Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_msb102 _database_code_CSD 190092 _journal_coden_Cambridge 186 loop_ _publ_author_name 'Balakrishna Maravanji' 'Joel T. Mague' 'Rashmishree Panda' _publ_contact_author_name 'Prof Maravanji S Balakrishna' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Bombay Mumbai 400 076 INDIA ; _publ_contact_author_email 'KRISHNA@IITB.AC.IN' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; New bis(phosphinite) derived from bis(2-hydroxy-1-naphthyl)methane. Synthesis, derivatization and transition metal chemistry of Ph2P{(-OC10H6)( -CH2)(C10H6O-)}PPh2. The crystal and molecular structures of Ph2P(Se){(-OC10H6)( -CH2)(C10H6O-)}P(Se)Ph2, [CpRuCl{ 2-Ph2P{(-OC10H6)( -CH2)(C10H6O-)}PPh2}- P, P], and cis-[PtCl2{ 2-Ph2P{(-OC10H6)( -CH2)(C10H6O-)}PPh2}- P, P] ; _publ_section_references ; Bruker AXS (1997). SHELXTL Version 5.1, Madison, WI. Enraf-Nonius (1989). CAD-4 Operations Manual, Delft, The Netherlands. Harms, K. (1996). Program for the Lp-correction of CAD-4 Diffractometer Data. University of Marburg, Germany. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1997). SHELXL-97. Program for Crystal Structure Refinement. University of Gottingen, Gottingen, Germany. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H34 O2 P2 Se2' _chemical_formula_weight 826.58 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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 44.656(3) _cell_length_b 11.1275(9) _cell_length_c 15.5265(18) _cell_angle_alpha 90.00 _cell_angle_beta 99.753(8) _cell_angle_gamma 90.00 _cell_volume 7603.7(12) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18.60 _cell_measurement_theta_max 22.97 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 2.067 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3784 _exptl_absorpt_correction_T_max 0.4679 _exptl_absorpt_process_details '\y scans (North, et al., 1968)' _exptl_special_details ; The crystal used was affixed to a thin glass fibre with epoxy cement. General procedures for crystal alignment, unit cell determination and refinement and collection of intensity data have been published (Mague & Lloyd, 1988). ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 5.0 _diffrn_reflns_number 6871 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.09 _reflns_number_total 6778 _reflns_number_gt 4413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data-reduction 'XCAD4 (Harms, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker AXS, 1997)' _computing_publication_material 'SHELXTL (Bruker AXS, 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^)+(0.0529P)^2^+5.6129P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6778 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.003 _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 Se1 Se 0.223106(9) 0.40255(4) 0.23928(3) 0.06735(14) Uani 1 1 d . . . Se2 Se 0.045656(12) 0.92582(4) 0.38059(3) 0.08213(16) Uani 1 1 d . . . P1 P 0.189924(18) 0.32639(7) 0.30048(5) 0.04282(19) Uani 1 1 d . . . P2 P 0.055607(19) 0.76941(7) 0.45186(5) 0.0461(2) Uani 1 1 d . . . O1 O 0.15779(5) 0.39739(18) 0.29263(14) 0.0485(5) Uani 1 1 d . . . O2 O 0.08743(5) 0.70500(19) 0.44477(14) 0.0518(6) Uani 1 1 d . . . C1 C 0.17793(7) 0.1776(3) 0.26441(19) 0.0426(7) Uani 1 1 d . . . C2 C 0.14847(8) 0.1406(3) 0.2626(2) 0.0613(9) Uani 1 1 d . . . H2 H 0.1340 0.1957 0.2739 0.074 Uiso 1 1 calc R . . C3 C 0.14019(9) 0.0228(4) 0.2444(3) 0.0709(11) Uani 1 1 d . . . H3 H 0.1202 -0.0012 0.2433 0.085 Uiso 1 1 calc R . . C4 C 0.16148(10) -0.0594(3) 0.2279(2) 0.0665(10) Uani 1 1 d . . . H4 H 0.1560 -0.1391 0.2161 0.080 Uiso 1 1 calc R . . C5 C 0.19068(9) -0.0237(3) 0.2288(2) 0.0655(10) Uani 1 1 d . . . H5 H 0.2050 -0.0794 0.2173 0.079 Uiso 1 1 calc R . . C6 C 0.19934(8) 0.0948(3) 0.2468(2) 0.0546(8) Uani 1 1 d . . . H6 H 0.2193 0.1185 0.2470 0.065 Uiso 1 1 calc R . . C7 C 0.19930(7) 0.3186(3) 0.4180(2) 0.0452(7) Uani 1 1 d . . . C8 C 0.22353(9) 0.3818(3) 0.4629(2) 0.0677(10) Uani 1 1 d . . . H8 H 0.2355 0.4281 0.4323 0.081 Uiso 1 1 calc R . . C9 C 0.23014(11) 0.3770(4) 0.5530(3) 0.0816(13) Uani 1 1 d . . . H9 H 0.2468 0.4190 0.5826 0.098 Uiso 1 1 calc R . . C10 C 0.21239(11) 0.3109(4) 0.5989(3) 0.0754(12) Uani 1 1 d . . . H10 H 0.2166 0.3091 0.6596 0.091 Uiso 1 1 calc R . . C11 C 0.18855(11) 0.2480(4) 0.5549(3) 0.0830(13) Uani 1 1 d . . . H11 H 0.1766 0.2026 0.5862 0.100 Uiso 1 1 calc R . . C12 C 0.18175(9) 0.2499(4) 0.4650(2) 0.0709(11) Uani 1 1 d . . . H12 H 0.1655 0.2055 0.4359 0.085 Uiso 1 1 calc R . . C13 C 0.14417(7) 0.4773(3) 0.22877(18) 0.0392(7) Uani 1 1 d . . . C14 C 0.14660(8) 0.4605(3) 0.1407(2) 0.0528(8) Uani 1 1 d . . . H14 H 0.1577 0.3965 0.1239 0.063 Uiso 1 1 calc R . . C15 C 0.13262(9) 0.5385(4) 0.0810(2) 0.0628(10) Uani 1 1 d . . . H15 H 0.1348 0.5290 0.0229 0.075 Uiso 1 1 calc R . . C16 C 0.11484(8) 0.6341(3) 0.1034(2) 0.0549(8) Uani 1 1 d . . . C17 C 0.09963(10) 0.7156(4) 0.0407(2) 0.0790(12) Uani 1 1 d . . . H17 H 0.1019 0.7076 -0.0175 0.095 Uiso 1 1 calc R . . C18 C 0.08193(11) 0.8044(4) 0.0633(3) 0.0843(13) Uani 1 1 d . . . H18 H 0.0726 0.8582 0.0212 0.101 Uiso 1 1 calc R . . C19 C 0.07753(9) 0.8156(3) 0.1504(3) 0.0715(11) Uani 1 1 d . . . H19 H 0.0645 0.8743 0.1653 0.086 Uiso 1 1 calc R . . C20 C 0.09228(7) 0.7410(3) 0.2133(2) 0.0521(8) Uani 1 1 d . . . H20 H 0.0896 0.7509 0.2709 0.062 Uiso 1 1 calc R . . C21 C 0.11166(6) 0.6485(3) 0.19236(18) 0.0398(7) Uani 1 1 d . . . C22 C 0.12769(6) 0.5696(2) 0.25693(17) 0.0341(6) Uani 1 1 d . . . C23 C 0.12514(7) 0.5803(2) 0.35283(18) 0.0375(6) Uani 1 1 d . . . H23A H 0.1367 0.5148 0.3835 0.045 Uiso 1 1 calc R . . H23B H 0.1040 0.5673 0.3578 0.045 Uiso 1 1 calc R . . C24 C 0.13537(6) 0.6959(2) 0.40136(17) 0.0365(6) Uani 1 1 d . . . C25 C 0.16566(6) 0.7400(3) 0.40896(18) 0.0405(7) Uani 1 1 d . . . C26 C 0.18815(7) 0.6811(3) 0.3698(2) 0.0465(7) Uani 1 1 d . . . H26 H 0.1831 0.6117 0.3373 0.056 Uiso 1 1 calc R . . C27 C 0.21728(8) 0.7254(3) 0.3793(2) 0.0590(9) Uani 1 1 d . . . H27 H 0.2316 0.6857 0.3528 0.071 Uiso 1 1 calc R . . C28 C 0.22561(8) 0.8291(4) 0.4281(2) 0.0646(10) Uani 1 1 d . . . H28 H 0.2454 0.8578 0.4344 0.078 Uiso 1 1 calc R . . C29 C 0.20467(8) 0.8879(3) 0.4664(2) 