Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Maurizio Peruzzini' 'Pierluigi Barbaro' 'V. Bertolasi' 'Claudio Bianchini' 'de los Rios,Isaac' 'Nicoletta, Mantovani' 'Lorenza, Marvelli' "Roberto, Rossi'" _publ_contact_author_name 'Dr Maurizio Peruzzini' _publ_contact_author_address ; ICCOM CNR Via Jacopo Nardi, 39 Firenze 50132 ITALY ; _publ_contact_author_email PERUZ@FI.CNR.IT _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Nucleophilic Addition of Phosphines to Rhenium Allenylidenes. Unprecedented Double P-H Bond Activation to Give an h1-P-Phosphabutadienyl Ligand ; data_(I) _database_code_CSD 207882 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H49 O2 P3 Re, C24 H20 B' _chemical_formula_sum 'C82 H69 B O2 P3 Re' _chemical_formula_weight 1376.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 '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' P P 0.1023 0.0942 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2030(2) _cell_length_b 16.7569(3) _cell_length_c 19.3716(5) _cell_angle_alpha 113.430(1) _cell_angle_beta 105.697(1) _cell_angle_gamma 93.961(1) _cell_volume 3428.3(1) _cell_formula_units_Z 2 _cell_measurement_temperature 295 _cell_measurement_reflns_used 52404 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 1.889 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.645 _exptl_absorpt_correction_T_max 0.829 _exptl_absorpt_process_details ; SORTAV: R.H. Blessing, Acta Crystallogr. Sect A, 1995, 51, 33 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295 _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 'Nonius Kappa CCD' _diffrn_measurement_method '\f scans and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52404 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_av_sigmaI/netI 0.0720 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3 _diffrn_reflns_theta_max 30 _reflns_number_total 19771 _reflns_number_gt 15139 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Kappa CCD server software' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III (Burnett & Johnson, 1996)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995) ; _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^)+(0.0494P)^2^+2.1037P] 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 19771 _refine_ls_number_parameters 803 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Re1 Re 0.003840(11) -0.179574(9) -0.154312(8) 0.04434(6) Uani 1 1 d . . . P1 P 0.08134(8) -0.30425(7) -0.23415(6) 0.0493(2) Uani 1 1 d . . . P2 P -0.16520(8) -0.29630(7) -0.19345(6) 0.0484(2) Uani 1 1 d . . . P3 P -0.08640(8) -0.17056(6) -0.28086(6) 0.04507(19) Uani 1 1 d . . . O1 O -0.1158(3) -0.0345(2) -0.0644(2) 0.0853(11) Uani 1 1 d . . . O2 O 0.2247(3) -0.0391(2) -0.0975(2) 0.0823(10) Uani 1 1 d . . . C1 C -0.0721(3) -0.0892(3) -0.0985(2) 0.0586(10) Uani 1 1 d . . . C2 C 0.1421(4) -0.0920(3) -0.1221(2) 0.0574(9) Uani 1 1 d . . . C3 C 0.0801(3) -0.1812(2) -0.0499(2) 0.0506(8) Uani 1 1 d . . . C4 C 0.1350(4) -0.1712(3) 0.0177(2) 0.0592(10) Uani 1 1 d . . . C5 C 0.2088(4) -0.1579(3) 0.0896(2) 0.0586(9) Uani 1 1 d . . . C6 C 0.3337(4) -0.1236(3) 0.1106(2) 0.0612(10) Uani 1 1 d . . . C7 C 0.3702(4) -0.0680(3) 0.0805(3) 0.0693(11) Uani 1 1 d . . . H7 H 0.3155 -0.0516 0.0474 0.083 Uiso 1 1 calc R . . C8 C 0.4879(5) -0.0365(4) 0.0994(3) 0.0818(14) Uani 1 1 d . . . H8 H 0.5115 0.0008 0.0789 0.098 Uiso 1 1 calc R . . C9 C 0.5693(5) -0.0603(4) 0.1479(4) 0.0851(16) Uani 1 1 d . . . H9 H 0.6479 -0.0380 0.1616 0.102 Uiso 1 1 calc R . . C10 C 0.5347(5) -0.1171(4) 0.1763(4) 