Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Jimenez, M. Victoria' 'Perez-Torrente, Jesus J.' _publ_contact_author_name 'Jimenez, M. Victoria' _publ_contact_author_email vjimenez@unizar.es _publ_section_title ; Rational Design of Efficient Rhodium Catalysts for the Anti-Markovni-kov Oxidative Amination of Styrene ; # Attachment 'Compnd-4.cif.txt' data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 770962' #TrackingRef 'Compnd-4.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H42 O2 P2 Rh, F6 P' _chemical_formula_sum 'C34 H42 F6 O2 P3 Rh' _chemical_formula_weight 792.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.813(2) _cell_length_b 17.919(2) _cell_length_c 20.796(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7010.4(14) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6872 _cell_measurement_theta_min 2.273 _cell_measurement_theta_max 25.070 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3248 _exptl_absorpt_coefficient_mu 0.686 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8576 _exptl_absorpt_correction_T_max 0.9548 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within SAINT+ package, v. 6.45. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 60267 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.02 _reflns_number_total 7662 _reflns_number_gt 6198 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.45 (Bruker AXS, 2003)' _computing_data_reduction 'SAINT+ v. 6.45 (Bruker AXS, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, SHELXTLv6.12, BrukerAXS' _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. All non-hydrogen atoms were refined with anisotropic displacement parameters, except four disordered fluorine atoms of the PF6 counteranion; these were were refined with isotropic displacement parameters and complementary occupancy factors (0.549(8)) Hydrogen atoms were included in observed positions and refined as free isotropic atoms. ; _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^)+(0.0515P)^2^+15.8200P] 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 7662 _refine_ls_number_parameters 562 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1301 _refine_ls_wR_factor_gt 0.1225 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.022 _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 Rh Rh 0.109215(15) 0.260101(16) 0.050032(15) 0.01808(10) Uani 1 1 d . . . P1 P 0.07804(5) 0.14602(5) 0.02844(5) 0.0188(2) Uani 1 1 d . . . P2 P 0.19124(5) 0.27336(6) -0.02369(5) 0.0194(2) Uani 1 1 d . . . C1 C -0.0193(2) 0.1378(2) 0.0367(2) 0.0227(9) Uani 1 1 d . . . H1A H -0.034(2) 0.168(3) 0.004(2) 0.030(13) Uiso 