# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_complex1a_m _database_code_depnum_ccdc_archive 'CCDC 895738' #TrackingRef 'Complex 1a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H64 I2 P4 Pt2' _chemical_formula_sum 'C34 H64 I2 P4 Pt2' _chemical_formula_weight 1240.71 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.395(6) _cell_length_b 13.955(9) _cell_length_c 17.449(11) _cell_angle_alpha 90.00 _cell_angle_beta 93.387(11) _cell_angle_gamma 90.00 _cell_volume 2284(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1754 _cell_measurement_theta_min 0.35 _cell_measurement_theta_max 30.50 _exptl_crystal_description 'needle shaped' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 7.630 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.289 _exptl_absorpt_correction_T_max 0.400 _exptl_absorpt_process_details SADABS _exptl_special_details ; 'The refinement was carried out employing OMIT -2 50 restrain keep the coverage 25 and therby to increase the data completeness. Moreover, PART command was employed for partitioning electron density of the thermally disrordered C atoms around the P2 atoms. As the Et groups at the P atoms are thermally highly disorder, to maintain bond distances between P-C and C-C of these phosphine groups we have used DFIX restrains and to maintain the non-bonded distance, especially between C4T and C12B, we have used DANG restrain' ; _diffrn_ambient_temperature 150(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 scan' _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19968 _diffrn_reflns_av_R_equivalents 0.1305 _diffrn_reflns_av_sigmaI/netI 0.0998 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4008 _reflns_number_gt 2187 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker kappa apex ccd' _computing_cell_refinement 'Bruker kappa apex ccd' _computing_data_reduction 'Bruker saint' _computing_structure_solution shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ortep-III _computing_publication_material WinGX1.80.05 _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^ > 2\s(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^)+(0.1077P)^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 4008 _refine_ls_number_parameters 184 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1526 _refine_ls_R_factor_gt 0.0817 _refine_ls_wR_factor_ref 0.2153 _refine_ls_wR_factor_gt 0.1782 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.003 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 0.93784(8) 0.39485(5) 0.75329(4) 0.0674(3) Uani 1 1 d . A . I1 I 1.12875(19) 0.34707(15) 0.86628(9) 0.1196(7) Uani 1 1 d . . . P1 P 1.1046(6) 0.3721(4) 0.6620(3) 0.0821(16) Uani 1 1 d D . . P2 P 0.7641(6) 0.4263(5) 0.8390(3) 0.0894(18) Uani 1 1 d D . . C1 C 0.799(2) 0.4297(15) 0.6702(10) 0.075(6) Uani 1 1 d . . . C4 C 0.542(2) 0.5654(17) 0.5586(11) 0.086(6) Uani 1 1 d . . . H4 H 0.5690 0.6099 0.5964 0.103 Uiso 1 1 calc R . . C2 C 0.7135(19) 0.4507(15) 0.6217(11) 0.073(5) Uani 1 1 d . A . C5 C 0.5667(18) 0.4099(13) 0.5012(11) 0.067(5) Uani 1 1 d . . . H5 H 0.6116 0.3504 0.5013 0.080 Uiso 1 1 calc R . . C3 C 0.6022(18) 0.4777(16) 0.5591(9) 0.072(6) Uani 1 1 d . . . C9 C 1.030(2) 0.3658(18) 0.5586(9) 0.100(7) Uani 1 1 d D A . H9A H 0.9722 0.4223 0.5474 0.121 Uiso 1 1 calc R . . H9B H 1.1084 0.3666 0.5249 0.121 Uiso 1 1 calc R . . C10 C 0.943(3) 0.2798(18) 0.5422(16) 0.146(11) Uani 1 1 d D . . H10A H 0.9070 0.2809 0.4895 0.219 Uiso 1 1 calc R A . H10B H 0.8643 0.2789 0.5750 0.219 Uiso 1 1 calc R . . H10C H 1.0001 0.2236 0.5513 0.219 Uiso 1 1 calc R . . C6 C 1.243(3) 0.473(2) 0.663(2) 0.178(14) Uani 1 1 d D A . H6A H 1.3029 0.4701 0.7105 0.214 Uiso 1 1 calc R . . H6B H 1.3030 0.4659 0.6205 0.214 Uiso 1 1 calc R . . C21 C 1.176(3) 0.557(2) 0.659(2) 0.181(17) Uani 1 1 d . . . H21A H 1.2452 0.6080 0.6597 0.272 Uiso 1 1 calc R A . H21B H 1.1171 0.5643 0.7015 0.272 Uiso 1 1 calc R . . H21C H 1.1177 0.5603 0.6118 0.272 Uiso 1 1 calc R . . C16 C 0.663(9) 0.231(5) 0.850(5) 0.15(3) Uiso 