0.0891(17) Uani 1 1 d . . . H10 H 0.5903 -0.1344 0.2081 0.107 Uiso 1 1 calc R . . C11 C 0.4179(4) -0.1491(4) 0.1583(3) 0.0742(12) Uani 1 1 d . . . H11 H 0.3954 -0.1876 0.1780 0.089 Uiso 1 1 calc R . . C12 C 0.1634(4) -0.1796(4) 0.1439(3) 0.0684(11) Uani 1 1 d . . . C13 C 0.0637(5) -0.2455(4) 0.1137(4) 0.0893(16) Uani 1 1 d . . . H13 H 0.0257 -0.2741 0.0591 0.107 Uiso 1 1 calc R . . C14 C 0.0219(7) -0.2682(7) 0.1628(5) 0.124(3) Uani 1 1 d . . . H14 H -0.0428 -0.3136 0.1419 0.148 Uiso 1 1 calc R . . C15 C 0.0765(9) -0.2231(10) 0.2448(7) 0.167(5) Uani 1 1 d . . . H15 H 0.0486 -0.2385 0.2789 0.200 Uiso 1 1 calc R . . C16 C 0.1706(8) -0.1568(8) 0.2747(5) 0.151(4) Uani 1 1 d . . . H16 H 0.2053 -0.1260 0.3296 0.181 Uiso 1 1 calc R . . C17 C 0.2151(5) -0.1344(5) 0.2260(3) 0.0975(19) Uani 1 1 d . . . H17 H 0.2800 -0.0889 0.2477 0.117 Uiso 1 1 calc R . . C18 C -0.2338(3) -0.3487(3) -0.3023(2) 0.0517(8) Uani 1 1 d . . . H181 H -0.2807 -0.4060 -0.3179 0.062 Uiso 1 1 calc R . . H182 H -0.2858 -0.3124 -0.3165 0.062 Uiso 1 1 calc R . . C19 C -0.1487(3) -0.3627(3) -0.3514(2) 0.0504(8) Uani 1 1 d . . . C20 C -0.2120(4) -0.4401(3) -0.4341(3) 0.0637(11) Uani 1 1 d . . . H201 H -0.1642 -0.4474 -0.4674 0.076 Uiso 1 1 calc R . . H202 H -0.2843 -0.4273 -0.4579 0.076 Uiso 1 1 calc R . . H203 H -0.2268 -0.4938 -0.4284 0.076 Uiso 1 1 calc R . . C21 C -0.1168(3) -0.2802(3) -0.3658(2) 0.0509(8) Uani 1 1 d . . . H211 H -0.1803 -0.2815 -0.4093 0.061 Uiso 1 1 calc R . . H212 H -0.0490 -0.2862 -0.3831 0.061 Uiso 1 1 calc R . . C22 C -0.0397(3) -0.3921(3) -0.3146(2) 0.0551(9) Uani 1 1 d . . . H221 H -0.0102 -0.4258 -0.3570 0.066 Uiso 1 1 calc R . . H222 H -0.0635 -0.4321 -0.2941 0.066 Uiso 1 1 calc R . . C23 C 0.1783(3) -0.2869(3) -0.2867(2) 0.0545(9) Uani 1 1 d . . . C24 C 0.2194(3) -0.2033(3) -0.2788(3) 0.0622(10) Uani 1 1 d . . . H24 H 0.1970 -0.1540 -0.2463 0.075 Uiso 1 1 calc R . . C25 C 0.2937(4) -0.1926(4) -0.3191(3) 0.0750(13) Uani 1 1 d . . . H25 H 0.3208 -0.1362 -0.3132 0.090 Uiso 1 1 calc R . . C26 C 0.3275(4) -0.2650(4) -0.3675(3) 0.0791(15) Uani 1 1 d . . . H26 H 0.3771 -0.2578 -0.3945 0.095 Uiso 1 1 calc R . . C27 C 0.2878(4) -0.3474(4) -0.3757(3) 0.0791(15) Uani 1 1 d . . . H27 H 0.3105 -0.3963 -0.4085 0.095 Uiso 1 1 calc R . . C28 C 0.2139(4) -0.3595(3) -0.3359(3) 0.0706(12) Uani 1 1 d . . . H28 H 0.1881 -0.4161 -0.3419 0.085 Uiso 1 1 calc R . . C29 C 0.1658(4) -0.3608(3) -0.1813(3) 0.0610(10) Uani 1 1 d . . . C30 C 0.2524(4) -0.3087(4) -0.1096(3) 0.0709(12) Uani 1 1 d . . . H30 H 0.2652 -0.2472 -0.0902 0.085 Uiso 1 1 calc R . . C31 C 0.3199(5) -0.3469(5) -0.0666(4) 0.0952(19) Uani 1 1 d . . . H31 H 0.3771 -0.3115 -0.0182 0.114 Uiso 1 1 calc R . . C32 C 0.3016(7) -0.4381(6) -0.0962(5) 0.111(2) Uani 1 1 d . . . H32 H 0.3463 -0.4642 -0.0673 0.133 Uiso 1 1 calc R . . C33 C 0.2199(7) -0.4894(5) -0.1664(5) 0.104(2) Uani 1 1 d . . . H33 H 0.2096 -0.5508 -0.1858 0.125 Uiso 1 1 calc R . . C34 C 0.1499(5) -0.4525(4) -0.2110(3) 0.0791(14) Uani 1 1 d . . . H34 H 0.0936 -0.4888 -0.2596 0.095 Uiso 1 1 calc R . . C35 C -0.2801(3) -0.2596(3) -0.1507(2) 0.0536(9) Uani 1 1 d . . . C36 C -0.2470(4) -0.2182(4) -0.0688(3) 0.0746(13) Uani 1 1 d . . . H36 H -0.1696 -0.2088 -0.0386 0.090 Uiso 1 1 calc R . . C37 C -0.3286(5) -0.1905(4) -0.0311(3) 0.0908(17) Uani 1 1 d . . . H37 H -0.3065 -0.1640 0.0241 0.109 Uiso 1 1 calc R . . C38 C -0.4426(5) -0.2026(5) -0.0761(4) 0.0960(19) Uani 1 1 d . . . H38 H -0.4970 -0.1828 -0.0510 0.115 Uiso 1 1 calc R . . C39 C -0.4762(4) -0.2436(4) -0.1574(4) 0.0913(18) Uani 1 