1 1 d . . . H1B H -0.034(2) 0.085(2) 0.027(2) 0.022(11) Uiso 1 1 d . . . C2 C -0.0493(2) 0.1621(2) 0.1019(2) 0.0252(9) Uani 1 1 d . . . H2A H -0.099(3) 0.158(3) 0.102(2) 0.039(14) Uiso 1 1 d . . . H2B H -0.031(2) 0.134(2) 0.137(2) 0.020(11) Uiso 1 1 d . . . C3 C -0.0387(2) 0.2436(2) 0.1185(2) 0.0269(9) Uani 1 1 d . . . H3A H -0.054(3) 0.275(3) 0.084(2) 0.035(13) Uiso 1 1 d . . . H3B H -0.066(2) 0.255(2) 0.154(2) 0.020(11) Uiso 1 1 d . . . C6 C 0.2603(2) 0.3378(2) 0.0064(2) 0.0244(9) Uani 1 1 d . . . H6A H 0.296(2) 0.344(2) -0.028(2) 0.017(10) Uiso 1 1 d . . . H6B H 0.285(2) 0.317(2) 0.040(2) 0.013(10) Uiso 1 1 d . . . C7 C 0.2330(2) 0.4142(2) 0.0264(2) 0.0266(9) Uani 1 1 d . . . H7A H 0.210(2) 0.440(2) -0.009(2) 0.016(10) Uiso 1 1 d . . . H7B H 0.270(3) 0.446(3) 0.036(2) 0.038(14) Uiso 1 1 d . . . C8 C 0.1867(2) 0.4136(3) 0.0861(2) 0.0285(10) Uani 1 1 d . . . H8A H 0.210(2) 0.386(2) 0.120(2) 0.022(11) Uiso 1 1 d . . . H8B H 0.174(2) 0.466(2) 0.0988(19) 0.016(10) Uiso 1 1 d . . . O1 O 0.03537(14) 0.26322(15) 0.13021(14) 0.0242(6) Uani 1 1 d . . . O2 O 0.11903(15) 0.37688(15) 0.07550(15) 0.0262(6) Uani 1 1 d . . . C4 C 0.0607(3) 0.2370(3) 0.1921(2) 0.0285(10) Uani 1 1 d . . . H4A H 0.025(2) 0.253(2) 0.217(2) 0.020(11) Uiso 1 1 d . . . H4B H 0.062(2) 0.181(3) 0.190(2) 0.026(12) Uiso 1 1 d . . . C5 C 0.1317(3) 0.2718(3) 0.2061(2) 0.0299(10) Uani 1 1 d . . . H5A H 0.127(3) 0.321(3) 0.208(2) 0.038(14) Uiso 1 1 d . . . H5B H 0.152(2) 0.259(2) 0.246(2) 0.029(13) Uiso 1 1 d . . . H5C H 0.164(2) 0.257(2) 0.174(2) 0.017(10) Uiso 1 1 d . . . C9 C 0.0636(3) 0.4249(3) 0.0527(3) 0.0458(14) Uani 1 1 d . . . H9A H 0.083(3) 0.456(3) 0.016(3) 0.065(19) Uiso 1 1 d . . . H9B H 0.028(3) 0.392(3) 0.035(3) 0.048(16) Uiso 1 1 d . . . C10 C 0.0341(3) 0.4729(4) 0.1033(4) 0.077(2) Uani 1 1 d . . . H10A H 0.0275 0.4437 0.1427 0.050 Uiso 1 1 calc . . . H10B H -0.0118 0.4930 0.0893 0.050 Uiso 1 1 calc . . . H10C H 0.0670 0.5142 0.1119 0.050 Uiso 1 1 calc . . . C11 C 0.1122(2) 0.0745(2) 0.0834(2) 0.0212(8) Uani 1 1 d . . . C12 C 0.0781(2) 0.0067(2) 0.0943(2) 0.0255(9) Uani 1 1 d . . . H12 H 0.036(3) -0.004(3) 0.073(2) 0.033(13) Uiso 1 1 d . . . C13 C 0.1074(2) -0.0457(3) 0.1353(2) 0.0303(10) Uani 1 1 d . . . H13 H 0.085(2) -0.090(3) 0.141(2) 0.024(11) Uiso 1 1 d . . . C14 C 0.1709(2) -0.0315(3) 0.1659(2) 0.0288(10) Uani 1 1 d . . . H14 H 0.191(3) -0.067(3) 0.193(2) 0.038(14) Uiso 1 1 d . . . C15 C 0.2053(2) 0.0357(3) 0.1557(2) 0.0276(9) Uani 1 1 d . . . H15 H 0.247(3) 0.044(3) 0.177(2) 0.032(13) Uiso 1 1 d . . . C16 C 0.1763(2) 0.0887(2) 0.1151(2) 0.0217(8) Uani 1 1 d . . . H16 H 0.196(2) 0.136(3) 0.111(2) 0.029(12) Uiso 