# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dmitri Gelman' _publ_contact_author_email dgelman@chem.ch.huji.ac.il loop_ _publ_author_name 'Sanaa Mussa' 'Ronit Romm' 'Clarite Azerraf' 'Dmitri Gelman' data_klarit2m _database_code_depnum_ccdc_archive 'CCDC 808730' #TrackingRef 'Klarit21.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H41 Cl2 Ir P2' _chemical_formula_sum 'C32 H41 Cl2 Ir P2' _chemical_formula_weight 750.69 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 '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 _symmetry_space_group_name_Hall '-P 2ybc' 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 12.9018(11) _cell_length_b 11.8906(10) _cell_length_c 19.6359(17) _cell_angle_alpha 90.00 _cell_angle_beta 95.424(2) _cell_angle_gamma 90.00 _cell_volume 2998.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 4.758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4496 _exptl_absorpt_correction_T_max 0.7633 _exptl_absorpt_process_details 'Bruker SADABS V2.05' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 24891 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 28.00 _reflns_number_total 7029 _reflns_number_gt 5651 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0610P)^2^+1.0130P] 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 7029 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.055 _refine_ls_shift/su_mean 0.001 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 C1 C 0.7313(4) 0.5327(4) 0.1537(3) 0.0320(11) Uani 1 1 d . . . H1 H 0.782(4) 0.609(5) 0.153(3) 0.050(17) Uiso 1 1 d . . . C2 C 0.6247(5) 0.3501(5) 0.1442(3) 0.0443(15) Uani 1 1 d . . . H2 H 0.5827 0.2793 0.1402 0.053 Uiso 1 1 calc R . . C3 C 0.6150(4) 0.5549(4) 0.1354(3) 0.0308(11) Uani 1 1 d . . . C4 C 0.5673(4) 0.6603(4) 0.1224(3) 0.0340(12) Uani 1 1 d . . . C5 C 0.4590(5) 0.6583(5) 0.1017(3) 0.0433(14) Uani 1 1 d . . . H5 H 0.4235 0.7269 0.0907 0.052 Uiso 1 1 calc R . . C6 C 0.4049(5) 0.5593(5) 0.0972(3) 0.0504(16) Uani 1 1 d . . . H6 H 0.3322 0.5611 0.0840 0.061 Uiso 1 1 calc R . . C7 C 0.4519(5) 0.4580(5) 0.1110(3) 0.0474(15) Uani 1 1 d . . . H7 H 0.4125 0.3904 0.1080 0.057 Uiso 1 1 calc R . . C8 C 0.5585(4) 0.4557(4) 0.1297(3) 0.0371(13) Uani 1 1 d . . . C9 C 0.7431(4) 0.4632(4) 0.2205(3) 0.0297(11) Uani 1 1 d . . . C10 C 0.8063(4) 0.4872(4) 0.2811(3) 0.0331(12) Uani 1 1 d . . . C11 C 0.8092(4) 0.4064(5) 0.3325(3) 0.0404(13) Uani 1 1 d . . . H11 H 0.8539 0.4178 0.3732 0.048 Uiso 1 1 calc R . . C12 C 0.7497(5) 0.3110(5) 0.3263(3) 0.0449(14) Uani 1 1 d . . . H12 H 0.7525 0.2589 0.3632 0.054 Uiso 1 1 calc R . . C13 C 0.6856(5) 0.2892(5) 0.2674(3) 0.0395(13) Uani 1 1 d . . . H13 H 0.6440 0.2232 0.2634 0.047 Uiso 1 1 calc R . . C14 C 0.6835(4) 0.3650(4) 0.2148(3) 0.0351(12) Uani 1 1 d . . . C15 C 0.7648(5) 0.4532(5) 0.0983(3) 0.0413(14) Uani 1 1 d . . . C16 C 0.8428(5) 0.4704(6) 0.0571(3) 0.0523(17) Uani 1 1 d . . . H16 H 0.8813 0.5386 0.0599 0.063 Uiso 1 1 calc R . . C17 C 0.8652(6) 0.3873(8) 0.0113(4) 0.073(2) Uani 1 1 d . . . H17 H 0.9191 0.3988 -0.0177 0.087 Uiso 1 1 calc R . . C18 C 0.8101(8) 0.2888(8) 0.0077(4) 0.076(3) Uani 1 1 d . . . H18 H 0.8273 0.2317 -0.0232 0.091 Uiso 1 1 calc R . . C19 C 0.7296(7) 0.2713(6) 0.0485(4) 0.065(3) Uani 1 1 d . . . H19 H 0.6904 0.2036 0.0451 0.078 Uiso 1 1 calc R . . C20 C 0.7073(5) 0.3541(5) 0.0944(3) 0.0483(16) Uani 1 1 d . . . C21 C 0.6677(6) 0.8332(6) 0.0478(3) 0.0563(18) Uani 1 1 d . . . H21 H 0.5939 0.8503 0.0319 0.068 Uiso 0.50 1 d PR . . H21A H 0.7334 0.7997 