# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Andrew Weller' 'Adrian B. Chaplin' 'Romaeo Dallanegra' 'Jennifer Tsim' _publ_contact_author_email ANDREW.WELLER@CHEM.OX.AC.UK _publ_section_title ; Amino-Borane Oligomers Bound to a Rh(I) Metal Fragment. ; # Attachment '3b.cif' data_3b _database_code_depnum_ccdc_archive 'CCDC 767949' #TrackingRef '3b.cif' #--------------------------------------- # [Rh(PiPr2Cyp')(BH3NMe2BH2NMe2H)]BArF4 #--------------------------------------- # start Validation Reply Form _vrf_PLAT301_3b ; PROBLEM: Note Main Residue Disorder .................... 24.00 Perc. RESPONSE: The structure contains a significant degree of disorder. See details in supplementary information or _refine_special_details. ; _vrf_PLAT605_3b ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 398.00 A**3 RESPONSE: Problematic solvent disorder in the solution was treated using the SQUEEZE algorithm. See _platon_squeeze for details. ; # end Validation Reply Form #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic . _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety 'C32 H12 B F24, C15 H39 B2 N2 P Rh' _chemical_formula_sum 'C47 H51 B3 F24 N2 P Rh' _chemical_formula_weight 1266.21 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' N N 0.0061 0.0033 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.11340(10) _cell_length_b 15.09320(10) _cell_length_c 15.6507(2) _cell_angle_alpha 84.6142(4) _cell_angle_beta 78.4318(4) _cell_angle_gamma 86.9282(4) _cell_volume 3019.40(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13406 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 0.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.935 _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 'horizonally mounted graphite crystal' _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 23676 _diffrn_reflns_av_R_equivalents 0.0154 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12244 _reflns_number_gt 10413 _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 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Solved with sir2004. H1A, H1B, H1C, H2A, H2B, H7 and H8 were located on the Fourier difference map; their isotropic displacement parameters were fixed to ride on the parent atoms. C7-H7 and C8-H8 were restrained to equal length. Disorder of the phosphine ligand was treated by modelling the non-coordinated phosphine substituents over two sites and restraining their geometry. Rotational disorder of the CF3 groups of the anion was treated by modelling the fluorine atoms, or the entire CF3 group, over two sites and restraining their geometry. Problematic solvent disorder was treated using the SQUEEZE algorithm see #_platon_squeeze for details. Restraints to thermal parameters were applied where necessary in order to maintain sensible values. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.011 0.500 396 -10 ' ' _platon_squeeze_details ; ; _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^)+(0.0747P)^2^+2.7887P] 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 12244 _refine_ls_number_parameters 962 _refine_ls_number_restraints 982 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.346 _refine_ls_shift/su_max 0.008 _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 0.069870(19) 0.164707(17) 0.196373(19) 0.03466(11) Uani 1 1 d . A . B1 B 0.1066(3) 0.2608(3) 0.2859(4) 0.0512(12) Uani 1 1 d . . . H1A H 0.089(4) 0.182(3) 0.307(3) 0.061 Uiso 1 1 d . . . H1B H 0.138(4) 0.265(3) 0.207(3) 0.061 Uiso 1 1 d . . . H1C H 0.169(4) 0.280(3) 0.320(3) 0.061 Uiso 1 1 d . . . N1 N 0.0008(2) 0.3202(2) 0.3072(2) 0.0412(7) Uani 1 1 d . . . C1 C -0.0535(3) 0.2899(3) 0.3971(3) 0.0554(11) Uani 1 1 d . . . H1D H -0.0053 0.2901 0.4376 0.083 Uiso 1 1 calc R . . H1E H -0.0775 0.2294 0.3977 0.083 Uiso 1 1 calc R . . H1F H -0.1134 0.3302 0.4154 0.083 Uiso 1 1 calc R . . C2 C 0.0268(4) 0.4154(3) 0.3038(4) 0.0629(13) Uani 1 1 d . . . H2C H -0.0376 0.4521 0.3151 0.094 Uiso 1 1 calc R . . H2D H 0.0673 0.4340 0.2457 0.094 Uiso 1 1 calc R . . H2E H 0.0680 0.4228 0.3483 0.094 Uiso 1 1 calc R . . B2 B -0.0572(3) 0.3025(3) 0.2328(3) 0.0398(9) Uani 1 1 d . . . H2A H -0.064(3) 0.228(3) 0.235(3) 0.048 Uiso 1 1 d . . . H2B H -0.019(3) 0.338(3) 0.169(3) 0.048 Uiso 1 1 d . . . N2 N -0.1800(2) 0.3308(2) 0.2552(2) 0.0406(7) Uani 1 1 d . . . H2 H -0.1935 0.3507 0.3110 0.049 Uiso 1 1 calc R . . C3 C -0.2493(3) 0.2537(3) 0.2582(4) 0.0627(12) Uani 1 1 d . . . H3A H -0.3224 0.2744 0.2721 0.094 Uiso 1 1 calc R . . H3B H -0.2354 0.2077 0.3033 0.094 Uiso 1 1 calc R . . H3C H -0.2352 0.2289 0.2011 0.094 Uiso 1 1 calc R . . C4 C -0.2091(4) 0.4051(4) 0.1953(4) 0.0791(17) Uani 1 1 d . . . H4A H -0.1943 0.3872 0.1353 0.119 Uiso 1 1 calc R . . H4B H -0.1687 0.4571 0.1983 0.119 Uiso 1 1 calc R . . H4C H -0.2836 0.4202 0.2125 