1 1 d . . . C17 C 0.0909(2) 0.1051(2) -0.0514(2) 0.0212(8) Uani 1 1 d . . . C18 C 0.1326(2) 0.0422(2) -0.0619(2) 0.0259(9) Uani 1 1 d . . . H18 H 0.156(2) 0.020(2) -0.028(2) 0.017(11) Uiso 1 1 d . . . C19 C 0.1402(2) 0.0132(3) -0.1234(2) 0.0312(10) Uani 1 1 d . . . H19 H 0.167(3) -0.027(3) -0.132(2) 0.039(14) Uiso 1 1 d . . . C20 C 0.1062(3) 0.0459(3) -0.1742(2) 0.0334(10) Uani 1 1 d . . . H20 H 0.113(3) 0.030(3) -0.212(3) 0.041(15) Uiso 1 1 d . . . C21 C 0.0649(3) 0.1092(3) -0.1651(2) 0.0315(10) Uani 1 1 d . . . H21 H 0.043(2) 0.131(2) -0.199(2) 0.022(12) Uiso 1 1 d . . . C22 C 0.0574(2) 0.1387(2) -0.1039(2) 0.0232(9) Uani 1 1 d . . . H22 H 0.029(2) 0.184(2) -0.100(2) 0.024(11) Uiso 1 1 d . . . C23 C 0.2482(2) 0.1972(2) -0.0517(2) 0.0233(8) Uani 1 1 d . . . C24 C 0.2926(2) 0.1631(3) -0.0070(3) 0.0289(10) Uani 1 1 d . . . H24 H 0.291(2) 0.179(3) 0.030(2) 0.025(13) Uiso 1 1 d . . . C25 C 0.3374(2) 0.1055(3) -0.0251(3) 0.0350(11) Uani 1 1 d . . . H25 H 0.3678 0.0829 0.0057 0.050(16) Uiso 1 1 calc R . . C26 C 0.3377(3) 0.0811(3) -0.0881(3) 0.0382(12) Uani 1 1 d . . . H26 H 0.368(2) 0.039(3) -0.099(2) 0.024(11) Uiso 1 1 d . . . C27 C 0.2948(3) 0.1146(3) -0.1325(3) 0.0356(11) Uani 1 1 d . . . H27 H 0.296(3) 0.101(3) -0.175(3) 0.037(14) Uiso 1 1 d . . . C28 C 0.2497(3) 0.1723(3) -0.1147(2) 0.0300(10) Uani 1 1 d . . . H28 H 0.221(2) 0.193(3) -0.142(2) 0.024(12) Uiso 1 1 d . . . C29 C 0.1630(2) 0.3220(2) -0.0964(2) 0.0218(8) Uani 1 1 d . . . C30 C 0.2120(2) 0.3507(3) -0.1403(2) 0.0305(10) Uani 1 1 d . . . H30 H 0.2613 0.3407 -0.1351 0.037(14) Uiso 1 1 calc R . . C31 C 0.1889(3) 0.3938(3) -0.1914(2) 0.0373(12) Uani 1 1 d . . . H31 H 0.220(3) 0.411(3) -0.219(3) 0.057(18) Uiso 1 1 d . . . C32 C 0.1177(3) 0.4071(3) -0.2008(2) 0.0339(11) Uani 1 1 d . . . H32 H 0.102(3) 0.437(3) -0.233(3) 0.043(15) Uiso 1 1 d . . . C33 C 0.0684(3) 0.3773(2) -0.1590(2) 0.0304(10) Uani 1 1 d . . . H33 H 0.021(2) 0.387(2) -0.167(2) 0.021(11) Uiso 1 1 d . . . C34 C 0.0908(2) 0.3358(2) -0.1063(2) 0.0238(9) Uani 1 1 d . . . H34 H 0.058(3) 0.319(3) -0.077(2) 0.029(13) Uiso 1 1 d . . . P3 P 0.86620(6) 0.21756(8) 0.31090(6) 0.0330(3) Uani 1 1 d . . . F1 F 0.91575(19) 0.16698(19) 0.26725(17) 0.0604(9) Uani 1 1 d . A . F2 F 0.8156(2) 0.2671(3) 0.35399(19) 0.0873(14) Uani 1 1 d . A . F3A F 0.8201(5) 0.2307(5) 0.2467(5) 0.075(3) Uiso 0.451(8) 1 d P A 1 F4A F 0.9130(5) 0.2876(5) 0.2860(4) 0.071(3) Uiso 0.451(8) 1 d P A 1 F5A F 0.9165(5) 0.2163(6) 0.3722(5) 0.069(3) Uiso 0.451(8) 1 d P A 1 F6A F 0.8158(6) 0.1582(6) 0.3329(5) 0.086(3) Uiso 0.451(8) 1 d P A 1 F3B F 0.7997(4) 0.1857(4) 0.2708(4) 0.073(2) Uiso 0.549(8) 1 d P A 