0.0611(9) Uani 1 1 d . . . H29 H 0.2103 0.9572 0.4986 0.073 Uiso 1 1 calc R . . C30 C 0.17455(7) 0.8458(3) 0.45837(19) 0.0474(7) Uani 1 1 d . . . C31 C 0.15296(9) 0.9034(3) 0.5008(2) 0.0623(10) Uani 1 1 d . . . H31 H 0.1584 0.9731 0.5327 0.075 Uiso 1 1 calc R . . C32 C 0.12462(8) 0.8598(3) 0.4961(2) 0.0586(9) Uani 1 1 d . . . H32 H 0.1108 0.8977 0.5257 0.070 Uiso 1 1 calc R . . C33 C 0.11611(7) 0.7564(3) 0.44613(19) 0.0432(7) Uani 1 1 d . . . C34 C 0.05644(7) 0.7866(3) 0.5682(2) 0.0437(7) Uani 1 1 d . . . C35 C 0.03733(8) 0.8685(3) 0.5982(2) 0.0599(9) Uani 1 1 d . . . H35 H 0.0249 0.9178 0.5590 0.072 Uiso 1 1 calc R . . C36 C 0.03663(11) 0.8769(4) 0.6871(3) 0.0762(12) Uani 1 1 d . . . H36 H 0.0239 0.9326 0.7073 0.091 Uiso 1 1 calc R . . C37 C 0.05436(10) 0.8043(4) 0.7445(3) 0.0727(11) Uani 1 1 d . . . H37 H 0.0536 0.8098 0.8039 0.087 Uiso 1 1 calc R . . C38 C 0.07338(8) 0.7233(4) 0.7160(2) 0.0666(10) Uani 1 1 d . . . H38 H 0.0856 0.6743 0.7559 0.080 Uiso 1 1 calc R . . C39 C 0.07447(8) 0.7142(3) 0.6273(2) 0.0578(9) Uani 1 1 d . . . H39 H 0.0874 0.6589 0.6079 0.069 Uiso 1 1 calc R . . C40 C 0.03121(7) 0.6435(3) 0.4177(2) 0.0492(8) Uani 1 1 d . . . C41 C 0.04087(9) 0.5276(3) 0.4401(2) 0.0619(9) Uani 1 1 d . . . H41 H 0.0600 0.5154 0.4735 0.074 Uiso 1 1 calc R . . C42 C 0.02255(10) 0.4301(4) 0.4138(3) 0.0736(11) Uani 1 1 d . . . H42 H 0.0294 0.3526 0.4285 0.088 Uiso 1 1 calc R . . C43 C -0.00541(11) 0.4478(5) 0.3663(3) 0.0826(13) Uani 1 1 d . . . H43 H -0.0176 0.3819 0.3478 0.099 Uiso 1 1 calc R . . C44 C -0.01590(10) 0.5604(5) 0.3453(3) 0.0945(15) Uani 1 1 d . . . H44 H -0.0354 0.5712 0.3138 0.113 Uiso 1 1 calc R . . C45 C 0.00248(9) 0.6599(4) 0.3710(3) 0.0741(11) Uani 1 1 d . . . H45 H -0.0047 0.7370 0.3566 0.089 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 Se1 0.0649(2) 0.0682(3) 0.0764(3) 0.0086(2) 0.0334(2) -0.0065(2) Se2 0.1196(4) 0.0554(2) 0.0706(3) 0.01201(19) 0.0138(3) 0.0034(2) P1 0.0465(4) 0.0376(4) 0.0468(4) 0.0013(3) 0.0150(4) 0.0025(4) P2 0.0511(5) 0.0444(4) 0.0458(5) -0.0057(4) 0.0171(4) -0.0028(4) O1 0.0580(14) 0.0409(11) 0.0509(12) 0.0092(9) 0.0217(10) 0.0130(10) O2 0.0490(12) 0.0491(12) 0.0640(14) -0.0154(10) 0.0286(11) -0.0077(10) C1 0.0483(18) 0.0377(16) 0.0414(16) -0.0008(13) 0.0064(13) 0.0053(14) C2 0.054(2) 0.054(2) 0.076(2) -0.0113(18) 0.0141(18) 0.0023(17) C3 0.071(3) 0.062(2) 0.083(3) -0.013(2) 0.020(2) -0.018(2) C4 0.097(3) 0.045(2) 0.057(2) -0.0093(17) 0.011(2) -0.012(2) C5 0.079(3) 0.050(2) 0.065(2) -0.0127(18) 0.007(2) 0.018(2) C6 0.0505(19) 0.054(2) 0.057(2) -0.0093(16) 0.0041(16) 0.0066(16) C7 0.0525(19) 0.0368(15) 0.0464(17) -0.0028(14) 0.0081(15) 0.0035(15) C8 0.080(3) 0.059(2) 0.061(2) 0.0015(18) 0.005(2) -0.017(2) C9 0.105(3) 0.064(2) 0.067(3) -0.008(2) -0.011(2) -0.017(2) C10 0.118(4) 0.059(2) 0.046(2) -0.0044(18) 0.003(2) 0.005(2) C11 0.104(3) 0.088(3) 0.059(3) 0.016(2) 0.021(2) -0.019(3) C12 0.075(3) 0.087(3) 0.051(2) 0.0054(19) 0.0117(19) -0.025(2) C13 0.0440(16) 0.0352(15) 0.0383(16) 0.0004(12) 0.0070(13) -0.0012(13) C14 0.065(2) 0.0536(19) 0.0418(18) -0.0142(16) 0.0149(16) 0.0018(17) C15 0.082(3) 0.078(2) 0.0292(17) -0.0072(17) 0.0110(17) 0.002(2) C16 0.067(2) 0.057(2) 0.0361(17) 0.0054(15) -0.0024(15) -0.0039(18) C17 0.099(3) 0.089(3) 0.043(2) 0.015(2) -0.007(2) 0.005(3) C18 0.094(3) 0.072(3) 0.075(3) 0.028(2) -0.020(2) 0.012(2) C19 0.079(3) 0.051(2) 0.076(3) 0.004(2) -0.010(2) 0.010(2) C20 0.0532(19) 0.0422(17) 0.057(2) -0.0022(15) -0.0026(16) 0.0034(15) C21 0.0411(16) 0.0362(15) 0.0388(16) -0.0008(13) -0.0026(12) -0.0060(13) C22 0.0381(15) 0.0302(14) 0.0342(14) -0.0029(12) 0.0067(12) -0.0052(12) C23 0.0428(16) 0.0351(15) 0.0363(15) 0.0015(12) 0.0117(12) -0.0010(13) C24 0.0430(16) 0.0384(15) 0.0286(14) -0.0006(12) 0.0072(12) -0.0025(13) C25 0.0414(16) 0.0468(17) 0.0326(15) 0.0036(13) 0.0039(12) -0.0042(14) C26 0.0442(18) 0.0488(18) 0.0469(18) -0.0007(14) 0.0084(14) -0.0021(15) C27 0.0436(19) 0.064(2) 0.071(2) 0.0053(19) 0.0138(17) -0.0008(17) C28 0.045(2) 0.074(3) 0.072(2) 0.006(2) 0.0023(17) -0.0192(19) C29 0.063(2) 0.062(2) 0.057(2) -0.0085(17) 0.0071(18) -0.0203(19) C30 0.0484(18) 0.0540(19) 0.0394(17) -0.0032(15) 0.0063(14) -0.0116(16) C31 0.074(2) 0.058(2) 0.056(2) -0.0266(17) 0.0140(18) -0.0234(19) C32 0.065(2) 0.060(2) 0.057(2) -0.0243(17) 0.0271(17) -0.0133(18) C33 0.0459(17) 0.0448(17) 0.0415(17) -0.0041(13) 0.0146(14) -0.0102(14) C34 0.0437(17) 0.0427(17) 0.0471(18) -0.0124(14) 0.0144(14) -0.0069(14) C35 0.071(2) 0.0483(19) 0.065(2) -0.0083(17) 0.0251(18) 0.0020(18) C36 0.102(3) 0.064(2) 0.073(3) -0.027(2) 0.045(3) -0.009(2) C37 0.092(3) 0.078(3) 0.053(2) -0.022(2) 0.025(2) -0.031(2) C38 0.061(2) 0.087(3) 0.049(2) -0.003(2) 0.0022(17) -0.015(2) C39 0.0454(19) 0.070(2) 0.059(2) -0.0103(18) 0.0130(16) -0.0005(18) C40 0.0481(19) 0.056(2) 0.0470(18) -0.0122(15) 0.0173(15) -0.0059(16) C41 0.061(2) 0.056(2) 0.070(2) -0.0084(18) 0.0148(18) -0.0098(19) C42 0.078(3) 0.057(2) 0.091(3) -0.015(2) 0.027(2) -0.023(2) C43 0.081(3) 0.085(3) 0.086(3) -0.025(3) 0.026(3) -0.039(3) C44 0.057(3) 0.129(5) 0.094(3) -0.018(3) 0.002(2) -0.033(3) C45 0.061(2) 0.082(3) 0.079(3) -0.010(2) 0.009(2) -0.001(2) _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 Se1 P1 2.0722(8) . ? Se2 P2 2.0699(10) . ? P1 O1 1.624(2) . ? P1 C1 1.800(3) . ? P1 C7 1.804(3) . ? P2 O2 1.612(2) . ? P2 C40 1.799(3) . ? P2 C34 1.811(3) . ? O1 C13 1.393(3) . ? O2 C33 1.399(3) . ? C1 C2 1.374(4) . ? C1 C6 1.388(4) . ? C2 C3 1.378(5) . ? C3 C4 1.374(5) . ? C4 C5 1.361(5) . ? C5 C6 1.390(5) . ? C7 C8 1.377(5) . ? C7 C12 1.386(5) . ? C8 C9 1.381(5) . ? C9 C10 1.367(6) . ? C10 C11 1.358(6) . ? C11 C12 1.379(5) . ? C13 C22 1.377(4) . ? C13 C14 1.403(4) . ? C14 C15 1.344(5) . ? C15 C16 1.406(5) . ? C16 C17 1.417(5) . ? C16 C21 1.421(4) . ? C17 C18 1.349(6) . ? C18 C19 1.406(6) . ? C19 C20 1.363(5) . ? C20 C21 1.417(4) . ? C21 C22 1.430(4) . ? C22 C23 1.517(4) . ? C23 C24 1.522(4) . ? C24 C33 1.371(4) . ? C24 C25 1.425(4) . ? C25 C26 1.419(4) . ? C25 C30 1.425(4) . ? C26 C27 1.375(4) . ? C27 C28 1.396(5) . ? C28 C29 1.358(5) . ? C29 C30 1.409(5) . ? C30 C31 1.411(5) . ? C31 C32 1.346(5) . ? C32 C33 1.404(4) . ? C34 C39 1.374(5) . ? C34 C35 1.382(4) . ? C35 