0.0501 0.068 Uiso 0.50 1 d PR . . C22 C 0.7030(13) 0.7415(10) 0.0074(8) 0.058(4) Uani 0.50 1 d P . . H22A H 0.6545 0.6783 0.0083 0.086 Uiso 0.50 1 calc PR . . H22B H 0.7725 0.7176 0.0265 0.086 Uiso 0.50 1 calc PR . . H22C H 0.7060 0.7666 -0.0399 0.086 Uiso 0.50 1 calc PR . . C22A C 0.5972(13) 0.8042(14) -0.0094(7) 0.065(4) Uani 0.50 1 d P . . H22D H 0.6264 0.8268 -0.0516 0.098 Uiso 0.50 1 calc PR . . H22E H 0.5308 0.8431 -0.0062 0.098 Uiso 0.50 1 calc PR . . H22F H 0.5856 0.7228 -0.0099 0.098 Uiso 0.50 1 calc PR . . C23 C 0.7211(5) 0.9454(6) 0.0459(4) 0.0607(19) Uani 1 1 d . . . H23A H 0.7901 0.9408 0.0713 0.091 Uiso 1 1 calc R . . H23B H 0.6794 1.0025 0.0669 0.091 Uiso 1 1 calc R . . H23C H 0.7284 0.9662 -0.0017 0.091 Uiso 1 1 calc R . . C24 C 0.5493(5) 0.8968(5) 0.1658(4) 0.0488(16) Uani 1 1 d . . . H24 H 0.5054 0.8552 0.1968 0.059 Uiso 1 1 calc R . . C25 C 0.4743(5) 0.9538(6) 0.1123(4) 0.063(2) Uani 1 1 d . . . H25A H 0.4297 1.0061 0.1348 0.094 Uiso 1 1 calc R . . H25B H 0.4310 0.8968 0.0873 0.094 Uiso 1 1 calc R . . H25C H 0.5138 0.9954 0.0803 0.094 Uiso 1 1 calc R . . C26 C 0.6087(6) 0.9865(6) 0.2101(4) 0.064(2) Uani 1 1 d . . . H26A H 0.6506 1.0322 0.1814 0.097 Uiso 1 1 calc R . . H26B H 0.6546 0.9498 0.2460 0.097 Uiso 1 1 calc R . . H26C H 0.5590 1.0349 0.2310 0.097 Uiso 1 1 calc R . . C27 C 1.0131(4) 0.5820(5) 0.2820(3) 0.0487(16) Uani 1 1 d . . . H27 H 1.0349 0.5265 0.3189 0.058 Uiso 1 1 calc R . . C28 C 1.0242(5) 0.5249(6) 0.2134(4) 0.065(2) Uani 1 1 d . . . H28A H 1.0110 0.5799 0.1764 0.097 Uiso 1 1 calc R . . H28B H 0.9737 0.4633 0.2067 0.097 Uiso 1 1 calc R . . H28C H 1.0948 0.4949 0.2130 0.097 Uiso 1 1 calc R . . C29 C 1.0859(6) 0.6821(7) 0.2913(5) 0.076(2) Uani 1 1 d . . . H29A H 1.1580 0.6567 0.2901 0.114 Uiso 1 1 calc R . . H29B H 1.0782 0.7179 0.3355 0.114 Uiso 1 1 calc R . . H29C H 1.0687 0.7363 0.2544 0.114 Uiso 1 1 calc R . . C30 C 0.8738(5) 0.6588(6) 0.3829(3) 0.0510(16) Uani 1 1 d . . . H30 H 0.8046 0.6334 0.3960 0.061 Uiso 1 1 calc R . . C31 C 0.9566(6) 0.6028(7) 0.4339(4) 0.070(2) Uani 1 1 d . . . H31A H 1.0251 0.6352 0.4283 0.105 Uiso 1 1 calc R . . H31B H 0.9582 0.5217 0.4250 0.105 Uiso 1 1 calc R . . H31C H 0.9391 0.6158 0.4807 0.105 Uiso 1 1 calc R . . C32 C 0.8772(8) 0.7870(6) 0.3926(4) 0.078(3) Uani 1 1 d . . . H32A H 0.8710 0.8050 0.4407 0.116 Uiso 1 1 calc R . . H32B H 0.8195 0.8215 0.3639 0.116 Uiso 1 1 calc R . . H32C H 0.9434 0.8161 0.3792 0.116 Uiso 1 1 calc R . . Cl1 Cl 0.64365(12) 0.70197(13) 0.28565(8) 0.0444(3) Uani 1 1 d . . . Cl2 Cl 0.91207(13) 0.77926(14) 0.14324(9) 0.0543(4) Uani 1 1 d . . . Ir1 Ir 0.777830(16) 0.733421(18) 0.212773(11) 0.03369(9) Uani 1 1 d . . . H1IR H 0.820(5) 0.876(5) 0.246(3) 0.064(19) Uiso 1 1 d . . . P1 P 0.64138(12) 0.79137(11) 0.13461(8) 0.0339(3) Uani 1 1 d . . . P2 P 0.87752(11) 0.62127(12) 0.29138(7) 0.0358(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 C1 0.038(3) 0.027(3) 0.030(3) -0.001(2) -0.001(2) 0.001(2) C2 0.055(4) 0.025(3) 0.049(4) -0.004(2) -0.012(3) -0.002(2) C3 0.037(3) 0.031(3) 0.024(3) -0.001(2) -0.002(2) 0.001(2) C4 0.044(3) 0.027(3) 0.029(3) 0.000(2) -0.001(2) 0.001(2) C5 0.042(3) 0.042(3) 0.044(4) 0.004(3) -0.006(3) 0.003(3) C6 0.038(4) 0.056(4) 0.054(4) 0.006(3) -0.012(3) 0.002(3) C7 0.045(4) 0.046(3) 0.048(4) 0.001(3) -0.011(3) -0.011(3) C8 0.045(3) 0.029(3) 0.035(3) -0.002(2) -0.007(3) -0.003(2) C9 0.029(3) 0.027(2) 0.033(3) 0.002(2) 0.002(2) 0.002(2) C10 0.033(3) 0.036(3) 0.030(3) 0.005(2) 0.002(2) -0.003(2) C11 0.042(3) 