2 F4B F 0.8673(4) 0.2860(4) 0.2651(4) 0.066(2) Uiso 0.549(8) 1 d P A 2 F5B F 0.9314(5) 0.2453(5) 0.3473(4) 0.081(3) Uiso 0.549(8) 1 d P A 2 F6B F 0.8610(4) 0.1425(4) 0.3560(3) 0.060(2) Uiso 0.549(8) 1 d P A 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 Rh 0.01655(15) 0.01806(15) 0.01964(17) 0.00066(12) 0.00176(12) -0.00102(11) P1 0.0169(5) 0.0192(5) 0.0203(5) 0.0015(4) 0.0003(4) -0.0008(4) P2 0.0180(5) 0.0211(5) 0.0192(5) 0.0012(4) 0.0004(4) -0.0012(4) C1 0.0164(19) 0.026(2) 0.026(2) 0.0018(17) 0.0007(16) -0.0035(15) C2 0.0142(19) 0.030(2) 0.031(3) 0.0018(19) 0.0015(18) -0.0022(16) C3 0.021(2) 0.031(2) 0.029(2) 0.0006(19) 0.0031(18) 0.0021(17) C6 0.019(2) 0.032(2) 0.022(2) 0.0043(18) -0.0025(18) -0.0060(16) C7 0.027(2) 0.028(2) 0.025(2) 0.0019(18) -0.0037(19) -0.0083(18) C8 0.027(2) 0.027(2) 0.032(3) -0.0016(19) -0.0009(19) -0.0081(17) O1 0.0202(14) 0.0268(14) 0.0256(16) 0.0000(12) 0.0034(12) -0.0007(11) O2 0.0217(15) 0.0225(14) 0.0346(17) -0.0025(12) 0.0011(13) -0.0019(11) C4 0.030(2) 0.034(2) 0.022(2) -0.0009(19) 0.0049(18) -0.0074(19) C5 0.029(2) 0.037(3) 0.024(3) -0.003(2) -0.001(2) -0.0036(19) C9 0.032(3) 0.026(2) 0.079(5) -0.001(3) -0.010(3) 0.001(2) C10 0.042(3) 0.055(4) 0.133(7) -0.042(4) -0.004(4) 0.012(3) C11 0.0206(19) 0.0202(18) 0.023(2) -0.0002(15) 0.0005(17) 0.0026(15) C12 0.024(2) 0.026(2) 0.026(2) 0.0009(17) -0.0007(18) -0.0026(17) C13 0.031(2) 0.030(2) 0.030(3) 0.0077(18) 0.006(2) -0.0003(19) C14 0.032(2) 0.035(2) 0.019(2) 0.0054(18) 0.0009(18) 0.0093(19) C15 0.024(2) 0.036(2) 0.022(2) -0.0041(18) 0.0000(18) 0.0072(18) C16 0.023(2) 0.024(2) 0.018(2) -0.0019(16) 0.0017(16) -0.0001(16) C17 0.0195(19) 0.0210(18) 0.023(2) 0.0002(16) 0.0007(16) -0.0037(14) C18 0.023(2) 0.026(2) 0.029(3) 0.0033(18) 0.0029(18) -0.0002(16) C19 0.031(2) 0.027(2) 0.036(3) -0.0032(19) 0.011(2) -0.0017(18) C20 0.039(3) 0.034(2) 0.027(3) -0.005(2) 0.008(2) -0.006(2) C21 0.033(2) 0.038(3) 0.024(3) 0.005(2) -0.004(2) -0.0077(19) C22 0.0203(19) 0.028(2) 0.021(2) 0.0030(17) 0.0020(17) -0.0030(16) C23 0.0189(19) 0.0224(19) 0.028(2) 0.0031(17) 0.0057(17) -0.0028(15) C24 0.025(2) 0.031(2) 0.031(3) 0.006(2) 0.007(2) 0.0030(17) C25 0.027(2) 0.030(2) 0.048(3) 0.009(2) 0.004(2) 0.0025(18) C26 0.028(2) 0.029(2) 0.058(4) -0.003(2) 0.011(2) 0.0032(19) C27 0.034(3) 0.035(2) 0.038(3) -0.013(2) 0.014(2) -0.003(2) C28 0.029(2) 0.035(2) 0.027(3) 0.000(2) 0.003(2) 0.0001(19) C29 0.024(2) 0.0220(19) 0.019(2) -0.0020(16) -0.0027(17) -0.0029(15) C30 0.029(2) 0.039(2) 0.024(2) 0.0054(19) -0.0003(19) -0.0052(19) C31 0.046(3) 0.043(3) 0.023(3) 0.009(2) -0.001(2) -0.013(2) C32 0.052(3) 0.027(2) 0.023(2) 0.0034(18) -0.008(2) 