C36 1.389(5) . ? C36 C37 1.354(6) . ? C37 C38 1.362(6) . ? C38 C39 1.391(5) . ? C40 C45 1.375(5) . ? C40 C41 1.385(5) . ? C41 C42 1.378(5) . ? C42 C43 1.352(6) . ? C43 C44 1.358(7) . ? C44 C45 1.396(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 C1 102.21(13) . . ? O1 P1 C7 98.62(13) . . ? C1 P1 C7 106.04(14) . . ? O1 P1 Se1 117.25(8) . . ? C1 P1 Se1 115.57(10) . . ? C7 P1 Se1 114.98(11) . . ? O2 P2 C40 97.50(13) . . ? O2 P2 C34 104.22(13) . . ? C40 P2 C34 106.57(14) . . ? O2 P2 Se2 116.69(9) . . ? C40 P2 Se2 115.67(12) . . ? C34 P2 Se2 114.26(10) . . ? C13 O1 P1 129.63(18) . . ? C33 O2 P2 129.23(19) . . ? C2 C1 C6 119.1(3) . . ? C2 C1 P1 121.0(2) . . ? C6 C1 P1 119.5(2) . . ? C1 C2 C3 120.8(3) . . ? C4 C3 C2 120.1(4) . . ? C5 C4 C3 119.7(3) . . ? C4 C5 C6 120.8(3) . . ? C1 C6 C5 119.5(3) . . ? C8 C7 C12 118.8(3) . . ? C8 C7 P1 121.0(3) . . ? C12 C7 P1 120.2(3) . . ? C7 C8 C9 120.5(4) . . ? C10 C9 C8 120.3(4) . . ? C11 C10 C9 119.3(4) . . ? C10 C11 C12 121.4(4) . . ? C11 C12 C7 119.6(4) . . ? C22 C13 O1 116.3(2) . . ? C22 C13 C14 122.9(3) . . ? O1 C13 C14 120.8(3) . . ? C15 C14 C13 118.9(3) . . ? C14 C15 C16 122.2(3) . . ? C15 C16 C17 122.6(3) . . ? C15 C16 C21 118.7(3) . . ? C17 C16 C21 118.8(3) . . ? C18 C17 C16 121.5(4) . . ? C17 C18 C19 120.0(4) . . ? C20 C19 C18 120.4(4) . . ? C19 C20 C21 121.2(3) . . ? C20 C21 C16 118.0(3) . . ? C20 C21 C22 122.5(3) . . ? C16 C21 C22 119.4(3) . . ? C13 C22 C21 117.8(2) . . ? C13 C22 C23 120.2(2) . . ? C21 C22 C23 121.9(2) . . ? C22 C23 C24 119.1(2) . . ? C33 C24 C25 117.2(3) . . ? C33 C24 C23 120.3(2) . . ? C25 C24 C23 122.2(2) . . ? C26 C25 C30 117.3(3) . . ? C26 C25 C24 122.5(3) . . ? C30 C25 C24 120.2(3) . . ? C27 C26 C25 121.0(3) . . ? C26 C27 C28 120.9(3) . . ? C29 C28 C27 119.8(3) . . ? C28 C29 C30 121.2(3) . . ? C29 C30 C31 121.7(3) . . ? C29 C30 C25 119.8(3) . . ? C31 C30 C25 118.5(3) . . ? C32 C31 C30 121.4(3) . . ? C31 C32 C33 119.3(3) . . ? C24 C33 O2 116.3(3) . . ? C24 C33 C32 123.3(3) . . ? O2 C33 C32 120.3(3) . . ? C39 C34 C35 119.1(3) . . ? C39 C34 P2 121.0(2) . . ? C35 C34 P2 119.8(3) . . ? C34 C35 C36 119.9(4) . . ? C37 C36 C35 120.3(4) . . ? C36 C37 C38 120.5(4) . . ? C37 C38 C39 119.9(4) . . ? C34 C39 C38 120.2(3) . . ? C45 C40 C41 118.6(3) . . ? C45 C40 P2 121.1(3) . . ? C41 C40 P2 120.3(3) . . ? C42 C41 C40 120.9(4) . . ? C43 C42 C41 119.6(4) . . ? C42 C43 C44 121.0(4) . . ? C43 C44 C45 120.1(4) . . ? C40 C45 C44 119.7(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 Se1 P1 O1 C13 25.2(3) . . . . ? P1 O1 C13 C22 -145.5(2) . . . . ? O1 C13 C22 C23 0.1(4) . . . . ? C13 C22 C23 C24 123.0(3) . . . . ? C22 C23 C24 C33 126.5(3) . . . . ? C23 C24 C33 O2 0.7(4) . . . . ? C24 C33 O2 P2 -151.3(2) . . . . ? C33 O2 P2 Se2 42.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.464 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.055 data_msb111 _database_code_CSD 190093 _journal_coden_Cambridge 186 loop_ _publ_author_name 'Balakrishna Maravanji' 'Joel T. Mague' 'Rashmishree Panda' _publ_contact_author_name 'Prof Maravanji S Balakrishna' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Bombay Mumbai 400 076 INDIA ; _publ_contact_author_email 'KRISHNA@IITB.AC.IN' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; New bis(phosphinite) derived from bis(2-hydroxy-1-naphthyl)methane. Synthesis, derivatization and transition metal chemistry of Ph2P{(-OC10H6)( -CH2)(C10H6O-)}PPh2. The crystal and molecular structures of Ph2P(Se){(-OC10H6)( -CH2)(C10H6O-)}P(Se)Ph2, [CpRuCl{ 2-Ph2P{(-OC10H6)( -CH2)(C10H6O-)}PPh2}- P, P], and cis-[PtCl2{ 2-Ph2P{(-OC10H6)( -CH2)(C10H6O-)}PPh2}- P, P] ; _publ_section_references ; Bruker AXS (1997). SHELXTL Version 5.1, Madison, WI. Enraf-Nonius (1989). CAD-4 Operations Manual, Delft, The Netherlands. Harms, K. (1996). Program for the Lp-correction of CAD-4 Diffractometer Data. University of Marburg, Germany. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1997). SHELXL-97. Program for Crystal Structure Refinement. University of Gottingen, Gottingen, Germany. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H42 Cl3 O2.50 P2 Ru' _chemical_formula_weight 964.21 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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 41.312(2) _cell_length_b 12.8234(17) _cell_length_c 22.770(2) _cell_angle_alpha 90.00 _cell_angle_beta 122.897(8) _cell_angle_gamma 90.00 _cell_volume 10128.4(18) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 19.03 _cell_measurement_theta_max 23.10 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3944 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7942 _exptl_absorpt_correction_T_max 0.9056 _exptl_absorpt_process_details '\y scans (North, et al., 1968)' _exptl_special_details ; A large crystal was cut to size and mounted on a thin glass fiber with a coat of epoxy cement. General procedures for cyrstal alignment, unit cell determination and refinement and collection of intensity data have been published (Mague & Lloyd, 1988). ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enray-Nonius CAD-4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 11 _diffrn_reflns_number 9164 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.1125 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.13 _reflns_number_total 9030 _reflns_number_gt 5018 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data-reduction 'XCAD4 (Harms, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker AXS, 1997)' _computing_publication_material 'SHELXTL (Bruker AXS, 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^)+(0.1590P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00035(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9030 _refine_ls_number_parameters 569 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1585 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.2354 _refine_ls_wR_factor_gt 0.1947 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.033 _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 Ru Ru 0.657297(16) 0.93365(4) 0.78760(3) 0.0370(2) Uani 1 1 d . . . Cl Cl 0.72029(5) 0.92330(16) 0.80397(11) 0.0562(5) Uani 1 1 d . . . P1 P 0.63633(5) 0.77882(13) 0.73267(9) 0.0329(4) Uani 