# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1270 #=============================================================================== data_global #=============================================================================== _audit_creation_date 22-02-99 # 1. SUBMISSION DETAILS _publ_contact_author ; Louis Ricard, Labo DCPH, Ecole Polytechnique Route de Saclay 91128 Palaiseau France ; _publ_contact_author_phone '01-69-33-45-72' _publ_contact_author_fax '01-69-33-39-90' _publ_contact_author_email louis.ricard@polytechnique.fr _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in Chem. Comm.. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; 2,5-di-(tert -butyl)phospholyl Sandwich Complexes Containing Group 14 Elements (Ge, Sn, Pb). Synthesis, Molecular Structure, and Ring Transfer Chemistry of [M(PC4H2tBu2)2] M= Sn, Pb. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name ; Forissier Kareen, Ricard Louis, Charmichael Duncan and Mathey Francois ; _publ_author_address ; Laboratoire Heteroelements et Coordination, CNRS UMR 7653, DCPH Ecole Polytechnique, F-91128 Palaiseau Cedex France ; #=============================================================================== # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. Enraf-Nonius, Cad4-Express Operations Manual, Delft, 1994. Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal Structure Analysis, User Manual, Enraf - Nonius, Delft, The Netherlands. North, A.C.T., Phillips, D.C., Mathews, F.S. (1968). Acta Cryst., A24, 351-359. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_(NoName) #=============================================================================== data_pbp2_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H40 P2 Pb' _chemical_formula_weight 597.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pb' 'Pb' -3.3944 10.1111 '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' '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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.0550(2) _cell_length_b 20.3550(4) _cell_length_c 16.4910(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.3230(10) _cell_angle_gamma 90.00 _cell_volume 5284.35(16) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 343 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description 'plate' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 6.513 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10807 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10807 _reflns_number_gt 9859 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0369P)^2^+3.6311P] 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 10807 _refine_ls_number_parameters 570 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.214151(7) 0.178916(5) 0.841325(6) 0.02655(4) Uani 1 1 d . . . Pb2 Pb 0.232033(7) 0.075916(5) 0.344132(6) 0.02675(4) Uani 1 1 d . . . P1 P 0.22775(5) 0.30497(4) 0.76661(5) 0.02892(17) Uani 1 1 d . . . P2 P 0.30155(5) 0.14750(4) 1.00798(5) 0.02463(15) Uani 1 1 d . . . P3 P 0.25903(5) -0.05204(4) 0.28118(5) 0.02885(17) Uani 1 1 d . . . P4 P 0.30121(5) 0.11167(4) 0.51317(5) 0.02656(16) Uani 1 1 d . . . C1 C 0.31636(18) 0.25330(14) 0.76021(17) 0.0246(6) Uani 1 1 d . . . C2 C 0.29142(19) 0.20177(15) 0.70608(18) 0.0279(6) Uani 1 1 d . . . H2 H 0.3285 0.1693 0.6953 0.034 Uiso 1 1 calc R . . C3 C 0.20404(19) 0.20313(15) 0.66863(17) 0.0281(6) Uani 1 1 d . . . H3 H 0.1790 0.1719 0.6304 0.034 Uiso 1 1 calc R . . C4 C 0.15909(18) 0.25464(15) 0.69359(17) 0.0271(6) Uani 1 1 d . . . C5 C 0.25444(19) 0.07385(13) 0.96090(18) 0.0239(6) Uani 1 1 d . A . C6 C 0.1664(2) 0.07810(14) 0.94821(19) 0.0276(6) Uani 1 1 d . . . H6 H 0.1306 0.0444 0.9245 0.033 Uiso 1 1 calc R . . C7 C 0.13587(18) 0.13806(14) 0.97452(18) 0.0265(6) Uani 1 1 d . . . H7 H 0.0783 0.1473 0.9693 0.032 Uiso 1 1 calc R . . C8 C 0.19944(19) 0.18190(14) 1.00889(18) 0.0241(6) Uani 1 1 d . . . C9 C 0.40787(19) 0.26780(15) 0.80323(19) 0.0299(7) Uani 1 1 d . . . C10 C 0.4464(3) 0.3138(3) 0.7484(3) 0.0821(18) Uani 1 1 d . . . H10A H 0.4178 0.3554 0.7450 0.123 Uiso 1 1 calc R . . H10B H 0.4402 0.2951 0.6940 0.123 Uiso 1 1 calc R . . H10C H 0.5056 0.3199 0.7714 0.123 Uiso 1 1 calc R . . C11 C 0.4598(2) 0.2058(2) 0.8172(4) 0.0798(18) Uani 1 1 d . . . H11A H 0.5171 0.2164 0.8430 0.120 Uiso 1 1 calc R . . H11B H 0.4595 0.1847 0.7651 0.120 Uiso 1 1 calc R . . H11C H 0.4359 0.1768 0.8524 0.120 Uiso 1 1 calc R . . C12 C 0.4103(3) 0.3012(2) 0.8851(2) 0.0583(11) Uani 1 1 d . . . H12A H 0.3896 0.2716 0.9219 0.087 Uiso 1 1 calc R . . H12B H 0.3752 0.3398 0.8770 0.087 Uiso 1 1 calc R . . H12C H 0.4677 0.3136 0.9085 0.087 Uiso 1 1 calc R . . C13 C 0.0649(2) 0.26862(17) 0.6615(2) 0.0383(8) Uani 1 1 d . . . C14 C 0.0214(3) 0.2849(4) 0.7326(4) 0.112(3) Uani 1 1 d . . . H14A H 0.0328 0.2509 0.7736 0.169 Uiso 1 1 calc R . . H14B H -0.0388 0.2882 0.7125 0.169 Uiso 1 1 calc R . . H14C H 0.0425 0.3261 0.7568 0.169 Uiso 1 1 calc R . . C15 C 0.0193(2) 0.2085(3) 0.6200(3) 0.0738(15) Uani 1 1 d . . . H15A H 0.0454 0.1950 0.5750 0.111 Uiso 1 1 calc R . . H15B H -0.0393 0.2189 0.5993 0.111 Uiso 1 1 calc R . . H15C H 0.0232 0.1734 0.6595 0.111 Uiso 1 1 calc R . . C16 C 0.0580(3) 0.3224(4) 0.5989(5) 0.168(5) Uani 1 1 d . . . H16A H 0.0716 0.3636 0.6266 0.252 Uiso 1 1 calc R . . H16B H 0.0011 0.3239 0.5672 0.252 Uiso 1 1 calc R . . H16C H 0.0970 0.3142 0.5627 0.252 Uiso 1 1 calc R . . C17 C 0.3040(2) 0.01411(15) 0.9405(2) 0.0338(7) Uani 1 1 d . . . C18 C 0.3408(5) -0.0219(3) 1.0206(4) 0.0478(18) Uani 0.653(10) 1 d P A 1 H18A H 0.3230 -0.0670 1.0161 0.072 Uiso 0.653(10) 1 calc PR A 1 H18B H 0.3210 -0.0015 1.0658 0.072 Uiso 