0.504(19) 1 d PD A 1 H16A H 0.6512 0.1756 0.8822 0.226 Uiso 0.504(19) 1 calc PR A 1 H16B H 0.7229 0.2143 0.8094 0.226 Uiso 0.504(19) 1 calc PR A 1 H16C H 0.5715 0.2511 0.8287 0.226 Uiso 0.504(19) 1 calc PR A 1 C5T C 0.730(5) 0.310(2) 0.897(2) 0.096(14) Uiso 0.504(19) 1 d PD A 1 H5T1 H 0.8206 0.2877 0.9204 0.115 Uiso 0.504(19) 1 calc PR A 1 H5T2 H 0.6693 0.3257 0.9383 0.115 Uiso 0.504(19) 1 calc PR A 1 C4T C 0.886(6) 0.603(3) 0.892(3) 0.13(2) Uiso 0.504(19) 1 d PD A 1 H4T1 H 0.9145 0.6444 0.9336 0.202 Uiso 0.504(19) 1 calc PR A 1 H4T2 H 0.8163 0.6349 0.8581 0.202 Uiso 0.504(19) 1 calc PR A 1 H4T3 H 0.9676 0.5872 0.8634 0.202 Uiso 0.504(19) 1 calc PR A 1 C1T C 0.584(3) 0.473(4) 0.798(3) 0.115(17) Uiso 0.504(19) 1 d PD A 1 H1T1 H 0.5960 0.5308 0.7688 0.138 Uiso 0.504(19) 1 calc PR A 1 H1T2 H 0.5372 0.4250 0.7649 0.138 Uiso 0.504(19) 1 calc PR A 1 C3T C 0.823(6) 0.513(3) 0.922(2) 0.14(2) Uiso 0.504(19) 1 d PD A 1 H3T1 H 0.7410 0.5286 0.9509 0.164 Uiso 0.504(19) 1 calc PR A 1 H3T2 H 0.8927 0.4810 0.9564 0.164 Uiso 0.504(19) 1 calc PR A 1 C12A C 0.496(8) 0.493(6) 0.865(4) 0.23(4) Uiso 0.504(19) 1 d PD A 1 H12A H 0.4029 0.5145 0.8473 0.339 Uiso 0.504(19) 1 calc PR A 1 H12B H 0.5415 0.5411 0.8972 0.339 Uiso 0.504(19) 1 calc PR A 1 H12C H 0.4866 0.4351 0.8948 0.339 Uiso 0.504(19) 1 calc PR A 1 C7A C 1.188(5) 0.245(2) 0.675(3) 0.085(14) Uiso 0.504(19) 1 d PD A 1 H7A1 H 1.2232 0.2380 0.7278 0.102 Uiso 0.504(19) 1 calc PR A 1 H7A2 H 1.1135 0.1980 0.6650 0.102 Uiso 0.504(19) 1 calc PR A 1 C8A C 1.309(5) 0.221(4) 0.625(3) 0.123(19) Uiso 0.504(19) 1 d PD A 1 H8A1 H 1.3404 0.1566 0.6349 0.184 Uiso 0.504(19) 1 calc PR A 1 H8A2 H 1.3864 0.2646 0.6353 0.184 Uiso 0.504(19) 1 calc PR A 1 H8A3 H 1.2760 0.2265 0.5716 0.184 Uiso 0.504(19) 1 calc PR A 1 C11T C 0.669(5) 0.456(4) 0.987(3) 0.15(2) Uiso 0.496(19) 1 d PD A 2 H11A H 0.6890 0.4563 1.0415 0.225 Uiso 0.496(19) 1 calc PR A 2 H11B H 0.5940 0.4107 0.9742 0.225 Uiso 0.496(19) 1 calc PR A 2 H11C H 0.6384 0.5188 0.9704 0.225 Uiso 0.496(19) 1 calc PR A 2 C9T C 0.667(7) 0.546(3) 0.814(4) 0.16(3) Uiso 0.496(19) 1 d PD A 2 H9T1 H 0.6077 0.5361 0.7679 0.196 Uiso 0.496(19) 1 calc PR A 2 H9T2 H 0.6039 0.5591 0.8552 0.196 Uiso 0.496(19) 1 calc PR A 2 C8T C 0.800(5) 0.428(4) 0.9476(11) 0.118(17) Uiso 0.496(19) 1 d PD A 2 H8T1 H 0.8312 0.3655 0.9652 0.142 Uiso 0.496(19) 1 calc PR A 2 H8T2 H 0.8753 0.4738 0.9610 0.142 Uiso 0.496(19) 1 calc PR A 2 C10T C 0.631(11) 0.249(4) 0.829(6) 0.19(5) Uiso 0.496(19) 1 d PD A 2 H10D H 0.5478 0.2096 0.8177 0.280 Uiso 0.496(19) 1 calc PR A 2 H10E H 0.6637 0.2402 0.8813 0.280 Uiso 0.496(19) 1 calc PR A 2 H10F H 0.7044 0.2299 0.7959 0.280 Uiso 0.496(19) 1 calc PR A 2 C6T C 0.594(4) 0.351(4) 0.815(3) 0.14(2) Uiso 0.496(19) 1 d PD A 2 H6T1 H 0.5180 0.3709 0.8468 0.163 Uiso 0.496(19) 1 calc PR A 2 H6T2 H 0.5610 0.3610 0.7614 0.163 Uiso 0.496(19) 1 calc PR A 2 C12B C 0.751(11) 0.636(7) 0.803(6) 0.43(10) Uiso 0.496(19) 1 d PD A 2 H12D H 0.6875 0.6875 0.7897 0.648 Uiso 0.496(19) 1 calc PR A 2 H12E H 0.8147 0.6259 0.7627 0.648 Uiso 0.496(19) 1 calc PR A 2 H12F H 0.8058 0.6511 0.8498 0.648 Uiso 0.496(19) 1 calc PR A 2 C8B C 1.349(8) 0.282(7) 0.616(4) 0.23(4) Uiso 0.496(19) 1 d PD A 2 H8B1 H 1.4208 0.2334 0.6224 0.352 Uiso 0.496(19) 1 calc PR A 2 H8B2 H 1.3927 0.3440 0.6173 0.352 Uiso 0.496(19) 1 calc PR A 2 H8B3 H 1.2969 0.2732 0.5672 0.352 Uiso 0.496(19) 1 calc PR A 2 C7B C 1.248(5) 0.274(3) 0.679(3) 0.103(18) Uiso 0.496(19) 1 d PD A 2 H7B1 H 1.2989 0.2838 0.7286 0.124 Uiso 0.496(19) 1 calc PR A 2 H7B2 H 1.2039 0.2115 0.6788 0.124 Uiso 0.496(19) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0685(5) 0.0831(6) 0.0495(4) 0.0099(4) -0.0048(3) 0.0026(4) I1 0.1129(13) 0.1716(17) 0.0708(10) 0.0178(10) -0.0252(9) 0.0397(12) P1 0.080(4) 0.107(5) 0.060(3) 0.000(3) 0.005(3) -0.004(3) P2 0.081(4) 0.122(5) 0.066(3) 0.004(3) 0.011(3) 0.006(3) C1 0.078(14) 0.092(14) 0.055(11) 0.003(10) -0.015(10) 0.004(11) C4 0.078(14) 0.111(17) 0.068(13) 0.008(12) -0.001(11) 0.026(13) C2 0.048(11) 0.101(15) 