# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1a #---------------------- # [(tBu2HP)2BH2]Br #---------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic . _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety . _chemical_formula_sum 'C16 H40 B Br P2' _chemical_formula_weight 385.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 orthorhombic _symmetry_space_group_name_H-M 'P21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.6330(3) _cell_length_b 11.8889(3) _cell_length_c 17.0844(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2159.72(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2684 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 2.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor 1997)' _exptl_special_details . _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 4859 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_unetI/netI 0.1193 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 5.14 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4859 _reflns_number_gt 3263 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_publication_material 'Bruker SHELXTL' _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. H1, H2, H3 and H4 were located on the Fourier difference map. ; _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^)+(0.0256P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.022(10) _refine_ls_number_reflns 4859 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1030 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.001 _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 Br01 Br 0.62675(4) -0.34686(3) 0.16360(3) 0.03638(14) Uani 1 1 d . . . P2 P 0.60404(8) 0.13260(7) 0.14669(7) 0.0212(2) Uani 1 1 d . . . P1 P 0.82642(8) -0.06603(8) 0.15124(7) 0.0210(2) Uani 1 1 d . . . C15 C 1.0311(4) -0.0056(4) 0.2456(3) 0.0351(12) Uani 1 1 d . . . H15A H 1.0856 -0.0503 0.2133 0.053 Uiso 1 1 calc R . . H15B H 1.0657 -0.0002 0.2973 0.053 Uiso 1 1 calc R . . H15C H 1.0233 0.0683 0.2235 0.053 Uiso 1 1 calc R . . C7 C 0.4774(3) 0.3420(3) 0.1571(3) 0.0338(10) Uani 1 1 d . . . H7A H 0.4324 0.3271 0.1095 0.051 Uiso 1 1 calc R . . H7B H 0.4856 0.4218 0.1641 0.051 Uiso 1 1 calc R . . H7C H 0.4322 0.3107 0.2006 0.051 Uiso 1 1 calc R . . C9 C 0.9240(3) -0.1293(3) 0.0724(3) 0.0258(10) Uani 1 1 d . . . C2 C 0.3478(3) 0.0977(3) 0.1125(3) 0.0349(11) Uani 1 1 d . . . H2A H 0.3338 0.1774 0.1099 0.052 Uiso 1 1 calc R . . H2B H 0.3395 0.0728 0.1657 0.052 Uiso 1 1 calc R . . H2C H 0.2869 0.0598 0.0805 0.052 Uiso 1 1 calc R . . C13 C 0.9006(4) -0.0612(3) 0.2496(3) 0.0272(10) Uani 1 1 d . . . C1 C 0.4814(3) 0.0706(3) 0.0826(3) 0.0256(10) Uani 1 1 d . . . B1 B 0.7720(4) 0.0817(4) 0.1181(3) 0.0247(12) Uani 1 1 d . . . C10 C 0.8335(4) -0.1562(4) 0.0054(3) 0.0367(11) Uani 1 1 d . . . H10A H 0.7932 -0.0883 -0.0117 0.055 Uiso 1 1 calc R . . H10B H 0.7711 -0.2086 0.0233 0.055 Uiso 1 1 calc R . . H10C H 0.8795 -0.1886 -0.0373 0.055 Uiso 1 1 calc R . . C6 C 0.6798(4) 0.3368(4) 0.0828(3) 0.0453(13) Uani 1 1 d . . . H6A H 0.7621 0.3037 0.0801 0.068 Uiso 1 1 calc R . . H6B H 0.6876 0.4168 0.0887 0.068 Uiso 1 1 calc R . . H6C H 0.6346 0.3205 0.0355 0.068 Uiso 1 1 calc R . . C16 C 0.9086(4) -0.1799(3) 0.2849(3) 0.0346(12) Uani 1 1 d . . . H16A H 0.8261 -0.2125 0.2869 0.052 Uiso 1 1 calc R . . H16B H 0.9425 -0.1755 0.3369 0.052 Uiso 1 1 calc R . . H16C H 0.9624 -0.2259 0.2531 0.052 Uiso 1 1 calc R . . C4 C 0.5010(4) -0.0563(4) 0.0866(3) 0.0412(13) Uani 1 1 d . . . H4A H 0.5835 -0.0745 0.0677 0.062 Uiso 1 1 calc R . . H4B H 0.4391 -0.0931 0.0547 0.062 Uiso 1 1 calc R . . H4C H 0.4926 -0.0810 0.1398 0.062 Uiso 1 1 calc R . . C11 C 1.0224(4) -0.0448(4) 0.0429(3) 0.0412(13) Uani 1 1 d . . . H11A H 0.9809 0.0228 0.0261 0.062 Uiso 1 1 calc R . . H11B H 1.0676 -0.0769 -0.0003 0.062 Uiso 1 1 calc R . . H11C H 1.0800 -0.0274 0.0844 0.062 Uiso 1 1 calc R . . C14 C 0.8140(4) 0.0113(4) 0.3012(3) 0.0343(11) Uani 1 1 d . . . H14A H 0.7324 -0.0229 0.3040 0.051 Uiso 1 1 calc R . . H14B H 0.8067 0.0851 0.2789 0.051 Uiso 1 1 calc R . . H14C H 0.8490 0.0168 0.3528 0.051 Uiso 1 1 calc R . . C3 C 0.4969(4) 0.1124(4) -0.0018(3) 0.0438(13) Uani 1 1 d . . . H3A H 0.4838 0.1923 -0.0035 0.066 Uiso 1 1 calc R . . H3B H 0.4364 0.0758 -0.0348 0.066 Uiso 1 1 calc R . . H3C H 0.5802 0.0954 -0.0199 0.066 Uiso 1 1 calc R . . C8 C 0.6778(4) 0.3156(4) 0.2293(3) 0.0402(13) Uani 1 1 d . . . H8A H 0.7604 0.2832 0.2280 0.060 Uiso 1 1 calc R . . H8B H 0.6316 0.2849 0.2726 0.060 Uiso 1 1 calc R . . H8C H 0.6844 0.3957 0.2352 0.060 Uiso 1 1 calc R . . C5 C 0.6088(3) 0.2884(3) 0.1525(3) 0.0289(10) Uani 1 1 d . . . C12 C 0.9880(4) -0.2379(3) 0.0982(3) 0.0377(12) Uani 1 1 d . . . H12A H 1.0450 -0.2221 0.1403 0.057 Uiso 1 1 calc R . . H12B H 1.0337 -0.2694 0.0550 0.057 Uiso 1 1 calc R . . H12C H 0.9255 -0.2906 0.1156 0.057 Uiso 1 1 calc R . . H1 H 0.736(2) -0.137(2) 0.161(2) 0.019(8) Uiso 1 1 d . . . H3 H 0.837(4) 0.143(3) 0.146(3) 0.056(13) Uiso 1 1 d . . . H2 H 0.560(3) 0.105(3) 0.215(3) 0.028(11) Uiso 1 1 d . . . H4 H 0.773(3) 0.084(3) 0.055(3) 0.026(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br01 0.0501(3) 0.0258(2) 0.0333(3) -0.0021(2) 0.0003(2) -0.00861(19) P2 0.0202(5) 0.0192(5) 0.0244(7) 0.0013(4) 0.0010(5) 0.0006(4) P1 0.0215(5) 0.0173(5) 0.0242(7) -0.0004(5) -0.0013(5) -0.0005(4) C15 0.026(2) 0.034(3) 0.046(4) -0.011(2) -0.012(2) -0.0028(19) C7 0.0251(19) 0.0228(19) 0.054(3) 0.001(3) 0.004(2) 0.0025(16) C9 0.026(2) 0.017(2) 0.034(3) -0.0022(19) 0.0019(19) 0.0045(16) C2 0.028(2) 0.037(2) 0.039(3) -0.007(2) 0.000(2) -0.0033(18) C13 0.029(2) 0.022(2) 0.030(3) -0.0035(18) -0.004(2) 0.0001(18) C1 0.020(2) 0.029(2) 0.028(3) -0.008(2) -0.002(2) 0.0025(17) B1 0.024(3) 0.024(3) 0.026(3) 0.001(2) -0.001(2) 0.0000(19) C10 0.039(3) 0.042(3) 0.029(3) -0.003(2) 0.003(2) 0.003(2) C6 0.036(2) 0.026(2) 0.074(4) 0.014(3) 0.020(3) 0.006(2) C16 0.047(3) 0.020(2) 0.037(3) 0.0042(19) -0.005(2) 0.0043(18) C4 0.038(3) 0.033(2) 0.052(4) -0.012(3) -0.010(3) -0.001(2) C11 0.042(3) 0.041(3) 0.040(4) 0.002(2) 0.016(2) -0.001(2) C14 0.037(2) 0.036(3) 0.030(3) -0.004(2) -0.001(2) 0.004(2) C3 0.036(3) 0.070(3) 0.026(3) 0.001(3) -0.003(2) 0.011(2) C8 0.032(2) 0.029(3) 0.060(4) -0.011(2) -0.004(3) -0.0005(19) C5 0.0227(19) 0.0172(18) 0.047(3) -0.001(2) -0.001(2) 0.0018(15) C12 0.042(3) 0.026(2) 0.045(4) -0.008(2) -0.003(2) 0.0122(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P2 C1 1.856(4) . ? P2 C5 1.856(3) . ? P2 B1 1.948(5) . ? P2 H2 1.31(4) . ? P1 C13 1.858(4) . ? P1 C9 1.860(4) . ? P1 B1 1.934(5) . ? P1 H1 1.29(3) . ? C15 C13 1.538(6) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C7 C5 1.537(5) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C9 C12 1.525(5) . ? C9 C10 1.528(6) . ? C9 C11 1.536(6) . ? C2 C1 1.544(5) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C13 C16 1.537(6) . ? C13 C14 1.538(6) . ? C1 C4 1.525(6) . ? C1 C3 1.533(7) . ? B1 H3 1.11(4) . ? B1 H4 1.07(4) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C6 C5 1.524(6) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C8 C5 1.537(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 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 P2 C5 116.55(18) . . ? C1 P2 B1 111.9(2) . . ? C5 P2 B1 107.40(18) . . ? C1 P2 H2 100.2(16) . . ? C5 P2 H2 102.1(16) . . ? B1 P2 H2 118.7(15) . . ? C13 P1 C9 115.54(19) . . ? C13 P1 B1 111.4(2) . . ? C9 P1 B1 108.8(2) . . ? C13 P1 H1 102.4(17) . . ? C9 P1 H1 104.5(15) . . ? B1 P1 H1 114.1(13) . . ? 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 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C12 C9 C10 108.7(3) . . ? C12 C9 C11 110.2(3) . . ? C10 C9 C11 108.7(4) . . ? C12 C9 P1 112.5(3) . . ? C10 C9 P1 106.0(3) . . ? C11 C9 P1 110.7(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C16 C13 C15 111.3(3) . . ? C16 C13 C14 108.8(4) . . ? C15 C13 C14 109.0(3) . . ? C16 C13 P1 110.5(3) . . ? C15 C13 P1 110.8(3) . . ? C14 C13 P1 106.3(3) . . ? C4 C1 C3 110.4(4) . . ? C4 C1 C2 108.5(3) . . ? C3 C1 C2 110.0(3) . . ? C4 C1 P2 105.7(3) . . ? C3 C1 P2 110.5(3) . . ? C2 C1 P2 111.6(3) . . ? P1 B1 P2 118.9(3) . . ? P1 B1 H3 107(2) . . ? P2 B1 H3 105(2) . . ? P1 B1 H4 108.3(19) . . ? P2 B1 H4 104(2) . . ? H3 B1 H4 114(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 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 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 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 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 . . ? 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 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C5 C7 109.5(4) . . ? C6 C5 C8 110.6(3) . . ? C7 C5 C8 107.7(4) . . ? C6 C5 P2 110.4(3) . . ? C7 C5 P2 113.1(2) . . ? C8 C5 P2 105.6(3) . . ? 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 . . ? 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 C13 P1 C9 C12 45.0(3) . . . . ? B1 P1 C9 C12 171.0(3) . . . . ? C13 P1 C9 C10 163.6(3) . . . . ? B1 P1 C9 C10 -70.3(3) . . . . ? C13 P1 C9 C11 -78.7(3) . . . . ? B1 P1 C9 C11 47.3(3) . . . . ? C9 P1 C13 C16 -71.4(3) . . . . ? B1 P1 C13 C16 163.8(3) . . . . ? C9 P1 C13 C15 52.4(3) . . . . ? B1 P1 C13 C15 -72.4(3) . . . . ? C9 P1 C13 C14 170.6(2) . . . . ? B1 P1 C13 C14 45.9(3) . . . . ? C5 P2 C1 C4 178.3(3) . . . . ? B1 P2 C1 C4 54.2(4) . . . . ? C5 P2 C1 C3 58.9(4) . . . . ? B1 P2 C1 C3 -65.2(3) . . . . ? C5 P2 C1 C2 -63.9(4) . . . . ? B1 P2 C1 C2 172.0(3) . . . . ? C13 P1 B1 P2 -88.4(3) . . . . ? C9 P1 B1 P2 143.2(3) . . . . ? C1 P2 B1 P1 -78.8(4) . . . . ? C5 P2 B1 P1 152.1(3) . . . . ? C1 P2 C5 C6 -81.8(3) . . . . ? B1 P2 C5 C6 44.6(4) . . . . ? C1 P2 C5 C7 41.2(4) . . . . ? B1 P2 C5 C7 167.6(4) . . . . ? C1 P2 C5 C8 158.7(3) . . . . ? B1 P2 C5 C8 -75.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.361 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.085 _database_code_depnum_ccdc_archive 'CCDC 912134' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1b _audit_creation_method SHELXL-97 _chemical_name_systematic . _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C17 H40 B F3 O3 P2 S' _chemical_formula_weight 454.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 '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 monoclinic _symmetry_space_group_name_H-M P21/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 8.84740(10) _cell_length_b 11.1909(2) _cell_length_c 25.1074(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.6590(10) _cell_angle_gamma 90.00 _cell_volume 2483.22(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5741 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.295 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 9241 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_unetI/netI 0.0515 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5676 _reflns_number_gt 4083 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'Bruker SHELXTL' _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. H1, H2, H3 and H4 were located on the Fourier difference map. ; _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^)+(0.0568P)^2^+2.5272P] 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 5676 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.881 _refine_ls_shift/su_max 0.000 _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 C1 C 0.0700(2) -0.00104(19) 0.17149(8) 0.0243(4) Uani 1 1 d . . . C2 C -0.0293(2) -0.0847(2) 0.13660(10) 0.0358(5) Uani 1 1 d . . . H2A H -0.0274 -0.0591 0.0993 0.054 Uiso 1 1 calc R . . H2B H -0.1335 -0.0820 0.1482 0.054 Uiso 1 1 calc R . . H2C H 0.0094 -0.1665 0.1399 0.054 Uiso 1 1 calc R . . C3 C 0.0699(3) -0.0381(2) 0.23033(9) 0.0363(6) Uani 1 1 d . . . H3A H 0.1341 0.0167 0.2518 0.054 Uiso 1 1 calc R . . H3B H 0.1092 -0.1197 0.2343 0.054 Uiso 1 1 calc R . . H3C H -0.0337 -0.0351 0.2425 0.054 Uiso 1 1 calc R . . C4 C 0.0093(3) 0.1270(2) 0.16623(10) 0.0350(5) Uani 1 1 d . . . H4A H 0.0085 0.1518 0.1288 0.053 Uiso 1 1 calc R . . H4B H 0.0745 0.1810 0.1878 0.053 Uiso 1 1 calc R . . H4C H -0.0938 0.1302 0.1788 0.053 Uiso 1 1 calc R . . C5 C 0.3644(2) -0.14396(19) 0.14453(8) 0.0244(4) Uani 1 1 d . . . C6 C 0.3391(3) -0.2241(2) 0.19268(9) 0.0360(5) Uani 1 1 d . . . H6A H 0.3708 -0.1816 0.2255 0.054 Uiso 1 1 calc R . . H6B H 0.3988 -0.2974 0.1898 0.054 Uiso 1 1 calc R . . H6C H 0.2316 -0.2445 0.1936 0.054 Uiso 1 1 calc R . . C7 C 0.3154(3) -0.2094(2) 0.09299(9) 0.0309(5) Uani 1 1 d . . . H7A H 0.3323 -0.1576 0.0623 0.046 Uiso 1 1 calc R . . H7B H 0.2078 -0.2297 0.0936 0.046 Uiso 1 1 calc R . . H7C H 0.3749 -0.2827 0.0900 0.046 Uiso 1 1 calc R . . C8 C 0.5338(2) -0.1129(2) 0.14369(10) 0.0341(5) Uani 1 1 d . . . H8A H 0.5514 -0.0617 0.1129 0.051 Uiso 1 1 calc R . . H8B H 0.5928 -0.1866 0.1410 0.051 Uiso 1 1 calc R . . H8C H 0.5650 -0.0707 0.1766 0.051 Uiso 1 1 calc R . . C9 C 0.4758(2) 0.31714(19) 0.09556(8) 0.0244(4) Uani 1 1 d . . . C10 C 0.5311(3) 0.2541(2) 0.14733(9) 0.0325(5) Uani 1 1 d . . . H10A H 0.4604 0.2703 0.1754 0.049 Uiso 1 1 calc R . . H10B H 0.6318 0.2839 0.1585 0.049 Uiso 1 1 calc R . . H10C H 0.5362 0.1677 0.1411 0.049 Uiso 1 1 calc R . . C11 C 0.4676(3) 0.4515(2) 0.10704(10) 0.0347(5) Uani 1 1 d . . . H11A H 0.3961 0.4659 0.1350 0.052 Uiso 1 1 calc R . . H11B H 0.4336 0.4939 0.0745 0.052 Uiso 1 1 calc R . . H11C H 0.5680 0.4806 0.1190 0.052 Uiso 1 1 calc R . . C12 C 0.5868(2) 0.2912(2) 0.05195(9) 0.0333(5) Uani 1 1 d . . . H12A H 0.5520 0.3310 0.0188 0.050 Uiso 1 1 calc R . . H12B H 0.5921 0.2048 0.0460 0.050 Uiso 1 1 calc R . . H12C H 0.6874 0.3213 0.0631 0.050 Uiso 1 1 calc R . . C13 C 0.1959(2) 0.3046(2) 0.01351(8) 0.0247(4) Uani 1 1 d . . . C14 C 0.0266(2) 0.2737(2) 0.01549(9) 0.0323(5) Uani 1 1 d . . . H14A H -0.0173 0.3169 0.0450 0.048 Uiso 1 1 calc R . . H14B H 0.0151 0.1875 0.0209 0.048 Uiso 1 1 calc R . . H14C H -0.0257 0.2971 -0.0182 0.048 Uiso 1 1 calc R . . C15 C 0.2638(3) 0.2371(2) -0.03286(8) 0.0333(5) Uani 1 1 d . . . H15A H 0.2532 0.1509 -0.0273 0.050 Uiso 1 1 calc R . . H15B H 0.3713 0.2573 -0.0345 0.050 Uiso 1 1 calc R . . H15C H 0.2104 0.2599 -0.0664 0.050 Uiso 1 1 calc R . . C16 C 0.2120(3) 0.4397(2) 0.00520(9) 0.0351(5) Uani 1 1 d . . . H16A H 0.1685 0.4823 0.0350 0.053 Uiso 1 1 calc R . . H16B H 0.1583 0.4629 -0.0282 0.053 Uiso 1 1 calc R . . H16C H 0.3193 0.4602 0.0036 0.053 Uiso 1 1 calc R . . C101 C -0.1298(3) 0.5736(3) 0.20215(10) 0.0400(6) Uani 1 1 d . . . O100 O -0.1115(2) 0.41534(17) 0.12933(8) 0.0490(5) Uani 1 1 d . . . O200 O 0.1092(2) 0.4523(2) 0.18724(8) 0.0526(5) Uani 1 1 d . . . O300 O 0.0293(2) 0.59846(17) 0.12102(7) 0.0488(5) Uani 1 1 d . . . F100 F -0.1866(2) 0.4956(2) 0.23563(7) 0.0730(6) Uani 1 1 d . . . F200 F -0.0528(2) 0.65358(19) 0.23150(7) 0.0735(6) Uani 1 1 d . . . F300 F -0.24741(18) 0.62918(17) 0.17829(7) 0.0636(5) Uani 1 1 d . . . P1 P 0.26536(5) 0.00228(5) 0.148186(19) 0.01899(13) Uani 1 1 d . . . P2 P 0.28529(6) 0.25492(5) 0.078185(19) 0.01995(13) Uani 1 1 d . . . S100 S -0.01189(6) 0.50159(5) 0.15458(2) 0.02765(14) Uani 1 1 d . . . B1 B 0.2816(3) 0.0818(2) 0.08001(9) 0.0223(5) Uani 1 1 d . . . H1 H 0.340(2) 0.059(2) 0.1878(8) 0.023(5) Uiso 1 1 d . . . H2 H 0.203(2) 0.3060(19) 0.1134(8) 0.019(5) Uiso 1 1 d . . . H3 H 0.395(3) 0.054(2) 0.0643(9) 0.036(7) Uiso 1 1 d . . . H4 H 0.181(3) 0.055(2) 0.0549(9) 0.039(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0200(9) 0.0240(11) 0.0294(10) 0.0020(9) 0.0054(8) -0.0002(8) C2 0.0236(11) 0.0377(14) 0.0463(13) 0.0004(11) 0.0017(10) -0.0085(10) C3 0.0342(12) 0.0424(14) 0.0336(12) 0.0050(11) 0.0143(10) 0.0044(11) C4 0.0283(11) 0.0324(13) 0.0454(13) 0.0025(11) 0.0120(10) 0.0064(10) C5 0.0252(10) 0.0210(11) 0.0270(10) 0.0008(8) 0.0000(8) 0.0036(8) C6 0.0472(14) 0.0280(13) 0.0327(12) 0.0075(10) 0.0021(10) 0.0076(11) C7 0.0368(12) 0.0243(11) 0.0321(11) -0.0026(9) 0.0063(9) 0.0003(10) C8 0.0255(11) 0.0325(13) 0.0443(13) -0.0030(11) 0.0003(9) 0.0074(10) C9 0.0232(10) 0.0226(11) 0.0274(10) 0.0002(8) -0.0012(8) -0.0050(8) C10 0.0334(12) 0.0319(13) 0.0311(11) 0.0020(10) -0.0100(9) -0.0072(10) C11 0.0401(13) 0.0230(12) 0.0404(13) -0.0036(10) -0.0046(10) -0.0089(10) C12 0.0262(11) 0.0361(13) 0.0379(12) -0.0031(10) 0.0050(9) -0.0075(10) C13 0.0277(11) 0.0250(11) 0.0213(10) 0.0032(8) -0.0006(8) -0.0005(9) C14 0.0266(11) 0.0361(14) 0.0335(12) 0.0046(10) -0.0056(9) 0.0016(10) C15 0.0354(12) 0.0415(14) 0.0230(10) -0.0002(10) 0.0000(9) -0.0012(11) C16 0.0409(13) 0.0298(13) 0.0341(12) 0.0119(10) -0.0029(10) -0.0014(11) C101 0.0357(13) 0.0515(17) 0.0326(12) -0.0033(11) 0.0009(10) -0.0002(12) O100 0.0503(11) 0.0363(11) 0.0596(11) -0.0160(9) -0.0055(9) -0.0093(9) O200 0.0351(10) 0.0633(13) 0.0585(12) 0.0100(10) -0.0073(8) 0.0133(9) O300 0.0627(12) 0.0451(11) 0.0394(10) 0.0084(8) 0.0100(9) -0.0130(9) F100 0.0538(10) 0.1124(17) 0.0548(10) 0.0279(10) 0.0237(8) -0.0030(10) F200 0.0737(12) 0.0921(15) 0.0544(10) -0.0450(10) 0.0001(9) -0.0088(11) F300 0.0505(9) 0.0704(12) 0.0691(11) -0.0099(9) -0.0063(8) 0.0314(9) P1 0.0189(2) 0.0174(3) 0.0207(2) -0.0003(2) 0.00101(18) -0.0009(2) P2 0.0211(2) 0.0184(3) 0.0203(2) 0.0003(2) 0.00043(18) -0.0010(2) S100 0.0262(3) 0.0271(3) 0.0296(3) 0.0006(2) 0.0003(2) -0.0014(2) B1 0.0250(11) 0.0195(11) 0.0225(11) 0.0014(9) 0.0019(9) -0.0003(9) _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 C1 C2 1.531(3) . ? C1 C3 1.535(3) . ? C1 C4 1.534(3) . ? C1 P1 1.850(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.530(3) . ? C5 C7 1.532(3) . ? C5 C8 1.540(3) . ? C5 P1 1.860(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C12 1.532(3) . ? C9 C11 1.534(3) . ? C9 C10 1.539(3) . ? C9 P2 1.857(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C16 1.533(3) . ? C13 C15 1.534(3) . ? C13 C14 1.540(3) . ? C13 P2 1.858(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C101 F100 1.327(3) . ? C101 F200 1.327(3) . ? C101 F300 1.330(3) . ? C101 S100 1.811(3) . ? O100 S100 1.4346(18) . ? O200 S100 1.4291(18) . ? O300 S100 1.4305(18) . ? P1 B1 1.941(2) . ? P1 H1 1.33(2) . ? P2 B1 1.938(2) . ? P2 H2 1.30(2) . ? B1 H3 1.13(2) . ? B1 H4 1.11(2) . ? 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 C1 C3 111.06(19) . . ? C2 C1 C4 109.44(18) . . ? C3 C1 C4 108.64(18) . . ? C2 C1 P1 110.55(15) . . ? C3 C1 P1 110.62(15) . . ? C4 C1 P1 106.40(14) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C7 109.98(18) . . ? C6 C5 C8 108.71(18) . . ? C7 C5 C8 109.47(18) . . ? C6 C5 P1 112.96(15) . . ? C7 C5 P1 110.30(14) . . ? C8 C5 P1 105.26(15) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C12 C9 C11 110.94(18) . . ? C12 C9 C10 109.13(18) . . ? C11 C9 C10 107.89(18) . . ? C12 C9 P2 111.47(14) . . ? C11 C9 P2 111.20(15) . . ? C10 C9 P2 106.01(14) . . ? 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 C15 109.90(18) . . ? C16 C13 C14 108.81(18) . . ? C15 C13 C14 109.24(18) . . ? C16 C13 P2 112.07(15) . . ? C15 C13 P2 110.47(15) . . ? C14 C13 P2 106.24(14) . . ? 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 . . ? F100 C101 F200 107.0(2) . . ? F100 C101 F300 106.3(2) . . ? F200 C101 F300 107.8(2) . . ? F100 C101 S100 111.8(2) . . ? F200 C101 S100 111.68(17) . . ? F300 C101 S100 111.93(17) . . ? C1 P1 C5 116.53(10) . . ? C1 P1 B1 113.36(10) . . ? C5 P1 B1 107.81(10) . . ? C1 P1 H1 102.3(9) . . ? C5 P1 H1 103.6(9) . . ? B1 P1 H1 112.8(9) . . ? C9 P2 C13 115.98(9) . . ? C9 P2 B1 112.67(10) . . ? C13 P2 B1 108.24(10) . . ? C9 P2 H2 101.8(9) . . ? C13 P2 H2 103.5(9) . . ? B1 P2 H2 114.3(9) . . ? O200 S100 O300 115.22(12) . . ? O200 S100 O100 114.97(13) . . ? O300 S100 O100 114.68(12) . . ? O200 S100 C101 103.46(12) . . ? O300 S100 C101 102.79(12) . . ? O100 S100 C101 103.30(12) . . ? P2 B1 P1 118.78(12) . . ? P2 B1 H3 104.3(13) . . ? P1 B1 H3 106.5(12) . . ? P2 B1 H4 105.6(13) . . ? P1 B1 H4 106.7(13) . . ? H3 B1 H4 115.4(17) . . ? 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 C2 C1 P1 C5 -56.38(18) . . . . ? C3 C1 P1 C5 67.05(18) . . . . ? C4 C1 P1 C5 -175.12(14) . . . . ? C2 C1 P1 B1 69.63(18) . . . . ? C3 C1 P1 B1 -166.93(16) . . . . ? C4 C1 P1 B1 -49.11(18) . . . . ? C6 C5 P1 C1 -42.37(19) . . . . ? C7 C5 P1 C1 81.17(16) . . . . ? C8 C5 P1 C1 -160.84(14) . . . . ? C6 C5 P1 B1 -171.11(16) . . . . ? C7 C5 P1 B1 -47.58(17) . . . . ? C8 C5 P1 B1 70.41(16) . . . . ? C12 C9 P2 C13 -56.06(18) . . . . ? C11 C9 P2 C13 68.31(18) . . . . ? C10 C9 P2 C13 -174.69(14) . . . . ? C12 C9 P2 B1 69.45(18) . . . . ? C11 C9 P2 B1 -166.18(15) . . . . ? C10 C9 P2 B1 -49.18(17) . . . . ? C16 C13 P2 C9 -44.80(19) . . . . ? C15 C13 P2 C9 78.12(18) . . . . ? C14 C13 P2 C9 -163.52(14) . . . . ? C16 C13 P2 B1 -172.54(16) . . . . ? C15 C13 P2 B1 -49.62(18) . . . . ? C14 C13 P2 B1 68.75(17) . . . . ? F100 C101 S100 O200 -63.1(2) . . . . ? F200 C101 S100 O200 56.7(2) . . . . ? F300 C101 S100 O200 177.68(19) . . . . ? F100 C101 S100 O300 176.64(17) . . . . ? F200 C101 S100 O300 -63.5(2) . . . . ? F300 C101 S100 O300 57.4(2) . . . . ? F100 C101 S100 O100 57.1(2) . . . . ? F200 C101 S100 O100 176.88(19) . . . . ? F300 C101 S100 O100 -62.1(2) . . . . ? C9 P2 B1 P1 81.66(15) . . . . ? C13 P2 B1 P1 -148.74(12) . . . . ? C1 P1 B1 P2 79.52(15) . . . . ? C5 P1 B1 P2 -149.95(12) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.352 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.057 _database_code_depnum_ccdc_archive 'CCDC 912135' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1c #---------------------- # [tBu2hPBH2PHtBu2][BArF4] #---------------------- # start Validation Reply Form _vrf_PLAT242_1c ; PROBLEM: Check Low Ueq as Compared to Neighbors for C215 RESPONSE: The anion contains a significant degree of disorder. See _refine_special_details. ; _audit_creation_method SHELXL-97 _chemical_name_systematic . _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C50.50 H58 B2 F24 P2' _chemical_formula_weight 1204.53 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.97400(10) _cell_length_b 18.19600(10) _cell_length_c 20.9650(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.8041(3) _cell_angle_gamma 90.00 _cell_volume 5657.79(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13192 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2468 _exptl_absorpt_coefficient_mu 0.