0.119 Uiso 1 1 calc R . . P1 P 0.21331(7) 0.08255(6) 0.15869(7) 0.0395(2) Uani 1 1 d D . . C5 C 0.1636(3) 0.0081(3) 0.0919(3) 0.0490(10) Uani 1 1 d . A . H5 H 0.2146 -0.0386 0.0665 0.059 Uiso 1 1 calc R . . C6 C 0.0634(3) -0.0276(3) 0.1528(4) 0.0556(11) Uani 1 1 d . . . H6A H 0.0318 -0.0733 0.1259 0.067 Uiso 1 1 calc R A . H6B H 0.0769 -0.0524 0.2105 0.067 Uiso 1 1 calc R . . C7 C -0.0041(3) 0.0575(3) 0.1601(3) 0.0484(10) Uani 1 1 d D A . H7 H -0.085(3) 0.057(3) 0.193(3) 0.058 Uiso 1 1 d D . . C8 C 0.0291(3) 0.1167(3) 0.0851(3) 0.0472(9) Uani 1 1 d D . . H8 H -0.024(3) 0.166(3) 0.062(3) 0.057 Uiso 1 1 d D . . C9 C 0.1191(3) 0.0716(3) 0.0250(3) 0.0530(10) Uani 1 1 d . A . H9A H 0.1708 0.1149 -0.0060 0.064 Uiso 1 1 calc R . . H9B H 0.0941 0.0387 -0.0183 0.064 Uiso 1 1 calc R . . C10 C 0.2583(6) 0.0151(4) 0.2488(4) 0.0621(16) Uani 0.769(6) 1 d PDU A 1 H10 H 0.1921 -0.0103 0.2833 0.075 Uiso 0.769(6) 1 calc PR A 1 C11 C 0.2946(6) 0.0673(5) 0.3154(5) 0.0756(18) Uani 0.769(6) 1 d PDU A 1 H11A H 0.2979 0.0281 0.3685 0.113 Uiso 0.769(6) 1 calc PR A 1 H11B H 0.2454 0.1173 0.3302 0.113 Uiso 0.769(6) 1 calc PR A 1 H11C H 0.3638 0.0900 0.2904 0.113 Uiso 0.769(6) 1 calc PR A 1 C12 C 0.3232(8) -0.0671(5) 0.2240(6) 0.078(2) Uani 0.769(6) 1 d PDU A 1 H12A H 0.3963 -0.0516 0.2047 0.116 Uiso 0.769(6) 1 calc PR A 1 H12B H 0.2990 -0.0922 0.1764 0.116 Uiso 0.769(6) 1 calc PR A 1 H12C H 0.3166 -0.1111 0.2748 0.116 Uiso 0.769(6) 1 calc PR A 1 C110 C 0.2877(14) 0.0199(13) 0.2341(9) 0.063(3) Uani 0.231(6) 1 d PDU A 2 H110 H 0.3438 0.0599 0.2400 0.076 Uiso 0.231(6) 1 calc PR A 2 C111 C 0.2205(17) 0.0047(14) 0.3259(7) 0.068(4) Uani 0.231(6) 1 d PDU A 2 H11D H 0.1631 -0.0336 0.3240 0.102 Uiso 0.231(6) 1 calc PR A 2 H11E H 0.1921 0.0621 0.3464 0.102 Uiso 0.231(6) 1 calc PR A 2 H11F H 0.2631 -0.0240 0.3660 0.102 Uiso 0.231(6) 1 calc PR A 2 C112 C 0.343(2) -0.0636(14) 0.1981(13) 0.056(4) Uani 0.231(6) 1 d PDU A 2 H11G H 0.3849 -0.0918 0.2393 0.084 Uiso 0.231(6) 1 calc PR A 2 H11H H 0.3891 -0.0477 0.1417 0.084 Uiso 0.231(6) 1 calc PR A 2 H11I H 0.2918 -0.1052 0.1900 0.084 Uiso 0.231(6) 1 calc PR A 2 C13 C 0.3187(3) 0.1454(3) 0.0808(3) 0.0332(10) Uani 0.769(6) 1 d PDU A 1 H13 H 0.2831 0.1850 0.0400 0.040 Uiso 0.769(6) 1 calc PR A 1 C14 C 0.3733(4) 0.2068(3) 0.1287(4) 0.0414(12) Uani 0.769(6) 1 d PDU A 1 H14A H 0.4152 0.1707 0.1652 0.062 Uiso 0.769(6) 1 calc PR A 1 H14B H 0.3209 0.2426 0.1657 0.062 Uiso 0.769(6) 1 calc PR A 1 H14C H 0.4185 0.2462 0.0857 0.062 Uiso 0.769(6) 1 calc PR A 1 C15 C 0.3959(4) 0.0858(4) 0.0240(4) 0.0427(13) Uani 0.769(6) 1 d PDU A 1 H15A H 0.4453 0.1227 -0.0179 0.064 Uiso 0.769(6) 1 calc PR A 1 H15B H 0.3582 0.0501 -0.0079 0.064 Uiso 0.769(6) 1 calc PR A 1 H15C H 0.4337 0.0462 0.0611 0.064 Uiso 0.769(6) 1 calc PR A 1 C113 C 0.3435(8) 0.1248(8) 0.1192(10) 0.042(2) Uani 0.231(6) 1 d PDU A 2 H113 H 0.3785 0.1188 0.1708 0.050 Uiso 0.231(6) 1 calc PR A 2 C114 C 0.3414(12) 0.2240(7) 0.0889(13) 0.053(3) Uani 0.231(6) 1 d PDU A 2 H11J H 0.4123 0.2423 0.0628 0.079 Uiso 0.231(6) 1 calc PR A 2 H11K H 0.3137 0.2583 0.1392 0.079 Uiso 0.231(6) 1 calc PR A 2 H11L H 0.2970 0.2352 0.0454 0.079 Uiso 0.231(6) 1 calc PR A 2 C115 C 0.4106(10) 0.0690(11) 0.0504(12) 0.044(4) Uani 0.231(6) 1 d PDU A 2 H11M H 0.3937 0.0870 -0.0071 0.066 Uiso 0.231(6) 1 calc PR A 2 H11N H 0.3965 0.0058 0.0661 0.066 Uiso 0.231(6) 1 calc PR A 2 H11O H 0.4844 0.0786 0.0483 0.066 Uiso 0.231(6) 1 calc PR A 2 B200 B 0.4611(3) 0.3256(2) 0.7774(2) 0.0242(6) Uani 1 1 d . . . C201 C 0.4502(2) 0.23626(19) 0.72816(19) 0.0251(6) Uani 1 1 d . . . C202 C 0.4008(2) 0.1602(2) 0.7717(2) 0.0282(6) Uani 1 1 d . . . H202 H 0.3658 0.1620 0.8309 0.034 Uiso 1 1 calc R . . C203 C 0.4012(3) 0.0816(2) 0.7309(2) 0.0329(7) Uani 1 1 d D B . C204 C 0.4535(3) 0.0756(2) 0.6456(2) 0.0366(7) Uani 1 1 d . B . H204 H 0.4546 0.0221 0.6179 0.044 Uiso 1 1 calc R . . C205 C 0.5041(3) 0.1494(2) 0.6018(2) 0.0351(7) Uani 1 1 d D . . C206 C 0.5012(3) 0.2282(2) 0.6412(2) 0.0295(6) Uani 1 1 d . C . H206 H 0.5348 0.2784 0.6084 0.035 Uiso 1 1 calc R . . C207 C 0.3499(3) 0.0016(2) 0.7803(2) 0.0474(9) Uani 1 1 d D . . F1 F 0.2921(9) -0.0381(7) 0.7331(5) 0.073(2) Uani 0.56(2) 1 d PDU B 1 F2 F 0.2858(8) 0.0160(5) 0.8540(5) 0.066(2) Uani 0.56(2) 1 d PDU B 1 F3 F 0.4171(5) -0.0623(5) 0.8004(9) 0.084(3) Uani 0.56(2) 1 d PDU B 1 F101 F 0.4068(9) -0.0362(9) 0.8378(9) 0.082(3) Uani 0.44(2) 1 d PDU B 2 F102 F 0.3376(13) -0.0607(6) 0.7313(6) 0.077(3) Uani 0.44(2) 1 d PDU B 2 F103 F 0.2584(7) 0.0210(7) 0.8287(10) 0.080(3) Uani 0.44(2) 1 d PDU B 2 C208 C 0.5587(4) 0.1412(3) 0.5089(3) 0.0470(11) Uani 0.808(13) 1 d PDU C 1 F4 F 0.6235(5) 0.0694(3) 0.5011(3) 0.0650(18) Uani 0.808(13) 1 d PDU C 1 F5 F 0.4928(4) 0.1322(4) 0.4545(2) 0.0704(14) Uani 0.808(13) 1 d PDU C 1 F6 F 0.6160(5) 0.2113(2) 0.4748(3) 0.0638(15) Uani 