0.048(3) 0.030(3) 0.005(3) -0.005(2) -0.007(3) C12 0.046(4) 0.045(3) 0.043(4) 0.012(3) -0.001(3) -0.007(3) C13 0.045(3) 0.031(3) 0.042(3) 0.009(2) 0.003(3) -0.006(2) C14 0.032(3) 0.032(3) 0.039(3) 0.000(2) -0.007(2) 0.001(2) C15 0.043(3) 0.046(3) 0.033(3) 0.001(3) -0.005(3) 0.013(3) C16 0.051(4) 0.060(4) 0.044(4) -0.002(3) -0.003(3) 0.021(3) C17 0.071(5) 0.113(7) 0.033(4) -0.015(4) -0.004(3) 0.041(5) C18 0.101(7) 0.088(6) 0.034(4) -0.021(4) -0.022(4) 0.053(5) C19 0.098(7) 0.044(4) 0.045(4) -0.012(3) -0.025(5) 0.030(4) C20 0.065(4) 0.038(3) 0.037(3) -0.007(3) -0.018(3) 0.015(3) C21 0.079(5) 0.051(4) 0.039(4) 0.012(3) 0.009(3) 0.000(3) C22 0.081(11) 0.052(8) 0.041(8) 0.002(6) 0.010(7) 0.004(7) C22A 0.081(11) 0.077(10) 0.035(8) 0.009(7) -0.006(7) -0.011(8) C23 0.075(5) 0.049(4) 0.061(5) 0.015(3) 0.019(4) 0.000(3) C24 0.056(4) 0.031(3) 0.060(4) 0.001(3) 0.010(3) 0.006(3) C25 0.055(4) 0.049(4) 0.085(6) 0.000(4) 0.008(4) 0.016(3) C26 0.082(5) 0.043(4) 0.071(5) -0.019(4) 0.018(4) 0.005(3) C27 0.033(3) 0.055(4) 0.056(4) 0.012(3) -0.007(3) -0.004(3) C28 0.042(4) 0.069(5) 0.084(6) 0.007(4) 0.007(4) 0.014(3) C29 0.044(4) 0.083(6) 0.098(7) 0.014(5) -0.005(4) -0.024(4) C30 0.055(4) 0.060(4) 0.036(3) -0.002(3) -0.008(3) -0.015(3) C31 0.087(6) 0.069(5) 0.048(4) 0.007(4) -0.023(4) -0.019(4) C32 0.118(7) 0.058(5) 0.053(5) -0.013(4) -0.014(5) -0.024(5) Cl1 0.0493(9) 0.0456(8) 0.0396(8) -0.0003(6) 0.0110(7) -0.0032(6) Cl2 0.0466(9) 0.0600(10) 0.0573(10) 0.0130(8) 0.0106(8) -0.0092(7) Ir1 0.03540(14) 0.03092(13) 0.03440(14) 0.00201(9) 0.00146(9) -0.00596(8) P1 0.0411(8) 0.0262(7) 0.0344(8) 0.0011(6) 0.0027(6) 0.0008(5) P2 0.0344(8) 0.0389(8) 0.0328(8) 0.0018(6) -0.0034(6) -0.0084(6) _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 C1 C15 1.533(8) . ? C1 C3 1.532(7) . ? C1 C9 1.545(7) . ? C1 H1 1.12(6) . ? C2 C20 1.514(9) . ? C2 C14 1.527(7) . ? C2 C8 1.530(7) . ? C2 H2 1.0000 . ? C3 C8 1.385(7) . ? C3 C4 1.409(7) . ? C4 C5 1.419(8) . ? C4 P1 1.832(5) . ? C5 C6 1.367(8) . ? C5 H5 0.9500 . ? C6 C7 1.364(8) . ? C6 H6 0.9500 . ? C7 C8 1.390(8) . ? C7 H7 0.9500 . ? C9 C14 1.397(7) . ? C9 C10 1.406(7) . ? C10 C11 1.393(7) . ? C10 P2 1.841(5) . ? C11 C12 1.368(8) . ? C11 H11 0.9500 . ? C12 C13 1.383(9) . ? C12 H12 0.9500 . ? C13 C14 1.368(8) . ? C13 H13 0.9500 . ? C15 C16 1.366(9) . ? C15 C20 1.390(9) . ? C16 C17 1.385(9) . ? C16 H16 0.9500 . ? C17 C18 1.368(12) . ? C17 H17 0.9500 . ? C18 C19 1.387(12) . ? C18 H18 0.9500 . ? C19 C20 1.382(9) . ? C19 H19 0.9500 . ? C21 C22A 1.420(15) . ? C21 C22 1.447(15) . ? C21 C23 1.504(9) . ? C21 P1 1.838(7) . ? C21 H21 0.9951 . ? C21 H21A 0.9338 . ? C22 H21A 1.1282 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C22A H21 0.9831 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.520(9) . ? C24 C26 1.535(9) . ? C24 P1 1.870(6) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.517(9) . ? C27 C28 1.528(10) . ? C27 P2 1.836(6) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C32 1.536(10) . ? C30 C31 1.545(9) . ? C30 P2 1.856(6) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? Cl1 Ir1 2.3776(15) . ? Cl2 Ir1 2.3681(16) . ? Ir1 P1 2.3279(15) . ? Ir1 P2 2.3324(15) . ? Ir1 H1 1.89(6) . ? Ir1 H1IR 1.88(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 C15 C1 C3 106.0(4) . . ? C15 C1 C9 105.1(4) . . ? C3 C1 C9 107.9(4) . . ? C15 C1 H1 107(3) . . ? C3 C1 H1 115(3) . . ? C9 C1 H1 115(3) . . ? C20 C2 C14 105.2(5) . . ? C20 C2 C8 105.6(5) . . ? C14 C2 C8 107.1(4) . . ? C20 C2 H2 112.8 . . ? C14 C2 H2 112.8 . . ? C8 C2 H2 112.8 . . ? C8 C3 C4 121.6(5) . . ? C8 C3 C1 111.6(4) . . ? C4 C3 C1 126.7(5) . . ? C3 C4 C5 116.0(5) . . ? C3 C4 P1 121.3(4) . . ? C5 C4 P1 122.6(4) . . ? C6 C5 C4 121.1(5) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C7 C6 C5 122.2(6) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C6 C7 C8 118.7(5) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? C3 C8 C7 120.3(5) . . ? C3 C8 C2 113.8(5) . . ? C7 C8 C2 125.9(5) . . ? C14 C9 C10 120.6(5) . . ? C14 C9 C1 111.7(4) . . ? C10 C9 C1 127.7(4) . . ? C11 C10 C9 116.5(5) . . ? C11 C10 P2 122.6(4) . . ? C9 C10 P2 120.9(4) . . ? C12 C11 C10 122.1(5) . . ? C12 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C11 C12 C13 121.0(5) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C14 C13 C12 118.4(5) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C9 121.2(5) . . ? C13 C14 C2 125.6(5) . . ? C9 C14 C2 113.1(5) . . ? C16 C15 C20 120.9(6) . . ? C16 C15 C1 126.9(6) . . ? C20 C15 C1 112.2(6) . . ? C15 C16 C17 119.3(8) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 120.3(8) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 120.8(7) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C18 C19 C20 118.9(8) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? C19 C20 C15 119.8(7) . . ? C19 C20 C2 126.9(7) . . ? C15 C20 C2 113.3(5) . . ? C22A C21 C22 66.1(10) . . ? C22A C21 C23 117.2(8) . . ? C22 C21 C23 119.1(9) . . ? C22A C21 P1 120.5(8) . . ? C22 C21 P1 113.6(7) . . ? C23 C21 P1 112.9(5) . . ? C22A C21 H21 43.8 . . ? C22 C21 H21 108.9 . . ? C23 C21 H21 103.8 . . ? P1 C21 H21 95.2 . . ? C22A C21 H21A 116.5 . . ? C22 C21 H21A 51.2 . . ? C23 C21 H21A 88.0 . . ? P1 C21 H21A 94.9 . . ? H21 C21 H21A 160.0 . . ? C21 C22 H21A 40.2 . . ? C21 C22 H22A 109.5 . . ? H21A C22 H22A 129.4 . . ? C21 C22 H22B 109.5 . . ? H21A C22 H22B 69.7 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H21A C22 H22C 118.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C22A H21 44.5 . . ? C21 C22A H22D 109.5 . . ? H21 C22A H22D 126.5 . . ? C21 C22A H22E 109.5 . . ? H21 C22A H22E 65.0 . . ? H22D C22A H22E 109.5 . . ? C21 C22A H22F 109.5 . . ? H21 C22A H22F 122.7 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C26 109.4(5) . . ? C25 C24 P1 117.1(5) . . ? C26 C24 P1 110.7(4) . . ? C25 C24 H24 106.3 . . ? C26 C24 H24 106.3 . . ? P1 C24 H24 106.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C28 110.2(6) . . ? C29 C27 P2 111.9(5) . . ? C28 C27 P2 111.8(4) . . ? C29 C27 H27 107.6 . . ? C28 C27 H27 107.6 . . ? P2 C27 H27 107.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C30 C31 109.7(5) . . ? C32 C30 P2 110.8(5) . . ? C31 C30 P2 116.4(5) . . ? C32 C30 H30 106.4 . . ? C31 C30 H30 106.4 . . ? P2 C30 H30 106.4 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? P1 Ir1 P2 160.21(5) . . ? P1 Ir1 Cl2 95.77(6) . . ? P2 Ir1 Cl2 97.21(6) . . ? P1 Ir1 Cl1 83.98(5) . . ? P2 Ir1 Cl1 84.21(5) . . ? Cl2 Ir1 Cl1 175.58(5) . . ? P1 Ir1 H1 83.6(17) . . ? P2 Ir1 H1 85.1(17) . . ? Cl2 Ir1 H1 76.0(18) . . ? Cl1 Ir1 H1 108.3(18) . . ? P1 Ir1 H1IR 98.0(19) . . ? P2 Ir1 H1IR 99.4(19) . . ? Cl2 Ir1 H1IR 77.6(19) . . ? Cl1 Ir1 H1IR 98.0(19) . . ? H1 Ir1 H1IR 154(3) . . ? C4 P1 C21 104.4(3) . . ? C4 P1 C24 105.9(3) . . ? C21 P1 C24 107.5(3) . . ? C4 P1 Ir1 100.77(18) . . ? C21 P1 Ir1 119.8(3) . . ? C24 P1 Ir1 116.5(2) . . ? C27 P2 C10 103.8(3) . . ? C27 P2 C30 105.6(3) . . ? C10 P2 C30 104.9(3) . . ? C27 P2 Ir1 123.4(2) . . ? C10 P2 Ir1 100.58(17) . . ? C30 P2 Ir1 