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 25113 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_unetI/netI 0.0293 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12867 _reflns_number_gt 9734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'Bruker SHELXTL' _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. H1, H2, H3 and H4 were located on the Fourier difference map. Rotational disorder of the CF3 groups of the anion was treated by modelling either the fluorine atoms over two sites or the entire CF3 group and restraining their geometry. Restraints to thermal parameters were applied where necessary in order to maintain sensible values. ; _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^)+(0.0588P)^2^+5.1434P] 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 12867 _refine_ls_number_parameters 854 _refine_ls_number_restraints 816 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1502 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.224 _refine_ls_shift/su_max 0.064 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.67903(19) 0.03025(17) 0.20134(16) 0.0347(6) Uani 1 1 d . . . P1 P 0.78199(4) 0.07750(4) 0.19117(3) 0.03357(16) Uani 1 1 d . . . C1 C 0.7448(2) 0.16647(18) 0.14615(18) 0.0540(8) Uani 1 1 d . . . C2 C 0.8244(3) 0.2122(3) 0.1446(3) 0.0913(16) Uani 1 1 d . . . H2A H 0.8630 0.1817 0.1284 0.137 Uiso 1 1 calc R . . H2B H 0.8594 0.2303 0.1909 0.137 Uiso 1 1 calc R . . H2C H 0.8018 0.2541 0.1135 0.137 Uiso 1 1 calc R . . C3 C 0.6889(3) 0.2090(2) 0.1794(2) 0.0719(11) Uani 1 1 d . . . H3A H 0.6675 0.2550 0.1543 0.108 Uiso 1 1 calc R . . H3B H 0.7263 0.2200 0.2273 0.108 Uiso 1 1 calc R . . H3C H 0.6371 0.1791 0.1778 0.108 Uiso 1 1 calc R . . C4 C 0.6851(3) 0.1466(2) 0.07202(19) 0.0693(11) Uani 1 1 d . . . H4A H 0.6335 0.1174 0.0721 0.104 Uiso 1 1 calc R . . H4B H 0.7202 0.1180 0.0511 0.104 Uiso 1 1 calc R . . H4C H 0.6633 0.1918 0.0455 0.104 Uiso 1 1 calc R . . C5 C 0.88118(17) 0.08120(17) 0.27266(15) 0.0412(6) Uani 1 1 d . . . C6 C 0.8668(2) 0.1380(2) 0.32187(18) 0.0607(9) Uani 1 1 d . . . H6A H 0.9164 0.1347 0.3667 0.091 Uiso 1 1 calc R . . H6B H 0.8095 0.1280 0.3274 0.091 Uiso 1 1 calc R . . H6C H 0.8652 0.1874 0.3030 0.091 Uiso 1 1 calc R . . C7 C 0.96738(19) 0.0982(2) 0.25942(19) 0.0565(8) Uani 1 1 d . . . H7A H 0.9646 0.1486 0.2423 0.085 Uiso 1 1 calc R . . H7B H 0.9728 0.0639 0.2252 0.085 Uiso 1 1 calc R . . H7C H 1.0198 0.0931 0.3023 0.085 Uiso 1 1 calc R . . C8 C 0.8912(2) 0.00466(19) 0.30481(17) 0.0532(8) Uani 1 1 d . . . H8A H 0.9468 0.0026 0.3457 0.080 Uiso 1 1 calc R . . H8B H 0.8937 -0.0322 0.2715 0.080 Uiso 1 1 calc R . . H8C H 0.8394 -0.0055 0.3179 0.080 Uiso 1 1 calc R . . P2 P 0.67375(4) -0.07587(4) 0.20071(4) 0.03356(16) Uani 1 1 d . . . C9 C 0.61467(19) -0.10543(17) 0.25735(16) 0.0446(7) Uani 1 1 d . . . C10 C 0.6817(2) -0.0904(2) 0.33107(17) 0.0587(9) Uani 1 1 d . . . H10A H 0.6977 -0.0382 0.3360 0.088 Uiso 1 1 calc R . . H10B H 0.7362 -0.1200 0.3401 0.088 Uiso 1 1 calc R . . H10C H 0.6538 -0.1036 0.3640 0.088 Uiso 1 1 calc R . . C11 C 0.5296(2) -0.05888(19) 0.24384(18) 0.0496(7) Uani 1 1 d . . . H11A H 0.4999 -0.0743 0.2750 0.074 Uiso 1 1 calc R . . H11B H 0.4882 -0.0658 0.1962 0.074 Uiso 1 1 calc R . . H11C H 0.5464 -0.0069 0.2517 0.074 Uiso 1 1 calc R . . C12 C 0.5898(3) -0.1870(2) 0.2491(2) 0.0696(11) Uani 1 1 d . . . H12A H 0.6430 -0.2161 0.2529 0.104 Uiso 1 1 calc R . . H12B H 0.5422 -0.1953 0.2040 0.104 Uiso 1 1 calc R . . H12C H 0.5681 -0.2019 0.2852 0.104 Uiso 1 1 calc R . . C13 C 0.6328(2) -0.1151(2) 0.11329(18) 0.0580(9) Uani 1 1 d . . . C14 C 0.6883(3) -0.0768(3) 0.07688(19) 0.0791(14) Uani 1 1 d . . . H14A H 0.6719 -0.0969 0.0305 0.119 Uiso 1 1 calc R . . H14B H 0.7527 -0.0851 0.1029 0.119 Uiso 1 1 calc R . . H14C H 0.6758 -0.0239 0.0741 0.119 Uiso 1 1 calc R . . C15 C 0.5327(3) -0.0990(3) 0.0754(2) 0.0838(14) Uani 1 1 d . . . H15A H 0.5148 -0.1131 0.0271 0.126 Uiso 1 1 calc R . . H15B H 0.5216 -0.0463 0.0784 0.126 Uiso 1 1 calc R . . H15C H 0.4973 -0.1271 0.0964 0.126 Uiso 1 1 calc R . . C16 C 0.6524(3) -0.1980(3) 0.1157(3) 0.0932(16) Uani 1 1 d . . . H16A H 0.6150 -0.2237 0.1366 0.140 Uiso 1 1 calc R . . H16B H 0.7162 -0.2068 0.1431 0.140 Uiso 1 1 calc R . . H16C H 0.6383 -0.2164 0.0689 0.140 Uiso 1 1 calc R . . B200 B 0.26833(16) 0.00850(13) 0.30490(13) 0.0230(5) Uani 1 1 d . . . C201 C 0.25687(15) 0.07568(12) 0.24958(11) 0.0243(4) Uani 1 1 d . . . C202 C 0.18699(16) 0.12727(13) 0.22902(12) 0.0283(5) Uani 1 1 d . A . H202 H 0.1446 0.1277 0.2510 0.034 Uiso 1 1 calc R . . C203 C 0.17776(17) 0.17820(14) 0.17708(13) 0.0325(5) Uani 1 1 d D . . C204 C 0.23707(17) 0.17930(14) 0.14286(13) 0.0331(5) Uani 1 1 d . A . H204 H 0.2302 0.2137 0.1072 0.040 Uiso 1 1 calc R . . C205 C 0.30667(17) 0.12859(13) 0.16228(12) 0.0291(5) Uani 1 1 d . . . C206 C 0.31612(16) 0.07843(13) 0.21425(12) 0.0269(5) Uani 1 1 d . A . H206 H 0.3647 0.0445 0.2265 0.032 Uiso 1 1 calc R . . C207 C 0.1006(3) 0.2314(3) 0.1557(2) 0.0479(7) Uani 0.601(6) 1 d PDU A 1 C307 C 0.1060(4) 0.2353(3) 0.1601(3) 0.0479(7) Uani 0.399(6) 1 d PDU A 2 F1 F 0.1246(3) 0.2971(2) 0.1425(4) 0.0836(17) Uani 0.601(6) 1 d PDU A 1 F2 F 0.0657(4) 0.2424(3) 0.2020(3) 0.0839(17) Uani 0.601(6) 1 d PDU A 1 F3 F 0.0335(3) 0.2116(3) 0.1008(3) 0.126(3) Uani 0.601(6) 1 d PDU A 1 F101 F 0.0288(3) 0.2094(4) 0.1566(5) 0.081(2) Uani 0.399(6) 1 d PDU A 2 F102 F 0.0888(5) 0.2667(5) 0.1005(4) 0.082(2) Uani 0.399(6) 1 d PDU A 2 F103 F 0.1244(5) 0.2883(4) 0.2056(5) 0.114(3) Uani 0.399(6) 1 d PDU A 2 C208 C 0.3753(2) 0.12803(15) 0.12918(14) 0.0388(6) Uani 1 1 d . A . F4 F 0.45624(13) 0.15056(14) 0.17221(11) 0.0666(6) Uani 1 1 d U . . F5 F 0.35325(13) 0.17156(10) 0.07431(9) 0.0522(5) Uani 1 1 d U . . F6 F 0.38815(15) 0.06112(10) 0.10860(11) 0.0613(5) Uani 1 1 d U . . C209 C 0.22372(15) -0.06080(12) 0.25298(11) 0.0252(4) Uani 1 1 d . . . C210 C 0.13033(16) -0.07348(13) 0.22807(12) 0.0286(5) Uani 1 1 d . . . H210 H 0.0944 -0.0467 0.2474 0.034 Uiso 1 1 calc R . . C211 C 0.08875(17) -0.12398(14) 0.17601(13) 0.0338(5) Uani 1 1 d . . . C212 C 0.13831(19) -0.16355(14) 0.14560(13) 0.0365(6) Uani 1 1 d . . . H212 H 0.1098 -0.1973 0.1094 0.044 Uiso 1 1 calc R . . C213 C 0.23058(18) -0.15228(14) 0.16963(13) 0.0349(5) Uani 1 1 d . . . C214 C 0.27225(16) -0.10251(13) 0.22243(12) 0.0294(5) Uani 1 1 d . . . H214 H 0.3358 -0.0967 0.2382 0.035 Uiso 1 1 calc R . . C215 C -0.0100(2) -0.13841(18) 0.15390(16) 0.0470(7) Uani 1 1 d . . . F7 F -0.05460(13) -0.08245(16) 0.16700(16) 0.1021(10) Uani 1 1 d U . . F8 F -0.02758(15) -0.19765(16) 0.18368(12) 0.0886(8) Uani 1 1 d U . . F9 F -0.04997(12) -0.15017(12) 0.08682(9) 0.0602(5) Uani 1 1 d U . . C216 C 0.2872(2) -0.19258(18) 0.13801(17) 0.0501(7) Uani 1 1 d . . . F10 F 0.24339(18) -0.24081(18) 0.09198(17) 0.1128(12) Uani 1 1 d U . . F11 F 0.3553(2) -0.22856(18) 0.18436(15) 0.1066(10) Uani 1 1 d U . . F12 F 0.32860(19) -0.14806(15) 0.10946(14) 0.0871(8) Uani 1 1 d U . . C217 C 0.37505(15) -0.00371(12) 0.35192(11) 0.0243(4) Uani 1 1 d . . . C218 C 0.43839(16) 0.05367(13) 0.36674(12) 0.0275(5) Uani 1 1 d . . . H218 H 0.4190 0.1008 0.3475 0.033 Uiso 1 1 calc R . . C219 C 0.52819(16) 0.04380(14) 0.40855(12) 0.0303(5) Uani 1 1 d . . . C220 C 0.55917(16) -0.02352(14) 0.43928(13) 0.0325(5) Uani 1 1 d . B . H220 H 0.6205 -0.0302 0.4684 0.039 Uiso 1 1 calc R . . C221 C 0.49781(16) -0.08074(13) 0.42608(12) 0.0294(5) Uani 1 1 d D . . C222 C 0.40812(16) -0.07107(13) 0.38310(12) 0.0268(5) Uani 1 1 d . B . H222 H 0.3680 -0.1116 0.3747 0.032 Uiso 1 1 calc R . . C223 C 0.59528(18) 0.10478(15) 0.41748(14) 0.0381(6) Uani 1 1 d . . . F13 F 0.55666(12) 0.17065(9) 0.39927(10) 0.0537(5) Uani 1 1 d U . . F14 F 0.64447(14) 0.09345(12) 0.37907(12) 0.0693(6) Uani 1 1 d U . . F15 F 0.65327(12) 0.11138(10) 0.48200(9) 0.0561(5) Uani 1 1 d U . . C224 C 0.5293(5) -0.1574(4) 0.4496(4) 0.0373(6) Uani 0.351(19) 1 d PDU B 1 C324 C 0.5298(3) -0.1552(2) 0.4558(2) 0.0373(6) Uani 0.649(19) 1 d PDU B 2 F116 F 0.5974(4) -0.1526(3) 0.5157(3) 0.0638(17) Uani 0.649(19) 1 d PDU B 2 F117 F 0.5563(7) -0.1949(3) 0.4137(4) 0.0689(16) Uani 0.649(19) 1 d PDU B 2 F118 F 0.4656(3) -0.1956(3) 0.4647(4) 0.0578(15) Uani 0.649(19) 1 d PDU B 2 F16 F 0.5200(10) -0.2022(4) 0.3977(5) 0.065(3) Uani 0.351(19) 1 d PDU B 1 F17 F 0.4835(9) -0.1879(5) 0.4838(7) 0.057(3) Uani 0.351(19) 1 d PDU B 1 F18 F 0.6151(5) -0.1616(5) 0.4892(9) 0.073(3) Uani 0.351(19) 1 d PDU B 1 C225 C 0.21818(14) 0.02216(12) 0.35918(11) 0.0233(4) Uani 1 1 d . . . C226 C 0.21387(15) 0.09142(12) 0.38714(11) 0.0251(4) Uani 1 1 d . . . H226 H 0.2384 0.1327 0.3724 0.030 Uiso 1 1 calc R . . C227 C 0.17488(15) 0.10155(13) 0.43573(11) 0.0273(5) Uani 1 1 d . . . C228 C 0.13990(16) 0.04268(14) 0.45980(12) 0.0307(5) Uani 1 1 d . C . H228 H 0.1131 0.0498 0.4929 0.037 Uiso 1 1 calc R . . C229 C 0.14505(16) -0.02658(13) 0.43445(12) 0.0293(5) Uani 1 1 d D . . C230 C 0.18371(15) -0.03667(13) 0.38528(12) 0.0263(5) Uani 1 1 d . C . H230 H 0.1868 -0.0849 0.3690 0.032 Uiso 1 1 calc R . . C231 C 0.16779(18) 0.17624(15) 0.46291(13) 0.0356(5) Uani 1 1 d . . . F19 F 0.19443(14) 0.23009(9) 0.43253(11) 0.0570(5) Uani 1 1 d U . . F20 F 0.08459(14) 0.19233(11) 0.45777(13) 0.0686(6) Uani 1 1 d U . . F21 F 0.2182(2) 0.18204(12) 0.52957(10) 0.0871(8) Uani 1 1 d U . . C232 C 0.1109(3) -0.0893(3) 0.4647(2) 0.0401(7) Uani 0.559(6) 1 d PDU C 1 C332 C 0.1024(4) -0.0924(3) 0.4536(3) 0.0401(7) Uani 0.441(6) 1 d PDU C 2 F22 F 0.0233(3) -0.0852(3) 0.4488(3) 0.0748(19) Uani 0.559(6) 1 d PDU C 1 F23 F 0.1469(3) -0.0918(3) 0.53205(17) 0.0777(15) Uani 0.559(6) 1 d PDU C 1 F24 F 0.1281(5) -0.15338(17) 0.4440(3) 0.0787(17) Uani 0.559(6) 1 d PDU C 1 F122 F 0.1609(3) -0.1354(4) 0.4980(4) 0.086(2) Uani 0.441(6) 1 d PDU C 2 F123 F 0.0580(4) -0.1360(3) 0.4020(3) 0.0752(19) Uani 0.441(6) 1 d PDU C 2 F124 F 0.0432(5) -0.0743(4) 0.4807(4) 0.071(2) Uani 0.441(6) 1 d PDU C 2 C801 C 1.1649(7) -0.0069(10) 0.0250(10) 0.078(4) Uani 0.50 1 d PD D -1 H80H H 1.2081 -0.0381 0.0144 0.118 Uiso 0.50 1 calc PR D -1 H80I H 1.1768 -0.0095 0.0743 0.118 Uiso 0.50 1 calc PR D -1 H80J H 1.1712 0.0440 0.0122 0.118 Uiso 0.50 1 calc PR D -1 C802 C 1.0688(7) -0.0338(6) -0.0157(6) 0.096(3) Uani 0.50 1 d PD D -1 H80K H 1.0647 -0.0870 -0.0072 0.116 Uiso 0.50 1 calc PR D -1 H80L H 1.0549 -0.0269 -0.0654 0.116 Uiso 0.50 1 calc PR D -1 C803 C 0.9991(10) 0.008(3) 0.005(3) 0.076(5) Uani 0.50 1 d PD D -1 H80A H 1.0127 0.0000 0.0545 0.092 Uiso 0.50 1 calc PR D -1 H80B H 1.0055 0.0614 -0.0017 0.092 Uiso 0.50 1 calc PR D -1 C804 C 0.9007(8) -0.0144(6) -0.0356(5) 0.095(3) Uani 0.50 1 d PD D -1 H80F H 0.8839 -0.0015 -0.0846 0.114 Uiso 0.50 1 calc PR D -1 H80G H 0.8941 -0.0682 -0.0323 0.114 Uiso 0.50 1 calc PR D -1 C805 C 0.8385(17) 0.0256(18) -0.0062(15) 0.163(14) Uani 0.50 1 d PD D -1 H80C H 0.7761 0.0225 -0.0389 0.245 Uiso 0.50 1 calc PR D -1 H80D H 0.8565 0.0773 0.0020 0.245 Uiso 0.50 1 calc PR D -1 H80E H 0.8432 0.0025 0.0373 0.245 Uiso 0.50 1 calc PR D -1 H3 H 0.622(2) 0.0483(19) 0.1600(18) 0.054(9) Uiso 1 1 d . . . H4 H 0.680(2) 0.0518(17) 0.2503(16) 0.043(8) Uiso 1 1 d . . . H1 H 0.811(2) 0.0412(17) 0.1497(16) 0.045(8) Uiso 1 1 d . . . H2 H 0.7519(18) -0.1084(15) 0.2276(14) 0.032(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0269(13) 0.0387(15) 0.0369(15) 0.0012(12) 0.0099(12) 0.0022(11) P1 0.0243(3) 0.0377(4) 0.0344(3) 0.0023(3) 0.0060(2) -0.0005(2) C1 0.0411(16) 0.0483(17) 0.061(2) 0.0189(15) 0.0059(14) -0.0009(13) C2 0.062(2) 0.076(3) 0.118(4) 0.047(3) 0.013(2) -0.018(2) C3 0.064(2) 0.0422(18) 0.094(3) 0.0082(19) 0.012(2) 0.0147(16) C4 0.061(2) 0.078(3) 0.053(2) 0.0303(19) 0.0043(17) 0.0045(19) C5 0.0264(12) 0.0486(16) 0.0396(14) -0.0013(12) 0.0018(11) -0.0028(11) C6 0.0508(19) 0.068(2) 0.0521(19) -0.0197(17) 0.0059(15) -0.0061(16) C7 0.0259(13) 0.070(2) 0.063(2) 0.0017(17) 0.0052(13) -0.0076(13) C8 0.0353(15) 0.060(2) 0.0479(17) 0.0124(15) -0.0029(13) 0.0035(13) P2 0.0290(3) 0.0358(3) 0.0375(3) -0.0041(3) 0.0142(3) -0.0001(3) C9 0.0390(14) 0.0484(16) 0.0521(17) 0.0141(13) 0.0236(13) 0.0062(12) C10 0.0537(19) 0.084(3) 0.0443(17) 0.0216(17) 0.0254(15) 0.0139(17) C11 0.0381(15) 0.0621(19) 0.0572(18) 0.0077(15) 0.0278(14) 0.0059(13) C12 0.067(2) 0.0485(19) 0.104(3) 0.022(2) 0.044(2) 0.0008(17) C13 0.0539(19) 0.071(2) 0.0542(19) -0.0320(17) 0.0255(16) -0.0250(17) C14 0.083(3) 0.118(4) 0.0462(19) -0.041(2) 0.0357(19) -0.043(3) C15 0.060(2) 0.123(4) 0.056(2) -0.029(2) 0.0067(18) -0.034(2) C16 0.097(3) 0.072(3) 0.128(4) -0.060(3) 0.063(3) -0.027(2) B200 0.0239(11) 0.0226(11) 0.0235(11) 0.0024(9) 0.0102(9) 0.0003(9) C201 0.0273(11) 0.0236(10) 0.0221(10) -0.0001(8) 0.0094(8) -0.0030(8) C202 0.0279(11) 0.0303(12) 0.0281(11) 0.0056(9) 0.0119(9) 0.0001(9) C203 0.0332(12) 0.0308(12) 0.0329(12) 0.0085(10) 0.0116(10) 0.0047(10) C204 0.0403(13) 0.0311(12) 0.0289(12) 0.0093(10) 0.0140(10) 0.0029(10) C205 0.0361(12) 0.0283(12) 0.0265(11) 0.0004(9) 0.0157(10) -0.0014(9) C206 0.0305(11) 0.0258(11) 0.0257(11) 0.0012(9) 0.0121(9) 0.0017(9) C207 0.0449(15) 0.0501(17) 0.0549(17) 0.0230(14) 0.0255(13) 0.0143(13) C307 0.0449(15) 0.0501(17) 0.0549(17) 0.0230(14) 0.0255(13) 0.0143(13) F1 0.059(2) 0.042(2) 0.156(5) 0.042(2) 0.048(3) 0.0170(16) F2 0.097(3) 0.092(3) 0.088(3) 0.045(2) 0.065(3) 0.065(3) F3 0.071(3) 0.126(4) 0.117(4) -0.037(3) -0.038(3) 0.056(3) F101 0.035(3) 0.080(4) 0.126(5) 0.046(4) 0.026(3) 0.013(2) F102 0.084(4) 0.103(5) 0.074(4) 0.062(3) 0.047(3) 0.056(4) F103 0.097(5) 0.081(4) 0.140(5) -0.033(4) 0.016(4) 0.046(4) C208 0.0519(16) 0.0352(14) 0.0389(14) 0.0054(11) 0.0280(13) 0.0034(12) F4 0.0431(10) 0.1046(16) 0.0622(12) -0.0026(11) 0.0311(9) -0.0099(10) F5 0.0768(12) 0.0491(10) 0.0481(10) 0.0171(8) 0.0435(9) 0.0099(9) F6 0.0956(15) 0.0422(10) 0.0752(13) 0.0075(9) 0.0655(12) 0.0141(9) C209 0.0286(11) 0.0242(11) 0.0228(10) 0.0034(8) 0.0096(9) -0.0006(8) C210 0.0296(11) 0.0279(11) 0.0277(11) -0.0002(9) 0.0101(9) 0.0000(9) C211 0.0321(12) 0.0340(13) 0.0314(12) -0.0020(10) 0.0072(10) -0.0043(10) C212 0.0452(15) 0.0323(13) 0.0305(12) -0.0074(10) 0.0123(11) -0.0066(11) C213 0.0436(14) 0.0306(13) 0.0342(13) -0.0049(10) 0.0187(11) -0.0010(10) C214 0.0311(12) 0.0294(12) 0.0291(11) 0.0006(9) 0.0128(9) 0.0001(9) C215 0.0380(15) 0.0536(18) 0.0438(16) -0.0122(14) 0.0085(12) -0.0100(13) F7 0.0313(10) 0.122(2) 0.137(2) -0.0770(18) 0.0127(12) -0.0048(11) F8 0.0555(12) 0.129(2) 0.0729(14) 0.0322(14) 0.0137(11) -0.0368(13) F9 0.0487(10) 0.0730(13) 0.0429(10) -0.0046(9) -0.0013(8) -0.0215(9) C216 0.0547(18) 0.0515(18) 0.0509(17) -0.0186(14) 0.0274(15) -0.0049(14) F10 0.0860(17) 0.128(2) 0.145(2) -0.106(2) 0.0660(17) -0.0363(16) F11 0.114(2) 0.125(2) 0.0925(18) -0.0012(16) 0.0523(16) 0.0704(18) F12 0.1048(18) 0.0876(16) 0.1069(19) -0.0176(14) 0.0836(17) -0.0089(14) C217 0.0268(11) 0.0267(11) 0.0210(10) -0.0002(8) 0.0109(8) 0.0001(9) C218 0.0300(11) 0.0257(11) 0.0270(11) 0.0031(9) 0.0108(9) -0.0009(9) C219 0.0285(12) 0.0330(13) 0.0284(11) 0.0002(9) 0.0096(9) -0.0044(9) C220 0.0257(11) 0.0386(13) 0.0296(12) 0.0022(10) 0.0061(9) 0.0006(10) C221 0.0292(11) 0.0301(12) 0.0275(11) 0.0040(9) 0.0089(9) 0.0026(9) C222 0.0286(11) 0.0264(11) 0.0264(11) 0.0020(9) 0.0114(9) -0.0015(9) C223 0.0318(13) 0.0391(14) 0.0418(14) 0.0002(11) 0.0117(11) -0.0059(11) F13 0.0459(9) 0.0364(9) 0.0679(12) 0.0096(8) 0.0087(8) -0.0107(7) F14 0.0666(13) 0.0700(13) 0.0932(15) -0.0208(11) 0.0551(12) -0.0308(10) F15 0.0434(9) 0.0552(11) 0.0515(10) -0.0007(8) -0.0034(8) -0.0171(8) C224 0.0340(12) 0.0342(13) 0.0382(15) 0.0060(11) 0.0072(11) 0.0035(10) C324 0.0340(12) 0.0342(13) 0.0382(15) 0.0060(11) 0.0072(11) 0.0035(10) F116 0.063(2) 0.0414(18) 0.052(3) 0.0118(16) -0.0193(18) 0.0039(16) F117 0.099(4) 0.049(2) 0.072(3) 0.0134(19) 0.047(3) 0.033(2) F118 0.0465(19) 0.043(2) 0.068(3) 0.0268(19) 0.0029(19) -0.0052(15) F16 0.068(5) 0.042(3) 0.069(4) 0.002(3) 0.008(4) 0.021(3) F17 0.070(5) 0.052(4) 0.063(5) 0.025(3) 0.040(4) 0.015(3) F18 0.038(3) 0.052(4) 0.097(6) 0.025(4) -0.011(3) 0.005(3) C225 0.0215(10) 0.0249(11) 0.0221(10) 0.0018(8) 0.0065(8) 0.0005(8) C226 0.0241(10) 0.0265(11) 0.0228(10) 0.0018(8) 0.0064(8) -0.0013(8) C227 0.0264(11) 0.0288(11) 0.0240(10) -0.0030(9) 0.0062(9) 0.0019(9) C228 0.0300(12) 0.0397(13) 0.0249(11) 0.0020(10) 0.0133(9) 0.0026(10) C229 0.0298(11) 0.0315(12) 0.0284(11) 0.0063(9) 0.0130(9) 0.0007(9) C230 0.0283(11) 0.0244(11) 0.0274(11) 0.0019(9) 0.0116(9) 0.0007(9) C231 0.0402(14) 0.0348(13) 0.0328(13) -0.0044(10) 0.0147(11) 0.0018(11) F19 0.0786(13) 0.0301(8) 0.0795(13) -0.0061(8) 0.0493(11) -0.0027(8) F20 0.0614(12) 0.0459(10) 0.1178(18) -0.0154(11) 0.0557(13) 0.0043(9) F21 0.134(2) 0.0565(12) 0.0401(10) -0.0222(9) -0.0027(12) 0.0214(13) C232 0.0455(16) 0.0392(15) 0.0445(18) 0.0077(13) 0.0269(14) -0.0007(12) C332 0.0455(16) 0.0392(15) 0.0445(18) 0.0077(13) 0.0269(14) -0.0007(12) F22 0.0373(19) 0.076(3) 0.104(4) 0.046(3) 0.018(2) -0.0097(18) F23 0.108(3) 0.077(3) 0.044(2) 0.0240(19) 0.024(2) -0.029(2) F24 0.136(4) 0.0334(18) 0.112(4) 0.002(2) 0.098(3) -0.005(2) F122 0.045(2) 0.073(4) 0.116(5) 0.068(4) 0.003(3) -0.006(2) F123 0.098(4) 0.066(3) 0.065(3) -0.008(2) 0.034(3) -0.057(3) F124 0.085(4) 0.064(3) 0.104(4) -0.002(3) 0.082(4) -0.008(3) C801 0.047(6) 0.091(7) 0.092(10) 0.023(7) 0.021(5) -0.001(5) C802 0.133(10) 0.085(7) 0.097(8) 0.013(6) 0.073(8) 0.019(7) C803 0.093(5) 0.076(16) 0.060(11) 0.013(9) 0.027(4) -0.014(5) C804 0.107(9) 0.098(8) 0.064(6) 0.020(5) 0.013(5) -0.033(6) C805 0.17(2) 0.23(3) 0.15(2) 0.09(2) 0.118(18) 0.093(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 P2 1.933(3) . ? B1 P1 1.936(3) . ? B1 H3 1.05(4) . ? B1 H4 1.09(3) . ? P1 C5 1.850(3) . ? P1 C1 1.857(3) . ? P1 H1 1.31(3) . ? C1 C2 1.530(5) . ? C1 C3 1.531(6) . ? C1 C4 1.535(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.530(4) . ? C5 C7 1.534(4) . ? C5 C6 1.537(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? P2 C13 1.845(3) . ? P2 C9 1.850(3) . ? P2 H2 1.31(3) . ? C9 C12 1.530(5) . ? C9 C11 1.535(4) . ? C9 C10 1.543(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.527(6) . ? C13 C14 1.535(5) . ? C13 C16 1.538(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? B200 C225 1.636(3) . ? B200 C217 1.637(3) . ? B200 C209 1.645(3) . ? B200 C201 1.648(3) . ? C201 C202 1.398(3) . ? C201 C206 1.403(3) . ? C202 C203 1.395(3) . ? C202 H202 0.9500 . ? C203 C204 1.385(3) . ? C203 C307 1.490(7) . ? C203 C207 1.499(5) . ? C204 C205 1.385(3) . ? C204 H204 0.9500 . ? C205 C206 1.386(3) . ? C205 C208 1.499(3) . ? C206 H206 0.9500 . ? C207 F3 1.298(5) . ? C207 F2 1.302(5) . ? C207 F1 1.316(5) . ? C307 F101 1.296(5) . ? C307 F102 1.306(5) . ? C307 F103 1.311(5) . ? C208 F5 1.332(3) . ? C208 F6 1.333(3) . ? C208 F4 1.337(4) . ? C209 C214 1.399(3) . ? C209 C210 1.405(3) . ? C210 C211 1.392(3) . ? C210 H210 0.9500 . ? C211 C212 1.388(4) . ? C211 C215 1.493(4) . ? C212 C213 1.385(4) . ? C212 H212 0.9500 . ? C213 C214 1.393(3) . ? C213 C216 1.497(4) . ? C214 H214 0.9500 . ? C215 F8 1.327(4) . ? C215 F9 1.328(3) . ? C215 F7 1.329(4) . ? C216 F10 1.300(4) . ? C216 F12 1.322(4) . ? C216 F11 1.331(4) . ? C217 C222 1.397(3) . ? C217 C218 1.406(3) . ? C218 C219 1.387(3) . ? C218 H218 0.9500 . ? C219 C220 1.387(4) . ? C219 C223 1.505(3) . ? C220 C221 1.386(3) . ? C220 H220 0.9500 . ? C221 C222 1.392(3) . ? C221 C324 1.499(5) . ? C221 C224 1.502(7) . ? C222 H222 0.9500 . ? C223 F15 1.331(3) . ? C223 F14 1.334(3) . ? C223 F13 1.337(3) . ? C224 F18 1.315(5) . ? C224 F17 1.321(5) . ? C224 F16 1.323(5) . ? C324 F116 1.319(4) . ? C324 F117 1.325(4) . ? C324 F118 1.329(4) . ? C225 C226 1.402(3) . ? C225 C230 1.404(3) . ? C226 C227 1.390(3) . ? C226 H226 0.9500 . ? C227 C228 1.387(3) . ? C227 C231 1.494(3) . ? C228 C229 1.382(4) . ? C228 H228 0.9500 . ? C229 C230 1.397(3) . ? C229 C232 1.503(5) . ? C229 C332 1.504(6) . ? C230 H230 0.9500 . ? C231 F19 1.322(3) . ? C231 F20 1.326(3) . ? C231 F21 1.333(3) . ? C232 F24 1.308(5) . ? C232 F22 1.314(5) . ? C232 F23 1.314(5) . ? C332 F122 1.306(5) . ? C332 F124 1.314(5) . ? C332 F123 1.316(5) . ? C801 C802 1.533(14) . ? C801 H80H 0.9800 . ? C801 H80I 0.9800 . ? C801 H80J 0.9800 . ? C802 C803 1.539(16) . ? C802 H80K 0.9900 . ? C802 H80L 0.9900 . ? C803 C804 1.539(16) . ? C803 H80A 0.9900 . ? C803 H80B 0.9900 . ? C804 C805 1.534(15) . ? C804 H80F 0.9900 . ? C804 H80G 0.9900 . ? C805 H80C 0.9800 . ? C805 H80D 0.9800 . ? C805 H80E 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 B1 P1 118.66(15) . . ? P2 B1 H3 106.5(19) . . ? P1 B1 H3 106.6(19) . . ? P2 B1 H4 110.5(17) . . ? P1 B1 H4 103.1(16) . . ? H3 B1 H4 111(2) . . ? C5 P1 C1 116.10(15) . . ? C5 P1 B1 112.68(13) . . ? C1 P1 B1 108.60(14) . . ? C5 P1 H1 103.8(14) . . ? C1 P1 H1 103.2(14) . . ? B1 P1 H1 112.1(14) . . ? C2 C1 C3 111.4(4) . . ? C2 C1 C4 108.4(3) . . ? C3 C1 C4 109.3(3) . . ? C2 C1 P1 112.0(2) . . ? C3 C1 P1 109.8(2) . . ? C4 C1 P1 105.7(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C8 C5 C7 108.1(3) . . ? C8 C5 C6 109.5(3) . . ? C7 C5 C6 110.7(3) . . ? C8 C5 P1 106.69(19) . . ? C7 C5 P1 111.0(2) . . ? C6 C5 P1 110.7(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C13 P2 C9 116.63(15) . . ? C13 P2 B1 113.06(16) . . ? C9 P2 B1 108.51(14) . . ? C13 P2 H2 100.5(12) . . ? C9 P2 H2 103.0(12) . . ? B1 P2 H2 114.7(12) . . ? C12 C9 C11 109.8(3) . . ? C12 C9 C10 109.8(3) . . ? C11 C9 C10 109.0(3) . . ? C12 C9 P2 112.5(2) . . ? C11 C9 P2 110.4(2) . . ? C10 C9 P2 105.2(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 . . ? C15 C13 