# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1785 data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 O3 P2' _chemical_formula_weight 398.35 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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' _cell_length_a 8.5253(12) _cell_length_b 9.4993(17) _cell_length_c 25.999(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2105.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.225 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.23409 _exptl_absorpt_correction_T_max 0.26468 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9888 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3694 _reflns_number_gt 3148 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+1.6000P] 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 SHELXL _refine_ls_extinction_coef 0.0080(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(14) _refine_ls_number_reflns 3694 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1280 _refine_ls_wR_factor_gt 0.1163 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.002 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 P1 P 0.49848(11) 0.80886(10) 0.13542(3) 0.0391(2) Uani 1 1 d . . . O1 O 0.5796(3) 0.9394(3) 0.12114(10) 0.0495(7) Uani 1 1 d . . . O2 O 0.5126(3) 0.7617(3) 0.19290(9) 0.0436(6) Uani 1 1 d . . . O3 O 0.5602(3) 0.6755(3) 0.10535(9) 0.0428(6) Uani 1 1 d . . . P2 P 0.25149(12) 0.53076(9) 0.14934(3) 0.0382(2) Uani 1 1 d . . . C1 C 0.1831(4) 0.7087(4) 0.13240(12) 0.0360(8) Uani 1 1 d . . . C2 C 0.2905(4) 0.8220(4) 0.12641(12) 0.0347(7) Uani 1 1 d . . . C3 C 0.2354(4) 0.9567(4) 0.11373(12) 0.0401(8) Uani 1 1 d . . . H3A H 0.3079 1.0317 0.1093 0.048 Uiso 1 1 calc R . . C4 C 0.0760(5) 0.9817(4) 0.10764(14) 0.0482(9) Uani 1 1 d . . . H4A H 0.0402 1.0732 0.0988 0.058 Uiso 1 1 calc R . . C5 C -0.0293(4) 0.8751(4) 0.11433(15) 0.0469(10) Uani 1 1 d . . . H5A H -0.1384 0.8935 0.1110 0.056 Uiso 1 1 calc R . . C6 C 0.0224(4) 0.7378(4) 0.12623(13) 0.0413(8) Uani 1 1 d . . . H6A H -0.0521 0.6643 0.1301 0.050 Uiso 1 1 calc R . . C7 C 0.6582(5) 0.7089(6) 0.21484(16) 0.0615(12) Uani 1 1 d . . . H7A H 0.7431 0.7788 0.2099 0.074 Uiso 1 1 calc R . . H7B H 0.6892 0.6204 0.1975 0.074 Uiso 1 1 calc R . . C8 C 0.6329(5) 0.6831(6) 0.27077(16) 0.0678(13) Uani 1 1 d . . . H8A H 0.7317 0.6534 0.2866 0.102 Uiso 1 1 calc R . . H8B H 0.5540 0.6091 0.2752 0.102 Uiso 1 1 calc R . . H8C H 0.5962 0.7699 0.2872 0.102 Uiso 1 1 calc R . . C9 C 0.5943(5) 0.6856(5) 0.05061(14) 0.0552(10) Uani 1 1 d . . . H9A H 0.6497 0.7748 0.0432 0.066 Uiso 1 1 calc R . . H9B H 0.4953 0.6845 0.0307 0.066 Uiso 1 1 calc R . . C10 C 0.6942(6) 0.5637(6) 0.03541(18) 0.0723(14) Uani 1 1 d . . . H10A H 0.7193 0.5704 -0.0013 0.109 Uiso 1 1 calc R . . H10B H 0.6375 0.4758 0.0420 0.109 Uiso 1 1 calc R . . H10C H 0.7914 0.5649 0.0555 0.109 Uiso 1 1 calc R . . C11 C 0.0710(4) 0.4473(4) 0.17240(13) 0.0407(8) Uani 1 1 d . . . C12 C -0.0281(5) 0.3642(4) 0.14264(15) 0.0527(10) Uani 1 1 d . . . H12A H -0.0066 0.3525 0.1070 0.063 Uiso 1 1 calc R . . C13 C -0.1578(5) 0.2982(5) 0.16412(17) 0.0609(11) Uani 1 1 d . . . H13A H -0.2238 0.2411 0.1433 0.073 Uiso 1 1 calc R . . C14 C -0.1913(5) 0.3156(5) 0.21615(17) 0.0570(11) Uani 1 1 d . . . H14A H -0.2802 0.2712 0.2310 0.068 Uiso 1 1 calc R . . C15 C -0.0945(5) 0.3973(5) 0.24557(16) 0.0550(10) Uani 1 1 d . . . H15A H -0.1171 0.4097 0.2811 0.066 Uiso 1 1 calc R . . C16 C 0.0355(5) 0.4622(4) 0.22455(13) 0.0485(9) Uani 1 1 d . . . H16A H 0.1017 0.5177 0.2458 0.058 Uiso 1 1 calc R . . C21 C 0.2720(4) 0.4504(4) 0.08569(13) 0.0394(8) Uani 1 1 d . . . C22 C 0.2129(5) 0.5036(4) 0.04001(13) 0.0471(10) Uani 1 1 d . . . H22A H 0.1550 0.5890 0.0406 0.057 Uiso 1 1 calc R . . C23 C 0.2359(6) 0.4355(4) -0.00677(14) 0.0521(10) Uani 1 1 d . . . H23A H 0.1961 0.4751 -0.0377 0.063 Uiso 1 1 calc R . . C24 C 0.3171(5) 0.3101(5) -0.00783(16) 0.0602(12) Uani 1 1 d . . . H24A H 0.3316 0.2617 -0.0394 0.072 Uiso 1 1 calc R . . C25 C 0.3767(6) 0.2557(4) 0.03670(18) 0.0595(12) Uani 1 1 d . . . H25A H 0.4323 0.1691 0.0357 0.071 Uiso 1 1 calc R . . C26 C 0.3577(4) 0.3244(4) 0.08329(16) 0.0491(10) Uani 1 1 d . . . H26A H 0.4027 0.2862 0.1137 0.059 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 P1 0.0363(4) 0.0445(5) 0.0364(5) 0.0001(4) 0.0036(4) -0.0009(4) O1 0.0399(14) 0.0500(16) 0.0587(17) 0.0036(13) 0.0064(12) -0.0104(12) O2 0.0410(13) 0.0565(15) 0.0332(12) -0.0001(11) -0.0013(11) 0.0029(12) O3 0.0454(14) 0.0512(15) 0.0320(13) 0.0007(11) 0.0083(10) 0.0102(12) P2 0.0444(5) 0.0377(4) 0.0325(4) 0.0017(4) 0.0010(4) 0.0002(4) C1 0.0405(18) 0.0415(19) 0.0260(16) 0.0006(15) -0.0002(14) 0.0012(15) C2 0.0387(18) 0.0394(17) 0.0259(16) 0.0011(14) 0.0035(13) 0.0020(15) C3 0.048(2) 0.0388(17) 0.0333(16) 0.0008(15) 0.0039(16) 0.0003(19) C4 0.050(2) 0.049(2) 0.046(2) 0.0058(17) 0.0014(17) 0.0095(19) C5 0.038(2) 0.049(2) 0.054(2) 0.0017(18) 0.0036(17) 0.0058(17) C6 0.0406(19) 0.0431(19) 0.0401(19) 0.0012(15) -0.0014(16) -0.0028(16) C7 0.052(2) 0.084(3) 0.049(2) 0.008(2) -0.0093(19) 0.014(2) C8 0.070(3) 0.087(3) 0.046(2) 0.003(2) -0.011(2) 0.014(3) C9 0.062(2) 0.070(3) 0.034(2) 0.0025(19) 0.0128(18) 0.002(2) C10 0.077(3) 0.089(4) 0.051(3) -0.023(3) 0.011(2) 0.014(3) C11 0.045(2) 0.043(2) 0.0336(18) 0.0031(16) 0.0039(15) 0.0034(16) C12 0.061(3) 0.055(2) 0.042(2) -0.0044(18) 0.004(2) -0.008(2) C13 0.060(3) 0.062(3) 0.061(3) -0.005(2) 0.009(2) -0.015(2) C14 0.057(2) 0.052(2) 0.062(3) 0.009(2) 