0.001(2) C33 0.037(3) 0.025(2) 0.029(3) -0.0051(18) -0.009(2) 0.0054(18) C34 0.022(2) 0.024(2) 0.025(2) -0.0027(17) -0.0023(18) 0.0000(16) P3 0.0237(6) 0.0455(7) 0.0299(7) -0.0062(5) 0.0049(5) -0.0050(5) F1 0.064(2) 0.058(2) 0.060(2) -0.0084(17) 0.0207(18) 0.0086(17) F2 0.076(3) 0.126(4) 0.060(3) -0.028(2) 0.019(2) 0.038(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh O2 2.166(3) . ? Rh O1 2.171(3) . ? Rh P1 2.1735(10) . ? Rh P2 2.1880(11) . ? P1 C17 1.832(4) . ? P1 C11 1.834(4) . ? P1 C1 1.846(4) . ? P2 C29 1.824(4) . ? P2 C23 1.831(4) . ? P2 C6 1.848(4) . ? C1 C2 1.530(6) . ? C1 H1A 0.90(5) . ? C1 H1B 1.01(4) . ? C2 C3 1.515(6) . ? C2 H2A 0.94(5) . ? C2 H2B 0.95(4) . ? C3 O1 1.457(5) . ? C3 H3A 0.96(5) . ? C3 H3B 0.93(5) . ? C6 C7 1.519(6) . ? C6 H6A 0.98(4) . ? C6 H6B 0.92(4) . ? C7 C8 1.517(6) . ? C7 H7A 0.97(4) . ? C7 H7B 0.92(5) . ? C8 O2 1.449(5) . ? C8 H8A 0.96(4) . ? C8 H8B 1.01(4) . ? O1 C4 1.451(5) . ? O2 C9 1.433(6) . ? C4 C5 1.503(6) . ? C4 H4A 0.90(5) . ? C4 H4B 1.01(5) . ? C5 H5A 0.89(5) . ? C5 H5B 0.95(5) . ? C5 H5C 0.95(5) . ? C9 C10 1.469(9) . ? C9 H9A 1.02(6) . ? C9 H9B 0.96(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.392(6) . ? C11 C16 1.396(6) . ? C12 C13 1.383(6) . ? C12 H12 0.92(5) . ? C13 C14 1.378(7) . ? C13 H13 0.90(5) . ? C14 C15 1.383(6) . ? C14 H14 0.92(5) . ? C15 C16 1.384(6) . ? C15 H15 0.91(5) . ? C16 H16 0.93(5) . ? C17 C18 1.390(6) . ? C17 C22 1.396(6) . ? C18 C19 1.389(6) . ? C18 H18 0.91(4) . ? C19 C20 1.368(7) . ? C19 H19 0.90(5) . ? C20 C21 1.388(7) . ? C20 H20 0.84(5) . ? C21 C22 1.385(6) . ? C21 H21 0.90(4) . ? C22 H22 0.97(4) . ? C23 C28 1.383(6) . ? C23 C24 1.391(6) . ? C24 C25 1.384(6) . ? C24 H24 0.82(5) . ? C25 C26 1.380(7) . ? C25 H25 0.9500 . ? C26 C27 1.366(7) . ? C26 H26 0.97(5) . ? C27 C28 1.388(6) . ? C27 H27 0.92(5) . ? C28 H28 0.86(5) . ? C29 C30 1.396(6) . ? C29 C34 1.396(6) . ? C30 C31 1.383(6) . ? C30 H30 0.9500 . ? C31 C32 1.375(7) . ? C31 H31 0.87(6) . ? C32 C33 1.379(7) . ? C32 H32 0.91(5) . ? C33 C34 1.389(6) . ? C33 H33 0.92(4) . ? C34 H34 0.91(5) . ? P3 F6A 1.496(10) . ? P3 F5B 1.524(9) . ? P3 F4B 1.553(7) . ? P3 F2 1.580(4) . ? P3 F1 1.586(3) . ? P3 F5A 1.588(9) . ? P3 F3B 1.608(8) . ? P3 F3A 1.610(10) . ? P3 F4A 1.618(9) . ? P3 F6B 1.642(7) . ? 