0.808(13) 1 d PDU C 1 C308 C 0.5737(10) 0.1451(9) 0.5131(7) 0.0470(11) Uani 0.192(13) 1 d PDU C 2 F104 F 0.5243(15) 0.1760(16) 0.4483(6) 0.067(4) Uani 0.192(13) 1 d PDU C 2 F105 F 0.6598(12) 0.1920(13) 0.5009(11) 0.061(5) Uani 0.192(13) 1 d PDU C 2 F106 F 0.6052(16) 0.0613(9) 0.4965(11) 0.044(5) Uani 0.192(13) 1 d PDU C 2 C209 C 0.5745(2) 0.31064(19) 0.80664(19) 0.0246(6) Uani 1 1 d . . . C210 C 0.5890(2) 0.27818(19) 0.8901(2) 0.0273(6) Uani 1 1 d . . . H210 H 0.5296 0.2670 0.9351 0.033 Uiso 1 1 calc R . . C211 C 0.6880(2) 0.2617(2) 0.9095(2) 0.0306(6) Uani 1 1 d D D . C212 C 0.7770(3) 0.2751(2) 0.8459(2) 0.0345(7) Uani 1 1 d . . . H212 H 0.8443 0.2635 0.8590 0.041 Uiso 1 1 calc R . . C213 C 0.7643(3) 0.3060(2) 0.7626(2) 0.0356(7) Uani 1 1 d D E . C214 C 0.6664(2) 0.3239(2) 0.7437(2) 0.0302(6) Uani 1 1 d . . . H214 H 0.6609 0.3461 0.6859 0.036 Uiso 1 1 calc R . . C215 C 0.6960(3) 0.2288(2) 1.0009(2) 0.0437(8) Uani 1 1 d D . . F7 F 0.6546(3) 0.1482(2) 1.02340(19) 0.0695(10) Uani 0.925(5) 1 d PDU D 1 F8 F 0.6429(3) 0.2787(2) 1.06092(16) 0.0691(10) Uani 0.925(5) 1 d PDU D 1 F9 F 0.7925(2) 0.2179(3) 1.0132(2) 0.0802(12) Uani 0.925(5) 1 d PDU D 1 F107 F 0.757(2) 0.2808(16) 1.0331(12) 0.067(6) Uani 0.075(5) 1 d PDU D 2 F108 F 0.739(2) 0.1479(10) 1.0083(11) 0.070(6) Uani 0.075(5) 1 d PDU D 2 F109 F 0.6067(11) 0.228(2) 1.0572(9) 0.078(6) Uani 0.075(5) 1 d PDU D 2 C216 C 0.8582(3) 0.3190(3) 0.6906(3) 0.0540(11) Uani 1 1 d D . . F10 F 0.9380(4) 0.2625(6) 0.7091(4) 0.084(2) Uani 0.523(8) 1 d PDU E 1 F11 F 0.8473(5) 0.2999(6) 0.6159(3) 0.072(2) Uani 0.523(8) 1 d PDU E 1 F12 F 0.8974(7) 0.3959(4) 0.6876(6) 0.106(3) Uani 0.523(8) 1 d PDU E 1 F110 F 0.8462(5) 0.3943(5) 0.6363(5) 0.094(3) Uani 0.477(8) 1 d PDU E 2 F111 F 0.9442(4) 0.3309(8) 0.7122(4) 0.081(2) Uani 0.477(8) 1 d PDU E 2 F112 F 0.8709(7) 0.2571(6) 0.6357(6) 0.100(3) Uani 0.477(8) 1 d PDU E 2 C217 C 0.4589(2) 0.4168(2) 0.71185(19) 0.0262(6) Uani 1 1 d . . . C218 C 0.3956(2) 0.4275(2) 0.6495(2) 0.0276(6) Uani 1 1 d . . . H218 H 0.3570 0.3787 0.6409 0.033 Uiso 1 1 calc R . . C219 C 0.3874(3) 0.5082(2) 0.5993(2) 0.0322(7) Uani 1 1 d . . . C220 C 0.4441(3) 0.5805(2) 0.6085(2) 0.0375(8) Uani 1 1 d . . . H220 H 0.4397 0.6350 0.5735 0.045 Uiso 1 1 calc R . . C221 C 0.5073(3) 0.5714(2) 0.6702(2) 0.0374(7) Uani 1 1 d D F . C222 C 0.5137(3) 0.4915(2) 0.7214(2) 0.0325(7) Uani 1 1 d . . . H222 H 0.5564 0.4874 0.7641 0.039 Uiso 1 1 calc R . . C223 C 0.3134(3) 0.5176(3) 0.5383(2) 0.0409(8) Uani 1 1 d . . . F13 F 0.3317(3) 0.5855(2) 0.4781(2) 0.0855(10) Uani 1 1 d U . . F14 F 0.21547(19) 0.5295(2) 0.58167(17) 0.0732(9) Uani 1 1 d U . . F15 F 0.3111(2) 0.44603(19) 0.49574(18) 0.0643(7) Uani 1 1 d U . . C224 C 0.5685(3) 0.6490(3) 0.6835(3) 0.0566(11) Uani 1 1 d D . . F16 F 0.6060(7) 0.6955(5) 0.6048(4) 0.0719(19) Uani 0.63(2) 1 d PDU F 1 F17 F 0.5111(5) 0.7082(5) 0.7299(8) 0.083(2) Uani 0.63(2) 1 d PDU F 1 F18 F 0.6505(6) 0.6261(5) 0.7173(8) 0.073(2) Uani 0.63(2) 1 d PDU F 1 F116 F 0.5275(10) 0.6795(11) 0.7622(8) 0.085(4) Uani 0.37(2) 1 d PDU F 2 F117 F 0.6664(5) 0.6243(8) 0.6858(11) 0.064(3) Uani 0.37(2) 1 d PDU F 2 F118 F 0.5689(14) 0.7160(7) 0.6251(10) 0.083(3) Uani 0.37(2) 1 d PDU F 2 C225 C 0.3627(2) 0.34401(19) 0.85767(19) 0.0253(6) Uani 1 1 d . . . C226 C 0.2605(2) 0.3237(2) 0.8546(2) 0.0288(6) Uani 1 1 d . . . H226 H 0.2491 0.2909 0.8086 0.035 Uiso 1 1 calc R . . C227 C 0.1753(2) 0.3501(2) 0.9165(2) 0.0328(7) Uani 1 1 d . . . C228 C 0.1880(3) 0.3971(2) 0.9849(2) 0.0364(7) Uani 1 1 d . . . H228 H 0.1299 0.4142 1.0277 0.044 Uiso 1 1 calc R . . C229 C 0.2884(3) 0.4187(2) 0.9893(2) 0.0347(7) Uani 1 1 d D G . C230 C 0.3732(2) 0.3932(2) 0.9269(2) 0.0289(6) Uani 1 1 d . . . H230 H 0.4407 0.4096 0.9313 0.035 Uiso 1 1 calc R . . C231 C 0.0676(3) 0.3326(3) 0.9054(3) 0.0465(9) Uani 1 1 d . . . F19 F -0.00438(19) 0.3395(3) 0.9771(2) 0.0794(9) Uani 1 1 d U . . F20 F 0.0385(2) 0.3885(2) 0.8428(2) 0.0826(10) Uani 1 1 d U . . F21 F 0.0590(2) 0.2516(2) 0.8806(2) 0.0718(8) Uani 1 1 d U . . C232 C 0.3034(3) 0.4736(3) 1.0598(2) 0.0514(10) Uani 1 1 d D . . F22 F 0.2661(7) 0.4348(5) 1.1381(3) 0.087(2) Uani 0.539(7) 1 d PDU G 1 F23 F 0.2374(6) 0.5481(4) 1.0597(5) 0.096(2) Uani 0.539(7) 1 d PDU G 1 F24 F 0.3910(4) 0.5029(6) 1.0552(5) 0.088(2) Uani 0.539(7) 1 d PDU G 1 F122 F 0.3400(9) 0.5523(4) 1.0291(5) 0.098(3) Uani 0.461(7) 1 d PDU G 2 F123 F 0.3878(6) 0.4394(5) 1.0958(5) 0.082(2) Uani 0.461(7) 1 d PDU G 2 F124 F 0.2308(5) 0.4815(7) 1.1242(5) 0.086(3) Uani 0.461(7) 1 d PDU G 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 0.02304(15) 0.03056(16) 0.04915(19) -0.00746(11) -0.00306(11) 0.00189(10) B1 0.031(2) 0.049(3) 0.077(3) -0.024(2) -0.011(2) 0.0069(18) N1 0.0316(15) 0.0388(16) 0.0517(18) -0.0138(14) -0.0010(13) 0.0029(12) C1 0.049(2) 0.068(3) 0.047(2) -0.010(2) -0.0059(18) 0.013(2) C2 