0.073(13) -0.001(11) 0.017(10) 0.010(11) C5 0.046(10) 0.080(13) 0.075(12) -0.008(11) 0.001(9) 0.013(9) C3 0.058(12) 0.113(17) 0.044(10) 0.014(11) -0.004(9) 0.025(11) C9 0.079(15) 0.14(2) 0.077(14) 0.007(14) -0.004(11) -0.019(14) C10 0.14(3) 0.16(3) 0.13(2) -0.06(2) -0.026(19) 0.02(2) C6 0.18(4) 0.18(4) 0.18(3) 0.01(3) 0.06(3) 0.00(3) C21 0.14(3) 0.13(3) 0.28(5) 0.04(3) 0.10(3) 0.01(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 1.954(19) . ? Pt1 P2 2.320(6) . ? Pt1 P1 2.321(6) . ? Pt1 I1 2.6704(19) . ? P1 C9 1.899(15) . ? P1 C6 1.916(18) . ? P1 C7B 1.928(19) . ? P1 C7A 1.949(18) . ? P2 C8T 1.905(19) . ? P2 C1T 1.913(19) . ? P2 C3T 1.937(19) . ? P2 C9T 1.94(2) . ? P2 C6T 1.939(19) . ? P2 C5T 1.948(18) . ? C1 C2 1.17(2) . ? C4 C3 1.35(3) . ? C4 C5 1.46(3) 3_666 ? C2 C3 1.51(2) . ? C5 C3 1.41(2) . ? C5 C4 1.46(3) 3_666 ? C9 C10 1.471(16) . ? C6 C21 1.33(4) . ? C16 C5T 1.498(10) . ? C4T C3T 1.503(18) . ? C1T C12A 1.50(2) . ? C7A C8A 1.506(17) . ? C11T C8T 1.50(2) . ? C9T C12B 1.495(18) . ? C10T C6T 1.49(2) . ? C8B C7B 1.50(2) . ? 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 Pt1 P2 88.1(6) . . ? C1 Pt1 P1 88.5(6) . . ? P2 Pt1 P1 175.9(2) . . ? C1 Pt1 I1 179.7(6) . . ? P2 Pt1 I1 92.22(16) . . ? P1 Pt1 I1 91.22(15) . . ? C9 P1 C6 105.0(13) . . ? C9 P1 C7B 109.3(17) . . ? C6 P1 C7B 93(2) . . ? C9 P1 C7A 100.9(17) . . ? C6 P1 C7A 113.6(19) . . ? C7B P1 C7A 21(2) . . ? C9 P1 Pt1 115.6(8) . . ? C6 P1 Pt1 112.0(11) . . ? C7B P1 Pt1 118.9(16) . . ? C7A P1 Pt1 109.4(12) . . ? C8T P2 C1T 118(2) . . ? C8T P2 C3T 38.9(19) . . ? C1T P2 C3T 106(2) . . ? C8T P2 C9T 105(3) . . ? C1T P2 C9T 40(2) . . ? C3T P2 C9T 75(3) . . ? C8T P2 C6T 109(2) . . ? C1T P2 C6T 53(2) . . ? C3T P2 C6T 134(2) . . ? C9T P2 C6T 93(3) . . ? C8T P2 C5T 61(2) . . ? C1T P2 C5T 108(2) . . ? C3T P2 C5T 100.2(19) . . ? C9T P2 C5T 138(3) . . ? C6T P2 C5T 61(2) . . ? C8T P2 Pt1 123.7(15) . . ? C1T P2 Pt1 117.8(15) . . ? C3T P2 Pt1 114.8(16) . . ? C9T P2 Pt1 111(2) . . ? C6T P2 Pt1 111.1(18) . . ? C5T P2 Pt1 108.7(13) . . ? C2 C1 Pt1 178.6(19) . . ? C3 C4 C5 119.7(19) . 3_666 ? C1 C2 C3 180(2) . . ? C3 C5 C4 118.7(16) . 3_666 ? C4 C3 C5 121.5(17) . . ? C4 C3 C2 120.2(19) . . ? C5 C3 C2 118.3(18) . . ? C10 C9 P1 113.2(16) . . ? C21 C6 P1 109(3) . . ? C16 C5T P2 114(4) . . ? C12A C1T P2 107(4) . . ? C4T C3T P2 111(3) . . ? C8A C7A P1 117(3) . . ? C12B C9T P2 120(6) . . ? C11T C8T P2 111(3) . . ? C10T C6T P2 107(4) . . ? C8B C7B P1 107(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.622 _refine_diff_density_min -0.974 _refine_diff_density_rms 0.216 data_complex2b _database_code_depnum_ccdc_archive 'CCDC 895739' #TrackingRef 'Complex 2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C108 H152 N4 P8 Pt4' _chemical_formula_sum 'C108 H152 N4 P8 Pt4' _chemical_formula_weight 2534.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0036 0.0018 '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 0.0071 0.0037 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1123 0.1055 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -2.1406 9.1612 '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)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.950(4) _cell_length_b 9.6820(19) _cell_length_c 37.661(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.19(3) _cell_angle_gamma 90.00 _cell_volume 6398(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 111462 _cell_measurement_theta_min 1.24 _cell_measurement_theta_max 32.40 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 4.982 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4070 _exptl_absorpt_correction_T_max 0.7218 _exptl_absorpt_process_details 'HKL2000 Scalepack' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.75000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'PLSII 2D bending magnet' _diffrn_radiation_monochromator 'Si(111) double crystal monochromator' _diffrn_measurement_device_type 'ADSC Q210 CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36378 