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 O2 Rh O1 80.90(11) . . ? O2 Rh P1 169.09(8) . . ? O1 Rh P1 90.58(8) . . ? O2 Rh P2 90.36(8) . . ? O1 Rh P2 170.60(8) . . ? P1 Rh P2 98.49(4) . . ? C17 P1 C11 103.80(18) . . ? C17 P1 C1 100.61(19) . . ? C11 P1 C1 103.55(19) . . ? C17 P1 Rh 121.88(13) . . ? C11 P1 Rh 115.73(13) . . ? C1 P1 Rh 108.87(14) . . ? C29 P2 C23 105.23(19) . . ? C29 P2 C6 100.77(19) . . ? C23 P2 C6 99.35(19) . . ? C29 P2 Rh 115.29(14) . . ? C23 P2 Rh 123.71(13) . . ? C6 P2 Rh 109.04(15) . . ? C2 C1 P1 115.2(3) . . ? C2 C1 H1A 113(3) . . ? P1 C1 H1A 100(3) . . ? C2 C1 H1B 110(2) . . ? P1 C1 H1B 109(2) . . ? H1A C1 H1B 109(4) . . ? C3 C2 C1 115.3(4) . . ? C3 C2 H2A 102(3) . . ? C1 C2 H2A 110(3) . . ? C3 C2 H2B 107(3) . . ? C1 C2 H2B 113(3) . . ? H2A C2 H2B 109(4) . . ? O1 C3 C2 113.3(3) . . ? O1 C3 H3A 105(3) . . ? C2 C3 H3A 111(3) . . ? O1 C3 H3B 110(3) . . ? C2 C3 H3B 109(3) . . ? H3A C3 H3B 108(4) . . ? C7 C6 P2 114.7(3) . . ? C7 C6 H6A 109(2) . . ? P2 C6 H6A 108(2) . . ? C7 C6 H6B 110(3) . . ? P2 C6 H6B 111(3) . . ? H6A C6 H6B 105(3) . . ? C8 C7 C6 114.3(4) . . ? C8 C7 H7A 112(2) . . ? C6 C7 H7A 112(2) . . ? C8 C7 H7B 105(3) . . ? C6 C7 H7B 111(3) . . ? H7A C7 H7B 102(4) . . ? O2 C8 C7 112.5(4) . . ? O2 C8 H8A 107(3) . . ? C7 C8 H8A 110(3) . . ? O2 C8 H8B 105(2) . . ? C7 C8 H8B 110(2) . . ? H8A C8 H8B 113(3) . . ? C4 O1 C3 112.6(3) . . ? C4 O1 Rh 117.6(2) . . ? C3 O1 Rh 118.5(3) . . ? C9 O2 C8 114.6(3) . . ? C9 O2 Rh 115.9(3) . . ? C8 O2 Rh 123.4(2) . . ? O1 C4 C5 109.2(4) . . ? O1 C4 H4A 99(3) . . ? C5 C4 H4A 115(3) . . ? O1 C4 H4B 107(3) . . ? C5 C4 H4B 113(3) . . ? H4A C4 H4B 112(4) . . ? C4 C5 H5A 110(3) . . ? C4 C5 H5B 115(3) . . ? H5A C5 H5B 104(4) . . ? C4 C5 H5C 109(3) . . ? H5A C5 H5C 112(4) . . ? H5B C5 H5C 108(4) . . ? O2 C9 C10 112.9(5) . . ? O2 C9 H9A 108(3) . . ? C10 C9 H9A 111(3) . . ? O2 C9 H9B 106(3) . . ? C10 C9 H9B 111(3) . . ? H9A C9 H9B 108(5) . . ? 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 . . ? C12 C11 C16 118.7(4) . . ? C12 C11 P1 123.3(3) . . ? C16 C11 P1 117.9(3) . . ? C13 C12 C11 120.6(4) . . ? C13 C12 H12 119(3) . . ? C11 C12 H12 120(3) . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H13 120(3) . . ? C12 C13 H13 120(3) . . ? C13 C14 C15 119.8(4) . . ? C13 C14 H14 120(3) . . ? C15 C14 H14 120(3) . . ? C16 C15 C14 120.4(4) . . ? C16 C15 H15 122(3) . . ? C14 C15 H15 118(3) . . ? C15 C16 C11 120.2(4) . . ? C15 C16 H16 122(3) . . ? C11 C16 H16 118(3) . . ? C18 C17 C22 118.9(4) . . ? C18 C17 P1 122.7(3) . . ? C22 C17 P1 118.4(3) . . ? C19 C18 C17 120.4(4) . . ? C19 C18 H18 120(3) . . ? C17 C18 H18 120(3) . . ? C20 C19 C18 120.2(4) . . ? C20 C19 H19 117(3) . . ? C18 C19 H19 123(3) . . ? C19 C20 C21 120.5(5) . . ? C19 C20 H20 121(4) . . ? C21 C20 H20 119(4) . . ? C22 C21 C20 119.6(5) . . ? C22 C21 H21 120(3) . . ? C20 C21 H21 120(3) . . ? C21 C22 C17 120.5(4) . . ? C21 C22 H22 116(3) . . ? C17 C22 H22 123(3) . . ? C28 C23 C24 118.6(4) . . ? C28 C23 P2 123.6(3) . . ? C24 