1 d . . . H39 H -0.5537 -0.2529 -0.1873 0.110 Uiso 1 1 calc R . . C40 C -0.3946(4) -0.2712(3) -0.1952(3) 0.0686(12) Uani 1 1 d . . . H40 H -0.4171 -0.2975 -0.2505 0.082 Uiso 1 1 calc R . . C41 C -0.1483(4) -0.3904(3) -0.1685(3) 0.0627(10) Uani 1 1 d . . . C42 C -0.0500(4) -0.3922(3) -0.1152(3) 0.0689(11) Uani 1 1 d . . . H42 H 0.0138 -0.3458 -0.0931 0.083 Uiso 1 1 calc R . . C43 C -0.0429(6) -0.4604(4) -0.0934(4) 0.0939(17) Uani 1 1 d . . . H43 H 0.0247 -0.4599 -0.0567 0.113 Uiso 1 1 calc R . . C44 C -0.1377(7) -0.5307(5) -0.1266(5) 0.113(2) Uani 1 1 d . . . H44 H -0.1338 -0.5772 -0.1119 0.136 Uiso 1 1 calc R . . C45 C -0.2345(7) -0.5307(5) -0.1801(6) 0.128(3) Uani 1 1 d . . . H45 H -0.2976 -0.5777 -0.2022 0.153 Uiso 1 1 calc R . . C46 C -0.2422(5) -0.4626(4) -0.2025(5) 0.104(2) Uani 1 1 d . . . H46 H -0.3095 -0.4642 -0.2402 0.124 Uiso 1 1 calc R . . C47 C -0.0003(3) -0.0952(3) -0.3027(2) 0.0511(8) Uani 1 1 d . . . C48 C 0.0273(4) -0.1194(3) -0.3720(3) 0.0647(11) Uani 1 1 d . . . H48 H 0.0003 -0.1769 -0.4121 0.078 Uiso 1 1 calc R . . C49 C 0.0960(4) -0.0569(4) -0.3814(3) 0.0791(14) Uani 1 1 d . . . H49 H 0.1147 -0.0734 -0.4280 0.095 Uiso 1 1 calc R . . C50 C 0.1360(4) 0.0276(4) -0.3237(3) 0.0804(14) Uani 1 1 d . . . H50 H 0.1835 0.0681 -0.3302 0.096 Uiso 1 1 calc R . . C51 C 0.1060(5) 0.0531(4) -0.2557(3) 0.0785(14) Uani 1 1 d . . . H51 H 0.1311 0.1114 -0.2168 0.094 Uiso 1 1 calc R . . C52 C 0.0382(4) -0.0083(3) -0.2451(3) 0.0658(11) Uani 1 1 d . . . H52 H 0.0184 0.0092 -0.1988 0.079 Uiso 1 1 calc R . . C53 C -0.2269(3) -0.1353(2) -0.3011(2) 0.0481(8) Uani 1 1 d . . . C54 C -0.2948(3) -0.1244(3) -0.2521(2) 0.0546(9) Uani 1 1 d . . . H54 H -0.2683 -0.1327 -0.2062 0.066 Uiso 1 1 calc R . . C55 C -0.4020(3) -0.1011(3) -0.2714(3) 0.0620(10) Uani 1 1 d . . . H55 H -0.4474 -0.0947 -0.2387 0.074 Uiso 1 1 calc R . . C56 C -0.4414(4) -0.0875(3) -0.3386(3) 0.0652(11) Uani 1 1 d . . . H56 H -0.5135 -0.0722 -0.3517 0.078 Uiso 1 1 calc R . . C57 C -0.3737(4) -0.0965(4) -0.3860(3) 0.0705(12) Uani 1 1 d . . . H57 H -0.3997 -0.0869 -0.4313 0.085 Uiso 1 1 calc R . . C58 C -0.2676(4) -0.1197(3) -0.3675(3) 0.0640(11) Uani 1 1 d . . . H58 H -0.2224 -0.1250 -0.4002 0.077 Uiso 1 1 calc R . . B1 B 0.2881(5) 0.2819(4) 0.6472(3) 0.0654(12) Uani 1 1 d . . . C59 C 0.3314(4) 0.3096(3) 0.7439(3) 0.0681(11) Uani 1 1 d . . . C60 C 0.2628(5) 0.2825(4) 0.7804(3) 0.0780(13) Uani 1 1 d . . . H60 H 0.1881 0.2496 0.7495 0.094 Uiso 1 1 calc R . . C61 C 0.3007(6) 0.3023(4) 0.8610(3) 0.0901(16) Uani 1 1 d . . . H61 H 0.2513 0.2827 0.8827 0.108 Uiso 1 1 calc R . . C62 C 0.4093(6) 0.3501(5) 0.9084(4) 0.0961(18) Uani 1 1 d . . . H62 H 0.4341 0.3647 0.9626 0.115 Uiso 1 1 calc R . . C63 C 0.4808(6) 0.3761(6) 0.8750(4) 0.118(3) Uani 1 1 d . . . H63 H 0.5562 0.4071 0.9060 0.142 Uiso 1 1 calc R . . C64 C 0.4414(5) 0.3565(6) 0.7942(4) 0.112(2) Uani 1 1 d . . . H64 H 0.4918 0.3761 0.7732 0.135 Uiso 1 1 calc R . . C65 C 0.2982(4) 0.1780(3) 0.6032(3) 0.0696(12) Uani 1 1 d . . . C66 C 0.2121(5) 0.1090(4) 0.5387(3) 0.0829(15) Uani 1 1 d . . . H66 H 0.1404 0.1214 0.5187 0.100 Uiso 1 1 calc R . . C67 C 0.2301(8) 0.0221(5) 0.5034(4) 0.109(2) Uani 1 1 d . . . H67 H 0.1699 -0.0219 0.4617 0.130 Uiso 1 1 calc R . . C68 C 0.3342(10) 0.0017(5) 0.5294(5) 0.120(3) Uani 1 1 d . . . H68 H 0.3464 -0.0558 0.5059 0.144 Uiso 1 1 calc R . . C69 C 0.4205(8) 0.0669(5) 0.5906(5) 0.113(2) Uani 1 1 d . . . H69 H 0.4929 0.0540 0.6079 0.136 Uiso 1 1 calc R . . C70 C 0.4029(6) 0.1519(4) 0.6276(4) 0.0871(15) Uani 1 1 d . . . H70 H 0.4634 0.1939 