0.020(2) 0.003(2) C15 0.062(3) 0.061(3) 0.042(2) 0.0081(19) 0.012(2) 0.007(2) C16 0.065(3) 0.047(2) 0.0342(18) 0.0034(16) 0.0041(17) 0.000(2) C21 0.0424(19) 0.0405(19) 0.0352(17) 0.0005(14) 0.0071(15) -0.0042(17) C22 0.064(3) 0.041(2) 0.0368(19) 0.0000(15) 0.0028(17) -0.0016(17) C23 0.072(3) 0.047(2) 0.0370(19) -0.0002(15) 0.006(2) -0.008(2) C24 0.083(3) 0.050(2) 0.047(2) -0.011(2) 0.024(2) -0.017(2) C25 0.071(3) 0.043(2) 0.065(3) -0.004(2) 0.025(2) 0.007(2) C26 0.052(2) 0.047(2) 0.049(2) 0.0063(18) 0.0097(18) 0.0083(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O1 1.468(3) . ? P1 O2 1.565(2) . ? P1 O3 1.579(3) . ? P1 C2 1.793(3) . ? O2 C7 1.455(5) . ? O3 C9 1.456(4) . ? P2 C21 1.831(3) . ? P2 C11 1.832(4) . ? P2 C1 1.842(4) . ? C1 C6 1.407(5) . ? C1 C2 1.421(5) . ? C2 C3 1.403(5) . ? C3 C4 1.388(5) . ? C4 C5 1.364(5) . ? C5 C6 1.411(5) . ? C7 C8 1.490(6) . ? C9 C10 1.490(6) . ? C11 C12 1.391(5) . ? C11 C16 1.396(5) . ? C12 C13 1.389(6) . ? C13 C14 1.392(6) . ? C14 C15 1.367(6) . ? C15 C16 1.381(6) . ? C21 C22 1.386(5) . ? C21 C26 1.404(5) . ? C22 C23 1.391(5) . ? C23 C24 1.378(6) . ? C24 C25 1.366(6) . ? C25 C26 1.386(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 O1 P1 O2 116.59(15) . . ? O1 P1 O3 113.31(14) . . ? O2 P1 O3 102.55(14) . . ? O1 P1 C2 111.96(16) . . ? O2 P1 C2 102.74(14) . . ? O3 P1 C2 108.72(15) . . ? C7 O2 P1 122.6(2) . . ? C9 O3 P1 119.9(3) . . ? C21 P2 C11 101.28(16) . . ? C21 P2 C1 101.34(15) . . ? C11 P2 C1 102.10(16) . . ? C6 C1 C2 117.8(3) . . ? C6 C1 P2 121.1(3) . . ? C2 C1 P2 121.1(2) . . ? C3 C2 C1 120.0(3) . . ? C3 C2 P1 115.2(3) . . ? C1 C2 P1 124.8(3) . . ? C4 C3 C2 120.7(3) . . ? C5 C4 C3 120.2(4) . . ? C4 C5 C6 120.5(4) . . ? C1 C6 C5 120.7(3) . . ? O2 C7 C8 108.4(3) . . ? O3 C9 C10 108.8(3) . . ? C12 C11 C16 117.8(4) . . ? C12 C11 P2 125.0(3) . . ? C16 C11 P2 117.1(3) . . ? C13 C12 C11 121.1(4) . . ? C12 C13 C14 120.0(4) . . ? C15 C14 C13 119.2(4) . . ? C14 C15 C16 121.1(4) . . ? C15 C16 C11 120.8(4) . . ? C22 C21 C26 117.5(3) . . ? C22 C21 P2 126.0(3) . . ? C26 C21 P2 116.4(3) . . ? C21 C22 C23 121.9(4) . . ? C24 C23 C22 119.4(4) . . ? C25 C24 C23 119.8(4) . . ? C24 C25 C26 121.3(4) . . ? C25 C26 C21 120.1(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 O1 P1 O2 C7 -70.4(4) . . . . ? O3 P1 O2 C7 54.0(3) . . . . ? C2 P1 O2 C7 166.8(3) . . . . ? O1 P1 O3 C9 -41.8(3) . . . . ? O2 P1 O3 C9 -168.3(3) . . . . ? C2 P1 O3 C9 83.4(3) . . . . ? C21 P2 C1 C6 88.0(3) . . . . ? C11 P2 C1 C6 -16.3(3) . . . . ? C21 P2 C1 C2 -93.6(3) . . . . ? C11 P2 C1 C2 162.1(3) . . . . ? C6 C1 C2 C3 -1.3(5) . . . . ? P2 C1 C2 C3 -179.7(2) . . . . ? C6 C1 C2 P1 177.1(3) . . . . ? P2 C1 C2 P1 -1.3(4) . . . . ? O1 P1 C2 C3 -7.6(3) . . . . ? O2 P1 C2 