0.653(10) 1 calc PR A 1 H18C H 0.4017 -0.0198 1.0303 0.072 Uiso 0.653(10) 1 calc PR A 1 C19 C 0.3713(5) 0.0335(3) 0.8944(5) 0.056(2) Uani 0.653(10) 1 d P A 1 H19A H 0.4175 0.0539 0.9318 0.084 Uiso 0.653(10) 1 calc PR A 1 H19B H 0.3482 0.0640 0.8514 0.084 Uiso 0.653(10) 1 calc PR A 1 H19C H 0.3916 -0.0048 0.8704 0.084 Uiso 0.653(10) 1 calc PR A 1 C20 C 0.2418(4) -0.0358(3) 0.8859(5) 0.060(2) Uani 0.653(10) 1 d P A 1 H20A H 0.2258 -0.0190 0.8306 0.089 Uiso 0.653(10) 1 calc PR A 1 H20B H 0.1919 -0.0414 0.9091 0.089 Uiso 0.653(10) 1 calc PR A 1 H20C H 0.2697 -0.0774 0.8847 0.089 Uiso 0.653(10) 1 calc PR A 1 C57 C 0.2922(12) 0.0047(9) 0.8460(8) 0.089(8) Uani 0.347(10) 1 d P A 2 C58 C 0.4048(9) 0.0312(7) 0.9647(14) 0.074(6) Uani 0.347(10) 1 d P A 2 C59 C 0.2848(14) -0.0428(7) 0.9880(14) 0.087(7) Uani 0.347(10) 1 d P A 2 C21 C 0.1832(2) 0.24712(15) 1.0486(2) 0.0325(7) Uani 1 1 d . . . C22 C 0.2624(3) 0.2896(2) 1.0642(4) 0.0817(17) Uani 1 1 d . . . H22A H 0.3065 0.2679 1.1026 0.123 Uiso 1 1 calc R . . H22B H 0.2498 0.3311 1.0867 0.123 Uiso 1 1 calc R . . H22C H 0.2810 0.2968 1.0130 0.123 Uiso 1 1 calc R . . C23 C 0.1544(4) 0.2341(2) 1.1295(3) 0.0825(18) Uani 1 1 d . . . H23A H 0.1075 0.2039 1.1200 0.124 Uiso 1 1 calc R . . H23B H 0.1369 0.2746 1.1509 0.124 Uiso 1 1 calc R . . H23C H 0.2005 0.2155 1.1688 0.124 Uiso 1 1 calc R . . C24 C 0.1144(4) 0.2860(2) 0.9912(3) 0.0810(17) Uani 1 1 d . . . H24A H 0.1326 0.2947 0.9401 0.122 Uiso 1 1 calc R . . H24B H 0.1047 0.3268 1.0170 0.122 Uiso 1 1 calc R . . H24C H 0.0628 0.2609 0.9803 0.122 Uiso 1 1 calc R . . C25 C 0.34370(18) 0.00285(14) 0.27250(18) 0.0274(6) Uani 1 1 d . . . C26 C 0.31590(19) 0.05027(15) 0.21284(18) 0.0268(6) Uani 1 1 d . . . H26 H 0.3512 0.0828 0.1988 0.032 Uiso 1 1 calc R . . C27 C 0.22883(19) 0.04462(15) 0.17522(17) 0.0272(6) Uani 1 1 d . . . H27 H 0.2017 0.0734 0.1348 0.033 Uiso 1 1 calc R . . C28 C 0.18782(18) -0.00758(14) 0.20406(17) 0.0254(6) Uani 1 1 d . . . C29 C 0.24919(19) 0.18233(13) 0.46212(18) 0.0246(6) Uani 1 1 d . B . C30 C 0.16231(19) 0.17221(14) 0.44274(19) 0.0274(6) Uani 1 1 d . . . H30 H 0.1245 0.2037 0.4164 0.033 Uiso 1 1 calc R . . C31 C 0.13575(18) 0.11014(14) 0.46627(18) 0.0276(6) Uani 1 1 d . . . H31 H 0.0792 0.0970 0.4565 0.033 Uiso 1 1 calc R . . C32 C 0.20225(19) 0.07024(14) 0.50560(18) 0.0249(6) Uani 1 1 d . . . C33 C 0.43620(19) -0.00587(17) 0.3167(2) 0.0341(7) Uani 1 1 d . . . C34 C 0.4875(3) -0.0278(3) 0.2542(3) 0.0855(18) Uani 1 1 d . . . H34A H 0.5462 -0.0315 0.2806 0.128 Uiso 1 1 calc R . . H34B H 0.4818 0.0038 0.2103 0.128 Uiso 1 1 calc R . . H34C H 0.4671 -0.0697 0.2320 0.128 Uiso 1 1 calc R . . C35 C 0.4721(3) 0.0589(2) 0.3556(3) 0.0621(12) Uani 1 1 d . . . H35A H 0.4399 0.0727 0.3958 0.093 Uiso 1 1 calc R . . H35B H 0.4685 0.0918 0.3133 0.093 Uiso 1 1 calc R . . H35C H 0.5304 0.0528 0.3820 0.093 Uiso 1 1 calc R . . C36 C 0.4440(3) -0.0554(3) 0.3858(3) 0.0801(17) Uani 1 1 d . . . H36A H 0.4196 -0.0964 0.3641 0.120 Uiso 1 1 calc R . . H36B H 0.4144 -0.0396 0.4271 0.120 Uiso 1 1 calc R . . H36C H 0.5028 -0.0617 0.4100 0.120 Uiso 1 1 calc R . . C37 C 0.09449(19) -0.02397(16) 0.1727(2) 0.0330(7) Uani 1 1 d . . . C38 C 0.0395(2) 0.0375(2) 0.1718(4) 0.0822(18) Uani 1 1 d . . . H38A H 0.0459 0.0547 0.2269 0.123 Uiso 1 1 calc R . . H38B H -0.0189 0.0264 0.1513 0.123 Uiso 1 1 calc R . . H38C H 0.0571 0.0701 0.1365 0.123 Uiso 1 1 calc R . . C39 C 0.0846(2) -0.04960(19) 0.0845(2) 0.0428(8) Uani 1 1 d . . . H39A H 0.1020 -0.0162 0.0502 0.064 Uiso 1 1 calc R . . H39B H 0.0263 -0.0608 0.0637 0.064 Uiso 1 1 calc R . . H39C H 0.1194 -0.0879 0.0841 0.064 Uiso 1 1 calc R . . C40 C 0.0641(3) -0.0769(3) 0.2251(3) 0.0731(16) Uani 1 1 d . . . H40A H 0.0994 -0.1152 0.2264 0.110 Uiso 1 1 calc R . . H40B H 0.0063 -0.0883 0.2016 0.110 Uiso 1 1 calc R . . H40C H 0.0673 -0.0608 0.2804 0.110 Uiso 1 1 calc R . . C41 C 0.2944(2) 0.24511(15) 0.4440(2) 0.0327(7) Uani 1 1 d . . . C42 C 0.2314(4) 0.2957(3) 0.3932(4) 0.0491(19) Uani 0.687(10) 1 d P B 1 H42A H 0.1863 0.3048 0.4221 0.074 Uiso 0.687(10) 1 calc PR B 1 H42B H 0.2081 0.2776 0.3398 0.074 Uiso 0.687(10) 1 calc PR B 1 H42C H 0.2611 0.3356 0.3866 0.074 Uiso 0.687(10) 1 calc PR B 1 C43 C 0.3622(4) 0.2303(3) 0.3907(4) 0.0480(18) Uani 0.687(10) 1 d P B 1 H43A H 0.3828 0.2709 0.3724 0.072 Uiso 0.687(10) 1 calc PR B 1 H43B H 0.3371 0.2044 0.3436 0.072 Uiso 0.687(10) 1 calc PR B 1 H43C H 0.4086 0.2065 0.4233 0.072 Uiso 0.687(10) 1 calc PR B 1 C44 C 0.3374(5) 0.2777(3) 0.5228(4) 0.052(2) Uani 0.687(10) 1 d P B 1 H44A H 0.378(6) 0.248(4) 0.543(5) 0.078 Uiso 0.687(10) 1 d P B 1 H44B H 0.298(5) 0.279(4) 0.559(5) 0.078 Uiso 0.687(10) 1 d P B 1 H44C H 0.348(5) 0.323(4) 0.518(4) 0.078 Uiso 0.687(10) 1 d P B 1 C60 C 0.279(2) 0.2572(9) 0.3585(11) 0.115(12) Uani 0.313(10) 1 d P B 2 C61 C 0.2646(14) 0.2991(7) 0.4999(12) 0.074(6) Uani 0.313(10) 1 d P B 2 C62 C 0.3920(10) 0.2355(8) 0.4814(18) 0.099(10) Uani 0.313(10) 1 d P B 2 C45 C 0.1897(2) 0.00355(15) 0.54379(19) 0.0317(7) Uani 1 1 d . . . C46 C 0.2736(3) -0.03419(19) 0.5642(3) 0.0582(11) Uani 1 1 d . . . H46A H 0.2926 -0.0443 0.5139 0.087 Uiso 1 1 calc R . . H46B H 0.2654 -0.0742 0.5924 0.087 Uiso 1 1 calc R . . H46C H 0.3155 -0.0077 0.5990 0.087 Uiso 1 1 calc R . . C47 C 0.1551(3) 0.0150(2) 0.6234(2) 0.0570(11) Uani 1 1 d . . . H47A H 0.1436 -0.0266 0.6464 0.085 Uiso 1 1 calc R . . H47B H 0.1037 0.0402 0.6107 0.085 Uiso 1 1 calc R . . H47C H 0.1965 0.0385 0.6627 0.085 Uiso 1 1 calc R . . C48 C 0.1246(2) -0.03773(17) 0.4844(2) 0.0433(8) Uani 1 1 d . . . H48A H 0.1461 -0.0469 0.4353 0.065 Uiso 1 1 calc R . . H48B H 0.0722 -0.0138 0.4701 0.065 Uiso 1 1 calc