0.6707 0.105 Uiso 1 1 calc R . . C71 C 0.1527(4) 0.2949(4) 0.6140(3) 0.0724(12) Uani 1 1 d . . . C72 C 0.1236(4) 0.3527(4) 0.5813(3) 0.0742(12) Uani 1 1 d . . . H72 H 0.1832 0.3866 0.5774 0.089 Uiso 1 1 calc R . . C73 C 0.0109(5) 0.3640(4) 0.5535(3) 0.0869(16) Uani 1 1 d . . . H73 H -0.0018 0.4047 0.5321 0.104 Uiso 1 1 calc R . . C74 C -0.0794(6) 0.3179(6) 0.5568(4) 0.110(2) Uani 1 1 d . . . H74 H -0.1530 0.3309 0.5446 0.133 Uiso 1 1 calc R . . C75 C -0.0591(5) 0.2480(6) 0.5795(4) 0.112(2) Uani 1 1 d . . . H75 H -0.1213 0.2089 0.5751 0.134 Uiso 1 1 calc R . . C76 C 0.0555(5) 0.2382(5) 0.6087(4) 0.0948(18) Uani 1 1 d . . . H76 H 0.0680 0.1935 0.6251 0.114 Uiso 1 1 calc R . . C77 C 0.3715(4) 0.3428(3) 0.6252(3) 0.0688(12) Uani 1 1 d . . . C78 C 0.4158(5) 0.3082(4) 0.5639(4) 0.0865(15) Uani 1 1 d . . . H78 H 0.4028 0.2468 0.5357 0.104 Uiso 1 1 calc R . . C79 C 0.4802(6) 0.3615(6) 0.5419(5) 0.111(2) Uani 1 1 d . . . H79 H 0.5079 0.3354 0.4995 0.133 Uiso 1 1 calc R . . C80 C 0.5017(6) 0.4517(7) 0.5832(6) 0.119(3) Uani 1 1 d . . . H80 H 0.5444 0.4877 0.5695 0.142 Uiso 1 1 calc R . . C81 C 0.4604(6) 0.4877(5) 0.6437(6) 0.117(3) Uani 1 1 d . . . H81 H 0.4747 0.5491 0.6718 0.140 Uiso 1 1 calc R . . C82 C 0.3971(5) 0.4358(4) 0.6655(4) 0.0935(18) Uani 1 1 d . . . H82 H 0.3706 0.4633 0.7082 0.112 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 Re1 0.04296(8) 0.04508(8) 0.04009(8) 0.01692(6) 0.00880(5) 0.00754(5) P1 0.0445(4) 0.0504(5) 0.0474(5) 0.0175(4) 0.0116(4) 0.0119(4) P2 0.0451(4) 0.0509(5) 0.0474(5) 0.0216(4) 0.0126(4) 0.0077(4) P3 0.0439(4) 0.0475(5) 0.0416(4) 0.0185(4) 0.0119(4) 0.0085(3) O1 0.080(2) 0.074(2) 0.069(2) 0.0017(17) 0.0142(17) 0.0306(17) O2 0.071(2) 0.080(2) 0.070(2) 0.0221(17) 0.0106(17) -0.0214(17) C1 0.054(2) 0.065(2) 0.0423(19) 0.0151(18) 0.0077(16) 0.0077(18) C2 0.057(2) 0.061(2) 0.048(2) 0.0211(18) 0.0129(17) 0.0086(18) C3 0.0499(18) 0.0485(19) 0.048(2) 0.0191(16) 0.0115(15) 0.0085(15) C4 0.061(2) 0.061(2) 0.049(2) 0.0224(18) 0.0105(18) 0.0125(18) C5 0.062(2) 0.063(2) 0.046(2) 0.0231(18) 0.0114(17) 0.0173(18) C6 0.061(2) 0.073(3) 0.045(2) 0.0230(19) 0.0131(17) 0.0150(19) C7 0.079(3) 0.075(3) 0.050(2) 0.026(2) 0.016(2) 0.014(2) C8 0.082(3) 0.087(4) 0.076(3) 0.030(3) 0.035(3) 0.010(3) C9 0.062(3) 0.101(4) 0.080(4) 0.027(3) 0.024(3) 0.014(3) C10 0.065(3) 0.105(4) 0.087(4) 0.037(3) 0.014(3) 0.032(3) C11 0.067(3) 0.087(3) 0.064(3) 0.034(2) 0.011(2) 0.017(2) C12 0.068(3) 0.086(3) 0.055(2) 0.034(2) 0.018(2) 0.020(2) C13 0.086(4) 0.112(4) 0.083(4) 0.056(3) 0.026(3) 0.014(3) C14 0.100(5) 0.185(8) 0.128(7) 0.105(6) 0.047(5) 0.017(5) C15 0.127(7) 0.312(15) 0.152(9) 0.164(10) 0.081(7) 0.062(8) C16 0.129(7) 0.274(13) 0.077(5) 0.091(7) 0.049(5) 0.048(8) C17 0.088(4) 0.146(6) 0.057(3) 0.041(3) 0.025(3) 0.021(4) C18 0.0470(18) 0.052(2) 0.048(2) 0.0176(16) 0.0114(15) 0.0027(15) C19 0.0467(18) 0.0505(19) 0.0430(18) 0.0135(15) 0.0104(15) 0.0033(15) C20 0.061(2) 0.058(2) 0.049(2) 0.0101(18) 0.0071(18) 0.0015(18) C21 0.0489(18) 0.056(2) 0.0427(18) 0.0173(16) 0.0120(15) 0.0117(15) C22 0.0490(19) 0.0488(19) 0.056(2) 0.0134(17) 0.0130(17) 0.0102(15) C23 0.0452(18) 0.060(2) 0.050(2) 0.0180(17) 0.0117(15) 0.0133(16) C24 0.050(2) 0.063(2) 0.071(3) 0.025(2) 0.0208(19) 0.0127(17) C25 0.060(2) 0.089(3) 0.084(3) 0.039(3) 0.031(2) 0.016(2) C26 0.061(3) 0.108(4) 0.063(3) 0.028(3) 0.028(2) 0.011(3) C27 0.067(3) 0.097(4) 0.059(3) 0.014(3) 0.028(2) 0.020(3) C28 0.065(3) 0.068(3) 0.063(3) 0.012(2) 0.022(2) 0.012(2) C29 0.063(2) 0.065(2) 0.060(2) 0.028(2) 0.0222(19) 0.0287(19) C30 