C3 118.2(2) . . . . ? O3 P1 C2 C3 -133.6(2) . . . . ? O1 P1 C2 C1 173.9(3) . . . . ? O2 P1 C2 C1 -60.2(3) . . . . ? O3 P1 C2 C1 48.0(3) . . . . ? C1 C2 C3 C4 0.9(5) . . . . ? P1 C2 C3 C4 -177.6(3) . . . . ? C2 C3 C4 C5 0.5(6) . . . . ? C3 C4 C5 C6 -1.6(6) . . . . ? C2 C1 C6 C5 0.2(5) . . . . ? P2 C1 C6 C5 178.6(3) . . . . ? C4 C5 C6 C1 1.2(6) . . . . ? P1 O2 C7 C8 176.2(3) . . . . ? P1 O3 C9 C10 162.8(3) . . . . ? C21 P2 C11 C12 -8.9(4) . . . . ? C1 P2 C11 C12 95.4(3) . . . . ? C21 P2 C11 C16 167.3(3) . . . . ? C1 P2 C11 C16 -88.4(3) . . . . ? C16 C11 C12 C13 -0.1(6) . . . . ? P2 C11 C12 C13 176.1(3) . . . . ? C11 C12 C13 C14 0.6(7) . . . . ? C12 C13 C14 C15 -0.4(7) . . . . ? C13 C14 C15 C16 -0.2(7) . . . . ? C14 C15 C16 C11 0.7(6) . . . . ? C12 C11 C16 C15 -0.5(6) . . . . ? P2 C11 C16 C15 -177.1(3) . . . . ? C11 P2 C21 C22 91.3(3) . . . . ? C1 P2 C21 C22 -13.7(4) . . . . ? C11 P2 C21 C26 -89.7(3) . . . . ? C1 P2 C21 C26 165.3(3) . . . . ? C26 C21 C22 C23 0.3(6) . . . . ? P2 C21 C22 C23 179.3(3) . . . . ? C21 C22 C23 C24 1.3(6) . . . . ? C22 C23 C24 C25 -1.4(6) . . . . ? C23 C24 C25 C26 -0.2(7) . . . . ? C24 C25 C26 C21 1.9(6) . . . . ? C22 C21 C26 C25 -1.9(5) . . . . ? P2 C21 C26 C25 179.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.286 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.053 data_2.2Me2CO _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C50 H60 Cl2 O8 P4 Pt' _chemical_formula_weight 1178.85 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2995(10) _cell_length_b 11.7240(11) _cell_length_c 13.483(3) _cell_angle_alpha 64.608(12) _cell_angle_beta 76.108(6) _cell_angle_gamma 72.660(7) _cell_volume 1256.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(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 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method ? _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 3.077 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.724989 _exptl_absorpt_correction_T_max 0.831102 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12712 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5658 _reflns_number_observed 5536 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995b)' _computing_cell_refinement 'SAINT (Siemens, 1995b)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0163P)^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 5658 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0209 _refine_ls_R_factor_obs 0.0203 _refine_ls_wR_factor_all 0.0451 _refine_ls_wR_factor_obs 0.0449 _refine_ls_goodness_of_fit_all 0.999 _refine_ls_goodness_of_fit_obs 1.007 _refine_ls_restrained_S_all 0.999 _refine_ls_restrained_S_obs 1.007 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_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 