R . . H48C H 0.1148 -0.0783 0.5108 0.065 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 Pb1 0.03055(7) 0.02638(7) 0.02201(7) 0.00261(4) 0.00340(5) -0.00418(4) Pb2 0.03190(7) 0.02500(7) 0.02274(7) -0.00406(4) 0.00390(5) 0.00024(4) P1 0.0308(4) 0.0203(4) 0.0347(4) -0.0022(3) 0.0039(3) -0.0004(3) P2 0.0220(3) 0.0271(4) 0.0243(4) -0.0012(3) 0.0033(3) -0.0011(3) P3 0.0330(4) 0.0199(4) 0.0343(4) 0.0026(3) 0.0082(3) -0.0013(3) P4 0.0226(3) 0.0301(4) 0.0252(4) -0.0027(3) 0.0003(3) 0.0022(3) C1 0.0274(14) 0.0237(14) 0.0223(14) 0.0009(11) 0.0037(11) -0.0016(11) C2 0.0318(16) 0.0279(15) 0.0239(15) -0.0072(12) 0.0048(12) -0.0004(12) C3 0.0330(16) 0.0325(16) 0.0181(14) -0.0049(12) 0.0034(12) -0.0028(13) C4 0.0272(15) 0.0318(16) 0.0206(14) 0.0050(12) 0.0002(11) -0.0016(12) C5 0.0305(15) 0.0206(14) 0.0215(14) 0.0036(11) 0.0069(12) 0.0015(11) C6 0.0295(16) 0.0254(15) 0.0277(16) 0.0020(11) 0.0049(12) -0.0070(12) C7 0.0207(13) 0.0287(15) 0.0309(16) 0.0027(12) 0.0070(12) -0.0025(11) C8 0.0268(15) 0.0255(15) 0.0208(14) 0.0009(11) 0.0071(12) -0.0007(11) C9 0.0269(15) 0.0304(16) 0.0319(16) -0.0030(13) 0.0050(12) -0.0087(12) C10 0.053(3) 0.132(5) 0.056(3) 0.030(3) 0.000(2) -0.052(3) C11 0.0277(19) 0.051(3) 0.143(5) -0.029(3) -0.026(2) 0.0057(18) C12 0.038(2) 0.086(3) 0.047(2) -0.029(2) -0.0015(17) -0.014(2) C13 0.0275(16) 0.0417(19) 0.0424(19) 0.0070(15) -0.0014(14) 0.0015(14) C14 0.038(2) 0.189(7) 0.100(4) -0.082(4) -0.011(3) 0.047(3) C15 0.0279(19) 0.103(4) 0.086(3) -0.035(3) 0.001(2) -0.005(2) C16 0.041(3) 0.175(7) 0.262(10) 0.180(7) -0.035(4) -0.015(4) C17 0.0434(18) 0.0263(16) 0.0341(17) -0.0020(13) 0.0133(14) 0.0062(14) C18 0.063(4) 0.043(4) 0.038(3) 0.004(3) 0.012(3) 0.024(3) C19 0.065(5) 0.044(3) 0.075(6) 0.009(3) 0.050(4) 0.014(3) C20 0.062(4) 0.041(4) 0.072(5) -0.028(3) 0.004(4) 0.012(3) C57 0.109(14) 0.107(14) 0.041(7) -0.043(8) -0.008(8) 0.059(12) C58 0.048(7) 0.051(8) 0.127(17) -0.023(9) 0.024(9) 0.015(6) C59 0.113(16) 0.030(7) 0.136(18) 0.033(9) 0.072(15) 0.046(9) C21 0.0397(17) 0.0271(16) 0.0326(17) -0.0069(13) 0.0119(14) 0.0015(13) C22 0.076(3) 0.043(2) 0.136(5) -0.051(3) 0.045(3) -0.023(2) C23 0.158(6) 0.046(3) 0.062(3) -0.009(2) 0.068(3) 0.001(3) C24 0.100(4) 0.051(3) 0.081(3) -0.023(2) -0.011(3) 0.041(3) C25 0.0271(15) 0.0277(15) 0.0279(15) -0.0046(12) 0.0065(12) -0.0016(12) C26 0.0277(15) 0.0283(15) 0.0244(15) 0.0031(12) 0.0052(12) -0.0025(12) C27 0.0322(15) 0.0319(16) 0.0180(14) -0.0019(12) 0.0061(12) -0.0009(13) C28 0.0282(15) 0.0264(15) 0.0216(14) -0.0074(11) 0.0049(11) -0.0010(12) C29 0.0262(15) 0.0238(15) 0.0249(15) -0.0049(11) 0.0077(12) 0.0002(11) C30 0.0274(15) 0.0275(15) 0.0271(16) -0.0002(12) 0.0045(12) 0.0040(12) C31 0.0228(14) 0.0281(15) 0.0319(16) -0.0019(12) 0.0055(12) 0.0010(12) C32 0.0281(15) 0.0277(15) 0.0201(14) -0.0018(11) 0.0078(12) 0.0001(11) C33 0.0261(15) 0.0419(18) 0.0333(17) 0.0036(14) 0.0030(13) 0.0052(13) C34 0.039(2) 0.150(5) 0.066(3) -0.029(3) 0.006(2) 0.036(3) C35 0.033(2) 0.061(3) 0.082(3) -0.003(2) -0.013(2) -0.0021(19) C36 0.044(2) 0.100(4) 0.087(4) 0.055(3) -0.011(2) -0.001(2) C37 0.0287(15) 0.0350(17) 0.0360(17) -0.0109(14) 0.0078(13) -0.0066(13) C38 0.0258(19) 0.067(3) 0.147(5) -0.055(3) 0.001(2) 0.0019(19) C39 0.0348(18) 0.049(2) 0.041(2) -0.0098(16) -0.0019(15) -0.0081(16) C40 0.050(2) 0.125(5) 0.043(2) 0.009(2) 0.0043(19) -0.047(3) C41 0.0363(17) 0.0252(15) 0.0372(18) -0.0032(13) 0.0088(14) -0.0057(13) C42 0.048(3) 0.024(3) 0.070(4) 0.018(3) -0.001(3) -0.003(2) C43 0.049(3) 0.039(3) 0.064(4) -0.001(3) 0.030(3) -0.013(3) C44 0.081(5) 0.033(3) 0.038(3) -0.005(2) 0.005(3) -0.027(3) C60 0.22(3) 0.060(12) 0.072(12) -0.005(9) 0.044(15) -0.090(18) C61 0.114(17) 0.028(7) 0.099(14) -0.015(7) 0.067(13) -0.023(8) C62 0.041(8) 0.055(10) 0.20(3) 0.002(12) 0.031(12) -0.026(7) C45 0.0384(17) 0.0272(16) 0.0297(16) 0.0033(13) 0.0072(13) 0.0000(13) C46 0.053(2) 0.039(2) 0.079(3) 0.022(2) 0.005(2) 0.0087(18) C47 0.096(3) 0.044(2) 0.037(2) 0.0031(17) 0.028(2) -0.005(2) C48 0.054(2) 0.0284(17) 0.049(2) 0.0031(15) 0.0123(17) -0.0090(16) _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 Pb1 C1 2.763(3) . ? Pb1 C2 2.796(3) . ? Pb1 C8 2.820(3) . ? Pb1 C7 2.860(3) . ? Pb1 C3 2.863(3) . ? Pb1 C4 2.872(3) . ? Pb1 P1 2.8732(8) . ? Pb1 C5 2.895(3) . ? Pb1 P2 2.9012(7) . ? Pb1 C6 2.905(3) . ? Pb2 C25 2.767(3) . ? Pb2 C32 2.799(3) . ? Pb2 C26 2.814(3) . ? Pb2 C28 2.843(3) . ? Pb2 C27 2.848(3) . ? Pb2 C31 2.856(3) . ? Pb2 P3 2.8681(8) . ? Pb2 P4 2.8842(8) . ? Pb2 C29 2.889(3) . ? Pb2 C30 2.908(3) . ? P1 C4 1.787(3) . ? P1 C1 1.789(3) . ? P2 C8 1.785(3) . ? P2 C5 1.787(3) . ? P3 C28 1.781(3) . ? P3 C25 1.787(3) . ? P4 C32 1.781(3) . ? P4 C29 1.789(3) . ? C1 C2 1.385(4) . ? C1 C9 1.530(4) . ? C2 C3 1.418(4) . ? C2 H2 0.9300 . ? C3 C4 1.381(4) . ? C3 H3 0.9300 . ? C4 C13 1.528(4) . ? C5 C6 1.391(4) . ? C5 C17 1.526(4) . ? C6 C7 1.415(4) . ? C6 H6 0.9300 . ? C7 C8 1.390(4) . ? C7 H7 0.9300 . ? C8 C21 1.525(4) . ? C9 C11 1.505(5) . ? C9 C12 1.505(5) . ? C9 C10 1.515(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C16 1.493(6) . ? C13 C14 1.516(6) . ? C13 C15 1.518(5) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C59 1.465(14) . ? C17 C19 1.491(6) . ? C17 C18 1.524(7) . ? C17 C57 1.545(13) . ? C17 C20 1.577(7) . ? C17 C58 1.626(14) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.517(5) . ? C21 C23 1.519(5) . ? C21 C24 1.527(5) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.388(4) . ? C25 C33 1.531(4) . ? C26 C27 1.418(4) . ? C26 H26 0.9300 . ? C27 C28 1.383(4) . ? C27 H27 0.9300 . ? C28 C37 1.523(4) . ? C29 C30 1.384(4) . ? C29 C41 1.528(4) . ? C30 C31 1.412(4) . ? C30 