# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 # CCDC Number: 440/244 data_CSD_CIF_PULRIX _publ_author_name ; Ulrich Herber, Rita Guerrero Sanchez, Olaf Gevert, Matthias Laubender and Helmut Werner ; _publ_author_address ; Prof. Dr. Helmut Werner Institut f\"ur Anorganische Chemie Universit\"at W\"urzburg Am Hubland D-97074 W\"urzburg Deutschland ; _publ_contact_author ; Prof. Dr. Helmut Werner Institut f\"ur Anorganische Chemie Universit\"at W\"urzburg Am Hubland D-97074 W\"urzburg Deutschland ; _publ_contact_author_phone '049 931 888 5261' _publ_contact_author_fax '049 931 888 4605' _publ_contact_author_email helmut.werner@mail.uni-wuerzburg.de _publ_requested_journal 'New J. Chem.' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication in "New J. Chem." ; _publ_section_title ; PX3-Induced migratory insertion reactions of halfsandwich-type carbenerhodium(I) complexes ; _publ_section_abstract ; The carbenerhodium(I) complexes trans-[RhCl(=CPh2)(L)2] (L = PPri3, 1a; SbPri3, 1b) react with PF3 by cleavage of the rhodium-carbene bond to give the corresponding PF3 derivatives trans-[RhCl(PF3)(L)2] 5a,b in good yield. In contrast, treatment of the halfsandwich-type compound [((5-C5H5)Rh(=CPh2)(PPri3)] 2a with both PF3 and P(OPh)3 leads to the migratory insertion of the CPh2 unit into one of the cyclopentadienyl C-H bonds to form the ring-substituted products [{(5-C5H4(CHPh2)}Rh(PX3)(PPri3)] (X = F, 6a; OPh, 6b). The molecular structures of 6a and 6b have been determined by X-ray crystallography. The reaction of the stibine complex [((5-C5H5)Rh(=CPh2)(SbPri3)] 2b with PF3 proceeds by ligand displacement to afford the new carbenerhodium(I) compound [((5-C5H5)Rh(=CPh2)(PF3)] 7. The mechanism of the migratory insertion reaction will be discussed. ; _audit_creation_date 1999-01-07 _audit_creation_method CSD-ConQuest-V1 _database_code_CSD PULRIX _chemical_formula_sum 'C27 H36 F3 P2 Rh1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 1/2+x,1/2+y,z 4 1/2-x,1/2+y,1/2-z 5 -x,-y,-z 6 x,-y,-1/2+z 7 -1/2-x,-1/2-y,-z 8 -1/2+x,-1/2-y,-1/2+z _cell_length_a 34.48(9) _cell_length_b 8.96(2) _cell_length_c 17.67(3) _cell_angle_alpha 90 _cell_angle_beta 96.82(9) _cell_angle_gamma 90 _cell_formula_units_Z 8 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 F 0.64 P 1.05 Rh 1.40 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Rh1 Rh 0.4117(1) 0.1698(1) 0.4995(1) P1 P 0.4159(1) 0.2625(1) 0.3810(1) P2 P 0.4582(1) 0.2898(1) 0.5558(1) F1 F 0.4723(1) 0.2463(5) 0.6379(2) F2 F 0.4986(1) 0.3023(6) 0.5310(2) F3 F 0.4577(1) 0.4577(4) 0.5730(3) C1 C 0.3638(1) 0.1139(4) 0.5757(2) C2 C 0.3976(1) 0.0208(4) 0.5926(2) C3 C 0.4015(1) -0.0745(4) 0.5306(2) C4 C 0.3731(1) -0.0314(5) 0.4728(2) C5 C 0.3489(1) 0.0824(4) 0.5005(2) C6 C 0.3478(1) 0.2192(4) 0.6316(2) C7 C 0.3670(1) 0.2551(5) 0.3229(2) C8 C 0.4364(1) 0.4541(4) 0.3736(2) C9 C 0.4474(1) 0.1479(5) 0.3251(2) C10 C 0.3365(2) 0.3531(6) 0.3554(3) C11 C 0.3666(2) 0.2827(9) 0.2378(3) C12 C 0.4129(2) 0.5715(5) 0.4101(3) C13 C 0.4453(2) 0.5052(7) 0.2948(3) C14 C 0.4330(2) -0.0132(5) 0.3177(3) C15 C 0.4900(2) 0.1532(7) 0.3600(4) C16 C 0.3276(1) 0.3537(4) 0.5925(2) C17 C 0.2878(1) 0.3566(5) 0.5680(2) C18 C 0.2710(2) 0.4794(6) 0.5306(3) C19 C 0.2925(2) 0.6024(6) 0.5173(3) C20 C 0.3317(2) 0.6020(5) 0.5422(3) C21 C 0.3490(1) 0.4790(5) 0.5787(3) C22 C 0.3220(1) 0.1388(5) 0.6829(2) C23 C 0.3004(2) 