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10239 _reflns_number_gt 7524 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PAL ADSC Quantum-210 ADX Program' _computing_cell_refinement HKL3000 _computing_data_reduction HKL3000 _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Diamond 3' _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The geometry restraints and displacement parameter restraints such as DFIX ,DANG, ISOR, SIMU, DELU, EXYZ, EADP for serveral atoms around terminal PEt3 residues. ; _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^)+(0.1151P)^2^+2.2135P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0006(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10239 _refine_ls_number_parameters 635 _refine_ls_number_restraints 357 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1834 _refine_ls_wR_factor_gt 0.1748 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 2.882 _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 Pt1 Pt 0.37496(6) 1.12879(10) 0.08977(3) 0.0655(5) Uani 1 1 d . . . P1 P 0.3783(5) 1.2883(8) 0.0455(2) 0.084(2) Uani 1 1 d D B . C1P C 0.4136(19) 1.459(2) 0.0613(8) 0.090(9) Uani 1 1 d D . . H1P1 H 0.3787 1.4986 0.0758 0.108 Uiso 1 1 calc R . . H1P2 H 0.4640 1.4479 0.0778 0.108 Uiso 1 1 calc R . . C2P C 0.422(2) 1.563(3) 0.0322(9) 0.112(12) Uani 1 1 d D . . H2P1 H 0.4622 1.5326 0.0200 0.167 Uiso 1 1 calc R . . H2P2 H 0.4351 1.6535 0.0434 0.167 Uiso 1 1 calc R . . H2P3 H 0.3736 1.5699 0.0144 0.167 Uiso 1 1 calc R . . C3P C 0.2798(18) 1.329(5) 0.0184(9) 0.120(12) Uani 1 1 d DU . . H3P1 H 0.2809 1.3341 -0.0077 0.144 Uiso 1 1 calc R A 1 H3P2 H 0.2443 1.2544 0.0218 0.144 Uiso 1 1 calc R A 1 C4P C 0.251(16) 1.47(3) 0.031(11) 0.13(4) Uani 0.08 1 d PDU B 1 H4P1 H 0.2579 1.5399 0.0135 0.200 Uiso 0.08 1 calc PR B 1 H4P2 H 0.2807 1.4906 0.0549 0.200 Uiso 0.08 1 calc PR B 1 H4P3 H 0.1973 1.4591 0.0314 0.200 Uiso 0.08 1 calc PR B 1 C54P C 0.225(2) 1.361(5) 0.0437(13) 0.132(14) Uani 0.92 1 d PDU B 2 H54A H 0.2444 1.4404 0.0592 0.198 Uiso 0.92 1 calc PR B 2 H54B H 0.2211 1.2808 0.0589 0.198 Uiso 0.92 1 calc PR B 2 H54C H 0.1745 1.3839 0.0290 0.198 Uiso 0.92 1 calc PR B 2 C5P C 0.4262(18) 1.232(4) 0.0124(9) 0.108(11) Uani 1 1 d DU . . H5P1 H 0.3989 1.1516 -0.0004 0.129 Uiso 1 1 calc R B . H5P2 H 0.4254 1.3067 -0.0056 0.129 Uiso 1 1 calc R . . C6P C 0.5092(17) 1.191(4) 0.0283(12) 0.124(14) Uani 1 1 d D B . H6P1 H 0.5357 1.2687 0.0424 0.185 Uiso 1 1 calc R . . H6P2 H 0.5348 1.1687 0.0085 0.185 Uiso 1 1 calc R . . H6P3 H 0.5103 1.1108 0.0441 0.185 Uiso 1 1 calc R . . P2 P 0.3519(6) 0.9577(8) 0.1277(2) 0.097(3) Uani 1 1 d D D . C7P C 0.2466(18) 0.938(4) 0.1249(13) 0.133(13) Uani 1 1 d DU . . H7P1 H 0.2217 0.9062 0.1003 0.159 Uiso 1 1 calc R C 1 H7P2 H 0.2378 0.8683 0.1427 0.159 Uiso 1 1 calc R C 1 C8P C 0.211(3) 1.076(5) 0.133(2) 0.14(2) Uani 0.79(8) 1 d PDU D 1 H8P1 H 0.2217 1.1467 0.1158 0.206 Uiso 0.79(8) 1 calc PR D 1 H8P2 H 0.2333 1.1051 0.1578 0.206 Uiso 0.79(8) 1 calc PR D 1 H8P3 H 0.1560 1.0651 0.1299 0.206 Uiso 0.79(8) 1 calc PR D 1 C58P C 0.201(7) 1.058(12) 0.103(2) 0.15(4) Uani 0.21(8) 1 d PDU D 2 H58A H 0.1484 1.0566 0.1071 0.227 Uiso 0.21(8) 1 calc PR D 2 H58B H 0.2001 1.0467 0.0774 0.227 Uiso 0.21(8) 1 calc PR D 2 H58C H 0.2247 1.1463 0.1117 0.227 Uiso 0.21(8) 1 calc PR D 2 C9P C 0.380(2) 0.784(4) 0.1155(13) 0.137(15) Uani 1 1 d DU . . H9P1 H 0.3665 0.7134 0.1321 0.164 Uiso 1 1 calc R D . H9P2 H 0.3544 0.7601 0.0902 0.164 Uiso 1 1 calc R . . C10P C 0.467(2) 0.794(4) 0.1194(11) 0.144(17) Uani 1 1 d D D . H10A H 0.4787 0.8656 0.1029 0.216 Uiso 1 1 calc R . . H10B H 0.4869 0.7051 0.1132 0.216 Uiso 1 1 calc R . . H10C H 0.4908 0.8183 0.1445 0.216 Uiso 1 1 calc R . . C11P C 0.387(3) 0.989(3) 0.1763(7) 0.117(13) Uani 1 1 d D . . H11A H 0.4411 1.0154 0.1805 0.140 Uiso 1 1 calc R D . H11B H 0.3585 1.0683 0.1836 0.140 Uiso 1 1 calc R . . C12P C 0.379(3) 0.865(4) 0.2014(11) 0.143(15) Uani 1 1 d DU D . H12A H 0.4103 0.7882 0.1960 0.214 Uiso 1 1 calc R . . H12B H 0.3256 0.8364 0.1973 0.214 Uiso 