0.050(2) 0.043(2) 0.093(4) -0.028(2) 0.002(2) -0.0024(19) B2 0.0315(19) 0.041(2) 0.044(2) -0.0108(18) 0.0011(16) 0.0056(16) N2 0.0347(15) 0.0452(17) 0.0405(16) -0.0123(13) -0.0033(12) 0.0097(13) C3 0.036(2) 0.061(3) 0.089(4) -0.008(2) -0.010(2) 0.0026(19) C4 0.065(3) 0.070(3) 0.088(4) 0.024(3) -0.003(3) 0.024(3) P1 0.0259(4) 0.0296(4) 0.0651(6) -0.0155(4) -0.0096(4) 0.0037(3) C5 0.0350(19) 0.0362(19) 0.080(3) -0.0261(19) -0.0114(19) 0.0019(15) C6 0.040(2) 0.037(2) 0.094(3) -0.017(2) -0.017(2) -0.0056(16) C7 0.0285(18) 0.045(2) 0.074(3) -0.0171(19) -0.0091(18) -0.0041(15) C8 0.0359(19) 0.050(2) 0.060(2) -0.0173(19) -0.0142(17) 0.0042(16) C9 0.042(2) 0.059(3) 0.062(3) -0.026(2) -0.0099(19) 0.0040(18) C10 0.065(3) 0.049(2) 0.080(3) -0.007(2) -0.034(3) 0.015(2) C11 0.083(4) 0.067(3) 0.082(3) -0.011(3) -0.033(3) 0.019(3) C12 0.079(4) 0.057(3) 0.100(4) -0.010(3) -0.031(4) 0.019(3) C110 0.067(4) 0.055(4) 0.072(4) -0.006(4) -0.024(4) 0.012(4) C111 0.070(5) 0.063(5) 0.071(5) -0.003(4) -0.020(4) 0.014(4) C112 0.057(6) 0.048(6) 0.061(6) -0.001(5) -0.014(5) 0.012(5) C13 0.0266(18) 0.036(2) 0.038(2) -0.0099(17) -0.0083(16) 0.0046(16) C14 0.035(2) 0.043(2) 0.047(3) -0.013(2) -0.0034(19) -0.0049(19) C15 0.038(2) 0.044(3) 0.044(3) -0.011(2) -0.004(2) 0.0071(19) C113 0.036(4) 0.044(4) 0.046(4) -0.010(3) -0.007(3) 0.003(3) C114 0.049(5) 0.052(5) 0.052(5) -0.003(4) -0.001(4) 0.002(4) C115 0.040(5) 0.048(5) 0.047(5) -0.011(4) -0.014(4) 0.010(4) B200 0.0257(16) 0.0235(15) 0.0243(15) -0.0043(12) -0.0059(13) -0.0022(12) C201 0.0265(14) 0.0244(14) 0.0258(14) -0.0042(11) -0.0084(11) 0.0012(11) C202 0.0310(16) 0.0270(15) 0.0279(15) -0.0047(12) -0.0079(12) -0.0003(12) C203 0.0397(18) 0.0236(15) 0.0380(17) -0.0039(13) -0.0126(14) -0.0029(13) C204 0.054(2) 0.0233(15) 0.0356(17) -0.0100(13) -0.0143(15) 0.0011(14) C205 0.050(2) 0.0277(16) 0.0280(16) -0.0064(13) -0.0075(14) 0.0055(14) C206 0.0382(17) 0.0232(14) 0.0270(15) -0.0025(12) -0.0066(13) 0.0016(12) C207 0.055(2) 0.0330(18) 0.053(2) -0.0084(17) -0.0038(19) -0.0114(17) F1 0.085(5) 0.060(4) 0.080(4) -0.010(3) -0.017(3) -0.037(4) F2 0.084(4) 0.043(3) 0.061(3) -0.011(2) 0.020(3) -0.028(3) F3 0.075(3) 0.049(3) 0.104(5) 0.037(3) 0.013(3) 0.012(3) F101 0.098(5) 0.070(5) 0.074(5) 0.034(4) -0.022(4) -0.020(4) F102 0.107(6) 0.037(4) 0.082(4) -0.023(3) 0.007(4) -0.028(4) F103 0.064(5) 0.067(5) 0.100(6) -0.015(4) 0.015(4) -0.031(4) C208 0.076(3) 0.0293(17) 0.0336(18) -0.0081(15) -0.0047(18) 0.0066(18) F4 0.092(3) 0.045(2) 0.047(2) -0.0084(18) 0.008(2) 0.026(2) F5 0.113(3) 0.069(3) 0.0342(17) -0.0134(16) -0.0240(18) 0.004(2) F6 0.102(3) 0.0395(17) 0.0367(18) -0.0065(13) 0.020(2) -0.0036(19) C308 0.076(3) 0.0293(17) 0.0336(18) -0.0081(15) -0.0047(18) 0.0066(18) F104 0.089(7) 0.067(7) 0.043(6) 0.003(5) -0.012(5) 0.001(6) F105 0.071(7) 0.059(7) 0.048(7) -0.015(5) 0.008(5) -0.012(6) F106 0.058(7) 0.034(7) 0.040(7) -0.015(5) -0.003(5) -0.003(5) C209 0.0274(14) 0.0206(13) 0.0270(14) -0.0069(11) -0.0054(12) -0.0024(11) C210 0.0287(15) 0.0240(14) 0.0292(15) -0.0051(12) -0.0040(12) -0.0019(11) C211 0.0335(16) 0.0273(15) 0.0330(16) -0.0067(12) -0.0102(13) 0.0014(12) C212 0.0268(16) 0.0382(17) 0.0416(18) -0.0112(14) -0.0114(14) 0.0023(13) C213 0.0285(16) 0.0431(19) 0.0348(17) -0.0110(14) -0.0008(13) -0.0037(14) C214 0.0294(16) 0.0339(16) 0.0276(15) -0.0054(12) -0.0047(12) -0.0012(12) C215 0.0387(19) 0.052(2) 0.041(2) 0.0006(17) -0.0138(16) 0.0056(16) F7 0.088(2) 0.0634(18) 0.0565(16) 0.0215(14) -0.0224(15) -0.0113(16) F8 0.093(2) 0.082(2) 0.0348(13) -0.0156(13) -0.0219(14) 0.0277(18) F9 0.0419(15) 0.140(3) 0.0599(17) 0.0197(19) -0.0279(13) 0.0043(17) F107 0.073(8) 0.081(9) 0.054(8) -0.003(7) -0.029(7) -0.004(7) F108 0.068(8) 0.078(9) 0.064(8) 0.009(7) -0.021(7) 0.002(7) F109 0.082(9) 0.087(9) 0.065(9) 0.001(7) -0.018(7) 0.002(7) C216 0.0310(19) 0.084(3) 0.045(2) -0.012(2) 0.0014(16) -0.004(2) F10 0.044(3) 0.113(5) 0.075(4) 0.014(4) 0.018(2) 0.031(3) F11 0.048(3) 0.135(6) 0.030(2) -0.012(3) 0.003(2) -0.012(3) F12 0.093(5) 0.088(4) 0.116(5) -0.020(4) 0.047(4) -0.054(4) F110 0.058(4) 0.124(5) 0.079(4) 0.029(4) 0.020(3) -0.015(4) F111 0.037(3) 0.148(6) 0.059(3) -0.002(4) -0.012(2) -0.020(4) F112 0.095(5) 0.111(5) 0.078(5) -0.037(4) 0.034(4) -0.005(4) C217 0.0277(15) 0.0247(14) 0.0254(14) -0.0062(11) -0.0024(11) 0.0014(11) C218 0.0284(15) 0.0275(15) 0.0259(14) -0.0055(12) -0.0027(12) 0.0035(12) C219 0.0321(16) 0.0347(17) 0.0260(15) -0.0021(13) 0.0002(12) 0.0090(13) C220 0.0408(19) 0.0286(16) 0.0387(18) 0.0032(14) -0.0019(15) 0.0049(14) C221 0.0397(18) 0.0262(16) 0.0452(19) -0.0030(14) -0.0059(15) -0.0016(13) C222 0.0352(17) 0.0270(15) 0.0359(17) -0.0055(13) -0.0074(13) -0.0009(13) C223 0.042(2) 0.046(2) 0.0321(17) -0.0001(15) -0.0070(15) 0.0115(16) F13 0.105(2) 0.087(2) 0.0709(18) 0.0421(16) -0.0492(17) -0.0204(18) F14 