116.1(2) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 3.272 _refine_diff_density_min -1.197 _refine_diff_density_rms 0.157 data_sanaa41m _database_code_depnum_ccdc_archive 'CCDC 808731' #TrackingRef 'Sanaa4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H41 Cl P2 Pt, 2(C H Cl3)' _chemical_formula_sum 'C34 H43 Cl7 P2 Pt' _chemical_formula_weight 956.86 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 14.0962(8) _cell_length_b 14.0210(8) _cell_length_c 20.1340(11) _cell_angle_alpha 90.00 _cell_angle_beta 108.2680(10) _cell_angle_gamma 90.00 _cell_volume 3778.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description shapeless _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 4.317 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 42671 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 28.03 _reflns_number_total 9011 _reflns_number_gt 8098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0407P)^2^+8.8355P] 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 9011 _refine_ls_number_parameters 412 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 C1 C 0.6405(2) 0.2759(2) 0.25916(16) 0.0162(6) Uani 1 1 d . . . H1 H 0.707(3) 0.269(3) 0.259(2) 0.019 Uiso 1 1 d . . . C2 C 0.4607(2) 0.2863(2) 0.26452(18) 0.0202(6) Uani 1 1 d . . . H2 H 0.3907 0.2909 0.2663 0.024 Uiso 1 1 calc R . . C3 C 0.5636(2) 0.2847(2) 0.18628(17) 0.0167(6) Uani 1 1 d . . . C4 C 0.5808(2) 0.2913(2) 0.12121(17) 0.0193(6) Uani 1 1 d . . . C5 C 0.4966(3) 0.2933(3) 0.06109(18) 0.0251(7) Uani 1 1 d . . . H5 H 0.5060 0.2966 0.0164 0.030 Uiso 1 1 calc R . . C6 C 0.4004(3) 0.2906(3) 0.06517(19) 0.0267(7) Uani 1 1 d . . . H6 H 0.3451 0.2904 0.0235 0.032 Uiso 1 1 calc R . . C7 C 0.3843(3) 0.2880(2) 0.12996(19) 0.0227(7) Uani 1 1 d . . . H7 H 0.3183 0.2875 0.1329 0.027 Uiso 1 1 calc R . . C8 C 0.4657(2) 0.2862(2) 0.18975(17) 0.0190(6) Uani 1 1 d . . . C9 C 0.6249(2) 0.3640(2) 0.29960(16) 0.0166(6) Uani 1 1 d . . . C10 C 0.6937(2) 0.4361(2) 0.32971(17) 0.0196(6) Uani 1 1 d . . . C11 C 0.6615(3) 0.5112(3) 0.36390(19) 0.0248(7) Uani 1 1 d . . . H11 H 0.7072 0.5601 0.3858 0.030 Uiso 1 1 calc R . . C12 C 0.5639(3) 0.5149(3) 0.3662(2) 0.0281(8) Uani 1 1 d . . . H12 H 0.5436 0.5665 0.3892 0.034 Uiso 1 1 calc R . . C13 C 0.4964(3) 0.4441(3) 0.33515(19) 0.0244(7) Uani 1 1 d . . . H13 H 0.4296 0.4473 0.3364 0.029 Uiso 1 1 calc R . . C14 C 0.5263(3) 0.3684(2) 0.30218(18) 0.0196(6) Uani 1 1 d . . . C15 C 0.6096(2) 0.1891(2) 0.29331(17) 0.0189(6) Uani 1 1 d . . . C16 C 0.6671(3) 0.1089(2) 0.31709(18) 0.0214(7) Uani 1 1 d . . . H16 H 0.7331 0.1050 0.3144 0.026 Uiso 1 1 calc R . . C17 C 0.6272(3) 0.0342(2) 0.34493(19) 0.0262(7) Uani 1 1 d . . . H17 H 0.6663 -0.0212 0.3614 0.031 Uiso 1 1 calc R . . C18 C 0.5310(3) 0.0394(3) 0.34904(19) 0.0277(8) Uani 1 1 d . . . H18 H 0.5045 -0.0124 0.3679 0.033 Uiso 1 1 calc R . . C19 C 0.4733(3) 0.1203(3) 0.3256(2) 0.0254(7) Uani 1 1 d . . . H19 H 0.4077 0.1245 0.3291 0.031 Uiso 1 1 calc R . . C20 C 0.5124(2) 0.1949(2) 0.29697(17) 0.0201(6) Uani 1 1 d . . . C21 C 0.7398(3) 0.1826(3) 0.09353(19) 0.0271(7) Uani 1 1 d . . . H21 H 0.8070 0.1862 0.0867 0.033 Uiso 1 1 calc R . . C22 C 0.7501(3) 0.1174(3) 0.1560(2) 0.0356(9) Uani 1 1 d . . . H22A H 0.6859 0.1139 0.1653 0.053 Uiso 1 1 calc R . . H22B H 0.8011 0.1430 0.1972 0.053 Uiso 1 1 calc R . . H22C H 0.7697 0.0534 0.1457 0.053 Uiso 1 1 calc R . . C23 C 0.6678(4) 0.1400(3) 0.0267(2) 0.0413(10) Uani 1 1 d . . . H23A H 0.6896 0.0754 0.0198 0.062 Uiso 1 1 calc R . . H23B H 0.6674 0.1799 -0.0134 