C23 P2 117.8(3) . . ? C25 C24 C23 120.8(5) . . ? C25 C24 H24 123(3) . . ? C23 C24 H24 117(3) . . ? C26 C25 C24 119.8(5) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C27 C26 C25 119.9(4) . . ? C27 C26 H26 122(3) . . ? C25 C26 H26 118(3) . . ? C26 C27 C28 120.6(5) . . ? C26 C27 H27 121(3) . . ? C28 C27 H27 118(3) . . ? C23 C28 C27 120.3(5) . . ? C23 C28 H28 118(3) . . ? C27 C28 H28 122(3) . . ? C30 C29 C34 118.7(4) . . ? C30 C29 P2 121.8(3) . . ? C34 C29 P2 119.4(3) . . ? C31 C30 C29 120.1(4) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C30 120.8(5) . . ? C32 C31 H31 120(4) . . ? C30 C31 H31 120(4) . . ? C31 C32 C33 119.9(4) . . ? C31 C32 H32 122(3) . . ? C33 C32 H32 118(3) . . ? C32 C33 C34 120.0(4) . . ? C32 C33 H33 118(3) . . ? C34 C33 H33 122(3) . . ? C33 C34 C29 120.4(4) . . ? C33 C34 H34 119(3) . . ? C29 C34 H34 120(3) . . ? F6A P3 F5B 126.1(6) . . ? F6A P3 F4B 139.2(5) . . ? F5B P3 F4B 92.1(4) . . ? F6A P3 F2 81.1(4) . . ? F5B P3 F2 91.1(4) . . ? F4B P3 F2 85.0(3) . . ? F6A P3 F1 98.1(4) . . ? F5B P3 F1 89.9(4) . . ? F4B P3 F1 95.3(3) . . ? F2 P3 F1 179.0(2) . . ? F6A P3 F5A 97.0(6) . . ? F4B P3 F5A 119.7(5) . . ? F2 P3 F5A 84.9(4) . . ? F1 P3 F5A 95.8(4) . . ? F6A P3 F3B 54.1(5) . . ? F5B P3 F3B 177.5(4) . . ? F4B P3 F3B 88.4(4) . . ? F2 P3 F3B 91.4(3) . . ? F1 P3 F3B 87.6(3) . . ? F5A P3 F3B 151.0(5) . . ? F6A P3 F3A 90.9(5) . . ? F5B P3 F3A 142.9(5) . . ? F4B P3 F3A 51.9(4) . . ? F2 P3 F3A 93.6(4) . . ? F1 P3 F3A 85.8(4) . . ? F5A P3 F3A 171.6(5) . . ? F6A P3 F4A 173.6(5) . . ? F5B P3 F4A 57.9(5) . . ? F2 P3 F4A 94.2(4) . . ? F1 P3 F4A 86.6(4) . . ? F5A P3 F4A 86.8(5) . . ? F3B P3 F4A 122.1(5) . . ? F3A P3 F4A 85.1(5) . . ? F5B P3 F6B 91.8(4) . . ? F4B P3 F6B 176.0(4) . . ? F2 P3 F6B 95.8(3) . . ? F1 P3 F6B 83.9(3) . . ? F5A P3 F6B 64.3(4) . . ? F3B P3 F6B 87.7(4) . . ? F3A P3 F6B 124.1(4) . . ? F4A P3 F6B 148.3(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Rh P1 C17 119.3(5) . . . . ? O1 Rh P1 C17 157.77(17) . . . . ? P2 Rh P1 C17 -24.68(16) . . . . ? O2 Rh P1 C11 -113.0(5) . . . . ? O1 Rh P1 C11 -74.53(16) . . . . ? P2 Rh P1 C11 103.03(15) . . . . ? O2 Rh P1 C1 3.0(5) . . . . ? O1 Rh P1 C1 41.56(17) . . . . ? P2 Rh P1 C1 -140.89(16) . . . . ? O2 Rh P2 C29 -74.82(16) . . . . ? P1 Rh P2 C29 98.78(14) . . . . ? O2 Rh P2 C23 153.54(19) . . . . ? P1 Rh P2 C23 -32.86(17) . . . . ? O2 Rh P2 C6 37.63(17) . . . . ? P1 Rh P2 C6 -148.77(15) . . . . ? C17 P1 C1 C2 175.6(3) . . . . ? C11 P1 C1 C2 68.4(3) . . . . ? Rh P1 C1 C2 -55.3(3) . . . . ? P1 C1 C2 C3 63.3(5) . . . . ? C1 C2 C3 O1 -68.4(5) . . . . ? C29 P2 C6 C7 64.8(4) . . . . ? C23 P2 C6 C7 172.3(3) . . . . ? Rh