0.0000 0.0000 0.0000 0.01646(4) Uani 1 2 d S . . Cl1 Cl 0.16617(7) 0.04004(6) -0.16319(5) 0.02710(14) Uani 1 1 d . . . P1 P -0.13426(7) -0.01935(6) -0.27016(5) 0.02356(14) Uani 1 1 d . . . P2 P -0.03253(6) -0.18559(6) -0.00645(5) 0.01717(13) Uani 1 1 d . . . O1 O -0.19997(18) 0.04115(17) -0.18968(14) 0.0276(4) Uani 1 1 d . . . O2 O -0.23829(18) -0.08912(18) -0.29103(15) 0.0309(4) Uani 1 1 d . . . O3 O -0.0938(2) 0.07874(18) -0.39220(14) 0.0324(4) Uani 1 1 d . . . O4 O 0.4304(3) -0.6381(3) 0.4831(2) 0.0971(11) Uani 1 1 d . . . C11 C 0.0490(2) -0.3247(2) 0.11104(19) 0.0198(5) Uani 1 1 d . . . C12 C 0.0185(3) -0.4470(2) 0.1492(2) 0.0268(6) Uani 1 1 d . . . H12A H -0.0530 -0.4598 0.1171 0.032 Uiso 1 1 calc R . . C13 C 0.0914(3) -0.5501(2) 0.2334(2) 0.0314(6) Uani 1 1 d . . . H13A H 0.0696 -0.6331 0.2591 0.038 Uiso 1 1 calc R . . C14 C 0.1953(3) -0.5326(3) 0.2800(2) 0.0337(6) Uani 1 1 d . . . H14A H 0.2479 -0.6042 0.3360 0.040 Uiso 1 1 calc R . . C15 C 0.2233(3) -0.4114(3) 0.2456(2) 0.0319(6) Uani 1 1 d . . . H15A H 0.2933 -0.3990 0.2791 0.038 Uiso 1 1 calc R . . C16 C 0.1498(3) -0.3081(2) 0.1625(2) 0.0243(5) Uani 1 1 d . . . H16A H 0.1681 -0.2245 0.1402 0.029 Uiso 1 1 calc R . . C21 C -0.2185(2) -0.2141(2) 0.00102(19) 0.0200(5) Uani 1 1 d . . . C22 C -0.3518(3) -0.1506(3) 0.0452(2) 0.0269(6) Uani 1 1 d . . . H22A H -0.3485 -0.0892 0.0726 0.032 Uiso 1 1 calc R . . C23 C -0.4902(3) -0.1764(3) 0.0498(2) 0.0336(6) Uani 1 1 d . . . H23A H -0.5807 -0.1340 0.0818 0.040 Uiso 1 1 calc R . . C24 C -0.4969(3) -0.2630(3) 0.0081(2) 0.0340(6) Uani 1 1 d . . . H24A H -0.5922 -0.2784 0.0097 0.041 Uiso 1 1 calc R . . C25 C -0.3660(3) -0.3273(3) -0.0357(2) 0.0297(6) Uani 1 1 d . . . H25A H -0.3705 -0.3879 -0.0635 0.036 Uiso 1 1 calc R . . C26 C -0.2266(3) -0.3032(2) -0.0392(2) 0.0256(5) Uani 1 1 d . . . H26A H -0.1362 -0.3479 -0.0692 0.031 Uiso 1 1 calc R . . C31 C 0.0745(2) -0.2200(2) -0.12847(19) 0.0186(5) Uani 1 1 d . . . C32 C 0.2048(3) -0.3196(2) -0.1145(2) 0.0233(5) Uani 1 1 d . . . H32A H 0.2336 -0.3695 -0.0424 0.028 Uiso 1 1 calc R . . C33 C 0.2937(3) -0.3478(3) -0.2036(2) 0.0296(6) Uani 1 1 d . . . H33A H 0.3816 -0.4165 -0.1918 0.036 Uiso 1 1 calc R . . C34 C 0.2544(3) -0.2760(3) -0.3092(2) 0.0313(6) Uani 1 1 d . . . H34A H 0.3152 -0.2947 -0.3702 0.038 Uiso 1 1 calc R . . C35 C 0.1255(3) -0.1765(3) -0.3250(2) 0.0263(6) Uani 1 1 d . . . H35A H 0.0989 -0.1271 -0.3978 0.032 Uiso 1 1 calc R . . C36 C 0.0339(2) -0.1471(2) -0.23693(19) 0.0203(5) Uani 1 1 d . . . C37 C -0.3995(3) -0.0279(3) -0.2984(3) 0.0527(9) Uani 1 1 d . . . H37A H -0.4106 0.0600 -0.3576 0.063 Uiso 1 1 calc R . . H37B H -0.4500 -0.0197 -0.2275 0.063 Uiso 1 1 calc R . . C38 C -0.4709(4) -0.1071(4) -0.3230(3) 0.0653(11) Uani 1 1 d . . . H38A H -0.5789 -0.0662 -0.3282 0.098 Uiso 1 1 calc R . . H38B H -0.4607 -0.1936 -0.2637 0.098 Uiso 1 1 calc R . . H38C H -0.4210 -0.1144 -0.3934 0.098 Uiso 1 1 calc R . . C39 C -0.0270(4) 0.1860(3) -0.4125(3) 0.0495(8) Uani 1 1 d . . . H39A H -0.0329 0.1953 -0.3420 0.059 Uiso 1 1 calc R . . H39B H -0.0846 0.2676 -0.4633 0.059 Uiso 1 1 calc R . . C40 C 0.1339(4) 0.1618(4) -0.4623(3) 0.0656(11) Uani 1 1 d . . . H40A H 0.1763 0.2363 -0.4795 0.098 Uiso 1 1 calc R . . H40B H 0.1397 0.1490 -0.5304 0.098 Uiso 1 1 calc R . . H40C H 0.1921 0.0841 -0.4097 0.098 Uiso 1 1 calc R . . C51 C 0.3762(4) -0.6281(3) 0.5696(3) 0.0512(8) Uani 1 1 d . . . C52 C 0.2100(5) -0.5658(5) 0.5870(4) 0.0999(17) Uani 1 1 d . . . H52A H 0.1644 -0.5394 0.5198 0.150 Uiso 1 1 calc R . . H52B H 0.1996 -0.4896 0.6031 0.150 Uiso 1 1 calc R . . H52C H 0.1580 -0.6279 0.6493 0.150 Uiso 1 1 calc R . . C53 C 0.4617(6) -0.6695(5) 0.6588(4) 0.116(2) Uani 1 1 d . . . H53A H 0.5700 -0.6952 0.6339 0.174 Uiso 1 1 calc R . . H53B H 0.4283 -0.7435 0.7207 0.174 Uiso 1 1 calc R . . H53C H 0.4454 -0.5983 0.6829 0.174 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 0.02044(7) 0.01637(7) 0.01529(7) -0.00908(5) 0.00047(5) -0.00558(5) Cl1 0.0330(3) 0.0334(4) 0.0222(3) -0.0171(3) 0.0080(3) -0.0170(3) P1 0.0262(3) 0.0258(4) 0.0205(3) -0.0107(3) -0.0032(3) -0.0053(3) P2 0.0198(3) 0.0175(3) 0.0173(3) -0.0102(3) 0.0004(2) -0.0053(2) O1 0.0284(9) 0.0306(10) 0.0250(9) -0.0152(8) -0.0015(7) -0.0029(8) O2 0.0266(9) 0.0375(11) 0.0372(11) -0.0211(9) -0.0072(8) -0.0064(8) O3 0.0419(11) 0.0323(11) 0.0217(9) -0.0078(8) -0.0040(8) -0.0103(9) O4 0.0724(18) 0.156(3) 0.0649(19) -0.072(2) -0.0020(14) 0.0114(18) C11 0.0208(11) 0.0201(13) 0.0190(12) -0.0105(10) 0.0022(9) -0.0044(10) C12 0.0352(14) 0.0234(14) 0.0253(13) -0.0110(11) -0.0037(11) -0.0093(11) C13 0.0481(16) 0.0170(13) 0.0262(14) -0.0063(11) -0.0029(12) -0.0081(12) C14 0.0425(16) 0.0276(15) 0.0232(14) -0.0064(12) -0.0081(12) 0.0013(12) C15 0.0332(14) 0.0354(16) 0.0287(15) -0.0111(13) -0.0099(12) -0.0072(12) C16 0.0272(13) 0.0227(13) 0.0246(13) -0.0099(11) -0.0017(10) -0.0080(11) C21 0.0208(11) 0.0209(13) 0.0182(12) -0.0064(10) -0.0008(9) -0.0077(10) C22 0.0263(13) 0.0329(15) 0.0255(14) -0.0176(12) 0.0008(10) -0.0057(11) C23 0.0222(13) 0.0441(18) 0.0377(16) -0.0226(14) 0.0019(11) -0.0060(12) C24 0.0246(13) 0.0438(18) 0.0380(16) -0.0164(14) -0.0011(12) -0.0154(12) C25 0.0303(14) 0.0298(15) 0.0365(15) -0.0177(13) -0.0028(12) -0.0110(12) C26 0.0238(12) 0.0259(14) 0.0306(14) -0.0152(12) -0.0009(11) -0.0060(11) C31 0.0193(11) 0.0195(12) 0.0230(12) -0.0126(10) -0.0001(9) -0.0080(9) C32 0.0249(12) 0.0236(13) 