0.0153(7) 0.6595(3) C24 C 0.2752(2) -0.0510(8) 0.7068(5) C25 C 0.2722(2) 0.0047(11) 0.7764(5) C26 C 0.2947(2) 0.1235(11) 0.8022(4) C27 C 0.3193(2) 0.1921(7) 0.7553(3) H1 H 0.4132(12) 0.0235(46) 0.6375(25) H2 H 0.4227(13) -0.1433(51) 0.5309(25) H3 H 0.3685(13) -0.0608(52) 0.4291(26) H4 H 0.3265(12) 0.1306(47) 0.4754(23) H5 H 0.3712(12) 0.2606(47) 0.6684(23) H6 H 0.3607(13) 0.1614(49) 0.3326(26) H7 H 0.4623(12) 0.4411(46) 0.4074(23) H8 H 0.4470(12) 0.1970(49) 0.2746(27) H9 H 0.3409(18) 0.3503(63) 0.4153(39) H10 H 0.3136(19) 0.3255(65) 0.3374(37) H11 H 0.3398(17) 0.4539(73) 0.3402(34) H12 H 0.3879(21) 0.2307(91) 0.2148(42) H13 H 0.3733(21) 0.3867(87) 0.2271(41) H14 H 0.3426(22) 0.2636(84) 0.2174(44) H15 H 0.4107(17) 0.5484(72) 0.4570(36) H16 H 0.3902(18) 0.5965(69) 0.3806(34) H17 H 0.4314(17) 0.6723(65) 0.4212(32) H18 H 0.4608(21) 0.4369(84) 0.2702(41) H19 H 0.4591(20) 0.6004(92) 0.3016(39) H20 H 0.4214(22) 0.5191(77) 0.2626(40) H21 H 0.4058(19) -0.0170(67) 0.2977(35) H22 H 0.4362(16) -0.0575(67) 0.3691(35) H23 H 0.4512(16) -0.0673(70) 0.2849(34) H24 H 0.4952(18) 0.1137(78) 0.4111(40) H25 H 0.5010(19) 0.2470(83) 0.3638(39) H26 H 0.5044(19) 0.0922(77) 0.3354(38) H27 H 0.2728(13) 0.2772(55) 0.5791(25) H28 H 0.2449(16) 0.4724(57) 0.5123(29) H29 H 0.2790(15) 0.6871(59) 0.4816(31) H30 H 0.3440(16) 0.6782(59) 0.5286(33) H31 H 0.3755(14) 0.4776(52) 0.5964(25) H32 H 0.3020(16) -0.0296(65) 0.6210(31) H33 H 0.2625(21) -0.1426(80) 0.6831(40) H34 H 0.2569(20) -0.0334(78) 0.8126(39) H35 H 0.2929(20) 0.1632(69) 0.8503(43) H36 H 0.3316(17) 0.2711(64) 0.7654(36) #===END data_6b _publ_section_exptl_prep ; "crystals were grown from acetone at -20_C" ; _publ_section_exptl_refinement ; ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C45 H51 O3 P2 Rh' _chemical_formula_weight 804.71 _chemical_melting_point '89_C' _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Rh' 'Rh' -1.2870 0.9190 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.170(3) _cell_length_b 11.177(2) _cell_length_c 17.401(3) _cell_angle_alpha 85.68(1) _cell_angle_beta 84.78(2) _cell_angle_gamma 88.03(2) _cell_volume 1963.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method ? _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.551 _exptl_absorpt_correction_type 'empirical (psi-scans)' _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; empirical absorption correction by psi-scans from 6 reflections with chi-angles near 90 degrees ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CAD4 (Enraf-Nonius)' _diffrn_measurement_method 'Omega/Theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 6553 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.1013 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 24.00 _reflns_number_total 6159 _reflns_number_observed 4323 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius)' _computing_cell_refinement 'CAD4 (Enraf-Nonius)' _computing_data_reduction 'BEGIN (SDP)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R-factor(obs) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0973P)^2^+3.4371P] 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 'refxyz; H6 refiso' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6159 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1115 _refine_ls_R_factor_obs 0.0730 _refine_ls_wR_factor_all 0.1943 _refine_ls_wR_factor_obs 0.1633 _refine_ls_goodness_of_fit_all 