1 1 calc R . . H12C H 0.3964 0.8930 0.2269 0.214 Uiso 1 1 calc R . . Pt2 Pt 0.94433(6) 0.69965(9) 0.12577(2) 0.0616(5) Uani 1 1 d . E . P3 P 0.9403(8) 0.8501(11) 0.0784(3) 0.132(5) Uani 1 1 d D . . C13P C 0.999(2) 1.000(4) 0.0860(12) 0.130(12) Uani 0.34(6) 1 d PDU E 1 H13A H 1.0376 0.9932 0.1088 0.156 Uiso 0.34(6) 1 calc PR E 1 H13B H 1.0237 1.0183 0.0655 0.156 Uiso 0.34(6) 1 calc PR E 1 C14P C 0.935(6) 1.113(8) 0.089(4) 0.14(2) Uani 0.34(6) 1 d PDU E 1 H14A H 0.8858 1.0810 0.0750 0.211 Uiso 0.34(6) 1 calc PR E 1 H14B H 0.9488 1.2001 0.0785 0.211 Uiso 0.34(6) 1 calc PR E 1 H14C H 0.9330 1.1261 0.1142 0.211 Uiso 0.34(6) 1 calc PR E 1 C63P C 0.999(2) 1.000(4) 0.0860(12) 0.130(12) Uani 0.66(6) 1 d PU E 2 H63A H 0.9863 1.0483 0.1072 0.156 Uiso 0.66(6) 1 calc PR E 2 H63B H 1.0520 0.9678 0.0934 0.156 Uiso 0.66(6) 1 calc PR E 2 C64P C 0.997(4) 1.101(7) 0.0580(18) 0.133(18) Uani 0.66(6) 1 d PU E 2 H64A H 1.0221 1.0645 0.0394 0.199 Uiso 0.66(6) 1 calc PR E 2 H64B H 1.0232 1.1850 0.0686 0.199 Uiso 0.66(6) 1 calc PR E 2 H64C H 0.9437 1.1238 0.0470 0.199 Uiso 0.66(6) 1 calc PR E 2 C15P C 0.841(3) 0.923(11) 0.065(3) 0.22(4) Uani 0.59(11) 1 d PDU E 1 H15A H 0.8419 1.0187 0.0748 0.266 Uiso 0.59(11) 1 calc PR E 1 H15B H 0.8271 0.9296 0.0384 0.266 Uiso 0.59(11) 1 calc PR E 1 C16P C 0.777(4) 0.847(11) 0.078(3) 0.21(4) Uani 0.59(11) 1 d PDU E 1 H16A H 0.7304 0.8528 0.0585 0.308 Uiso 0.59(11) 1 calc PR E 1 H16B H 0.7678 0.8896 0.0999 0.308 Uiso 0.59(11) 1 calc PR E 1 H16C H 0.7913 0.7503 0.0821 0.308 Uiso 0.59(11) 1 calc PR E 1 C65P C 0.856(4) 0.971(9) 0.085(3) 0.12(3) Uani 0.41(11) 1 d PDU E 2 H65A H 0.8714 1.0140 0.1090 0.143 Uiso 0.41(11) 1 calc PR E 2 H65B H 0.8527 1.0461 0.0667 0.143 Uiso 0.41(11) 1 calc PR E 2 C66P C 0.768(6) 0.913(17) 0.082(4) 0.14(3) Uani 0.41(11) 1 d PDU E 2 H66A H 0.7334 0.9910 0.0806 0.214 Uiso 0.41(11) 1 calc PR E 2 H66B H 0.7664 0.8563 0.1031 0.214 Uiso 0.41(11) 1 calc PR E 2 H66C H 0.7536 0.8566 0.0597 0.214 Uiso 0.41(11) 1 calc PR E 2 C17P C 0.939(4) 0.779(7) 0.0333(14) 0.24(2) Uani 0.50(10) 1 d PDU E 1 H17A H 0.8882 0.7408 0.0231 0.294 Uiso 0.50(10) 1 calc PR E 1 H17B H 0.9492 0.8543 0.0171 0.294 Uiso 0.50(10) 1 calc PR E 1 C18P C 1.001(6) 0.662(10) 0.034(3) 0.22(3) Uani 0.50(10) 1 d PDU E 1 H18A H 0.9753 0.5718 0.0309 0.331 Uiso 0.50(10) 1 calc PR E 1 H18B H 1.0376 0.6644 0.0571 0.331 Uiso 0.50(10) 1 calc PR E 1 H18C H 1.0271 0.6769 0.0139 0.331 Uiso 0.50(10) 1 calc PR E 1 C67P C 0.939(4) 0.779(7) 0.0333(14) 0.24(2) Uani 0.50(10) 1 d PDU E 2 H67A H 0.9120 0.6897 0.0292 0.294 Uiso 0.50(10) 1 calc PR E 2 H67B H 0.9182 0.8445 0.0136 0.294 Uiso 0.50(10) 1 calc PR E 2 C68P C 1.029(5) 0.761(16) 0.038(3) 0.23(3) Uani 0.50(10) 1 d PDU E 2 H68A H 1.0484 0.7046 0.0600 0.347 Uiso 0.50(10) 1 calc PR E 2 H68B H 1.0535 0.8518 0.0413 0.347 Uiso 0.50(10) 1 calc PR E 2 H68C H 1.0404 0.7149 0.0169 0.347 Uiso 0.50(10) 1 calc PR E 2 P4 P 0.9397(5) 0.5454(7) 0.1726(2) 0.087(2) Uani 1 1 d D . . C19P C 0.8506(17) 0.456(3) 0.1689(8) 0.102(9) Uani 1 1 d DU E . H19A H 0.8376 0.4095 0.1450 0.122 Uiso 1 1 calc R . . H19B H 0.8568 0.3831 0.1879 0.122 Uiso 1 1 calc R . . C20P C 0.785(2) 0.549(5) 0.1730(12) 0.137(13) Uani 1 1 d DU . . H20A H 0.7978 0.5978 0.1963 0.205 Uiso 1 1 calc R E . H20B H 0.7389 0.4935 0.1721 0.205 Uiso 1 1 calc R . . H20C H 0.7755 0.6168 0.1532 0.205 Uiso 1 1 calc R . . C21P C 1.014(2) 0.414(4) 0.1794(12) 0.136(13) Uani 1 1 d DU E . H21A H 1.0648 0.4587 0.1832 0.163 Uiso 1 1 calc R . . H21B H 1.0120 0.3588 0.2013 0.163 Uiso 1 1 calc R . . C22P C 1.003(3) 0.320(4) 0.1467(12) 0.136(13) Uani 1 1 d DU . . H22A H 0.9574 0.2641 0.1454 0.204 Uiso 1 1 calc R E . H22B H 1.0477 0.2593 0.1488 0.204 Uiso 1 1 calc R . . H22C H 0.9980 0.3760 0.1246 0.204 Uiso 1 1 calc R . . C23P C 0.960(2) 0.626(4) 0.2195(9) 0.125(12) Uani 1 1 d DU E . H23A H 1.0155 0.6450 0.2266 0.150 Uiso 1 1 calc R . . H23B H 0.9333 0.7155 0.2181 0.150 Uiso 1 1 calc R . . C24P C 0.937(3) 0.540(5) 0.2500(11) 0.137(13) Uani 1 1 d DU . . H24A H 0.8821 0.5467 