0.0380(13) 0.124(2) 0.0553(15) -0.0121(15) -0.0110(11) 0.0334(14) F15 0.0686(16) 0.0747(17) 0.0607(15) -0.0234(13) -0.0365(13) 0.0186(13) C224 0.055(3) 0.0320(19) 0.084(3) 0.003(2) -0.021(2) -0.0048(18) F16 0.074(4) 0.033(2) 0.098(4) 0.003(2) 0.010(3) -0.017(2) F17 0.068(3) 0.060(3) 0.124(5) -0.049(4) -0.007(3) -0.011(3) F18 0.059(3) 0.050(3) 0.116(6) 0.014(3) -0.037(3) -0.023(2) F116 0.094(6) 0.063(6) 0.111(7) -0.048(5) -0.027(5) -0.013(5) F117 0.051(5) 0.063(5) 0.078(6) 0.000(4) -0.008(4) -0.024(4) F118 0.092(6) 0.044(5) 0.115(6) 0.014(4) -0.035(5) -0.013(4) C225 0.0283(15) 0.0212(13) 0.0271(15) -0.0028(11) -0.0067(12) -0.0007(11) C226 0.0302(16) 0.0276(15) 0.0299(15) -0.0039(12) -0.0083(12) -0.0020(12) C227 0.0253(15) 0.0334(16) 0.0390(18) -0.0002(13) -0.0060(13) -0.0010(12) C228 0.0308(17) 0.0374(18) 0.0374(18) -0.0088(14) 0.0039(13) 0.0004(13) C229 0.0367(18) 0.0332(17) 0.0336(17) -0.0105(13) -0.0014(14) -0.0028(13) C230 0.0277(15) 0.0286(15) 0.0311(16) -0.0061(12) -0.0049(12) -0.0034(12) C231 0.0292(18) 0.057(2) 0.053(2) -0.0052(18) -0.0068(16) -0.0004(16) F19 0.0305(12) 0.127(3) 0.0783(19) -0.0276(18) 0.0051(12) -0.0134(14) F20 0.0516(15) 0.097(2) 0.104(2) 0.0287(18) -0.0422(16) -0.0070(15) F21 0.0431(14) 0.0696(17) 0.111(2) -0.0225(16) -0.0243(14) -0.0156(12) C232 0.058(3) 0.050(2) 0.046(2) -0.0231(19) 0.0010(19) -0.0089(19) F22 0.132(5) 0.089(4) 0.043(3) -0.023(3) -0.012(3) -0.028(4) F23 0.111(5) 0.072(4) 0.120(5) -0.069(3) -0.038(4) 0.022(3) F24 0.050(3) 0.129(5) 0.092(4) -0.083(4) 0.008(3) -0.031(3) F122 0.151(6) 0.062(4) 0.090(5) -0.034(3) -0.021(5) -0.029(4) F123 0.105(5) 0.083(4) 0.077(4) -0.050(3) -0.045(4) 0.008(4) F124 0.066(4) 0.126(6) 0.065(4) -0.064(4) 0.019(3) -0.015(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 C7 2.107(4) . ? Rh1 C8 2.121(4) . ? Rh1 P1 2.2058(9) . ? Rh1 B1 2.242(5) . ? Rh1 B2 2.626(4) . ? Rh1 H1A 1.85(5) . ? Rh1 H1B 1.84(5) . ? Rh1 H2A 1.96(4) . ? B1 N1 1.606(5) . ? B1 H1A 1.23(5) . ? B1 H1B 1.22(5) . ? B1 H1C 1.13(5) . ? N1 C1 1.486(5) . ? N1 C2 1.488(5) . ? N1 B2 1.562(6) . ? C1 H1D 0.9800 . ? C1 H1E 0.9800 . ? C1 H1F 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C2 H2E 0.9800 . ? B2 N2 1.621(5) . ? B2 H2A 1.13(4) . ? B2 H2B 1.12(4) . ? N2 C4 1.477(6) . ? N2 C3 1.506(6) . ? N2 H2 0.9300 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? P1 C113 1.823(9) . ? P1 C5 1.831(4) . ? P1 C10 1.837(5) . ? P1 C110 1.841(10) . ? P1 C13 1.882(4) . ? C5 C9 1.533(6) . ? C5 C6 1.550(6) . ? C5 H5 1.0000 . ? C6 C7 1.521(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.416(6) . ? C7 H7 1.08(4) . ? C8 C9 1.526(6) . ? C8 H8 1.08(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C12 1.503(6) . ? C10 C11 1.526(7) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C110 C112 1.520(10) . ? C110 C111 1.532(10) . ? C110 H110 1.0000 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C111 H11F 0.9800 . ? C112 H11G 0.9800 . ? C112 H11H 0.9800 . ? C112 H11I 0.9800 . ? C13 C15 1.522(5) . ? C13 C14 1.533(5) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C113 C114 1.528(9) . ? C113 C115 1.534(9) . ? C113 H113 1.0000 . ? C114 H11J 0.9800 . ? C114 H11K 0.9800 . ? C114 H11L 0.9800 . ? C115 H11M 0.9800 . ? C115 H11N 0.9800 . ? C115 H11O 0.9800 . ? B200 C201 1.640(4) . ? B200 C217 1.640(4) . ? B200 C209 1.640(4) . ? B200 C225 1.643(4) . ? C201 C202 1.399(4) . ? C201 C206 1.405(4) . ? C202 C203 1.398(4) . ? C202 H202 0.9500 . ? C203 C204 1.382(5) . ? C203 C207 1.488(5) . ? C204 C205 1.381(5) . ? C204 H204 0.9500 . ? C205 C206 1.385(4) . ? C205 C208 1.500(5) . ? C205 C308 1.505(10) . ? C206 H206 0.9500 . ? C207 F102 1.304(6) . ? C207 F2 1.313(5) . ? C207 F103 1.319(6) . ? C207 F3 1.330(6) . ? C207 F101 1.349(6) . ? C207 F1 1.354(6) . ? C208 F6 1.336(5) . ? C208 F4 1.340(5) . ? C208 F5 1.349(5) . ? C308 F105 1.337(9) . ? C308 F106 1.341(9) . ? C308 F104 1.344(9) . ? C209 C210 1.397(4) . ? C209 C214 1.405(4) . ? C210 C211 1.395(4) . ? C210 H210 0.9500 . ? C211 C212 1.384(5) . ? C211 C215 1.493(5) . ? C212 C213 1.381(5) . ? C212 H212 0.9500 . ? C213 C214 1.382(5) . ? C213 C216 1.500(5) . ? C214 H214 0.9500 . ? C215 F109 1.316(8) . ? C215 F9 1.317(4) . ? C215 F8 1.322(4) . ? C215 F108 1.322(8) . ? C215 F107 1.345(8) . ? C215 F7 1.347(4) . ? C216 F111 1.266(5) . ? C216 F11 1.267(5) . ? C216 F12 1.287(6) . ? C216 F112 1.309(6) . ? C216 F10 1.373(6) . ? C216 F110 1.377(6) . ? C217 C218 1.397(4) . ? C217 C222 1.404(4) . ? C218 C219 1.396(4) . ? C218 H218 0.9500 . ? C219 C220 1.388(5) . ? C219 C223 1.485(5) . ? C220 C221 1.386(5) . ? C220 H220 0.9500 . ? C221 C222 1.392(5) . ? C221 C224 1.508(5) . ? C222 H222 0.9500 . ? C223 F13 1.324(5) . ? C223 F15 1.327(5) . ? C223 F14 1.338(4) . ? C224 F118 1.298(7) . ? C224 F18 1.308(6) . ? C224 F17 1.313(6) . ? C224 F117 