1.068 _refine_ls_goodness_of_fit_obs 1.084 _refine_ls_restrained_S_all 1.068 _refine_ls_restrained_S_obs 1.084 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh Rh 0.58269(6) -0.06989(6) 0.72616(4) 0.0201(2) Uani 1 d . . O1 O 0.5693(5) -0.2144(4) 0.8947(3) 0.0241(12) Uani 1 d . . O2 O 0.7846(5) -0.1330(5) 0.8631(3) 0.0240(12) Uani 1 d . . O3 O 0.5847(5) -0.0040(5) 0.9043(3) 0.0244(12) Uani 1 d . . P1 P 0.6347(2) -0.1019(2) 0.84132(11) 0.0204(5) Uani 1 d . . P2 P 0.7608(2) -0.1599(2) 0.66464(11) 0.0209(5) Uani 1 d . . C1 C 0.3876(7) 0.0172(7) 0.7528(5) 0.027(2) Uani 1 d . . H1 H 0.3692(7) 0.0354(7) 0.8052(5) 0.032 Uiso 1 calc R . C2 C 0.3599(7) -0.0935(7) 0.7221(5) 0.029(2) Uani 1 d . . H2 H 0.3115(7) -0.1578(7) 0.7484(5) 0.034 Uiso 1 calc R . C3 C 0.4184(8) -0.0886(7) 0.6453(5) 0.028(2) Uani 1 d . . H3 H 0.4220(8) -0.1518(7) 0.6115(5) 0.033 Uiso 1 calc R . C4 C 0.4715(7) 0.0282(7) 0.6272(4) 0.025(2) Uani 1 d . . H4 H 0.5161(7) 0.0547(7) 0.5789(4) 0.030 Uiso 1 calc R . C5 C 0.4482(7) 0.0975(7) 0.6910(4) 0.024(2) Uani 1 d . . C6 C 0.4691(8) 0.2298(7) 0.6962(5) 0.024(2) Uani 1 d . . H6 H 0.5009(82) 0.2473(72) 0.7511(47) 0.037 Uiso 1 d . . C10 C 0.9265(8) -0.1310(7) 0.6945(5) 0.027(2) Uani 1 d . . H10 H 0.9261(8) -0.1664(7) 0.7490(5) 0.033 Uiso 1 calc R . C11 C 0.7591(8) -0.3267(7) 0.6719(5) 0.028(2) Uani 1 d . . H11 H 0.8327(8) -0.3564(7) 0.6355(5) 0.034 Uiso 1 calc R . C12 C 0.7599(8) -0.1251(8) 0.5587(4) 0.031(2) Uani 1 d . . H12 H 0.6658(8) -0.1308(8) 0.5472(4) 0.037 Uiso 1 calc R . C13 C 1.0445(8) -0.1932(8) 0.6497(5) 0.039(2) Uani 1 d . . H13A H 1.0248(25) -0.2776(15) 0.6455(29) 0.059 Uiso 1 calc R . H13B H 1.1236(16) -0.1887(46) 0.6775(18) 0.059 Uiso 1 calc R . H13C H 1.0599(36) -0.1530(33) 0.5978(13) 0.059 Uiso 1 calc R . C14 C 0.9512(8) 0.0022(8) 0.6985(5) 0.033(2) Uani 1 d . . H14A H 0.8736(22) 0.0409(12) 0.7247(29) 0.050 Uiso 1 calc R . H14B H 0.9678(55) 0.0400(13) 0.6459(5) 0.050 Uiso 1 calc R . H14C H 1.0282(34) 0.0114(8) 0.7273(28) 0.050 Uiso 1 calc R . C15 C 0.7796(9) -0.3815(7) 0.7525(5) 0.037(2) Uani 1 d . . H15A H 0.8681(23) -0.3632(45) 0.7656(14) 0.055 Uiso 1 calc R . H15B H 0.7709(58) -0.4687(9) 0.7541(10) 0.055 Uiso 1 calc R . H15C H 0.7132(36) -0.3480(39) 0.7900(7) 0.055 Uiso 1 calc R . C16 C 0.6296(9) -0.3685(8) 0.6467(6) 0.043(2) Uani 1 d . . H16A H 0.6215(30) -0.3401(49) 0.5926(13) 0.065 Uiso 1 calc R . H16B H 0.5554(10) -0.3360(47) 0.6794(24) 0.065 Uiso 1 calc R . H16C H 0.6286(28) -0.4564(8) 0.6517(35) 0.065 Uiso 1 calc R . C17 C 0.7973(9) 0.0070(8) 0.5353(5) 0.036(2) Uani 1 d . . H17A H 0.7502(43) 0.0599(9) 0.5717(20) 0.054 Uiso 1 calc R . H17B H 0.7727(51) 0.0297(18) 0.4829(14) 0.054 Uiso 1 calc R . H17C H 0.8928(11) 0.0150(13) 0.5366(31) 0.054 Uiso 1 calc R . C18 C 0.8397(10) -0.2073(9) 0.5043(5) 0.044(2) Uani 1 d . . H18A H 0.8071(41) -0.2891(15) 0.5135(25) 0.067 Uiso 1 calc R . H18B H 0.9331(13) -0.2073(44) 0.5141(25) 0.067 Uiso 1 calc R . H18C H 0.8300(50) -0.1781(33) 0.4505(5) 0.067 Uiso 1 calc R . C20 C 0.8179(7) -0.1714(7) 0.9380(4) 0.025(2) Uani 1 d . . C21 C 0.8261(9) -0.2917(9) 0.9585(5) 0.039(2) Uani 1 d . . H21 H 0.8062(9) -0.3484(9) 0.9235(5) 0.046 Uiso 1 calc R . C22 C 0.8637(9) -0.3298(9) 1.0310(5) 0.044(3) Uani 1 d . . H22 H 0.8738(9) -0.4133(9) 1.0445(5) 0.053 Uiso 1 calc R . C23 C 0.8866(9) -0.2505(11) 1.0830(6) 0.054(3) Uani 1 d . . H23 H 0.9076(9) -0.2781(11) 