0.062 Uiso 1 1 calc R . . H23C H 0.6004 0.1375 0.0308 0.062 Uiso 1 1 calc R . . C24 C 0.6920(3) 0.3754(3) 0.03338(19) 0.0264(8) Uani 1 1 d . . . H24 H 0.6458 0.3412 -0.0077 0.032 Uiso 1 1 calc R . . C25 C 0.7952(3) 0.3839(4) 0.0237(2) 0.0405(10) Uani 1 1 d . . . H25A H 0.7894 0.4192 -0.0194 0.061 Uiso 1 1 calc R . . H25B H 0.8218 0.3201 0.0207 0.061 Uiso 1 1 calc R . . H25C H 0.8404 0.4180 0.0637 0.061 Uiso 1 1 calc R . . C26 C 0.6497(3) 0.4743(3) 0.0393(2) 0.0337(9) Uani 1 1 d . . . H26A H 0.6956 0.5085 0.0789 0.050 Uiso 1 1 calc R . . H26B H 0.5845 0.4677 0.0468 0.050 Uiso 1 1 calc R . . H26C H 0.6418 0.5101 -0.0039 0.050 Uiso 1 1 calc R . . C27 C 0.8985(3) 0.3703(2) 0.39635(18) 0.0224(7) Uani 1 1 d . . . H27 H 0.9688 0.3742 0.3953 0.027 Uiso 1 1 calc R . . C28 C 0.8694(3) 0.2654(3) 0.3911(2) 0.0284(8) Uani 1 1 d . . . H28A H 0.9140 0.2307 0.4310 0.043 Uiso 1 1 calc R . . H28B H 0.8752 0.2388 0.3476 0.043 Uiso 1 1 calc R . . H28C H 0.8003 0.2591 0.3914 0.043 Uiso 1 1 calc R . . C29 C 0.8971(3) 0.4109(3) 0.4664(2) 0.0337(9) Uani 1 1 d . . . H29A H 0.8293 0.4066 0.4697 0.051 Uiso 1 1 calc R . . H29B H 0.9182 0.4778 0.4700 0.051 Uiso 1 1 calc R . . H29C H 0.9430 0.3743 0.5046 0.051 Uiso 1 1 calc R . . C30 C 0.8665(3) 0.5618(2) 0.33590(19) 0.0254(7) Uani 1 1 d . . . H30 H 0.8632 0.5839 0.3824 0.030 Uiso 1 1 calc R . . C31 C 0.9762(3) 0.5620(3) 0.3369(2) 0.0343(9) Uani 1 1 d . . . H31A H 0.9807 0.5339 0.2935 0.051 Uiso 1 1 calc R . . H31B H 1.0166 0.5246 0.3769 0.051 Uiso 1 1 calc R . . H31C H 1.0010 0.6277 0.3411 0.051 Uiso 1 1 calc R . . C32 C 0.8037(4) 0.6286(3) 0.2788(2) 0.0370(10) Uani 1 1 d . . . H32A H 0.8309 0.6934 0.2873 0.056 Uiso 1 1 calc R . . H32B H 0.7345 0.6288 0.2795 0.056 Uiso 1 1 calc R . . H32C H 0.8055 0.6065 0.2330 0.056 Uiso 1 1 calc R . . C33 C 0.8198(3) 0.7048(3) 0.6096(2) 0.0344(9) Uani 1 1 d . . . H33 H 0.8696 0.6832 0.6544 0.041 Uiso 1 1 calc R . . C34 C 0.9244(3) 0.9085(3) 0.3542(3) 0.0417(10) Uani 1 1 d . . . H34 H 0.9796 0.8805 0.3392 0.050 Uiso 1 1 calc R . . Cl1 Cl 0.95632(6) 0.28553(7) 0.24139(5) 0.02626(17) Uani 1 1 d . . . Cl2 Cl 0.81861(10) 0.62283(10) 0.54377(8) 0.0612(4) Uani 1 1 d . . . Cl3 Cl 0.70121(9) 0.70906(12) 0.62084(7) 0.0592(4) Uani 1 1 d . . . Cl4 Cl 0.85346(10) 0.81743(10) 0.58907(8) 0.0582(3) Uani 1 1 d . . . Cl5 Cl 0.81402(9) 0.90552(9) 0.28274(6) 0.0460(3) Uani 1 1 d . . . Cl6 Cl 0.90979(14) 0.8394(2) 0.42283(9) 0.1035(8) Uani 1 1 d . . . Cl7 Cl 0.95550(13) 1.02469(12) 0.38044(18) 0.1391(12) Uani 1 1 d . . . P1 P 0.70690(6) 0.30474(6) 0.11321(4) 0.01871(16) Uani 1 1 d . . . P2 P 0.81960(6) 0.43856(6) 0.32070(4) 0.01758(16) Uani 1 1 d . . . Pt1 Pt 0.802529(9) 0.376718(9) 0.213188(6) 0.01794(5) Uani 1 1 d . . . H1PT H 0.712(4) 0.441(4) 0.189(3) 0.058(16) Uiso 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 C1 0.0158(14) 0.0136(14) 0.0189(15) 0.0002(11) 0.0050(12) -0.0009(11) C2 0.0168(14) 0.0220(16) 0.0229(16) -0.0009(13) 0.0081(13) -0.0001(12) C3 0.0165(14) 0.0117(13) 0.0204(15) -0.0012(11) 0.0037(12) 0.0010(11) C4 0.0184(15) 0.0171(15) 0.0212(16) -0.0027(12) 0.0044(12) -0.0011(12) C5 0.0253(17) 0.0268(18) 0.0204(16) -0.0032(14) 0.0033(14) -0.0007(14) C6 0.0221(17) 0.0252(18) 0.0265(18) -0.0028(14) -0.0016(14) -0.0011(14) C7 0.0183(15) 0.0181(15) 0.0307(18) -0.0017(13) 0.0062(14) 0.0001(12) C8 0.0213(15) 0.0139(14) 0.0214(16) -0.0023(12) 0.0061(13) 0.0003(12) C9 0.0179(15) 0.0175(15) 0.0154(14) 0.0021(11) 0.0068(12) 0.0019(12) C10 0.0211(15) 0.0201(16) 0.0165(15) 0.0008(12) 