H30 0.9300 . ? C31 C32 1.396(4) . ? C31 H31 0.9300 . ? C32 C45 1.527(4) . ? C33 C36 1.507(5) . ? C33 C34 1.508(5) . ? C33 C35 1.528(5) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C40 1.521(5) . ? C37 C39 1.524(4) . ? C37 C38 1.530(5) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C60 1.406(19) . ? C41 C44 1.500(6) . ? C41 C43 1.557(6) . ? C41 C42 1.566(6) . ? C41 C61 1.568(15) . ? C41 C62 1.579(18) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.90(9) . ? C44 H44B 0.96(8) . ? C44 H44C 0.94(7) . ? C61 H44B 1.10(7) . ? C61 H44C 1.40(8) . ? C62 H44A 1.11(7) . ? C45 C46 1.530(5) . ? C45 C48 1.534(5) . ? C45 C47 1.540(5) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pb1 C2 28.84(8) . . ? C1 Pb1 C8 129.38(8) . . ? C2 Pb1 C8 156.04(9) . . ? C1 Pb1 C7 157.41(8) . . ? C2 Pb1 C7 172.65(8) . . ? C8 Pb1 C7 28.32(8) . . ? C1 Pb1 C3 49.26(8) . . ? C2 Pb1 C3 28.99(8) . . ? C8 Pb1 C3 166.33(9) . . ? C7 Pb1 C3 150.03(8) . . ? C1 Pb1 C4 53.73(8) . . ? C2 Pb1 C4 49.07(9) . . ? C8 Pb1 C4 138.48(8) . . ? C7 Pb1 C4 134.36(8) . . ? C3 Pb1 C4 27.86(9) . . ? C1 Pb1 P1 36.94(6) . . ? C2 Pb1 P1 55.00(6) . . ? C8 Pb1 P1 115.41(6) . . ? C7 Pb1 P1 132.13(6) . . ? C3 Pb1 P1 54.13(6) . . ? C4 Pb1 P1 36.25(6) . . ? C1 Pb1 C5 131.30(8) . . ? C2 Pb1 C5 126.27(9) . . ? C8 Pb1 C5 53.05(8) . . ? C7 Pb1 C5 48.33(8) . . ? C3 Pb1 C5 140.01(8) . . ? C4 Pb1 C5 164.76(8) . . ? P1 Pb1 C5 157.86(6) . . ? C1 Pb1 P2 110.89(6) . . ? C2 Pb1 P2 125.77(6) . . ? C8 Pb1 P2 36.33(6) . . ? C7 Pb1 P2 53.99(6) . . ? C3 Pb1 P2 154.50(6) . . ? C4 Pb1 P2 158.92(6) . . ? P1 Pb1 P2 122.67(2) . . ? C5 Pb1 P2 35.91(6) . . ? C1 Pb1 C6 158.98(8) . . ? C2 Pb1 C6 144.39(9) . . ? C8 Pb1 C6 48.52(8) . . ? C7 Pb1 C6 28.40(8) . . ? C3 Pb1 C6 139.03(9) . . ? C4 Pb1 C6 145.09(8) . . ? P1 Pb1 C6 160.48(6) . . ? C5 Pb1 C6 27.75(8) . . ? P2 Pb1 C6 53.53(6) . . ? C25 Pb2 C32 129.06(9) . . ? C25 Pb2 C26 28.79(8) . . ? C32 Pb2 C26 157.13(9) . . ? C25 Pb2 C28 53.92(8) . . ? C32 Pb2 C28 133.34(8) . . ? C26 Pb2 C28 49.07(8) . . ? C25 Pb2 C27 49.53(9) . . ? C32 Pb2 C27 161.38(9) . . ? C26 Pb2 C27 29.01(8) . . ? C28 Pb2 C27 28.12(8) . . ? C25 Pb2 C31 156.67(8) . . ? C32 Pb2 C31 28.56(8) . . ? C26 Pb2 C31 174.30(8) . . ? C28 Pb2 C31 129.46(8) . . ? C27 Pb2 C31 146.73(8) . . ? C25 Pb2 P3 36.92(6) . . ? C32 Pb2 P3 111.91(6) . . ? C26 Pb2 P3 54.82(6) . . ? C28 Pb2 P3 36.34(6) . . ? C27 Pb2 P3 54.40(6) . . ? C31 Pb2 P3 128.17(6) . . ? C25 Pb2 P4 112.92(6) . . ? C32 Pb2 P4 36.50(6) . . ? C26 Pb2 P4 129.71(6) . . ? C28 Pb2 P4 157.43(6) . . ? C27 Pb2 P4 158.65(6) . . ? C31 Pb2 P4 54.25(6) . . ? P3 Pb2 P4 121.47(2) . . ? C25 Pb2 C29 134.97(8) . . ? C32 Pb2 C29 53.24(8) . . ? C26 Pb2 C29 131.35(8) . . ? C28 Pb2 C29 166.19(8) . . ? C27 Pb2 C29 143.86(9) . . ? C31 Pb2 C29 48.33(8) . . ? P3 Pb2 C29 157.46(6) . . ? P4 Pb2 C29 36.10(6) . . ? C25 Pb2 C30 162.58(8) . . ? C32 Pb2 C30 48.64(8) . . ? C26 Pb2 C30 148.24(8) . . ? C28 Pb2 C30 142.68(8) . . ? C27 Pb2 C30 139.71(9) . . ? C31 Pb2 C30 28.35(8) . . ? P3 Pb2 C30 156.46(6) . . ? P4 Pb2 C30 53.62(6) . . ? C29 Pb2 C30 27.62(8) . . ? C4 P1 C1 90.89(13) . . ? C4 P1 Pb1 71.83(9) . . ? C1 P1 Pb1 68.19(9) . . ? C8 P2 C5 91.24(14) . . ? C8 P2 Pb1 69.36(10) . . ? C5 P2 Pb1 71.85(9) . . ? C28 P3 C25 90.97(14) . . ? C28 P3 Pb2 71.07(9) . . ? C25 P3 Pb2 68.45(10) . . ? C32 P4 C29 91.15(14) . . ? C32 P4 Pb2 69.14(10) . . ? C29 P4 Pb2 72.08(9) . . ? C2 C1 C9 125.1(3) . . ? C2 C1 P1 110.5(2) . . ? C9 C1 P1 124.2(2) . . ? C2 C1 Pb1 76.87(17) . . ? C9 C1 Pb1 119.26(18) . . ? P1 C1 Pb1 74.86(10) . . ? C1 C2 C3 113.7(3) . . ? C1 C2 Pb1 74.29(17) . . ? C3 C2 Pb1 78.15(17) . . ? C1 C2 H2 123.1 . . ? C3 C2 H2 123.1 . . ? Pb1 C2 H2 115.8 . . ? C4 C3 C2 114.5(3) . . ? C4 C3 Pb1 76.41(16) . . ? C2 C3 Pb1 72.86(16) . . ? C4 C3 H3 122.7 . . ? C2 C3 H3 122.7 . . ? Pb1 C3 H3 119.3 . . ? C3 C4 C13 125.3(3) . . ? C3 C4 P1 110.3(2) . . ? C13 C4 P1 124.4(2) . . ? C3 C4 Pb1 75.73(17) . . ? C13 C4 Pb1 120.9(2) . . ? P1 C4 Pb1 71.92(9) . . ? C6 C5 C17 125.1(3) . . ? C6 C5 P2 110.1(2) . . ? C17 C5 P2 124.7(2) . . ? C6 C5 Pb1 76.52(16) . . ? C17 C5 Pb1 119.66(19) . . ? P2 C5 Pb1 72.24(9) . . ? C5 C6 C7 114.2(3) . . ? C5 C6 Pb1 75.73(16) . . ? C7 C6 Pb1 74.05(16) . . ? C5 C6 H6 122.9 . . ? C7 C6 H6 122.9 . . ? Pb1 C6 H6 118.7 . . ? C8 C7 C6 114.1(3) . . ? C8 C7 Pb1 74.24(17) . . ? C6 C7 Pb1 77.56(17) . . ? C8 C7 H7 123.0 . . ? C6 C7 H7 123.0 . . ? Pb1 C7 H7 116.6 . . ? C7 C8 C21 124.1(3) . . ? C7 C8 P2 110.3(2) . . ? C21 C8 P2 125.4(2) . . ? C7 C8 Pb1 77.44(17) . . ? C21 C8 Pb1 119.60(19) . . ? P2 C8 Pb1 74.31(10) . . ? C11 C9 C12 109.0(3) . . ? C11 C9 C10 109.3(4) . . ? C12 C9 C10 108.3(3) . . ? C11 C9 C1 111.2(3) . . ? C12 C9 C1 110.9(3) . . ? C10 C9 C1 108.1(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C16 C13 C14 113.1(5) . . ? C16 C13 C15 108.5(5) . . ? C14 C13 C15 105.7(4) . . ? C16 C13 C4 108.0(3) . . ? C14 C13 C4 110.3(3) . . ? C15 C13 C4 111.2(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C59 C17 C19 137.0(7) . . ? C59 C17 C18 40.8(9) . . ? C19 C17 C18 111.9(5) . . ? C59 C17 C5 109.8(6) . . ? C19 C17 C5 111.2(3) . . ? C18 C17 C5 108.8(3) . . ? C59 C17 C57 116.4(12) . . ? C19 C17 C57 58.4(8) . . ? C18 C17 C57 139.9(6) . . ? C5 C17 C57 110.8(6) . . ? C59 C17 C20 67.7(10) . . ? C19 C17 C20 108.7(5) . . ? C18 C17 C20 106.3(5) . . ? C5 C17 C20 109.9(3) . . ? C57 C17 C20 53.5(8) . . ? C59 C17 C58 110.0(11) . . ? C19 C17 C58 44.1(7) . . ? C18 C17 C58 72.1(8) . . ? C5 C17 C58 108.2(5) . . ? C57 C17 C58 101.1(10) . . ? C20 C17 C58 140.0(6) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C23 110.0(4) . . ? C22 C21 C8 111.1(3) . . ? C23 C21 C8 