0.065(3) 0.083(3) 0.063(3) 0.033(2) 0.011(2) 0.029(2) C31 0.083(4) 0.123(5) 0.078(4) 0.049(4) 0.010(3) 0.047(4) C32 0.120(5) 0.131(6) 0.101(5) 0.069(5) 0.028(4) 0.070(5) C33 0.133(6) 0.089(4) 0.111(5) 0.057(4) 0.041(5) 0.063(4) C34 0.099(4) 0.072(3) 0.072(3) 0.033(2) 0.027(3) 0.042(3) C35 0.0521(19) 0.056(2) 0.054(2) 0.0242(17) 0.0191(17) 0.0080(16) C36 0.064(3) 0.093(4) 0.058(3) 0.025(2) 0.021(2) 0.011(2) C37 0.091(4) 0.112(4) 0.061(3) 0.023(3) 0.037(3) 0.014(3) C38 0.070(3) 0.118(5) 0.095(4) 0.030(4) 0.046(3) 0.015(3) C39 0.055(3) 0.119(5) 0.087(4) 0.029(3) 0.027(3) 0.016(3) C40 0.056(2) 0.083(3) 0.061(3) 0.025(2) 0.021(2) 0.008(2) C41 0.063(2) 0.063(2) 0.069(3) 0.037(2) 0.019(2) 0.0099(19) C42 0.078(3) 0.063(3) 0.065(3) 0.034(2) 0.013(2) 0.009(2) C43 0.105(4) 0.089(4) 0.099(4) 0.062(4) 0.017(3) 0.021(3) C44 0.124(5) 0.096(4) 0.147(7) 0.090(5) 0.028(5) 0.019(4) C45 0.108(5) 0.096(5) 0.178(8) 0.094(5) 0.001(5) -0.019(4) C46 0.077(3) 0.094(4) 0.142(6) 0.077(4) 0.002(3) -0.005(3) C47 0.0463(17) 0.057(2) 0.053(2) 0.0299(17) 0.0125(15) 0.0086(15) C48 0.062(2) 0.077(3) 0.058(2) 0.032(2) 0.0193(19) 0.007(2) C49 0.076(3) 0.098(4) 0.078(3) 0.050(3) 0.033(3) 0.009(3) C50 0.075(3) 0.085(3) 0.087(4) 0.053(3) 0.017(3) -0.005(3) C51 0.086(3) 0.066(3) 0.080(3) 0.040(3) 0.014(3) -0.003(2) C52 0.072(3) 0.062(3) 0.063(3) 0.030(2) 0.018(2) 0.008(2) C53 0.0464(17) 0.0495(19) 0.0454(19) 0.0190(15) 0.0126(14) 0.0107(14) C54 0.0497(19) 0.067(2) 0.046(2) 0.0250(18) 0.0129(16) 0.0084(17) C55 0.050(2) 0.073(3) 0.064(3) 0.028(2) 0.0220(19) 0.0156(18) C56 0.053(2) 0.077(3) 0.073(3) 0.038(2) 0.018(2) 0.025(2) C57 0.066(2) 0.095(3) 0.068(3) 0.053(3) 0.018(2) 0.027(2) C58 0.061(2) 0.089(3) 0.059(2) 0.044(2) 0.0240(19) 0.027(2) B1 0.064(3) 0.076(3) 0.066(3) 0.037(3) 0.023(2) 0.020(2) C59 0.066(2) 0.075(3) 0.067(3) 0.034(2) 0.019(2) 0.026(2) C60 0.094(3) 0.076(3) 0.062(3) 0.032(2) 0.021(3) 0.012(3) C61 0.112(4) 0.092(4) 0.069(3) 0.039(3) 0.025(3) 0.021(3) C62 0.108(4) 0.111(5) 0.064(3) 0.040(3) 0.014(3) 0.036(4) C63 0.078(4) 0.174(8) 0.086(4) 0.062(5) -0.002(3) 0.011(4) C64 0.070(3) 0.175(7) 0.084(4) 0.061(4) 0.009(3) 0.009(4) C65 0.082(3) 0.075(3) 0.060(3) 0.038(2) 0.023(2) 0.010(2) C66 0.098(4) 0.088(4) 0.065(3) 0.041(3) 0.021(3) 0.003(3) C67 0.170(7) 0.081(4) 0.067(4) 0.028(3) 0.043(4) -0.012(4) C68 0.208(10) 0.086(5) 0.093(5) 0.050(4) 0.068(6) 0.041(6) C69 0.162(7) 0.097(5) 0.109(5) 0.060(4) 0.057(5) 0.059(5) C70 0.105(4) 0.076(3) 0.083(4) 0.039(3) 0.025(3) 0.031(3) C71 0.061(2) 0.102(4) 0.068(3) 0.051(3) 0.020(2) 0.022(2) C72 0.077(3) 0.082(3) 0.064(3) 0.033(2) 0.018(2) 0.026(2) C73 0.092(4) 0.100(4) 0.070(3) 0.041(3) 0.018(3) 0.039(3) C74 0.073(4) 0.182(8) 0.108(5) 0.089(5) 0.031(3) 0.053(4) C75 0.073(4) 0.173(7) 0.085(4) 0.055(5) 0.022(3) 0.016(4) C76 0.079(3) 0.134(5) 0.091(4) 0.066(4) 0.028(3) 0.024(3) C77 0.057(2) 0.076(3) 0.072(3) 0.038(2) 0.010(2) 0.011(2) C78 0.083(3) 0.098(4) 0.097(4) 0.055(3) 0.038(3) 0.017(3) C79 0.088(4) 0.150(7) 0.126(6) 0.087(6) 0.042(4) 0.018(4) C80 0.073(4) 0.146(7) 0.136(7) 0.094(6) -0.005(4) -0.024(4) C81 0.080(4) 0.087(4) 0.153(7) 0.064(5) -0.018(4) -0.018(3) C82 0.077(3) 0.077(3) 0.103(4) 0.031(3) 0.009(3) -0.004(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 Re1 C2 1.937(4) . ? Re1 C1 1.938(4) . ? Re1 C3 1.996(4) . ? Re1 P2 2.4643(9) . ? Re1 P3 2.4703(10) . ? Re1 P1 2.4791(10) . ? P1 C29 1.829(4) . ? P1 C23 1.832(4) . ? P1 C22 1.846(4) . ? P2 C41 1.833(5) . ? P2 C35 1.837(4) . ? P2 C18 1.841(4) . ? P3 C47 1.832(4) . ? P3 C21 1.842(4) . ? P3 C53 