1.1336(6) 0.064 Uiso 1 calc R . C24 C 0.8789(9) -0.1260(10) 1.0613(5) 0.042(2) Uani 1 d . . H24 H 0.8983(9) -0.0693(10) 1.0963(5) 0.050 Uiso 1 calc R . C25 C 0.8429(8) -0.0877(8) 0.9885(5) 0.032(2) Uani 1 d . . H25 H 0.8356(8) -0.0044(8) 0.9735(5) 0.038 Uiso 1 calc R . C30 C 0.6043(8) 0.1186(7) 0.8926(4) 0.025(2) Uani 1 d . . C31 C 0.5009(8) 0.1943(8) 0.9169(5) 0.031(2) Uani 1 d . . H31 H 0.4173(8) 0.1628(8) 0.9351(5) 0.037 Uiso 1 calc R . C32 C 0.5206(9) 0.3176(8) 0.9143(5) 0.033(2) Uani 1 d . . H32 H 0.4504(9) 0.3706(8) 0.9309(5) 0.039 Uiso 1 calc R . C33 C 0.6404(10) 0.3613(8) 0.8880(5) 0.040(2) Uani 1 d . . H33 H 0.6532(10) 0.4452(8) 0.8876(5) 0.048 Uiso 1 calc R . C34 C 0.7445(9) 0.2881(8) 0.8618(5) 0.037(2) Uani 1 d . . H34 H 0.8269(9) 0.3210(8) 0.8426(5) 0.044 Uiso 1 calc R . C35 C 0.7258(8) 0.1636(7) 0.8643(4) 0.027(2) Uani 1 d . . H35 H 0.7957(8) 0.1111(7) 0.8467(4) 0.033 Uiso 1 calc R . C40 C 0.4387(7) -0.2472(7) 0.8922(4) 0.025(2) Uani 1 d . . C41 C 0.4155(9) -0.3556(7) 0.8666(5) 0.033(2) Uani 1 d . . H41 H 0.4876(9) -0.4057(7) 0.8491(5) 0.040 Uiso 1 calc R . C42 C 0.2876(9) -0.3936(9) 0.8660(6) 0.043(2) Uani 1 d . . H42 H 0.2716(9) -0.4690(9) 0.8472(6) 0.052 Uiso 1 calc R . C43 C 0.1830(9) -0.3207(9) 0.8929(6) 0.044(2) Uani 1 d . . H43 H 0.0946(9) -0.3455(9) 0.8929(6) 0.053 Uiso 1 calc R . C44 C 0.2087(8) -0.2127(9) 0.9194(5) 0.038(2) Uani 1 d . . H44 H 0.1368(8) -0.1630(9) 0.9379(5) 0.045 Uiso 1 calc R . C45 C 0.3353(8) -0.1734(7) 0.9204(5) 0.028(2) Uani 1 d . . H45 H 0.3515(8) -0.0985(7) 0.9396(5) 0.034 Uiso 1 calc R . C50 C 0.3348(8) 0.2977(7) 0.6980(4) 0.025(2) Uani 1 d . . C51 C 0.3320(9) 0.4237(8) 0.6988(5) 0.038(2) Uani 1 d . . H51 H 0.4126(9) 0.4638(8) 0.7000(5) 0.045 Uiso 1 calc R . C52 C 0.2171(10) 0.4897(8) 0.6979(6) 0.048(3) Uani 1 d . . H52 H 0.2191(10) 0.5747(8) 0.6977(6) 0.058 Uiso 1 calc R . C53 C 0.0992(10) 0.4355(9) 0.6971(6) 0.045(2) Uani 1 d . . H53 H 0.0196(10) 0.4823(9) 0.6962(6) 0.054 Uiso 1 calc R . C54 C 0.0964(8) 0.3118(8) 0.6977(5) 0.034(2) Uani 1 d . . H54 H 0.0146(8) 0.2730(8) 0.6981(5) 0.041 Uiso 1 calc R . C55 C 0.2150(7) 0.2441(7) 0.6978(4) 0.022(2) Uani 1 d . . H55 H 0.2127(7) 0.1592(7) 0.6976(4) 0.026 Uiso 1 calc R . C60 C 0.5658(8) 0.2793(7) 0.6320(5) 0.027(2) Uani 1 d . . C61 C 0.5300(8) 0.3193(7) 0.5593(5) 0.030(2) Uani 1 d . . H61 H 0.4403(8) 0.3161(7) 0.5485(5) 0.035 Uiso 1 calc R . C62 C 0.6234(9) 0.3640(8) 0.5021(5) 0.039(2) Uani 1 d . . H62 H 0.5969(9) 0.3908(8) 0.4526(5) 0.046 Uiso 1 calc R . C63 C 0.7538(9) 0.3699(8) 0.5162(6) 0.040(2) Uani 1 d . . H63 H 0.8166(9) 0.4013(8) 0.4767(6) 0.048 Uiso 1 calc R . C64 C 0.7928(9) 0.3304(9) 0.5875(5) 0.041(2) Uani 1 d . . H64 H 0.8829(9) 0.3342(9) 0.5972(5) 0.049 Uiso 1 calc R . C65 C 0.7003(8) 0.2846(8) 0.6460(5) 0.033(2) Uani 1 d . . H65 H 0.7280(8) 0.2570(8) 0.6951(5) 0.040 Uiso 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 Rh 0.0159(3) 0.0193(3) 0.0248(4) 0.0014(2) -0.0041(2) 0.0054(2) O1 0.027(3) 0.014(3) 0.029(3) 0.008(2) -0.003(2) 0.007(2) O2 0.016(3) 0.032(3) 0.023(3) 0.006(2) -0.001(2) 0.004(2) O3 0.020(3) 0.026(3) 0.026(3) 0.001(2) 0.002(2) 0.002(2) P1 0.0160(11) 0.0204(11) 0.0238(10) 0.0026(8) -0.0022(8) 0.0057(8) P2 0.0169(11) 0.0207(11) 0.0244(10) 0.0000(8) -0.0010(8) 0.0030(8) C1 0.016(4) 0.024(4) 0.038(5) 0.008(4) -0.001(4) 0.002(3) C2 0.011(4) 0.028(5) 0.048(5) 0.004(4) -0.009(4) 0.004(3) C3 0.026(5) 