109.4(3) . . ? C22 C21 C24 106.8(4) . . ? C23 C21 C24 109.1(4) . . ? C8 C21 C24 110.4(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C33 124.4(3) . . ? C26 C25 P3 110.3(2) . . ? C33 C25 P3 124.9(2) . . ? C26 C25 Pb2 77.50(17) . . ? C33 C25 Pb2 120.55(19) . . ? P3 C25 Pb2 74.63(10) . . ? C25 C26 C27 113.9(3) . . ? C25 C26 Pb2 73.71(17) . . ? C27 C26 Pb2 76.83(17) . . ? C25 C26 H26 123.0 . . ? C27 C26 H26 123.0 . . ? Pb2 C26 H26 117.8 . . ? C28 C27 C26 114.0(3) . . ? C28 C27 Pb2 75.75(16) . . ? C26 C27 Pb2 74.16(16) . . ? C28 C27 H27 123.0 . . ? C26 C27 H27 123.0 . . ? Pb2 C27 H27 118.5 . . ? C27 C28 C37 123.7(3) . . ? C27 C28 P3 110.7(2) . . ? C37 C28 P3 125.6(2) . . ? C27 C28 Pb2 76.13(16) . . ? C37 C28 Pb2 118.58(19) . . ? P3 C28 Pb2 72.59(9) . . ? C30 C29 C41 125.2(3) . . ? C30 C29 P4 110.2(2) . . ? C41 C29 P4 124.6(2) . . ? C30 C29 Pb2 76.95(17) . . ? C41 C29 Pb2 118.80(19) . . ? P4 C29 Pb2 71.82(9) . . ? C29 C30 C31 114.5(3) . . ? C29 C30 Pb2 75.42(17) . . ? C31 C30 Pb2 73.78(17) . . ? C29 C30 H30 122.7 . . ? C31 C30 H30 122.7 . . ? Pb2 C30 H30 119.4 . . ? C32 C31 C30 113.8(3) . . ? C32 C31 Pb2 73.45(17) . . ? C30 C31 Pb2 77.87(18) . . ? C32 C31 H31 123.1 . . ? C30 C31 H31 123.1 . . ? Pb2 C31 H31 116.9 . . ? C31 C32 C45 123.9(3) . . ? C31 C32 P4 110.3(2) . . ? C45 C32 P4 125.5(2) . . ? C31 C32 Pb2 77.99(17) . . ? C45 C32 Pb2 119.37(19) . . ? P4 C32 Pb2 74.37(10) . . ? C36 C33 C34 110.1(4) . . ? C36 C33 C35 106.9(4) . . ? C34 C33 C35 109.3(4) . . ? C36 C33 C25 111.5(3) . . ? C34 C33 C25 108.5(3) . . ? C35 C33 C25 110.5(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C40 C37 C28 111.5(3) . . ? C40 C37 C39 108.3(3) . . ? C28 C37 C39 108.0(3) . . ? C40 C37 C38 109.7(4) . . ? C28 C37 C38 110.6(3) . . ? C39 C37 C38 108.6(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C60 C41 C44 139.0(7) . . ? C60 C41 C29 110.0(7) . . ? C44 C41 C29 110.9(3) . . ? C60 C41 C43 58.4(13) . . ? C44 C41 C43 108.7(5) . . ? C29 C41 C43 111.1(3) . . ? C60 C41 C42 51.5(12) . . ? C44 C41 C42 108.2(4) . . ? C29 C41 C42 111.8(3) . . ? C43 C41 C42 106.0(4) . . ? C60 C41 C61 116.8(14) . . ? C44 C41 C61 47.4(9) . . ? C29 C41 C61 105.0(6) . . ? C43 C41 C61 142.7(6) . . ? C42 C41 C61 67.3(9) . . ? C60 C41 C62 112.6(16) . . ? C44 C41 C62 57.7(10) . . ? C29 C41 C62 107.1(7) . . ? C43 C41 C62 56.4(10) . . ? C42 C41 C62 141.1(7) . . ? C61 C41 C62 104.6(13) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 102(5) . . ? C41 C44 H44B 108(4) . . ? H44A C44 H44B 108(7) . . ? C41 C44 H44C 115(4) . . ? H44A C44 H44C 123(7) . . ? H44B C44 H44C 101(6) . . ? C41 C61 H44B 97(4) . . ? C41 C61 H44C 88(3) . . ? H44B C61 H44C 70(5) . . ? C41 C62 H44A 88(5) . . ? C32 C45 C46 110.8(3) . . ? C32 C45 C48 110.6(3) . . ? C46 C45 C48 109.0(3) . . ? C32 C45 C47 108.5(3) . . ? C46 C45 C47 109.7(3) . . ? C48 C45 C47 108.2(3) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.616 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.093 data_snp2_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H40 P2 Sn' _chemical_formula_weight 509.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Sn' 'Sn' -0.6537 1.4246 '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' '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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.0460(2) _cell_length_b 20.3280(2) _cell_length_c 16.3740(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.0890(6) _cell_angle_gamma 90.00 _cell_volume 5241.20(11) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 545 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 1.104 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10683 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 26.35 _reflns_number_total 10683 _reflns_number_gt 9926 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0319P)^2^+6.4407P] 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 10683 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0754 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.268616(9) 0.076663(7) 0.156816(9) 0.02278(5) Uani 1 1 d . . . Sn2 Sn 0.284305(9) 0.176695(7) 0.660133(9) 0.02287(5) Uani 1 1 d . . . P3 P 0.24295(4) -0.04933(3) 0.21594(4) 0.02583(12) Uani 1 1 d . . . P4 P 0.27269(4) 0.30156(3) 0.72944(4) 0.02585(12) Uani 1 1 d . . . P5 P 0.19874(3) 0.11093(3) -0.00912(3) 0.02367(12) Uani 1 1 d . . . P6 P 0.19834(3) 0.14753(3) 0.49614(3) 0.02267(12) Uani 1 1 d . . . C1 C 0.31332(14) -0.00535(11) 0.29482(13) 0.0238(4) Uani 1 1 d . . . C2 C 0.27148(14) 0.04618(11) 0.32511(13) 0.0251(4) Uani 1 1 d . . . H2 H 0.2978 0.0741 0.3673 0.030 Uiso 1 1 calc R . . C3 C 0.18482(14) 0.05242(11) 0.28592(13) 0.0251(4) Uani 1 1 d . . . H3 H 0.1494 0.0851 0.2996 0.030 Uiso 1 1 calc R . . C4 C 0.15780(14) 0.00501(11) 0.22511(13) 0.0240(4) Uani 1 1 d . . . C5 C 0.25079(14) 0.18227(10) 0.04053(14) 0.0230(4) Uani 1 1 d . A . C6 C 0.33796(14) 0.17239(11) 0.05901(14) 0.0243(4) Uani 1 1 d . . . H6 H 0.3758 0.2043 0.0844 0.029 Uiso 1 1 calc R . . C7 C 0.36441(14) 0.10987(11) 0.03601(14) 0.0247(4) Uani 1 1 d . . . H7 H 0.4210 0.0967 0.0459 0.030 Uiso 1 1 calc R . . C8 C 0.29811(14) 0.06978(11) -0.00277(13) 0.0225(4) Uani 1 1 d . . . C9 C 0.40681(15) -0.02201(12) 0.32664(15) 0.0302(5) Uani 1 1 d . . . C10 C 0.46114(19) 0.04019(18) 0.3305(3) 0.0815(15) Uani 1 1 d . . . H10A H 0.4584 0.0570 0.2753 0.122 Uiso 1 1 calc R . . H10B H 0.5190 0.0298 0.3547 0.122 Uiso 1 1 calc R . . H10C H 0.4401 0.0727 0.3639 0.122 Uiso 1 1 calc R . . C11 C 0.41549(17) -0.04917(14) 0.41487(16) 0.0386(6) Uani 1 1 d . . . H11A H 0.4742 -0.0578 0.4374 0.058 Uiso 1 1 calc R . . H11B H 0.3836 -0.0892 0.4135 0.058 Uiso 1 1 