1.845(4) . ? O1 C1 1.155(5) . ? O2 C2 1.144(5) . ? C3 C4 1.237(6) . ? C4 C5 1.359(6) . ? C5 C12 1.462(6) . ? C5 C6 1.476(6) . ? C6 C7 1.387(7) . ? C6 C11 1.397(6) . ? C7 C8 1.390(7) . ? C7 H7 0.9300 . ? C8 C9 1.372(8) . ? C8 H8 0.9300 . ? C9 C10 1.368(9) . ? C9 H9 0.9300 . ? C10 C11 1.385(7) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C17 1.391(7) . ? C12 C13 1.398(7) . ? C13 C14 1.353(8) . ? C13 H13 0.9300 . ? C14 C15 1.393(13) . ? C14 H14 0.9300 . ? C15 C16 1.356(14) . ? C15 H15 0.9300 . ? C16 C17 1.364(10) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.559(5) . ? C18 H181 0.9700 . ? C18 H182 0.9700 . ? C19 C22 1.542(5) . ? C19 C20 1.544(5) . ? C19 C21 1.558(6) . ? C20 H201 0.9600 . ? C20 H202 0.9600 . ? C20 H203 0.9600 . ? C21 H211 0.9700 . ? C21 H212 0.9700 . ? C22 H221 0.9700 . ? C22 H222 0.9700 . ? C23 C24 1.389(6) . ? C23 C28 1.397(6) . ? C24 C25 1.391(6) . ? C24 H24 0.9300 . ? C25 C26 1.378(7) . ? C25 H25 0.9300 . ? C26 C27 1.363(8) . ? C26 H26 0.9300 . ? C27 C28 1.388(7) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.387(6) . ? C29 C34 1.388(7) . ? C30 C31 1.381(7) . ? C30 H30 0.9300 . ? C31 C32 1.379(10) . ? C31 H31 0.9300 . ? C32 C33 1.342(10) . ? C32 H32 0.9300 . ? C33 C34 1.398(8) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.379(6) . ? C35 C40 1.382(6) . ? C36 C37 1.388(7) . ? C36 H36 0.9300 . ? C37 C38 1.378(8) . ? C37 H37 0.9300 . ? C38 C39 1.367(8) . ? C38 H38 0.9300 . ? C39 C40 1.390(7) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C42 1.366(6) . ? C41 C46 1.406(7) . ? C42 C43 1.367(7) . ? C42 H42 0.9300 . ? C43 C44 1.395(9) . ? C43 H43 0.9300 . ? C44 C45 1.344(10) . ? C44 H44 0.9300 . ? C45 C46 1.375(8) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C48 1.383(6) . ? C47 C52 1.385(6) . ? C48 C49 1.394(6) . ? C48 H48 0.9300 . ? C49 C50 1.358(8) . ? C49 H49 0.9300 . ? C50 C51 1.374(8) . ? C50 H50 0.9300 . ? C51 C52 1.388(7) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C58 1.382(6) . ? C53 C54 1.389(5) . ? C54 C55 1.387(6) . ? C54 H54 0.9300 . ? C55 C56 1.377(7) . ? C55 H55 0.9300 . ? C56 C57 1.366(7) . ? C56 H56 0.9300 . ? C57 C58 1.372(6) . ? C57 H57 0.9300 . ? C58 H58 0.9300 . ? B1 C65 1.637(8) . ? B1 C77 1.642(7) . ? B1 C59 1.656(7) . ? B1 C71 1.667(7) . ? C59 C64 1.382(8) . ? C59 C60 1.389(7) . ? C60 C61 1.393(8) . ? C60 H60 0.9300 . ? C61 C62 1.361(9) . ? C61 H61 0.9300 . ? C62 C63 1.359(10) . ? C62 H62 0.9300 . ? C63 C64 1.396(9) . ? C63 H63 0.9300 . ? C64 H64 0.9300 . ? C65 C70 1.400(8) . ? C65 C66 1.405(7) . ? C66 C67 1.404(10) . ? C66 H66 0.9300 . ? C67 C68 1.355(11) . ? C67 H67 0.9300 . ? C68 C69 1.357(11) . ? C68 H68 0.9300 . ? C69 C70 1.379(9) . ? C69 H69 0.9300 . ? C70 H70 0.9300 . ? C71 C72 1.372(7) . ? C71 C76 1.422(8) . ? C72 C73 1.391(7) . ? C72 H72 0.9300 . ? C73 C74 1.332(9) . ? C73 H73 0.9300 . ? C74 C75 1.420(11) . ? C74 H74 0.9300 . ? C75 C76 1.408(9) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? C77 C78 1.371(8) . ? C77 C82 1.402(8) . ? C78 C79 1.409(8) . ? C78 H78 0.9300 . ? C79 C80 1.366(11) . ? C79 H79 0.9300 . ? C80 C81 1.338(11) . ? C80 H80 0.9300 . ? C81 C82 1.380(10) . ? C81 H81 0.9300 . ? C82 H82 0.9300 . ? 