0.023(4) 0.037(5) -0.004(4) -0.018(4) 0.007(3) C4 0.019(4) 0.035(5) 0.020(4) 0.002(3) -0.010(3) 0.015(4) C5 0.014(4) 0.026(4) 0.030(4) 0.004(3) -0.005(3) 0.015(3) C6 0.022(4) 0.023(4) 0.027(4) 0.006(3) -0.006(4) 0.004(3) C10 0.020(4) 0.029(5) 0.035(5) -0.005(4) -0.011(4) 0.001(3) C11 0.024(5) 0.024(4) 0.035(5) -0.005(4) 0.005(4) 0.010(4) C12 0.026(5) 0.039(5) 0.026(4) 0.002(4) -0.004(4) 0.007(4) C13 0.022(5) 0.046(6) 0.052(6) -0.009(5) -0.007(4) 0.008(4) C14 0.027(5) 0.034(5) 0.040(5) -0.006(4) -0.003(4) -0.002(4) C15 0.045(6) 0.021(5) 0.042(5) 0.005(4) 0.007(4) 0.004(4) C16 0.038(6) 0.027(5) 0.066(7) -0.007(5) -0.011(5) 0.000(4) C17 0.028(5) 0.046(6) 0.031(5) 0.012(4) 0.006(4) 0.000(4) C18 0.044(6) 0.065(7) 0.023(5) -0.002(4) 0.001(4) 0.007(5) C20 0.010(4) 0.037(5) 0.026(4) 0.003(4) -0.005(3) 0.009(3) C21 0.031(5) 0.046(6) 0.038(5) 0.006(4) -0.005(4) 0.004(4) C22 0.035(6) 0.045(6) 0.047(6) 0.027(5) -0.002(5) 0.017(5) C23 0.030(6) 0.097(9) 0.032(5) 0.008(6) -0.009(4) 0.007(6) C24 0.032(5) 0.061(7) 0.034(5) -0.003(5) -0.007(4) 0.004(5) C25 0.021(5) 0.038(5) 0.035(5) 0.005(4) -0.009(4) 0.010(4) C30 0.025(5) 0.025(4) 0.025(4) -0.003(3) -0.002(3) 0.002(3) C31 0.027(5) 0.035(5) 0.030(4) -0.004(4) -0.001(4) 0.004(4) C32 0.040(5) 0.027(5) 0.029(4) 0.003(4) 0.002(4) 0.010(4) C33 0.046(6) 0.027(5) 0.047(6) -0.004(4) -0.002(5) 0.006(4) C34 0.030(5) 0.035(5) 0.046(5) 0.003(4) -0.001(4) -0.001(4) C35 0.027(5) 0.024(4) 0.028(4) -0.001(3) 0.003(4) 0.004(4) C40 0.010(4) 0.031(5) 0.030(4) 0.014(4) -0.001(3) 0.004(3) C41 0.030(5) 0.023(5) 0.046(5) -0.004(4) 0.000(4) 0.006(4) C42 0.040(6) 0.037(6) 0.052(6) -0.005(5) 0.004(5) 0.000(4) C43 0.027(5) 0.044(6) 0.061(6) -0.004(5) -0.004(5) -0.006(4) C44 0.020(5) 0.047(6) 0.044(5) -0.003(4) 0.004(4) 0.007(4) C45 0.021(5) 0.026(5) 0.037(5) 0.000(4) -0.002(4) 0.004(4) C50 0.024(4) 0.024(4) 0.024(4) 0.002(3) 0.001(3) 0.009(3) C51 0.032(5) 0.024(5) 0.058(6) -0.005(4) -0.009(4) 0.003(4) C52 0.054(7) 0.023(5) 0.068(7) -0.003(5) -0.013(5) 0.024(5) C53 0.040(6) 0.043(6) 0.053(6) -0.014(5) -0.009(5) 0.022(5) C54 0.021(5) 0.046(6) 0.034(5) 0.009(4) -0.005(4) 0.010(4) C55 0.019(4) 0.020(4) 0.027(4) -0.004(3) -0.003(3) 0.008(3) C60 0.027(5) 0.018(4) 0.036(5) -0.002(3) -0.001(4) 0.005(3) C61 0.023(5) 0.032(5) 0.033(5) 0.002(4) -0.007(4) 0.006(4) C62 0.034(5) 0.046(6) 0.035(5) 0.004(4) -0.009(4) 0.004(4) C63 0.030(5) 0.037(5) 0.051(6) 0.004(4) 0.000(4) -0.003(4) C64 0.023(5) 0.054(6) 0.047(6) -0.003(5) -0.008(4) 0.000(4) C65 0.025(5) 0.036(5) 0.039(5) 0.007(4) -0.014(4) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh P1 2.120(2) . ? Rh C1 2.206(8) . ? Rh P2 2.263(2) . ? Rh C2 2.298(8) . ? Rh C3 2.304(7) . ? Rh C4 2.330(7) . ? Rh C5 2.356(7) . ? O1 C40 1.396(9) . ? O1 P1 1.630(5) . ? O2 C20 1.409(9) . ? O2 P1 1.624(5) . ? O3 C30 1.388(9) . ? O3 P1 1.642(5) . ? P2 C10 1.854(8) . ? P2 C12 1.856(8) . ? P2 C11 1.859(8) . ? C1 C2 1.431(11) . ? C1 C5 1.454(11) . ? C2 C3 1.410(12) . ? C3 C4 1.432(11) . ? C4 C5 1.399(11) . ? C5 C6 1.511(11) . ? C6 C60 1.504(11) . ? C6 C50 1.539(10) . ? C10 C14 1.526(11) . ? C10 C13 1.544(11) . ? C11 C15 1.517(11) . ? C11 C16 1.525(12) . ? C12 C18 1.530(12) . ? C12 C17 1.553(12) . ? C20 C21 1.367(12) . ? C20 C25 1.375(11) . ? C21 C22 1.383(12) . ? C22 C23 1.354(14) . ? C23 C24 1.416(15) . ? C24 C25 1.383(12) . ? C30 C31 1.383(11) . ? C30 C35 1.385(11) . ? C31 C32 1.396(12) . ? C32 C33 1.356(13) . ? C33 C34 1.380(13) . ? C34 C35 1.408(11) . ? C40 C41 1.357(11) . ? C40 C45 1.391(11) . ? C41 C42 1.384(13) . ? C42 C43 1.386(13) . ? C43 C44 1.367(13) . ? C44 C45 1.376(12) . ? C50 C55 1.376(11) . ? C50 C51 1.409(11) . ? C51 C52 1.361(13) . ? C52 C53 1.363(14) . ? C53 C54 1.383(13) . ? C54 C55 1.402(11) . ? C60 C61 1.386(11) . ? C60 C65 1.415(11) . ? C61 C62 1.389(12) . ? C62 C63 1.374(12) . ? C63 C64 1.374(12) . ? C64 C65 1.400(12) . ? 