1 1 d . . . P2 P 0.63544(5) 1.02362(14) 0.68781(10) 0.0366(4) Uani 1 1 d . . . O1 O 0.60713(12) 0.7884(3) 0.6478(2) 0.0378(10) Uani 1 1 d . . . O2 O 0.58918(13) 1.0300(4) 0.6268(2) 0.0431(11) Uani 1 1 d . . . C1 C 0.67446(19) 0.6907(5) 0.7476(4) 0.0414(16) Uani 1 1 d . . . C2 C 0.7032(2) 0.6699(6) 0.8168(4) 0.0545(19) Uani 1 1 d . . . H2 H 0.7012 0.6978 0.8524 0.065 Uiso 1 1 calc R . . C3 C 0.7353(2) 0.6069(7) 0.8341(5) 0.067(2) Uani 1 1 d . . . H3 H 0.7535 0.5894 0.8803 0.080 Uiso 1 1 calc R . . C4 C 0.7392(3) 0.5718(7) 0.7809(7) 0.076(3) Uani 1 1 d . . . H4 H 0.7605 0.5319 0.7916 0.091 Uiso 1 1 calc R . . C5 C 0.7112(3) 0.5959(6) 0.7110(6) 0.068(3) Uani 1 1 d . . . H5 H 0.7141 0.5723 0.6754 0.081 Uiso 1 1 calc R . . C6 C 0.6794(2) 0.6549(6) 0.6950(4) 0.0502(18) Uani 1 1 d . . . H6 H 0.6610 0.6708 0.6486 0.060 Uiso 1 1 calc R . . C7 C 0.60718(19) 0.7038(5) 0.7556(4) 0.0394(15) Uani 1 1 d . . . C8 C 0.6201(2) 0.6161(7) 0.7985(5) 0.063(2) Uani 1 1 d . . . H8 H 0.6438 0.5861 0.8130 0.075 Uiso 1 1 calc R . . C9 C 0.5964(3) 0.5737(8) 0.8196(5) 0.079(3) Uani 1 1 d . . . H9 H 0.6053 0.5172 0.8501 0.095 Uiso 1 1 calc R . . C10 C 0.5610(3) 0.6131(8) 0.7965(5) 0.069(3) Uani 1 1 d . . . H10 H 0.5460 0.5846 0.8115 0.083 Uiso 1 1 calc R . . C11 C 0.5478(2) 0.6943(7) 0.7517(5) 0.063(2) Uani 1 1 d . . . H11 H 0.5229 0.7186 0.7337 0.075 Uiso 1 1 calc R . . C12 C 0.5707(2) 0.7422(6) 0.7319(4) 0.0521(19) Uani 1 1 d . . . H12 H 0.5614 0.8002 0.7028 0.062 Uiso 1 1 calc R . . C13 C 0.58226(19) 0.7142(5) 0.5964(4) 0.0377(15) Uani 1 1 d . . . C14 C 0.5890(2) 0.6071(5) 0.6093(4) 0.0461(17) Uani 1 1 d . . . H14 H 0.6082 0.5819 0.6529 0.055 Uiso 1 1 calc R . . C15 C 0.5664(3) 0.5424(6) 0.5558(4) 0.059(2) Uani 1 1 d . . . H15 H 0.5704 0.4709 0.5632 0.071 Uiso 1 1 calc R . . C16 C 0.5372(2) 0.5770(6) 0.4897(4) 0.055(2) Uani 1 1 d . . . C17 C 0.5145(3) 0.5073(8) 0.4328(6) 0.083(3) Uani 1 1 d . . . H17 H 0.5187 0.4358 0.4399 0.100 Uiso 1 1 calc R . . C18 C 0.4875(3) 0.5426(9) 0.3699(5) 0.089(3) Uani 1 1 d . . . H18 H 0.4733 0.4959 0.3333 0.107 Uiso 1 1 calc R . . C19 C 0.4804(3) 0.6479(9) 0.3585(5) 0.080(3) Uani 1 1 d . . . H19 H 0.4610 0.6713 0.3145 0.096 Uiso 1 1 calc R . . C20 C 0.5014(2) 0.7190(7) 0.4110(4) 0.063(2) Uani 1 1 d . . . H20 H 0.4967 0.7899 0.4016 0.076 Uiso 1 1 calc R . . C21 C 0.5302(2) 0.6853(6) 0.4791(4) 0.0479(18) Uani 1 1 d . . . C22 C 0.55279(19) 0.7561(5) 0.5353(3) 0.0385(15) Uani 1 1 d . . . C23 C 0.5448(2) 0.8726(5) 0.5283(4) 0.0421(16) Uani 1 1 d . . . H23A H 0.5235 0.8871 0.4810 0.051 Uiso 1 1 calc R . . H23B H 0.5673 0.9087 0.5352 0.051 Uiso 1 1 calc R . . C24 C 0.53522(19) 0.9172(5) 0.5795(4) 0.0385(16) Uani 1 1 d . . . C25 C 0.5016(2) 0.8825(6) 0.5775(4) 0.0445(17) Uani 1 1 d . . . C26 C 0.4750(2) 0.8106(6) 0.5278(5) 0.058(2) Uani 1 1 d . . . H26 H 0.4783 0.7851 0.4932 0.070 Uiso 1 1 calc R . . C27 C 0.4436(2) 0.7776(8) 0.5307(6) 0.073(3) Uani 1 1 d . . . H27 H 0.4263 0.7297 0.4980 0.088 Uiso 1 1 calc R . . C28 C 0.4377(3) 0.8149(9) 0.5814(6) 0.078(3) Uani 1 1 d . . . H28 H 0.4174 0.7892 0.5840 0.093 Uiso 1 1 calc R . . C29 C 0.4610(3) 0.8874(9) 0.6261(5) 0.072(3) Uani 1 1 d . . . H29 H 0.4555 0.9149 0.6576 0.087 Uiso 1 1 calc R . . C30 C 0.4939(2) 0.9251(6) 0.6279(4) 0.055(2) Uani 1 1 d . . . C31 C 0.5186(3) 1.0022(7) 0.6747(4) 0.059(2) Uani 1 1 d . . . H31 H 0.5137 1.0309 0.7067 0.071 Uiso 1 1 calc R . . C32 C 0.5499(2) 1.0354(6) 0.6738(4) 0.0461(17) Uani 1 1 d . . . H32 H 0.5656 1.0881 0.7039 0.055 Uiso 1 1 calc R . . C33 C 0.55833(19) 0.9906(5) 0.6280(4) 0.0390(16) Uani 1 1 d . . . C34 C 0.6456(2) 1.1617(5) 0.7038(4) 0.0441(17) Uani 1 1 d . . . C35 C 0.6835(2) 1.1948(7) 0.7418(5) 0.071(3) Uani 1 1 d . . . H35 H 0.7032 1.1464 0.7563 0.085 Uiso 1 1 calc R . . C36 C 0.6926(3) 1.2991(8) 0.7586(6) 0.094(4) Uani 1 1 d . . . H36 H 0.7182 1.3202 0.7835 0.112 Uiso 1 1 calc R . . C37 C 0.6647(3) 1.3699(7) 0.7391(6) 0.083(3) Uani 1 1 d . . . H37 H 0.6713 1.4395 0.7510 0.099 Uiso 1 1 calc R . . C38 C 0.6267(3) 1.3416(7) 0.7022(6) 0.081(3) Uani 1 1 d . . . H38 H 0.6073 1.3906 0.6895 0.097 Uiso 1 1 calc R . . C39 C 0.6178(3) 1.2358(6) 0.6839(5) 0.060(2) Uani 1 1 d . . . H39 H 0.5920 1.2157 0.6573 0.072 Uiso 1 1 calc R . . C40 C 0.6513(2) 0.9951(5) 0.6292(4) 0.0404(16) Uani 1 1 d . . . C41 C 0.6418(3) 1.0643(8) 0.5740(5) 0.073(3) Uani 1 1 d . . . H41 H 0.6286 1.1257 0.5692 0.087 Uiso 1 1 calc R . . C42 C 0.6519(4) 1.0414(10) 0.5274(6) 0.094(4) Uani 1 1 d . . . H42 H 0.6454 1.0873 0.4910 0.113 Uiso 1 1 calc R . . C43 C 0.6719(3) 0.9498(8) 0.5339(5) 0.071(3) Uani 1 1 d . . . H43 H 0.6786 0.9341 0.5019 0.085 Uiso 1 1 calc R . . C44 C 0.6813(3) 0.8856(7) 0.5865(5) 0.065(2) Uani 1 1 d . . . H44 H 0.6950 0.8253 0.5916 0.078 Uiso 1 1 calc R . . C45 C 0.6710(2) 0.9061(6) 0.6345(4) 0.0487(18) Uani 1 1 d . . . H45 H 0.6776 0.8590 0.6704 0.058 Uiso 1 1 calc R . . C46 C 0.6527(3) 0.8875(7) 0.8772(4) 0.064(2) Uani 1 1 d . . . H46 H 0.6500 0.8192 0.8877 0.077 Uiso 1 1 calc R . . C47 C 0.6874(3) 0.9390(8) 0.9034(4) 0.068(3) Uani 1 1 d . . . H47 H 0.7119 0.9111 0.9329 0.082 Uiso 1 1 calc R . . C48 C 0.6785(3) 1.0429(7) 0.8766(4) 0.067(3) Uani 1 1 d . . . H48 H 0.6963 1.0953 0.8865 0.081 Uiso 1 1 calc R . . C49 C 0.6383(3) 1.0529(7) 0.8328(5) 0.069(3) Uani 1 1 d . . . H49 H 0.6247 1.1126 0.8088 0.082 Uiso 1 1 calc R . . C50 C 0.6220(3) 0.9546(7) 0.8320(4) 0.061(2) Uani 1 1 d . . . H50 H 0.5960 0.9378 0.8064 0.073 Uiso 1 1 calc R . . Cl1S Cl 0.2971(3) 0.6858(8) 0.4916(4) 0.153(4) Uani 0.50 1 d P . . Cl2S Cl 0.3517(2) 0.6099(8) 0.4595(5) 0.158(4) Uani 0.50 1 d P . . C1S C 0.3095(9) 0.670(3) 0.439(2) 0.19(2) Uani 0.50 1 d P . . Cl3S Cl 0.5580(3) 1.2058(9) 0.8265(5) 0.171(4) Uani 0.50 1 d PD . . C2SA C 0.5879(14) 1.194(3) 0.9181(12) 0.101(9) Uiso 0.25 1 d PD A 1 Cl4A Cl 0.6100(6) 1.3215(13) 0.9473(11) 0.150(5) Uani 0.25 1 d PD A 1 C2SB C 0.5909(10) 1.232(4) 0.9159(15) 0.101(9) Uiso 0.25 1 d PD A 2 Cl4B Cl 0.6272(6) 1.3004(13) 0.9132(11) 0.150(5) Uani 0.25 1 d PD A 2 O1S O 0.7141(10) 0.445(3) 0.9421(18) 0.106(10) Uiso 0.25 1 d P . . O2S O 0.7582(10) 1.239(3) 0.9749(18) 0.113(11) Uiso 0.25 1 d P . . 