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 C2 Re1 C1 91.40(17) . . ? C2 Re1 C3 83.36(16) . . ? C1 Re1 C3 86.84(17) . . ? C2 Re1 P2 176.87(13) . . ? C1 Re1 P2 90.84(13) . . ? C3 Re1 P2 94.58(11) . . ? C2 Re1 P3 94.49(13) . . ? C1 Re1 P3 91.90(13) . . ? C3 Re1 P3 177.47(11) . . ? P2 Re1 P3 87.62(3) . . ? C2 Re1 P1 93.83(13) . . ? C1 Re1 P1 174.29(12) . . ? C3 Re1 P1 96.02(11) . . ? P2 Re1 P1 84.02(3) . . ? P3 Re1 P1 85.42(3) . . ? C29 P1 C23 100.12(19) . . ? C29 P1 C22 104.7(2) . . ? C23 P1 C22 103.01(19) . . ? C29 P1 Re1 116.43(14) . . ? C23 P1 Re1 120.78(14) . . ? C22 P1 Re1 109.84(12) . . ? C41 P2 C35 98.3(2) . . ? C41 P2 C18 103.9(2) . . ? C35 P2 C18 106.66(18) . . ? C41 P2 Re1 120.72(14) . . ? C35 P2 Re1 115.70(13) . . ? C18 P2 Re1 109.99(12) . . ? C47 P3 C21 105.57(18) . . ? C47 P3 C53 99.73(17) . . ? C21 P3 C53 102.05(17) . . ? C47 P3 Re1 115.98(13) . . ? C21 P3 Re1 110.59(13) . . ? C53 P3 Re1 120.99(13) . . ? O1 C1 Re1 179.0(4) . . ? O2 C2 Re1 175.0(4) . . ? C4 C3 Re1 171.7(4) . . ? C3 C4 C5 172.1(5) . . ? C4 C5 C12 119.5(4) . . ? C4 C5 C6 119.2(4) . . ? C12 C5 C6 121.3(4) . . ? C7 C6 C11 118.4(4) . . ? C7 C6 C5 120.4(4) . . ? C11 C6 C5 121.1(4) . . ? C6 C7 C8 120.5(5) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 120.3(5) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 119.9(5) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.7(5) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C6 120.2(5) . . ? C10 C11 H11 119.9 . . ? C6 C11 H11 119.9 . . ? C17 C12 C13 118.4(5) . . ? C17 C12 C5 121.6(5) . . ? C13 C12 C5 120.0(4) . . ? C14 C13 C12 121.0(6) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 119.5(8) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 119.9(7) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 121.3(8) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C12 119.8(7) . . ? C16 C17 H17 120.1 . . ? C12 C17 H17 120.1 . . ? C19 C18 P2 115.6(2) . . ? C19 C18 H181 108.4 . . ? P2 C18 H181 108.4 . . ? C19 C18 H182 108.4 . . ? P2 C18 H182 108.4 . . ? H181 C18 H182 107.4 . . ? C22 C19 C20 106.0(3) . . ? C22 C19 C18 111.9(3) . . ? C20 C19 C18 107.3(3) . . ? C22 C19 C21 111.9(3) . . ? C20 C19 C21 106.7(3) . . ? C18 C19 C21 112.4(3) . . ? C19 C20 H201 109.5 . . ? C19 C20 H202 109.5 . . ? H201 C20 H202 109.5 . . ? C19 C20 H203 109.5 . . ? H201 C20 H203 109.5 . . ? H202 C20 H203 109.5 . . ? C19 C21 P3 116.8(3) . . ? C19 C21 H211 108.1 . . ? P3 C21 H211 108.1 . . ? C19 C21 H212 108.1 . . ? P3 C21 H212 108.1 . . ? H211 C21 H212 107.3 . . ? C19 C22 P1 117.4(3) . . ? C19 C22 H221 108.0 . . ? P1 C22 H221 108.0 . . ? C19 C22 H222 108.0 . . ? P1 C22 H222 108.0 . . ? H221 C22 H222 107.2 . . ? C24 C23 C28 118.1(4) . . ? C24 C23 P1 122.3(3) . . ? C28 C23 P1 119.6(4) . . ? C23 C24 C25 120.7(4) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 120.3(5) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 119.6(5) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 121.0(5) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C27 C28 C23 120.3(5) . . ? C27 C28 H28 119.9 . . ? C23 C28 H28 119.9 . . ? C30 C29 C34 119.1(4) . . ? C30 C29 P1 117.7(4) . . ? C34 C29 P1 123.1(4) . . ? C31 C30 C29 120.8(5) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C32 C31 C30 119.3(6) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? C33 C32 C31 120.5(6) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 121.4(6) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C29 C34 C33 118.8(6) . . ? C29 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C36 C35 C40 119.6(4) . . ? C36 C35 P2 116.2(3) . . ? C40 C35 P2 124.2(3) . . ? C35 C36 C37 120.3(5) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C38 C37 C36 119.6(5) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C39 C38 C37 120.5(5) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C40 120.0(5) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C35 C40 C39 