C14 110.0(4) . . ? C15 C13 C16 111.5(3) . . ? C14 C13 C16 108.3(3) . . ? C15 C13 P2 111.0(3) . . ? C14 C13 P2 105.2(2) . . ? C16 C13 P2 110.7(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 . . ? C225 B200 C217 105.74(17) . . ? C225 B200 C209 111.90(18) . . ? C217 B200 C209 113.13(18) . . ? C225 B200 C201 114.95(18) . . ? C217 B200 C201 110.07(17) . . ? C209 B200 C201 101.27(17) . . ? C202 C201 C206 115.5(2) . . ? C202 C201 B200 125.60(19) . . ? C206 C201 B200 118.54(19) . . ? C203 C202 C201 121.8(2) . . ? C203 C202 H202 119.1 . . ? C201 C202 H202 119.1 . . ? C204 C203 C202 121.3(2) . . ? C204 C203 C307 118.7(3) . . ? C202 C203 C307 119.9(3) . . ? C204 C203 C207 118.7(3) . . ? C202 C203 C207 120.0(3) . . ? C307 C203 C207 4.7(4) . . ? C205 C204 C203 117.8(2) . . ? C205 C204 H204 121.1 . . ? C203 C204 H204 121.1 . . ? C204 C205 C206 120.7(2) . . ? C204 C205 C208 120.9(2) . . ? C206 C205 C208 118.3(2) . . ? C205 C206 C201 122.7(2) . . ? C205 C206 H206 118.6 . . ? C201 C206 H206 118.6 . . ? F3 C207 F2 105.2(5) . . ? F3 C207 F1 106.0(5) . . ? F2 C207 F1 104.8(4) . . ? F3 C207 C203 113.7(4) . . ? F2 C207 C203 114.1(4) . . ? F1 C207 C203 112.3(4) . . ? F101 C307 F102 104.3(5) . . ? F101 C307 F103 105.1(6) . . ? F102 C307 F103 106.6(6) . . ? F101 C307 C203 113.0(5) . . ? F102 C307 C203 113.8(5) . . ? F103 C307 C203 113.2(5) . . ? F5 C208 F6 106.7(2) . . ? F5 C208 F4 106.2(2) . . ? F6 C208 F4 105.7(2) . . ? F5 C208 C205 113.1(2) . . ? F6 C208 C205 112.5(2) . . ? F4 C208 C205 112.1(2) . . ? C214 C209 C210 115.7(2) . . ? C214 C209 B200 122.8(2) . . ? C210 C209 B200 120.7(2) . . ? C211 C210 C209 122.1(2) . . ? C211 C210 H210 118.9 . . ? C209 C210 H210 118.9 . . ? C212 C211 C210 121.0(2) . . ? C212 C211 C215 118.9(2) . . ? C210 C211 C215 120.1(2) . . ? C213 C212 C211 117.9(2) . . ? C213 C212 H212 121.1 . . ? C211 C212 H212 121.1 . . ? C212 C213 C214 121.0(2) . . ? C212 C213 C216 120.2(2) . . ? C214 C213 C216 118.8(2) . . ? C213 C214 C209 122.3(2) . . ? C213 C214 H214 118.9 . . ? C209 C214 H214 118.9 . . ? F8 C215 F9 105.3(2) . . ? F8 C215 F7 107.5(3) . . ? F9 C215 F7 105.0(3) . . ? F8 C215 C211 112.4(3) . . ? F9 C215 C211 113.2(3) . . ? F7 C215 C211 112.8(2) . . ? F10 C216 F12 107.4(3) . . ? F10 C216 F11 106.2(3) . . ? F12 C216 F11 102.8(3) . . ? F10 C216 C213 114.4(3) . . ? F12 C216 C213 112.8(3) . . ? F11 C216 C213 112.4(3) . . ? C222 C217 C218 115.6(2) . . ? C222 C217 B200 121.9(2) . . ? C218 C217 B200 122.4(2) . . ? C219 C218 C217 122.3(2) . . ? C219 C218 H218 118.9 . . ? C217 C218 H218 118.9 . . ? C220 C219 C218 121.0(2) . . ? C220 C219 C223 118.6(2) . . ? C218 C219 C223 120.3(2) . . ? C221 C220 C219 117.8(2) . . ? C221 C220 H220 121.1 . . ? C219 C220 H220 121.1 . . ? C220 C221 C222 121.1(2) . . ? C220 C221 C324 119.3(3) . . ? C222 C221 C324 119.6(3) . . ? C220 C221 C224 120.4(3) . . ? C222 C221 C224 117.9(3) . . ? C324 C221 C224 5.1(4) . . ? C221 C222 C217 122.2(2) . . ? C221 C222 H222 118.9 . . ? C217 C222 H222 118.9 . . ? F15 C223 F14 106.5(2) . . ? F15 C223 F13 106.4(2) . . ? F14 C223 F13 106.2(2) . . ? F15 C223 C219 112.8(2) . . ? F14 C223 C219 111.3(2) . . ? F13 C223 C219 113.2(2) . . ? F18 C224 F17 106.8(6) . . ? F18 C224 F16 104.7(6) . . ? F17 C224 F16 105.8(6) . . ? F18 C224 C221 113.9(6) . . ? F17 C224 C221 112.5(6) . . ? F16 C224 C221 112.4(6) . . ? F116 C324 F117 107.6(4) . . ? F116 C324 F118 106.7(4) . . ? F117 C324 F118 104.2(4) . . ? F116 C324 C221 113.4(4) . . ? F117 C324 C221 111.1(4) . . ? F118 C324 C221 113.3(4) . . ? C226 C225 C230 115.8(2) . . ? C226 C225 B200 122.69(19) . . ? C230 C225 B200 121.30(19) . . ? C227 C226 C225 122.0(2) . . ? C227 C226 H226 119.0 . . ? C225 C226 H226 119.0 . . ? C228 C227 C226 121.0(2) . . ? C228 C227 C231 117.8(2) . . ? C226 C227 C231 121.2(2) . . ? C229 C228 C227 118.3(2) . . ? C229 C228 H228 120.8 . . ? C227 C228 H228 120.8 . . ? C228 C229 C230 120.6(2) . . ? C228 C229 C232 116.6(3) . . ? C230 C229 C232 122.7(3) . . ? C228 C229 C332 121.7(3) . . ? C230 C229 C332 117.4(3) . . ? C232 C229 C332 8.7(3) . . ? C229 C230 C225 122.2(2) . . ? C229 C230 H230 118.9 . . ? C225 C230 H230 118.9 . . ? F19 C231 F20 106.8(2) . . ? F19 C231 F21 105.6(2) . . ? F20 C231 F21 105.3(2) . . ? F19 C231 C227 114.0(2) . . ? F20 C231 C227 112.7(2) . . ? F21 C231 C227 111.7(2) . . ? F24 C232 F22 107.6(5) . . ? F24 C232 F23 105.2(5) . . ? F22 C232 F23 106.0(4) . . ? F24 C232 C229 112.6(4) . . ? F22 C232 C229 111.7(4) . . ? F23 C232 C229 113.3(4) . . ? F122 C332 F124 106.3(5) . . ? F122 C332 F123 104.4(5) . . ? F124 C332 F123 104.6(5) . . ? F122 C332 C229 113.1(4) . . ? F124 C332 C229 112.7(5) . . ? F123 C332 C229 114.8(4) . . ? C801 C802 C803 111.4(17) . . ? C801 C802 H80K 109.3 . . ? C803 C802 H80K 109.3 . . ? C801 C802 H80L 109.3 . . ? C803 C802 H80L 109.3 . . ? H80K C802 H80L 108.0 . . ? C804 C803 C802 114(2) . . ? C804 C803 H80A 108.7 . . ? C802 C803 H80A 108.7 . . ? C804 C803 H80B 108.7 . . ? C802 C803 H80B 108.7 . . ? H80A C803 H80B 107.6 . . ? C805 C804 C803 109(2) . . ? C805 C804 H80F 109.8 . . ? C803 C804 H80F 109.8 . . ? C805 C804 H80G 109.8 . . ? C803 C804 H80G 109.8 . . ? H80F C804 H80G 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 B1 P1 C5 -81.3(2) . . . . ? P2 B1 P1 C1 148.59(18) . . . . ? C5 P1 C1 C2 44.1(4) . . . . ? B1 P1 C1 C2 172.2(3) . . . . ? C5 P1 C1 C3 -80.2(3) . . . . ? B1 P1 C1 C3 47.9(3) . . . . ? C5 P1 C1 C4 161.9(2) . . . . ? B1 P1 C1 C4 -69.9(3) . . . . ? C1 P1 C5 C8 172.5(2) . . . . ? B1 P1 C5 C8 46.4(2) . . . . ? C1 P1 C5 C7 -70.0(3) . . . . ? B1 P1 C5 C7 163.9(2) . . . . ? C1 P1 C5 C6 53.5(3) . . . . ? B1 P1 C5 C6 -72.7(3) . . . . ? P1 B1 P2 C13 -81.2(2) . . . . ? P1 B1 P2 C9 147.80(17) . . . . ? C13 P2 C9 C12 39.2(3) . . . . ? B1 P2 C9 C12 168.2(2) . . . . ? C13 P2 C9 C11 -83.9(3) . . . . ? B1 P2 C9 C11 45.1(3) . . . . ? C13 P2 C9 C10 158.7(2) . . . . ? B1 P2 C9 C10 -72.3(2) . . . . ? C9 P2 C13 C15 56.8(3) . . . . ? B1 P2 C13 C15 -70.0(3) . . . . ? C9 P2 C13 C14 175.7(3) . . . . ? B1 P2 C13 C14 48.9(3) . . . . ? C9 P2 C13 C16 -67.5(3) . . . . ? B1 P2 C13 C16 165.7(2) . . . . ? C225 B200 C201 C202 -23.8(3) . . . . ? C217 B200 C201 C202 -143.1(2) . . . . ? C209 B200 C201 C202 97.0(2) . . . . ? C225 B200 C201 C206 162.89(19) . . . . ? C217 B200 C201 C206 43.6(3) . . . . ? C209 B200 C201 C206 -76.3(2) . . . . ? C206 C201 C202 C203 -0.4(3) . . . . ? B200 C201 C202 C203 -173.9(2) . . . . ? C201 C202 C203 C204 0.8(4) . . . . ? C201 C202 C203 C307 -175.9(3) . . . . ? C201 C202 C203 C207 178.7(3) . . . . ? C202 C203 C204 C205 -0.6(4) . . . . ? C307 C203 C204 C205 176.1(3) . . . . ? C207 C203 C204 C205 -178.5(3) . . . . ? C203 C204 C205 C206 0.1(4) . . . . ? C203 C204 C205 C208 -178.0(2) . . . . ? C204 C205 C206 C201 0.3(4) . . . . ? C208 C205 C206 C201 178.4(2) . . . . ? C202 C201 C206 C205 -0.1(3) . . . . ? B200 C201 C206 C205 173.8(2) . . . . ? C204 C203 C207 F3 79.3(6) . . . . ? C202 C203 C207 F3 -98.6(6) . . . . ? C307 C203 C207 F3 171(5) . . . . ? C204 C203 C207 F2 -160.1(5) . . . . ? C202 C203 C207 F2 22.0(6) . . . . ? C307 C203 C207 F2 -69(4) . . . . ? C204 C203 C207 F1 -41.1(6) . . . . ? C202 C203 C207 F1 141.0(5) . . . . ? C307 C203 C207 F1 50(4) . . . . ? C204 C203 C307 F101 138.8(6) . . . . ? C202 C203 C307 F101 -44.4(7) . . . . ? C207 C203 C307 F101 48(4) . . . . ? C204 C203 C307 F102 20.1(8) . . . . ? C202 C203 C307 F102 -163.1(6) . . . . ? C207 C203 C307 F102 -71(4) . . . . ? C204 C203 C307 F103 -101.9(7) . . . . ? C202 C203 C307 F103 74.9(7) . . . . ? C207 C203 C307 F103 167(5) . . . . ? C204 C205 C208 F5 -10.1(4) . . . . ? C206 C205 C208 F5 171.7(2) . . . . ? C204 C205 C208 F6 -131.0(3) . . . . ? C206 C205 C208 F6 50.8(3) . . . . ? C204 C205 C208 F4 109.9(3) . . . . ? C206 C205 C208 F4 -68.2(3) . . . . ? C225 B200 C209 C214 -153.3(2) . . . . ? C217 B200 C209 C214 -34.0(3) . . . . ? C201 B200 C209 C214 83.7(2) . . . . ? C225 B200 C209 C210 37.3(3) . . . . ? C217 B200 C209 C210 156.6(2) . . . . ? C201 B200 C209 C210 -85.6(2) . . . . ? C214 C209 C210 C211 -0.4(3) . . . . ? B200 C209 C210 C211 169.7(2) . . . . ? C209 C210 C211 C212 -0.9(4) . . . . ? C209 C210 C211 C215 176.7(2) . . . . ? C210 C211 C212 C213 1.3(4) . . . . ? C215 C211 C212 C213 -176.4(3) . . . . ? C211 C212 C213 C214 -0.3(4) . . . . ? C211 C212 C213 C216 -179.0(3) . . . . ? C212 C213 C214 C209 -1.1(4) . . . . ? C216 C213 C214 C209 177.7(2) . . . . ? C210 C209 C214 C213 1.4(3) . . . . ? B200 C209 C214 C213 -168.5(2) . . . . ? C212 C211 C215 F8 80.6(3) . . . . ? C210 C211 C215 F8 -97.1(3) . . . . ? C212 C211 C215 F9 -38.6(4) . . . . ? C210 C211 C215 F9 143.7(3) . . . . ? C212 C211 C215 F7 -157.7(3) . . . . ? C210 C211 C215 F7 24.6(4) . . . . ? C212 C213 C216 F10 -5.0(5) . . . . ? C214 C213 C216 F10 176.3(3) . . . . ? C212 C213 C216 F12 118.1(3) . . . . ? C214 C213 C216 F12 -60.6(4) . . . . ? C212 C213 C216 F11 -126.2(3) . . . . ? C214 C213 C216 F11 55.1(4) . . . . ? C225 B200 C217 C222 80.3(2) . . . . ? C209 B200 C217 C222 -42.5(3) . . . . ? C201 B200 C217 C222 -155.0(2) . . . . ? C225 B200 C217 C218 -96.1(2) . . . . ? C209 B200 C217 C218 141.1(2) . . . . ? C201 B200 C217 C218 28.6(3) . . . . ? C222 C217 C218 C219 1.1(3) . . . . ? B200 C217 C218 C219 177.7(2) . . . . ? C217 C218 C219 C220 -1.7(4) . . . . ? C217 C218 C219 C223 174.1(2) . . . . ? C218 C219 C220 C221 0.9(4) . . . . ? C223 C219 C220 C221 -175.0(2) . . . . ? C219 C220 C221 C222 0.3(4) . . . . ? C219 C220 C221 C324 177.2(3) . . . . ? C219 C220 C221 C224 171.5(4) . . . . ? C220 C221 C222 C217 -0.8(4) . . . . ? C324 C221 C222 C217 -177.7(3) . . . . ? C224 C221 C222 C217 -172.2(4) . . . . ? C218 C217 C222 C221 0.1(3) . . . . ? B200 C217 C222 C221 -176.5(2) . . . . ? C220 C219 C223 F15 -45.1(3) . . . . ? C218 C219 C223 F15 139.0(2) . . . . ? C220 C219 C223 F14 74.5(3) . . . . ? C218 C219 C223 F14 -101.4(3) . . . . ? C220 C219 C223 F13 -166.0(2) . . . . ? C218 C219 C223 F13 18.2(3) . . . . ? C220 C221 C224 F18 7.7(9) . . . . ? C222 C221 C224 F18 179.1(9) . . . . ? C324 C221 C224 F18 -71(5) . . . . ? C220 C221 C224 F17 129.5(8) . . . . ? C222 C221 C224 F17 -59.1(10) . . . . ? C324 C221 C224 F17 51(5) . . . . ? C220 C221 C224 F16 -111.3(8) . . . . ? C222 C221 C224 F16 60.2(9) . . . . ? C324 C221 C224 F16 170(5) . . . . ? C220 C221 C324 F116 32.0(6) . . . . ? C222 C221 C324 F116 -151.0(5) . . . . ? C224 C221 C324 F116 136(5) . . . . ? C220 C221 C324 F117 -89.3(6) . . . . ? C222 C221 C324 F117 87.7(6) . . . . ? C224 C221 C324 F117 15(5) . . . . ? C220 C221 C324 F118 153.8(5) . . . . ? C222 C221 C324 F118 -29.2(6) . . . . ? C224 C221 C324 F118 -102(5) . . . . ? C217 B200 C225 C226 84.7(2) . . . . ? C209 B200 C225 C226 -151.7(2) . . . . ? C201 B200 C225 C226 -36.9(3) . . . . ? C217 B200 C225 C230 -89.5(2) . . . . ? C209 B200 C225 C230 34.1(3) . . . . ? C201 B200 C225 C230 148.9(2) . . . . ? C230 C225 C226 C227 -2.3(3) . . . . ? B200 C225 C226 C227 -176.8(2) . . . . ? C225 C226 C227 C228 1.3(3) . . . . ? C225 C226 C227 C231 -177.6(2) . . . . ? C226 C227 C228 C229 0.3(3) . . . . ? C231 C227 C228 C229 179.2(2) . . . . ? C227 C228 C229 C230 -0.7(3) . . . . ? C227 C228 C229 C232 176.8(3) . . . . ? C227 C228 C229 C332 -175.1(3) . . . . ? C228 C229 C230 C225 -0.4(4) . . . . ? C232 C229 C230 C225 -177.8(3) . . . . ? C332 C229 C230 C225 174.3(3) . . . . ? C226 C225 C230 C229 1.9(3) . . . . ? B200 C225 C230 C229 176.5(2) . . . . ? C228 C227 C231 F19 -173.6(2) . . . . ? C226 C227 C231 F19 5.4(3) . . . . ? C228 C227 C231 F20 -51.6(3) . . . . ? C226 C227 C231 F20 127.3(3) . . . . ? C228 C227 C231 F21 66.7(3) . . . . ? C226 C227 C231 F21 -114.3(3) . . . . ? C228 C229 C232 F24 -172.2(4) . . . . ? C230 C229 C232 F24 5.2(6) . . . . ? C332 C229 C232 F24 60(2) . . . . ? C228 C229 C232 F22 66.6(5) . . . . ? C230 C229 C232 F22 -115.9(5) . . . . ? C332 C229 C232 F22 -62(2) . . . . ? C228 C229 C232 F23 -52.9(5) . . . . ? C230 C229 C232 F23 124.5(4) . . . . ? C332 C229 C232 F23 179(3) . . . . ? C228 C229 C332 F122 -104.4(6) . . . . ? C230 C229 C332 F122 81.0(6) . . . . ? C232 C229 C332 F122 -49(2) . . . . ? C228 C229 C332 F124 16.3(7) . . . . ? C230 C229 C332 F124 -158.4(5) . . . . ? C232 C229 C332 F124 72(2) . . . . ? C228 C229 C332 F123 135.9(5) . . . . ? C230 C229 C332 F123 -38.8(6) . . . . ? C232 C229 C332 F123 -168(3) . . . . ? C801 C802 C803 C804 178(3) . . . . ? C802 C803 C804 C805 175(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.673 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.053 _database_code_depnum_ccdc_archive 'CCDC 912136' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6 #---------------------- # [Rh(PPh3)2(PPh3BH2PPh2)][BArF4].CH2Cl2 #---------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic . _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety . _chemical_formula_sum 'C99 H71 B2 Cl2 F24 P4 Rh' _chemical_formula_weight 2035.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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 12.9019(3) _cell_length_b 17.2700(4) _cell_length_c 21.5728(5) _cell_angle_alpha 99.512(2) _cell_angle_beta 91.448(2) _cell_angle_gamma 99.925(2) _cell_volume 4662.57(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16782 _cell_measurement_theta_min 3.4802 _cell_measurement_theta_max 74.2937 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2060 _exptl_absorpt_coefficient_mu 3.487 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_method Area _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 34348 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_unetI/netI 0.0577 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 74.46 _reflns_number_total 18397 _reflns_number_gt 16159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'Bruker SHELXTL' _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. Rotational disorder of the CF3 groups of the anion was treated by modelling either the fluorine atoms over two sites or the entire CF3 group and restraining their geometry. Restraints to thermal parameters were applied where necessary in order to maintain sensible values. ; _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^)+(0.0866P)^2^+16.0113P] 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 18397 _refine_ls_number_parameters 1396 _refine_ls_number_restraints 1372 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.1848 _refine_ls_wR_factor_gt 0.1771 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.154 _refine_ls_shift/su_max 0.014 _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 Rh1 Rh 0.80915(2) 0.101127(18) 0.734127(14) 0.02041(11) Uani 1 1 d . . . B1 B 0.6660(4) 0.1621(3) 0.7765(2) 0.0232(10) Uani 1 1 d . . . C1 C 0.9476(4) 0.0713(3) 0.8639(2) 0.0277(9) Uani 1 1 d . . . C2 C 0.9508(4) 0.1534(3) 0.8772(2) 0.0327(10) Uani 1 1 d . . . H2 H 0.9104 0.1777 0.8512 0.039 Uiso 1 1 calc R . . C3 C 1.0124(4) 0.1999(3) 0.9280(3) 0.0383(12) Uani 1 1 d . . . H3 H 1.0137 0.2558 0.9369 0.046 Uiso 1 1 calc R . . C4 C 1.0718(4) 0.1650(4) 0.9656(3) 0.0401(12) Uani 1 1 d . . . H4 H 1.1149 0.1971 1.0000 0.048 Uiso 1 1 calc R . . C5 C 1.0688(5) 0.0837(4) 0.9536(3) 0.0435(13) Uani 1 1 d . . . H5 H 1.1087 0.0596 0.9801 0.052 Uiso 1 1 calc R . . C6 C 1.0073(5) 0.0370(3) 0.9025(3) 0.0392(12) Uani 1 1 d . . . H6 H 1.0063 -0.0189 0.8939 0.047 Uiso 1 1 calc R . . C7 C 0.7590(4) -0.0478(3) 0.8283(2) 0.0274(9) Uani 1 1 d . . . C8 C 0.6552(4) -0.0434(3) 0.8134(3) 0.0345(11) Uani 1 1 d . . . H8 H 0.6403 -0.0091 0.7856 0.041 Uiso 1 1 calc R . . C9 C 0.5727(5) -0.0890(3) 0.8391(3) 0.0400(12) Uani 1 1 d . . . H9 H 0.5020 -0.0846 0.8293 0.048 Uiso 1 1 calc R . . C10 C 0.5930(5) -0.1403(3) 0.8784(3) 0.0401(12) Uani 1 1 d . . . H10 H 0.5367 -0.1716 0.8956 0.048 Uiso 1 1 calc R . . C11 C 0.6963(5) -0.1460(4) 0.8926(3) 0.0497(15) Uani 1 1 d . . . H11 H 0.7108 -0.1815 0.9196 0.060 Uiso 1 1 calc R . . C12 C 0.7779(5) -0.1007(4) 0.8679(3) 0.0443(14) Uani 1 1 d . . . H12 H 0.8484 -0.1055 0.8779 0.053 Uiso 1 1 calc R . . C13 C 0.9459(4) -0.0604(3) 0.7632(2) 0.0270(9) Uani 1 1 d . . . C14 C 0.8974(4) -0.1376(3) 0.7369(3) 0.0354(11) Uani 1 1 d . . . H14 H 0.8231 -0.1526 0.7375 0.042 Uiso 1 1 calc R . . C15 C 0.9566(5) -0.1927(3) 0.7099(3) 0.0437(13) Uani 1 1 d . . . H15 H 0.9227 -0.2453 0.6921 0.052 Uiso 1 1 calc R . . C16 C 1.0639(5) -0.1716(4) 0.7088(3) 0.0455(14) Uani 1 1 d . . . H16 H 1.1043 -0.2095 0.6902 0.055 Uiso 1 1 calc R . . C17 C 1.1134(5) -0.0951(4) 0.7345(3) 0.0446(13) Uani 1 1 d . . . H17 H 1.1876 -0.0805 0.7334 0.054 Uiso 1 1 calc R . . C18 C 1.0548(4) -0.0399(3) 0.7619(3) 0.0355(11) Uani 1 1 d . . . H18 H 1.0892 0.0124 0.7800 0.043 Uiso 1 1 calc R . . C19 C 0.8652(4) -0.0358(3) 0.6145(2) 0.0242(9) Uani 1 1 d . . . C20 C 0.7586(4) -0.0718(3) 0.6112(2) 0.0294(10) Uani 1 1 d . . . H20 H 0.7081 -0.0422 0.6293 0.035 Uiso 1 1 calc R . . C21 C 0.7267(4) -0.1502(3) 0.5818(2) 0.0332(11) Uani 1 1 d . . . H21 H 0.6540 -0.1734 0.5785 0.040 Uiso 1 1 calc R . . C22 C 0.7997(5) -0.1949(3) 0.5571(3) 0.0405(13) Uani 1 1 d . . . H22 H 0.7776 -0.2488 0.5371 0.049 Uiso 1 1 calc R . . C23 C 0.9048(5) -0.1607(3) 0.5617(3) 0.0431(13) Uani 1 1 d . . . H23 H 0.9551 -0.1918 0.5455 0.052 Uiso 1 1 calc R . . C24 C 0.9387(4) -0.0814(3) 0.5897(2) 0.0332(11) Uani 1 1 d . . . H24 H 1.0114 -0.0585 0.5918 0.040 Uiso 1 1 calc R . . C25 C 1.0387(4) 0.0996(3) 0.6533(2) 0.0260(9) Uani 1 1 d . . . C26 C 1.0904(4) 0.1334(3) 0.7116(2) 0.0321(10) Uani 1 1 d . . . H26 H 1.0510 0.1417 0.7479 0.039 Uiso 1 1 calc R . . C27 C 1.1996(5) 0.1550(4) 0.7162(3) 0.0443(13) Uani 1 1 d . . . H27 H 1.2348 0.1773 0.7560 0.053 Uiso 1 1 calc R . . C28 C 1.2571(4) 0.1441(4) 0.6634(3) 0.0442(13) Uani 1 1 d . . . H28 H 1.3318 0.1579 0.6670 0.053 Uiso 1 1 calc R . . C29 C 1.2060(4) 0.1131(3) 0.6051(3) 0.0404(12) Uani 1 1 d . . . H29 H 1.2455 0.1067 0.5686 0.048 Uiso 1 1 calc R . . C30 C 1.0979(4) 0.0914(3) 0.5998(2) 0.0321(10) Uani 1 1 d . . . H30 H 1.0632 0.0707 0.5596 0.039 Uiso 1 1 calc R . . C31 C 0.8649(4) 0.1152(3) 0.5789(2) 0.0255(9) Uani 1 1 d . . . C32 C 0.8061(4) 0.0721(3) 0.5250(2) 0.0326(10) Uani 1 1 d . . . H32 H 0.7791 0.0169 0.5229 0.039 Uiso 1 1 calc R . . C37 C 0.6298(3) 0.1639(3) 0.6346(2) 0.0228(8) Uani 1 1 d . . . C38 C 0.5605(4) 0.0915(3) 0.6293(2) 0.0308(10) Uani 1 1 d . . . H38 H 0.5627 0.0595 0.6610 0.037 Uiso 1 1 calc R . . C39 C 0.4880(4) 0.0656(3) 0.5782(3) 0.0376(12) Uani 1 1 d . . . H39 H 0.4418 0.0158 0.5750 0.045 Uiso 1 1 calc R . . C40 C 0.4827(4) 0.1119(4) 0.5319(3) 0.0415(13) Uani 1 1 d . . . H40 H 0.4326 0.0943 0.4972 0.050 Uiso 1 1 calc R . . C41 C 0.5513(5) 0.1840(4) 0.5368(3) 0.0434(13) Uani 1 1 d . . . H41 H 0.5483 0.2160 0.5051 0.052 Uiso 1 1 calc R . . C42 C 0.6244(4) 0.2101(3) 0.5875(2) 0.0328(11) Uani 1 1 d . . . H42 H 0.6711 0.2596 0.5903 0.039 Uiso 1 1 calc R . . C43 C 0.7890(4) 0.2943(3) 0.7070(2) 0.0250(9) Uani 1 1 d . . . C44 C 0.7346(4) 0.3552(3) 0.6988(2) 0.0333(11) Uani 1 1 d . . . H44 H 0.6616 0.3431 0.6864 0.040 Uiso 1 1 calc R . . C45 C 0.7881(6) 0.4345(3) 0.7088(3) 0.0482(15) Uani 1 1 d . . . H45 H 0.7511 0.4763 0.7037 0.058 Uiso 1 1 calc R . . C046 C 0.9033(4) 0.1961(3) 0.5806(2) 0.0302(10) Uani 1 1 d . . . H046 H 0.9449 0.2262 0.6163 0.036 Uiso 1 1 calc R . . C46 C 0.8933(6) 0.4518(3) 0.7259(3) 0.0511(17) Uani 1 1 d . . . H46 H 0.9289 0.5057 0.7326 0.061 Uiso 1 1 calc R . . C47 C 0.9489(5) 0.3916(4) 0.7336(3) 0.0461(15) Uani 1 1 d . . . H47 H 1.0222 0.4042 0.7451 0.055 Uiso 1 1 calc R . . C48 C 0.8966(4) 0.3130(3) 0.7244(2) 0.0329(11) Uani 1 1 d . . . H48 H 0.9342 0.2717 0.7300 0.040 Uiso 1 1 calc R . . C49 C 0.5638(4) 0.3100(3) 0.8090(2) 0.0294(10) Uani 1 1 d . . . C50 C 0.4951(4) 0.2796(3) 0.7566(3) 0.0373(12) Uani 1 1 d . . . H50 H 0.4805 0.2238 0.7415 0.045 Uiso 1 1 calc R . . C51 C 0.4472(5) 0.3306(4) 0.7261(4) 0.0505(16) Uani 1 1 d . . . H51 H 0.3993 0.3095 0.6908 0.061 Uiso 1 1 calc R . . C52 C 0.4697(5) 0.4120(4) 0.7476(4) 0.0530(16) Uani 1 1 d . . . H52 H 0.4393 0.4470 0.7260 0.064 Uiso 1 1 calc R . . C53 C 0.5364(5) 0.4424(3) 0.8003(3) 0.0462(14) Uani 1 1 d . . . H53 H 0.5501 0.4982 0.8155 0.055 Uiso 1 1 calc R . . C54 C 0.5837(5) 0.3919(3) 0.8313(3) 0.0361(11) Uani 1 1 d . . . H54 H 0.6294 0.4132 0.8676 0.043 Uiso 1 1 calc R . . C055 C 0.8813(4) 0.2332(3) 0.5304(3) 0.0360(11) Uani 1 1 d . . . H055 H 0.9061 0.2887 0.5325 0.043 Uiso 1 1 calc R . . C55 C 0.7307(4) 0.2995(3) 0.8991(2) 0.0281(9) Uani 1 1 d . . . C56 C 0.8116(5) 0.3504(3) 0.8774(3) 0.0404(12) Uani 1 1 d . . . H56 H 0.8142 0.3523 0.8337 0.048 Uiso 1 1 calc R . . C57 C 0.8891(5) 0.3988(4) 0.9198(3) 0.0460(14) Uani 1 1 d . . . H57 H 0.9435 0.4346 0.9051 0.055 Uiso 1 1 calc R . . C58 C 0.8863(5) 0.3943(4) 0.9828(3) 0.0428(13) Uani 1 1 d . . . H58 H 0.9397 0.4265 1.0116 0.051 Uiso 1 1 calc R . . C59 C 0.8071(5) 0.3438(4) 1.0043(3) 0.0422(13) Uani 1 1 d . . . H59 H 0.8057 0.3415 1.0480 0.051 Uiso 1 1 calc R . . C60 C 0.7289(4) 0.2961(3) 0.9629(2) 0.0351(11) Uani 1 1 d . . . H60 H 0.6742 0.2612 0.9782 0.042 Uiso 1 1 calc R . . C61 C 0.5312(4) 0.1875(3) 0.8872(2) 0.0300(10) Uani 1 1 d . . . C062 C 0.8232(4) 0.1889(3) 0.4773(3) 0.0383(12) Uani 1 1 d . . . H062 H 0.8086 0.2140 0.4430 0.046 Uiso 1 1 calc R . . C62 C 0.4350(5) 0.2110(3) 0.8976(3) 0.0431(13) Uani 1 1 d . . . H62 H 0.4199 0.2573 0.8834 0.052 Uiso 1 1 calc R . . C63 C 0.3604(6) 0.1659(4) 0.9291(4) 0.061(2) Uani 1 1 d . . . H63 H 0.2938 0.1812 0.9361 0.073 Uiso 1 1 calc R . . C64 C 0.3831(6) 0.0995(4) 0.9502(3) 0.059(2) Uani 1 1 d . . . H64 H 0.3322 0.0693 0.9720 0.071 Uiso 1 1 calc R . . C65 C 0.4792(6) 0.0764(4) 0.9399(3) 0.0566(18) Uani 1 1 d . . . H65 H 0.4945 0.0306 0.9548 0.068 Uiso 1 1 calc R . . C66 C 0.5532(5) 0.1200(3) 0.9079(3) 0.0421(13) Uani 1 1 d . . . H66 H 0.6190 0.1036 0.9002 0.051 Uiso 1 1 calc R . . C090 C 0.7867(5) 0.1087(4) 0.4745(3) 0.0401(12) Uani 1 1 d . . . H090 H 0.7481 0.0784 0.4378 