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 Ru 0.0428(3) 0.0374(3) 0.0336(3) 0.0001(3) 0.0226(3) 0.0000(3) Cl 0.0409(10) 0.0655(13) 0.0580(12) 0.0032(10) 0.0241(9) -0.0045(9) P1 0.0333(9) 0.0328(9) 0.0346(9) 0.0034(7) 0.0197(8) 0.0036(7) P2 0.0410(10) 0.0336(9) 0.0398(10) 0.0022(8) 0.0249(9) 0.0002(8) O1 0.036(2) 0.034(2) 0.036(2) 0.004(2) 0.015(2) 0.003(2) O2 0.040(3) 0.040(3) 0.045(3) 0.003(2) 0.020(2) -0.002(2) C1 0.034(4) 0.040(4) 0.054(4) 0.001(3) 0.027(4) 0.003(3) C2 0.042(4) 0.053(5) 0.058(5) 0.008(4) 0.020(4) 0.013(4) C3 0.042(5) 0.060(5) 0.077(6) 0.021(5) 0.018(5) 0.012(4) C4 0.059(6) 0.056(5) 0.124(9) 0.009(6) 0.057(6) 0.016(5) C5 0.078(6) 0.048(5) 0.112(8) 0.000(5) 0.074(7) 0.010(4) C6 0.051(5) 0.046(4) 0.060(5) -0.006(4) 0.034(4) -0.003(4) C7 0.039(4) 0.040(4) 0.040(4) 0.004(3) 0.022(3) -0.002(3) C8 0.056(5) 0.061(5) 0.073(6) 0.026(5) 0.036(5) 0.005(4) C9 0.083(7) 0.083(7) 0.072(6) 0.028(5) 0.043(6) -0.010(6) C10 0.076(6) 0.079(6) 0.077(6) -0.001(5) 0.057(6) -0.025(5) C11 0.051(5) 0.070(6) 0.086(6) -0.003(5) 0.049(5) -0.007(4) C12 0.047(4) 0.055(5) 0.060(5) 0.008(4) 0.033(4) 0.005(4) C13 0.036(4) 0.034(3) 0.046(4) -0.001(3) 0.024(3) 0.003(3) C14 0.049(4) 0.034(4) 0.046(4) 0.002(3) 0.019(4) 0.000(3) C15 0.069(6) 0.036(4) 0.063(6) -0.006(4) 0.029(5) -0.003(4) C16 0.050(5) 0.048(5) 0.051(5) -0.005(4) 0.017(4) -0.004(4) C17 0.086(8) 0.060(6) 0.077(7) -0.023(5) 0.026(6) -0.010(5) C18 0.086(8) 0.080(8) 0.058(6) -0.029(5) 0.011(6) -0.013(6) C19 0.077(7) 0.089(8) 0.042(5) -0.012(5) 0.011(5) 0.003(6) C20 0.061(5) 0.059(5) 0.044(5) 0.001(4) 0.012(4) 0.005(4) C21 0.043(4) 0.055(5) 0.044(4) -0.002(4) 0.022(4) 0.001(4) C22 0.038(4) 0.044(4) 0.035(4) 0.001(3) 0.021(3) -0.002(3) C23 0.042(4) 0.041(4) 0.039(4) 0.006(3) 0.019(3) 0.007(3) C24 0.033(3) 0.040(4) 0.040(4) 0.010(3) 0.018(3) 0.007(3) C25 0.040(4) 0.040(4) 0.056(4) 0.013(3) 0.028(4) 0.008(3) C26 0.038(4) 0.060(5) 0.063(5) 0.008(4) 0.019(4) 0.003(4) C27 0.039(5) 0.069(6) 0.092(7) 0.003(5) 0.023(5) -0.007(4) C28 0.041(5) 0.090(7) 0.102(8) 0.023(6) 0.039(5) -0.004(5) C29 0.056(6) 0.098(7) 0.086(7) 0.020(6) 0.053(6) 0.013(5) C30 0.042(4) 0.056(5) 0.065(5) 0.020(4) 0.029(4) 0.016(4) C31 0.068(6) 0.068(6) 0.052(5) 0.008(4) 0.040(5) 0.019(5) C32 0.047(4) 0.041(4) 0.050(4) 0.001(3) 0.025(4) 0.005(3) C33 0.034(4) 0.037(4) 0.048(4) 0.012(3) 0.024(4) 0.010(3) C34 0.050(4) 0.032(4) 0.054(4) 0.004(3) 0.031(4) -0.001(3) C35 0.048(5) 0.048(5) 0.101(7) -0.007(5) 0.030(5) -0.005(4) C36 0.063(6) 0.062(6) 0.126(10) -0.012(6) 0.032(7) -0.020(5) C37 0.078(7) 0.039(5) 0.117(9) -0.006(5) 0.044(7) -0.009(5) C38 0.099(8) 0.033(4) 0.109(8) 0.004(5) 0.056(7) 0.003(5) C39 0.060(5) 0.043(4) 0.068(6) 0.006(4) 0.028(5) -0.006(4) C40 0.046(4) 0.044(4) 0.040(4) 0.005(3) 0.028(4) 0.003(3) C41 0.089(7) 0.080(6) 0.066(6) 0.021(5) 0.053(6) 0.024(5) C42 0.126(10) 0.119(9) 0.074(7) 0.047(6) 0.078(7) 0.033(8) C43 0.087(7) 0.097(7) 0.048(5) 0.004(5) 0.051(5) 0.011(6) C44 0.081(6) 0.062(5) 0.077(6) -0.014(5) 0.059(6) 0.002(5) C45 0.060(5) 0.049(4) 0.049(4) 0.000(3) 0.037(4) -0.009(4) C46 0.103(7) 0.061(5) 0.048(5) 0.005(4) 0.053(5) 0.006(5) C47 0.083(7) 0.087(7) 0.037(4) -0.009(5) 0.035(5) 0.006(6) C48 0.087(7) 0.073(6) 0.048(5) -0.029(5) 0.040(5) -0.024(5) C49 0.102(8) 0.063(6) 0.069(6) -0.006(5) 0.065(6) 0.010(5) C50 0.073(6) 0.082(6) 0.048(5) 0.000(4) 0.046(5) 0.008(5) Cl1S 0.162(8) 0.167(8) 0.080(4) -0.073(5) 0.033(5) -0.042(6) Cl2S 0.064(4) 0.197(9) 0.168(8) 0.019(7) 0.034(5) -0.022(5) C1S 0.09(2) 0.13(3) 0.18(3) 0.06(3) -0.03(2) -0.064(19) Cl3S 0.155(8) 0.223(11) 0.164(8) -0.045(7) 0.106(7) 0.029(7) Cl4A 0.151(11) 0.121(8) 0.204(14) 0.045(9) 0.113(10) 0.019(8) Cl4B 0.151(11) 0.121(8) 0.204(14) 0.045(9) 0.113(10) 0.019(8) _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 Ru C50 2.196(7) . ? Ru C49 2.213(8) . ? Ru C48 2.216(8) . ? Ru C47 2.223(8) . ? Ru C46 2.230(7) . ? Ru P1 2.2539(18) . ? Ru P2 2.2542(19) . ? Ru Cl 2.4239(19) . ? P1 O1 1.636(5) . ? P1 C1 1.814(7) . ? P1 C7 1.825(7) . ? P2 O2 1.645(5) . ? P2 C34 1.811(7) . ? P2 C40 1.813(7) . ? O1 C13 1.423(8) . ? O2 C33 1.385(8) . ? C1 C2 1.390(11) . ? C1 C6 1.396(10) . ? C2 C3 1.415(11) . ? C3 C4 1.379(14) . ? C4 C5 1.403(14) . ? C5 C6 1.384(11) . ? C7 C12 1.388(10) . ? C7 C8 1.393(10) . ? C8 C9 1.413(12) . ? C9 C10 1.353(14) . ? C10 C11 1.347(13) . ? C11 C12 1.390(10) . ? C13 C22 1.366(9) . ? C13 C14 1.400(9) . ? C14 C15 1.346(11) . ? C15 C16 1.395(11) . ? C16 C21 1.411(11) . ? C16 C17 1.428(12) . ? C17 C18 1.329(14) . ? C18 C19 1.376(14) . ? C19 C20 1.373(12) . ? C20 C21 1.416(11) . ? C21 C22 1.426(10) . ? C22 C23 1.520(9) . ? C23 C24 1.533(9) . ? C24 C33 1.368(10) . ? C24 C25 1.434(9) . ? C25 C26 1.410(11) . ? C25 C30 1.454(11) . ? C26 C27 1.401(11) . ? C27 C28 1.388(14) . ? C28 C29 1.328(14) . ? C29 C30 1.424(11) . ? C30 C31 1.405(12) . ? C31 C32 1.374(11) . ? C32 C33 1.389(9) . ? C34 C39 1.366(11) . ? C34 C35 1.383(11) . ? C35 C36 1.385(12) . ? C36 C37 1.340(14) . ? C37 C38 1.367(14) . ? C38 C39 1.408(11) . ? C40 C45 1.369(10) . ? C40 C41 1.410(11) . ? C41 C42 1.366(12) . ? C42 C43 1.397(14) . ? C43 C44 1.326(12) . ? C44 C45 1.395(10) . ? C46 C47 1.388(13) . ? C46 C50 1.409(12) . ? C47 C48 1.429(13) . ? C48 C49 1.405(14) . ? C49 C50 1.423(12) . ? Cl1S C1S 1.54(5) . ? Cl2S C1S 1.73(4) . ? Cl3S C2SA 1.76(2) . ? Cl3S C2SB 1.76(2) . ? C2SA Cl4A 1.81(2) . ? C2SB Cl4B 1.77(2) . ? O2S O2S 1.64(6) 7_677 ? 