25 C24 C23 -2.1(8) . . . . ? Hf C25 C24 C23 -68.1(5) . . . . ? C21 C25 C24 Hf 66.0(5) . . . . ? C1 Hf C24 C23 152.1(4) . . . . ? C12 Hf C24 C23 -64.9(5) . . . . ? C15 Hf C24 C23 -119.6(4) . . . . ? C11 Hf C24 C23 -90.0(4) . . . . ? C13 Hf C24 C23 -76.2(5) . . . . ? C22 Hf C24 C23 36.8(4) . . . . ? C25 Hf C24 C23 113.3(6) . . . . ? C14 Hf C24 C23 -118.3(4) . . . . ? C21 Hf C24 C23 77.1(4) . . . . ? P Hf C24 C23 38.9(5) . . . . ? C1 Hf C24 C25 38.8(5) . . . . ? C23 Hf C24 C25 -113.3(6) . . . . ? C12 Hf C24 C25 -178.2(4) . . . . ? C15 Hf C24 C25 127.1(4) . . . . ? C11 Hf C24 C25 156.6(4) . . . . ? C13 Hf C24 C25 170.5(4) . . . . ? C22 Hf C24 C25 -76.6(4) . . . . ? C14 Hf C24 C25 128.4(4) . . . . ? C21 Hf C24 C25 -36.2(4) . . . . ? P Hf C24 C25 -74.5(5) . . . . ? C11 C12 C13 C14 -1.8(7) . . . . ? C121 C12 C13 C14 -175.2(6) . . . . ? Hf C12 C13 C14 65.9(4) . . . . ? C11 C12 C13 C131 167.1(5) . . . . ? C121 C12 C13 C131 -6.4(10) . . . . ? Hf C12 C13 C131 -125.2(6) . . . . ? C11 C12 C13 Hf -67.7(4) . . . . ? C121 C12 C13 Hf 118.8(6) . . . . ? C1 Hf C13 C12 150.3(4) . . . . ? C24 Hf C13 C12 20.8(5) . . . . ? C23 Hf C13 C12 -16.2(4) . . . . ? C15 Hf C13 C12 78.3(4) . . . . ? C11 Hf C13 C12 37.8(3) . . . . ? C22 Hf C13 C12 -52.8(4) . . . . ? C25 Hf C13 C12 40.0(9) . . . . ? C14 Hf C13 C12 115.9(5) . . . . ? C21 Hf C13 C12 -77.4(7) . . . . ? P Hf C13 C12 -116.3(3) . . . . ? C1 Hf C13 C14 34.4(4) . . . . ? C24 Hf C13 C14 -95.1(4) . . . . ? C23 Hf C13 C14 -132.1(4) . . . . ? C12 Hf C13 C14 -115.9(5) . . . . ? C15 Hf C13 C14 -37.6(3) . . . . ? C11 Hf C13 C14 -78.1(4) . . . . ? C22 Hf C13 C14 -168.7(3) . . . . ? C25 Hf C13 C14 -75.8(9) . . . . ? C21 Hf C13 C14 166.7(5) . . . . ? P Hf C13 C14 127.8(3) . . . . ? C1 Hf C13 C131 -88.3(6) . . . . ? C24 Hf C13 C131 142.2(5) . . . . ? C23 Hf C13 C131 105.2(5) . . . . ? C12 Hf C13 C131 121.4(7) . . . . ? C15 Hf C13 C131 -160.2(6) . . . . ? C11 Hf C13 C131 159.2(6) . . . . ? C22 Hf C13 C131 68.6(6) . . . . ? C25 Hf C13 C131 161.5(7) . . . . ? C14 Hf C13 C131 -122.7(7) . . . . ? C21 Hf C13 C131 44.1(9) . . . . ? P Hf C13 C131 5.1(5) . . . . ? C12 C11 C15 C14 -2.7(6) . . . . ? C111 C11 C15 C14 171.1(5) . . . . ? Hf C11 C15 C14 -67.5(4) . . . . ? C12 C11 C15 C151 -178.3(6) . . . . ? C111 C11 C15 C151 -4.5(9) . . . . ? Hf C11 C15 C151 116.9(6) . . . . ? C12 C11 C15 Hf 64.8(4) . . . . ? C111 C11 C15 Hf -121.4(6) . . . . ? C1 Hf C15 C11 167.2(4) . . . . ? C24 Hf C15 C11 64.4(4) . . . . ? C23 Hf C15 C11 34.0(4) . . . . ? C12 Hf C15 C11 -36.1(3) . . . . ? C13 Hf C15 C11 -76.7(4) . . . . ? C22 Hf C15 C11 32.8(5) . . . . ? C25 Hf C15 C11 92.7(4) . . . . ? C14 Hf C15 C11 -113.7(5) . . . . ? C21 Hf C15 C11 88.1(5) . . . . ? P Hf C15 C11 -95.3(3) . . . . ? C1 Hf C15 C14 -79.1(4) . . . . ? C24 Hf C15 C14 178.1(4) . . . . ? C23 Hf C15 C14 147.7(4) . . . . ? C12 Hf C15 C14 77.6(4) . . . . ? C11 Hf C15 C14 113.7(5) . . . . ? C13 Hf C15 C14 37.0(3) . . . . ? C22 Hf C15 C14 146.5(4) . . . . ? C25 Hf C15 C14 -153.6(3) . . . . ? C21 Hf C15 C14 -158.2(4) . . . . ? P Hf C15 C14 18.4(4) . . . . ? C1 Hf C15 C151 43.2(5) . . . . ? C24 Hf C15 C151 -59.5(5) . . . . ? C23 Hf C15 C151 -89.9(5) . . . . ? C12 Hf C15 C151 -160.0(6) . . . . ? C11 Hf C15 C151 -123.9(6) . . . . ? C13 Hf C15 C151 159.4(5) . . . . ? C22 Hf C15 C151 -91.1(6) . . . . ? C25 Hf C15 C151 -31.2(5) . . . . ? C14 Hf C15 C151 122.4(6) . . . . ? C21 Hf C15 C151 -35.8(7) . . . . ? P Hf C15 C151 140.8(4) . . . . ? C35 C36 C31 C32 1.6(9) . . . . ? C35 C36 C31 P 179.5(5) . . . . ? Hf P C31 C32 -103.5(5) . . . . ? Hf P C31 C36 78.6(5) . . . . ? C12 C13 C14 C15 0.1(6) . . . . ? C131 C13 C14 C15 -168.8(5) . . . . ? Hf C13 C14 C15 65.0(4) . . . . ? C12 C13 C14 C141 173.6(5) . . . . ? C131 C13 C14 C141 4.7(9) . . . . ? Hf C13 C14 C141 -121.5(6) . . . . ? C12 C13 C14 Hf -64.9(4) . . . . ? C131 C13 C14 Hf 126.2(6) . . . . ? C11 C15 C14 C13 1.6(6) . . . . ? C151 C15 C14 C13 177.3(5) . . . . ? Hf C15 C14 C13 -65.6(4) . . . . ? C11 C15 C14 C141 -171.9(5) . . . . ? C151 C15 C14 C141 3.7(9) . . . . ? Hf C15 C14 C141 120.9(6) . . . . ? C11 C15 C14 Hf 67.1(4) . . . . ? C151 C15 C14 Hf -117.2(6) . . . . ? C1 Hf C14 C13 -147.5(4) . . . . ? C24 Hf C14 C13 112.4(4) . . . . ? C23 Hf C14 C13 69.0(5) . . . . ? C12 Hf C14 C13 36.8(3) . . . . ? C15 Hf C14 C13 114.8(5) . . . . ? C11 Hf C14 C13 77.2(3) . . . . ? C22 Hf C14 C13 26.3(8) . . . . ? C25 Hf C14 C13 155.1(4) . . . . ? C21 Hf C14 C13 -156.9(9) . . . . ? P Hf C14 C13 -51.0(3) . . . . ? C1 Hf C14 C15 97.8(4) . . . . ? C24 Hf C14 C15 -2.4(5) . . . . ? C23 Hf C14 C15 -45.8(5) . . . . ? C12 Hf C14 C15 -78.0(4) . . . . ? C11 Hf C14 C15 -37.5(3) . . . . ? C13 Hf C14 C15 -114.8(5) . . . . ? C22 Hf C14 C15 -88.4(7) . . . . ? C25 Hf C14 C15 40.4(5) . . . . ? C21 Hf C14 C15 88.3(10) . . . . ? P Hf C14 C15 -165.7(3) . . . . ? C1 Hf C14 C141 -24.0(5) . . . . ? C24 Hf C14 C141 -124.2(5) . . . . ? C23 Hf C14 C141 -167.6(5) . . . . ? C12 Hf C14 C141 160.2(6) . . . . ? C15 Hf C14 C141 -121.8(6) . . . . ? C11 Hf C14 C141 -159.3(6) . . . . ? C13 Hf C14 C141 123.4(7) . . . . ? C22 Hf C14 C141 149.8(6) . . . . ? C25 Hf C14 C141 -81.4(6) . . . . ? C21 Hf C14 C141 -33.5(12) . . . . ? P Hf C14 C141 72.5(5) . . . . ? C33 C34 C35 C36 0.3(10) . . . . ? C31 C36 C35 C34 -1.4(10) . . . . ? C21 C22 C23 C24 -0.3(8) . . . . ? Hf C22 C23 C24 65.8(5) . . . . ? C21 C22 C23 Hf -66.1(5) . . . . ? C25 C24 C23 C22 1.4(8) . . . . ? Hf C24 C23 C22 -68.2(5) . . . . ? C25 C24 C23 Hf 69.6(5) . . . . ? C1 Hf C23 C22 77.4(5) . . . . ? C24 Hf C23 C22 114.8(6) . . . . ? C12 Hf C23 C22 -128.4(4) . . . . ? C15 Hf C23 C22 -178.6(4) . . . . ? C11 Hf C23 C22 -160.9(4) . . . . ? C13 Hf C23 C22 -119.7(4) . . . . ? C25 Hf C23 C22 76.6(5) . . . . ? C14 Hf C23 C22 -154.2(4) . . . . ? C21 Hf C23 C22 36.8(4) . . . . ? P Hf C23 C22 -36.9(4) . . . . ? C1 Hf C23 C24 -37.4(6) . . . . ? C12 Hf C23 C24 116.8(4) . . . . ? C15 Hf C23 C24 66.6(5) . . . . ? C11 Hf C23 C24 84.3(4) . . . . ? C13 Hf C23 C24 125.6(4) . . . . ? C22 Hf C23 C24 -114.8(6) . . . . ? C25 Hf C23 C24 -38.2(4) . . . . ? C14 Hf C23 C24 91.0(5) . . . . ? C21 Hf C23 C24 -77.9(5) . . . . ? P Hf C23 C24 -151.6(4) . . . . ? C36 C31 C32 C33 -0.8(9) . . . . ? P C31 C32 C33 -178.9(5) . . . . ? C35 C34 C33 C32 0.4(10) . . . . ? C31 C32 C33 C34 -0.1(10) . . . . ? C24 C25 C21 C22 1.9(8) . . . . ? Hf C25 C21 C22 65.0(5) . . . . ? C24 C25 C21 Hf -63.1(5) . . . . ? C23 C22 C21 C25 -1.0(8) . . . . ? Hf C22 C21 C25 -65.2(5) . . . . ? C23 C22 C21 Hf 64.2(5) . . . . ? C1 Hf C21 C25 -71.7(5) . . . . ? C24 Hf C21 C25 37.6(5) . . . . ? C23 Hf C21 C25 79.0(5) . . . . ? C12 Hf C21 C25 101.2(5) . . . . ? C15 Hf C21 C25 7.9(7) . . . . ? C11 Hf C21 C25 54.8(5) . . . . ? C13 Hf C21 C25 152.7(5) . . . . ? C22 Hf C21 C25 115.7(6) . . . . ? C14 Hf C21 C25 -62.2(12) . . . . ? P Hf C21 C25 -169.4(4) . . . . ? C1 Hf C21 C22 172.7(5) . . . . ? C24 Hf C21 C22 -78.1(4) . . . . ? C23 Hf C21 C22 -36.6(4) . . . . ? C12 Hf C21 C22 -14.5(5) . . . . ? C15 Hf C21 C22 -107.7(5) . . . . ? C11 Hf C21 C22 -60.8(5) . . . . ? C13 Hf C21 C22 37.0(8) . . . . ? C25 Hf C21 C22 -115.7(6) . . . . ? C14 Hf C21 C22 -177.9(8) . . . . ? P Hf C21 C22 74.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 1.238 _refine_diff_density_min -1.880 _refine_diff_density_rms 0.160 # Attachment '- phosphinidene.CIF' data_rw05m _database_code_depnum_ccdc_archive 'CCDC 815161' #TrackingRef '- phosphinidene.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H69 P5 Pt2' _chemical_formula_weight 1022.92 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.699(3) _cell_length_b 15.370(4) _cell_length_c 45.229(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8133(3) _cell_formula_units_Z 8 _cell_measurement_temperature 139(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4032 _exptl_absorpt_coefficient_mu 7.091 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4639 _exptl_absorpt_correction_T_max 0.6112 _exptl_absorpt_process_details 'SHELXL-97 (Sheldrick, 1997)' _exptl_special_details 'G. Sheldrick, Bruker Analytical X-ray Systems, Madison' _diffrn_ambient_temperature 139(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35685 _diffrn_reflns_av_R_equivalents 0.1434 _diffrn_reflns_av_sigmaI/netI 0.1246 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.25 _reflns_number_total 7118 _reflns_number_gt 3758 _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, 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^)+(0.0290P)^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 7118 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1243 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.0965 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_restrained_S_all 0.884 _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 0.02926(4) 0.79948(3) 0.403679(8) 0.02417(12) Uani 1 1 d . . . Pt2 Pt 0.03199(4) 0.80796(3) 0.343181(8) 0.02327(12) Uani 1 1 d . . . P4 P 0.0965(3) 0.7721(2) 0.29828(7) 0.0306(8) Uani 1 1 d . . . P5 P 0.1663(2) 0.74160(18) 0.37301(8) 0.0264(7) Uani 1 1 d . . . P3 P -0.1034(3) 0.8905(2) 0.32084(7) 0.0322(8) Uani 1 1 d . . . P2 P -0.1201(3) 0.8618(2) 0.42753(7) 0.0355(8) Uani 1 1 d . . . P1 P 0.0881(3) 0.74768(19) 0.44727(7) 0.0310(9) Uani 1 1 d . . . C1 C -0.0044(9) 0.7935(7) 0.4761(2) 0.038(3) Uani 1 1 d . . . H1A H -0.0074 0.7531 0.4931 0.045 Uiso 1 1 calc R . . H1B H 0.0282 0.8493 0.4831 0.045 Uiso 1 1 calc R . . C52 C 0.0413(9) 0.5810(7) 0.3698(2) 0.037(3) Uani 1 1 d . . . H52A H -0.0256 0.6146 0.3665 0.044 Uiso 1 1 calc R . . C4 C 0.0049(9) 0.8196(7) 0.2699(2) 0.039(3) Uani 1 1 d . . . H4A H 0.0541 0.8460 0.2545 0.046 Uiso 1 1 calc R . . H4B H -0.0392 0.7723 0.2604 0.046 Uiso 1 1 calc R . . C421 C 0.1004(11) 0.6541(7) 0.2876(3) 0.046(4) Uani 1 1 d . . . H42A H 0.1517 0.6240 0.3020 0.055 Uiso 1 1 calc R . . C53 C 0.0319(12) 0.4909(8) 0.3716(3) 0.056(4) Uani 1 1 d . . . H53A H -0.0411 0.4641 0.3704 0.068 Uiso 1 1 calc R . . C121 C 0.0765(10) 0.6289(7) 0.4518(2) 0.037(3) Uani 1 1 d . . . H12A H 0.1269 0.6023 0.4364 0.045 Uiso 1 1 calc R . . C123 C -0.0445(10) 0.5977(7) 0.4453(3) 0.051(4) Uani 1 1 d . . . H12B H -0.0481 0.5344 0.4477 0.076 Uiso 1 1 calc R . . H12C H -0.0653 0.6133 0.4250 0.076 Uiso 1 1 calc R . . H12D H -0.0978 0.6254 0.4591 0.076 Uiso 1 1 calc R . . C51 C 0.1455(8) 0.6229(7) 0.3726(2) 0.028(3) Uani 1 1 d . . . C211 C -0.1194(9) 0.9816(7) 0.4344(2) 0.033(3) Uani 1 1 d . . . H21A H -0.1763 1.0074 0.4204 0.039 Uiso 1 1 calc R . . C2 C -0.1260(10) 0.8091(8) 0.4644(2) 0.048(3) Uani 1 1 d . . . H2A H -0.1685 0.8467 0.4784 0.058 Uiso 1 1 calc R . . H2B H -0.1669 0.7529 0.4629 0.058 Uiso 1 1 calc R . . C411 C 0.2398(10) 0.8124(9) 0.2877(2) 0.047(4) Uani 1 1 d . . . H41A H 0.2489 0.8031 0.2659 0.057 Uiso 1 1 calc R . . C321 C -0.1122(11) 1.0087(7) 0.3262(3) 0.047(4) Uani 1 1 d . . . H32A H -0.1592 1.0342 0.3099 0.056 Uiso 1 1 calc R . . C111 C 0.2337(10) 0.7726(8) 0.4610(3) 0.037(3) Uani 1 1 d . . . H11A H 0.2370 0.7559 0.4823 0.044 Uiso 1 1 calc R . . C56 C 0.2417(9) 0.5686(7) 0.3763(3) 0.037(3) Uani 1 1 d . . . H56A H 0.3154 0.5940 0.3779 0.044 Uiso 1 1 calc R . . C54 C 0.1286(10) 0.4402(7) 0.3753(3) 0.042(3) Uani 1 1 d . . . H54A H 0.1234 0.3785 0.3761 0.050 Uiso 1 1 calc R . . C113 C 0.2597(10) 0.8701(8) 0.4588(3) 0.053(4) Uani 1 1 d . . . H11B H 0.3367 0.8814 0.4664 0.080 Uiso 1 1 calc R . . H11C H 0.2038 0.9028 0.4705 0.080 Uiso 1 1 calc R . . H11D H 0.2553 0.8885 0.4381 0.080 Uiso 1 1 calc R . . C122 C 0.1164(12) 0.5929(8) 0.4815(3) 0.070(5) Uani 1 1 d . . . H12E H 0.1078 0.5295 0.4816 0.105 Uiso 1 1 calc R . . H12F H 0.0700 0.6181 0.4974 0.105 Uiso 1 1 calc R . . H12G H 0.1969 0.6081 0.4846 0.105 Uiso 1 1 calc R . . C112 C 0.3238(10) 0.7214(9) 0.4449(3) 0.057(4) Uani 1 1 d . . . H11E H 0.3992 0.7356 0.4530 0.086 Uiso 1 1 calc R . . H11F H 0.3219 0.7362 0.4238 0.086 Uiso 1 1 calc R . . H11G H 0.3091 0.6591 0.4474 0.086 Uiso 1 1 calc R . . C223 C -0.3660(11) 0.8580(9) 0.4347(3) 0.070(5) Uani 1 1 d . . . H22A H -0.4385 0.8445 0.4249 0.105 Uiso 1 1 calc R . . H22B H -0.3652 0.9194 0.4405 0.105 Uiso 1 1 calc R . . H22C H -0.3577 0.8214 0.4523 0.105 Uiso 1 1 calc R . . C213 C -0.1529(10) 1.0132(8) 0.4653(2) 0.052(4) Uani 1 1 d . . . H21B H -0.1491 1.0769 0.4660 0.078 Uiso 1 1 calc R . . H21C H -0.1000 0.9888 0.4799 0.078 Uiso 1 1 calc R . . H21D H -0.2309 0.9942 0.4698 0.078 Uiso 1 1 calc R . . C3 C -0.0770(11) 0.8870(10) 0.2805(3) 0.077(5) Uani 1 1 d . . . H3A H -0.1510 0.8775 0.2705 0.092 Uiso 1 1 calc R . . H3B H -0.0482 0.9447 0.2743 0.092 Uiso 1 1 calc R . . C313 C -0.3409(10) 0.9070(9) 0.3055(3) 0.070(5) Uani 1 1 d . . . H31A H -0.4174 0.8827 0.3085 0.105 Uiso 1 1 calc R . . H31B H -0.3208 0.9036 0.2845 0.105 Uiso 1 1 calc R . . H31C H -0.3401 0.9680 0.3118 0.105 Uiso 1 1 calc R . . C413 C 0.2520(12) 0.9083(9) 0.2936(3) 0.086(6) Uani 1 1 d . . . H41B H 0.3285 0.9275 0.2877 0.130 Uiso 1 1 calc R . . H41C H 0.2408 0.9196 0.3147 0.130 Uiso 1 1 calc R . . H41D H 0.1945 0.9403 0.2822 0.130 Uiso 1 1 calc R . . C423 C 0.1489(12) 0.6368(8) 0.2566(2) 0.064(4) Uani 1 1 d . . . H42B H 0.1496 0.5740 0.2528 0.096 Uiso 1 1 calc R . . H42C H 0.2271 0.6595 0.2554 0.096 Uiso 1 1 calc R . . H42D H 0.1011 0.6658 0.2418 0.096 Uiso 1 1 calc R . . C221 C -0.2691(10) 0.8406(8) 0.4139(3) 0.050(4) Uani 1 1 d . . . H22D H -0.2807 0.8810 0.3969 0.060 Uiso 1 1 calc R . . C212 C -0.0033(10) 1.0215(7) 0.4264(3) 0.068(5) Uani 1 1 d . . . H21E H -0.0052 1.0843 0.4302 0.102 Uiso 1 1 calc R . . H21F H 0.0130 1.0111 0.4055 0.102 Uiso 1 1 calc R . . H21G H 0.0565 0.9947 0.4386 0.102 Uiso 1 1 calc R . . C55 C 0.2308(11) 0.4809(8) 0.3777(3) 0.047(3) Uani 1 1 d . . . H55A H 0.2976 0.4466 0.3805 0.056 Uiso 1 1 calc R . . C422 C -0.0166(12) 0.6143(9) 0.2908(3) 0.091(6) Uani 1 1 d . . . H42E H -0.0134 0.5526 0.2854 0.137 Uiso 1 1 calc R . . H42F H -0.0706 0.6446 0.2779 0.137 Uiso 1 1 calc R . . H42G H -0.0419 0.6196 0.3114 0.137 Uiso 1 1 calc R . . C311 C -0.2537(10) 0.8551(8) 0.3238(3) 0.051(4) Uani 1 1 d . . . H31D H -0.2759 0.8630 0.3449 0.061 Uiso 1 1 calc R . . C412 C 0.3351(12) 0.7611(11) 0.3033(3) 0.094(6) Uani 1 1 d . . . H41E H 0.4097 0.7836 0.2971 0.141 Uiso 1 1 calc R . . H41F H 0.3292 0.6994 0.2981 0.141 Uiso 1 1 calc R . . H41G H 0.3271 0.7677 0.3248 0.141 Uiso 1 1 calc R . . C312 C -0.2632(12) 0.7578(9) 0.3174(3) 0.077(5) Uani 1 1 d . . . H31E H -0.3432 0.7396 0.3191 0.116 Uiso 1 1 calc R . . H31F H -0.2169 0.7254 0.3318 0.116 Uiso 1 1 calc R . . H31G H -0.2355 0.7458 0.2974 0.116 Uiso 1 1 calc R . . C322 C 0.0066(11) 1.0490(9) 0.3252(4) 0.103(7) Uani 1 1 d . . . H32B H 0.0005 1.1121 0.3279 0.154 Uiso 1 1 calc R . . H32C H 0.0421 1.0365 0.3061 0.154 Uiso 1 1 calc R . . H32D H 0.0536 1.0244 0.3411 0.154 Uiso 1 1 calc R . . C323 C -0.1700(14) 1.0293(8) 0.3560(3) 0.086(5) Uani 1 1 d . . . H32E H -0.1759 1.0925 0.3584 0.130 Uiso 1 1 calc R . . H32F H -0.1243 1.0049 0.3721 0.130 Uiso 1 1 calc R . . H32G H -0.2467 1.0036 0.3563 0.130 Uiso 1 1 calc R . . C222 C -0.2784(12) 0.7478(9) 0.4011(3) 0.073(5) Uani 1 1 d . . . H22E H -0.3565 0.7378 0.3940 0.109 Uiso 1 1 calc R . . H22F H -0.2599 0.7053 0.4165 0.109 Uiso 1 1 calc R . . H22G H -0.2248 0.7415 0.3846 0.109 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 0.0273(3) 0.0257(2) 0.0195(2) 0.0005(2) -0.0003(2) 0.0005(3) Pt2 0.0265(2) 0.0252(2) 0.0181(2) 0.00268(19) -0.0009(2) -0.0001(3) P4 0.039(2) 0.0340(18) 0.0192(18) 0.0037(14) 0.0020(15) -0.0009(16) P5 0.0277(15) 0.0263(16) 0.0251(17) 0.0022(14) 0.0008(18) 0.0011(13) P3 0.033(2) 0.037(2) 0.0261(19) 0.0030(15) -0.0063(15) 0.0046(16) P2 0.037(2) 0.038(2) 0.032(2) 0.0033(15) 0.0057(16) 0.0030(16) P1 0.036(2) 0.035(2) 0.0215(19) -0.0013(14) -0.0010(16) 0.0010(15) C1 0.047(9) 0.024(7) 0.042(7) -0.004(6) -0.005(6) 0.010(6) C52 0.037(7) 0.026(6) 0.047(8) -0.002(6) -0.001(7) -0.003(6) C4 0.048(9) 0.042(8) 0.025(7) 0.010(6) 0.007(6) 0.011(6) C421 0.062(10) 0.034(8) 0.042(9) -0.004(6) 0.023(7) 0.003(7) C53 0.063(9) 0.046(8) 0.060(9) 