120.0(5) . . ? C35 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C42 C41 C46 117.9(5) . . ? C42 C41 P2 123.0(3) . . ? C46 C41 P2 119.0(4) . . ? C41 C42 C43 121.7(5) . . ? C41 C42 H42 119.2 . . ? C43 C42 H42 119.2 . . ? C42 C43 C44 119.7(6) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C45 C44 C43 119.5(6) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C44 C45 C46 121.2(6) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C45 C46 C41 120.0(6) . . ? C45 C46 H46 120.0 . . ? C41 C46 H46 120.0 . . ? C48 C47 C52 118.8(4) . . ? C48 C47 P3 124.6(3) . . ? C52 C47 P3 116.6(3) . . ? C47 C48 C49 119.7(5) . . ? C47 C48 H48 120.2 . . ? C49 C48 H48 120.2 . . ? C50 C49 C48 121.1(5) . . ? C50 C49 H49 119.4 . . ? C48 C49 H49 119.4 . . ? C49 C50 C51 119.7(5) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C50 C51 C52 120.0(5) . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C47 C52 C51 120.7(5) . . ? C47 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C58 C53 C54 118.2(4) . . ? C58 C53 P3 119.5(3) . . ? C54 C53 P3 122.3(3) . . ? C55 C54 C53 120.3(4) . . ? C55 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? C56 C55 C54 120.4(4) . . ? C56 C55 H55 119.8 . . ? C54 C55 H55 119.8 . . ? C57 C56 C55 119.3(4) . . ? C57 C56 H56 120.3 . . ? C55 C56 H56 120.3 . . ? C56 C57 C58 120.7(4) . . ? C56 C57 H57 119.6 . . ? C58 C57 H57 119.6 . . ? C57 C58 C53 121.1(4) . . ? C57 C58 H58 119.5 . . ? C53 C58 H58 119.5 . . ? C65 B1 C77 109.1(4) . . ? C65 B1 C59 106.4(4) . . ? C77 B1 C59 111.4(4) . . ? C65 B1 C71 110.8(4) . . ? C77 B1 C71 107.0(4) . . ? C59 B1 C71 112.2(4) . . ? C64 C59 C60 114.2(5) . . ? C64 C59 B1 122.9(5) . . ? C60 C59 B1 122.8(4) . . ? C59 C60 C61 123.0(5) . . ? C59 C60 H60 118.5 . . ? C61 C60 H60 118.5 . . ? C62 C61 C60 120.5(6) . . ? C62 C61 H61 119.7 . . ? C60 C61 H61 119.7 . . ? C63 C62 C61 118.6(6) . . ? C63 C62 H62 120.7 . . ? C61 C62 H62 120.7 . . ? C62 C63 C64 120.3(6) . . ? C62 C63 H63 119.8 . . ? C64 C63 H63 119.8 . . ? C59 C64 C63 123.3(7) . . ? C59 C64 H64 118.3 . . ? C63 C64 H64 118.3 . . ? C70 C65 C66 113.7(5) . . ? C70 C65 B1 119.5(5) . . ? C66 C65 B1 126.7(5) . . ? C67 C66 C65 122.6(6) . . ? C67 C66 H66 118.7 . . ? C65 C66 H66 118.7 . . ? C68 C67 C66 120.5(7) . . ? C68 C67 H67 119.7 . . ? C66 C67 H67 119.7 . . ? C69 C68 C67 118.7(7) . . ? C69 C68 H68 120.7 . . ? C67 C68 H68 120.7 . . ? C68 C69 C70 121.4(8) . . ? C68 C69 H69 119.3 . . ? C70 C69 H69 119.3 . . ? C69 C70 C65 123.0(6) . . ? C69 C70 H70 118.5 . . ? C65 C70 H70 118.5 . . ? C72 C71 C76 113.9(5) . . ? C72 C71 B1 124.1(4) . . ? C76 C71 B1 121.6(5) . . ? C71 C72 C73 124.4(6) . . ? C71 C72 H72 117.8 . . ? C73 C72 H72 117.8 . . ? C74 C73 C72 121.5(6) . . ? C74 C73 H73 119.2 . . ? C72 C73 H73 119.2 . . ? C73 C74 C75 117.6(6) . . ? C73 C74 H74 121.2 . . ? C75 C74 H74 121.2 . . ? C76 C75 C74 119.7(7) . . ? C76 C75 H75 120.1 . . ? C74 C75 H75 120.1 . . ? C75 C76 C71 121.8(7) . . ? C75 C76 H76 119.1 . . ? C71 C76 H76 119.1 . . ? C78 C77 C82 114.8(5) . . ? C78 C77 B1 123.3(5) . . ? C82 C77 B1 121.8(5) . . ? C77 C78 C79 122.9(7) . . ? C77 C78 H78 118.6 . . ? C79 C78 H78 118.6 . . ? C80 C79 C78 119.5(8) . . ? C80 C79 H79 120.2 . . ? C78 C79 H79 120.2 . . ? C81 C80 C79 119.1(7) . . ? C81 C80 H80 120.4 . . ? C79 C80 H80 120.4 . . ? C80 C81 C82 121.6(7) . . ? C80 C81 H81 119.2 . . ? C82 C81 H81 119.2 . . ? C81 C82 C77 122.1(7) . . ? C81 C82 H82 118.9 . . ? C77 C82 H82 118.9 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.965 _refine_diff_density_min -1.920 _refine_diff_density_rms 0.090