1.324(7) . ? C224 F116 1.354(7) . ? C224 F16 1.372(6) . ? C225 C226 1.401(4) . ? C225 C230 1.402(4) . ? C226 C227 1.393(5) . ? C226 H226 0.9500 . ? C227 C228 1.380(5) . ? C227 C231 1.497(5) . ? C228 C229 1.389(5) . ? C228 H228 0.9500 . ? C229 C230 1.389(4) . ? C229 C232 1.490(5) . ? C230 H230 0.9500 . ? C231 F19 1.322(5) . ? C231 F20 1.333(5) . ? C231 F21 1.334(5) . ? C232 F24 1.239(5) . ? C232 F124 1.250(6) . ? C232 F122 1.317(6) . ? C232 F22 1.318(6) . ? C232 F23 1.382(6) . ? C232 F123 1.394(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 C7 Rh1 C8 39.14(18) . . ? C7 Rh1 P1 84.17(11) . . ? C8 Rh1 P1 83.46(11) . . ? C7 Rh1 B1 156.8(2) . . ? C8 Rh1 B1 159.77(19) . . ? P1 Rh1 B1 106.15(12) . . ? C7 Rh1 B2 112.88(14) . . ? C8 Rh1 B2 105.24(15) . . ? P1 Rh1 B2 161.66(10) . . ? B1 Rh1 B2 60.79(15) . . ? C7 Rh1 H1A 126.7(15) . . ? C8 Rh1 H1A 165.8(15) . . ? P1 Rh1 H1A 96.6(15) . . ? B1 Rh1 H1A 33.2(15) . . ? B2 Rh1 H1A 78.9(15) . . ? C7 Rh1 H1B 169.5(15) . . ? C8 Rh1 H1B 130.4(15) . . ? P1 Rh1 H1B 94.9(15) . . ? B1 Rh1 H1B 33.0(15) . . ? B2 Rh1 H1B 67.1(15) . . ? H1A Rh1 H1B 64(2) . . ? C7 Rh1 H2A 91.9(13) . . ? C8 Rh1 H2A 95.6(12) . . ? P1 Rh1 H2A 174.8(13) . . ? B1 Rh1 H2A 76.4(12) . . ? B2 Rh1 H2A 23.3(13) . . ? H1A Rh1 H2A 83.0(19) . . ? H1B Rh1 H2A 90(2) . . ? N1 B1 Rh1 103.1(3) . . ? N1 B1 H1A 110(2) . . ? Rh1 B1 H1A 55(2) . . ? N1 B1 H1B 109(2) . . ? Rh1 B1 H1B 55(2) . . ? H1A B1 H1B 105(3) . . ? N1 B1 H1C 113(2) . . ? Rh1 B1 H1C 143(2) . . ? H1A B1 H1C 108(3) . . ? H1B B1 H1C 110(3) . . ? C1 N1 C2 109.6(3) . . ? C1 N1 B2 114.9(3) . . ? C2 N1 B2 112.1(4) . . ? C1 N1 B1 107.4(3) . . ? C2 N1 B1 109.1(3) . . ? B2 N1 B1 103.3(3) . . ? N1 C1 H1D 109.5 . . ? N1 C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? N1 C1 H1F 109.5 . . ? H1D C1 H1F 109.5 . . ? H1E C1 H1F 109.5 . . ? N1 C2 H2C 109.5 . . ? N1 C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? N1 C2 H2E 109.5 . . ? H2C C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? N1 B2 N2 112.7(3) . . ? N1 B2 Rh1 89.3(2) . . ? N2 B2 Rh1 141.8(3) . . ? N1 B2 H2A 107(2) . . ? N2 B2 H2A 99(2) . . ? Rh1 B2 H2A 43(2) . . ? N1 B2 H2B 111(2) . . ? N2 B2 H2B 110(2) . . ? Rh1 B2 H2B 89(2) . . ? H2A B2 H2B 117(3) . . ? C4 N2 C3 109.9(4) . . ? C4 N2 B2 113.0(3) . . ? C3 N2 B2 112.8(3) . . ? C4 N2 H2 106.9 . . ? C3 N2 H2 106.9 . . ? B2 N2 H2 106.9 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C113 P1 C5 118.3(5) . . ? C113 P1 C10 90.6(6) . . ? C5 P1 C10 108.6(3) . . ? C113 P1 C110 78.2(9) . . ? C5 P1 C110 111.3(7) . . ? C10 P1 C110 12.9(7) . . ? C113 P1 C13 24.0(5) . . ? C5 P1 C13 105.2(2) . . ? C10 P1 C13 114.4(3) . . ? C110 P1 C13 101.7(7) . . ? C113 P1 Rh1 125.5(4) . . ? C5 P1 Rh1 98.24(13) . . ? C10 P1 Rh1 115.6(2) . . ? C110 P1 Rh1 126.1(5) . . ? C13 P1 Rh1 112.86(14) . . ? C9 C5 C6 102.0(3) . . ? C9 C5 P1 104.0(3) . . ? C6 C5 P1 103.6(3) . . ? C9 C5 H5 115.2 . . ? C6 C5 H5 115.2 . . ? P1 C5 H5 115.2 . . ? C7 C6 C5 100.4(3) . . ? C7 C6 H6A 111.7 . . ? C5 C6 H6A 111.7 . . ? C7 C6 H6B 111.7 . . ? C5 C6 H6B 111.7 . . ? H6A C6 H6B 109.5 . . ? C8 C7 C6 109.0(4) . . ? C8 C7 Rh1 70.9(2) . . ? C6 C7 Rh1 113.6(3) . . ? C8 C7 H7 121(3) . . ? C6 C7 H7 122(3) . . ? Rh1 C7 H7 110(2) . . ? C7 C8 C9 108.6(4) . . ? C7 C8 Rh1 69.9(2) . . ? C9 C8 Rh1 114.4(3) . . ? C7 C8 H8 121(3) . . ? C9 C8 H8 123(3) . . ? Rh1 C8 H8 107(2) . . ? C8 C9 C5 100.6(4) . . ? C8 C9 H9A 111.7 . . ? C5 C9 H9A 111.7 . . ? C8 C9 H9B 111.7 . . ? C5 C9 H9B 111.7 . . ? H9A C9 H9B 109.4 . . ? C12 C10 C11 115.3(5) . . ? C12 C10 P1 115.8(5) . . ? C11 C10 P1 115.6(4) . . ? C12 C10 H10 102.3 . . ? C11 C10 H10 102.3 . . ? P1 C10 H10 102.3 . . ? C112 C110 C111 114.4(11) . . ? C112 C110 P1 113.3(9) . . ? C111 C110 P1 110.9(8) . . ? C112 C110 H110 105.8 . . ? C111 C110 H110 105.8 . . ? P1 C110 H110 105.8 . . ? C110 C111 H11D 109.5 . . ? C110 C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? C110 C111 H11F 109.5 . . ? H11D C111 H11F 109.5 . . ? H11E C111 H11F 109.5 . . ? C110 C112 H11G 109.5 . . ? C110 C112 H11H 109.5 . . ? H11G C112 H11H 109.5 . . ? C110 C112 H11I 109.5 . . ? H11G C112 H11I 109.5 . . ? H11H C112 H11I 109.5 . . ? C15 C13 C14 112.1(4) . . ? C15 C13 P1 113.6(3) . . ? C14 C13 P1 111.4(3) . . ? C15 C13 H13 106.4 . . ? C14 C13 H13 106.4 . . ? P1 C13 H13 106.4 . . ? C114 C113 C115 112.5(9) . . ? C114 C113 P1 112.4(8) . . ? C115 C113 P1 112.9(8) . . ? C114 C113 H113 106.1 . . ? C115 C113 H113 106.1 . . ? P1 C113 H113 106.1 . . ? C113 C114 H11J 109.5 . . ? C113 C114 H11K 109.5 . . ? H11J C114 H11K 109.5 . . ? C113 C114 H11L 109.5 . . ? H11J C114 H11L 109.5 . . ? H11K C114 H11L 109.5 . . ? C113 C115 H11M 109.5 . . ? C113 C115 H11N 109.5 . . ? H11M C115 H11N 109.5 . . ? C113 C115 H11O 109.5 . . ? H11M C115 H11O 109.5 . . ? H11N C115 H11O 109.5 . . ? C201 B200 C217 112.0(2) . . ? C201 B200 C209 