0.0253(13) -0.0131(11) -0.0020(10) -0.0060(10) C33 0.0225(13) 0.0309(15) 0.0371(16) -0.0214(13) 0.0024(11) -0.0009(11) C34 0.0304(14) 0.0395(17) 0.0314(15) -0.0260(14) 0.0087(11) -0.0094(12) C35 0.0314(13) 0.0304(15) 0.0210(13) -0.0127(12) 0.0018(10) -0.0122(11) C36 0.0218(12) 0.0229(13) 0.0215(12) -0.0127(11) 0.0014(10) -0.0095(10) C37 0.0299(16) 0.058(2) 0.082(3) -0.037(2) -0.0176(16) -0.0010(15) C38 0.0378(18) 0.089(3) 0.089(3) -0.050(3) -0.0161(18) -0.0116(18) C39 0.076(2) 0.0389(19) 0.0313(17) -0.0068(15) -0.0003(16) -0.0252(17) C40 0.081(3) 0.084(3) 0.042(2) -0.020(2) 0.0058(18) -0.050(2) C51 0.061(2) 0.054(2) 0.042(2) -0.0230(18) -0.0010(16) -0.0158(18) C52 0.074(3) 0.139(5) 0.116(4) -0.097(4) 0.008(3) -0.008(3) C53 0.159(5) 0.099(4) 0.104(4) -0.033(3) -0.084(4) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 Cl1 2.3159(7) . ? Pt1 Cl1 2.3159(7) 2 ? Pt1 P2 2.3239(6) . ? Pt1 P2 2.3239(6) 2 ? P1 O1 1.4620(17) . ? P1 O2 1.5761(18) . ? P1 O3 1.5842(19) . ? P1 C36 1.804(2) . ? P2 C21 1.829(2) . ? P2 C11 1.835(2) . ? P2 C31 1.845(2) . ? O2 C37 1.463(3) . ? O3 C39 1.460(3) . ? O4 C51 1.194(4) . ? C11 C16 1.391(3) . ? C11 C12 1.394(3) . ? C12 C13 1.383(3) . ? C13 C14 1.375(4) . ? C14 C15 1.378(4) . ? C15 C16 1.378(3) . ? C21 C22 1.386(3) . ? C21 C26 1.393(3) . ? C22 C23 1.389(3) . ? C23 C24 1.376(4) . ? C24 C25 1.374(4) . ? C25 C26 1.393(3) . ? C31 C32 1.395(3) . ? C31 C36 1.419(3) . ? C32 C33 1.391(3) . ? C33 C34 1.380(4) . ? C34 C35 1.386(3) . ? C35 C36 1.395(3) . ? C37 C38 1.466(4) . ? C39 C40 1.482(4) . ? C51 C53 1.429(5) . ? C51 C52 1.510(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 Cl1 Pt1 Cl1 180.0 . 2 ? Cl1 Pt1 P2 91.91(2) . . ? Cl1 Pt1 P2 88.09(2) 2 . ? Cl1 Pt1 P2 88.09(2) . 2 ? Cl1 Pt1 P2 91.91(2) 2 2 ? P2 Pt1 P2 180.0 . 2 ? O1 P1 O2 116.47(10) . . ? O1 P1 O3 114.37(11) . . ? O2 P1 O3 100.85(10) . . ? O1 P1 C36 115.78(10) . . ? O2 P1 C36 101.14(10) . . ? O3 P1 C36 106.31(11) . . ? C21 P2 C11 103.40(10) . . ? C21 P2 C31 102.28(10) . . ? C11 P2 C31 103.90(10) . . ? C21 P2 Pt1 123.43(8) . . ? C11 P2 Pt1 107.59(8) . . ? C31 P2 Pt1 114.21(8) . . ? C37 O2 P1 119.13(17) . . ? C39 O3 P1 121.06(17) . . ? C16 C11 C12 118.3(2) . . ? C16 C11 P2 118.34(18) . . ? C12 C11 P2 123.29(18) . . ? C13 C12 C11 120.5(2) . . ? C14 C13 C12 120.1(2) . . ? C13 C14 C15 120.1(2) . . ? C16 C15 C14 120.0(2) . . ? C15 C16 C11 120.9(2) . . ? C22 C21 C26 118.7(2) . . ? C22 C21 P2 122.53(18) . . ? C26 C21 P2 118.78(17) . . ? C21 C22 C23 120.3(2) . . ? C24 C23 C22 120.4(2) . . ? C25 C24 C23 120.2(2) . . ? C24 C25 C26 119.8(2) . . ? C25 C26 C21 120.7(2) . . ? C32 C31 C36 118.1(2) . . ? C32 C31 P2 118.63(17) . . ? C36 C31 P2 123.23(17) . . ? C33 C32 C31 121.6(2) . . ? C34 C33 C32 120.2(2) . . ? C33 C34 