0.2482 0.206 Uiso 1 1 calc R E . H24B H 0.9640 0.5745 0.2737 0.206 Uiso 1 1 calc R . . H24C H 0.9510 0.4426 0.2475 0.206 Uiso 1 1 calc R . . N1 N 0.4138(12) 1.267(2) 0.1327(5) 0.064(5) Uani 1 1 d . . . C1 C 0.3644(16) 1.353(3) 0.1424(7) 0.071(7) Uani 1 1 d . . . H1 H 0.3130 1.3482 0.1295 0.085 Uiso 1 1 calc R . . C2 C 0.3822(15) 1.446(3) 0.1696(7) 0.068(6) Uani 1 1 d . . . H2 H 0.3451 1.5086 0.1748 0.082 Uiso 1 1 calc R . . C3 C 0.4575(14) 1.447(2) 0.1900(7) 0.065(6) Uani 1 1 d . . . H3 H 0.4721 1.5085 0.2099 0.078 Uiso 1 1 calc R . . C4 C 0.5103(13) 1.357(2) 0.1806(6) 0.059(6) Uani 1 1 d . . . C5 C 0.4856(14) 1.267(2) 0.1501(6) 0.062(6) Uani 1 1 d . . . H5 H 0.5212 1.2079 0.1423 0.074 Uiso 1 1 calc R . . N2 N 1.0033(12) 0.8412(19) 0.1627(5) 0.057(5) Uani 1 1 d . . . C6 C 1.0796(15) 0.839(3) 0.1728(7) 0.069(6) Uani 1 1 d . E . H6 H 1.1077 0.7762 0.1615 0.083 Uiso 1 1 calc R . . C7 C 1.1185(17) 0.928(3) 0.1995(7) 0.081(8) Uani 1 1 d . . . H7 H 1.1726 0.9267 0.2059 0.097 Uiso 1 1 calc R E . C8 C 1.0772(15) 1.017(3) 0.2168(7) 0.071(7) Uani 1 1 d . E . H8 H 1.1028 1.0771 0.2354 0.085 Uiso 1 1 calc R . . C9 C 0.9983(13) 1.018(2) 0.2067(6) 0.051(5) Uani 1 1 d . . . C10 C 0.9635(13) 0.929(2) 0.1791(6) 0.054(5) Uani 1 1 d . E . H10 H 0.9096 0.9295 0.1717 0.065 Uiso 1 1 calc R . . C11 C 0.5860(14) 1.348(2) 0.2015(6) 0.056(5) Uani 1 1 d . . . C12 C 0.6460(15) 1.342(3) 0.2210(6) 0.060(6) Uani 1 1 d . . . C13 C 0.7776(13) 1.252(2) 0.2303(6) 0.059(6) Uani 1 1 d . . . H13 H 0.7662 1.2166 0.2063 0.071 Uiso 1 1 calc R . . C14 C 0.7223(14) 1.326(2) 0.2435(6) 0.059(6) Uani 1 1 d . . . C15 C 0.7403(15) 1.379(2) 0.2792(7) 0.070(7) Uani 1 1 d . . . H15 H 0.7032 1.4299 0.2885 0.084 Uiso 1 1 calc R . . C16 C 0.8107(16) 1.358(3) 0.3004(7) 0.084(8) Uani 1 1 d . . . H16 H 0.8226 1.3946 0.3243 0.101 Uiso 1 1 calc R . . C17 C 0.8651(16) 1.283(3) 0.2878(7) 0.081(8) Uani 1 1 d . . . H17 H 0.9134 1.2666 0.3032 0.098 Uiso 1 1 calc R . . C18 C 0.8495(15) 1.231(3) 0.2524(7) 0.068(7) Uani 1 1 d . E . C19 C 0.9062(15) 1.159(3) 0.2379(6) 0.062(6) Uani 1 1 d . . . C20 C 0.9507(14) 1.102(2) 0.2238(6) 0.059(6) Uani 1 1 d . E . C21 C 0.8880(17) 0.562(3) 0.0908(7) 0.076(7) Uani 1 1 d . . . C22 C 0.8541(16) 0.480(2) 0.0707(7) 0.067(7) Uani 1 1 d . E . C23 C 0.8146(15) 0.378(2) 0.0466(7) 0.064(6) Uani 1 1 d . . . C24 C 0.7567(17) 0.303(3) 0.0551(8) 0.078(7) Uani 1 1 d . E . H24 H 0.7432 0.3168 0.0779 0.093 Uiso 1 1 calc R . . C25 C 0.7166(16) 0.205(3) 0.0306(9) 0.082(8) Uani 1 1 d . . . H25 H 0.6749 0.1566 0.0365 0.099 Uiso 1 1 calc R E . C26 C 0.7378(15) 0.179(3) -0.0022(7) 0.068(7) Uani 1 1 d . E . C27 C 0.795(2) 0.254(3) -0.0105(8) 0.094(10) Uani 1 1 d . . . H27 H 0.8098 0.2386 -0.0330 0.113 Uiso 1 1 calc R E . C28 C 0.834(2) 0.353(4) 0.0133(9) 0.100(11) Uani 1 1 d . E . H28 H 0.8742 0.4046 0.0066 0.120 Uiso 1 1 calc R . . C29 C 0.6976(15) 0.082(3) -0.0281(7) 0.072(7) Uani 1 1 d . . . C30 C 0.6670(16) 0.001(3) -0.0508(8) 0.080(8) 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 0.0727(7) 0.0541(7) 0.0594(7) -0.0019(4) -0.0099(5) -0.0102(5) P1 0.109(6) 0.065(4) 0.067(4) 0.006(3) -0.009(4) 0.001(4) C1P 0.11(2) 0.062(16) 0.081(19) 0.009(14) -0.012(17) 0.002(16) C2P 0.17(3) 0.07(2) 0.10(2) 0.026(18) 0.03(2) 0.00(2) C3P 0.11(3) 0.16(3) 0.08(2) 0.00(2) -0.011(16) 0.02(2) C4P 0.13(4) 0.13(4) 0.13(4) 0.000(3) 0.028(8) 0.000(3) C54P 0.132(14) 0.132(14) 0.132(14) 0.000(3) 0.028(4) 0.000(3) C5P 0.12(2) 0.100(18) 0.101(19) 0.006(16) 0.015(16) 0.009(17) C6P 0.08(2) 0.15(4) 0.14(3) 0.06(3) 0.02(2) 0.01(2) P2 0.141(8) 0.066(4) 0.082(5) -0.006(4) 0.021(5) -0.035(5) C7P 0.12(3) 0.11(2) 0.16(4) -0.01(2) 0.02(2) -0.04(2) C8P 0.14(2) 0.14(2) 0.14(2) 0.000(3) 0.029(5) 0.000(3) C58P 0.15(4) 0.15(4) 0.15(4) 0.000(3) 0.032(8) 0.000(3) C9P 0.137(15) 0.136(15) 0.137(15) 0.000(3) 0.029(4) 0.000(3) C10P 0.20(5) 0.09(3) 0.12(3) -0.02(2) -0.03(3) 0.04(3) C11P 0.19(4) 0.09(2) 0.067(19) 0.005(17) 0.02(2) -0.06(2) C12P 0.143(16) 0.143(16) 0.142(16) 0.000(3) 0.030(4) 0.000(3) Pt2 0.0815(8) 