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 P1 Rh C1 97.8(2) . . ? P1 Rh P2 98.54(8) . . ? C1 Rh P2 163.3(2) . . ? P1 Rh C2 110.1(2) . . ? C1 Rh C2 37.0(3) . . ? P2 Rh C2 131.8(2) . . ? P1 Rh C3 144.5(2) . . ? C1 Rh C3 60.7(3) . . ? P2 Rh C3 103.4(2) . . ? C2 Rh C3 35.7(3) . . ? P1 Rh C4 155.2(2) . . ? C1 Rh C4 59.9(3) . . ? P2 Rh C4 104.6(2) . . ? C2 Rh C4 59.6(3) . . ? C3 Rh C4 36.0(3) . . ? P1 Rh C5 120.7(2) . . ? C1 Rh C5 37.0(3) . . ? P2 Rh C5 132.7(2) . . ? C2 Rh C5 60.7(3) . . ? C3 Rh C5 59.8(3) . . ? C4 Rh C5 34.7(3) . . ? C40 O1 P1 123.0(5) . . ? C20 O2 P1 124.0(5) . . ? C30 O3 P1 124.3(5) . . ? O2 P1 O1 95.1(3) . . ? O2 P1 O3 101.7(3) . . ? O1 P1 O3 93.4(3) . . ? O2 P1 Rh 123.5(2) . . ? O1 P1 Rh 118.6(2) . . ? O3 P1 Rh 118.4(2) . . ? C10 P2 C12 109.3(4) . . ? C10 P2 C11 102.2(4) . . ? C12 P2 C11 101.6(4) . . ? C10 P2 Rh 118.3(3) . . ? C12 P2 Rh 109.4(3) . . ? C11 P2 Rh 114.7(3) . . ? C2 C1 C5 109.2(7) . . ? C2 C1 Rh 75.0(5) . . ? C5 C1 Rh 77.1(4) . . ? C3 C2 C1 106.7(7) . . ? C3 C2 Rh 72.4(4) . . ? C1 C2 Rh 68.0(4) . . ? C2 C3 C4 108.0(7) . . ? C2 C3 Rh 71.9(4) . . ? C4 C3 Rh 73.0(4) . . ? C5 C4 C3 110.2(7) . . ? C5 C4 Rh 73.7(4) . . ? C3 C4 Rh 71.0(4) . . ? C4 C5 C1 105.3(7) . . ? C4 C5 C6 129.3(7) . . ? C1 C5 C6 125.3(7) . . ? C4 C5 Rh 71.6(4) . . ? C1 C5 Rh 65.9(4) . . ? C6 C5 Rh 129.9(5) . . ? C60 C6 C5 111.8(7) . . ? C60 C6 C50 112.4(6) . . ? C5 C6 C50 109.3(6) . . ? C14 C10 C13 110.7(7) . . ? C14 C10 P2 113.2(6) . . ? C13 C10 P2 116.1(5) . . ? C15 C11 C16 109.9(7) . . ? C15 C11 P2 112.9(6) . . ? C16 C11 P2 109.9(6) . . ? C18 C12 C17 109.0(7) . . ? C18 C12 P2 118.5(6) . . ? C17 C12 P2 111.3(6) . . ? C21 C20 C25 121.5(8) . . ? C21 C20 O2 118.9(7) . . ? C25 C20 O2 119.6(7) . . ? C20 C21 C22 119.0(9) . . ? C23 C22 C21 121.4(9) . . ? C22 C23 C24 119.2(9) . . ? C25 C24 C23 119.4(9) . . ? C20 C25 C24 119.4(8) . . ? C31 C30 C35 120.9(8) . . ? C31 C30 O3 117.2(7) . . ? C35 C30 O3 121.6(7) . . ? C30 C31 C32 119.3(8) . . ? C33 C32 C31 119.6(8) . . ? C32 C33 C34 122.2(9) . . ? C33 C34 C35 118.6(8) . . ? C30 C35 C34 119.2(8) . . ? C41 C40 C45 121.0(7) . . ? C41 C40 O1 118.6(7) . . ? C45 C40 O1 120.2(7) . . ? C40 C41 C42 120.5(8) . . ? C41 C42 C43 119.4(9) . . ? C44 C43 C42 119.1(9) . . ? C43 C44 C45 122.2(8) . . ? C44 C45 C40 117.7(8) . . ? C55 C50 C51 116.7(7) . . ? C55 C50 C6 124.6(7) . . ? C51 C50 C6 118.8(7) . . ? C52 C51 C50 121.8(9) . . ? C51 C52 C53 120.8(9) . . ? C52 C53 C54 119.6(9) . . ? C53 C54 C55 119.5(8) . . ? C50 C55 C54 121.6(8) . . ? C61 C60 C65 118.0(8) . . ? C61 C60 C6 123.2(7) . . ? C65 C60 C6 118.7(7) . . ? C60 C61 C62 120.8(8) . . ? C63 C62 C61 120.9(8) . . ? C64 C63 C62 119.8(9) . . ? C63 C64 C65 120.3(8) . . ? C64 C65 C60 120.2(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20 O2 P1 O1 -40.9(6) . . . . ? C20 O2 P1 O3 53.6(6) . . . . ? C20 O2 P1 Rh -170.4(5) . . . . ? C40 O1 P1 O2 -170.7(6) . . . . ? C40 O1 P1 O3 