0.007(7) -0.027(9) -0.014(8) C121 0.052(8) 0.042(8) 0.017(7) 0.005(6) 0.005(6) 0.008(7) C123 0.049(9) 0.043(8) 0.061(10) 0.011(7) 0.000(8) 0.003(8) C51 0.027(6) 0.032(7) 0.025(6) -0.012(6) 0.001(6) -0.012(5) C211 0.030(7) 0.032(7) 0.036(8) -0.001(6) 0.009(6) 0.006(6) C2 0.049(9) 0.058(9) 0.038(8) 0.002(7) 0.013(6) 0.018(8) C411 0.040(8) 0.076(11) 0.026(8) 0.016(7) 0.015(6) -0.018(8) C321 0.062(10) 0.031(8) 0.047(9) 0.004(6) -0.016(7) 0.015(7) C111 0.030(8) 0.059(9) 0.022(7) -0.004(6) -0.010(6) -0.001(7) C56 0.043(7) 0.024(7) 0.044(8) -0.004(6) -0.002(7) 0.000(6) C54 0.060(9) 0.026(7) 0.038(8) 0.007(6) -0.014(7) 0.009(7) C113 0.056(9) 0.059(10) 0.044(9) -0.016(7) -0.020(7) -0.003(8) C122 0.132(15) 0.052(9) 0.026(8) 0.023(7) 0.002(8) -0.004(9) C112 0.027(8) 0.096(12) 0.048(10) 0.002(8) -0.011(7) 0.011(8) C223 0.047(10) 0.070(11) 0.094(13) -0.015(9) 0.014(8) 0.002(8) C213 0.057(9) 0.064(10) 0.034(9) -0.015(7) -0.007(7) 0.011(7) C3 0.069(10) 0.139(14) 0.023(8) 0.018(9) -0.012(7) 0.053(11) C313 0.034(8) 0.116(14) 0.061(11) -0.008(9) -0.022(8) 0.017(9) C413 0.109(14) 0.090(13) 0.060(11) -0.028(9) 0.045(9) -0.066(11) C423 0.113(13) 0.052(9) 0.027(9) -0.016(7) 0.013(8) -0.001(9) C221 0.024(7) 0.043(8) 0.083(12) -0.002(8) 0.002(7) -0.001(7) C212 0.075(13) 0.031(8) 0.098(12) -0.031(8) 0.020(8) -0.017(7) C55 0.057(9) 0.035(8) 0.049(9) -0.001(7) 0.004(8) 0.011(7) C422 0.111(14) 0.083(12) 0.079(12) -0.035(9) 0.049(10) -0.047(11) C311 0.038(8) 0.053(9) 0.060(10) 0.001(7) -0.014(7) 0.014(7) C412 0.043(11) 0.20(2) 0.042(11) 0.013(10) -0.001(9) 0.007(11) C312 0.059(12) 0.065(11) 0.109(15) 0.006(10) -0.024(10) -0.022(9) C322 0.053(13) 0.056(11) 0.20(2) 0.025(11) -0.033(11) -0.012(9) C323 0.159(17) 0.042(10) 0.058(12) 0.001(8) -0.012(11) 0.004(10) C222 0.061(11) 0.082(12) 0.075(13) -0.013(9) -0.007(9) -0.019(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 P1 2.235(3) . ? Pt1 P2 2.266(3) . ? Pt1 P5 2.299(3) . ? Pt1 Pt2 2.7396(9) . ? Pt2 P4 2.236(3) . ? Pt2 P3 2.267(3) . ? Pt2 P5 2.309(3) . ? P4 C4 1.825(11) . ? P4 C411 1.851(12) . ? P4 C421 1.877(11) . ? P5 C51 1.841(10) . ? P3 C321 1.835(11) . ? P3 C311 1.845(13) . ? P3 C3 1.850(12) . ? P2 C2 1.855(11) . ? P2 C211 1.867(11) . ? P2 C221 1.877(12) . ? P1 C1 1.834(11) . ? P1 C121 1.841(11) . ? P1 C111 1.853(11) . ? C1 C2 1.536(14) . ? C52 C51 1.385(13) . ? C52 C53 1.391(14) . ? C4 C3 1.490(14) . ? C421 C422 1.507(15) . ? C421 C423 1.535(14) . ? C53 C54 1.384(14) . ? C121 C123 1.522(14) . ? C121 C122 1.528(13) . ? C51 C56 1.411(13) . ? C211 C213 1.532(13) . ? C211 C212 1.533(13) . ? C411 C413 1.505(16) . ? C411 C412 1.537(17) . ? C321 C322 1.522(15) . ? C321 C323 1.538(16) . ? C111 C112 1.503(15) . ? C111 C113 1.533(14) . ? C56 C55 1.356(13) . ? C54 C55 1.355(14) . ? C223 C221 1.496(15) . ? C313 C311 1.536(15) . ? C221 C222 1.544(16) . ? C311 C312 1.528(15) . ? 