0.0456(6) 0.0525(6) -0.0015(4) 0.0026(5) -0.0049(4) P3 0.191(11) 0.105(7) 0.070(5) 0.038(5) -0.040(6) -0.072(7) C13P 0.131(12) 0.130(12) 0.130(12) 0.0001(19) 0.027(3) -0.0003(19) C14P 0.14(2) 0.14(2) 0.14(2) 0.000(3) 0.030(6) 0.000(3) C63P 0.131(12) 0.130(12) 0.130(12) 0.0001(19) 0.027(3) -0.0003(19) C64P 0.133(19) 0.133(19) 0.133(19) 0.000(3) 0.028(5) -0.013(3) C15P 0.22(4) 0.22(4) 0.22(4) 0.0001(19) 0.047(8) 0.0000(19) C16P 0.16(5) 0.14(7) 0.27(10) 0.06(7) -0.09(5) 0.02(5) C65P 0.12(3) 0.12(3) 0.12(3) 0.000(3) 0.025(7) 0.001(3) C66P 0.14(3) 0.14(3) 0.14(3) 0.000(3) 0.028(7) 0.000(3) C17P 0.27(2) 0.21(2) 0.24(2) 0.0001(19) 0.052(5) -0.1260(19) C18P 0.23(3) 0.22(3) 0.21(3) 0.000(3) 0.047(7) -0.123(3) C67P 0.27(2) 0.21(2) 0.24(2) 0.0001(19) 0.052(5) -0.1260(19) C68P 0.28(3) 0.18(3) 0.23(3) 0.000(3) 0.050(7) -0.051(3) P4 0.130(7) 0.055(4) 0.069(4) 0.005(3) 0.004(4) -0.016(4) C19P 0.15(3) 0.09(2) 0.063(17) 0.003(15) 0.012(18) -0.017(18) C20P 0.137(14) 0.137(14) 0.137(14) 0.000(3) 0.029(4) 0.000(3) C21P 0.136(13) 0.136(13) 0.136(13) 0.000(3) 0.029(4) 0.000(3) C22P 0.136(13) 0.136(13) 0.136(13) 0.000(3) 0.029(4) 0.000(3) C23P 0.126(12) 0.125(12) 0.125(12) 0.000(3) 0.027(4) 0.000(3) C24P 0.137(13) 0.137(13) 0.137(13) 0.000(3) 0.029(4) 0.000(3) N1 0.064(12) 0.063(12) 0.057(12) -0.003(10) -0.008(10) -0.006(11) C1 0.067(16) 0.072(16) 0.067(16) -0.001(14) -0.001(13) -0.010(14) C2 0.069(15) 0.053(14) 0.075(17) 0.000(12) -0.002(12) 0.003(12) C3 0.065(15) 0.052(13) 0.074(16) -0.007(12) 0.005(12) -0.008(12) C4 0.062(14) 0.057(13) 0.053(13) 0.003(11) 0.000(11) 0.003(12) C5 0.068(15) 0.057(13) 0.055(13) 0.004(11) 0.000(11) -0.015(12) N2 0.073(13) 0.042(9) 0.049(10) 0.007(8) 0.000(9) -0.005(10) C6 0.065(16) 0.072(15) 0.070(16) -0.007(13) 0.016(13) 0.008(14) C7 0.079(18) 0.088(19) 0.071(17) -0.022(15) 0.006(14) -0.001(16) C8 0.079(17) 0.072(16) 0.064(15) -0.013(13) 0.018(13) -0.006(14) C9 0.060(13) 0.047(11) 0.046(12) -0.005(9) 0.008(10) -0.007(11) C10 0.056(13) 0.049(12) 0.057(13) 0.012(10) 0.010(10) 0.008(11) C11 0.062(14) 0.050(12) 0.052(13) -0.005(10) 0.001(11) 0.001(11) C12 0.072(16) 0.060(13) 0.045(12) -0.003(11) 0.009(12) -0.002(12) C13 0.073(15) 0.053(12) 0.046(12) -0.004(10) -0.003(11) 0.018(12) C14 0.065(14) 0.056(12) 0.049(13) 0.004(10) -0.006(11) 0.007(12) C15 0.079(17) 0.066(15) 0.057(14) -0.015(12) -0.001(13) 0.015(13) C16 0.081(19) 0.11(2) 0.057(15) -0.014(15) 0.000(14) 0.005(17) C17 0.072(17) 0.11(2) 0.056(15) -0.017(15) 0.000(12) 0.032(16) C18 0.071(16) 0.072(15) 0.055(14) 0.003(12) 0.000(12) 0.022(14) C19 0.073(16) 0.062(14) 0.045(13) 0.006(11) 0.001(12) 0.011(13) C20 0.066(15) 0.055(13) 0.052(13) 0.005(11) 0.004(11) 0.002(12) C21 0.10(2) 0.064(16) 0.062(16) -0.007(13) 0.012(14) -0.015(15) C22 0.095(18) 0.043(12) 0.056(14) 0.001(11) -0.002(13) -0.010(13) C23 0.075(16) 0.047(13) 0.062(15) 0.011(11) 0.002(12) -0.013(12) C24 0.088(19) 0.067(17) 0.074(18) -0.008(13) 0.006(14) 0.004(15) C25 0.076(18) 0.072(18) 0.09(2) -0.011(15) 0.002(15) -0.018(14) C26 0.075(17) 0.050(13) 0.067(16) -0.004(12) -0.011(13) 0.001(13) C27 0.13(3) 0.10(2) 0.055(16) -0.026(15) 0.013(16) -0.05(2) C28 0.11(2) 0.12(3) 0.08(2) -0.032(18) 0.023(18) -0.05(2) C29 0.077(17) 0.050(13) 0.077(17) -0.006(13) -0.008(14) -0.006(13) C30 0.083(18) 0.071(17) 0.071(17) 0.002(14) -0.019(14) -0.007(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C30 1.96(3) 3_665 ? Pt1 N1 2.10(2) . ? Pt1 P2 2.281(8) . ? Pt1 P1 2.283(8) . ? P1 C5P 1.74(3) . ? P1 C1P 1.83(3) . ? P1 C3P 1.89(3) . ? C1P C2P 1.52(3) . ? C3P C4P 1.54(5) . ? C3P C54P 1.54(3) . ? C5P C6P 1.54(3) . ? P2 C11P 1.83(3) . ? P2 C9P 1.84(3) . ? P2 C7P 1.88(3) . ? C7P C8P 1.53(4) . ? C7P C58P 1.55(5) . ? C9P C10P 1.55(4) . ? C11P C12P 1.55(4) . ? Pt2 C21 1.99(3) . ? Pt2 N2 2.077(19) . ? Pt2 P3 2.291(8) . ? Pt2 P4 2.327(7) . ? P3 C13P 1.77(3) . ? P3 C17P 1.83(4) . ? P3 C15P 1.89(5) . ? P3 C65P 1.97(5) . ? C13P C14P 1.59(5) . ? C15P C16P 1.51(5) . ? C65P C66P 1.65(5) . ? C17P C18P 1.57(5) . ? P4 C19P 1.80(3) . ? P4 