87.2(6) . . . . ? C40 O1 P1 Rh -37.9(6) . . . . ? C30 O3 P1 O2 86.8(6) . . . . ? C30 O3 P1 O1 -177.3(6) . . . . ? C30 O3 P1 Rh -52.0(6) . . . . ? C1 Rh P1 O2 -163.2(3) . . . . ? P2 Rh P1 O2 20.3(3) . . . . ? C2 Rh P1 O2 160.8(3) . . . . ? C3 Rh P1 O2 148.1(4) . . . . ? C4 Rh P1 O2 -138.6(5) . . . . ? C5 Rh P1 O2 -132.1(3) . . . . ? C1 Rh P1 O1 78.0(3) . . . . ? P2 Rh P1 O1 -98.6(2) . . . . ? C2 Rh P1 O1 42.0(3) . . . . ? C3 Rh P1 O1 29.3(4) . . . . ? C4 Rh P1 O1 102.6(5) . . . . ? C5 Rh P1 O1 109.1(3) . . . . ? C1 Rh P1 O3 -33.8(3) . . . . ? P2 Rh P1 O3 149.6(2) . . . . ? C2 Rh P1 O3 -69.8(3) . . . . ? C3 Rh P1 O3 -82.5(4) . . . . ? C4 Rh P1 O3 -9.3(6) . . . . ? C5 Rh P1 O3 -2.7(3) . . . . ? P1 Rh P2 C10 -44.4(3) . . . . ? C1 Rh P2 C10 147.4(8) . . . . ? C2 Rh P2 C10 -171.3(4) . . . . ? C3 Rh P2 C10 163.7(4) . . . . ? C4 Rh P2 C10 126.6(4) . . . . ? C5 Rh P2 C10 102.7(4) . . . . ? P1 Rh P2 C12 -170.4(3) . . . . ? C1 Rh P2 C12 21.5(8) . . . . ? C2 Rh P2 C12 62.7(4) . . . . ? C3 Rh P2 C12 37.7(4) . . . . ? C4 Rh P2 C12 0.6(4) . . . . ? C5 Rh P2 C12 -23.3(4) . . . . ? P1 Rh P2 C11 76.3(3) . . . . ? C1 Rh P2 C11 -91.9(8) . . . . ? C2 Rh P2 C11 -50.6(4) . . . . ? C3 Rh P2 C11 -75.6(4) . . . . ? C4 Rh P2 C11 -112.7(4) . . . . ? C5 Rh P2 C11 -136.6(4) . . . . ? P1 Rh C1 C2 -113.3(4) . . . . ? P2 Rh C1 C2 54.8(9) . . . . ? C2 Rh C1 C2 0.000(1) . . . . ? C3 Rh C1 C2 36.6(5) . . . . ? C4 Rh C1 C2 78.3(5) . . . . ? C5 Rh C1 C2 114.3(7) . . . . ? P1 Rh C1 C5 132.4(4) . . . . ? P2 Rh C1 C5 -59.4(9) . . . . ? C2 Rh C1 C5 -114.3(7) . . . . ? C3 Rh C1 C5 -77.6(5) . . . . ? C4 Rh C1 C5 -36.0(4) . . . . ? C5 Rh C1 C5 0.000(2) . . . . ? C5 C1 C2 C3 7.7(8) . . . . ? Rh C1 C2 C3 -62.5(5) . . . . ? C5 C1 C2 Rh 70.3(5) . . . . ? Rh C1 C2 Rh 0.0 . . . . ? P1 Rh C2 C3 -167.4(4) . . . . ? C1 Rh C2 C3 116.9(7) . . . . ? P2 Rh C2 C3 -44.7(6) . . . . ? C3 Rh C2 C3 0.000(2) . . . . ? C4 Rh C2 C3 37.7(5) . . . . ? C5 Rh C2 C3 78.0(5) . . . . ? P1 Rh C2 C1 75.7(5) . . . . ? C1 Rh C2 C1 0.000(1) . . . . ? P2 Rh C2 C1 -161.7(4) . . . . ? C3 Rh C2 C1 -116.9(7) . . . . ? C4 Rh C2 C1 -79.2(5) . . . . ? C5 Rh C2 C1 -39.0(5) . . . . ? C1 C2 C3 C4 -4.8(8) . . . . ? Rh C2 C3 C4 -64.5(5) . . . . ? C1 C2 C3 Rh 59.7(5) . . . . ? Rh C2 C3 Rh 0.000(1) . . . . ? P1 Rh C3 C2 20.7(7) . . . . ? C1 Rh C3 C2 -37.9(5) . . . . ? P2 Rh C3 C2 147.3(4) . . . . ? C2 Rh C3 C2 0.000(2) . . . . ? C4 Rh C3 C2 -116.1(7) . . . . ? C5 Rh C3 C2 -80.8(5) . . . . ? P1 Rh C3 C4 136.8(4) . . . . ? C1 Rh C3 C4 78.2(5) . . . . ? P2 Rh C3 C4 -96.5(4) . . . . ? C2 Rh C3 C4 116.1(7) . . . . ? C4 Rh C3 C4 0.0 . . . . ? C5 Rh C3 C4 35.3(4) . . . . ? C2 C3 C4 C5 0.1(9) . . . . ? Rh C3 C4 C5 -63.7(5) . . . . ? C2 C3 C4 Rh 63.8(5) . . . . ? Rh C3 C4 Rh 0.0 . . . . ? P1 Rh C4 C5 9.9(8) . . . . ? C1 Rh C4 C5 38.3(5) . . . . ? P2 Rh C4 C5 -148.5(4) . . . . ? C2 Rh C4 C5 81.4(5) . . . . ? C3 Rh C4 C5 118.7(7) . . . . ? C5 Rh C4 C5 0.000(3) . . . . ? P1 Rh C4 C3 -108.9(6) . . . . ? C1 Rh C4 C3 -80.4(5) . . . . ? P2 Rh C4 C3 92.8(5) . . . . ? C2 Rh C4 C3 -37.4(5) . . . . ? C3 Rh C4 C3 0.0 . . . . ? C5 Rh C4 C3 -118.7(7) . . . . ? C3 C4 C5 C1 4.5(8) . . . . ? Rh C4 C5 C1 -57.5(5) . . . . ? C3 C4 C5 C6 -170.9(7) . . . . ? Rh C4 C5 C6 127.0(8) . . . . ? C3 C4 C5 Rh 62.1(5) . . . . ? Rh C4 C5 Rh 0.000(2) . . . . ? C2 C1 C5 C4 -7.6(8) . . . . ? Rh C1 C5 C4 61.3(5) . . . . ? C2 C1 C5 C6 168.1(7) . . . . ? Rh C1 C5 