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 C50 Ru C49 37.7(3) . . ? C50 Ru C48 62.1(4) . . ? C49 Ru C48 37.0(4) . . ? C50 Ru C47 62.2(4) . . ? C49 Ru C47 62.5(4) . . ? C48 Ru C47 37.6(3) . . ? C50 Ru C46 37.1(3) . . ? C49 Ru C46 61.9(3) . . ? C48 Ru C46 61.2(3) . . ? C47 Ru C46 36.3(3) . . ? C50 Ru P1 102.3(3) . . ? C49 Ru P1 137.8(3) . . ? C48 Ru P1 155.0(3) . . ? C47 Ru P1 119.0(3) . . ? C46 Ru P1 94.3(2) . . ? C50 Ru P2 113.5(2) . . ? C49 Ru P2 93.8(3) . . ? C48 Ru P2 109.9(3) . . ? C47 Ru P2 147.1(3) . . ? C46 Ru P2 150.6(3) . . ? P1 Ru P2 93.94(7) . . ? C50 Ru Cl 149.5(3) . . ? C49 Ru Cl 126.1(3) . . ? C48 Ru Cl 92.1(3) . . ? C47 Ru Cl 87.5(3) . . ? C46 Ru Cl 117.6(3) . . ? P1 Ru Cl 95.39(7) . . ? P2 Ru Cl 89.53(7) . . ? O1 P1 C1 106.0(3) . . ? O1 P1 C7 101.5(3) . . ? C1 P1 C7 105.0(3) . . ? O1 P1 Ru 113.83(17) . . ? C1 P1 Ru 114.3(2) . . ? C7 P1 Ru 114.9(2) . . ? O2 P2 C34 99.0(3) . . ? O2 P2 C40 96.1(3) . . ? C34 P2 C40 102.1(3) . . ? O2 P2 Ru 121.50(18) . . ? C34 P2 Ru 112.0(2) . . ? C40 P2 Ru 122.1(2) . . ? C13 O1 P1 131.4(4) . . ? C33 O2 P2 128.7(4) . . ? C2 C1 C6 118.5(7) . . ? C2 C1 P1 116.8(5) . . ? C6 C1 P1 124.1(6) . . ? C1 C2 C3 121.2(8) . . ? C4 C3 C2 118.8(9) . . ? C3 C4 C5 120.5(8) . . ? C6 C5 C4 119.8(9) . . ? C5 C6 C1 121.0(8) . . ? C12 C7 C8 118.7(7) . . ? C12 C7 P1 116.7(5) . . ? C8 C7 P1 124.4(6) . . ? C7 C8 C9 118.5(8) . . ? C10 C9 C8 121.7(9) . . ? C11 C10 C9 119.4(8) . . ? C10 C11 C12 121.3(8) . . ? C7 C12 C11 120.2(8) . . ? C22 C13 C14 124.4(7) . . ? C22 C13 O1 114.9(6) . . ? C14 C13 O1 120.7(6) . . ? C15 C14 C13 117.0(7) . . ? C14 C15 C16 123.3(7) . . ? C15 C16 C21 118.3(7) . . ? C15 C16 C17 122.4(8) . . ? C21 C16 C17 119.2(8) . . ? C18 C17 C16 121.2(10) . . ? C17 C18 C19 120.3(9) . . ? C20 C19 C18 121.3(9) . . ? C19 C20 C21 120.5(9) . . ? C16 C21 C20 117.4(7) . . ? C16 C21 C22 119.9(7) . . ? C20 C21 C22 122.6(7) . . ? C13 C22 C21 116.8(6) . . ? C13 C22 C23 121.0(6) . . ? C21 C22 C23 122.2(6) . . ? C22 C23 C24 114.7(6) . . ? C33 C24 C25 118.6(6) . . ? C33 C24 C23 121.0(6) . . ? C25 C24 C23 120.4(6) . . ? C26 C25 C24 123.3(7) . . ? C26 C25 C30 118.0(7) . . ? C24 C25 C30 118.7(7) . . ? C27 C26 C25 119.9(9) . . ? C28 C27 C26 121.4(9) . . ? C29 C28 C27 119.8(8) . . ? C28 C29 C30 122.9(9) . . ? C31 C30 C29 123.3(8) . . ? C31 C30 C25 118.9(7) . . ? C29 C30 C25 117.8(8) . . ? C32 C31 C30 120.5(7) . . ? C31 C32 C33 120.3(7) . . ? C24 C33 O2 118.8(6) . . ? C24 C33 C32 122.7(6) . . ? O2 C33 C32 118.1(7) . . ? C39 C34 C35 117.3(7) . . ? C39 C34 P2 123.5(6) . . ? C35 C34 P2 119.1(6) . . ? C34 C35 C36 120.9(8) . . ? C37 C36 C35 120.5(10) . . ? C36 C37 C38 121.2(9) . . ? C37 C38 C39 117.7(9) . . ? C34 C39 C38 122.3(9) . . ? C45 C40 C41 117.8(7) . . ? C45 C40 P2 122.6(5) . . ? C41 C40 P2 119.6(6) . . ? C42 C41 C40 120.3(9) . . ? C41 C42 C43 120.8(9) . . ? C44 C43 C42 118.8(8) . . ? C43 C44 C45 121.8(8) . . ? C40 C45 C44 120.5(7) . . ? C47 C46 C50 109.4(8) . . ? C47 C46 Ru 71.6(5) . . ? C50 C46 Ru 70.1(4) . . ? C46 C47 C48 107.0(9) . . ? C46 C47 Ru 72.1(5) . . ? C48 C47 Ru 70.9(5) . . ? C49 C48 C47 108.7(9) . . ? C49 C48 Ru 71.4(5) . . ? C47 C48 Ru 71.5(5) . . ? C48 C49 C50 107.2(9) . . ? C48 C49 Ru 71.6(5) . . ? C50 C49 Ru 70.5(4) . . ? C46 C50 C49 107.6(9) . . ? C46 C50 Ru 72.8(5) . . ? C49 C50 Ru 71.8(4) . . ? Cl1S C1S Cl2S 124(2) . . ? C2SA Cl3S C2SB 16.6(17) . . ? Cl3S C2SA Cl4A 105(2) . . ? Cl3S C2SB Cl4B 101(2) . . ? 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 Ru P1 O1 C13 -166.3(5) . . . . ? P1 O1 C13 C22 158.3(5) . . . . ? O1 C13 C22 C23 -8.0(9) . . . . ? C13 C22 C23 C24 -60.1(9) . . . . ? C22 C23 C24 C33 117.6(7) . . . . ? C23 C24 C33 O2 4.7(9) . . . . ? C24 C33 O2 P2 -118.6(6) . . . . ? C33 O2 P2 Ru 4.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.13 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.412 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.144 data_msb121 _database_code_CSD 190094 _journal_coden_Cambridge 186 loop_ _publ_author_name 'Balakrishna Maravanji' 'Joel T. Mague' 'Rashmishree Panda' _publ_contact_author_name 'Prof Maravanji S Balakrishna' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Bombay Mumbai 400 076 INDIA ; _publ_contact_author_email 'KRISHNA@IITB.AC.IN' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; New bis(phosphinite) derived from bis(2-hydroxy-1-naphthyl)methane. Synthesis, derivatization and transition metal chemistry of Ph2P{(-OC10H6)( -CH2)(C10H6O-)}PPh2. The crystal and molecular structures of Ph2P(Se){(-OC10H6)( -CH2)(C10H6O-)}P(Se)Ph2, [CpRuCl{ 2-Ph2P{(-OC10H6)( -CH2)(C10H6O-)}PPh2}- P, P], and cis-[PtCl2{ 2-Ph2P{(-OC10H6)( -CH2)(C10H6O-)}PPh2}- P, P] ; _publ_section_references ; Bruker AXS (1997). SHELXTL Version 5.1, Madison, WI. Enraf-Nonius (1989). CAD-4 Operations Manual, Delft, The Netherlands. Harms, K. (1996). Program for the Lp-correction of CAD-4 Diffractometer Data. University of Marburg, Germany. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1997). SHELXL-97. Program for Crystal Structure Refinement. University of Gottingen, Gottingen, Germany. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H38 Cl4 O3 P2 Pt' _chemical_formula_weight 1037.58 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.357(3) _cell_length_b 11.005(2) _cell_length_c 26.594(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.30(1) _cell_angle_gamma 90.00 _cell_volume 4314(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20.06 _cell_measurement_theta_max 23.54 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 3.614 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1974 _exptl_absorpt_correction_T_max 0.2587 _exptl_absorpt_process_details '\y scans (North, et al., 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\q/2\q scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 20 _diffrn_reflns_number 7934 _diffrn_reflns_av_R_equivalents 0.1381 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.13 _reflns_number_total 7630 _reflns_number_gt 5065 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data-reduction 'XCAD4 (Harms, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker AXS, 1997)' _computing_publication_material 'SHELXTL (Bruker AXS, 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^)+(0.1246P)^2^+1.4790P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7630 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1185 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1858 _refine_ls_wR_factor_gt 0.1585 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.003 _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 Pt Pt 0.24507(2) 0.08910(3) 0.771645(15) 0.04095(16) Uani 1 1 d . . . Cl1 Cl 0.2794(2) 0.1255(3) 0.69240(12) 0.0649(8) Uani 1 1 d . . . Cl2 Cl 0.1704(2) -0.0855(3) 0.73304(13) 0.0677(8) Uani 1 1 d . . . P1 P 0.20845(16) 0.0571(2) 0.84593(10) 0.0410(6) Uani 1 1 d . . . P2 P 0.32767(16) 0.2544(2) 0.79974(10) 0.0402(6) Uani 1 1 d . . . O1 O 0.2940(4) 0.0335(6) 0.8959(3) 0.0439(15) Uani 1 1 d . . . O2 O 0.3527(4) 0.2682(6) 0.8627(3) 0.0436(15) Uani 1 1 d . . . C1 C 0.1549(6) 0.1805(9) 