C21P 1.82(3) . ? P4 C23P 1.89(3) . ? C19P C20P 1.52(4) . ? C21P C22P 1.51(4) . ? C23P C24P 1.54(4) . ? N1 C5 1.32(3) . ? N1 C1 1.32(3) . ? C1 C2 1.35(4) . ? C2 C3 1.41(3) . ? C3 C4 1.39(3) . ? C4 C11 1.42(3) . ? C4 C5 1.43(3) . ? N2 C10 1.34(3) . ? N2 C6 1.34(3) . ? C6 C7 1.39(4) . ? C7 C8 1.39(4) . ? C8 C9 1.39(3) . ? C9 C10 1.40(3) . ? C9 C20 1.43(3) . ? C11 C12 1.17(3) . ? C12 C14 1.46(3) . ? C13 C18 1.39(3) . ? C13 C14 1.40(3) . ? C14 C15 1.41(3) . ? C15 C16 1.36(4) . ? C16 C17 1.38(4) . ? C17 C18 1.40(3) . ? C18 C19 1.43(4) . ? C19 C20 1.19(3) . ? C21 C22 1.18(3) . ? C22 C23 1.42(3) . ? C23 C24 1.36(4) . ? C23 C28 1.39(4) . ? C24 C25 1.41(4) . ? C25 C26 1.39(4) . ? C26 C27 1.35(4) . ? C26 C29 1.44(3) . ? C27 C28 1.39(4) . ? C29 C30 1.20(4) . ? C30 Pt1 1.96(3) 3_665 ? 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 C30 Pt1 N1 176.6(11) 3_665 . ? C30 Pt1 P2 85.0(9) 3_665 . ? N1 Pt1 P2 93.2(6) . . ? C30 Pt1 P1 87.2(9) 3_665 . ? N1 Pt1 P1 94.3(6) . . ? P2 Pt1 P1 170.0(3) . . ? C5P P1 C1P 109.1(18) . . ? C5P P1 C3P 103.1(16) . . ? C1P P1 C3P 101.9(17) . . ? C5P P1 Pt1 113.8(13) . . ? C1P P1 Pt1 115.8(9) . . ? C3P P1 Pt1 111.7(14) . . ? C2P C1P P1 116(2) . . ? C4P C3P C54P 49(10) . . ? C4P C3P P1 111(7) . . ? C54P C3P P1 111(2) . . ? C6P C5P P1 113(3) . . ? C11P P2 C9P 110(2) . . ? C11P P2 C7P 101(2) . . ? C9P P2 C7P 102.6(18) . . ? C11P P2 Pt1 116.0(10) . . ? C9P P2 Pt1 114.4(15) . . ? C7P P2 Pt1 110.5(14) . . ? C8P C7P C58P 42(2) . . ? C8P C7P P2 111(3) . . ? C58P C7P P2 112(6) . . ? C10P C9P P2 104(3) . . ? C12P C11P P2 115(2) . . ? C21 Pt2 N2 179.4(9) . . ? C21 Pt2 P3 89.0(8) . . ? N2 Pt2 P3 91.7(5) . . ? C21 Pt2 P4 88.8(8) . . ? N2 Pt2 P4 90.6(5) . . ? P3 Pt2 P4 176.2(4) . . ? C13P P3 C17P 110(2) . . ? C13P P3 C15P 103(3) . . ? C17P P3 C15P 94(4) . . ? C13P P3 C65P 86(3) . . ? C17P P3 C65P 119(4) . . ? C15P P3 C65P 26(4) . . ? C13P P3 Pt2 118.3(15) . . ? C17P P3 Pt2 118(2) . . ? C15P P3 Pt2 108(3) . . ? C65P P3 Pt2 100(3) . . ? C14P C13P P3 100(4) . . ? C16P C15P P3 118(6) . . ? C66P C65P P3 122(7) . . ? C18P C17P P3 113(5) . . ? C19P P4 C21P 106.7(18) . . ? C19P P4 C23P 105.3(16) . . ? C21P P4 C23P 99.5(19) . . ? C19P P4 Pt2 115.1(11) . . ? C21P P4 Pt2 114.3(15) . . ? C23P P4 Pt2 114.4(12) . . ? C20P C19P P4 114(2) . . ? C22P C21P P4 110(3) . . ? C24P C23P P4 116(3) . . ? C5 N1 C1 120(2) . . ? C5 N1 Pt1 120.9(18) . . ? C1 N1 Pt1 118.6(16) . . ? N1 C1 C2 124(2) . . ? C1 C2 C3 118(3) . . ? C4 C3 C2 119(2) . . ? C3 C4 C11 121(2) . . ? C3 C4 C5 118(2) . . ? C11 C4 C5 121(2) . . ? N1 C5 C4 120(2) . . ? C10 N2 C6 119(2) . . ? C10 N2 Pt2 118.7(16) . . ? C6 N2 Pt2 121.8(17) . . ? N2 C6 C7 122(2) . . ? C8 C7 C6 119(3) . . ? C9 C8 C7 120(2) . . ? C8 C9 C10 118(2) . . ? C8 C9 C20 124(2) . . ? C10 C9 C20 118(2) . . ? N2 C10 C9 123(2) . . ? C12 C11 C4 175(3) . . ? C11 C12 C14 175(3) . . ? C18 C13 C14 120(2) . . ? C13 C14 C15 119(2) . . ? C13 C14 C12 120(2) . . ? C15 C14 C12 121(2) . . ? C16 C15 C14 120(2) . . ? C15 C16 C17 121(3) . . ? C16 C17 C18 120(2) . . ? C13 C18 C17 119(2) . . ? C13 C18 C19 119(2) . . ? C17 C18 C19 121(2) . . ? C20 C19 C18 176(2) . . ? C19 C20 C9 173(3) . . ? C22 C21 Pt2 179(2) . . ? C21 C22 C23 179(3) . . ? C24 C23 C28 118(2) . . ? C24 C23 C22 121(2) . . ? C28 C23 C22 121(2) . . ? C23 C24 C25 121(3) . . ? C26 C25 C24 120(3) . . ? C27 C26 C25 118(2) . . ? C27 C26 C29 120(3) . . ? C25 C26 C29 122(3) . . ? C26 C27 C28 121(3) . . ? C23 C28 C27 121(3) . . ? C30 C29 C26 177(3) . . ? C29 C30 Pt1 175(3) . 3_665 ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 1.889 _refine_diff_density_min -2.086 _refine_diff_density_rms 0.137 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.130 0.012 0.013 9 2 ' ' 2 0.652 -0.056 0.109 155 46 ' ' 3 0.250 0.017 0.250 329 113 ' ' 4 0.848 -0.071 0.390 155 45 ' ' 5 0.152 0.020 0.609 155 45 ' ' 6 0.750 0.002 0.750 329 112 ' ' 7 0.348 0.012 0.890 155 43 ' ' 8 0.869 -0.012 0.987 9 2 ' ' 9 0.630 0.488 0.513 9 2 ' ' 10 0.369 0.512 0.487 9 2 ' ' _platon_squeeze_details ; ? ; #