calc R . . H11C H 0.3941 -0.0175 0.4492 0.058 Uiso 1 1 calc R . . C12 C 0.4376(2) -0.0740(2) 0.2731(2) 0.0707(12) Uani 1 1 d . . . H12A H 0.4382 -0.0562 0.2189 0.106 Uiso 1 1 calc R . . H12B H 0.4002 -0.1113 0.2679 0.106 Uiso 1 1 calc R . . H12C H 0.4939 -0.0875 0.2986 0.106 Uiso 1 1 calc R . . C13 C 0.06544(15) -0.00385(13) 0.18083(15) 0.0306(5) Uani 1 1 d . . . C14 C 0.0156(2) -0.0282(3) 0.2444(2) 0.0797(14) Uani 1 1 d . . . H14A H 0.0391 -0.0692 0.2672 0.120 Uiso 1 1 calc R . . H14B H -0.0426 -0.0345 0.2181 0.120 Uiso 1 1 calc R . . H14C H 0.0189 0.0036 0.2882 0.120 Uiso 1 1 calc R . . C15 C 0.02781(19) 0.06131(17) 0.1440(2) 0.0568(9) Uani 1 1 d . . . H15A H -0.0307 0.0550 0.1187 0.085 Uiso 1 1 calc R . . H15B H 0.0587 0.0763 0.1028 0.085 Uiso 1 1 calc R . . H15C H 0.0319 0.0935 0.1875 0.085 Uiso 1 1 calc R . . C16 C 0.0586(2) -0.0522(2) 0.1095(2) 0.0720(12) Uani 1 1 d . . . H16A H 0.0807 -0.0941 0.1305 0.108 Uiso 1 1 calc R . . H16B H 0.0907 -0.0362 0.0698 0.108 Uiso 1 1 calc R . . H16C H 0.0001 -0.0570 0.0830 0.108 Uiso 1 1 calc R . . C17 C 0.31078(16) 0.00298(11) -0.04136(15) 0.0287(5) Uani 1 1 d . . . C18 C 0.3438(2) 0.01542(15) -0.12227(17) 0.0503(8) Uani 1 1 d . . . H18A H 0.3526 -0.0259 -0.1477 0.076 Uiso 1 1 calc R . . H18B H 0.3966 0.0390 -0.1097 0.076 Uiso 1 1 calc R . . H18C H 0.3029 0.0409 -0.1598 0.076 Uiso 1 1 calc R . . C19 C 0.37590(18) -0.03873(13) 0.01726(17) 0.0381(6) Uani 1 1 d . . . H19A H 0.3546 -0.0485 0.0668 0.057 Uiso 1 1 calc R . . H19B H 0.4283 -0.0148 0.0317 0.057 Uiso 1 1 calc R . . H19C H 0.3857 -0.0790 -0.0100 0.057 Uiso 1 1 calc R . . C20 C 0.22690(19) -0.03507(15) -0.0612(2) 0.0506(8) Uani 1 1 d . . . H20A H 0.2356 -0.0758 -0.0879 0.076 Uiso 1 1 calc R . . H20B H 0.1853 -0.0093 -0.0976 0.076 Uiso 1 1 calc R . . H20C H 0.2072 -0.0439 -0.0105 0.076 Uiso 1 1 calc R . . C21 C 0.20591(15) 0.24525(11) 0.05856(15) 0.0290(5) Uani 1 1 d . . . C22 C 0.2689(3) 0.2955(2) 0.1089(3) 0.0495(13) Uani 0.737(7) 1 d P A 1 H22A H 0.2383 0.3338 0.1206 0.074 Uiso 0.737(7) 1 calc PR A 1 H22B H 0.3107 0.3078 0.0770 0.074 Uiso 0.737(7) 1 calc PR A 1 H22C H 0.2965 0.2757 0.1603 0.074 Uiso 0.737(7) 1 calc PR A 1 C23 C 0.1386(3) 0.2306(2) 0.1126(3) 0.0498(13) Uani 0.737(7) 1 d P A 1 H23A H 0.1099 0.2706 0.1217 0.075 Uiso 0.737(7) 1 calc PR A 1 H23B H 0.1662 0.2128 0.1652 0.075 Uiso 0.737(7) 1 calc PR A 1 H23C H 0.0981 0.1994 0.0844 0.075 Uiso 0.737(7) 1 calc PR A 1 C24 C 0.1630(4) 0.2772(2) -0.0216(3) 0.0537(15) Uani 0.737(7) 1 d P A 1 H24A H 0.1222 0.2473 -0.0522 0.080 Uiso 0.737(7) 1 calc PR A 1 H24B H 0.2047 0.2881 -0.0542 0.080 Uiso 0.737(7) 1 calc PR A 1 H24C H 0.1346 0.3165 -0.0093 0.080 Uiso 0.737(7) 1 calc PR A 1 C25 C 0.2351(11) 0.2985(5) 0.0012(10) 0.059(5) Uani 0.263(7) 1 d P A 2 H25A H 0.2155 0.2867 -0.0560 0.089 Uiso 0.263(7) 1 calc PR A 2 H25B H 0.2960 0.3010 0.0126 0.089 Uiso 0.263(7) 1 calc PR A 2 H25C H 0.2119 0.3404 0.0120 0.089 Uiso 0.263(7) 1 calc PR A 2 C26 C 0.2294(16) 0.2617(9) 0.1441(9) 0.096(9) Uani 0.263(7) 1 d P A 2 H26A H 0.2047 0.2306 0.1767 0.145 Uiso 0.263(7) 1 calc PR A 2 H26B H 0.2092 0.3051 0.1530 0.145 Uiso 0.263(7) 1 calc PR A 2 H26C H 0.2901 0.2606 0.1606 0.145 Uiso 0.263(7) 1 calc PR A 2 C27 C 0.1091(8) 0.2359(7) 0.0234(16) 0.092(8) Uani 0.263(7) 1 d P A 2 H27A H 0.0998 0.2318 -0.0360 0.139 Uiso 0.263(7) 1 calc PR A 2 H27B H 0.0784 0.2734 0.0379 0.139 Uiso 0.263(7) 1 calc PR A 2 H27C H 0.0894 0.1969 0.0468 0.139 Uiso 0.263(7) 1 calc PR A 2 C28 C 0.34057(14) 0.25206(11) 0.80476(13) 0.0252(4) Uani 1 1 d . . . C29 C 0.29572(15) 0.20145(12) 0.83183(13) 0.0262(5) Uani 1 1 d . . . H29 H 0.3204 0.1710 0.8716 0.031 Uiso 1 1 calc R . . C30 C 0.20813(14) 0.19979(11) 0.79349(13) 0.0252(4) Uani 1 1 d . . . H30 H 0.1708 0.1677 0.8051 0.030 Uiso 1 1 calc R . . C31 C 0.18377(14) 0.25062(11) 0.73720(13) 0.0224(4) Uani 1 1 d . . . C32 C 0.24509(15) 0.07309(10) 0.54146(13) 0.0238(4) Uani 1 1 d . . . C33 C 0.33297(15) 0.07715(11) 0.55410(14) 0.0249(5) Uani 1 1 d . . . H33 H 0.3685 0.0430 0.5770 0.030 Uiso 1 1 calc R . . C34 C 0.36391(14) 0.13779(11) 0.52911(14) 0.0248(4) Uani 1 1 d . . . H34 H 0.4215 0.1473 0.5351 0.030 Uiso 1 1 calc R . . C35 C 0.30066(14) 0.18163(10) 0.49495(13) 0.0218(4) Uani 1 1 d . . . C36 C 0.43490(16) 0.26603(13) 0.83630(17) 0.0359(6) Uani 1 1 d . . . C37 C 0.4426(3) 0.3208(3) 0.8987(5) 0.158(4) Uani 1 1 d . . . H37A H 0.4217 0.3609 0.8711 0.237 Uiso 1 1 calc R . . H37B H 0.5011 0.3263 0.9247 0.237 Uiso 1 1 calc R . . H37C H 0.4099 0.3103 0.9403 0.237 Uiso 1 1 calc R . . C38 C 0.47967(19) 0.2054(2) 0.8795(3) 0.0675(11) Uani 1 1 d . . . H38A H 0.4537 0.1933 0.9254 0.101 Uiso 1 1 calc R . . H38B H 0.5386 0.2153 0.8995 0.101 Uiso 1 1 calc R . . H38C H 0.4749 0.1696 0.8406 0.101 Uiso 1 1 calc R . . C39 C 0.4789(2) 0.2812(3) 0.7645(3) 0.0979(19) Uani 1 1 d . . . H39A H 0.4693 0.2458 0.7249 0.147 Uiso 1 1 calc R . . H39B H 0.5387 0.2861 0.7850 0.147 Uiso 1 1 calc R . . H39C H 0.4564 0.3212 0.7380 0.147 Uiso 1 1 calc R . . C40 C 0.09208(14) 0.26563(11) 0.69524(14) 0.0265(5) Uani 1 1 d . . . C41 C 0.0544(2) 0.3106(2) 0.7527(2) 0.0729(13) Uani 1 1 d . . . H41A H 0.0878 0.3500 0.7628 0.109 Uiso 1 1 calc R . . H41B H 0.0543 0.2885 0.8044 0.109 Uiso 1 1 calc R . . H41C H -0.0028 0.3218 0.7270 0.109 Uiso 1 1 calc R . . C42 C 0.04021(19) 0.20309(16) 0.6786(3) 0.0685(12) Uani 1 1 d . . . H42A H -0.0172 0.2139 0.6531 0.103 Uiso 1 1 calc R . . H42B H 0.0405 0.1805 0.7301 0.103 Uiso 1 1 calc R . . H42C H 0.0644 0.1752 0.6419 0.103 Uiso 1 1 calc R . . C43 C 0.08979(18) 0.30061(18) 0.61273(19) 0.0514(8) Uani 1 1 d . . . H43A H 0.1126 0.2722 0.5756 0.077 Uiso 1 1 calc R . . H43B H 0.1232 0.3401 0.6219 0.077 Uiso 1 1 calc R . . H43C H 0.0322 0.3117 0.5885 0.077 Uiso 1 1 calc R . . C44 C 0.31699(16) 0.24746(11) 0.45564(15) 0.0291(5) Uani 1 1 d . . . C45 C 0.2374(2) 0.28959(17) 0.4384(3) 0.0703(12) Uani 1 1 d . . . H45A H 0.2493 0.3300 0.4125 0.106 Uiso 1 1 calc R . . H45B H 0.2194 0.2991 0.4897 0.106 Uiso 1 1 calc R . . H45C H 0.1931 0.2663 0.4019 0.106 Uiso 1 1 calc R . . C46 C 0.3859(3) 0.28633(17) 0.5130(2) 0.0664(11) Uani 1 1 d . . . H46A H 0.3980 0.3259 0.4856 0.100 Uiso 1 1 calc R . . H46B H 0.4365 0.2601 0.5263 0.100 Uiso 1 1 calc R . . H46C H 0.3665 0.2973 0.5633 0.100 Uiso 1 1 calc R . . C47 C 0.3455(3) 0.23346(16) 0.3735(2) 0.0684(11) Uani 1 1 d . . . H47A H 0.3022 0.2089 0.3375 0.103 Uiso 1 1 calc R . . H47B H 0.3972 0.2084 0.3842 0.103 Uiso 1 1 calc R . . H47C H 0.3551 0.2743 0.3473 0.103 Uiso 1 1 calc R . . C48 C 0.19548(16) 0.01301(12) 0.56125(15) 0.0321(5) Uani 1 1 d . . . C49 C 0.2543(3) -0.0346(3) 0.6186(4) 0.121(2) Uani 1 1 d . . . H49A H 0.2766 -0.0132 0.6704 0.182 Uiso 1 1 calc R . . H49B H 0.3003 -0.0476 0.5923 0.182 Uiso 1 1 calc R . . H49C H 0.2228 -0.0729 0.6289 0.182 Uiso 1 1 calc R . . C50 C 0.1243(4) 0.0315(2) 0.6009(5) 0.158(4) Uani 1 1 d . . . H50A H 0.1452 0.0564 0.6504 0.236 Uiso 1 1 calc R . . H50B H 0.0965 -0.0075 0.6151 0.236 Uiso 1 1 calc R . . H50C H 0.0846 0.0577 0.5630 0.236 Uiso 1 1 calc R . . C51 C 0.1649(4) -0.0249(2) 0.4829(3) 0.1002(19) Uani 1 1 d . . . H51A H 0.1341 -0.0630 0.4952 0.150 Uiso 1 1 calc R . . H51B H 0.2127 -0.0385 0.4597 0.150 Uiso 1 1 calc R . . H51C H 0.1283 0.0024 0.4437 0.150 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 Sn1 0.02713(9) 0.02154(9) 0.01926(8) 0.00279(5) 0.00343(6) -0.00042(5) Sn2 0.02644(9) 0.02290(9) 0.01884(8) -0.00131(5) 0.00330(6) 0.00372(6) P3 0.0292(3) 0.0189(3) 0.0301(3) -0.0020(2) 0.0075(2) 0.0011(2) P4 0.0276(3) 0.0190(3) 0.0300(3) 0.0027(2) 0.0030(2) 0.0006(2) P5 0.0206(3) 0.0267(3) 0.0223(3) 0.0022(2) 0.0006(2) -0.0019(2) P6 0.0205(3) 0.0253(3) 0.0218(3) 0.0011(2) 0.0031(2) 0.0009(2) C1 0.0253(11) 0.0249(11) 0.0216(10) 0.0058(8) 0.0055(8) 0.0021(8) C2 0.0284(11) 0.0291(12) 0.0174(10) -0.0016(9) 0.0037(8) -0.0001(9) C3 0.0251(11) 0.0283(11) 0.0227(10) -0.0028(9) 0.0070(9) 0.0039(9) C4 0.0240(11) 0.0258(11) 0.0229(10) 0.0010(9) 0.0061(9) -0.0001(8) C5 0.0261(11) 0.0219(11) 0.0214(10) 0.0041(8) 0.0052(9) 0.0008(8) C6 0.0233(11) 0.0236(11) 0.0257(11) 0.0005(9) 0.0043(9) -0.0037(8) C7 0.0207(10) 0.0255(11) 0.0280(11) 0.0007(9) 0.0052(9) -0.0009(8) C8 0.0253(11) 0.0227(11) 0.0205(10) 0.0013(8) 0.0073(8) -0.0004(8) C9 0.0251(11) 0.0337(13) 0.0317(12) 0.0085(10) 0.0050(9) 0.0066(9) C10 0.0241(14) 0.061(2) 0.150(4) 0.060(3) -0.0072(19) -0.0046(14) C11 0.0354(13) 0.0435(15) 0.0338(13) 0.0092(11) -0.0009(11) 0.0092(11) C12 0.0474(19) 0.120(3) 0.0413(17) -0.0141(19) 0.0014(14) 0.047(2) C13 0.0238(11) 0.0370(13) 0.0306(12) -0.0036(10) 0.0044(9) -0.0046(9) C14 0.0409(18) 0.139(4) 0.057(2) 0.028(2) 0.0043(16) -0.041(2) C15 0.0276(14) 0.0545(19) 0.080(2) -0.0003(17) -0.0103(14) 0.0043(13) C16 0.0403(17) 0.093(3) 0.074(2) -0.049(2) -0.0110(16) -0.0006(18) C17 0.0363(12) 0.0233(11) 0.0273(11) -0.0045(9) 0.0083(10) -0.0017(9) C18 0.090(2) 0.0358(15) 0.0311(14) -0.0041(12) 0.0255(15) 0.0042(15) C19 0.0482(15) 0.0263(12) 0.0404(14) -0.0052(11) 0.0100(12) 0.0086(11) C20 0.0467(17) 0.0344(15) 0.068(2) -0.0200(14) 0.0043(15) -0.0083(12) C21 0.0318(12) 0.0231(11) 0.0325(12) 0.0028(9) 0.0073(10) 0.0062(9) C22 0.047(2) 0.032(2) 0.068(3) -0.019(2) 0.005(2) 0.0053(17) C23 0.049(3) 0.037(2) 0.072(3) -0.001(2) 0.033(2) 0.0134(18) C24 0.084(4) 0.038(2) 0.036(2) 0.0025(17) 0.005(2) 0.032(2) C25 0.093(12) 0.021(5) 0.079(10) 0.010(6) 0.050(9) 0.020(6) C26 0.18(2) 0.066(11) 0.057(9) 0.005(8) 0.054(11) 0.076(14) C27 0.040(7) 0.033(7) 0.21(3) -0.002(10) 0.027(10) 0.014(5) C28 0.0262(11) 0.0275(11) 0.0204(10) -0.0038(9) 0.0007(8) 0.0022(9) C29 0.0303(12) 0.0309(12) 0.0163(10) 0.0044(9) 0.0018(9) 0.0042(9) C30 0.0275(11) 0.0275(11) 0.0210(10) 0.0042(9) 0.0059(9) 0.0007(9) C31 0.0242(10) 0.0230(10) 0.0202(10) -0.0007(8) 0.0050(8) 0.0031(8) C32 0.0316(12) 0.0213(11) 0.0192(10) -0.0010(8) 0.0071(9) -0.0016(8) C33 0.0292(11) 0.0221(11) 0.0239(11) 0.0002(8) 0.0061(9) 0.0058(8) C34 0.0214(10) 0.0259(11) 0.0280(11) -0.0010(9) 0.0071(9) 0.0017(8) C35 0.0239(11) 0.0222(11) 0.0200(10) -0.0004(8) 0.0065(8) 0.0001(8) C36 0.0253(12) 0.0405(14) 0.0387(14) -0.0052(11) -0.0020(10) -0.0017(10) C37 0.041(2) 0.158(5) 0.246(8) -0.166(6) -0.045(3) 0.020(3) C38 0.0250(14) 0.095(3) 0.079(2) 0.033(2) 0.0003(15) 0.0054(16) C39 0.0376(18) 0.164(5) 0.085(3) 0.069(3) -0.0063(18) -0.039(2) C40 0.0224(11) 0.0286(12) 0.0280(11) 0.0028(9) 0.0038(9) 0.0070(9) C41 0.0473(19) 0.118(3) 0.0490(19) -0.026(2) -0.0007(15) 0.048(2) C42 0.0264(14) 0.0427(17) 0.123(3) 0.023(2) -0.0185(17) -0.0041(12) C43 0.0328(14) 0.074(2) 0.0444(16) 0.0270(16) 0.0000(12) 0.0111(14) C44 0.0357(12) 0.0240(11) 0.0295(12) 0.0046(9) 0.0115(10) -0.0015(9) C45 0.063(2) 0.0413(18) 0.115(3) 0.043(2) 0.038(2) 0.0178(16) C46 0.083(3) 0.0452(18) 0.064(2) 0.0173(16) -0.0041(19) -0.0343(18) C47 0.131(4) 0.0381(17) 0.0503(19) 0.0086(14) 0.052(2) -0.0028(19) C48 0.0413(14) 0.0250(12) 0.0325(12) 0.0002(10) 0.0129(11) -0.0089(10) C49 0.120(4) 0.089(3) 0.134(5) 0.077(3) -0.032(3) -0.053(3) C50 0.171(6) 0.044(2) 0.320(9) -0.021(4) 0.203(7) -0.031(3) C51 0.167(5) 0.073(3) 0.077(3) -0.033(2) 0.065(3) -0.082(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 P3 2.7965(6) . ? Sn1 P5 2.8200(6) . ? Sn2 P4 2.8012(6) . ? Sn2 P6 2.8354(6) . ? P3 C1 1.784(2) . ? P3 C4 1.786(2) . ? P4 C31 1.787(2) . ? P4 