0.8686(5) 0.050(3) Uani 1 1 d . . . C2 C 0.1682(9) 0.1981(12) 0.9220(6) 0.074(4) Uani 1 1 d . . . H2 H 0.2067 0.1463 0.9458 0.089 Uiso 1 1 calc R . . C3 C 0.1252(12) 0.2915(14) 0.9402(7) 0.093(5) Uani 1 1 d . . . H3 H 0.1369 0.3046 0.9761 0.112 Uiso 1 1 calc R . . C4 C 0.0650(11) 0.3653(15) 0.9053(9) 0.099(6) Uani 1 1 d . . . H4 H 0.0339 0.4260 0.9175 0.119 Uiso 1 1 calc R . . C5 C 0.0503(10) 0.3487(15) 0.8506(9) 0.106(6) Uani 1 1 d . . . H5 H 0.0104 0.3993 0.8269 0.127 Uiso 1 1 calc R . . C6 C 0.0954(9) 0.2571(13) 0.8327(6) 0.081(4) Uani 1 1 d . . . H6 H 0.0864 0.2462 0.7969 0.097 Uiso 1 1 calc R . . C7 C 0.1346(7) -0.0685(9) 0.8496(4) 0.049(2) Uani 1 1 d . . . C8 C 0.0494(7) -0.0748(11) 0.8151(5) 0.060(3) Uani 1 1 d . . . H8 H 0.0303 -0.0168 0.7889 0.072 Uiso 1 1 calc R . . C9 C -0.0086(8) -0.1704(15) 0.8200(6) 0.082(4) Uani 1 1 d . . . H9 H -0.0660 -0.1755 0.7963 0.098 Uiso 1 1 calc R . . C10 C 0.0169(10) -0.2547(14) 0.8581(7) 0.084(4) Uani 1 1 d . . . H10 H -0.0227 -0.3164 0.8611 0.101 Uiso 1 1 calc R . . C11 C 0.1019(10) -0.2478(12) 0.8920(7) 0.088(5) Uani 1 1 d . . . H11 H 0.1211 -0.3071 0.9177 0.106 Uiso 1 1 calc R . . C12 C 0.1604(8) -0.1533(11) 0.8888(5) 0.067(3) Uani 1 1 d . . . H12 H 0.2170 -0.1475 0.9133 0.080 Uiso 1 1 calc R . . C13 C 0.3784(6) -0.0116(9) 0.8926(4) 0.043(2) Uani 1 1 d . . . C14 C 0.3793(8) -0.1133(9) 0.8615(4) 0.051(3) Uani 1 1 d . . . H14 H 0.3252 -0.1480 0.8419 0.061 Uiso 1 1 calc R . . C15 C 0.4592(8) -0.1603(9) 0.8603(4) 0.055(3) Uani 1 1 d . . . H15 H 0.4602 -0.2276 0.8394 0.066 Uiso 1 1 calc R . . C16 C 0.5415(7) -0.1095(9) 0.8903(4) 0.049(3) Uani 1 1 d . . . C17 C 0.6281(9) -0.1597(11) 0.8902(5) 0.063(3) Uani 1 1 d . . . H17 H 0.6302 -0.2265 0.8692 0.076 Uiso 1 1 calc R . . C18 C 0.7068(9) -0.1105(13) 0.9204(6) 0.079(4) Uani 1 1 d . . . H18 H 0.7623 -0.1450 0.9209 0.095 Uiso 1 1 calc R . . C19 C 0.7035(8) -0.0077(12) 0.9507(6) 0.069(3) Uani 1 1 d . . . H19 H 0.7573 0.0261 0.9712 0.082 Uiso 1 1 calc R . . C20 C 0.6238(7) 0.0434(11) 0.9506(5) 0.060(3) Uani 1 1 d . . . H20 H 0.6245 0.1128 0.9706 0.072 Uiso 1 1 calc R . . C21 C 0.5386(6) -0.0042(9) 0.9213(4) 0.043(2) Uani 1 1 d . . . C22 C 0.4538(6) 0.0454(8) 0.9219(4) 0.039(2) Uani 1 1 d . . . C23 C 0.4457(6) 0.1556(9) 0.9558(4) 0.043(2) Uani 1 1 d . . . H23A H 0.3827 0.1632 0.9556 0.052 Uiso 1 1 calc R . . H23B H 0.4806 0.1388 0.9915 0.052 Uiso 1 1 calc R . . C24 C 0.4765(6) 0.2776(8) 0.9400(4) 0.040(2) Uani 1 1 d . . . C25 C 0.5489(7) 0.3433(9) 0.9745(4) 0.047(2) Uani 1 1 d . . . C26 C 0.5967(7) 0.3073(10) 1.0246(4) 0.055(3) Uani 1 1 d . . . H26 H 0.5810 0.2343 1.0373 0.066 Uiso 1 1 calc R . . C27 C 0.6646(8) 0.3727(12) 1.0558(5) 0.064(3) Uani 1 1 d . . . H27 H 0.6932 0.3450 1.0894 0.077 Uiso 1 1 calc R . . C28 C 0.6928(8) 0.4812(12) 1.0386(5) 0.071(3) Uani 1 1 d . . . H28 H 0.7425 0.5228 1.0596 0.085 Uiso 1 1 calc R . . C29 C 0.6459(8) 0.5272(11) 0.9894(5) 0.061(3) Uani 1 1 d . . . H29 H 0.6614 0.6022 0.9783 0.073 Uiso 1 1 calc R . . C30 C 0.5754(7) 0.4588(10) 0.9570(4) 0.051(2) Uani 1 1 d . . . C31 C 0.5240(8) 0.5048(10) 0.9075(5) 0.061(3) Uani 1 1 d . . . H31 H 0.5404 0.5786 0.8957 0.074 Uiso 1 1 calc R . . C32 C 0.4528(7) 0.4445(9) 0.8775(5) 0.054(3) Uani 1 1 d . . . H32 H 0.4188 0.4781 0.8460 0.065 Uiso 1 1 calc R . . C33 C 0.4293(6) 0.3308(9) 0.8933(4) 0.042(2) Uani 1 1 d . . . C34 C 0.4376(6) 0.2543(8) 0.7878(4) 0.044(2) Uani 1 1 d . . . C35 C 0.4903(7) 0.1520(9) 0.8035(4) 0.047(2) Uani 1 1 d . . . H35 H 0.4645 0.0830 0.8136 0.057 Uiso 1 1 calc R . . C36 C 0.5809(7) 0.1504(11) 0.8043(5) 0.057(3) Uani 1 1 d . . . H36 H 0.6164 0.0820 0.8162 0.069 Uiso 1 1 calc R . . C37 C 0.6184(7) 0.2526(11) 0.7872(5) 0.059(3) Uani 1 1 d . . . H37 H 0.6793 0.2534 0.7880 0.071 Uiso 1 1 calc R . . C38 C 0.5663(8) 0.3488(11) 0.7698(5) 0.064(3) Uani 1 1 d . . . H38 H 0.5914 0.4150 0.7572 0.077 Uiso 1 1 calc R . . C39 C 0.4751(7) 0.3547(10) 0.7697(4) 0.056(3) Uani 1 1 d . . . H39 H 0.4405 0.4238 0.7578 0.067 Uiso 1 1 calc R . . C40 C 0.2706(7) 0.3912(9) 0.7722(4) 0.047(2) Uani 1 1 d . . . C41 C 0.2534(7) 0.4226(10) 0.7202(5) 0.061(3) Uani 1 1 d . . . H41 H 0.2773 0.3744 0.6986 0.074 Uiso 1 1 calc R . . C42 C 0.2031(8) 0.5206(10) 0.6993(5) 0.063(3) Uani 1 1 d . . . H42 H 0.1919 0.5383 0.6639 0.076 Uiso 1 1 calc R . . C43 C 0.1679(8) 0.5954(10) 0.7317(8) 0.086(5) Uani 1 1 d . . . H43 H 0.1343 0.6639 0.7179 0.104 Uiso 1 1 calc R . . C44 C 0.1831(10) 0.5674(12) 0.7839(7) 0.086(4) Uani 1 1 d . . . H44 H 0.1585 0.6158 0.8051 0.103 Uiso 1 1 calc R . . C45 C 0.2353(8) 0.4662(10) 0.8048(6) 0.066(3) Uani 1 1 d . . . H45 H 0.2470 0.4481 0.8402 0.079 Uiso 1 1 calc R . . C46 C 0.1983(15) -0.0879(14) 0.5933(8) 0.114(6) Uani 1 1 d . . . H46A H 0.2597 -0.0575 0.5994 0.137 Uiso 1 1 calc R . . H46B H 0.1841 -0.0861 0.6266 0.137 Uiso 1 1 calc R . . Cl3 Cl 0.1286(5) 0.0069(9) 0.5527(3) 0.202(4) Uani 1 1 d . . . Cl4 Cl 0.1968(10) -0.2291(8) 0.5746(4) 0.281(6) Uani 1 1 d . . . O3 O 0.9627(11) -0.029(2) 0.9508(7) 0.203(9) 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 Pt 0.0473(2) 0.0331(2) 0.0439(2) 0.00040(17) 0.01529(16) -0.00101(16) Cl1 0.092(2) 0.0586(15) 0.0492(17) -0.0023(13) 0.0281(15) -0.0137(15) Cl2 0.085(2) 0.0560(16) 0.0689(19) -0.0193(14) 0.0319(16) -0.0259(15) P1 0.0413(12) 0.0390(13) 0.0451(14) 0.0036(11) 0.0158(11) 0.0023(10) P2 0.0479(13) 0.0310(12) 0.0432(14) 0.0041(10) 0.0153(11) 0.0015(10) O1 0.043(3) 0.049(4) 0.043(4) 0.002(3) 0.020(3) 0.001(3) O2 0.051(4) 0.040(4) 0.041(4) 0.000(3) 0.015(3) -0.001(3) C1 0.039(5) 0.050(6) 0.068(8) -0.005(5) 0.025(5) 0.002(4) C2 0.081(9) 0.072(8) 0.077(9) -0.002(7) 0.034(7) 0.017(7) C3 0.125(13) 0.069(9) 0.105(13) -0.023(9) 0.065(11) -0.001(9) C4 0.088(11) 0.073(10) 0.155(18) -0.043(12) 0.062(12) 0.005(8) C5 0.067(9) 0.072(10) 0.17(2) 0.002(11) 0.016(10) 0.032(8) C6 0.066(8) 0.084(10) 0.084(11) 0.010(8) 0.006(7) 0.021(7) C7 0.054(6) 0.039(6) 0.058(7) -0.003(5) 0.022(5) -0.002(4) C8 0.040(5) 0.074(8) 0.068(8) -0.003(6) 0.019(5) 0.004(5) C9 0.048(7) 0.111(12) 0.089(11) -0.019(9) 0.022(7) -0.019(7) C10 0.081(10) 0.077(10) 0.109(13) -0.005(9) 0.053(9) -0.016(8) C11 0.095(10) 0.052(8) 0.129(14) 0.026(8) 0.049(10) -0.009(7) C12 0.060(7) 0.066(8) 0.079(9) -0.001(7) 