0.048 Uiso 1 1 calc R . . P1 P 0.86634(9) 0.01381(6) 0.79467(5) 0.0228(2) Uani 1 1 d . . . P2 P 0.89497(9) 0.07049(6) 0.64752(5) 0.0216(2) Uani 1 1 d . . . P3 P 0.72474(8) 0.19125(6) 0.70119(5) 0.0199(2) Uani 1 1 d . . . P4 P 0.62830(9) 0.24093(7) 0.84334(5) 0.0233(2) Uani 1 1 d . . . B100 B 0.7411(4) 0.3729(3) 0.2295(2) 0.0229(10) Uani 1 1 d . . . C201 C 0.6399(4) 0.3226(3) 0.2583(2) 0.0247(9) Uani 1 1 d . A . C202 C 0.6447(4) 0.2511(3) 0.2801(2) 0.0275(9) Uani 1 1 d . . . H202 H 0.7083 0.2304 0.2774 0.033 Uiso 1 1 calc R . . C203 C 0.5584(4) 0.2097(3) 0.3057(2) 0.0302(10) Uani 1 1 d D A . C207 C 0.5688(3) 0.1332(3) 0.3273(2) 0.0382(12) Uani 1 1 d D . . F1 F 0.5151(8) 0.1197(6) 0.3763(5) 0.075(3) Uani 0.478(10) 1 d PDU A 1 F2 F 0.6679(5) 0.1311(5) 0.3463(5) 0.055(2) Uani 0.478(10) 1 d PDU A 1 F3 F 0.5446(10) 0.0694(4) 0.2844(4) 0.081(3) Uani 0.478(10) 1 d PDU A 1 F101 F 0.6063(8) 0.0832(4) 0.2839(4) 0.063(2) Uani 0.522(10) 1 d PDU A 2 F102 F 0.4759(5) 0.0910(4) 0.3362(5) 0.062(2) Uani 0.522(10) 1 d PDU A 2 F103 F 0.6261(9) 0.1417(5) 0.3783(4) 0.094(3) Uani 0.522(10) 1 d PDU A 2 C204 C 0.4649(4) 0.2379(3) 0.3109(3) 0.0356(11) Uani 1 1 d . . . H204 H 0.4057 0.2089 0.3274 0.043 Uiso 1 1 calc R A . C205 C 0.4599(4) 0.3094(3) 0.2915(3) 0.0393(12) Uani 1 1 d D A . C208 C 0.3599(6) 0.3406(3) 0.2969(3) 0.0706(15) Uani 0.490(9) 1 d PDU A 1 F4 F 0.2853(6) 0.2990(6) 0.2544(5) 0.099(3) Uani 0.490(9) 1 d PDU A 1 F5 F 0.3652(6) 0.4142(4) 0.2886(6) 0.070(2) Uani 0.490(9) 1 d PDU A 1 F6 F 0.3165(8) 0.3348(7) 0.3513(4) 0.094(3) Uani 0.490(9) 1 d PDU A 1 C308 C 0.3620(6) 0.3440(4) 0.2975(3) 0.0706(15) Uani 0.510(9) 1 d PDU A 2 F104 F 0.3775(7) 0.4147(4) 0.3340(6) 0.093(3) Uani 0.510(9) 1 d PDU A 2 F105 F 0.2832(5) 0.3002(4) 0.3204(5) 0.063(2) Uani 0.510(9) 1 d PDU A 2 F106 F 0.3242(8) 0.3577(8) 0.2436(4) 0.102(3) Uani 0.510(9) 1 d PDU A 2 C206 C 0.5450(4) 0.3508(3) 0.2659(3) 0.0320(10) Uani 1 1 d . . . H206 H 0.5388 0.3999 0.2531 0.038 Uiso 1 1 calc R A . C209 C 0.8108(4) 0.3147(3) 0.1878(2) 0.0239(9) Uani 1 1 d . . . C210 C 0.9169(4) 0.3426(3) 0.1774(2) 0.0270(9) Uani 1 1 d . B . H210 H 0.9496 0.3943 0.1980 0.032 Uiso 1 1 calc R . . C211 C 0.9754(4) 0.2970(3) 0.1379(2) 0.0320(10) Uani 1 1 d D . . C215 C 1.0869(6) 0.3308(4) 0.1282(3) 0.0475(12) Uani 0.352(19) 1 d PDU B 1 F7 F 1.1374(8) 0.3660(10) 0.1833(4) 0.057(3) Uani 0.352(19) 1 d PDU B 1 F8 F 1.1430(8) 0.2775(7) 0.1037(8) 0.060(4) Uani 0.352(19) 1 d PDU B 1 F9 F 1.0965(8) 0.3875(10) 0.0932(9) 0.070(3) Uani 0.352(19) 1 d PDU B 1 C315 C 1.0867(5) 0.3296(3) 0.1265(3) 0.0475(12) Uani 0.648(19) 1 d PDU B 2 F107 F 1.0950(5) 0.3508(7) 0.0701(3) 0.063(2) Uani 0.648(19) 1 d PDU B 2 F108 F 1.1298(5) 0.3927(5) 0.1683(5) 0.071(2) Uani 0.648(19) 1 d PDU B 2 F109 F 1.1485(5) 0.2755(4) 0.1263(5) 0.059(2) Uani 0.648(19) 1 d PDU B 2 C212 C 0.9296(4) 0.2221(3) 0.1055(3) 0.0353(11) Uani 1 1 d . B . H212 H 0.9693 0.1907 0.0785 0.042 Uiso 1 1 calc R . . C213 C 0.8247(4) 0.1945(3) 0.1138(2) 0.0319(10) Uani 1 1 d D . . C216 C 0.7711(4) 0.1143(3) 0.0803(2) 0.0447(13) Uani 1 1 d D B . F10 F 0.7768(14) 0.0571(4) 0.1134(7) 0.067(4) Uani 0.49(3) 1 d PDU B 1 F11 F 0.8133(12) 0.0925(9) 0.0263(6) 0.085(4) Uani 0.49(3) 1 d PDU B 1 F12 F 0.6702(6) 0.1107(6) 0.0661(8) 0.053(3) Uani 0.49(3) 1 d PDU B 1 F110 F 0.6882(10) 0.1177(6) 0.0447(8) 0.068(4) Uani 0.51(3) 1 d PDU B 2 F111 F 0.7340(16) 0.0666(6) 0.1208(4) 0.070(4) Uani 0.51(3) 1 d PDU B 2 F112 F 0.8326(7) 0.0755(6) 0.0449(7) 0.069(3) Uani 0.51(3) 1 d PDU B 2 C214 C 0.7667(4) 0.2397(3) 0.1545(2) 0.0276(9) Uani 1 1 d . B . H214 H 0.6951 0.2186 0.1596 0.033 Uiso 1 1 calc R . . C217 C 0.7025(4) 0.4234(3) 0.1781(2) 0.0257(9) Uani 1 1 d . . . C218 C 0.6180(4) 0.3884(3) 0.1350(2) 0.0300(10) Uani 1 1 d . . . H218 H 0.5789 0.3380 0.1395 0.036 Uiso 1 1 calc R . . C219 C 0.5890(5) 0.4246(3) 0.0859(3) 0.0364(11) Uani 1 1 d . . . C220 C 0.6441(5) 0.4979(3) 0.0776(3) 0.0389(12) Uani 1 1 d . C . H220 H 0.6247 0.5228 0.0440 0.047 Uiso 1 1 calc R . . C221 C 0.7283(4) 0.5342(3) 0.1195(2) 0.0356(11) Uani 1 1 d D . . C224 C 0.7889(4) 0.6118(4) 0.1107(3) 0.0567(14) Uani 0.547(8) 1 d PDU C 1 F16 F 0.8524(7) 0.6035(5) 0.0626(4) 0.084(3) Uani 0.547(8) 1 d PDU C 1 F17 F 0.8538(7) 0.6498(5) 0.1580(4) 0.078(3) Uani 0.547(8) 1 d PDU C 1 F18 F 0.7317(5) 0.6615(4) 0.0940(5) 0.074(2) Uani 0.547(8) 1 d PDU C 1 C324 C 0.7862(5) 0.6140(4) 0.1131(3) 0.0567(14) Uani 0.453(8) 1 d PDU C 2 F116 F 0.7478(8) 0.6721(4) 0.1475(6) 0.082(3) Uani 0.453(8) 1 d PDU C 2 F117 F 0.7835(10) 0.6306(6) 0.0557(4) 0.089(3) Uani 0.453(8) 1 d PDU C 2 F118 F 0.8864(5) 0.6282(5) 0.1331(6) 0.066(3) Uani 0.453(8) 1 d PDU C 2 C222 C 0.7572(4) 0.4972(3) 0.1686(2) 0.0295(10) Uani 1 1 d . C . H222 H 0.8158 0.5231 0.1964 0.035 Uiso 1 1 calc R . . C223 C 0.4957(6) 0.3857(4) 0.0427(3) 0.0492(15) Uani 1 1 d . . . C225 C 0.8095(4) 0.4294(3) 0.2905(2) 0.0236(9) Uani 1 1 d . . . C226 C 0.7844(4) 0.5028(3) 0.3173(2) 0.0287(10) Uani 1 1 d . D . H226 H 0.7281 0.5213 0.2985 0.034 Uiso 1 1 calc R . . C227 C 0.8391(4) 0.5495(3) 0.3706(2) 0.0343(11) Uani 1 1 d D . . C228 C 0.9207(4) 0.5244(3) 0.4004(2) 0.0320(10) Uani 1 1 d . D . H228 H 0.9580 0.5564 0.4369 0.038 Uiso 1 1 calc R . . C229 C 0.9459(4) 0.4518(3) 0.3755(2) 0.0283(10) Uani 1 1 d . . . C230 C 0.8911(4) 0.4047(3) 0.3218(2) 0.0260(9) Uani 1 1 d . D . H230 H 0.9097 0.3545 0.3062 0.031 Uiso 1 1 calc R . . C231 C 0.8103(4) 0.6285(4) 0.3944(2) 0.0587(14) Uani 0.725(9) 1 d PDU D 1 F19 F 0.8359(6) 0.6800(3) 0.3542(3) 0.081(2) Uani 0.725(9) 1 d PDU D 1 F20 F 0.7087(4) 0.6270(3) 0.3982(4) 0.0706(19) Uani 0.725(9) 1 d PDU D 1 F21 F 0.8606(5) 0.6663(4) 0.4473(3) 0.073(2) Uani 0.725(9) 1 d PDU D 1 C331 C 0.8081(6) 0.6269(5) 0.3971(4) 0.0587(14) Uani 0.275(9) 1 d PDU D 2 F119 F 0.7423(12) 0.6191(7) 0.4424(7) 0.080(4) Uani 0.275(9) 1 d PDU D 2 F120 F 0.8878(8) 0.6821(6) 0.4238(7) 0.061(4) Uani 0.275(9) 1 d PDU D 2 F121 F 0.7603(14) 0.6599(7) 0.3560(6) 0.078(4) Uani 0.275(9) 1 d PDU D 2 C232 C 1.0330(5) 0.4212(3) 0.4052(3) 0.0387(12) Uani 1 1 d . D . F13 F 0.4704(4) 0.3077(3) 0.0429(2) 0.0808(16) Uani 1 1 d U . . F14 F 0.4108(3) 0.4186(3) 0.0572(2) 0.0701(12) Uani 1 1 d U . . F15 F 0.5118(4) 0.3930(2) -0.01729(17) 0.0587(10) Uani 1 1 d U . . F22 F 0.9985(4) 0.3610(3) 0.4347(2) 0.0774(14) Uani 1 1 d U . . F23 F 1.0923(3) 0.4771(2) 0.44844(18) 0.0593(10) Uani 1 1 d U . . F24 F 1.0998(3) 0.3957(2) 0.36372(18) 0.0539(9) Uani 1 1 d U . . Cl1 Cl 0.4573(6) 0.5914(4) 0.4430(4) 0.163(4) Uani 0.638(9) 1 d PDU E 1 C500 C 0.353(2) 0.5602(13) 0.4844(15) 0.22(2) Uani 0.638(9) 1 d PD E 1 H50A H 0.3709 0.5171 0.5055 0.268 Uiso 0.638(9) 1 calc PR E 1 H50B H 0.2931 0.5359 0.4538 0.268 Uiso 0.638(9) 1 calc PR E 1 Cl01 Cl 0.5115(11) 0.6234(8) 0.5238(8) 0.164(6) Uani 0.362(9) 1 d PDU E 2 C005 C 0.4046(13) 0.576(2) 0.5548(19) 0.118(12) Uani 0.362(9) 1 d PD E 2 H00A H 0.3861 0.5197 0.5342 0.141 Uiso 0.362(9) 1 calc PR E 2 H00B H 0.4169 0.5788 0.6006 0.141 Uiso 0.362(9) 1 calc PR E 2 Cl3 Cl 0.3090(5) 0.6271(3) 0.5400(3) 0.203(2) Uani 1 1 d DU . . H1A H 0.595(4) 0.123(3) 0.766(3) 0.026(13) Uiso 1 1 d . . . H1B H 0.721(6) 0.131(4) 0.799(4) 0.06(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02476(18) 0.02088(17) 0.01934(16) 0.00952(12) 0.00527(12) 0.00813(12) B1 0.024(2) 0.017(2) 0.030(3) 0.0067(19) 0.0062(19) 0.0043(18) C1 0.031(2) 0.027(2) 0.025(2) 0.0066(18) 0.0010(18) 0.0038(18) C2 0.036(3) 0.028(2) 0.034(3) 0.009(2) 0.003(2) 0.005(2) C3 0.040(3) 0.034(3) 0.039(3) 0.003(2) 0.007(2) 0.005(2) C4 0.036(3) 0.053(3) 0.029(3) 0.000(2) 0.003(2) 0.005(2) C5 0.045(3) 0.054(3) 0.033(3) 0.009(2) -0.008(2) 0.014(3) C6 0.050(3) 0.035(3) 0.034(3) 0.008(2) -0.008(2) 0.012(2) C7 0.034(2) 0.027(2) 0.025(2) 0.0111(18) 0.0062(18) 0.0094(19) C8 0.038(3) 0.030(2) 0.038(3) 0.017(2) -0.002(2) 0.005(2) C9 0.035(3) 0.039(3) 0.048(3) 0.017(2) 0.002(2) 0.002(2) C10 0.045(3) 0.038(3) 0.041(3) 0.019(2) 0.015(2) 0.002(2) C11 0.052(4) 0.058(4) 0.051(4) 0.037(3) 0.016(3) 0.015(3) C12 0.041(3) 0.056(4) 0.049(3) 0.035(3) 0.012(3) 0.019(3) C13 0.036(2) 0.023(2) 0.026(2) 0.0088(17) 0.0037(19) 0.0123(19) C14 0.037(3) 0.031(3) 0.041(3) 0.009(2) 0.004(2) 0.009(2) C15 0.056(4) 0.028(3) 0.050(3) 0.007(2) 0.009(3) 0.014(2) C16 0.055(4) 0.039(3) 0.051(3) 0.011(3) 0.014(3) 0.027(3) C17 0.036(3) 0.050(3) 0.053(3) 0.012(3) 0.006(3) 0.018(3) C18 0.036(3) 0.032(3) 0.042(3) 0.010(2) 0.002(2) 0.013(2) C19 0.028(2) 0.026(2) 0.021(2) 0.0100(17) 0.0067(17) 0.0023(17) C20 0.031(2) 0.031(2) 0.028(2) 0.0085(19) 0.0092(19) 0.0071(19) C21 0.038(3) 0.031(2) 0.030(2) 0.011(2) 0.005(2) -0.002(2) C22 0.056(3) 0.026(2) 0.037(3) 0.002(2) 0.013(2) 0.002(2) C23 0.052(3) 0.029(3) 0.050(3) 0.002(2) 0.021(3) 0.014(2) C24 0.034(3) 0.031(2) 0.036(3) 0.007(2) 0.014(2) 0.008(2) C25 0.025(2) 0.026(2) 0.029(2) 0.0092(18) 0.0052(18) 0.0069(17) C26 0.031(2) 0.035(3) 0.030(2) 0.007(2) 0.0022(19) 0.004(2) C27 0.036(3) 0.047(3) 0.045(3) 0.003(3) -0.005(2) 0.001(2) C28 0.025(3) 0.047(3) 0.058(4) 0.006(3) 0.004(2) 0.002(2) C29 0.033(3) 0.040(3) 0.048(3) 0.007(2) 0.015(2) 0.004(2) C30 0.030(2) 0.035(3) 0.030(2) 0.007(2) 0.0085(19) 0.002(2) C31 0.025(2) 0.028(2) 0.025(2) 0.0073(18) 0.0067(17) 0.0070(18) C32 0.039(3) 0.029(2) 0.030(2) 0.008(2) -0.001(2) 0.003(2) C37 0.023(2) 0.027(2) 0.0197(19) 0.0099(17) 0.0027(16) 0.0030(17) C38 0.037(3) 0.030(2) 0.027(2) 0.0116(19) 0.002(2) 0.005(2) C39 0.033(3) 0.037(3) 0.040(3) 0.007(2) -0.003(2) -0.002(2) C40 0.033(3) 0.054(3) 0.036(3) 0.011(2) -0.008(2) 0.003(2) C41 0.050(3) 0.050(3) 0.034(3) 0.021(2) -0.006(2) 0.007(3) C42 0.035(3) 0.034(3) 0.033(3) 0.017(2) 0.001(2) 0.003(2) C43 0.031(2) 0.022(2) 0.022(2) 0.0081(17) 0.0061(17) 0.0012(17) C44 0.041(3) 0.024(2) 0.037(3) 0.013(2) 0.010(2) 0.005(2) C45 0.072(4) 0.023(3) 0.052(3) 0.014(2) 0.020(3) 0.005(3) C046 0.034(3) 0.033(2) 0.025(2) 0.0082(19) 0.0062(19) 0.007(2) C46 0.070(4) 0.029(3) 0.046(3) 0.006(2) 0.019(3) -0.016(3) C47 0.041(3) 0.049(3) 0.037(3) 0.001(2) 0.012(2) -0.016(3) C48 0.032(3) 0.038(3) 0.026(2) 0.006(2) 0.0056(19) -0.002(2) C49 0.028(2) 0.027(2) 0.036(3) 0.0075(19) 0.0076(19) 0.0083(18) C50 0.032(3) 0.030(3) 0.053(3) 0.012(2) -0.003(2) 0.009(2) C51 0.038(3) 0.044(3) 0.074(4) 0.019(3) -0.012(3) 0.014(3) C52 0.044(3) 0.043(3) 0.082(5) 0.027(3) 0.000(3) 0.021(3) C53 0.055(4) 0.030(3) 0.059(4) 0.011(3) 0.010(3) 0.020(3) C54 0.044(3) 0.028(2) 0.039(3) 0.006(2) 0.010(2) 0.013(2) C055 0.042(3) 0.035(3) 0.036(3) 0.019(2) 0.011(2) 0.007(2) C55 0.031(2) 0.028(2) 0.026(2) 0.0026(18) 0.0038(18) 0.0082(19) C56 0.043(3) 0.043(3) 0.031(3) 0.004(2) 0.009(2) -0.002(2) C57 0.041(3) 0.044(3) 0.045(3) 0.004(3) 0.006(3) -0.010(2) C58 0.044(3) 0.040(3) 0.041(3) 0.003(2) -0.007(2) 0.004(2) C59 0.049(3) 0.045(3) 0.033(3) 0.011(2) -0.006(2) 0.006(3) C60 0.040(3) 0.037(3) 0.030(2) 0.012(2) 0.002(2) 0.005(2) C61 0.035(3) 0.028(2) 0.025(2) 0.0029(18) 0.0094(19) -0.0029(19) C062 0.041(3) 0.048(3) 0.033(3) 0.022(2) 0.006(2) 0.012(2) C62 0.038(3) 0.038(3) 0.051(3) 0.003(2) 0.022(3) 0.002(2) C63 0.047(4) 0.053(4) 0.072(5) -0.005(3) 0.031(3) -0.009(3) C64 0.069(4) 0.047(4) 0.046(3) -0.004(3) 0.031(3) -0.023(3) C65 0.087(5) 0.043(3) 0.037(3) 0.015(3) 0.017(3) -0.009(3) C66 0.052(3) 0.044(3) 0.034(3) 0.018(2) 0.015(2) 0.004(3) C090 0.046(3) 0.048(3) 0.027(2) 0.015(2) -0.005(2) 0.006(2) P1 0.0285(6) 0.0214(5) 0.0229(5) 0.0111(4) 0.0033(4) 0.0092(4) P2 0.0236(5) 0.0240(5) 0.0199(5) 0.0084(4) 0.0063(4) 0.0064(4) P3 0.0220(5) 0.0189(5) 0.0216(5) 0.0097(4) 0.0036(4) 0.0056(4) P4 0.0249(5) 0.0220(5) 0.0247(5) 0.0078(4) 0.0073(4) 0.0048(4) B100 0.023(2) 0.020(2) 0.027(2) 0.0113(19) 0.0045(19) 0.0032(18) C201 0.027(2) 0.025(2) 0.023(2) 0.0097(17) 0.0018(17) 0.0033(17) C202 0.028(2) 0.031(2) 0.027(2) 0.0137(19) 0.0024(18) 0.0054(18) C203 0.033(2) 0.030(2) 0.031(2) 0.017(2) 0.0026(19) 0.0054(19) C207 0.038(3) 0.037(3) 0.047(3) 0.027(2) 0.007(2) 0.008(2) F1 0.090(6) 0.082(5) 0.083(6) 0.064(5) 0.047(5) 0.043(5) F2 0.044(4) 0.056(4) 0.083(5) 0.056(4) 0.003(4) 0.013(3) F3 0.106(7) 0.052(5) 0.086(6) 0.024(4) -0.035(5) 0.010(5) F101 0.076(5) 0.046(4) 0.088(5) 0.040(3) 0.036(4) 0.037(4) F102 0.048(4) 0.038(4) 0.112(6) 0.048(4) 0.019(4) 0.004(3) F103 0.122(7) 0.081(5) 0.081(6) 0.052(5) -0.045(5) -0.001(5) C204 0.031(3) 0.035(3) 0.046(3) 0.021(2) 0.009(2) 0.004(2) C205 0.033(3) 0.038(3) 0.054(3) 0.022(2) 0.013(2) 0.011(2) C208 0.049(3) 0.064(3) 0.116(4) 0.046(3) 0.028(3) 0.023(2) F4 0.055(4) 0.093(5) 0.154(6) 0.026(5) -0.008(5) 0.026(4) F5 0.048(4) 0.054(4) 0.133(6) 0.055(4) 0.037(4) 0.034(3) F6 0.075(5) 0.099(6) 0.125(6) 0.039(5) 0.046(5) 0.039(4) C308 0.049(3) 0.064(3) 0.116(4) 0.046(3) 0.028(3) 0.023(2) F104 0.070(5) 0.079(5) 0.139(6) 0.014(5) 0.025(5) 0.041(4) F105 0.029(3) 0.046(4) 0.123(6) 0.034(4) 0.033(4) 0.011(3) F106 0.073(5) 0.126(6) 0.129(6) 0.053(5) 0.007(5) 0.046(5) C206 0.031(2) 0.026(2) 0.044(3) 0.017(2) 0.007(2) 0.0068(19) C209 0.030(2) 0.021(2) 0.023(2) 0.0098(17) 0.0015(17) 0.0055(17) C210 0.030(2) 0.028(2) 0.025(2) 0.0097(18) 0.0015(18) 0.0054(18) C211 0.031(2) 0.034(3) 0.031(2) 0.006(2) 0.004(2) 0.007(2) C215 0.036(2) 0.052(3) 0.052(3) 0.002(2) 0.010(2) 0.007(2) F7 0.038(5) 0.059(6) 0.064(6) -0.006(5) 0.002(4) 0.000(4) F8 0.041(5) 0.074(6) 0.054(6) -0.022(5) 0.009(4) 0.011(4) F9 0.053(5) 0.074(6) 0.082(6) 0.024(5) 0.012(5) -0.001(5) C315 0.036(2) 0.052(3) 0.052(3) 0.002(2) 0.010(2) 0.007(2) F107 0.052(3) 0.076(5) 0.058(4) 0.021(4) 0.018(3) -0.008(3) F108 0.042(3) 0.063(4) 0.090(5) -0.025(4) 0.019(3) -0.005(3) F109 0.038(3) 0.075(4) 0.065(5) 0.002(3) 0.002(3) 0.022(3) C212 0.040(3) 0.035(3) 0.033(3) 0.003(2) 0.003(2) 0.014(2) C213 0.038(3) 0.024(2) 0.034(3) 0.0034(19) -0.002(2) 0.008(2) C216 0.049(3) 0.031(3) 0.052(3) 0.000(2) -0.002(3) 0.007(2) F10 0.083(7) 0.028(4) 0.089(6) 0.009(4) -0.025(5) 0.013(4) F11 0.083(7) 0.076(7) 0.074(6) -0.028(5) 0.022(5) -0.006(5) F12 0.046(4) 0.045(4) 0.059(6) -0.015(4) -0.009(4) 0.007(3) F110 0.078(6) 0.055(5) 0.062(6) -0.010(4) -0.032(5) 0.014(4) F111 0.092(8) 0.039(4) 0.069(5) 0.007(4) 0.006(5) -0.015(4) F112 0.068(5) 0.037(4) 0.091(7) -0.028(4) -0.001(5) 0.021(4) C214 0.031(2) 0.024(2) 0.029(2) 0.0105(18) 0.0020(19) 0.0039(18) C217 0.029(2) 0.024(2) 0.027(2) 0.0097(18) 0.0046(18) 0.0064(18) C218 0.036(3) 0.027(2) 0.029(2) 0.0122(19) 0.001(2) 0.0036(19) C219 0.045(3) 0.036(3) 0.031(3) 0.012(2) -0.004(2) 0.011(2) C220 0.047(3) 0.041(3) 0.036(3) 0.023(2) 0.002(2) 0.014(2) C221 0.037(3) 0.036(3) 0.041(3) 0.023(2) 0.007(2) 0.009(2) C224 0.056(3) 0.046(3) 0.079(3) 0.045(2) 0.003(2) 0.006(2) F16 0.076(5) 0.071(4) 0.106(5) 0.035(4) 0.041(4) -0.011(4) F17 0.096(5) 0.051(4) 0.082(5) 0.032(4) -0.013(4) -0.021(4) F18 0.061(4) 0.045(3) 0.128(6) 0.055(4) -0.005(4) 0.009(3) C324 0.056(3) 0.046(3) 0.079(3) 0.045(2) 0.003(2) 0.006(2) F116 0.085(5) 0.042(4) 0.117(6) 0.020(4) 0.022(5) -0.003(4) F117 0.111(6) 0.077(5) 0.082(5) 0.055(4) -0.005(5) -0.016(5) F118 0.047(4) 0.055(4) 0.106(6) 0.049(4) 0.003(4) 0.001(3) C222 0.030(2) 0.028(2) 0.035(3) 0.015(2) 0.0031(19) 0.0061(19) C223 0.064(4) 0.047(3) 0.038(3) 0.016(3) -0.015(3) 0.007(3) C225 0.026(2) 0.023(2) 0.024(2) 0.0116(17) 0.0062(17) 0.0023(17) C226 0.029(2) 0.028(2) 0.031(2) 0.0062(19) 0.0020(19) 0.0071(18) C227 0.034(3) 0.033(3) 0.036(3) 0.003(2) 0.003(2) 0.008(2) C228 0.038(3) 0.032(2) 0.025(2) 0.0034(19) -0.0013(19) 0.006(2) C229 0.033(2) 0.029(2) 0.025(2) 0.0122(18) 0.0023(18) 0.0051(19) C230 0.031(2) 0.023(2) 0.026(2) 0.0106(17) 0.0049(18) 0.0049(18) C231 0.061(3) 0.047(3) 0.067(3) -0.009(2) -0.006(3) 0.024(2) F19 0.105(5) 0.042(3) 0.101(4) 0.012(3) 0.012(4) 0.026(3) F20 0.049(3) 0.060(3) 0.099(4) -0.020(3) -0.002(3) 0.032(2) F21 0.079(4) 0.062(3) 0.070(4) -0.029(3) -0.022(3) 0.035(3) C331 0.061(3) 0.047(3) 0.067(3) -0.009(2) -0.006(3) 0.024(2) F119 0.079(6) 0.061(6) 0.095(6) -0.015(5) 0.025(6) 0.022(5) F120 0.064(6) 0.037(5) 0.077(6) -0.009(5) 0.008(5) 0.010(5) F121 0.080(6) 0.064(6) 0.091(6) -0.005(5) -0.022(6) 0.040(5) C232 0.043(3) 0.041(3) 0.035(3) 0.012(2) -0.006(2) 0.010(2) F13 0.110(4) 0.052(2) 0.071(3) 0.026(2) -0.053(3) -0.017(2) F14 0.049(2) 0.105(3) 0.054(2) 0.012(2) -0.0137(18) 0.012(2) F15 0.082(3) 0.063(2) 0.0340(17) 0.0102(16) -0.0143(17) 0.020(2) F22 0.073(3) 0.082(3) 0.091(3) 0.066(3) -0.017(2) 0.007(2) F23 0.056(2) 0.067(2) 0.051(2) -0.0053(18) -0.0252(17) 0.0198(18) F24 0.052(2) 0.065(2) 0.050(2) 0.0040(17) -0.0071(16) 0.0331(18) Cl1 0.161(6) 0.135(5) 0.206(8) 0.047(5) 0.055(5) 0.039(4) C500 0.12(2) 0.100(18) 0.42(6) -0.01(3) 0.07(3) -0.011(15) Cl01 0.159(9) 0.156(9) 0.196(11) 0.060(7) 0.021(7) 0.050(7) C005 0.13(3) 0.11(3) 0.11(3) 0.03(2) 0.02(2) 0.00(2) Cl3 0.203(5) 0.159(4) 0.247(6) 0.051(4) 0.096(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 Rh1 P2 2.2308(11) . ? Rh1 P3 2.2414(11) . ? Rh1 P1 2.3473(11) . ? Rh1 B1 2.407(5) . ? Rh1 H1B 1.89(8) . ? B1 P3 1.915(5) . ? B1 P4 1.945(5) . ? B1 H1A 1.04(6) . ? B1 H1B 1.11(8) . ? C1 C6 1.387(7) . ? C1 C2 1.392(7) . ? C1 P1 1.841(5) . ? C2 C3 1.388(8) . ? C2 H2 0.9500 . ? C3 C4 1.377(8) . ? C3 H3 0.9500 . ? C4 C5 1.379(9) . ? C4 H4 0.9500 . ? C5 C6 1.392(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.386(7) . ? C7 C12 1.396(7) . ? C7 P1 1.837(5) . ? C8 C9 1.394(7) . ? C8 H8 0.9500 . ? C9 C10 1.375(8) . ? C9 H9 0.9500 . ? C10 C11 1.383(9) . ? C10 H10 0.9500 . ? C11 C12 1.374(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.390(7) . ? C13 C14 1.391(7) . ? C13 P1 1.833(5) . ? C14 C15 1.385(8) . ? C14 H14 0.9500 . ? C15 C16 1.373(9) . ? C15 H15 0.9500 . ? C16 C17 1.381(9) . ? C16 H16 0.9500 . ? C17 C18 1.384(8) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.396(7) . ? C19 C20 1.403(7) . ? C19 P2 1.826(5) . ? C20 C21 1.384(7) . ? C20 H20 0.9500 . ? C21 C22 1.381(8) . ? C21 H21 0.9500 . ? C22 C23 1.376(9) . ? C22 H22 0.9500 . ? C23 C24 1.392(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.395(7) . ? C25 C30 1.400(7) . ? C25 P2 1.832(5) . ? C26 C27 1.390(8) . ? C26 H26 0.9500 . ? C27 C28 1.381(9) . ? C27 H27 0.9500 . ? C28 C29 1.385(9) . ? C28 H28 0.9500 . ? C29 C30 1.377(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C046 1.394(7) . ? C31 C32 1.400(7) . ? C31 P2 1.840(5) . ? C32 C090 1.385(7) . ? C32 H32 0.9500 . ? C37 C38 1.392(7) . ? C37 C42 1.399(6) . ? C37 P3 1.809(4) . ? C38 C39 1.389(7) . ? C38 H38 0.9500 . ? C39 C40 1.385(8) . ? C39 H39 0.9500 . ? C40 C41 1.385(8) . ? C40 H40 0.9500 . ? C41 C42 1.390(8) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.393(7) . ? C43 C48 1.398(7) . ? C43 P3 1.811(4) . ? C44 C45 1.403(7) . ? C44 H44 0.9500 . ? C45 C46 1.366(10) . ? C45 H45 0.9500 . ? C046 C055 1.392(7) . ? C046 H046 0.9500 . ? C46 C47 1.390(10) . ? C46 H46 0.9500 . ? C47 C48 1.388(8) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.389(8) . ? C49 C54 1.394(7) . ? C49 P4 1.808(5) . ? C50 C51 1.396(8) . ? C50 H50 0.9500 . ? C51 C52 1.382(9) . ? C51 H51 0.9500 . ? C52 C53 1.381(10) . ? C52 H52 0.9500 . ? C53 C54 1.392(8) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C055 C062 1.389(8) . ? C055 H055 0.9500 . ? C55 C56 1.387(7) . ? C55 C60 1.388(7) . ? C55 P4 1.809(5) . ? C56 C57 1.394(8) . ? C56 H56 0.9500 . ? C57 C58 1.376(9) . ? C57 H57 0.9500 . ? C58 C59 1.367(9) . ? C58 H58 0.9500 . ? C59 C60 1.384(8) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.383(8) . ? C61 C66 1.387(8) . ? C61 P4 1.807(5) . ? C062 C090 1.374(8) . ? C062 H062 0.9500 . ? C62 C63 1.395(8) . ? C62 H62 0.9500 . ? C63 C64 1.375(12) . ? C63 H63 0.9500 . ? C64 C65 1.378(11) . ? C64 H64 0.9500 . ? C65 C66 1.383(8) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C090 H090 0.9500 . ? B100 C201 1.636(6) . ? B100 C217 1.637(6) . ? B100 C209 1.637(7) . ? B100 C225 1.638(7) . ? C201 C206 1.398(7) . ? C201 C202 1.401(6) . ? C202 C203 1.393(6) . ? C202 H202 0.9500 . ? C203 C204 1.377(7) . ? C203 C207 1.498(7) . ? C207 F103 1.283(6) . ? C207 F3 1.303(7) . ? C207 F1 1.311(6) . ? C207 F101 1.324(6) . ? C207 F102 1.327(6) . ? C207 F2 1.341(6) . ? C204 C205 1.380(7) . ? C204 H204 0.9500 . ? C205 C206 1.383(7) . ? C205 C208 1.481(9) . ? C205 C308 1.487(9) . ? C208 F5 1.303(5) . ? C208 F6 1.324(5) . ? C208 F4 1.335(5) . ? C308 F105 1.316(6) . ? C308 F104 1.319(6) . ? C308 F106 1.322(6) . ? C206 H206 0.9500 . ? C209 C214 1.392(6) . ? C209 C210 1.406(7) . ? C210 C211 1.389(7) . ? C210 H210 0.9500 . ? C211 C212 1.389(7) . ? C211 C215 1.491(9) . ? C211 C315 1.492(8) . ? C215 F8 1.318(5) . ? C215 F9 1.323(5) . ? C215 F7 1.338(5) . ? C315 F108 1.323(5) . ? C315 F109 1.328(5) . ? C315 F107 1.329(5) . ? C212 C213 1.381(7) . ? C212 H212 0.9500 . ? C213 C214 1.395(7) . ? C213 C216 1.495(7) . ? C216 F112 1.308(7) . ? C216 F110 1.317(7) . ? C216 F12 1.318(7) . ? C216 F10 1.321(7) . ? C216 F11 1.325(7) . ? C216 F111 1.338(7) . ? C214 H214 0.9500 . ? C217 C222 1.395(6) . ? C217 C218 1.398(7) . ? C218 C219 1.389(7) . ? C218 H218 0.9500 . ? C219 C220 1.383(8) . ? C219 C223 1.492(8) . ? C220 C221 1.385(8) . ? C220 H220 0.9500 . ? C221 C222 1.398(7) . ? C221 C224 1.475(8) . ? C221 C324 1.481(9) . ? C224 F18 1.310(5) . ? C224 F17 1.312(5) . ? C224 F16 1.343(5) . ? C324 F117 1.317(6) . ? C324 F118 1.320(6) . ? C324 F116 1.321(6) . ? C222 H222 0.9500 . ? C223 F13 1.332(7) . ? C223 F15 1.339(7) . ? C223 F14 1.339(8) . ? C225 C226 1.399(7) . ? C225 C230 1.401(7) . ? C226 C227 1.388(7) . ? C226 H226 0.9500 . ? C227 C228 1.386(7) . ? C227 C231 1.488(8) . ? C227 C331 1.489(10) . ? C228 C229 1.377(7) . ? C228 H228 0.9500 . ? C229 C230 1.396(7) . ? C229 C232 1.495(7) . ? C230 H230 0.9500 . ? C231 F21 1.311(5) . ? C231 F20 1.312(5) . ? C231 F19 1.351(5) . ? C331 F119 1.319(6) . ? C331 F120 1.322(6) . ? C331 F121 1.323(6) . ? C232 F22 1.326(7) . ? C232 F24 1.332(7) . ? C232 F23 1.341(7) . ? Cl1 C500 1.695(12) . ? C500 Cl3 1.701(12) . ? C500 H50A 0.9900 . ? C500 H50B 0.9900 . ? Cl01 C005 1.689(13) . ? C005 Cl3 1.685(13) . ? C005 H00A 0.9900 . ? C005 H00B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Rh1 P3 98.18(4) . . ? P2 Rh1 P1 99.05(4) . . ? P3 Rh1 P1 162.70(4) . . ? P2 Rh1 B1 144.80(13) . . ? P3 Rh1 B1 48.50(12) . . ? P1 Rh1 B1 114.31(13) . . ? P2 Rh1 H1B 171(2) . . ? P3 Rh1 H1B 74(2) . . ? P1 Rh1 H1B 89(2) . . ? B1 Rh1 H1B 27(2) . . ? P3 B1 P4 121.8(3) . . ? P3 B1 Rh1 61.22(14) . . ? P4 B1 Rh1 144.1(3) . . ? P3 B1 H1A 110(3) . . ? P4 B1 H1A 102(3) . . ? Rh1 B1 H1A 111(3) . . ? P3 B1 H1B 109(4) . . ? P4 B1 H1B 106(4) . . ? Rh1 B1 H1B 50(4) . . ? H1A B1 H1B 108(5) . . ? C6 C1 C2 118.7(5) . . ? C6 C1 P1 123.1(4) . . ? C2 C1 P1 118.1(4) . . ? C3 C2 C1 120.6(5) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 120.0(5) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.2(5) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 119.9(5) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 120.6(5) . . ? C1 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C8 C7 C12 118.1(5) . . ? C8 C7 P1 119.7(4) . . ? C12 C7 P1 122.2(4) . . ? C7 C8 C9 120.6(5) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 120.4(5) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 119.4(5) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 120.4(5) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C7 121.1(5) . . ? C11 C12 H12 119.5 . . ? C7 C12 H12 119.5 . . ? C18 C13 C14 118.7(5) . . ? C18 C13 P1 121.0(4) . . ? C14 C13 P1 120.2(4) . . ? C15 C14 C13 120.5(5) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 120.2(5) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.1(5) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 120.0(6) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.5(5) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? C24 C19 C20 118.7(4) . . ? C24 C19 P2 125.1(4) . . ? C20 C19 P2 116.0(4) . . ? C21 C20 C19 120.5(5) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 120.4(5) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 119.4(5) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 121.3(5) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C23 C24 C19 119.6(5) . . ? C23 C24 H24 120.2 . . ? C19 C24 H24 120.2 . . ? C26 C25 C30 119.1(5) . . ? C26 C25 P2 119.7(4) . . ? C30 C25 P2 121.2(4) . . ? C27 C26 C25 119.8(5) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 120.4(5) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 120.0(5) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.1(5) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C25 120.5(5) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? C046 C31 C32 118.2(4) . . ? C046 C31 P2 118.3(4) . . ? C32 C31 P2 123.5(4) . . ? C090 C32 C31 121.0(5) . . ? C090 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C38 C37 C42 118.4(4) . . ? C38 C37 P3 117.8(3) . . ? C42 C37 P3 123.7(4) . . ? C39 C38 C37 120.7(5) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C40 C39 C38 120.5(5) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C41 C40 C39 119.2(5) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C40 C41 C42 120.5(5) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C41 C42 C37 120.5(5) . . ? C41 C42 H42 119.7 . . ? C37 C42 H42 119.7 . . ? C44 C43 C48 119.4(4) . . ? C44 C43 P3 122.9(4) . . ? C48 C43 P3 117.6(4) . . ? C43 C44 C45 119.8(5) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C46 C45 C44 120.1(6) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C055 C046 C31 120.7(5) . . ? C055 C046 H046 119.6 . . ? C31 C046 H046 119.6 . . ? C45 C46 C47 120.9(5) . . ? C45 C46 H46 119.6 . . ? C47 C46 H46 119.6 . . ? C48 C47 C46 119.6(6) . . ? C48 C47 H47 120.2 . . ? C46 C47 H47 120.2 . . ? C47 C48 C43 120.3(5) . . ? C47 C48 H48 119.9 . . ? C43 C48 H48 119.9 . . ? C50 C49 C54 119.4(5) . . ? C50 C49 P4 117.9(4) . . ? C54 C49 P4 122.6(4) . . ? C49 C50 C51 120.5(5) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C52 C51 C50 119.7(6) . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? C53 C52 C51 120.1(6) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 120.5(5) . . ? C52 C53 H53 119.7 . . ? C54 C53 H53 119.7 . . ? C53 C54 C49 119.8(5) . . ? C53 C54 H54 120.1 . . ? C49 C54 H54 120.1 . . ? C062 C055 C046 119.8(5) . . ? C062 C055 H055 120.1 . . ? C046 C055 H055 120.1 . . ? C56 C55 C60 119.4(5) . . ? C56 C55 P4 118.8(4) . . ? C60 C55 P4 121.7(4) . . ? C55 C56 C57 120.1(5) . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C58 C57 C56 119.7(5) . . ? C58 C57 H57 120.2 . . ? C56 C57 H57 120.2 . . ? C59 C58 C57 120.4(5) . . ? C59 C58 H58 119.8 . . ? C57 C58 H58 119.8 . . ? C58 C59 C60 120.5(5) . . ? C58 C59 H59 119.7 . . ? C60 C59 H59 119.7 . . ? C59 C60 C55 119.9(5) . . ? C59 C60 H60 120.1 . . ? C55 C60 H60 120.1 . . ? C62 C61 C66 120.4(5) . . ? C62 C61 P4 121.1(4) . . ? C66 C61 P4 118.5(4) . . ? C090 C062 C055 120.1(5) . . ? C090 C062 H062 119.9 . . ? C055 C062 H062 119.9 . . ? C61 C62 C63 119.2(6) . . ? C61 C62 H62 120.4 . . ? C63 C62 H62 120.4 . . ? C64 C63 C62 120.2(7) . . ? C64 C63 H63 119.9 . . ? C62 C63 H63 119.9 . . ? C63 C64 C65 120.5(6) . . ? C63 C64 H64 119.8 . . ? C65 C64 H64 119.8 . . ? C64 C65 C66 119.9(7) . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C65 C66 C61 119.9(6) . . ? C65 C66 H66 120.1 . . ? C61 C66 H66 120.1 . . ? C062 C090 C32 120.2(5) . . ? C062 C090 H090 119.9 . . ? C32 C090 H090 119.9 . . ? C13 P1 C7 101.6(2) . . ? C13 P1 C1 102.8(2) . . ? C7 P1 C1 104.0(2) . . ? C13 P1 Rh1 122.67(15) . . ? C7 P1 Rh1 113.90(16) . . ? C1 P1 Rh1 109.89(16) . . ? C19 P2 C25 106.9(2) . . ? C19 P2 C31 101.4(2) . . ? C25 P2 C31 99.4(2) . . ? C19 P2 Rh1 112.59(14) . . ? C25 P2 Rh1 117.36(16) . . ? C31 P2 Rh1 117.19(15) . . ? C37 P3 C43 110.1(2) . . ? C37 P3 B1 112.1(2) . . ? C43 P3 B1 115.9(2) . . ? C37 P3 Rh1 121.36(15) . . ? C43 P3 Rh1 120.88(16) . . ? B1 P3 Rh1 70.28(15) . . ? C61 P4 C49 106.7(2) . . ? C61 P4 C55 107.6(2) . . ? C49 P4 C55 107.4(2) . . ? C61 P4 B1 106.5(2) . . ? C49 P4 B1 109.2(2) . . ? C55 P4 B1 118.8(2) . . ? C201 B100 C217 110.9(4) . . ? C201 B100 C209 112.4(4) . . ? C217 B100 C209 102.7(4) . . ? C201 B100 C225 105.4(4) . . ? C217 B100 C225 113.5(4) . . ? C209 B100 C225 112.2(4) . . ? C206 C201 C202 115.9(4) . . ? C206 C201 B100 121.7(4) . . ? C202 C201 B100 122.3(4) . . ? C203 C202 C201 121.7(4) . . ? C203 C202 H202 119.2 . . ? C201 C202 H202 119.2 . . ? C204 C203 C202 121.1(4) . . ? C204 C203 C207 120.2(4) . . ? C202 C203 C207 118.7(4) . . ? F103 C207 F3 127.3(7) . . ? F103 C207 F1 66.1(6) . . ? F3 C207 F1 107.0(6) . . ? F103 C207 F101 107.7(6) . . ? F3 C207 F101 35.1(5) . . ? F1 C207 F101 130.3(6) . . ? F103 C207 F102 107.0(5) . . ? F3 C207 F102 68.6(6) . . ? F1 C207 F102 44.5(5) . . ? F101 C207 F102 102.0(5) . . ? F103 C207 F2 40.0(6) . . ? F3 C207 F2 103.1(5) . . ? F1 C207 F2 103.2(5) . . ? F101 C207 F2 72.4(5) . . ? F102 C207 F2 133.1(6) . . ? F103 C207 C203 114.6(5) . . ? F3 C207 C203 115.1(5) . . ? F1 C207 C203 114.4(5) . . ? F101 C207 C203 112.5(4) . . ? F102 C207 C203 112.1(4) . . ? F2 C207 C203 112.8(4) . . ? C203 C204 C205 118.0(5) . . ? C203 C204 H204 121.0 . . ? C205 C204 H204 121.0 . . ? C204 C205 C206 121.2(5) . . ? C204 C205 C208 118.7(4) . . ? C206 C205 C208 120.1(4) . . ? C204 C205 C308 120.6(5) . . ? C206 C205 C308 118.2(5) . . ? C208 C205 C308 2.3(3) . . ? F5 C208 F6 107.1(6) . . ? F5 C208 F4 104.2(6) . . ? F6 C208 F4 103.5(6) . . ? F5 C208 C205 115.7(5) . . ? F6 C208 C205 113.2(6) . . ? F4 C208 C205 112.1(6) . . ? F105 C308 F104 106.1(6) . . ? F105 C308 F106 105.7(6) . . ? F104 C308 F106 103.6(7) . . ? F105 C308 C205 114.8(6) . . ? F104 C308 C205 112.3(6) . . ? F106 C308 C205 113.4(6) . . ? C205 C206 C201 122.0(4) . . ? C205 C206 H206 119.0 . . ? C201 C206 H206 119.0 . . ? C214 C209 C210 115.9(4) . . ? C214 C209 B100 122.7(4) . . ? C210 C209 B100 120.9(4) . . ? C211 C210 C209 122.2(4) . . ? C211 C210 H210 118.9 . . ? C209 C210 H210 118.9 . . ? C210 C211 C212 120.7(5) . . ? C210 C211 C215 119.4(4) . . ? C212 C211 C215 119.9(4) . . ? C210 C211 C315 120.6(4) . . ? C212 C211 C315 118.6(4) . . ? C215 C211 C315 1.5(3) . . ? F8 C215 F9 107.6(7) . . ? F8 C215 F7 105.4(6) . . ? F9 C215 F7 104.8(6) . . ? F8 C215 C211 114.4(6) . . ? F9 C215 C211 113.4(6) . . ? F7 C215 C211 110.4(6) . . ? F108 C315 F109 107.1(5) . . ? F108 C315 F107 107.0(6) . . ? F109 C315 F107 104.7(5) . . ? F108 C315 C211 113.8(5) . . ? F109 C315 C211 112.0(5) . . ? F107 C315 C211 111.6(5) . . ? C213 C212 C211 118.0(5) . . ? C213 C212 H212 121.0 . . ? C211 C212 H212 121.0 . . ? C212 C213 C214 121.2(5) . . ? C212 C213 C216 120.6(4) . . ? C214 C213 C216 118.2(4) . . ? F112 C216 F110 107.4(6) . . ? F112 C216 F12 123.9(8) . . ? F110 C216 F12 23.8(7) . . ? F112 C216 F10 81.4(7) . . ? F110 C216 F10 124.3(8) . . ? F12 C216 F10 106.5(6) . . ? F112 C216 F11 26.6(8) . . ? F110 C216 F11 84.7(8) . . ? F12 C216 F11 105.7(6) . . ? F10 C216 F11 105.8(6) . . ? F112 C216 F111 105.7(6) . . ? F110 C216 F111 104.9(6) . . ? F12 C216 F111 83.2(7) . . ? F10 C216 F111 27.0(6) . . ? F11 C216 F111 126.4(8) . . ? F112 C216 C213 113.7(5) . . ? F110 C216 C213 112.8(5) . . ? F12 C216 C213 113.4(5) . . ? F10 C216 C213 112.7(5) . . ? F11 C216 C213 112.2(6) . . ? F111 C216 C213 111.7(5) . . ? C209 C214 C213 121.9(5) . . ? C209 C214 H214 119.0 . . ? C213 C214 H214 119.0 . . ? C222 C217 C218 115.9(4) . . ? C222 C217 B100 123.8(4) . . ? C218 C217 B100 119.9(4) . . ? C219 C218 C217 122.5(5) . . ? C219 C218 H218 118.7 . . ? C217 C218 H218 118.7 . . ? C220 C219 C218 120.6(5) . . ? C220 C219 C223 119.2(5) . . ? C218 C219 C223 120.2(5) . . ? C219 C220 C221 118.3(5) . . ? C219 C220 H220 120.9 . . ? C221 C220 H220 120.9 . . ? C220 C221 C222 120.7(5) . . ? C220 C221 C224 118.9(4) . . ? C222 C221 C224 120.3(4) . . ? C220 C221 C324 119.4(5) . . ? C222 C221 C324 119.8(5) . . ? C224 C221 C324 2.8(3) . . ? F18 C224 F17 108.4(6) . . ? F18 C224 F16 102.0(5) . . ? F17 C224 F16 103.2(6) . . ? F18 C224 C221 114.7(5) . . ? F17 C224 C221 115.6(5) . . ? F16 C224 C221 111.5(5) . . ? F117 C324 F118 106.7(6) . . ? F117 C324 F116 104.2(6) . . ? F118 C324 F116 103.3(6) . . ? F117 C324 C221 114.9(6) . . ? F118 C324 C221 114.4(6) . . ? F116 C324 C221 112.2(6) . . ? C217 C222 C221 122.0(5) . . ? C217 C222 H222 119.0 . . ? C221 C222 H222 119.0 . . ? F13 C223 F15 105.8(5) . . ? F13 C223 F14 108.2(6) . . ? F15 C223 F14 105.5(5) . . ? F13 C223 C219 112.5(5) . . ? F15 C223 C219 112.5(6) . . ? F14 C223 C219 111.8(5) . . ? C226 C225 C230 115.9(4) . . ? C226 C225 B100 121.7(4) . . ? C230 C225 B100 122.2(4) . . ? C227 C226 C225 122.1(5) . . ? C227 C226 H226 119.0 . . ? C225 C226 H226 119.0 . . ? C228 C227 C226 121.1(5) . . ? C228 C227 C231 120.4(4) . . ? C226 C227 C231 118.6(4) . . ? C228 C227 C331 119.4(5) . . ? C226 C227 C331 119.5(5) . . ? C231 C227 C331 2.8(3) . . ? C229 C228 C227 118.0(5) . . ? C229 C228 H228 121.0 . . ? C227 C228 H228 121.0 . . ? C228 C229 C230 121.1(5) . . ? C228 C229 C232 120.8(5) . . ? C230 C229 C232 118.1(4) . . ? C229 C230 C225 121.8(4) . . ? C229 C230 H230 119.1 . . ? C225 C230 H230 119.1 . . ? F21 C231 F20 110.2(5) . . ? F21 C231 F19 103.2(5) . . ? F20 C231 F19 102.0(5) . . ? F21 C231 C227 114.6(5) . . ? F20 C231 C227 114.2(4) . . ? F19 C231 C227 111.3(4) . . ? F119 C331 F120 104.3(7) . . ? F119 C331 F121 105.5(7) . . ? F120 C331 F121 106.0(7) . . ? F119 C331 C227 111.6(6) . . ? F120 C331 C227 113.8(7) . . ? F121 C331 C227 114.8(7) . . ? F22 C232 F24 106.7(5) . . ? F22 C232 F23 105.8(5) . . ? F24 C232 F23 105.6(5) . . ? F22 C232 C229 112.9(5) . . ? F24 C232 C229 112.7(4) . . ? F23 C232 C229 112.5(5) . . ? Cl1 C500 Cl3 119.5(13) . . ? Cl1 C500 H50A 107.5 . . ? Cl3 C500 H50A 107.5 . . ? Cl1 C500 H50B 107.5 . . ? Cl3 C500 H50B 107.5 . . ? H50A C500 H50B 107.0 . . ? Cl3 C005 Cl01 103.8(13) . . ? Cl3 C005 H00A 111.0 . . ? Cl01 C005 H00A 111.0 . . ? Cl3 C005 H00B 111.0 . . ? Cl01 C005 H00B 111.0 . . ? H00A C005 H00B 109.0 . . ? C005 Cl3 C500 56.5(17) . . ? 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 P2 Rh1 B1 P3 -22.4(3) . . . . ? P1 Rh1 B1 P3 177.57(7) . . . . ? P2 Rh1 B1 P4 -127.9(4) . . . . ? P3 Rh1 B1 P4 -105.5(4) . . . . ? P1 Rh1 B1 P4 72.1(4) . . . . ? C6 C1 C2 C3 -0.1(8) . . . . ? P1 C1 C2 C3 -178.7(4) . . . . ? C1 C2 C3 C4 0.5(8) . . . . ? C2 C3 C4 C5 -1.1(9) . . . . ? C3 C4 C5 C6 1.3(9) . . . . ? C2 C1 C6 C5 0.3(8) . . . . ? P1 C1 C6 C5 178.8(5) . . . . ? C4 C5 C6 C1 -0.9(9) . . . . ? C12 C7 C8 C9 2.0(8) . . . . ? P1 C7 C8 C9 -179.3(4) . . . . ? C7 C8 C9 C10 -1.5(9) . . . . ? C8 C9 C10 C11 0.3(9) . . . . ? C9 C10 C11 C12 0.2(10) . . . . ? C10 C11 C12 C7 0.3(11) . . . . ? C8 C7 C12 C11 -1.4(9) . . . . ? P1 C7 C12 C11 179.9(5) . . . . ? C18 C13 C14 C15 -0.1(8) . . . . ? P1 C13 C14 C15 176.3(4) . . . . ? C13 C14 C15 C16 -0.1(9) . . . . ? C14 C15 C16 C17 -0.1(10) . . . . ? C15 C16 C17 C18 0.5(10) . . . . ? C16 C17 C18 C13 -0.7(9) . . . . ? C14 C13 C18 C17 0.5(8) . . . . ? P1 C13 C18 C17 -175.9(4) . . . . ? C24 C19 C20 C21 -2.4(7) . . . . ? P2 C19 C20 C21 174.1(4) . . . . ? C19 C20 C21 C22 2.3(8) . . . . ? C20 C21 C22 C23 -0.4(8) . . . . ? C21 C22 C23 C24 -1.2(9) . . . . ? C22 C23 C24 C19 1.0(9) . . . . ? C20 C19 C24 C23 0.8(7) . . . . ? P2 C19 C24 C23 -175.4(4) . . . . ? C30 C25 C26 C27 -2.9(8) . . . . ? P2 C25 C26 C27 179.4(4) . . . . ? C25 C26 C27 C28 0.9(9) . . . . ? C26 C27 C28 C29 1.3(10) . . . . ? C27 C28 C29 C30 -1.4(9) . . . . ? C28 C29 C30 C25 -0.7(9) . . . . ? C26 C25 C30 C29 2.9(8) . . . . ? P2 C25 C30 C29 -179.5(4) . . . . ? C046 C31 C32 C090 0.1(8) . . . . ? P2 C31 C32 C090 -179.4(4) . . . . ? C42 C37 C38 C39 0.4(8) . . . . ? P3 C37 C38 C39 -177.8(4) . . . . ? C37 C38 C39 C40 -0.7(9) . . . . ? C38 C39 C40 C41 0.6(9) . . . . ? C39 C40 C41 C42 -0.2(10) . . . . ? C40 C41 C42 C37 -0.1(9) . . . . ? C38 C37 C42 C41 0.0(8) . . . . ? P3 C37 C42 C41 178.1(4) . . . . ? C48 C43 C44 C45 -0.8(7) . . . . ? P3 C43 C44 C45 175.0(4) . . . . ? C43 C44 C45 C46 0.7(9) . . . . ? C32 C31 C046 C055 1.6(7) . . . . ? P2 C31 C046 C055 -178.9(4) . . . . ? C44 C45 C46 C47 0.0(9) . . . . ? C45 C46 C47 C48 -0.7(9) . . . . ? C46 C47 C48 C43 0.5(8) . . . . ? C44 C43 C48 C47 0.2(7) . . . . ? P3 C43 C48 C47 -175.9(4) . . . . ? C54 C49 C50 C51 0.8(8) . . . . ? P4 C49 C50 C51 -176.7(5) . . . . ? C49 C50 C51 C52 1.0(10) . . . . ? C50 C51 C52 C53 -2.3(11) . . . . ? C51 C52 C53 C54 1.8(10) . . . . ? C52 C53 C54 C49 0.1(9) . . . . ? C50 C49 C54 C53 -1.4(8) . . . . ? P4 C49 C54 C53 176.0(4) . . . . ? C31 C046 C055 C062 -1.9(8) . . . . ? C60 C55 C56 C57 -1.2(9) . . . . ? P4 C55 C56 C57 177.2(5) . . . . ? C55 C56 C57 C58 1.6(10) . . . . ? C56 C57 C58 C59 -1.1(10) . . . . ? C57 C58 C59 C60 0.4(10) . . . . ? C58 C59 C60 C55 0.0(9) . . . . ? C56 C55 C60 C59 0.4(8) . . . . ? P4 C55 C60 C59 -177.9(4) . . . . ? C046 C055 C062 C090 0.5(8) . . . . ? C66 C61 C62 C63 0.0(9) . . . . ? P4 C61 C62 C63 177.1(5) . . . . ? C61 C62 C63 C64 0.7(10) . . . . ? C62 C63 C64 C65 -0.5(11) . . . . ? C63 C64 C65 C66 -0.3(10) . . . . ? C64 C65 C66 C61 1.1(10) . . . . ? C62 C61 C66 C65 -0.9(9) . . . . ? P4 C61 C66 C65 -178.0(5) . . . . ? C055 C062 C090 C32 1.2(9) . . . . ? C31 C32 C090 C062 -1.5(9) . . . . ? C18 C13 P1 C7 -147.6(4) . . . . ? C14 C13 P1 C7 36.0(5) . . . . ? C18 C13 P1 C1 -40.2(4) . . . . ? C14 C13 P1 C1 143.4(4) . . . . ? C18 C13 P1 Rh1 83.9(4) . . . . ? C14 C13 P1 Rh1 -92.5(4) . . . . ? C8 C7 P1 C13 -129.8(4) . . . . ? C12 C7 P1 C13 48.9(5) . . . . ? C8 C7 P1 C1 123.7(4) . . . . ? C12 C7 P1 C1 -57.6(5) . . . . ? C8 C7 P1 Rh1 4.1(5) . . . . ? C12 C7 P1 Rh1 -177.2(4) . . . . ? C6 C1 P1 C13 -36.4(5) . . . . ? C2 C1 P1 C13 142.1(4) . . . . ? C6 C1 P1 C7 69.2(5) . . . . ? C2 C1 P1 C7 -112.3(4) . . . . ? C6 C1 P1 Rh1 -168.5(4) . . . . ? C2 C1 P1 Rh1 10.0(4) . . . . ? P2 Rh1 P1 C13 -6.2(2) . . . . ? P3 Rh1 P1 C13 168.4(2) . . . . ? B1 Rh1 P1 C13 162.3(2) . . . . ? P2 Rh1 P1 C7 -129.22(17) . . . . ? P3 Rh1 P1 C7 45.4(2) . . . . ? B1 Rh1 P1 C7 39.3(2) . . . . ? P2 Rh1 P1 C1 114.57(17) . . . . ? P3 Rh1 P1 C1 -70.8(2) . . . . ? B1 Rh1 P1 C1 -76.9(2) . . . . ? C24 C19 P2 C25 -9.1(5) . . . . ? C20 C19 P2 C25 174.7(3) . . . . ? C24 C19 P2 C31 94.6(4) . . . . ? C20 C19 P2 C31 -81.7(4) . . . . ? C24 C19 P2 Rh1 -139.4(4) . . . . ? C20 C19 P2 Rh1 44.4(4) . . . . ? C26 C25 P2 C19 -122.3(4) . . . . ? C30 C25 P2 C19 60.1(4) . . . . ? C26 C25 P2 C31 132.6(4) . . . . ? C30 C25 P2 C31 -45.0(4) . . . . ? C26 C25 P2 Rh1 5.2(4) . . . . ? C30 C25 P2 Rh1 -172.4(3) . . . . ? C046 C31 P2 C19 -163.6(4) . . . . ? C32 C31 P2 C19 15.9(5) . . . . ? C046 C31 P2 C25 -54.1(4) . . . . ? C32 C31 P2 C25 125.4(4) . . . . ? C046 C31 P2 Rh1 73.4(4) . . . . ? C32 C31 P2 Rh1 -107.1(4) . . . . ? P3 Rh1 P2 C19 -122.47(17) . . . . ? P1 Rh1 P2 C19 55.91(17) . . . . ? B1 Rh1 P2 C19 -105.7(3) . . . . ? P3 Rh1 P2 C25 112.76(17) . . . . ? P1 Rh1 P2 C25 -68.86(17) . . . . ? B1 Rh1 P2 C25 129.5(3) . . . . ? P3 Rh1 P2 C31 -5.46(18) . . . . ? P1 Rh1 P2 C31 172.92(17) . . . . ? B1 Rh1 P2 C31 11.3(3) . . . . ? C38 C37 P3 C43 -169.2(4) . . . . ? C42 C37 P3 C43 12.8(5) . . . . ? C38 C37 P3 B1 -38.6(4) . . . . ? C42 C37 P3 B1 143.3(4) . . . . ? C38 C37 P3 Rh1 41.1(4) . . . . ? C42 C37 P3 Rh1 -137.0(4) . . . . ? C44 C43 P3 C37 42.8(5) . . . . ? C48 C43 P3 C37 -141.2(4) . . . . ? C44 C43 P3 B1 -85.7(4) . . . . ? C48 C43 P3 B1 90.2(4) . . . . ? C44 C43 P3 Rh1 -167.3(3) . . . . ? C48 C43 P3 Rh1 8.7(4) . . . . ? P4 B1 P3 C37 -104.8(3) . . . . ? Rh1 B1 P3 C37 116.81(18) . . . . ? P4 B1 P3 C43 22.7(4) . . . . ? Rh1 B1 P3 C43 -115.6(2) . . . . ? P4 B1 P3 Rh1 138.3(3) . . . . ? P2 Rh1 P3 C37 62.70(17) . . . . ? P1 Rh1 P3 C37 -111.9(2) . . . . ? B1 Rh1 P3 C37 -104.5(2) . . . . ? P2 Rh1 P3 C43 -83.84(17) . . . . ? P1 Rh1 P3 C43 101.5(2) . . . . ? B1 Rh1 P3 C43 109.0(2) . . . . ? P2 Rh1 P3 B1 167.16(17) . . . . ? P1 Rh1 P3 B1 -7.5(2) . . . . ? C62 C61 P4 C49 -9.8(5) . . . . ? C66 C61 P4 C49 167.3(4) . . . . ? C62 C61 P4 C55 105.2(5) . . . . ? C66 C61 P4 C55 -77.7(5) . . . . ? C62 C61 P4 B1 -126.4(5) . . . . ? C66 C61 P4 B1 50.7(5) . . . . ? C50 C49 P4 C61 -76.2(5) . . . . ? C54 C49 P4 C61 106.3(4) . . . . ? C50 C49 P4 C55 168.6(4) . . . . ? C54 C49 P4 C55 -8.8(5) . . . . ? C50 C49 P4 B1 38.5(5) . . . . ? C54 C49 P4 B1 -138.9(4) . . . . ? C56 C55 P4 C61 -175.7(4) . . . . ? C60 C55 P4 C61 2.6(5) . . . . ? C56 C55 P4 C49 -61.2(5) . . . . ? C60 C55 P4 C49 117.2(4) . . . . ? C56 C55 P4 B1 63.3(5) . . . . ? C60 C55 P4 B1 -118.4(4) . . . . ? P3 B1 P4 C61 157.2(3) . . . . ? Rh1 B1 P4 C61 -119.1(4) . . . . ? P3 B1 P4 C49 42.3(4) . . . . ? Rh1 B1 P4 C49 126.1(4) . . . . ? P3 B1 P4 C55 -81.2(4) . . . . ? Rh1 B1 P4 C55 2.5(5) . . . . ? C217 B100 C201 C206 -32.1(6) . . . . ? C209 B100 C201 C206 -146.4(5) . . . . ? C225 B100 C201 C206 91.1(5) . . . . ? C217 B100 C201 C202 151.5(4) . . . . ? C209 B100 C201 C202 37.2(6) . . . . ? C225 B100 C201 C202 -85.3(5) . . . . ? C206 C201 C202 C203 2.1(7) . . . . ? B100 C201 C202 C203 178.7(4) . . . . ? C201 C202 C203 C204 -0.4(8) . . . . ? C201 C202 C203 C207 179.2(4) . . . . ? C204 C203 C207 F103 -107.5(8) . . . . ? C202 C203 C207 F103 72.8(9) . . . . ? C204 C203 C207 F3 90.7(8) . . . . ? C202 C203 C207 F3 -89.0(8) . . . . ? C204 C203 C207 F1 -33.9(9) . . . . ? C202 C203 C207 F1 146.4(8) . . . . ? C204 C203 C207 F101 129.0(7) . . . . ? C202 C203 C207 F101 -50.6(7) . . . . ? C204 C203 C207 F102 14.8(8) . . . . ? C202 C203 C207 F102 -164.9(6) . . . . ? C204 C203 C207 F2 -151.4(7) . . . . ? C202 C203 C207 F2 29.0(7) . . . . ? C202 C203 C204 C205 -1.6(8) . . . . ? C207 C203 C204 C205 178.8(5) . . . . ? C203 C204 C205 C206 1.8(9) . . . . ? C203 C204 C205 C208 -179.9(5) . . . . ? C203 C204 C205 C308 -178.4(5) . . . . ? C204 C205 C208 F5 168.3(8) . . . . ? C206 C205 C208 F5 -13.3(9) . . . . ? C308 C205 C208 F5 23(8) . . . . ? C204 C205 C208 F6 44.2(9) . . . . ? C206 C205 C208 F6 -137.5(8) . . . . ? C308 C205 C208 F6 -101(8) . . . . ? C204 C205 C208 F4 -72.4(8) . . . . ? C206 C205 C208 F4 105.9(8) . . . . ? C308 C205 C208 F4 142(8) . . . . ? C204 C205 C308 F105 -1.8(9) . . . . ? C206 C205 C308 F105 178.0(7) . . . . ? C208 C205 C308 F105 33(7) . . . . ? C204 C205 C308 F104 119.5(8) . . . . ? C206 C205 C308 F104 -60.7(9) . . . . ? C208 C205 C308 F104 155(8) . . . . ? C204 C205 C308 F106 -123.5(8) . . . . ? C206 C205 C308 F106 56.3(9) . . . . ? C208 C205 C308 F106 -88(8) . . . . ? C204 C205 C206 C201 0.0(9) . . . . ? C208 C205 C206 C201 -178.3(5) . . . . ? C308 C205 C206 C201 -179.8(5) . . . . ? C202 C201 C206 C205 -2.0(8) . . . . ? B100 C201 C206 C205 -178.6(5) . . . . ? C201 B100 C209 C214 30.3(6) . . . . ? C217 B100 C209 C214 -88.9(5) . . . . ? C225 B100 C209 C214 148.9(4) . . . . ? C201 B100 C209 C210 -157.9(4) . . . . ? C217 B100 C209 C210 82.9(5) . . . . ? C225 B100 C209 C210 -39.3(5) . . . . ? C214 C209 C210 C211 -2.1(7) . . . . ? B100 C209 C210 C211 -174.4(4) . . . . ? C209 C210 C211 C212 1.7(7) . . . . ? C209 C210 C211 C215 179.1(4) . . . . ? C209 C210 C211 C315 178.1(4) . . . . ? C210 C211 C215 F8 163.6(10) . . . . ? C212 C211 C215 F8 -19.0(11) . . . . ? C315 C211 C215 F8 -49(12) . . . . ? C210 C211 C215 F9 -72.3(11) . . . . ? C212 C211 C215 F9 105.0(11) . . . . ? C315 C211 C215 F9 76(12) . . . . ? C210 C211 C215 F7 44.9(10) . . . . ? C212 C211 C215 F7 -137.8(10) . . . . ? C315 C211 C215 F7 -167(13) . . . . ? C210 C211 C315 F108 16.8(9) . . . . ? C212 C211 C315 F108 -166.7(8) . . . . ? C215 C211 C315 F108 -16(12) . . . . ? C210 C211 C315 F109 138.5(7) . . . . ? C212 C211 C315 F109 -45.0(8) . . . . ? C215 C211 C315 F109 106(12) . . . . ? C210 C211 C315 F107 -104.5(7) . . . . ? C212 C211 C315 F107 72.0(8) . . . . ? C215 C211 C315 F107 -137(13) . . . . ? C210 C211 C212 C213 0.1(7) . . . . ? C215 C211 C212 C213 -177.2(5) . . . . ? C315 C211 C212 C213 -176.4(5) . . . . ? C211 C212 C213 C214 -1.4(7) . . . . ? C211 C212 C213 C216 -179.9(4) . . . . ? C212 C213 C216 F112 0.6(11) . . . . ? C214 C213 C216 F112 -178.0(10) . . . . ? C212 C213 C216 F110 -122.0(11) . . . . ? C214 C213 C216 F110 59.4(12) . . . . ? C212 C213 C216 F12 -148.0(10) . . . . ? C214 C213 C216 F12 33.5(11) . . . . ? C212 C213 C216 F10 90.9(11) . . . . ? C214 C213 C216 F10 -87.6(11) . . . . ? C212 C213 C216 F11 -28.4(12) . . . . ? C214 C213 C216 F11 153.1(12) . . . . ? C212 C213 C216 F111 120.1(11) . . . . ? C214 C213 C216 F111 -58.5(11) . . . . ? C210 C209 C214 C213 0.7(7) . . . . ? B100 C209 C214 C213 172.9(4) . . . . ? C212 C213 C214 C209 1.0(7) . . . . ? C216 C213 C214 C209 179.5(4) . . . . ? C201 B100 C217 C222 147.2(5) . . . . ? C209 B100 C217 C222 -92.6(5) . . . . ? C225 B100 C217 C222 28.8(6) . . . . ? C201 B100 C217 C218 -41.3(6) . . . . ? C209 B100 C217 C218 79.0(5) . . . . ? C225 B100 C217 C218 -159.6(4) . . . . ? C222 C217 C218 C219 -0.5(8) . . . . ? B100 C217 C218 C219 -172.7(5) . . . . ? C217 C218 C219 C220 0.2(9) . . . . ? C217 C218 C219 C223 -177.9(5) . . . . ? C218 C219 C220 C221 -0.2(9) . . . . ? C223 C219 C220 C221 177.9(6) . . . . ? C219 C220 C221 C222 0.4(8) . . . . ? C219 C220 C221 C224 179.1(5) . . . . ? C219 C220 C221 C324 -177.7(5) . . . . ? C220 C221 C224 F18 40.2(8) . . . . ? C222 C221 C224 F18 -141.1(7) . . . . ? C324 C221 C224 F18 -61(6) . . . . ? C220 C221 C224 F17 167.5(7) . . . . ? C222 C221 C224 F17 -13.8(8) . . . . ? C324 C221 C224 F17 66(6) . . . . ? C220 C221 C224 F16 -75.1(7) . . . . ? C222 C221 C224 F16 103.6(7) . . . . ? C324 C221 C224 F16 -176(6) . . . . ? C220 C221 C324 F117 -26.9(9) . . . . ? C222 C221 C324 F117 154.9(8) . . . . ? C224 C221 C324 F117 54(6) . . . . ? C220 C221 C324 F118 -150.9(8) . . . . ? C222 C221 C324 F118 31.0(9) . . . . ? C224 C221 C324 F118 -70(6) . . . . ? C220 C221 C324 F116 91.9(8) . . . . ? C222 C221 C324 F116 -86.3(8) . . . . ? C224 C221 C324 F116 172(7) . . . . ? C218 C217 C222 C221 0.7(7) . . . . ? B100 C217 C222 C221 172.6(5) . . . . ? C220 C221 C222 C217 -0.7(8) . . . . ? C224 C221 C222 C217 -179.4(5) . . . . ? C324 C221 C222 C217 177.4(5) . . . . ? C220 C219 C223 F13 160.7(6) . . . . ? C218 C219 C223 F13 -21.2(9) . . . . ? C220 C219 C223 F15 41.3(8) . . . . ? C218 C219 C223 F15 -140.6(6) . . . . ? C220 C219 C223 F14 -77.3(7) . . . . ? C218 C219 C223 F14 100.8(6) . . . . ? C201 B100 C225 C226 -83.5(5) . . . . ? C217 B100 C225 C226 38.0(6) . . . . ? C209 B100 C225 C226 153.9(4) . . . . ? C201 B100 C225 C230 91.5(5) . . . . ? C217 B100 C225 C230 -147.0(4) . . . . ? C209 B100 C225 C230 -31.1(5) . . . . ? C230 C225 C226 C227 2.0(7) . . . . ? B100 C225 C226 C227 177.2(4) . . . . ? C225 C226 C227 C228 -1.1(8) . . . . ? C225 C226 C227 C231 177.3(4) . . . . ? C225 C226 C227 C331 -179.7(5) . . . . ? C226 C227 C228 C229 0.1(8) . . . . ? C231 C227 C228 C229 -178.3(4) . . . . ? C331 C227 C228 C229 178.6(5) . . . . ? C227 C228 C229 C230 0.0(7) . . . . ? C227 C228 C229 C232 180.0(5) . . . . ? C228 C229 C230 C225 1.0(7) . . . . ? C232 C229 C230 C225 -179.0(4) . . . . ? C226 C225 C230 C229 -1.9(6) . . . . ? B100 C225 C230 C229 -177.1(4) . . . . ? C228 C227 C231 F21 -6.1(8) . . . . ? C226 C227 C231 F21 175.5(6) . . . . ? C331 C227 C231 F21 66(6) . . . . ? C228 C227 C231 F20 -134.6(6) . . . . ? C226 C227 C231 F20 47.0(7) . . . . ? C331 C227 C231 F20 -63(6) . . . . ? C228 C227 C231 F19 110.5(6) . . . . ? C226 C227 C231 F19 -67.9(6) . . . . ? C331 C227 C231 F19 -178(100) . . . . ? C228 C227 C331 F119 -83.9(10) . . . . ? C226 C227 C331 F119 94.7(10) . . . . ? C231 C227 C331 F119 166(7) . . . . ? C228 C227 C331 F120 33.8(11) . . . . ? C226 C227 C331 F120 -147.6(9) . . . . ? C231 C227 C331 F120 -76(6) . . . . ? C228 C227 C331 F121 156.2(10) . . . . ? C226 C227 C331 F121 -25.2(11) . . . . ? C231 C227 C331 F121 46(6) . . . . ? C228 C229 C232 F22 107.9(6) . . . . ? C230 C229 C232 F22 -72.1(7) . . . . ? C228 C229 C232 F24 -131.1(5) . . . . ? C230 C229 C232 F24 48.9(7) . . . . ? C228 C229 C232 F23 -11.9(7) . . . . ? C230 C229 C232 F23 168.1(5) . . . . ? Cl01 C005 Cl3 C500 76.5(19) . . . . ? Cl1 C500 Cl3 C005 -88(2) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 74.46 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.743 _refine_diff_density_min -1.498 _refine_diff_density_rms 0.108 _database_code_depnum_ccdc_archive 'CCDC 926700' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_7 #---------------------- # [Rh(PiBu3)2(PPh3)][BArF4] #---------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic . _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety 'C42 H69 P3 Rh, C32 H12 B F24' _chemical_formula_sum 'C74 H81 B F24 P3 Rh' _chemical_formula_weight 1633.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 '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' F F 0.0171 0.0103 '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' Rh Rh -1.1178 0.9187 '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 monoclinic _symmetry_space_group_name_H-M P21/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 16.33210(10) _cell_length_b 25.1406(2) _cell_length_c 18.8993(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.56 _cell_angle_gamma 90.00 _cell_volume 7735.48(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17803 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 0.381 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.958 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 30821 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_unetI/netI 0.0626 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 26.37 _reflns_number_total 15712 _reflns_number_gt 10746 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'Bruker SHELXTL' _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. Disorder of two of the phosphine ligands was treated by modelling the appropriate phosphine substituents over two sites and restraining their geometry. Rotational disorder of the CF3 groups of the anion was treated by modelling either the fluorine atoms over two sites or the entire CF3 group and restraining their geometry. Restraints to thermal parameters were applied where necessary in order to maintain sensible values. ; _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^)+(0.0560P)^2^+4.6690P] 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 15712 _refine_ls_number_parameters 1315 _refine_ls_number_restraints 2298 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1278 _refine_ls_wR_factor_gt 0.1124 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.309 _refine_ls_shift/su_max 0.001 _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 Rh1 Rh 0.755236(17) 0.440486(12) 0.737783(15) 0.02718(10) Uani 1 1 d . A . P1 P 0.63217(6) 0.48731(4) 0.73080(5) 0.0320(2) Uani 1 1 d D . . P2 P 0.89215(6) 0.41088(5) 0.73461(5) 0.0376(3) Uani 1 1 d D . . P3 P 0.71788(5) 0.37566(4) 0.80698(5) 0.0263(2) Uani 1 1 d . . . C1 C 0.5745(7) 0.5062(6) 0.8072(5) 0.035(2) Uani 0.63(2) 1 d PDU A 1 H10A H 0.5451 0.5399 0.7955 0.042 Uiso 0.63(2) 1 calc PR A 1 H10B H 0.5325 0.4786 0.8134 0.042 Uiso 0.63(2) 1 calc PR A 1 C2 C 0.6256(8) 0.5134(4) 0.8777(5) 0.039(2) Uani 0.63(2) 1 d PDU A 1 H102 H 0.6608 0.4811 0.8859 0.047 Uiso 0.63(2) 1 calc PR A 1 C3 C 0.5687(9) 0.5170(5) 0.9382(5) 0.053(3) Uani 0.63(2) 1 d PDU A 1 H10C H 0.6017 0.5216 0.9834 0.079 Uiso 0.63(2) 1 calc PR A 1 H10D H 0.5364 0.4842 0.9398 0.079 Uiso 0.63(2) 1 calc PR A 1 H10E H 0.5316 0.5474 0.9301 0.079 Uiso 0.63(2) 1 calc PR A 1 C4 C 0.6818(10) 0.5616(4) 0.8778(5) 0.057(3) Uani 0.63(2) 1 d PDU A 1 H10F H 0.7132 0.5645 0.9240 0.086 Uiso 0.63(2) 1 calc PR A 1 H10G H 0.6487 0.5937 0.8689 0.086 Uiso 0.63(2) 1 calc PR A 1 H10H H 0.7197 0.5575 0.8405 0.086 Uiso 0.63(2) 1 calc PR A 1 C101 C 0.5947(12) 0.5121(11) 0.8142(8) 0.038(3) Uani 0.37(2) 1 d PDU A 2 H1A H 0.5716 0.5480 0.8044 0.046 Uiso 0.37(2) 1 calc PR A 2 H1B H 0.5485 0.4889 0.8255 0.046 Uiso 0.37(2) 1 calc PR A 2 C102 C 0.6530(13) 0.5162(8) 0.8812(9) 0.044(3) Uani 0.37(2) 1 d PDU A 2 H2 H 0.6771 0.4801 0.8911 0.052 Uiso 0.37(2) 1 calc PR A 2 C103 C 0.6027(15) 0.5310(10) 0.9435(8) 0.059(5) Uani 0.37(2) 1 d PDU A 2 H3A H 0.6394 0.5342 0.9869 0.089 Uiso 0.37(2) 1 calc PR A 2 H3B H 0.5618 0.5032 0.9499 0.089 Uiso 0.37(2) 1 calc PR A 2 H3C H 0.5748 0.5650 0.9335 0.089 Uiso 0.37(2) 1 calc PR A 2 C104 C 0.7233(14) 0.5545(6) 0.8737(8) 0.054(4) Uani 0.37(2) 1 d PDU A 2 H4A H 0.7584 0.5556 0.9182 0.080 Uiso 0.37(2) 1 calc PR A 2 H4B H 0.7014 0.5901 0.8627 0.080 Uiso 0.37(2) 1 calc PR A 2 H4C H 0.7558 0.5425 0.8352 0.080 Uiso 0.37(2) 1 calc PR A 2 C5 C 0.6538(3) 0.55086(16) 0.6871(2) 0.0391(10) Uani 1 1 d . A 2 H5A H 0.6013 0.5697 0.6751 0.047 Uiso 1 1 calc R A 2 H5B H 0.6878 0.5734 0.7208 0.047 Uiso 1 1 calc R A 2 C6 C 0.6980(3) 0.54382(17) 0.6198(2) 0.0442(11) Uani 1 1 d . A 2 H6 H 0.6631 0.5211 0.5861 0.053 Uiso 1 1 calc R A 2 C7 C 0.7783(3) 0.5155(2) 0.6378(3) 0.0608(14) Uani 1 1 d . A 2 H7A H 0.8070 0.5109 0.5946 0.091 Uiso 1 1 calc R A 2 H7B H 0.7676 0.4805 0.6581 0.091 Uiso 1 1 calc R A 2 H7C H 0.8125 0.5365 0.6723 0.091 Uiso 1 1 calc R A 2 C8 C 0.7107(4) 0.5972(2) 0.5844(3) 0.0718(16) Uani 1 1 d . A 2 H8A H 0.7393 0.5917 0.5413 0.108 Uiso 1 1 calc R A 2 H8B H 0.7437 0.6203 0.6172 0.108 Uiso 1 1 calc R A 2 H8C H 0.6572 0.6138 0.5719 0.108 Uiso 1 1 calc R A 2 C9 C 0.5513(2) 0.45783(17) 0.6699(2) 0.0378(9) Uani 1 1 d . A 2 H9A H 0.5792 0.4389 0.6326 0.045 Uiso 1 1 calc R A 2 H9B H 0.5238 0.4303 0.6970 0.045 Uiso 1 1 calc R A 2 C10 C 0.4831(3) 0.49192(19) 0.6317(2) 0.0461(11) Uani 1 1 d . A 2 H10 H 0.5099 0.5215 0.6068 0.055 Uiso 1 1 calc R A 2 C11 C 0.4253(3) 0.5163(3) 0.6811(3) 0.0752(17) Uani 1 1 d . A 2 H11X H 0.3836 0.5374 0.6535 0.113 Uiso 1 1 calc R A 2 H11Y H 0.4563 0.5393 0.7154 0.113 Uiso 1 1 calc R A 2 H11Z H 0.3984 0.4880 0.7064 0.113 Uiso 1 1 calc R A 2 C12 C 0.4356(3) 0.4580(2) 0.5755(3) 0.0738(17) Uani 1 1 d . A 2 H12X H 0.4739 0.4427 0.5436 0.111 Uiso 1 1 calc R A 2 H12Y H 0.3953 0.4802 0.5481 0.111 Uiso 1 1 calc R A 2 H12Z H 0.4072 0.4293 0.5987 0.111 Uiso 1 1 calc R A 2 C13 C 0.9532(7) 0.4734(4) 0.7422(7) 0.033(3) Uani 0.505(8) 1 d PDU A 1 H13A H 1.0105 0.4643 0.7334 0.039 Uiso 0.505(8) 1 calc PR A 1 H13B H 0.9321 0.4971 0.7032 0.039 Uiso 0.505(8) 1 calc PR A 1 C14 C 0.9560(8) 0.5059(4) 0.8119(6) 0.038(3) Uani 0.505(8) 1 d PDU A 1 H14 H 0.9559 0.4805 0.8526 0.046 Uiso 0.505(8) 1 calc PR A 1 C15 C 0.8813(5) 0.5418(4) 0.8132(5) 0.052(3) Uani 0.505(8) 1 d PDU A 1 H15A H 0.8845 0.5619 0.8578 0.077 Uiso 0.505(8) 1 calc PR A 1 H15B H 0.8314 0.5201 0.8096 0.077 Uiso 0.505(8) 1 calc PR A 1 H15C H 0.8800 0.5666 0.7731 0.077 Uiso 0.505(8) 1 calc PR A 1 C16 C 1.0344(5) 0.5407(4) 0.8224(6) 0.066(3) Uani 0.505(8) 1 d PDU A 1 H16A H 1.0831 0.5180 0.8216 0.099 Uiso 0.505(8) 1 calc PR A 1 H16B H 1.0352 0.5591 0.8681 0.099 Uiso 0.505(8) 1 calc PR A 1 H16C H 1.0343 0.5669 0.7840 0.099 Uiso 0.505(8) 1 calc PR A 1 C113 C 0.9678(8) 0.4649(4) 0.7329(8) 0.033(3) Uani 0.495(8) 1 d PDU A 2 H11A H 1.0236 0.4501 0.7428 0.040 Uiso 0.495(8) 1 calc PR A 2 H11B H 0.9645 0.4809 0.6849 0.040 Uiso 0.495(8) 1 calc PR A 2 C114 C 0.9536(9) 0.5087(4) 0.7877(6) 0.043(3) Uani 0.495(8) 1 d PDU A 2 H114 H 0.8930 0.5128 0.7904 0.051 Uiso 0.495(8) 1 calc PR A 2 C115 C 0.9865(8) 0.5605(4) 0.7599(7) 0.081(4) Uani 0.495(8) 1 d PDU A 2 H11D H 0.9784 0.5891 0.7938 0.121 Uiso 0.495(8) 1 calc PR A 2 H11E H 0.9572 0.5691 0.7141 0.121 Uiso 0.495(8) 1 calc PR A 2 H11F H 1.0453 0.5566 0.7539 0.121 Uiso 0.495(8) 1 calc PR A 2 C116 C 0.9926(7) 0.4966(5) 0.8636(5) 0.068(3) Uani 0.495(8) 1 d PDU A 2 H11G H 0.9700 0.4633 0.8807 0.101 Uiso 0.495(8) 1 calc PR A 2 H11H H 0.9801 0.5257 0.8956 0.101 Uiso 0.495(8) 1 calc PR A 2 H11I H 1.0522 0.4932 0.8626 0.101 Uiso 0.495(8) 1 calc PR A 2 C17 C 0.9202(3) 0.3712(2) 0.6576(3) 0.0349(14) Uani 0.740(7) 1 d PDU A 1 H17A H 0.9806 0.3667 0.6612 0.042 Uiso 0.740(7) 1 calc PR A 1 H17B H 0.8955 0.3354 0.6606 0.042 Uiso 0.740(7) 1 calc PR A 1 C18 C 0.8936(3) 0.3949(3) 0.5848(3) 0.0394(14) Uani 0.740(7) 1 d PDU A 1 H18 H 0.9032 0.4342 0.5868 0.047 Uiso 0.740(7) 1 calc PR A 1 C19 C 0.8036(4) 0.3849(4) 0.5615(5) 0.051(2) Uani 0.740(7) 1 d PDU A 1 H19A H 0.7902 0.4009 0.5147 0.076 Uiso 0.740(7) 1 calc PR A 1 H19B H 0.7691 0.4009 0.5959 0.076 Uiso 0.740(7) 1 calc PR A 1 H19C H 0.7934 0.3465 0.5588 0.076 Uiso 0.740(7) 1 calc PR A 1 C20 C 0.9471(4) 0.3711(3) 0.5306(3) 0.0500(18) Uani 0.740(7) 1 d PDU A 1 H20A H 0.9308 0.3858 0.4835 0.075 Uiso 0.740(7) 1 calc PR A 1 H20B H 0.9401 0.3324 0.5295 0.075 Uiso 0.740(7) 1 calc PR A 1 H20C H 1.0048 0.3797 0.5438 0.075 Uiso 0.740(7) 1 calc PR A 1 C117 C 0.9153(9) 0.4057(6) 0.6386(6) 0.035(3) Uani 0.260(7) 1 d PDU A 2 H11O H 0.8992 0.4397 0.6149 0.042 Uiso 0.260(7) 1 calc PR A 2 H11P H 0.9755 0.4020 0.6371 0.042 Uiso 0.260(7) 1 calc PR A 2 C118 C 0.8746(8) 0.3608(6) 0.5954(7) 0.036(3) Uani 0.260(7) 1 d PDU A 2 H118 H 0.8720 0.3301 0.6289 0.043 Uiso 0.260(7) 1 calc PR A 2 C119 C 0.7868(9) 0.3710(11) 0.5665(15) 0.050(6) Uani 0.260(7) 1 d PDU A 2 H11J H 0.7661 0.3401 0.5389 0.076 Uiso 0.260(7) 1 calc PR A 2 H11K H 0.7849 0.4025 0.5359 0.076 Uiso 0.260(7) 1 calc PR A 2 H11L H 0.7524 0.3769 0.6060 0.076 Uiso 0.260(7) 1 calc PR A 2 C120 C 0.9248(11) 0.3415(9) 0.5365(9) 0.047(5) Uani 0.260(7) 1 d PDU A 2 H12D H 0.8952 0.3129 0.5103 0.071 Uiso 0.260(7) 1 calc PR A 2 H12E H 0.9779 0.3281 0.5570 0.071 Uiso 0.260(7) 1 calc PR A 2 H12F H 0.9339 0.3710 0.5042 0.071 Uiso 0.260(7) 1 calc PR A 2 C21 C 0.9384(6) 0.3687(5) 0.8078(5) 0.046(3) Uani 0.582(8) 1 d PDU A 1 H21A H 0.9311 0.3866 0.8536 0.055 Uiso 0.582(8) 1 calc PR A 1 H21B H 0.9084 0.3345 0.8077 0.055 Uiso 0.582(8) 1 calc PR A 1 C22 C 1.0307(5) 0.3573(5) 0.8029(6) 0.070(2) Uani 0.582(8) 1 d PDU A 1 H22 H 1.0482 0.3780 0.7616 0.083 Uiso 0.582(8) 1 calc PR A 1 C23 C 1.0780(9) 0.3759(6) 0.8637(8) 0.131(5) Uani 0.582(8) 1 d PDU A 1 H23A H 1.0667 0.4138 0.8705 0.197 Uiso 0.582(8) 1 calc PR A 1 H23B H 1.1365 0.3710 0.8574 0.197 Uiso 0.582(8) 1 calc PR A 1 H23C H 1.0635 0.3559 0.9055 0.197 Uiso 0.582(8) 1 calc PR A 1 C24 C 1.0483(6) 0.2977(4) 0.7879(6) 0.077(3) Uani 0.582(8) 1 d PDU A 1 H24A H 1.0160 0.2866 0.7446 0.115 Uiso 0.582(8) 1 calc PR A 1 H24B H 1.0331 0.2760 0.8279 0.115 Uiso 0.582(8) 1 calc PR A 1 H24C H 1.1069 0.2931 0.7818 0.115 Uiso 0.582(8) 1 calc PR A 1 C121 C 0.9421(9) 0.3613(7) 0.7940(9) 0.055(3) Uani 0.418(8) 1 d PDU A 2 H12A H 0.9550 0.3813 0.8386 0.066 Uiso 0.418(8) 1 calc PR A 2 H12B H 0.8965 0.3371 0.8040 0.066 Uiso 0.418(8) 1 calc PR A 2 C122 C 1.0156(7) 0.3236(6) 0.7911(7) 0.067(3) Uani 0.418(8) 1 d PDU A 2 H122 H 1.0041 0.3011 0.7478 0.081 Uiso 0.418(8) 1 calc PR A 2 C123 C 1.0913(7) 0.3496(6) 0.7831(7) 0.071(4) Uani 0.418(8) 1 d PDU A 2 H12G H 1.0852 0.3736 0.7422 0.107 Uiso 0.418(8) 1 calc PR A 2 H12H H 1.1336 0.3230 0.7754 0.107 Uiso 0.418(8) 1 calc PR A 2 H12I H 1.1075 0.3700 0.8261 0.107 Uiso 0.418(8) 1 calc PR A 2 C124 C 1.0239(8) 0.2848(6) 0.8549(8) 0.081(4) Uani 0.418(8) 1 d PDU A 2 H12J H 0.9715 0.2666 0.8591 0.121 Uiso 0.418(8) 1 calc PR A 2 H12K H 1.0389 0.3048 0.8986 0.121 Uiso 0.418(8) 1 calc PR A 2 H12L H 1.0667 0.2586 0.8475 0.121 Uiso 0.418(8) 1 calc PR A 2 C31 C 0.6071(2) 0.36287(15) 0.8108(2) 0.0305(8) Uani 1 1 d . A . C32 C 0.5636(2) 0.33776(16) 0.7542(2) 0.0372(9) Uani 1 1 d . . . H32 H 0.5919 0.3251 0.7156 0.045 Uiso 1 1 calc R A . C33 C 0.4786(2) 0.33086(17) 0.7535(3) 0.0470(11) Uani 1 1 d . A . H33 H 0.4493 0.3139 0.7144 0.056 Uiso 1 1 calc R . . C34 C 0.4376(3) 0.34867(19) 0.8095(3) 0.0525(12) Uani 1 1 d . . . H34 H 0.3797 0.3444 0.8089 0.063 Uiso 1 1 calc R A . C35 C 0.4800(3) 0.3727(2) 0.8667(3) 0.0546(13) Uani 1 1 d . A . H35 H 0.4515 0.3842 0.9058 0.065 Uiso 1 1 calc R . . C36 C 0.5646(2) 0.38020(18) 0.8674(2) 0.0431(10) Uani 1 1 d . . . H36 H 0.5933 0.3972 0.9068 0.052 Uiso 1 1 calc R A . C37 C 0.7540(2) 0.31038(16) 0.7786(2) 0.0351(9) Uani 1 1 d . A . C38 C 0.7449(3) 0.29846(19) 0.7069(3) 0.0460(11) Uani 1 1 d . . . H38 H 0.7199 0.3236 0.6745 0.055 Uiso 1 1 calc R A . C39 C 0.7718(3) 0.2501(2) 0.6817(3) 0.0656(16) Uani 1 1 d . A . H39 H 0.7646 0.2422 0.6324 0.079 Uiso 1 1 calc R . . C40 C 0.8092(4) 0.2133(2) 0.7284(5) 0.081(2) Uani 1 1 d . . . H40 H 0.8280 0.1803 0.7115 0.097 Uiso 1 1 calc R A . C41 C 0.8185(3) 0.2249(2) 0.7983(4) 0.0721(17) Uani 1 1 d . A . H41 H 0.8444 0.1998 0.8302 0.087 Uiso 1 1 calc R . . C42 C 0.7912(3) 0.27265(19) 0.8247(3) 0.0506(12) Uani 1 1 d . . . H42 H 0.7979 0.2797 0.8742 0.061 Uiso 1 1 calc R A . C43 C 0.7550(2) 0.38163(16) 0.90058(19) 0.0322(9) Uani 1 1 d . A . C44 C 0.7327(3) 0.34601(18) 0.9526(2) 0.0430(10) Uani 1 1 d . . . H44 H 0.6957 0.3177 0.9403 0.052 Uiso 1 1 calc R A . C45 C 0.7649(3) 0.3521(2) 1.0225(2) 0.0542(13) Uani 1 1 d . A . H45 H 0.7500 0.3278 1.0578 0.065 Uiso 1 1 calc R . . C46 C 0.8181(3) 0.3930(2) 1.0407(2) 0.0549(13) Uani 1 1 d . . . H46 H 0.8403 0.3967 1.0885 0.066 Uiso 1 1 calc R A . C47 C 0.8394(3) 0.4288(2) 0.9905(2) 0.0485(11) Uani 1 1 d . A . H47 H 0.8756 0.4573 1.0035 0.058 Uiso 1 1 calc R . . C48 C 0.8077(2) 0.42296(17) 0.9203(2) 0.0361(9) Uani 1 1 d . . . H48 H 0.8226 0.4477 0.8855 0.043 Uiso 1 1 calc R A . B200 B 0.2885(2) 0.16944(17) 0.7811(2) 0.0242(8) Uani 1 1 d . . . C201 C 0.2512(2) 0.19132(14) 0.85368(17) 0.0242(8) Uani 1 1 d . . . C202 C 0.1874(2) 0.16485(17) 0.8838(2) 0.0376(9) Uani 1 1 d . B . H202 H 0.1696 0.1315 0.8646 0.045 Uiso 1 1 calc R . . C203 C 0.1490(3) 0.18546(17) 0.9407(2) 0.0477(12) Uani 1 1 d D . . C204 C 0.1729(2) 0.23407(17) 0.9700(2) 0.0389(10) Uani 1 1 d . B . H204 H 0.1468 0.2482 1.0090 0.047 Uiso 1 1 calc R . . C205 C 0.2355(2) 0.26142(15) 0.94126(17) 0.0274(8) Uani 1 1 d D . . C206 C 0.2737(2) 0.24018(14) 0.88456(17) 0.0246(8) Uani 1 1 d . B . H206 H 0.3169 0.2597 0.8660 0.030 Uiso 1 1 calc R . . C207 C 0.0807(4) 0.1563(2) 0.9716(3) 0.0824(15) Uani 0.480(7) 1 d PDU B 1 F1 F 0.0599(6) 0.1109(3) 0.9415(5) 0.120(3) Uani 0.480(7) 1 d PDU B 1 F2 F 0.0116(3) 0.1865(3) 0.9679(4) 0.095(2) Uani 0.480(7) 1 d PDU B 1 F3 F 0.0955(4) 0.1497(3) 1.0419(3) 0.082(2) Uani 0.480(7) 1 d PDU B 1 C307 C 0.0828(4) 0.1522(3) 0.9701(3) 0.0824(15) Uani 0.520(7) 1 d PDU B 2 F101 F 0.0600(6) 0.1682(3) 1.0324(4) 0.108(3) Uani 0.520(7) 1 d PDU B 2 F102 F 0.1058(4) 0.10149(19) 0.9810(4) 0.073(2) Uani 0.520(7) 1 d PDU B 2 F103 F 0.0172(3) 0.1473(4) 0.9240(4) 0.104(3) Uani 0.520(7) 1 d PDU B 2 C208 C 0.2653(3) 0.3128(2) 0.9726(2) 0.0415(10) Uani 0.56(2) 1 d PDU B 1 F4 F 0.3429(5) 0.3086(3) 1.0017(7) 0.075(3) Uani 0.56(2) 1 d PDU B 1 F5 F 0.2695(8) 0.3508(3) 0.9244(4) 0.053(2) Uani 0.56(2) 1 d PDU B 1 F6 F 0.2230(7) 0.3310(3) 1.0241(5) 0.064(2) Uani 0.56(2) 1 d PDU B 1 C308 C 0.2623(4) 0.3135(3) 0.9727(3) 0.0415(10) Uani 0.44(2) 1 d PDU B 2 F104 F 0.1997(6) 0.3407(4) 0.9958(9) 0.070(3) Uani 0.44(2) 1 d PDU B 2 F105 F 0.3164(9) 0.3087(4) 1.0287(6) 0.072(3) Uani 0.44(2) 1 d PDU B 2 F106 F 0.2963(8) 0.3458(3) 0.9278(5) 0.047(2) Uani 0.44(2) 1 d PDU B 2 C209 C 0.2316(2) 0.19971(15) 0.71796(18) 0.0271(8) Uani 1 1 d . . . C210 C 0.1522(2) 0.18256(16) 0.6950(2) 0.0336(9) Uani 1 1 d . . . H210 H 0.1316 0.1510 0.7149 0.040 Uiso 1 1 calc R . . C211 C 0.1029(2) 0.20992(17) 0.6447(2) 0.0400(10) Uani 1 1 d D C . C212 C 0.1296(3) 0.25624(18) 0.6150(2) 0.0435(10) Uani 1 1 d . C . H212 H 0.0960 0.2747 0.5798 0.052 Uiso 1 1 calc R . . C213 C 0.2068(2) 0.27510(16) 0.6379(2) 0.0373(9) Uani 1 1 d D . . C214 C 0.2561(2) 0.24714(15) 0.68845(19) 0.0309(8) Uani 1 1 d . D . H214 H 0.3087 0.2610 0.7034 0.037 Uiso 1 1 calc R . . C215 C 0.0195(3) 0.18932(19) 0.6197(2) 0.0613(14) Uani 1 1 d D . . F7 F -0.0162(7) 0.1646(9) 0.6724(7) 0.084(4) Uani 0.48(4) 1 d PDU C 1 F8 F 0.0214(7) 0.1538(8) 0.5677(10) 0.093(4) Uani 0.48(4) 1 d PDU C 1 F9 F -0.0325(6) 0.2276(4) 0.5961(13) 0.089(4) Uani 0.48(4) 1 d PDU C 1 F107 F 0.0166(6) 0.1722(9) 0.5524(6) 0.077(4) Uani 0.52(4) 1 d PDU C 2 F108 F -0.0387(5) 0.2273(4) 0.6209(11) 0.071(3) Uani 0.52(4) 1 d PDU C 2 F109 F -0.0059(7) 0.1490(6) 0.6579(9) 0.076(4) Uani 0.52(4) 1 d PDU C 2 C216 C 0.2410(3) 0.3248(2) 0.6083(2) 0.0614(12) Uani 0.724(17) 1 d PDU D 1 F10 F 0.3146(4) 0.3179(2) 0.5829(5) 0.083(2) Uani 0.724(17) 1 d PDU D 1 F11 F 0.1927(4) 0.3470(2) 0.5568(3) 0.0607(16) Uani 0.724(17) 1 d PDU D 1 F12 F 0.2551(6) 0.3620(2) 0.6593(3) 0.0760(19) Uani 0.724(17) 1 d PDU D 1 C316 C 0.2397(5) 0.3242(3) 0.6062(4) 0.0614(12) Uani 0.276(17) 1 d PDU D 2 F110 F 0.1794(7) 0.3561(5) 0.5802(11) 0.074(4) Uani 0.276(17) 1 d PDU D 2 F111 F 0.2882(11) 0.3531(5) 0.6514(7) 0.073(4) Uani 0.276(17) 1 d PDU D 2 F112 F 0.2830(14) 0.3122(5) 0.5513(9) 0.093(4) Uani 0.276(17) 1 d PDU D 2 C217 C 0.2835(2) 0.10433(15) 0.77782(18) 0.0266(8) Uani 1 1 d . . . C218 C 0.2532(2) 0.07390(16) 0.7194(2) 0.0317(9) Uani 1 1 d . . . H218 H 0.2305 0.0916 0.6779 0.038 Uiso 1 1 calc R . . C219 C 0.2554(2) 0.01869(16) 0.7203(2) 0.0393(10) Uani 1 1 d D E . C220 C 0.2900(3) -0.00879(17) 0.7786(2) 0.0436(10) Uani 1 1 d . E . H220 H 0.2922 -0.0466 0.7787 0.052 Uiso 1 1 calc R . . C221 C 0.3215(2) 0.02036(16) 0.8371(2) 0.0396(10) Uani 1 1 d D . . C222 C 0.3176(2) 0.07517(15) 0.8363(2) 0.0327(9) Uani 1 1 d . F . H222 H 0.3389 0.0941 0.8772 0.039 Uiso 1 1 calc R . . C223 C 0.2201(3) -0.01153(17) 0.6565(2) 0.0554(13) Uani 1 1 d D . . F13 F 0.2624(7) -0.0079(5) 0.6014(4) 0.080(3) Uani 0.57(2) 1 d PDU E 1 F14 F 0.2158(9) -0.0638(2) 0.6717(4) 0.081(3) Uani 0.57(2) 1 d PDU E 1 F15 F 0.1434(5) 0.0026(5) 0.6373(7) 0.090(3) Uani 0.57(2) 1 d PDU E 1 F113 F 0.1792(11) -0.0542(5) 0.6692(6) 0.087(4) Uani 0.43(2) 1 d PDU E 2 F114 F 0.1708(11) 0.0186(4) 0.6123(7) 0.092(4) Uani 0.43(2) 1 d PDU E 2 F115 F 0.2796(6) -0.0258(7) 0.6151(6) 0.078(4) Uani 0.43(2) 1 d PDU E 2 C224 C 0.3596(3) -0.0080(2) 0.9003(3) 0.0613(12) Uani 0.555(17) 1 d PDU F 1 F16 F 0.4336(4) 0.0129(3) 0.9212(5) 0.073(2) Uani 0.555(17) 1 d PDU F 1 F17 F 0.3144(6) -0.0079(5) 0.9552(4) 0.085(3) Uani 0.555(17) 1 d PDU F 1 F18 F 0.3767(6) -0.0589(2) 0.8859(5) 0.066(2) Uani 