104.0(2) . . ? C217 B200 C209 110.4(2) . . ? C201 B200 C225 113.7(2) . . ? C217 B200 C225 102.2(2) . . ? C209 B200 C225 114.7(2) . . ? C202 C201 C206 115.7(3) . . ? C202 C201 B200 122.9(3) . . ? C206 C201 B200 121.0(3) . . ? C203 C202 C201 122.1(3) . . ? C203 C202 H202 118.9 . . ? C201 C202 H202 118.9 . . ? C204 C203 C202 120.7(3) . . ? C204 C203 C207 118.9(3) . . ? C202 C203 C207 120.4(3) . . ? C205 C204 C203 118.2(3) . . ? C205 C204 H204 120.9 . . ? C203 C204 H204 120.9 . . ? C204 C205 C206 121.2(3) . . ? C204 C205 C208 116.9(3) . . ? C206 C205 C208 121.8(3) . . ? C204 C205 C308 121.5(6) . . ? C206 C205 C308 117.0(6) . . ? C208 C205 C308 8.8(6) . . ? C205 C206 C201 122.1(3) . . ? C205 C206 H206 119.0 . . ? C201 C206 H206 119.0 . . ? F102 C207 F2 123.3(6) . . ? F102 C207 F103 108.0(5) . . ? F2 C207 F103 25.7(6) . . ? F102 C207 F3 77.2(6) . . ? F2 C207 F3 106.0(5) . . ? F103 C207 F3 125.9(6) . . ? F102 C207 F101 106.1(5) . . ? F2 C207 F101 80.3(6) . . ? F103 C207 F101 104.7(5) . . ? F3 C207 F101 31.3(5) . . ? F102 C207 F1 29.0(5) . . ? F2 C207 F1 104.9(5) . . ? F103 C207 F1 83.5(6) . . ? F3 C207 F1 104.2(5) . . ? F101 C207 F1 128.9(6) . . ? F102 C207 C203 114.2(5) . . ? F2 C207 C203 115.5(4) . . ? F103 C207 C203 112.6(5) . . ? F3 C207 C203 113.3(4) . . ? F101 C207 C203 110.6(4) . . ? F1 C207 C203 112.0(4) . . ? F6 C208 F4 106.5(5) . . ? F6 C208 F5 106.3(4) . . ? F4 C208 F5 105.2(4) . . ? F6 C208 C205 113.0(3) . . ? F4 C208 C205 112.1(4) . . ? F5 C208 C205 113.1(4) . . ? F105 C308 F106 106.5(8) . . ? F105 C308 F104 105.6(8) . . ? F106 C308 F104 105.5(8) . . ? F105 C308 C205 114.6(8) . . ? F106 C308 C205 112.2(8) . . ? F104 C308 C205 111.8(8) . . ? C210 C209 C214 115.2(3) . . ? C210 C209 B200 124.8(3) . . ? C214 C209 B200 119.7(3) . . ? C211 C210 C209 122.1(3) . . ? C211 C210 H210 119.0 . . ? C209 C210 H210 119.0 . . ? C212 C211 C210 121.3(3) . . ? C212 C211 C215 120.4(3) . . ? C210 C211 C215 118.4(3) . . ? C213 C212 C211 117.6(3) . . ? C213 C212 H212 121.2 . . ? C211 C212 H212 121.2 . . ? C212 C213 C214 121.2(3) . . ? C212 C213 C216 119.7(3) . . ? C214 C213 C216 119.1(3) . . ? C213 C214 C209 122.6(3) . . ? C213 C214 H214 118.7 . . ? C209 C214 H214 118.7 . . ? F109 C215 F9 131.0(9) . . ? F109 C215 F8 41.7(15) . . ? F9 C215 F8 108.6(3) . . ? F109 C215 F108 106.3(8) . . ? F9 C215 F108 59.8(14) . . ? F8 C215 F108 130.9(9) . . ? F109 C215 F107 105.4(8) . . ? F9 C215 F107 47.8(14) . . ? F8 C215 F107 67.0(14) . . ? F108 C215 F107 104.7(8) . . ? F109 C215 F7 64.5(15) . . ? F9 C215 F7 104.9(3) . . ? F8 C215 F7 103.6(3) . . ? F108 C215 F7 47.9(14) . . ? F107 C215 F7 136.6(8) . . ? F109 C215 C211 114.5(8) . . ? F9 C215 C211 113.8(3) . . ? F8 C215 C211 113.8(3) . . ? F108 C215 C211 114.1(7) . . ? F107 C215 C211 111.0(7) . . ? F7 C215 C211 111.3(3) . . ? F111 C216 F11 125.4(5) . . ? F111 C216 F12 56.2(5) . . ? F11 C216 F12 112.1(5) . . ? F111 C216 F112 109.4(5) . . ? F11 C216 F112 34.6(5) . . ? F12 C216 F112 133.1(6) . . ? F111 C216 F10 46.4(4) . . ? F11 C216 F10 104.0(5) . . ? F12 C216 F10 102.0(5) . . ? F112 C216 F10 72.7(5) . . ? F111 C216 F110 102.4(5) . . ? F11 C216 F110 68.4(5) . . ? F12 C216 F110 51.0(5) . . ? F112 C216 F110 101.4(5) . . ? F10 C216 F110 137.7(5) . . ? F111 C216 C213 117.7(4) . . ? F11 C216 C213 115.5(4) . . ? F12 C216 C213 112.7(4) . . ? F112 C216 C213 112.9(5) . . ? F10 C216 C213 109.3(4) . . ? F110 C216 C213 111.3(4) . . ? C218 C217 C222 116.3(3) . . ? C218 C217 B200 122.2(3) . . ? C222 C217 B200 121.2(3) . . ? C219 C218 C217 121.7(3) . . ? C219 C218 H218 119.1 . . ? C217 C218 H218 119.1 . . ? C220 C219 C218 120.9(3) . . ? C220 C219 C223 119.7(3) . . ? C218 C219 C223 119.4(3) . . ? C221 C220 C219 118.3(3) . . ? C221 C220 H220 120.9 . . ? C219 C220 H220 120.9 . . ? C220 C221 C222 120.7(3) . . ? C220 C221 C224 120.0(3) . . ? C222 C221 C224 119.3(3) . . ? C221 C222 C217 122.0(3) . . ? C221 C222 H222 119.0 . . ? C217 C222 H222 119.0 . . ? F13 C223 F15 106.4(3) . . ? F13 C223 F14 106.6(3) . . ? F15 C223 F14 104.5(3) . . ? F13 C223 C219 113.9(3) . . ? F15 C223 C219 113.7(3) . . ? F14 C223 C219 111.0(3) . . ? F118 C224 F18 121.5(7) . . ? F118 C224 F17 78.9(7) . . ? F18 C224 F17 109.4(5) . . ? F118 C224 F117 108.1(6) . . ? F18 C224 F117 21.8(7) . . ? F17 C224 F117 126.7(7) . . ? F118 C224 F116 107.0(6) . . ? F18 C224 F116 85.4(7) . . ? F17 C224 F116 30.2(6) . . ? F117 C224 F116 106.3(6) . . ? F118 C224 F16 26.3(7) . . ? F18 C224 F16 105.3(5) . . ? F17 C224 F16 104.1(4) . . ? F117 C224 F16 87.0(6) . . ? F116 C224 F16 129.5(7) . . ? F118 C224 C221 114.6(5) . . ? F18 C224 C221 114.0(4) . . ? F17 C224 C221 112.8(4) . . ? F117 C224 C221 111.2(6) . . ? F116 C224 C221 109.2(5) . . ? F16 C224 C221 110.4(4) . . ? C226 C225 C230 115.5(3) . . ? C226 C225 B200 122.0(3) . . ? C230 C225 B200 121.8(3) . . ? C227 C226 