0.027(6) -0.011(6) C13 0.044(5) 0.043(5) 0.041(5) 0.016(4) 0.012(4) 0.009(4) C14 0.065(6) 0.035(5) 0.056(7) 0.004(4) 0.023(5) -0.005(4) C15 0.081(8) 0.038(6) 0.056(7) 0.014(5) 0.035(6) 0.019(5) C16 0.051(6) 0.046(6) 0.057(7) 0.016(5) 0.025(5) 0.008(4) C17 0.077(8) 0.049(7) 0.075(9) 0.017(6) 0.041(7) 0.021(6) C18 0.069(8) 0.078(9) 0.101(11) 0.028(8) 0.041(8) 0.030(7) C19 0.047(6) 0.066(8) 0.093(10) 0.025(7) 0.020(6) 0.012(5) C20 0.056(6) 0.063(7) 0.070(8) 0.008(6) 0.033(6) 0.000(5) C21 0.048(5) 0.042(5) 0.046(6) 0.019(4) 0.024(5) 0.009(4) C22 0.046(5) 0.035(5) 0.040(5) 0.013(4) 0.017(4) 0.007(4) C23 0.048(5) 0.042(5) 0.044(6) 0.010(4) 0.020(4) 0.002(4) C24 0.046(5) 0.041(5) 0.036(5) -0.002(4) 0.016(4) 0.007(4) C25 0.054(6) 0.041(6) 0.050(6) -0.005(5) 0.024(5) 0.009(4) C26 0.055(6) 0.058(7) 0.048(7) -0.001(5) 0.011(5) 0.003(5) C27 0.064(7) 0.073(8) 0.052(7) -0.003(6) 0.010(6) 0.004(6) C28 0.059(7) 0.079(9) 0.075(9) -0.024(7) 0.018(7) -0.021(6) C29 0.062(7) 0.048(6) 0.071(8) -0.010(6) 0.017(6) -0.010(5) C30 0.058(6) 0.050(6) 0.046(6) -0.009(5) 0.014(5) 0.008(5) C31 0.079(8) 0.035(5) 0.070(8) 0.006(5) 0.021(7) -0.003(5) C32 0.064(7) 0.040(5) 0.056(7) 0.003(5) 0.013(5) 0.000(5) C33 0.044(5) 0.045(5) 0.040(6) -0.004(4) 0.015(4) 0.000(4) C34 0.044(5) 0.041(5) 0.050(6) 0.002(4) 0.020(4) -0.001(4) C35 0.053(6) 0.037(5) 0.058(6) 0.003(5) 0.025(5) 0.002(4) C36 0.054(6) 0.054(7) 0.068(8) -0.002(6) 0.024(6) 0.007(5) C37 0.044(6) 0.072(8) 0.061(7) 0.011(6) 0.015(5) 0.003(5) C38 0.061(7) 0.053(7) 0.089(10) 0.006(6) 0.040(7) -0.019(6) C39 0.063(6) 0.048(6) 0.056(7) 0.015(5) 0.016(6) -0.004(5) C40 0.050(5) 0.047(6) 0.038(6) 0.003(4) 0.004(4) -0.016(4) C41 0.057(6) 0.053(7) 0.064(8) 0.000(6) 0.002(6) -0.005(5) C42 0.058(7) 0.048(7) 0.071(8) 0.025(6) -0.001(6) -0.005(5) C43 0.058(7) 0.033(6) 0.155(16) 0.031(8) 0.007(9) 0.007(5) C44 0.086(10) 0.055(8) 0.113(13) -0.006(8) 0.023(9) 0.022(7) C45 0.062(7) 0.046(6) 0.085(10) -0.017(6) 0.014(6) -0.001(5) C46 0.145(16) 0.088(12) 0.110(15) -0.013(10) 0.036(13) -0.005(11) Cl3 0.167(6) 0.249(9) 0.214(8) 0.146(7) 0.096(6) 0.046(6) Cl4 0.433(16) 0.137(7) 0.245(11) -0.087(7) 0.051(10) 0.035(8) O3 0.147(13) 0.30(2) 0.156(14) -0.104(16) 0.037(11) 0.043(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 Pt P2 2.223(2) . ? Pt P1 2.229(3) . ? Pt Cl2 2.324(3) . ? Pt Cl1 2.346(3) . ? P1 O1 1.606(7) . ? P1 C1 1.779(10) . ? P1 C7 1.808(10) . ? P2 O2 1.617(7) . ? P2 C40 1.792(11) . ? P2 C34 1.803(9) . ? O1 C13 1.413(11) . ? O2 C33 1.407(11) . ? C1 C2 1.391(16) . ? C1 C6 1.402(16) . ? C2 C3 1.381(18) . ? C3 C4 1.38(2) . ? C4 C5 1.42(3) . ? C5 C6 1.38(2) . ? C7 C8 1.372(15) . ? C7 C12 1.373(16) . ? C8 C9 1.408(18) . ? C9 C10 1.35(2) . ? C10 C11 1.37(2) . ? C11 C12 1.392(16) . ? C13 C22 1.355(13) . ? C13 C14 1.393(14) . ? C14 C15 1.340(14) . ? C15 C16 1.407(16) . ? C16 C21 1.430(15) . ? C16 C17 1.441(14) . ? C17 C18 1.362(19) . ? C18 C19 1.398(19) . ? C19 C20 1.346(15) . ? C20 C21 1.422(15) . ? C21 C22 1.416(12) . ? C22 C23 1.537(14) . ? C23 C24 1.521(13) . ? C24 C33 1.381(13) . ? C24 C25 1.424(14) . ? C25 C26 1.387(15) . ? C25 C30 1.450(15) . ? C26 C27 1.344(16) . ? C27 C28 1.391(18) . ? C28 C29 1.399(17) . ? C29 C30 1.398(15) . ? C30 C31 1.426(15) . ? C31 C32 1.335(15) . ? C32 C33 1.399(14) . ? C34 C35 1.381(13) . ? C34 C39 1.393(13) . ? C35 C36 1.385(13) . ? C36 C37 1.397(15) . ? C37 C38 1.329(16) . ? C38 C39 1.401(15) . ? C40 C41 1.378(15) . ? C40 C45 1.410(16) . ? C41 C42 1.352(15) . ? C42 C43 1.41(2) . ? C43 C44 1.38(2) . ? C44 C45 1.394(18) . ? C46 Cl4 1.630(16) . ? C46 Cl3 1.658(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pt P1 95.37(9) . . ? P2 Pt Cl2 171.54(10) . . ? P1 Pt Cl2 92.56(10) . . ? P2 Pt Cl1 84.91(10) . . ? P1 Pt Cl1 178.29(10) . . ? Cl2 Pt Cl1 87.25(11) . . ? O1 P1 C1 101.1(5) . . ? O1 P1 C7 102.2(4) . . ? C1 P1 C7 102.0(4) . . ? O1 P1 Pt 114.0(2) . . ? C1 P1 Pt 115.8(4) . . ? C7 P1 Pt 119.1(4) . . ? O2 P2 C40 106.9(4) . . ? O2 P2 C34 102.7(4) . . ? C40 P2 C34 107.7(5) . . ? O2 P2 Pt 111.9(3) . . ? C40 P2 Pt 112.5(3) . . ? C34 P2 Pt 114.5(3) . . ? C13 O1 P1 123.9(6) . . ? C33 O2 P2 124.2(6) . . ? C2 C1 C6 119.6(11) . . ? C2 C1 P1 120.2(9) . . ? C6 C1 P1 120.2(10) . . ? C3 C2 C1 120.9(14) . . ? C4 C3 C2 119.9(16) . . ? C3 C4 C5 120.0(13) . . ? C6 C5 C4 119.7(15) . . ? C5 C6 C1 119.8(15) . . ? C8 C7 C12 119.4(10) . . ? C8 C7 P1 119.9(9) . . ? C12 C7 P1 120.6(9) . . ? C7 C8 C9 119.1(12) . . ? C10 C9 C8 121.7(13) . . ? C9 C10 C11 118.7(13) . . ? C10 C11 C12 121.0(14) . . ? C7 C12 C11 120.0(13) . . ? C22 C13 C14 124.4(9) . . ? C22 C13 O1 116.9(9) . . ? C14 C13 O1 118.7(9) . . ? C15 C14 C13 119.0(11) . . ? C14 C15 C16 121.1(10) . . ? C15 C16 C21 118.7(9) . . ? C15 C16 C17 122.0(11) . . ? C21 C16 C17 119.3(10) . . ? C18 C17 C16 120.9(12) . . ? C17 C18 C19 119.4(11) . . ? C20 C19 C18 121.2(13) . . ? C19 C20 C21 122.9(12) . . ? C22 C21 C20 124.0(10) . . ? C22 C21 C16 119.8(9) . . ? C20 C21 C16 116.2(9) . . ? C13 C22 C21 117.1(9) . . ? C13 C22 C23 120.4(8) . . ? C21 C22 C23 122.5(9) . . ? C24 C23 C22 117.0(7) . . ? C33 C24 C25 118.9(9) . . ? C33 C24 C23 119.8(9) . . ? C25 C24 C23 121.2(9) . . ? C26 C25 C24 125.6(10) . . ? C26 C25 C30 115.9(10) . . ? C24 C25 C30 118.5(9) . . ? C27 C26 C25 123.3(12) . . ? C26 C27 C28 121.1(12) . . ? C27 C28 C29 119.5(11) . . ? C30 C29 C28 119.1(11) . . ? C29 C30 C31 120.6(11) . . ? C29 C30 C25 120.9(10) . . ? C31 C30 C25 118.3(10) . . ? C32 C31 C30 121.6(10) . . ? C31 C32 C33 120.2(11) . . ? C24 C33 C32 122.3(10) . . ? C24 C33 O2 117.1(8) . . ? C32 C33 O2 120.6(9) . . ? C35 C34 C39 119.2(9) . . ? C35 C34 P2 116.5(7) . . ? C39 C34 P2 123.9(8) . . ? C34 C35 C36 121.1(10) . . ? C35 C36 C37 119.2(10) . . ? C38 C37 C36 119.5(10) . . ? C37 C38 C39 122.8(10) . . ? C34 C39 C38 118.1(10) . . ? C41 C40 C45 118.1(11) . . ? C41 C40 P2 123.7(9) . . ? C45 C40 P2 118.0(8) . . ? C42 C41 C40 122.7(12) . . ? C41 C42 C43 119.2(13) . . ? C44 C43 C42 120.2(11) . . ? C43 C44 C45 119.8(13) . . ? C44 C45 C40 120.0(13) . . ? Cl4 C46 Cl3 116.7(13) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.13 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.367 _refine_diff_density_min -3.710 _refine_diff_density_rms 0.194