0.555(17) 1 d PDU F 1 C324 C 0.3562(4) -0.0080(3) 0.9022(4) 0.0613(12) Uani 0.445(17) 1 d PDU F 2 F116 F 0.2952(5) -0.0274(5) 0.9380(5) 0.065(3) Uani 0.445(17) 1 d PDU F 2 F117 F 0.4030(7) -0.0498(4) 0.8888(6) 0.068(3) Uani 0.445(17) 1 d PDU F 2 F118 F 0.3992(10) 0.0229(3) 0.9490(6) 0.086(3) Uani 0.445(17) 1 d PDU F 2 C225 C 0.3855(2) 0.18305(14) 0.77629(18) 0.0251(8) Uani 1 1 d . . . C226 C 0.4414(2) 0.18861(15) 0.83545(19) 0.0273(8) Uani 1 1 d . . . H226 H 0.4215 0.1870 0.8813 0.033 Uiso 1 1 calc R . . C227 C 0.5251(2) 0.19645(15) 0.8303(2) 0.0330(9) Uani 1 1 d D G . C228 C 0.5571(2) 0.19884(17) 0.7649(2) 0.0370(9) Uani 1 1 d . G . H228 H 0.6142 0.2043 0.7611 0.044 Uiso 1 1 calc R . . C229 C 0.5035(2) 0.19308(15) 0.7049(2) 0.0349(9) Uani 1 1 d D . . C230 C 0.4203(2) 0.18514(15) 0.71030(19) 0.0288(8) Uani 1 1 d . H . H230 H 0.3854 0.1809 0.6680 0.035 Uiso 1 1 calc R . . C231 C 0.5797(2) 0.20069(18) 0.8972(2) 0.0489(12) Uani 1 1 d D . . F19 F 0.5484(5) 0.2309(6) 0.9459(4) 0.075(2) Uani 0.77(4) 1 d PDU G 1 F20 F 0.5912(7) 0.1523(3) 0.9278(6) 0.077(2) Uani 0.77(4) 1 d PDU G 1 F21 F 0.6542(3) 0.2194(6) 0.8876(3) 0.0643(19) Uani 0.77(4) 1 d PDU G 1 F119 F 0.6592(4) 0.2027(15) 0.8846(8) 0.054(5) Uani 0.23(4) 1 d PDU G 2 F120 F 0.5649(18) 0.2457(9) 0.9328(13) 0.070(6) Uani 0.23(4) 1 d PDU G 2 F121 F 0.5716(17) 0.1610(10) 0.9421(10) 0.069(6) Uani 0.23(4) 1 d PDU G 2 C232 C 0.5368(2) 0.19603(16) 0.6340(2) 0.0534(11) Uani 0.812(5) 1 d PDU H 1 F22 F 0.6093(2) 0.17074(18) 0.6323(2) 0.0789(13) Uani 0.812(5) 1 d PDU H 1 F23 F 0.4899(3) 0.1736(2) 0.58298(17) 0.0840(16) Uani 0.812(5) 1 d PDU H 1 F24 F 0.5554(3) 0.24502(14) 0.61600(19) 0.0778(14) Uani 0.812(5) 1 d PDU H 1 C332 C 0.5336(5) 0.1970(3) 0.6329(5) 0.0534(11) Uani 0.188(5) 1 d PDU H 2 F122 F 0.4831(7) 0.2240(7) 0.5875(5) 0.067(3) Uani 0.188(5) 1 d PDU H 2 F123 F 0.6053(7) 0.2218(7) 0.6304(6) 0.071(4) Uani 0.188(5) 1 d PDU H 2 F124 F 0.5428(11) 0.1507(4) 0.6005(6) 0.080(4) Uani 0.188(5) 1 d PDU H 2 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 Rh1 0.02967(16) 0.02883(17) 0.02379(16) 0.00095(13) 0.00695(11) -0.00290(12) P1 0.0410(6) 0.0281(6) 0.0281(5) 0.0040(4) 0.0103(4) 0.0048(4) P2 0.0267(5) 0.0542(7) 0.0326(5) -0.0139(5) 0.0061(4) -0.0090(5) P3 0.0251(5) 0.0277(5) 0.0265(5) 0.0018(4) 0.0047(4) -0.0005(4) C1 0.037(5) 0.038(4) 0.031(4) 0.007(3) 0.008(3) 0.008(4) C2 0.043(5) 0.042(4) 0.034(3) -0.001(3) 0.007(4) 0.010(4) C3 0.069(7) 0.063(6) 0.028(4) -0.003(4) 0.015(4) 0.009(5) C4 0.063(7) 0.065(5) 0.043(4) -0.007(4) 0.001(5) -0.001(5) C101 0.041(6) 0.038(6) 0.036(5) 0.002(4) 0.006(5) 0.007(6) C102 0.051(7) 0.048(6) 0.033(5) -0.003(4) 0.007(5) 0.010(6) C103 0.065(8) 0.070(8) 0.043(7) -0.004(6) 0.007(6) 0.013(7) C104 0.056(8) 0.056(7) 0.048(7) -0.014(5) 0.001(7) 0.008(7) C5 0.054(3) 0.030(2) 0.035(2) 0.0028(17) 0.0100(18) 0.0004(18) C6 0.068(3) 0.030(2) 0.036(2) 0.0064(18) 0.014(2) 0.000(2) C7 0.071(3) 0.065(4) 0.050(3) 0.004(3) 0.028(2) 0.011(3) C8 0.111(5) 0.047(3) 0.063(3) 0.014(3) 0.042(3) -0.001(3) C9 0.035(2) 0.033(2) 0.047(2) 0.0059(19) 0.0081(18) 0.0074(17) C10 0.041(2) 0.045(3) 0.052(3) 0.012(2) 0.004(2) 0.010(2) C11 0.060(3) 0.091(5) 0.076(4) 0.010(3) 0.016(3) 0.039(3) C12 0.053(3) 0.079(4) 0.085(4) -0.012(3) -0.021(3) 0.018(3) C13 0.014(4) 0.049(5) 0.038(5) -0.004(4) 0.016(3) 0.004(4) C14 0.035(4) 0.035(4) 0.044(6) -0.003(4) 0.006(5) -0.006(3) C15 0.042(5) 0.051(5) 0.062(5) -0.008(4) 0.007(4) -0.002(4) C16 0.048(5) 0.062(6) 0.088(6) -0.023(5) 0.006(5) -0.016(4) C113 0.022(5) 0.042(5) 0.038(5) -0.006(4) 0.020(4) -0.003(4) C114 0.036(4) 0.040(4) 0.054(6) -0.007(4) 0.017(4) -0.007(3) C115 0.084(7) 0.051(6) 0.111(8) -0.016(6) 0.034(6) -0.021(5) C116 0.059(5) 0.078(6) 0.067(6) -0.037(5) 0.004(5) -0.012(5) C17 0.030(3) 0.044(3) 0.030(3) -0.004(2) 0.001(2) 0.005(2) C18 0.035(3) 0.051(4) 0.033(3) -0.004(3) 0.006(2) 0.004(3) C19 0.047(4) 0.067(6) 0.037(4) 0.001(4) -0.002(3) -0.005(4) C20 0.054(4) 0.062(5) 0.035(3) -0.007(3) 0.008(3) 0.004(3) C117 0.029(5) 0.044(6) 0.032(5) -0.004(5) 0.004(5) 0.007(5) C118 0.035(5) 0.044(6) 0.029(5) -0.006(5) 0.001(4) 0.004(5) C119 0.042(9) 0.057(10) 0.050(9) 0.009(8) -0.009(7) -0.004(8) C120 0.053(8) 0.055(9) 0.034(7) -0.010(7) 0.007(6) 0.009(7) C21 0.030(3) 0.047(4) 0.061(4) -0.003(4) 0.002(3) -0.001(3) C22 0.049(4) 0.065(4) 0.094(4) 0.005(4) 0.002(3) 0.007(3) C23 0.118(6) 0.125(7) 0.149(7) -0.022(5) 0.000(5) 0.010(5) C24 0.070(5) 0.076(5) 0.084(5) -0.001(4) 0.002(4) 0.027(4) C121 0.040(5) 0.051(5) 0.076(5) -0.006(4) 0.008(4) 0.001(4) C122 0.062(5) 0.065(5) 0.074(5) -0.008(4) -0.003(4) 0.009(4) C123 0.064(5) 0.079(6) 0.073(5) 0.003(5) 0.014(4) 0.012(4) C124 0.076(6) 0.079(6) 0.086(6) 0.014(5) 0.001(5) 0.009(5) C31 0.0277(19) 0.026(2) 0.038(2) 0.0086(17) 0.0070(16) 0.0016(15) C32 0.030(2) 0.032(2) 0.050(2) 0.0021(19) 0.0055(17) -0.0009(17) C33 0.033(2) 0.034(2) 0.073(3) 0.006(2) -0.001(2) -0.0032(18) C34 0.033(2) 0.042(3) 0.084(4) 0.013(3) 0.014(2) -0.002(2) C35 0.041(3) 0.058(3) 0.069(3) 0.002(3) 0.025(2) 0.006(2) C36 0.036(2) 0.046(3) 0.049(3) -0.001(2) 0.0120(19) 0.0022(19) C37 0.0260(19) 0.028(2) 0.053(3) 0.0009(18) 0.0131(17) -0.0025(16) C38 0.039(2) 0.045(3) 0.055(3) -0.013(2) 0.014(2) -0.0037(19) C39 0.058(3) 0.051(3) 0.093(4) -0.037(3) 0.037(3) -0.016(3) C40 0.069(4) 0.034(3) 0.148(7) -0.013(4) 0.062(4) -0.001(3) C41 0.064(3) 0.042(3) 0.117(5) 0.025(3) 0.046(3) 0.017(3) C42 0.043(2) 0.042(3) 0.070(3) 0.015(2) 0.023(2) 0.011(2) C43 0.034(2) 0.038(2) 0.0253(19) 0.0063(17) 0.0066(15) 0.0035(17) C44 0.048(2) 0.046(3) 0.036(2) 0.013(2) 0.0080(18) -0.003(2) C45 0.063(3) 0.066(3) 0.034(2) 0.021(2) 0.012(2) 0.010(3) C46 0.065(3) 0.073(4) 0.026(2) 0.002(2) -0.002(2) 0.007(3) C47 0.053(3) 0.059(3) 0.032(2) -0.005(2) -0.0034(19) -0.004(2) C48 0.039(2) 0.043(2) 0.027(2) 0.0023(18) 0.0036(16) -0.0022(18) B200 0.026(2) 0.026(2) 0.0210(19) 0.0014(17) 0.0029(15) -0.0023(16) C201 0.0226(17) 0.029(2) 0.0207(17) 0.0007(15) 0.0011(13) 0.0001(14) C202 0.039(2) 0.035(2) 0.040(2) -0.0107(18) 0.0138(18) -0.0124(18) C203 0.049(3) 0.045(3) 0.053(3) -0.018(2) 0.031(2) -0.020(2) C204 0.042(2) 0.044(3) 0.033(2) -0.0106(19) 0.0180(17) -0.0045(19) C205 0.0309(19) 0.028(2) 0.0232(18) -0.0004(15) 0.0032(15) 0.0011(15) C206 0.0235(17) 0.028(2) 0.0224(18) 0.0041(15) 0.0031(14) -0.0016(14) C207 0.079(3) 0.079(3) 0.095(3) -0.027(3) 0.047(2) -0.031(2) F1 0.118(6) 0.100(5) 0.151(6) -0.053(5) 0.067(5) -0.068(5) F2 0.048(3) 0.131(6) 0.112(5) -0.005(4) 0.038(3) -0.040(4) F3 0.076(4) 0.079(5) 0.099(4) 0.028(4) 0.061(4) -0.002(4) C307 0.079(3) 0.079(3) 0.095(3) -0.027(3) 0.047(2) -0.031(2) F101 0.120(6) 0.096(5) 0.122(5) -0.031(4) 0.092(4) -0.034(4) F102 0.072(4) 0.062(4) 0.088(4) 0.007(3) 0.028(3) -0.038(3) F103 0.047(3) 0.103(5) 0.164(6) 0.026(5) 0.020(4) -0.029(4) C208 0.051(2) 0.038(2) 0.036(2) -0.0044(18) 0.0098(18) -0.0053(18) F4 0.066(4) 0.072(4) 0.083(5) -0.036(4) -0.026(4) -0.006(3) F5 0.073(5) 0.035(3) 0.052(3) 0.007(3) 0.011(3) -0.002(3) F6 0.103(5) 0.053(4) 0.043(4) -0.023(3) 0.041(3) -0.030(3) C308 0.051(2) 0.038(2) 0.036(2) -0.0044(18) 0.0098(18) -0.0053(18) F104 0.078(5) 0.056(4) 0.080(6) -0.035(4) 0.034(4) 0.000(4) F105 0.106(5) 0.063(4) 0.040(4) 0.001(3) -0.024(4) -0.029(4) F106 0.059(5) 0.031(4) 0.057(4) -0.009(3) 0.034(3) -0.010(3) C209 0.0304(19) 0.027(2) 0.0235(18) -0.0021(15) 0.0031(14) 0.0012(15) C210 0.030(2) 0.037(2) 0.033(2) 0.0031(17) 0.0025(16) 0.0008(17) C211 0.030(2) 0.049(3) 0.040(2) 0.005(2) -0.0053(17) -0.0008(18) C212 0.043(2) 0.046(3) 0.040(2) 0.007(2) -0.0079(19) 0.008(2) C213 0.047(2) 0.030(2) 0.034(2) 0.0043(17) -0.0029(18) 0.0030(18) C214 0.037(2) 0.028(2) 0.0269(19) -0.0016(16) -0.0024(16) 0.0007(16) C215 0.039(3) 0.074(4) 0.069(4) 0.018(3) -0.013(2) -0.001(3) F7 0.039(4) 0.097(7) 0.116(7) 0.018(6) 0.006(4) -0.008(5) F8 0.074(5) 0.087(7) 0.112(7) -0.015(6) -0.029(5) -0.025(5) F9 0.051(5) 0.100(6) 0.111(8) 0.021(5) -0.027(5) 0.000(4) F107 0.065(4) 0.099(7) 0.064(5) -0.023(5) -0.016(3) -0.020(4) F108 0.033(4) 0.091(5) 0.087(7) -0.006(4) -0.006(3) 0.013(3) F109 0.048(4) 0.074(6) 0.101(6) 0.023(5) -0.015(4) -0.019(4) C216 0.069(3) 0.047(2) 0.066(3) 0.021(2) -0.008(2) 0.003(2) F10 0.064(3) 0.079(3) 0.108(4) 0.050(3) 0.014(3) -0.005(2) F11 0.085(3) 0.049(3) 0.045(3) 0.022(2) -0.013(2) -0.004(2) F12 0.094(4) 0.043(3) 0.086(3) 0.008(2) -0.024(3) -0.013(3) C316 0.069(3) 0.047(2) 0.066(3) 0.021(2) -0.008(2) 0.003(2) F110 0.089(7) 0.051(6) 0.076(7) 0.017(6) -0.021(6) 0.012(5) F111 0.059(6) 0.061(6) 0.094(6) 0.036(5) -0.025(5) -0.025(5) F112 0.104(7) 0.086(7) 0.090(7) 0.041(6) 0.021(6) -0.002(6) C217 0.0265(18) 0.029(2) 0.0254(18) -0.0004(16) 0.0091(14) -0.0009(15) C218 0.035(2) 0.032(2) 0.029(2) -0.0036(16) 0.0075(16) -0.0037(16) C219 0.043(2) 0.031(2) 0.045(2) -0.0104(19) 0.0128(19) -0.0081(18) C220 0.049(3) 0.026(2) 0.058(3) 0.000(2) 0.019(2) -0.0009(19) C221 0.039(2) 0.032(2) 0.048(2) 0.008(2) 0.0080(19) 0.0018(18) C222 0.034(2) 0.029(2) 0.035(2) 0.0021(17) 0.0037(16) -0.0007(16) C223 0.073(4) 0.037(3) 0.057(3) -0.019(2) 0.013(3) -0.009(2) F13 0.108(5) 0.090(6) 0.044(3) -0.015(4) 0.022(4) -0.034(4) F14 0.113(7) 0.048(4) 0.082(4) -0.022(3) 0.007(4) -0.024(4) F15 0.076(4) 0.098(6) 0.091(5) -0.046(4) -0.014(4) -0.012(4) F113 0.096(7) 0.081(6) 0.087(5) -0.034(5) 0.025(5) -0.057(5) F114 0.109(7) 0.075(6) 0.085(6) -0.037(5) -0.037(5) -0.011(5) F115 0.099(6) 0.086(7) 0.052(5) -0.029(5) 0.023(4) -0.006(5) C224 0.070(3) 0.045(2) 0.068(3) 0.016(2) 0.000(2) 0.004(2) F16 0.077(4) 0.063(4) 0.075(4) 0.019(3) -0.021(3) 0.011(3) F17 0.115(5) 0.090(5) 0.051(4) 0.020(4) 0.015(4) 0.032(4) F18 0.054(4) 0.040(3) 0.102(4) 0.025(3) -0.001(3) 0.008(3) C324 0.070(3) 0.045(2) 0.068(3) 0.016(2) 0.000(2) 0.004(2) F116 0.081(5) 0.063(5) 0.053(4) 0.014(4) 0.016(4) 0.010(4) F117 0.055(5) 0.067(5) 0.085(5) 0.030(4) 0.024(4) 0.023(4) F118 0.110(6) 0.064(5) 0.076(5) 0.021(4) -0.040(4) 0.002(4) C225 0.0296(19) 0.0213(19) 0.0255(18) 0.0037(15) 0.0088(15) 0.0011(14) C226 0.0262(18) 0.032(2) 0.0242(18) 0.0055(16) 0.0044(14) 0.0006(15) C227 0.0263(19) 0.041(2) 0.032(2) 0.0095(18) 0.0032(15) 0.0008(16) C228 0.028(2) 0.042(3) 0.042(2) 0.0081(19) 0.0108(17) -0.0005(17) C229 0.038(2) 0.033(2) 0.035(2) -0.0011(17) 0.0164(17) -0.0021(17) C230 0.034(2) 0.027(2) 0.0257(19) -0.0003(15) 0.0064(15) -0.0036(15) C231 0.023(2) 0.078(4) 0.045(3) 0.017(3) 0.0003(18) -0.007(2) F19 0.046(3) 0.139(5) 0.038(3) -0.011(3) -0.005(2) -0.012(3) F20 0.049(3) 0.116(4) 0.064(3) 0.053(3) -0.007(3) -0.004(3) F21 0.036(2) 0.100(5) 0.056(3) 0.016(3) -0.002(2) -0.026(2) F119 0.023(7) 0.077(10) 0.062(8) 0.021(6) 0.001(6) 0.001(6) F120 0.056(8) 0.099(9) 0.053(8) -0.015(7) -0.007(6) -0.005(7) F121 0.050(9) 0.105(9) 0.050(8) 0.040(7) 0.002(6) -0.013(7) C232 0.057(2) 0.067(3) 0.040(2) -0.003(2) 0.0237(19) -0.014(2) F22 0.069(2) 0.105(3) 0.069(2) -0.007(2) 0.0455(19) 0.012(2) F23 0.076(3) 0.144(4) 0.0352(18) -0.027(2) 0.0254(17) -0.048(3) F24 0.131(4) 0.058(2) 0.051(2) 0.0105(18) 0.050(2) -0.013(2) C332 0.057(2) 0.067(3) 0.040(2) -0.003(2) 0.0237(19) -0.014(2) F122 0.077(6) 0.093(7) 0.036(5) 0.020(6) 0.031(5) 0.008(6) F123 0.069(6) 0.088(7) 0.058(6) 0.000(6) 0.024(5) -0.026(6) F124 0.097(7) 0.090(7) 0.057(6) -0.008(6) 0.028(6) -0.006(6) _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 Rh1 P3 2.2057(10) . ? Rh1 P1 2.3240(10) . ? Rh1 P2 2.3620(11) . ? P1 C9 1.838(4) . ? P1 C101 1.843(9) . ? P1 C5 1.846(4) . ? P1 C1 1.847(6) . ? P2 C121 1.826(9) . ? P2 C113 1.838(8) . ? P2 C17 1.852(5) . ? P2 C21 1.855(7) . ? P2 C13 1.860(8) . ? P2 C117 1.887(10) . ? P3 C43 1.830(4) . ? P3 C37 1.839(4) . ? P3 C31 1.845(4) . ? C1 C2 1.526(9) . ? C1 H10A 0.9900 . ? C1 H10B 0.9900 . ? C2 C4 1.519(10) . ? C2 C3 1.533(9) . ? C2 H102 1.0000 . ? C3 H10C 0.9800 . ? C3 H10D 0.9800 . ? C3 H10E 0.9800 . ? C4 H10F 0.9800 . ? C4 H10G 0.9800 . ? C4 H10H 0.9800 . ? C101 C102 1.527(11) . ? C101 H1A 0.9900 . ? C101 H1B 0.9900 . ? C102 C104 1.514(12) . ? C102 C103 1.534(12) . ? C102 H2 1.0000 . ? C103 H3A 0.9800 . ? C103 H3B 0.9800 . ? C103 H3C 0.9800 . ? C104 H4A 0.9800 . ? C104 H4B 0.9800 . ? C104 H4C 0.9800 . ? C5 C6 1.522(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.508(7) . ? C6 C8 1.520(6) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.539(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.510(7) . ? C10 C12 1.524(7) . ? C10 H10 1.0000 . ? C11 H11X 0.9800 . ? C11 H11Y 0.9800 . ? C11 H11Z 0.9800 . ? C12 H12X 0.9800 . ? C12 H12Y 0.9800 . ? C12 H12Z 0.9800 . ? C13 C14 1.548(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.519(13) . ? C14 C16 1.549(12) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C113 C114 1.541(11) . ? C113 H11A 0.9900 . ? C113 H11B 0.9900 . ? C114 C115 1.518(14) . ? C114 C116 1.553(11) . ? C114 H114 1.0000 . ? C115 H11D 0.9800 . ? C115 H11E 0.9800 . ? C115 H11F 0.9800 . ? C116 H11G 0.9800 . ? C116 H11H 0.9800 . ? C116 H11I 0.9800 . ? C17 C18 1.531(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C20 1.522(7) . ? C18 C19 1.522(8) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C117 C118 1.516(11) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 C120 1.514(11) . ? C118 C119 1.516(12) . ? C118 H118 1.0000 . ? C119 H11J 0.9800 . ? C119 H11K 0.9800 . ? C119 H11L 0.9800 . ? C120 H12D 0.9800 . ? C120 H12E 0.9800 . ? C120 H12F 0.9800 . ? C21 C22 1.545(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.413(14) . ? C22 C24 1.555(13) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C121 C122 1.533(12) . ? C121 H12A 0.9900 . ? C121 H12B 0.9900 . ? C122 C123 1.417(16) . ? C122 C124 1.548(14) . ? C122 H122 1.0000 . ? C123 H12G 0.9800 . ? C123 H12H 0.9800 . ? C123 H12I 0.9800 . ? C124 H12J 0.9800 . ? C124 H12K 0.9800 . ? C124 H12L 0.9800 . ? C31 C32 1.388(6) . ? C31 C36 1.391(6) . ? C32 C33 1.399(5) . ? C32 H32 0.9500 . ? C33 C34 1.372(7) . ? C33 H33 0.9500 . ? C34 C35 1.375(7) . ? C34 H34 0.9500 . ? C35 C36 1.392(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.384(6) . ? C37 C42 1.395(6) . ? C38 C39 1.391(7) . ? C38 H38 0.9500 . ? C39 C40 1.386(9) . ? C39 H39 0.9500 . ? C40 C41 1.349(9) . ? C40 H40 0.9500 . ? C41 C42 1.386(7) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.381(6) . ? C43 C44 1.400(5) . ? C44 C45 1.391(6) . ? C44 H44 0.9500 . ? C45 C46 1.373(7) . ? C45 H45 0.9500 . ? C46 C47 1.372(7) . ? C46 H46 0.9500 . ? C47 C48 1.394(5) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? B200 C225 1.630(5) . ? B200 C201 1.640(5) . ? B200 C217 1.640(5) . ? B200 C209 1.640(5) . ? C201 C202 1.395(5) . ? C201 C206 1.396(5) . ? C202 C203 1.388(5) . ? C202 H202 0.9500 . ? C203 C204 1.385(6) . ? C203 C207 1.492(8) . ? C203 C307 1.508(8) . ? C204 C205 1.379(5) . ? C204 H204 0.9500 . ? C205 C206 1.389(5) . ? C205 C208 1.487(7) . ? C205 C308 1.489(8) . ? C206 H206 0.9500 . ? C207 F1 1.307(5) . ? C207 F3 1.342(5) . ? C207 F2 1.358(5) . ? C307 F101 1.325(6) . ? C307 F103 1.331(6) . ? C307 F102 1.341(6) . ? C208 F6 1.320(4) . ? C208 F5 1.326(5) . ? C208 F4 1.346(4) . ? C308 F106 1.327(5) . ? C308 F105 1.329(6) . ? C308 F104 1.332(6) . ? C209 C214 1.389(5) . ? C209 C210 1.402(5) . ? C210 C211 1.381(5) . ? C210 H210 0.9500 . ? C211 C212 1.379(6) . ? C211 C215 1.497(6) . ? C212 C213 1.383(6) . ? C212 H212 0.9500 . ? C213 C214 1.390(5) . ? C213 C316 1.492(9) . ? C213 C216 1.494(7) . ? C214 H214 0.9500 . ? C215 F109 1.329(6) . ? C215 F8 1.331(7) . ? C215 F9 1.337(7) . ? C215 F107 1.340(7) . ? C215 F7 1.346(7) . ? C215 F108 1.348(6) . ? C216 F11 1.327(4) . ? C216 F10 1.340(4) . ? C216 F12 1.351(4) . ? C316 F111 1.333(6) . ? C316 F110 1.333(6) . ? C316 F112 1.335(6) . ? C217 C218 1.401(5) . ? C217 C222 1.404(5) . ? C218 C219 1.389(6) . ? C218 H218 0.9500 . ? C219 C220 1.383(6) . ? C219 C223 1.500(6) . ? C220 C221 1.390(6) . ? C220 H220 0.9500 . ? C221 C222 1.380(6) . ? C221 C224 1.485(8) . ? C221 C324 1.495(8) . ? C222 H222 0.9500 . ? C223 F113 1.295(7) . ? C223 F13 1.299(6) . ? C223 F15 1.325(6) . ? C223 F115 1.344(7) . ? C223 F114 1.346(7) . ? C223 F14 1.349(6) . ? C224 F17 1.319(5) . ? C224 F18 1.343(5) . ? C224 F16 1.347(5) . ? C324 F118 1.334(6) . ? C324 F117 1.335(6) . ? C324 F116 1.339(6) . ? C225 C226 1.393(5) . ? C225 C230 1.412(5) . ? C226 C227 1.393(5) . ? C226 H226 0.9500 . ? C227 C228 1.382(5) . ? C227 C231 1.491(6) . ? C228 C229 1.383(5) . ? C228 H228 0.9500 . ? C229 C230 1.385(5) . ? C229 C332 1.486(9) . ? C229 C232 1.488(6) . ? C230 H230 0.9500 . ? C231 F121 1.323(8) . ? C231 F19 1.328(6) . ? C231 F21 1.330(5) . ? C231 F119 1.339(7) . ? C231 F120 1.348(8) . ? C231 F20 1.353(6) . ? C232 F23 1.310(4) . ? C232 F24 1.320(4) . ? C232 F22 1.347(4) . ? C332 F124 1.330(6) . ? C332 F122 1.330(6) . ? C332 F123 1.331(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P3 Rh1 P1 97.42(4) . . ? P3 Rh1 P2 95.12(4) . . ? P1 Rh1 P2 167.02(4) . . ? C9 P1 C101 113.6(7) . . ? C9 P1 C5 102.82(19) . . ? C101 P1 C5 100.3(9) . . ? C9 P1 C1 102.0(4) . . ? C101 P1 C1 11.7(7) . . ? C5 P1 C1 104.7(5) . . ? C9 P1 Rh1 113.99(13) . . ? C101 P1 Rh1 117.8(7) . . ? C5 P1 Rh1 105.59(14) . . ? C1 P1 Rh1 125.3(4) . . ? C121 P2 C113 104.4(8) . . ? C121 P2 C17 89.4(6) . . ? C113 P2 C17 100.1(4) . . ? C121 P2 C21 10.3(9) . . ? C113 P2 C21 101.6(7) . . ? C17 P2 C21 99.6(4) . . ? C121 P2 C13 108.6(8) . . ? C113 P2 C13 11.6(6) . . ? C17 P2 C13 110.5(4) . . ? C21 P2 C13 103.9(6) . . ? C121 P2 C117 115.5(8) . . ? C113 P2 C117 81.2(6) . . ? C17 P2 C117 29.1(5) . . ? C21 P2 C117 125.2(6) . . ? C13 P2 C117 89.1(6) . . ? C121 P2 Rh1 125.2(5) . . ? C113 P2 Rh1 114.0(5) . . ? C17 P2 Rh1 118.94(16) . . ? C21 P2 Rh1 119.4(3) . . ? C13 P2 Rh1 103.6(4) . . ? C117 P2 Rh1 108.0(5) . . ? C43 P3 C37 105.44(19) . . ? C43 P3 C31 103.11(17) . . ? C37 P3 C31 101.23(17) . . ? C43 P3 Rh1 115.24(13) . . ? C37 P3 Rh1 112.08(13) . . ? C31 P3 Rh1 118.07(12) . . ? C2 C1 P1 115.8(6) . . ? C2 C1 H10A 108.3 . . ? P1 C1 H10A 108.3 . . ? C2 C1 H10B 108.3 . . ? P1 C1 H10B 108.3 . . ? H10A C1 H10B 107.4 . . ? C4 C2 C1 112.6(7) . . ? C4 C2 C3 110.7(7) . . ? C1 C2 C3 109.7(7) . . ? C4 C2 H102 107.9 . . ? C1 C2 H102 107.9 . . ? C3 C2 H102 107.9 . . ? C2 C3 H10C 109.5 . . ? C2 C3 H10D 109.5 . . ? H10C C3 H10D 109.5 . . ? C2 C3 H10E 109.5 . . ? H10C C3 H10E 109.5 . . ? H10D C3 H10E 109.5 . . ? C2 C4 H10F 109.5 . . ? C2 C4 H10G 109.5 . . ? H10F C4 H10G 109.5 . . ? C2 C4 H10H 109.5 . . ? H10F C4 H10H 109.5 . . ? H10G C4 H10H 109.5 . . ? C102 C101 P1 120.3(11) . . ? C102 C101 H1A 107.3 . . ? P1 C101 H1A 107.3 . . ? C102 C101 H1B 107.3 . . ? P1 C101 H1B 107.3 . . ? H1A C101 H1B 106.9 . . ? C104 C102 C101 113.2(11) . . ? C104 C102 C103 111.9(11) . . ? C101 C102 C103 108.4(11) . . ? C104 C102 H2 107.7 . . ? C101 C102 H2 107.7 . . ? C103 C102 H2 107.7 . . ? C102 C103 H3A 109.5 . . ? C102 C103 H3B 109.5 . . ? H3A C103 H3B 109.5 . . ? C102 C103 H3C 109.5 . . ? H3A C103 H3C 109.5 . . ? H3B C103 H3C 109.5 . . ? C102 C104 H4A 109.5 . . ? C102 C104 H4B 109.5 . . ? H4A C104 H4B 109.5 . . ? C102 C104 H4C 109.5 . . ? H4A C104 H4C 109.5 . . ? H4B C104 H4C 109.5 . . ? C6 C5 P1 113.2(3) . . ? C6 C5 H5A 108.9 . . ? P1 C5 H5A 108.9 . . ? C6 C5 H5B 108.9 . . ? P1 C5 H5B 108.9 . . ? H5A C5 H5B 107.8 . . ? C7 C6 C8 111.7(4) . . ? C7 C6 C5 109.2(4) . . ? C8 C6 C5 110.8(4) . . ? C7 C6 H6 108.3 . . ? C8 C6 H6 108.3 . . ? C5 C6 H6 108.3 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P1 121.8(3) . . ? C10 C9 H9A 106.9 . . ? P1 C9 H9A 106.9 . . ? C10 C9 H9B 106.9 . . ? P1 C9 H9B 106.9 . . ? H9A C9 H9B 106.7 . . ? C11 C10 C12 110.5(4) . . ? C11 C10 C9 113.6(4) . . ? C12 C10 C9 108.9(4) . . ? C11 C10 H10 107.9 . . ? C12 C10 H10 107.9 . . ? C9 C10 H10 107.9 . . ? C10 C11 H11X 109.5 . . ? C10 C11 H11Y 109.5 . . ? H11X C11 H11Y 109.5 . . ? C10 C11 H11Z 109.5 . . ? H11X C11 H11Z 109.5 . . ? H11Y C11 H11Z 109.5 . . ? C10 C12 H12X 109.5 . . ? C10 C12 H12Y 109.5 . . ? H12X C12 H12Y 109.5 . . ? C10 C12 H12Z 109.5 . . ? H12X C12 H12Z 109.5 . . ? H12Y C12 H12Z 109.5 . . ? C14 C13 P2 119.5(8) . . ? C14 C13 H13A 107.5 . . ? P2 C13 H13A 107.5 . . ? C14 C13 H13B 107.5 . . ? P2 C13 H13B 107.5 . . ? H13A C13 H13B 107.0 . . ? C15 C14 C13 111.0(9) . . ? C15 C14 C16 108.6(8) . . ? C13 C14 C16 112.1(9) . . ? C15 C14 H14 108.4 . . ? C13 C14 H14 108.4 . . ? C16 C14 H14 108.4 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C114 C113 P2 112.3(8) . . ? C114 C113 H11A 109.2 . . ? P2 C113 H11A 109.2 . . ? C114 C113 H11B 109.2 . . ? P2 C113 H11B 109.2 . . ? H11A C113 H11B 107.9 . . ? C115 C114 C113 107.6(10) . . ? C115 C114 C116 110.9(10) . . ? C113 C114 C116 114.1(10) . . ? C115 C114 H114 108.0 . . ? C113 C114 H114 108.0 . . ? C116 C114 H114 108.0 . . ? C114 C115 H11D 109.5 . . ? C114 C115 H11E 109.5 . . ? H11D C115 H11E 109.5 . . ? C114 C115 H11F 109.5 . . ? H11D C115 H11F 109.5 . . ? H11E C115 H11F 109.5 . . ? C114 C116 H11G 109.5 . . ? C114 C116 H11H 109.5 . . ? H11G C116 H11H 109.5 . . ? C114 C116 H11I 109.5 . . ? H11G C116 H11I 109.5 . . ? H11H C116 H11I 109.5 . . ? C18 C17 P2 115.3(4) . . ? C18 C17 H17A 108.5 . . ? P2 C17 H17A 108.5 . . ? C18 C17 H17B 108.5 . . ? P2 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C20 C18 C19 109.4(5) . . ? C20 C18 C17 108.3(5) . . ? C19 C18 C17 113.3(6) . . ? C20 C18 H18 108.6 . . ? C19 C18 H18 108.6 . . ? C17 C18 H18 108.6 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C118 C117 P2 117.1(9) . . ? C118 C117 H11O 108.0 . . ? P2 C117 H11O 108.0 . . ? C118 C117 H11P 108.0 . . ? P2 C117 H11P 108.0 . . ? H11O C117 H11P 107.3 . . ? C120 C118 C119 110.0(12) . . ? C120 C118 C117 113.2(11) . . ? C119 C118 C117 115.5(13) . . ? C120 C118 H118 105.8 . . ? C119 C118 H118 105.8 . . ? C117 C118 H118 105.8 . . ? C118 C119 H11J 109.5 . . ? C118 C119 H11K 109.5 . . ? H11J C119 H11K 109.5 . . ? C118 C119 H11L 109.5 . . ? H11J C119 H11L 109.5 . . ? H11K C119 H11L 109.5 . . ? C118 C120 H12D 109.5 . . ? C118 C120 H12E 109.5 . . ? H12D C120 H12E 109.5 . . ? C118 C120 H12F 109.5 . . ? H12D C120 H12F 109.5 . . ? H12E C120 H12F 109.5 . . ? C22 C21 P2 113.8(7) . . ? C22 C21 H21A 108.8 . . ? P2 C21 H21A 108.8 . . ? C22 C21 H21B 108.8 . . ? P2 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C23 C22 C21 111.2(10) . . ? C23 C22 C24 111.8(9) . . ? C21 C22 C24 112.7(9) . . ? C23 C22 H22 106.9 . . ? C21 C22 H22 106.9 . . ? C24 C22 H22 106.