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 P1 Pt1 P2 88.18(12) . . ? P1 Pt1 P5 100.34(12) . . ? P2 Pt1 P5 171.32(12) . . ? P1 Pt1 Pt2 153.44(9) . . ? P2 Pt1 Pt2 117.67(8) . . ? P5 Pt1 Pt2 53.69(8) . . ? P4 Pt2 P3 88.24(12) . . ? P4 Pt2 P5 101.06(12) . . ? P3 Pt2 P5 169.50(11) . . ? P4 Pt2 Pt1 154.08(9) . . ? P3 Pt2 Pt1 117.62(8) . . ? P5 Pt2 Pt1 53.36(8) . . ? C4 P4 C411 102.5(5) . . ? C4 P4 C421 102.7(6) . . ? C411 P4 C421 103.6(6) . . ? C4 P4 Pt2 110.0(4) . . ? C411 P4 Pt2 117.3(4) . . ? C421 P4 Pt2 118.8(4) . . ? C51 P5 Pt1 107.3(3) . . ? C51 P5 Pt2 110.0(4) . . ? Pt1 P5 Pt2 72.95(8) . . ? C321 P3 C311 103.2(6) . . ? C321 P3 C3 99.8(6) . . ? C311 P3 C3 102.8(6) . . ? C321 P3 Pt2 122.3(4) . . ? C311 P3 Pt2 118.0(4) . . ? C3 P3 Pt2 107.8(4) . . ? C2 P2 C211 106.4(5) . . ? C2 P2 C221 100.6(6) . . ? C211 P2 C221 103.3(5) . . ? C2 P2 Pt1 105.8(4) . . ? C211 P2 Pt1 119.5(4) . . ? C221 P2 Pt1 119.1(4) . . ? C1 P1 C121 105.0(5) . . ? C1 P1 C111 103.0(5) . . ? C121 P1 C111 103.6(5) . . ? C1 P1 Pt1 107.9(4) . . ? C121 P1 Pt1 115.3(4) . . ? C111 P1 Pt1 120.3(4) . . ? C2 C1 P1 111.2(8) . . ? C51 C52 C53 121.8(11) . . ? C3 C4 P4 115.4(8) . . ? C422 C421 C423 110.8(11) . . ? C422 C421 P4 110.2(9) . . ? C423 C421 P4 114.4(8) . . ? C54 C53 C52 120.2(12) . . ? C123 C121 C122 109.8(10) . . ? C123 C121 P1 111.1(8) . . ? C122 C121 P1 115.7(8) . . ? C52 C51 C56 116.0(10) . . ? C52 C51 P5 125.4(8) . . ? C56 C51 P5 118.6(8) . . ? C213 C211 C212 108.2(9) . . ? C213 C211 P2 117.6(8) . . ? C212 C211 P2 111.1(7) . . ? C1 C2 P2 110.0(8) . . ? C413 C411 C412 110.6(12) . . ? C413 C411 P4 111.6(9) . . ? C412 C411 P4 111.5(9) . . ? C322 C321 C323 110.1(12) . . ? C322 C321 P3 110.4(9) . . ? C323 C321 P3 110.1(9) . . ? C112 C111 C113 110.0(10) . . ? C112 C111 P1 112.0(8) . . ? C113 C111 P1 111.3(8) . . ? C55 C56 C51 121.3(11) . . ? C55 C54 C53 118.1(12) . . ? C4 C3 P3 116.5(8) . . ? C223 C221 C222 110.4(11) . . ? C223 C221 P2 117.8(10) . . ? C222 C221 P2 110.4(8) . . ? C54 C55 C56 122.6(12) . . ? C312 C311 C313 111.1(11) . . ? C312 C311 P3 110.1(9) . . ? C313 C311 P3 116.2(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pt1 Pt2 P4 -3.1(3) . . . . ? P2 Pt1 Pt2 P4 -168.6(2) . . . . ? P5 Pt1 Pt2 P4 10.5(2) . . . . ? P1 Pt1 Pt2 P3 172.8(2) . . . . ? P2 Pt1 Pt2 P3 7.22(13) . . . . ? P5 Pt1 Pt2 P3 -173.63(13) . . . . ? P1 Pt1 Pt2 P5 -13.6(2) . . . . ? P2 Pt1 Pt2 P5 -179.15(13) . . . . ? P3 Pt2 P4 C4 -3.7(4) . . . . ? P5 Pt2 P4 C4 -178.8(4) . . . . ? Pt1 Pt2 P4 C4 172.6(4) . . . . ? P3 Pt2 P4 C411 112.8(5) . . . . ? P5 Pt2 P4 C411 -62.3(5) . . . . ? Pt1 Pt2 P4 C411 -70.9(5) . . . . ? P3 Pt2 P4 C421 -121.4(5) . . . . ? P5 Pt2 P4 C421 63.5(5) . . . . ? Pt1 Pt2 P4 C421 54.9(6) . . . . ? P1 Pt1 P5 C51 67.7(4) . . . . ? P2 Pt1 P5 C51 -101.1(8) . . . . ? Pt2 Pt1 P5 C51 -106.2(4) . . . . ? P1 Pt1 P5 Pt2 173.88(9) . . . . ? P2 Pt1 P5 Pt2 5.0(8) . . . . ? P4 Pt2 P5 C51 -72.6(4) . . . . ? P3 Pt2 P5 C51 135.4(6) . . . . ? Pt1 Pt2 P5 C51 102.7(4) . . . . ? P4 Pt2 P5 Pt1 -175.34(9) . . . . ? P3 Pt2 P5 Pt1 32.6(6) . . . . ? P4 Pt2 P3 C321 -118.3(5) . . . . ? P5 Pt2 P3 C321 34.3(9) . . . . ? Pt1 Pt2 P3 C321 63.5(5) . . . . ? P4 Pt2 P3 C311 111.8(5) . . . . ? P5 Pt2 P3 C311 -95.6(8) . . . . ? Pt1 Pt2 P3 C311 -66.4(5) . . . . ? P4 Pt2 P3 C3 -3.8(5) . . . . ? P5 Pt2 P3 C3 148.7(7) . . . . ? Pt1 Pt2 P3 C3 178.0(5) . . . . ? P1 Pt1 P2 C2 -15.2(4) . . . . ? P5 Pt1 P2 C2 153.9(7) . . . . ? Pt2 Pt1 P2 C2 158.4(4) . . . . ? P1 Pt1 P2 C211 104.6(4) . . . . ? P5 Pt1 P2 C211 -86.4(9) . . . . ? Pt2 Pt1 P2 C211 -81.8(4) . . . . ? P1 Pt1 P2 C221 -127.3(5) . . . . ? P5 Pt1 P2 C221 41.8(9) . . . . ? Pt2 Pt1 P2 C221 46.3(5) . . . . ? P2 Pt1 P1 C1 -6.1(4) . . . . ? P5 Pt1 P1 C1 175.6(4) . . . . ? Pt2 Pt1 P1 C1 -173.3(4) . . . . ? P2 Pt1 P1 C121 111.0(4) . . . . ? P5 Pt1 P1 C121 -67.4(4) . . . . ? Pt2 Pt1 P1 C121 -56.3(5) . . . . ? P2 Pt1 P1 C111 -123.7(5) . . . . ? P5 Pt1 P1 C111 58.0(5) . . . . ? Pt2 Pt1 P1 C111 69.1(5) . . . . ? C121 P1 C1 C2 -91.9(9) . . . . ? C111 P1 C1 C2 159.9(8) . . . . ? Pt1 P1 C1 C2 31.6(9) . . . . ? C411 P4 C4 C3 -112.7(10) . . . . ? C421 P4 C4 C3 140.1(10) . . . . ? Pt2 P4 C4 C3 12.7(11) . . . . ? C4 P4 C421 C422 -65.7(10) . . . . ? C411 P4 C421 C422 -172.0(9) . . . . ? Pt2 P4 C421 C422 55.8(11) . . . . ? C4 P4 C421 C423 59.9(11) . . . . ? C411 P4 C421 C423 -46.5(11) . . . . ? Pt2 P4 C421 C423 -178.6(8) . . . . ? C51 C52 C53 C54 -2.4(19) . . . . ? C1 P1 C121 C123 64.8(9) . . . . ? C111 P1 C121 C123 172.5(8) . . . . ? Pt1 P1 C121 C123 -53.9(9) . . . . ? C1 P1 C121 C122 -61.3(10) . . . . ? C111 P1 C121 C122 46.5(10) . . . . ? Pt1 P1 C121 C122 -179.9(8) . . . . ? C53 C52 C51 C56 2.3(17) . . . . ? C53 C52 C51 P5 -175.6(9) . . . . ? Pt1 P5 C51 C52 44.9(11) . . . . ? Pt2 P5 C51 C52 -32.8(11) . . . . ? Pt1 P5 C51 C56 -132.9(8) . . . . ? Pt2 P5 C51 C56 149.5(8) . . . . ? C2 P2 C211 C213 -14.8(10) . . . . ? C221 P2 C211 C213 90.7(9) . . . . ? Pt1 P2 C211 C213 -134.2(7) . . . . ? C2 P2 C211 C212 110.7(9) . . . . ? C221 P2 C211 C212 -143.8(9) . . . . ? Pt1 P2 C211 C212 -8.7(10) . . . . ? P1 C1 C2 P2 -45.3(10) . . . . ? C211 P2 C2 C1 -89.7(8) . . . . ? C221 P2 C2 C1 162.9(8) . . . . ? Pt1 P2 C2 C1 38.3(9) . . . . ? C4 P4 C411 C413 71.2(10) . . . . ? C421 P4 C411 C413 177.8(9) . . . . ? Pt2 P4 C411 C413 -49.3(10) . . . . ? C4 P4 C411 C412 -164.5(10) . . . . ? C421 P4 C411 C412 -58.0(11) . . . . ? Pt2 P4 C411 C412 75.0(11) . . . . ? C311 P3 C321 C322 178.6(10) . . . . ? C3 P3 C321 C322 -75.7(10) . . . . ? Pt2 P3 C321 C322 42.7(11) . . . . ? C311 P3 C321 C323 56.8(11) . . . . ? C3 P3 C321 C323 162.6(10) . . . . ? Pt2 P3 C321 C323 -79.0(10) . . . . ? C1 P1 C111 C112 165.4(9) . . . . ? C121 P1 C111 C112 56.2(10) . . . . ? Pt1 P1 C111 C112 -74.5(10) . . . . ? C1 P1 C111 C113 -71.0(9) . . . . ? C121 P1 C111 C113 179.7(8) . . . . ? Pt1 P1 C111 C113 49.0(9) . . . . ? C52 C51 C56 C55 -1.4(17) . . . . ? P5 C51 C56 C55 176.5(9) . . . . ? C52 C53 C54 C55 1.6(19) . . . . ? P4 C4 C3 P3 -16.7(14) . . . . ? C321 P3 C3 C4 141.5(11) . . . . ? C311 P3 C3 C4 -112.4(11) . . . . ? Pt2 P3 C3 C4 12.9(12) . . . . ? C2 P2 C221 C223 46.3(11) . . . . ? C211 P2 C221 C223 -63.5(11) . . . . ? Pt1 P2 C221 C223 161.2(9) . . . . ? C2 P2 C221 C222 -81.8(10) . . . . ? C211 P2 C221 C222 168.4(9) . . . . ? Pt1 P2 C221 C222 33.1(11) . . . . ? C53 C54 C55 C56 -0.8(19) . . . . ? C51 C56 C55 C54 0.8(19) . . . . ? C321 P3 C311 C312 175.8(9) . . . . ? C3 P3 C311 C312 72.4(10) . . . . ? Pt2 P3 C311 C312 -46.0(10) . . . . ? C321 P3 C311 C313 48.3(11) . . . . ? C3 P3 C311 C313 -55.1(11) . . . . ? Pt2 P3 C311 C313 -173.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.167 _refine_diff_density_min -1.549 _refine_diff_density_rms 0.190