C28 1.790(2) . ? P5 C8 1.786(2) . ? P5 C5 1.789(2) . ? P6 C32 1.786(2) . ? P6 C35 1.786(2) . ? C1 C2 1.386(3) . ? C1 C9 1.528(3) . ? C2 C3 1.421(3) . ? C2 H2 0.9300 . ? C3 C4 1.394(3) . ? C3 H3 0.9300 . ? C4 C13 1.530(3) . ? C5 C6 1.388(3) . ? C5 C21 1.525(3) . ? C6 C7 1.414(3) . ? C6 H6 0.9300 . ? C7 C8 1.393(3) . ? C7 H7 0.9300 . ? C8 C17 1.528(3) . ? C9 C12 1.516(4) . ? C9 C11 1.528(3) . ? C9 C10 1.530(4) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.513(4) . ? C13 C16 1.515(4) . ? C13 C15 1.530(4) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C19 1.532(4) . ? C17 C20 1.532(4) . ? C17 C18 1.540(3) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C26 1.419(16) . ? C21 C24 1.507(4) . ? C21 C23 1.551(5) . ? C21 C22 1.557(5) . ? C21 C27 1.561(15) . ? C21 C25 1.562(12) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.377(3) . ? C28 C36 1.529(3) . ? C29 C30 1.425(3) . ? C29 H29 0.9300 . ? C30 C31 1.390(3) . ? C30 H30 0.9300 . ? C31 C40 1.530(3) . ? C32 C33 1.388(3) . ? C32 C48 1.526(3) . ? C33 C34 1.418(3) . ? C33 H33 0.9300 . ? C34 C35 1.385(3) . ? C34 H34 0.9300 . ? C35 C44 1.529(3) . ? C36 C37 1.500(5) . ? C36 C39 1.515(5) . ? C36 C38 1.529(4) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C42 1.515(4) . ? C40 C41 1.518(4) . ? C40 C43 1.521(4) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C45 1.518(4) . ? C44 C46 1.526(4) . ? C44 C47 1.528(4) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C50 1.467(5) . ? C48 C51 1.496(4) . ? C48 C49 1.540(5) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? 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 P3 Sn1 P5 120.138(18) . . ? P4 Sn2 P6 120.999(18) . . ? C1 P3 C4 90.98(10) . . ? C1 P3 Sn1 71.14(7) . . ? C4 P3 Sn1 68.19(7) . . ? C31 P4 C28 90.78(10) . . ? C31 P4 Sn2 67.67(7) . . ? C28 P4 Sn2 71.98(7) . . ? C8 P5 C5 91.13(10) . . ? C8 P5 Sn1 69.09(7) . . ? C5 P5 Sn1 72.42(7) . . ? C32 P6 C35 91.15(10) . . ? C32 P6 Sn2 72.22(7) . . ? C35 P6 Sn2 69.41(7) . . ? C2 C1 C9 123.8(2) . . ? C2 C1 P3 110.80(16) . . ? C9 C1 P3 125.37(17) . . ? C1 C2 C3 113.9(2) . . ? C1 C2 H2 123.0 . . ? C3 C2 H2 123.0 . . ? C4 C3 C2 113.8(2) . . ? C4 C3 H3 123.1 . . ? C2 C3 H3 123.1 . . ? C3 C4 C13 124.0(2) . . ? C3 C4 P3 110.49(16) . . ? C13 C4 P3 125.05(17) . . ? C6 C5 C21 125.0(2) . . ? C6 C5 P5 110.16(16) . . ? C21 C5 P5 124.88(17) . . ? C5 C6 C7 114.4(2) . . ? C5 C6 H6 122.8 . . ? C7 C6 H6 122.8 . . ? C8 C7 C6 113.9(2) . . ? C8 C7 H7 123.0 . . ? C6 C7 H7 123.0 . . ? C7 C8 C17 123.9(2) . . ? C7 C8 P5 110.35(16) . . ? C17 C8 P5 125.50(17) . . ? C12 C9 C11 108.3(2) . . ? C12 C9 C1 111.4(2) . . ? C11 C9 C1 107.91(19) . . ? C12 C9 C10 110.7(3) . . ? C11 C9 C10 108.2(3) . . ? C1 C9 C10 110.2(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C16 110.4(3) . . ? C14 C13 C4 107.7(2) . . ? C16 C13 C4 111.2(2) . . ? C14 C13 C15 109.5(3) . . ? C16 C13 C15 107.1(3) . . ? C4 C13 C15 110.9(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C8 C17 C19 111.21(19) . . ? C8 C17 C20 110.8(2) . . ? C19 C17 C20 108.6(2) . . ? C8 C17 C18 107.8(2) . . ? C19 C17 C18 108.9(2) . . ? C20 C17 C18 109.5(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C24 138.4(6) . . ? C26 C21 C5 110.1(6) . . ? C24 C21 C5 110.3(2) . . ? C26 C21 C23 64.1(10) . . ? C24 C21 C23 109.1(3) . . ? C5 C21 C23 110.8(2) . . ? C26 C21 C22 45.6(10) . . ? C24 C21 C22 108.7(3) . . ? C5 C21 C22 111.7(2) . . ? C23 C21 C22 106.0(3) . . ? C26 C21 C27 116.7(12) . . ? C24 C21 C27 58.4(8) . . ? C5 C21 C27 107.5(6) . . ? C23 C21 C27 55.6(9) . . ? C22 C21 C27 140.7(6) . . ? C26 C21 C25 112.1(11) . . ? C24 C21 C25 47.0(7) . . ? C5 C21 C25 104.9(4) . . ? C23 C21 C25 142.9(5) . . ? C22 C21 C25 68.0(7) . . ? C27 C21 C25 104.8(10) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? C21 C25 H25A 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C21 C27 H27A 109.5 . . ? C21 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C21 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C36 125.1(2) . . ? C29 C28 P4 110.82(17) . . ? C36 C28 P4 124.06(18) . . ? C28 C29 C30 114.1(2) . . ? C28 C29 H29 123.0 . . ? C30 C29 H29 123.0 . . ? C31 C30 C29 113.7(2) . . ? C31 C30 H30 123.1 . . ? C29 C30 H30 123.1 . . ? C30 C31 C40 124.7(2) . . ? C30 C31 P4 110.57(16) . . ? C40 C31 P4 124.37(16) . . ? C33 C32 C48 124.9(2) . . ? C33 C32 P6 110.19(16) . . ? C48 C32 P6 124.87(18) . . ? C32 C33 C34 114.2(2) . . ? C32 C33 H33 122.9 . . ? C34 C33 H33 122.9 . . ? C35 C34 C33 113.9(2) . . ? C35 C34 H34 123.0 . . ? C33 C34 H34 123.0 . . ? C34 C35 C44 124.2(2) . . ? C34 C35 P6 110.45(16) . . ? C44 C35 P6 125.22(16) . . ? C37 C36 C39 112.9(4) . . ? C37 C36 C28 108.3(2) . . ? C39 C36 C28 110.7(2) . . ? C37 C36 C38 108.2(4) . . ? C39 C36 C38 106.0(3) . . ? C28 C36 C38 110.7(2) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C40 C41 110.3(3) . . ? C42 C40 C43 108.3(3) . . ? C41 C40 C43 108.9(3) . . ? C42 C40 C31 111.2(2) . . ? C41 C40 C31 107.8(2) . . ? C43 C40 C31 110.43(19) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C46 107.8(3) . . ? C45 C44 C47 108.9(3) . . ? C46 C44 C47 109.5(3) . . ? C45 C44 C35 111.5(2) . . ? C46 C44 C35 110.9(2) . . ? C47 C44 C35 108.2(2) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C50 C48 C51 110.9(4) . . ? C50 C48 C32 111.8(2) . . ? C51 C48 C32 109.2(2) . . ? C50 C48 C49 109.3(4) . . ? C51 C48 C49 105.1(4) . . ? C32 C48 C49 110.4(2) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C48 C51 H51A 109.5 . . ? C48 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C48 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.354 _refine_diff_density_min -0.921 _refine_diff_density_rms 0.069