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C122 C121 P2 135.4(11) . . ? C122 C121 H12A 103.3 . . ? P2 C121 H12A 103.3 . . ? C122 C121 H12B 103.3 . . ? P2 C121 H12B 103.3 . . ? H12A C121 H12B 105.2 . . ? C123 C122 C121 114.3(14) . . ? C123 C122 C124 110.4(10) . . ? C121 C122 C124 112.4(10) . . ? C123 C122 H122 106.3 . . ? C121 C122 H122 106.3 . . ? C124 C122 H122 106.3 . . ? C122 C123 H12G 109.5 . . ? C122 C123 H12H 109.5 . . ? H12G C123 H12H 109.5 . . ? C122 C123 H12I 109.5 . . ? H12G C123 H12I 109.5 . . ? H12H C123 H12I 109.5 . . ? C122 C124 H12J 109.5 . . ? C122 C124 H12K 109.5 . . ? H12J C124 H12K 109.5 . . ? C122 C124 H12L 109.5 . . ? H12J C124 H12L 109.5 . . ? H12K C124 H12L 109.5 . . ? C32 C31 C36 118.6(4) . . ? C32 C31 P3 119.5(3) . . ? C36 C31 P3 121.8(3) . . ? C31 C32 C33 120.7(4) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 119.8(4) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 120.2(4) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C34 C35 C36 120.3(4) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C31 C36 C35 120.3(4) . . ? C31 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C38 C37 C42 118.2(4) . . ? C38 C37 P3 117.8(3) . . ? C42 C37 P3 123.9(3) . . ? C37 C38 C39 120.8(5) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C40 C39 C38 120.1(5) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C41 C40 C39 119.2(5) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C40 C41 C42 121.7(5) . . ? C40 C41 H41 119.1 . . ? C42 C41 H41 119.1 . . ? C41 C42 C37 120.0(5) . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? C48 C43 C44 118.9(4) . . ? C48 C43 P3 118.3(3) . . ? C44 C43 P3 122.8(3) . . ? C45 C44 C43 119.8(4) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C46 C45 C44 120.3(4) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C47 C46 C45 120.6(4) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C46 C47 C48 119.6(4) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? C43 C48 C47 120.8(4) . . ? C43 C48 H48 119.6 . . ? C47 C48 H48 119.6 . . ? C225 B200 C201 113.8(3) . . ? C225 B200 C217 104.6(3) . . ? C201 B200 C217 110.2(3) . . ? C225 B200 C209 111.1(3) . . ? C201 B200 C209 103.1(3) . . ? C217 B200 C209 114.4(3) . . ? C202 C201 C206 115.4(3) . . ? C202 C201 B200 121.3(3) . . ? C206 C201 B200 122.8(3) . . ? C203 C202 C201 122.4(4) . . ? C203 C202 H202 118.8 . . ? C201 C202 H202 118.8 . . ? C204 C203 C202 120.6(4) . . ? C204 C203 C207 118.2(4) . . ? C202 C203 C207 121.2(4) . . ? C204 C203 C307 122.0(4) . . ? C202 C203 C307 117.4(4) . . ? C207 C203 C307 4.2(3) . . ? C205 C204 C203 118.5(4) . . ? C205 C204 H204 120.8 . . ? C203 C204 H204 120.8 . . ? C204 C205 C206 120.3(4) . . ? C204 C205 C208 120.4(3) . . ? C206 C205 C208 119.3(3) . . ? C204 C205 C308 119.0(4) . . ? C206 C205 C308 120.7(4) . . ? C208 C205 C308 2.0(3) . . ? C205 C206 C201 122.8(3) . . ? C205 C206 H206 118.6 . . ? C201 C206 H206 118.6 . . ? F1 C207 F3 110.1(6) . . ? F1 C207 F2 106.3(6) . . ? F3 C207 F2 101.7(5) . . ? F1 C207 C203 115.8(5) . . ? F3 C207 C203 111.5(5) . . ? F2 C207 C203 110.4(5) . . ? F101 C307 F103 110.0(6) . . ? F101 C307 F102 104.3(6) . . ? F103 C307 F102 102.3(6) . . ? F101 C307 C203 114.8(6) . . ? F103 C307 C203 112.0(5) . . ? F102 C307 C203 112.5(5) . . ? F6 C208 F5 108.4(5) . . ? F6 C208 F4 104.9(5) . . ? F5 C208 F4 103.8(5) . . ? F6 C208 C205 115.0(4) . . ? F5 C208 C205 112.6(5) . . ? F4 C208 C205 111.2(4) . . ? F106 C308 F105 106.1(6) . . ? F106 C308 F104 105.5(6) . . ? F105 C308 F104 105.3(6) . . ? F106 C308 C205 114.0(6) . . ? F105 C308 C205 113.2(6) . . ? F104 C308 C205 111.9(5) . . ? C214 C209 C210 115.4(3) . . ? C214 C209 B200 121.7(3) . . ? C210 C209 B200 122.6(3) . . ? C211 C210 C209 122.3(4) . . ? C211 C210 H210 118.8 . . ? C209 C210 H210 118.8 . . ? C212 C211 C210 121.0(4) . . ? C212 C211 C215 118.3(3) . . ? C210 C211 C215 120.7(4) . . ? C211 C212 C213 118.2(4) . . ? C211 C212 H212 120.9 . . ? C213 C212 H212 120.9 . . ? C212 C213 C214 120.3(4) . . ? C212 C213 C316 120.4(4) . . ? C214 C213 C316 119.2(4) . . ? C212 C213 C216 121.9(3) . . ? C214 C213 C216 117.8(3) . . ? C316 C213 C216 1.8(3) . . ? C209 C214 C213 122.7(4) . . ? C209 C214 H214 118.7 . . ? C213 C214 H214 118.7 . . ? F109 C215 F8 85.2(9) . . ? F109 C215 F9 120.7(9) . . ? F8 C215 F9 106.8(6) . . ? F109 C215 F107 106.4(6) . . ? F8 C215 F107 23.7(8) . . ? F9 C215 F107 86.7(8) . . ? F109 C215 F7 22.1(9) . . ? F8 C215 F7 105.9(6) . . ? F9 C215 F7 106.1(6) . . ? F107 C215 F7 124.7(8) . . ? F109 C215 F108 106.1(6) . . ? F8 C215 F108 123.1(8) . . ? F9 C215 F108 20.9(9) . . ? F107 C215 F108 105.8(5) . . ? F7 C215 F108 88.0(9) . . ? F109 C215 C211 114.1(5) . . ? F8 C215 C211 113.1(6) . . ? F9 C215 C211 113.2(6) . . ? F107 C215 C211 111.9(5) . . ? F7 C215 C211 111.3(6) . . ? F108 C215 C211 112.0(5) . . ? F11 C216 F10 106.8(4) . . ? F11 C216 F12 106.7(4) . . ? F10 C216 F12 103.8(5) . . ? F11 C216 C213 114.1(4) . . ? F10 C216 C213 113.6(4) . . ? F12 C216 C213 111.2(4) . . ? F111 C316 F110 107.1(7) . . ? F111 C316 F112 107.3(7) . . ? F110 C316 F112 105.7(7) . . ? F111 C316 C213 114.0(7) . . ? F110 C316 C213 111.6(7) . . ? F112 C316 C213 110.7(7) . . ? C218 C217 C222 115.4(4) . . ? C218 C217 B200 126.0(3) . . ? C222 C217 B200 118.4(3) . . ? C219 C218 C217 122.0(4) . . ? C219 C218 H218 119.0 . . ? C217 C218 H218 119.0 . . ? C220 C219 C218 121.1(4) . . ? C220 C219 C223 119.6(4) . . ? C218 C219 C223 119.3(4) . . ? C219 C220 C221 118.2(4) . . ? C219 C220 H220 120.9 . . ? C221 C220 H220 120.9 . . ? C222 C221 C220 120.3(4) . . ? C222 C221 C224 120.2(4) . . ? C220 C221 C224 119.5(4) . . ? C222 C221 C324 120.0(4) . . ? C220 C221 C324 119.7(4) . . ? C224 C221 C324 2.6(3) . . ? C221 C222 C217 123.0(4) . . ? C221 C222 H222 118.5 . . ? C217 C222 H222 118.5 . . ? F113 C223 F13 121.5(7) . . ? F113 C223 F15 77.4(6) . . ? F13 C223 F15 108.2(6) . . ? F113 C223 F115 107.1(6) . . ? F13 C223 F115 25.4(7) . . ? F15 C223 F115 128.5(7) . . ? F113 C223 F114 106.7(6) . . ? F13 C223 F114 78.0(7) . . ? F15 C223 F114 34.2(6) . . ? F115 C223 F114 102.3(6) . . ? F113 C223 F14 28.1(6) . . ? F13 C223 F14 106.3(5) . . ? F15 C223 F14 104.8(5) . . ? F115 C223 F14 85.1(7) . . ? F114 C223 F14 129.9(6) . . ? F113 C223 C219 116.2(6) . . ? F13 C223 C219 114.4(5) . . ? F15 C223 C219 112.3(4) . . ? F115 C223 C219 110.7(5) . . ? F114 C223 C219 112.7(5) . . ? F14 C223 C219 110.2(5) . . ? F17 C224 F18 107.4(5) . . ? F17 C224 F16 108.3(5) . . ? F18 C224 F16 103.5(5) . . ? F17 C224 C221 114.0(5) . . ? F18 C224 C221 111.9(5) . . ? F16 C224 C221 111.0(5) . . ? F118 C324 F117 107.8(6) . . ? F118 C324 F116 104.5(6) . . ? F117 C324 F116 105.7(6) . . ? F118 C324 C221 114.4(5) . . ? F117 C324 C221 113.9(6) . . ? F116 C324 C221 109.9(6) . . ? C226 C225 C230 114.9(3) . . ? C226 C225 B200 123.7(3) . . ? C230 C225 B200 121.2(3) . . ? C225 C226 C227 122.9(3) . . ? C225 C226 H226 118.6 . . ? C227 C226 H226 118.6 . . ? C228 C227 C226 120.8(3) . . ? C228 C227 C231 120.8(3) . . ? C226 C227 C231 118.4(3) . . ? C227 C228 C229 118.0(3) . . ? C227 C228 H228 121.0 . . ? C229 C228 H228 121.0 . . ? C228 C229 C230 121.0(3) . . ? C228 C229 C332 120.6(4) . . ? C230 C229 C332 118.3(4) . . ? C228 C229 C232 118.7(3) . . ? C230 C229 C232 120.3(3) . . ? C332 C229 C232 2.3(3) . . ? C229 C230 C225 122.4(3) . . ? C229 C230 H230 118.8 . . ? C225 C230 H230 118.8 . . ? F121 C231 F19 85.5(12) . . ? F121 C231 F21 119.5(10) . . ? F19 C231 F21 107.3(5) . . ? F121 C231 F119 106.9(7) . . ? F19 C231 F119 122.3(10) . . ? F21 C231 F119 18.7(13) . . ? F121 C231 F120 106.3(7) . . ? F19 C231 F120 22.9(13) . . ? F21 C231 F120 88.5(12) . . ? F119 C231 F120 105.8(7) . . ? F121 C231 F20 20.9(13) . . ? F19 C231 F20 105.4(4) . . ? F21 C231 F20 106.2(4) . . ? F119 C231 F20 90.4(12) . . ? F120 C231 F20 124.3(11) . . ? F121 C231 C227 114.0(7) . . ? F19 C231 C227 113.1(4) . . ? F21 C231 C227 113.7(4) . . ? F119 C231 C227 112.0(7) . . ? F120 C231 C227 111.3(6) . . ? F20 C231 C227 110.6(4) . . ? F23 C232 F24 110.3(4) . . ? F23 C232 F22 104.0(4) . . ? F24 C232 F22 102.3(4) . . ? F23 C232 C229 114.0(3) . . ? F24 C232 C229 112.7(3) . . ? F22 C232 C229 112.5(3) . . ? F124 C332 F122 103.7(7) . . ? F124 C332 F123 105.1(7) . . ? F122 C332 F123 103.9(7) . . ? F124 C332 C229 114.9(7) . . ? F122 C332 C229 113.1(6) . . ? F123 C332 C229 114.8(7) . . ? 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 P3 Rh1 P1 C9 -77.39(15) . . . . ? P2 Rh1 P1 C9 117.7(2) . . . . ? P3 Rh1 P1 C101 59.6(10) . . . . ? P2 Rh1 P1 C101 -105.3(10) . . . . ? P3 Rh1 P1 C5 170.50(14) . . . . ? P2 Rh1 P1 C5 5.6(2) . . . . ? P3 Rh1 P1 C1 49.1(6) . . . . ? P2 Rh1 P1 C1 -115.8(6) . . . . ? P3 Rh1 P2 C121 -14.0(9) . . . . ? P1 Rh1 P2 C121 151.0(9) . . . . ? P3 Rh1 P2 C113 -144.2(5) . . . . ? P1 Rh1 P2 C113 20.8(5) . . . . ? P3 Rh1 P2 C17 98.1(2) . . . . ? P1 Rh1 P2 C17 -97.0(3) . . . . ? P3 Rh1 P2 C21 -24.0(5) . . . . ? P1 Rh1 P2 C21 141.0(5) . . . . ? P3 Rh1 P2 C13 -138.9(4) . . . . ? P1 Rh1 P2 C13 26.1(5) . . . . ? P3 Rh1 P2 C117 127.6(5) . . . . ? P1 Rh1 P2 C117 -67.5(5) . . . . ? P1 Rh1 P3 C43 -101.37(14) . . . . ? P2 Rh1 P3 C43 75.25(14) . . . . ? P1 Rh1 P3 C37 138.04(14) . . . . ? P2 Rh1 P3 C37 -45.33(14) . . . . ? P1 Rh1 P3 C31 21.01(15) . . . . ? P2 Rh1 P3 C31 -162.36(15) . . . . ? C9 P1 C1 C2 158.7(8) . . . . ? C101 P1 C1 C2 -26(6) . . . . ? C5 P1 C1 C2 -94.4(9) . . . . ? Rh1 P1 C1 C2 27.4(11) . . . . ? P1 C1 C2 C4 68.3(11) . . . . ? P1 C1 C2 C3 -167.9(9) . . . . ? C9 P1 C101 C102 154.6(13) . . . . ? C5 P1 C101 C102 -96.4(17) . . . . ? C1 P1 C101 C102 150(8) . . . . ? Rh1 P1 C101 C102 18(2) . . . . ? P1 C101 C102 C104 62(2) . . . . ? P1 C101 C102 C103 -172.9(17) . . . . ? C9 P1 C5 C6 -71.0(3) . . . . ? C101 P1 C5 C6 171.7(7) . . . . ? C1 P1 C5 C6 -177.2(5) . . . . ? Rh1 P1 C5 C6 48.8(3) . . . . ? P1 C5 C6 C7 -59.1(5) . . . . ? P1 C5 C6 C8 177.4(4) . . . . ? C101 P1 C9 C10 69.3(11) . . . . ? C5 P1 C9 C10 -38.1(4) . . . . ? C1 P1 C9 C10 70.2(6) . . . . ? Rh1 P1 C9 C10 -151.9(3) . . . . ? P1 C9 C10 C11 -66.6(5) . . . . ? P1 C9 C10 C12 169.8(4) . . . . ? C121 P2 C13 C14 -68.6(12) . . . . ? C113 P2 C13 C14 -139(5) . . . . ? C17 P2 C13 C14 -165.2(9) . . . . ? C21 P2 C13 C14 -59.1(11) . . . . ? C117 P2 C13 C14 174.7(11) . . . . ? Rh1 P2 C13 C14 66.4(11) . . . . ? P2 C13 C14 C15 -83.0(12) . . . . ? P2 C13 C14 C16 155.4(9) . . . . ? C121 P2 C113 C114 -94.1(11) . . . . ? C17 P2 C113 C114 173.9(9) . . . . ? C21 P2 C113 C114 -83.9(11) . . . . ? C13 P2 C113 C114 19(4) . . . . ? C117 P2 C113 C114 151.7(12) . . . . ? Rh1 P2 C113 C114 45.8(11) . . . . ? P2 C113 C114 C115 -152.5(10) . . . . ? P2 C113 C114 C116 84.0(13) . . . . ? C121 P2 C17 C18 -179.2(7) . . . . ? C113 P2 C17 C18 -74.7(7) . . . . ? C21 P2 C17 C18 -178.4(5) . . . . ? C13 P2 C17 C18 -69.5(7) . . . . ? C117 P2 C17 C18 -24.4(9) . . . . ? Rh1 P2 C17 C18 50.0(5) . . . . ? P2 C17 C18 C20 158.5(5) . . . . ? P2 C17 C18 C19 -79.9(7) . . . . ? C121 P2 C117 C118 74.2(13) . . . . ? C113 P2 C117 C118 176.0(13) . . . . ? C17 P2 C117 C118 46.0(9) . . . . ? C21 P2 C117 C118 77.9(12) . . . . ? C13 P2 C117 C118 -175.5(12) . . . . ? Rh1 P2 C117 C118 -71.5(12) . . . . ? P2 C117 C118 C120 -150.4(13) . . . . ? P2 C117 C118 C119 81.6(19) . . . . ? C121 P2 C21 C22 59(5) . . . . ? C113 P2 C21 C22 -47.6(10) . . . . ? C17 P2 C21 C22 54.9(9) . . . . ? C13 P2 C21 C22 -59.2(10) . . . . ? C117 P2 C21 C22 39.8(12) . . . . ? Rh1 P2 C21 C22 -173.9(7) . . . . ? P2 C21 C22 C23 120.6(11) . . . . ? P2 C21 C22 C24 -112.9(10) . . . . ? C113 P2 C121 C122 -68(2) . . . . ? C17 P2 C121 C122 32(2) . . . . ? C21 P2 C121 C122 -144(7) . . . . ? C13 P2 C121 C122 -80(2) . . . . ? C117 P2 C121 C122 19(2) . . . . ? Rh1 P2 C121 C122 157.6(16) . . . . ? P2 C121 C122 C123 60(2) . . . . ? P2 C121 C122 C124 -173.3(17) . . . . ? C43 P3 C31 C32 -157.0(3) . . . . ? C37 P3 C31 C32 -48.1(4) . . . . ? Rh1 P3 C31 C32 74.6(3) . . . . ? C43 P3 C31 C36 26.4(4) . . . . ? C37 P3 C31 C36 135.4(3) . . . . ? Rh1 P3 C31 C36 -101.9(3) . . . . ? C36 C31 C32 C33 1.1(6) . . . . ? P3 C31 C32 C33 -175.5(3) . . . . ? C31 C32 C33 C34 -0.5(6) . . . . ? C32 C33 C34 C35 -0.8(7) . . . . ? C33 C34 C35 C36 1.5(7) . . . . ? C32 C31 C36 C35 -0.4(6) . . . . ? P3 C31 C36 C35 176.2(3) . . . . ? C34 C35 C36 C31 -0.9(7) . . . . ? C43 P3 C37 C38 -170.8(3) . . . . ? C31 P3 C37 C38 82.1(3) . . . . ? Rh1 P3 C37 C38 -44.7(3) . . . . ? C43 P3 C37 C42 8.1(4) . . . . ? C31 P3 C37 C42 -99.1(4) . . . . ? Rh1 P3 C37 C42 134.2(3) . . . . ? C42 C37 C38 C39 0.2(6) . . . . ? P3 C37 C38 C39 179.2(3) . . . . ? C37 C38 C39 C40 -0.7(7) . . . . ? C38 C39 C40 C41 0.4(8) . . . . ? C39 C40 C41 C42 0.3(8) . . . . ? C40 C41 C42 C37 -0.8(7) . . . . ? C38 C37 C42 C41 0.5(6) . . . . ? P3 C37 C42 C41 -178.4(3) . . . . ? C37 P3 C43 C48 119.4(3) . . . . ? C31 P3 C43 C48 -134.9(3) . . . . ? Rh1 P3 C43 C48 -4.8(4) . . . . ? C37 P3 C43 C44 -60.2(4) . . . . ? C31 P3 C43 C44 45.6(4) . . . . ? Rh1 P3 C43 C44 175.7(3) . . . . ? C48 C43 C44 C45 -1.2(6) . . . . ? P3 C43 C44 C45 178.3(3) . . . . ? C43 C44 C45 C46 0.4(7) . . . . ? C44 C45 C46 C47 0.7(8) . . . . ? C45 C46 C47 C48 -0.9(7) . . . . ? C44 C43 C48 C47 1.0(6) . . . . ? P3 C43 C48 C47 -178.6(3) . . . . ? C46 C47 C48 C43 0.1(7) . . . . ? C225 B200 C201 C202 -149.5(3) . . . . ? C217 B200 C201 C202 -32.4(4) . . . . ? C209 B200 C201 C202 90.1(4) . . . . ? C225 B200 C201 C206 38.2(5) . . . . ? C217 B200 C201 C206 155.4(3) . . . . ? C209 B200 C201 C206 -82.1(4) . . . . ? C206 C201 C202 C203 -0.2(6) . . . . ? B200 C201 C202 C203 -173.0(4) . . . . ? C201 C202 C203 C204 0.2(7) . . . . ? C201 C202 C203 C207 179.8(4) . . . . ? C201 C202 C203 C307 -178.0(4) . . . . ? C202 C203 C204 C205 0.1(7) . . . . ? C207 C203 C204 C205 -179.5(4) . . . . ? C307 C203 C204 C205 178.2(4) . . . . ? C203 C204 C205 C206 -0.4(6) . . . . ? C203 C204 C205 C208 -177.8(4) . . . . ? C203 C204 C205 C308 -179.5(4) . . . . ? C204 C205 C206 C201 0.4(5) . . . . ? C208 C205 C206 C201 177.8(3) . . . . ? C308 C205 C206 C201 179.5(4) . . . . ? C202 C201 C206 C205 -0.1(5) . . . . ? B200 C201 C206 C205 172.6(3) . . . . ? C204 C203 C207 F1 179.3(7) . . . . ? C202 C203 C207 F1 -0.3(8) . . . . ? C307 C203 C207 F1 -28(4) . . . . ? C204 C203 C207 F3 -53.8(7) . . . . ? C202 C203 C207 F3 126.6(6) . . . . ? C307 C203 C207 F3 99(4) . . . . ? C204 C203 C207 F2 58.5(6) . . . . ? C202 C203 C207 F2 -121.1(6) . . . . ? C307 C203 C207 F2 -149(4) . . . . ? C204 C203 C307 F101 -11.4(9) . . . . ? C202 C203 C307 F101 166.8(7) . . . . ? C207 C203 C307 F101 -40(4) . . . . ? C204 C203 C307 F103 115.0(7) . . . . ? C202 C203 C307 F103 -66.8(7) . . . . ? C207 C203 C307 F103 86(4) . . . . ? C204 C203 C307 F102 -130.4(6) . . . . ? C202 C203 C307 F102 47.8(7) . . . . ? C207 C203 C307 F102 -159(5) . . . . ? C204 C205 C208 F6 -5.5(8) . . . . ? C206 C205 C208 F6 177.1(7) . . . . ? C308 C205 C208 F6 42(9) . . . . ? C204 C205 C208 F5 -130.4(7) . . . . ? C206 C205 C208 F5 52.2(8) . . . . ? C308 C205 C208 F5 -83(9) . . . . ? C204 C205 C208 F4 113.5(8) . . . . ? C206 C205 C208 F4 -63.9(8) . . . . ? C308 C205 C208 F4 161(9) . . . . ? C204 C205 C308 F106 -154.4(8) . . . . ? C206 C205 C308 F106 26.6(9) . . . . ? C208 C205 C308 F106 73(9) . . . . ? C204 C205 C308 F105 84.1(9) . . . . ? C206 C205 C308 F105 -94.9(9) . . . . ? C208 C205 C308 F105 -49(9) . . . . ? C204 C205 C308 F104 -34.7(9) . . . . ? C206 C205 C308 F104 146.2(9) . . . . ? C208 C205 C308 F104 -168(9) . . . . ? C225 B200 C209 C214 -27.5(5) . . . . ? C201 B200 C209 C214 94.7(4) . . . . ? C217 B200 C209 C214 -145.7(3) . . . . ? C225 B200 C209 C210 158.8(3) . . . . ? C201 B200 C209 C210 -79.1(4) . . . . ? C217 B200 C209 C210 40.6(5) . . . . ? C214 C209 C210 C211 2.2(5) . . . . ? B200 C209 C210 C211 176.3(4) . . . . ? C209 C210 C211 C212 -0.8(6) . . . . ? C209 C210 C211 C215 177.8(4) . . . . ? C210 C211 C212 C213 -1.1(6) . . . . ? C215 C211 C212 C213 -179.7(4) . . . . ? C211 C212 C213 C214 1.3(6) . . . . ? C211 C212 C213 C316 178.4(5) . . . . ? C211 C212 C213 C216 179.6(4) . . . . ? C210 C209 C214 C213 -2.0(5) . . . . ? B200 C209 C214 C213 -176.1(3) . . . . ? C212 C213 C214 C209 0.3(6) . . . . ? C316 C213 C214 C209 -176.8(5) . . . . ? C216 C213 C214 C209 -178.1(4) . . . . ? C212 C211 C215 F109 -171.0(12) . . . . ? C210 C211 C215 F109 10.4(13) . . . . ? C212 C211 C215 F8 93.9(13) . . . . ? C210 C211 C215 F8 -84.8(13) . . . . ? C212 C211 C215 F9 -27.8(13) . . . . ? C210 C211 C215 F9 153.6(13) . . . . ? C212 C211 C215 F107 68.2(12) . . . . ? C210 C211 C215 F107 -110.4(12) . . . . ? C212 C211 C215 F7 -147.1(12) . . . . ? C210 C211 C215 F7 34.2(13) . . . . ? C212 C211 C215 F108 -50.4(11) . . . . ? C210 C211 C215 F108 131.0(11) . . . . ? C212 C213 C216 F11 -2.9(7) . . . . ? C214 C213 C216 F11 175.4(5) . . . . ? C316 C213 C216 F11 33(11) . . . . ? C212 C213 C216 F10 -125.6(6) . . . . ? C214 C213 C216 F10 52.7(6) . . . . ? C316 C213 C216 F10 -90(11) . . . . ? C212 C213 C216 F12 117.8(6) . . . . ? C214 C213 C216 F12 -63.8(6) . . . . ? C316 C213 C216 F12 154(11) . . . . ? C212 C213 C316 F111 147.1(12) . . . . ? C214 C213 C316 F111 -35.8(12) . . . . ? C216 C213 C316 F111 2(11) . . . . ? C212 C213 C316 F110 25.7(13) . . . . ? C214 C213 C316 F110 -157.2(11) . . . . ? C216 C213 C316 F110 -119(11) . . . . ? C212 C213 C316 F112 -91.8(12) . . . . ? C214 C213 C316 F112 85.3(12) . . . . ? C216 C213 C316 F112 124(11) . . . . ? C225 B200 C217 C218 -105.3(4) . . . . ? C201 B200 C217 C218 132.0(3) . . . . ? C209 B200 C217 C218 16.5(5) . . . . ? C225 B200 C217 C222 69.8(4) . . . . ? C201 B200 C217 C222 -52.9(4) . . . . ? C209 B200 C217 C222 -168.4(3) . . . . ? C222 C217 C218 C219 1.3(5) . . . . ? B200 C217 C218 C219 176.5(3) . . . . ? C217 C218 C219 C220 -1.9(6) . . . . ? C217 C218 C219 C223 178.6(3) . . . . ? C218 C219 C220 C221 1.0(6) . . . . ? C223 C219 C220 C221 -179.4(4) . . . . ? C219 C220 C221 C222 0.3(6) . . . . ? C219 C220 C221 C224 -179.6(4) . . . . ? C219 C220 C221 C324 177.5(4) . . . . ? C220 C221 C222 C217 -0.8(6) . . . . ? C224 C221 C222 C217 179.0(4) . . . . ? C324 C221 C222 C217 -178.0(4) . . . . ? C218 C217 C222 C221 0.0(5) . . . . ? B200 C217 C222 C221 -175.6(3) . . . . ? C220 C219 C223 F113 40.4(11) . . . . ? C218 C219 C223 F113 -140.1(10) . . . . ? C220 C219 C223 F13 -109.3(9) . . . . ? C218 C219 C223 F13 70.3(9) . . . . ? C220 C219 C223 F15 126.9(9) . . . . ? C218 C219 C223 F15 -53.5(9) . . . . ? C220 C219 C223 F115 -82.1(10) . . . . ? C218 C219 C223 F115 97.5(10) . . . . ? C220 C219 C223 F114 164.0(11) . . . . ? C218 C219 C223 F114 -16.5(11) . . . . ? C220 C219 C223 F14 10.4(9) . . . . ? C218 C219 C223 F14 -170.0(8) . . . . ? C222 C221 C224 F17 73.3(8) . . . . ? C220 C221 C224 F17 -106.8(8) . . . . ? C324 C221 C224 F17 -12(7) . . . . ? C222 C221 C224 F18 -164.5(6) . . . . ? C220 C221 C224 F18 15.4(8) . . . . ? C324 C221 C224 F18 110(7) . . . . ? C222 C221 C224 F16 -49.4(7) . . . . ? C220 C221 C224 F16 130.5(7) . . . . ? C324 C221 C224 F16 -135(7) . . . . ? C222 C221 C324 F118 -15.7(10) . . . . ? C220 C221 C324 F118 167.1(9) . . . . ? C224 C221 C324 F118 80(7) . . . . ? C222 C221 C324 F117 -140.2(8) . . . . ? C220 C221 C324 F117 42.6(9) . . . . ? C224 C221 C324 F117 -44(7) . . . . ? C222 C221 C324 F116 101.5(8) . . . . ? C220 C221 C324 F116 -75.7(9) . . . . ? C224 C221 C324 F116 -163(8) . . . . ? C201 B200 C225 C226 29.1(5) . . . . ? C217 B200 C225 C226 -91.2(4) . . . . ? C209 B200 C225 C226 144.9(3) . . . . ? C201 B200 C225 C230 -156.9(3) . . . . ? C217 B200 C225 C230 82.7(4) . . . . ? C209 B200 C225 C230 -41.2(5) . . . . ? C230 C225 C226 C227 0.9(5) . . . . ? B200 C225 C226 C227 175.2(3) . . . . ? C225 C226 C227 C228 -0.3(6) . . . . ? C225 C226 C227 C231 -178.7(4) . . . . ? C226 C227 C228 C229 -0.2(6) . . . . ? C231 C227 C228 C229 178.1(4) . . . . ? C227 C228 C229 C230 0.0(6) . . . . ? C227 C228 C229 C332 178.0(5) . . . . ? C227 C228 C229 C232 179.5(4) . . . . ? C228 C229 C230 C225 0.7(6) . . . . ? C332 C229 C230 C225 -177.4(5) . . . . ? C232 C229 C230 C225 -178.8(3) . . . . ? C226 C225 C230 C229 -1.1(5) . . . . ? B200 C225 C230 C229 -175.6(3) . . . . ? C228 C227 C231 F121 -126.2(19) . . . . ? C226 C227 C231 F121 52.1(19) . . . . ? C228 C227 C231 F19 138.2(9) . . . . ? C226 C227 C231 F19 -43.4(9) . . . . ? C228 C227 C231 F21 15.5(10) . . . . ? C226 C227 C231 F21 -166.2(8) . . . . ? C228 C227 C231 F119 -4.7(18) . . . . ? C226 C227 C231 F119 173.6(17) . . . . ? C228 C227 C231 F120 113.6(19) . . . . ? C226 C227 C231 F120 -68.1(19) . . . . ? C228 C227 C231 F20 -103.9(9) . . . . ? C226 C227 C231 F20 74.4(9) . . . . ? C228 C229 C232 F23 158.8(4) . . . . ? C230 C229 C232 F23 -21.7(6) . . . . ? C332 C229 C232 F23 -54(9) . . . . ? C228 C229 C232 F24 -74.5(5) . . . . ? C230 C229 C232 F24 105.0(5) . . . . ? C332 C229 C232 F24 72(9) . . . . ? C228 C229 C232 F22 40.6(5) . . . . ? C230 C229 C232 F22 -139.9(4) . . . . ? C332 C229 C232 F22 -172(9) . . . . ? C228 C229 C332 F124 102.3(10) . . . . ? C230 C229 C332 F124 -79.6(10) . . . . ? C232 C229 C332 F124 69(9) . . . . ? C228 C229 C332 F122 -138.9(9) . . . . ? C230 C229 C332 F122 39.2(10) . . . . ? C232 C229 C332 F122 -173(9) . . . . ? C228 C229 C332 F123 -19.8(11) . . . . ? C230 C229 C332 F123 158.3(9) . . . . ? C232 C229 C332 F123 -54(8) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.660 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.069 _database_code_depnum_ccdc_archive 'CCDC 926701'