0.0044(12) -0.0006(12) C11 0.0256(17) 0.0224(17) 0.0246(17) -0.0033(14) 0.0051(14) -0.0002(14) C12 0.0304(19) 0.0268(18) 0.0305(19) -0.0068(15) 0.0145(16) 0.0043(15) C13 0.0222(16) 0.0255(17) 0.0278(18) 0.0003(14) 0.0111(14) 0.0051(14) C14 0.0192(15) 0.0198(16) 0.0206(16) 0.0006(12) 0.0072(13) 0.0005(12) C15 0.0199(15) 0.0169(15) 0.0191(15) -0.0025(12) 0.0051(12) -0.0020(12) C16 0.0220(16) 0.0195(16) 0.0227(16) 0.0001(13) 0.0068(13) 0.0004(13) C17 0.0307(18) 0.0183(16) 0.0272(18) 0.0017(14) 0.0054(15) -0.0006(14) C18 0.0348(19) 0.0225(17) 0.0258(18) 0.0025(14) 0.0092(15) -0.0092(15) C19 0.0238(17) 0.0274(18) 0.0264(18) -0.0005(14) 0.0097(14) -0.0059(14) C20 0.0186(15) 0.0202(16) 0.0214(16) -0.0007(13) 0.0060(13) -0.0016(12) C21 0.0282(18) 0.0267(18) 0.0290(19) -0.0053(15) 0.0126(15) 0.0025(14) C22 0.043(2) 0.0224(19) 0.043(2) 0.0008(16) 0.0159(19) 0.0028(16) C23 0.044(2) 0.039(2) 0.040(2) -0.0217(19) 0.011(2) 0.0013(19) C24 0.0280(18) 0.034(2) 0.0168(16) 0.0010(14) 0.0072(14) -0.0014(15) C25 0.035(2) 0.060(3) 0.032(2) 0.0106(19) 0.0175(18) -0.001(2) C26 0.040(2) 0.033(2) 0.0282(19) 0.0085(16) 0.0109(17) 0.0033(17) C27 0.0191(16) 0.0250(17) 0.0219(16) 0.0037(13) 0.0048(13) -0.0022(13) C28 0.0302(19) 0.0251(18) 0.0267(18) 0.0072(14) 0.0043(15) 0.0002(15) C29 0.037(2) 0.039(2) 0.0213(18) -0.0018(16) 0.0037(16) -0.0029(18) C30 0.0288(18) 0.0196(16) 0.0262(18) -0.0023(13) 0.0066(14) -0.0047(14) C31 0.0294(19) 0.035(2) 0.037(2) 0.0011(17) 0.0079(17) -0.0134(16) C32 0.045(2) 0.0214(18) 0.037(2) 0.0056(16) 0.0027(19) -0.0029(16) C33 0.0281(19) 0.044(2) 0.0285(19) 0.0015(17) 0.0048(16) 0.0004(17) C34 0.037(2) 0.033(2) 0.056(3) -0.012(2) 0.016(2) -0.0011(18) Cl1 0.0177(4) 0.0347(5) 0.0269(4) -0.0022(3) 0.0077(3) 0.0051(3) Cl2 0.0477(7) 0.0643(9) 0.0624(8) -0.0260(6) 0.0038(6) 0.0153(6) Cl3 0.0388(6) 0.1038(11) 0.0408(6) 0.0103(7) 0.0205(5) 0.0013(7) Cl4 0.0504(7) 0.0478(7) 0.0679(8) 0.0098(6) 0.0063(6) -0.0123(6) Cl5 0.0453(6) 0.0398(6) 0.0494(6) -0.0010(5) 0.0096(5) 0.0058(5) Cl6 0.0631(10) 0.189(2) 0.0492(9) 0.0259(12) 0.0049(7) -0.0319(13) Cl7 0.0560(10) 0.0476(9) 0.266(3) -0.0650(14) -0.0176(14) -0.0019(7) P1 0.0193(4) 0.0218(4) 0.0151(4) -0.0023(3) 0.0056(3) 0.0005(3) P2 0.0174(4) 0.0175(4) 0.0171(4) -0.0007(3) 0.0042(3) -0.0028(3) Pt1 0.01807(7) 0.01985(7) 0.01599(7) -0.00027(4) 0.00548(5) -0.00225(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 C1 C15 1.527(4) . ? C1 C3 1.532(4) . ? C1 C9 1.534(4) . ? C1 H1 0.93(4) . ? C2 C20 1.517(5) . ? C2 C14 1.522(5) . ? C2 C8 1.529(5) . ? C2 H2 1.0000 . ? C3 C8 1.404(4) . ? C3 C4 1.408(5) . ? C4 C5 1.404(5) . ? C4 P1 1.845(3) . ? C5 C6 1.384(5) . ? C5 H5 0.9500 . ? C6 C7 1.393(5) . ? C6 H6 0.9500 . ? C7 C8 1.379(5) . ? C7 H7 0.9500 . ? C9 C10 1.401(5) . ? C9 C14 1.409(4) . ? C10 C11 1.408(5) . ? C10 P2 1.840(3) . ? C11 C12 1.393(5) . ? C11 H11 0.9500 . ? C12 C13 1.382(5) . ? C12 H12 0.9500 . ? C13 C14 1.385(5) . ? C13 H13 0.9500 . ? C15 C16 1.380(5) . ? C15 C20 1.398(4) . ? C16 C17 1.388(5) . ? C16 H16 0.9500 . ? C17 C18 1.386(5) . ? C17 H17 0.9500 . ? C18 C19 1.389(5) . ? C18 H18 0.9500 . ? C19 C20 1.389(5) . ? C19 H19 0.9500 . ? C21 C22 1.525(6) . ? C21 C23 1.530(6) . ? C21 P1 1.850(4) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.529(5) . ? C24 C25 1.531(5) . ? C24 P1 1.843(4) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.523(5) . ? C27 C29 1.527(5) . ? C27 P2 1.847(4) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C32 1.532(5) . ? C30 C31 1.540(5) . ? C30 P2 