C6 -123.0(7) . . . . ? C2 C1 C5 Rh -68.8(5) . . . . ? Rh C1 C5 Rh 0.000(1) . . . . ? P1 Rh C5 C4 -175.2(4) . . . . ? C1 Rh C5 C4 -116.9(7) . . . . ? P2 Rh C5 C4 43.5(6) . . . . ? C2 Rh C5 C4 -78.0(5) . . . . ? C3 Rh C5 C4 -36.6(5) . . . . ? C4 Rh C5 C4 0.000(3) . . . . ? P1 Rh C5 C1 -58.3(5) . . . . ? C1 Rh C5 C1 0.000(2) . . . . ? P2 Rh C5 C1 160.4(4) . . . . ? C2 Rh C5 C1 39.0(5) . . . . ? C3 Rh C5 C1 80.3(5) . . . . ? C4 Rh C5 C1 116.9(7) . . . . ? P1 Rh C5 C6 58.6(7) . . . . ? C1 Rh C5 C6 116.8(9) . . . . ? P2 Rh C5 C6 -82.8(7) . . . . ? C2 Rh C5 C6 155.8(8) . . . . ? C3 Rh C5 C6 -162.9(8) . . . . ? C4 Rh C5 C6 -126.2(9) . . . . ? C4 C5 C6 C60 -21.0(11) . . . . ? C1 C5 C6 C60 164.4(7) . . . . ? Rh C5 C6 C60 77.8(8) . . . . ? C4 C5 C6 C50 104.1(9) . . . . ? C1 C5 C6 C50 -70.6(9) . . . . ? Rh C5 C6 C50 -157.2(5) . . . . ? C12 P2 C10 C14 76.5(7) . . . . ? C11 P2 C10 C14 -176.5(6) . . . . ? Rh P2 C10 C14 -49.5(7) . . . . ? C12 P2 C10 C13 -53.1(7) . . . . ? C11 P2 C10 C13 53.9(7) . . . . ? Rh P2 C10 C13 -179.1(5) . . . . ? C10 P2 C11 C15 58.7(7) . . . . ? C12 P2 C11 C15 171.6(6) . . . . ? Rh P2 C11 C15 -70.5(6) . . . . ? C10 P2 C11 C16 -178.2(6) . . . . ? C12 P2 C11 C16 -65.3(7) . . . . ? Rh P2 C11 C16 52.6(7) . . . . ? C10 P2 C12 C18 69.7(8) . . . . ? C11 P2 C12 C18 -37.7(8) . . . . ? Rh P2 C12 C18 -159.3(6) . . . . ? C10 P2 C12 C17 -57.8(7) . . . . ? C11 P2 C12 C17 -165.3(6) . . . . ? Rh P2 C12 C17 73.1(6) . . . . ? P1 O2 C20 C21 92.3(8) . . . . ? P1 O2 C20 C25 -88.6(8) . . . . ? C25 C20 C21 C22 -1.7(13) . . . . ? O2 C20 C21 C22 177.5(7) . . . . ? C20 C21 C22 C23 3.1(14) . . . . ? C21 C22 C23 C24 -3.6(15) . . . . ? C22 C23 C24 C25 2.7(14) . . . . ? C21 C20 C25 C24 0.8(12) . . . . ? O2 C20 C25 C24 -178.3(7) . . . . ? C23 C24 C25 C20 -1.3(13) . . . . ? P1 O3 C30 C31 139.2(6) . . . . ? P1 O3 C30 C35 -46.3(9) . . . . ? C35 C30 C31 C32 -1.5(12) . . . . ? O3 C30 C31 C32 173.0(7) . . . . ? C30 C31 C32 C33 0.1(12) . . . . ? C31 C32 C33 C34 1.4(14) . . . . ? C32 C33 C34 C35 -1.5(14) . . . . ? C31 C30 C35 C34 1.4(12) . . . . ? O3 C30 C35 C34 -172.9(7) . . . . ? C33 C34 C35 C30 0.0(12) . . . . ? P1 O1 C40 C41 115.2(7) . . . . ? P1 O1 C40 C45 -69.2(9) . . . . ? C45 C40 C41 C42 1.9(13) . . . . ? O1 C40 C41 C42 177.5(7) . . . . ? C40 C41 C42 C43 -1.1(14) . . . . ? C41 C42 C43 C44 0.1(15) . . . . ? C42 C43 C44 C45 0.0(15) . . . . ? C43 C44 C45 C40 0.8(13) . . . . ? C41 C40 C45 C44 -1.8(12) . . . . ? O1 C40 C45 C44 -177.3(7) . . . . ? C60 C6 C50 C55 126.9(8) . . . . ? C5 C6 C50 C55 2.1(11) . . . . ? C60 C6 C50 C51 -52.0(10) . . . . ? C5 C6 C50 C51 -176.8(7) . . . . ? C55 C50 C51 C52 -1.2(13) . . . . ? C6 C50 C51 C52 177.8(9) . . . . ? C50 C51 C52 C53 0.8(16) . . . . ? C51 C52 C53 C54 0.3(16) . . . . ? C52 C53 C54 C55 -1.0(14) . . . . ? C51 C50 C55 C54 0.4(12) . . . . ? C6 C50 C55 C54 -178.5(7) . . . . ? C53 C54 C55 C50 0.7(13) . . . . ? C5 C6 C60 C61 85.1(9) . . . . ? C50 C6 C60 C61 -38.2(11) . . . . ? C5 C6 C60 C65 -94.3(9) . . . . ? C50 C6 C60 C65 142.3(7) . . . . ? C65 C60 C61 C62 -0.4(12) . . . . ? C6 C60 C61 C62 -179.9(8) . . . . ? C60 C61 C62 C63 -0.2(14) . . . . ? C61 C62 C63 C64 0.5(14) . . . . ? C62 C63 C64 C65 -0.2(14) . . . . ? C63 C64 C65 C60 -0.3(14) . . . . ? C61 C60 C65 C64 0.7(12) . . . . ? C6 C60 C65 C64 -179.8(8) . . . . ? _refine_diff_density_max 1.074 _refine_diff_density_min -1.273 _refine_diff_density_rms 0.144