P2 C6 C7 -57.0(3) . . . . ? P2 C6 C7 C8 68.5(5) . . . . ? C6 C7 C8 O2 -68.3(5) . . . . ? C2 C3 O1 C4 -75.0(5) . . . . ? C2 C3 O1 Rh 67.8(4) . . . . ? O2 Rh O1 C4 -99.3(3) . . . . ? P1 Rh O1 C4 87.6(3) . . . . ? O2 Rh O1 C3 119.7(3) . . . . ? P1 Rh O1 C3 -53.4(3) . . . . ? C7 C8 O2 C9 -88.8(5) . . . . ? C7 C8 O2 Rh 62.6(5) . . . . ? O1 Rh O2 C9 -79.8(4) . . . . ? P1 Rh O2 C9 -40.7(7) . . . . ? P2 Rh O2 C9 103.7(4) . . . . ? O1 Rh O2 C8 129.1(3) . . . . ? P1 Rh O2 C8 168.2(4) . . . . ? P2 Rh O2 C8 -47.4(3) . . . . ? C3 O1 C4 C5 -168.9(4) . . . . ? Rh O1 C4 C5 47.9(4) . . . . ? C8 O2 C9 C10 -75.8(6) . . . . ? Rh O2 C9 C10 130.6(4) . . . . ? C17 P1 C11 C12 -70.5(4) . . . . ? C1 P1 C11 C12 34.2(4) . . . . ? Rh P1 C11 C12 153.3(3) . . . . ? C17 P1 C11 C16 108.7(3) . . . . ? C1 P1 C11 C16 -146.6(3) . . . . ? Rh P1 C11 C16 -27.5(4) . . . . ? C16 C11 C12 C13 -0.6(6) . . . . ? P1 C11 C12 C13 178.6(3) . . . . ? C11 C12 C13 C14 0.0(7) . . . . ? C12 C13 C14 C15 0.3(7) . . . . ? C13 C14 C15 C16 0.1(7) . . . . ? C14 C15 C16 C11 -0.7(6) . . . . ? C12 C11 C16 C15 1.0(6) . . . . ? P1 C11 C16 C15 -178.3(3) . . . . ? C11 P1 C17 C18 -12.8(4) . . . . ? C1 P1 C17 C18 -119.8(4) . . . . ? Rh P1 C17 C18 120.0(3) . . . . ? C11 P1 C17 C22 167.3(3) . . . . ? C1 P1 C17 C22 60.3(3) . . . . ? Rh P1 C17 C22 -59.9(3) . . . . ? C22 C17 C18 C19 -0.5(6) . . . . ? P1 C17 C18 C19 179.6(3) . . . . ? C17 C18 C19 C20 -0.6(7) . . . . ? C18 C19 C20 C21 1.3(7) . . . . ? C19 C20 C21 C22 -0.9(7) . . . . ? C20 C21 C22 C17 -0.2(6) . . . . ? C18 C17 C22 C21 0.9(6) . . . . ? P1 C17 C22 C21 -179.2(3) . . . . ? C29 P2 C23 C28 -16.6(4) . . . . ? C6 P2 C23 C28 -120.5(4) . . . . ? Rh P2 C23 C28 119.0(3) . . . . ? C29 P2 C23 C24 162.9(3) . . . . ? C6 P2 C23 C24 59.0(4) . . . . ? Rh P2 C23 C24 -61.5(4) . . . . ? C28 C23 C24 C25 0.0(6) . . . . ? P2 C23 C24 C25 -179.5(3) . . . . ? C23 C24 C25 C26 -0.6(7) . . . . ? C24 C25 C26 C27 1.1(7) . . . . ? C25 C26 C27 C28 -1.2(7) . . . . ? C24 C23 C28 C27 -0.1(6) . . . . ? P2 C23 C28 C27 179.5(3) . . . . ? C26 C27 C28 C23 0.6(7) . . . . ? C23 P2 C29 C30 -56.1(4) . . . . ? C6 P2 C29 C30 46.8(4) . . . . ? Rh P2 C29 C30 164.0(3) . . . . ? C23 P2 C29 C34 128.7(3) . . . . ? C6 P2 C29 C34 -128.4(3) . . . . ? Rh P2 C29 C34 -11.2(4) . . . . ? C34 C29 C30 C31 1.8(7) . . . . ? P2 C29 C30 C31 -173.4(4) . . . . ? C29 C30 C31 C32 -1.9(7) . . . . ? C30 C31 C32 C33 0.0(8) . . . . ? C31 C32 C33 C34 2.0(7) . . . . ? C32 C33 C34 C29 -2.0(6) . . . . ? C30 C29 C34 C33 0.1(6) . . . . ? P2 C29 C34 C33 175.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.863 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.107