1.841(4) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 Cl4 1.736(5) . ? C33 Cl2 1.750(4) . ? C33 Cl3 1.756(4) . ? C33 H33 1.0000 . ? C34 Cl7 1.726(5) . ? C34 Cl6 1.752(5) . ? C34 Cl5 1.758(5) . ? C34 H34 1.0000 . ? Cl1 Pt1 2.4259(8) . ? P1 Pt1 2.2774(8) . ? P2 Pt1 2.2734(8) . ? Pt1 H1PT 1.52(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 C1 C3 106.2(2) . . ? C15 C1 C9 107.1(3) . . ? C3 C1 C9 105.5(2) . . ? C15 C1 H1 110(2) . . ? C3 C1 H1 115(2) . . ? C9 C1 H1 113(2) . . ? C20 C2 C14 106.8(3) . . ? C20 C2 C8 105.0(3) . . ? C14 C2 C8 106.4(3) . . ? C20 C2 H2 112.7 . . ? C14 C2 H2 112.7 . . ? C8 C2 H2 112.7 . . ? C8 C3 C4 120.2(3) . . ? C8 C3 C1 111.4(3) . . ? C4 C3 C1 128.3(3) . . ? C5 C4 C3 117.3(3) . . ? C5 C4 P1 120.0(3) . . ? C3 C4 P1 122.6(2) . . ? C6 C5 C4 121.8(3) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 120.5(3) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 118.8(3) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C7 C8 C3 121.3(3) . . ? C7 C8 C2 125.2(3) . . ? C3 C8 C2 113.5(3) . . ? C10 C9 C14 120.6(3) . . ? C10 C9 C1 128.0(3) . . ? C14 C9 C1 111.3(3) . . ? C9 C10 C11 117.7(3) . . ? C9 C10 P2 121.9(2) . . ? C11 C10 P2 120.2(3) . . ? C12 C11 C10 121.2(3) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.8(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C9 120.2(3) . . ? C13 C14 C2 126.1(3) . . ? C9 C14 C2 113.6(3) . . ? C16 C15 C20 120.6(3) . . ? C16 C15 C1 125.8(3) . . ? C20 C15 C1 113.6(3) . . ? C15 C16 C17 119.1(3) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C18 C17 C16 120.8(3) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 120.2(3) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C20 119.3(3) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C19 C20 C15 120.0(3) . . ? C19 C20 C2 128.0(3) . . ? C15 C20 C2 111.9(3) . . ? C22 C21 C23 110.9(4) . . ? C22 C21 P1 110.1(3) . . ? C23 C21 P1 114.0(3) . . ? C22 C21 H21 107.2 . . ? C23 C21 H21 107.2 . . ? P1 C21 H21 107.2 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C25 110.4(3) . . ? C26 C24 P1 111.1(3) . . ? C25 C24 P1 107.4(3) . . ? C26 C24 H24 109.3 . . ? C25 C24 H24 109.3 . . ? P1 C24 H24 109.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 110.0(3) . . ? C28 C27 P2 111.4(2) . . ? C29 C27 P2 113.0(3) . . ? C28 C27 H27 107.4 . . ? C29 C27 H27 107.4 . . ? P2 C27 H27 107.4 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C30 C31 110.5(3) . . ? C32 C30 P2 110.9(3) . . ? C31 C30 P2 108.1(3) . . ? C32 C30 H30 109.1 . . ? C31 C30 H30 109.1 . . ? P2 C30 H30 109.1 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Cl4 C33 Cl2 110.8(2) . . ? Cl4 C33 Cl3 110.0(2) . . ? Cl2 C33 Cl3 109.7(2) . . ? Cl4 C33 H33 108.8 . . ? Cl2 C33 H33 108.8 . . ? Cl3 C33 H33 108.8 . . ? Cl7 C34 Cl6 111.2(3) . . ? Cl7 C34 Cl5 110.4(3) . . ? Cl6 C34 Cl5 109.8(3) . . ? Cl7 C34 H34 108.4 . . ? Cl6 C34 H34 108.4 . . ? Cl5 C34 H34 108.4 . . ? C24 P1 C4 106.37(16) . . ? C24 P1 C21 106.17(17) . . ? C4 P1 C21 103.73(16) . . ? C24 P1 Pt1 114.00(12) . . ? C4 P1 Pt1 106.73(11) . . ? C21 P1 Pt1 118.74(12) . . ? C10 P2 C30 107.93(16) . . ? C10 P2 C27 105.02(15) . . ? C30 P2 C27 104.90(16) . . ? C10 P2 Pt1 105.63(11) . . ? C30 P2 Pt1 116.21(12) . . ? C27 P2 Pt1 116.39(12) . . ? P2 Pt1 P1 150.14(3) . . ? P2 Pt1 Cl1 99.09(3) . . ? P1 Pt1 Cl1 102.20(3) . . ? P2 Pt1 H1PT 84(2) . . ? P1 Pt1 H1PT 77(2) . . ? Cl1 Pt1 H1PT 172(2) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 4.037 _refine_diff_density_min -0.997 _refine_diff_density_rms 0.121