C35 119.3(2) . . ? C34 C35 C36 121.7(2) . . ? C35 C36 C31 119.2(2) . . ? C35 C36 P1 116.38(18) . . ? C31 C36 P1 124.38(17) . . ? O2 C37 C38 109.3(3) . . ? O3 C39 C40 110.0(3) . . ? O4 C51 C53 123.4(4) . . ? O4 C51 C52 119.6(3) . . ? C53 C51 C52 116.9(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 Cl1 Pt1 P2 C21 -126.11(9) . . . . ? Cl1 Pt1 P2 C21 53.89(9) 2 . . . ? P2 Pt1 P2 C21 106(5) 2 . . . ? Cl1 Pt1 P2 C11 113.85(8) . . . . ? Cl1 Pt1 P2 C11 -66.15(8) 2 . . . ? P2 Pt1 P2 C11 -14(5) 2 . . . ? Cl1 Pt1 P2 C31 -0.92(8) . . . . ? Cl1 Pt1 P2 C31 179.08(8) 2 . . . ? P2 Pt1 P2 C31 -129(5) 2 . . . ? O1 P1 O2 C37 41.1(2) . . . . ? O3 P1 O2 C37 -83.3(2) . . . . ? C36 P1 O2 C37 167.5(2) . . . . ? O1 P1 O3 C39 40.0(2) . . . . ? O2 P1 O3 C39 165.8(2) . . . . ? C36 P1 O3 C39 -89.0(2) . . . . ? C21 P2 C11 C16 -149.99(19) . . . . ? C31 P2 C11 C16 103.49(19) . . . . ? Pt1 P2 C11 C16 -18.0(2) . . . . ? C21 P2 C11 C12 31.9(2) . . . . ? C31 P2 C11 C12 -74.6(2) . . . . ? Pt1 P2 C11 C12 163.98(18) . . . . ? C16 C11 C12 C13 -2.4(4) . . . . ? P2 C11 C12 C13 175.66(19) . . . . ? C11 C12 C13 C14 -0.3(4) . . . . ? C12 C13 C14 C15 2.3(4) . . . . ? C13 C14 C15 C16 -1.5(4) . . . . ? C14 C15 C16 C11 -1.2(4) . . . . ? C12 C11 C16 C15 3.1(4) . . . . ? P2 C11 C16 C15 -175.0(2) . . . . ? C11 P2 C21 C22 100.9(2) . . . . ? C31 P2 C21 C22 -151.3(2) . . . . ? Pt1 P2 C21 C22 -21.0(2) . . . . ? C11 P2 C21 C26 -79.0(2) . . . . ? C31 P2 C21 C26 28.7(2) . . . . ? Pt1 P2 C21 C26 159.03(16) . . . . ? C26 C21 C22 C23 0.4(4) . . . . ? P2 C21 C22 C23 -179.53(19) . . . . ? C21 C22 C23 C24 -1.5(4) . . . . ? C22 C23 C24 C25 1.7(4) . . . . ? C23 C24 C25 C26 -0.8(4) . . . . ? C24 C25 C26 C21 -0.2(4) . . . . ? C22 C21 C26 C25 0.4(4) . . . . ? P2 C21 C26 C25 -179.61(19) . . . . ? C21 P2 C31 C32 -119.28(19) . . . . ? C11 P2 C31 C32 -11.9(2) . . . . ? Pt1 P2 C31 C32 104.99(18) . . . . ? C21 P2 C31 C36 62.9(2) . . . . ? C11 P2 C31 C36 170.29(19) . . . . ? Pt1 P2 C31 C36 -72.8(2) . . . . ? C36 C31 C32 C33 0.1(3) . . . . ? P2 C31 C32 C33 -177.78(19) . . . . ? C31 C32 C33 C34 0.4(4) . . . . ? C32 C33 C34 C35 -0.3(4) . . . . ? C33 C34 C35 C36 -0.2(4) . . . . ? C34 C35 C36 C31 0.7(4) . . . . ? C34 C35 C36 P1 -177.47(19) . . . . ? C32 C31 C36 C35 -0.6(3) . . . . ? P2 C31 C36 C35 177.17(18) . . . . ? C32 C31 C36 P1 177.37(17) . . . . ? P2 C31 C36 P1 -4.8(3) . . . . ? O1 P1 C36 C35 -159.67(18) . . . . ? O2 P1 C36 C35 73.5(2) . . . . ? O3 P1 C36 C35 -31.4(2) . . . . ? O1 P1 C36 C31 22.3(2) . . . . ? O2 P1 C36 C31 -104.6(2) . . . . ? O3 P1 C36 C31 150.52(19) . . . . ? P1 O2 C37 C38 177.5(2) . . . . ? P1 O3 C39 C40 109.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.645 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.077