C225 122.2(3) . . ? C227 C226 H226 118.9 . . ? C225 C226 H226 118.9 . . ? C228 C227 C226 121.1(3) . . ? C228 C227 C231 119.4(3) . . ? C226 C227 C231 119.4(3) . . ? C227 C228 C229 118.0(3) . . ? C227 C228 H228 121.0 . . ? C229 C228 H228 121.0 . . ? C230 C229 C228 120.8(3) . . ? C230 C229 C232 120.2(3) . . ? C228 C229 C232 118.9(3) . . ? C229 C230 C225 122.4(3) . . ? C229 C230 H230 118.8 . . ? C225 C230 H230 118.8 . . ? F19 C231 F20 107.1(3) . . ? F19 C231 F21 105.8(4) . . ? F20 C231 F21 104.8(4) . . ? F19 C231 C227 113.9(3) . . ? F20 C231 C227 111.5(3) . . ? F21 C231 C227 113.2(3) . . ? F24 C232 F124 123.0(5) . . ? F24 C232 F122 49.9(5) . . ? F124 C232 F122 110.0(5) . . ? F24 C232 F22 112.1(5) . . ? F124 C232 F22 38.9(4) . . ? F122 C232 F22 135.5(5) . . ? F24 C232 F23 105.0(5) . . ? F124 C232 F23 61.4(5) . . ? F122 C232 F23 59.4(5) . . ? F22 C232 F23 100.2(5) . . ? F24 C232 F123 48.8(4) . . ? F124 C232 F123 104.7(5) . . ? F122 C232 F123 98.2(5) . . ? F22 C232 F123 72.4(5) . . ? F23 C232 F123 140.5(4) . . ? F24 C232 C229 117.8(4) . . ? F124 C232 C229 118.9(4) . . ? F122 C232 C229 112.6(4) . . ? F22 C232 C229 111.4(4) . . ? F23 C232 C229 108.6(4) . . ? F123 C232 C229 110.2(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.744 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.071 # Attachment '4b.cif' data_4b _database_code_depnum_ccdc_archive 'CCDC 767950' #TrackingRef '4b.cif' #-------------------------------------------------------- # [Rh(PiPr2Cyp')(B3N3Me3H9)][BArF4].0.5(CH3CH2CH2CH2CH3) #-------------------------------------------------------- # start Validation Reply Form _vrf_PLAT431_4b ; PROBLEM: Short Inter HL..A Contact F110 .. F116 .. 2.42 Ang. RESPONSE: The anion contains a significant degree of disorder - the short contact occurs between disordered components (12%). ; _vrf_PLAT410_4b ; PROBLEM: Short Intra H...H Contact H5A .. H109 .. 1.81 Ang. RESPONSE: The structure contains a disordered phosphine ligand - the short contact occurs with a minor disordered component (22%). ; _vrf_PLAT301_4b ; PROBLEM: Note: Main Residue Disorder ................... 16.00 Perc. RESPONSE: The structure contains a significant degree of disorder. See details in supplementary information or _refine_special_details. ; _vrf_PLAT045_4b ; PROBLEM: Calculated and Reported Z Differ by ............ 0.50 Ratio RESPONSE: Artifact of the checkCIF - the structure contains a disordered pentane solvent molecule that lies on a special position. ; # end Validation Reply Form #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic . _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety 'C32 H12 B F24, C14 H39 B3 N3 P Rh, 0.5(C5 H12)' _chemical_formula_sum 'C48.50 H57 B4 F24 N3 P Rh' _chemical_formula_weight 1315.09 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' N N 0.0061 0.0033 '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 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 13.22060(10) _cell_length_b 18.33470(10) _cell_length_c 24.0722(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.7365(4) _cell_angle_gamma 90.00 _cell_volume 5767.30(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13437 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2660 _exptl_absorpt_coefficient_mu 0.438 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.918 _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 'horizonally mounted graphite crystal' _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 22949 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 5.14 _diffrn_reflns_theta_max 26.37 _reflns_number_total 11699 _reflns_number_gt 9473 _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 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Solved with sir2004. B-H and alkene protons were located on the Fourier difference map; their isotropic displacement parameters were fixed to ride on the parent atoms. C6-H6 and C7-H7 were restrained to equal length. Disorder of the phosphine ligand was treated by modelling the appropriate phosphine substituent over two sites and restraining its geometry. Disorder of the pentane solvent model was treated by modelling it over two sites and restraining its geometry. The central atom lies on a special position. Rotational disorder of the CF3 groups of the anion was treated by modelling the fluorine atoms over two sites 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^)+(0.0577P)^2^+5.3549P] 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 11699 _refine_ls_number_parameters 930 _refine_ls_number_restraints 590 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.187 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.364944(16) 0.224741(13) 1.019430(9) 0.02664(9) Uani 1 1 d . A . P1 P 0.47634(6) 0.20043(5) 0.96072(3) 0.03117(18) Uani 1 1 d D . . B1 B 0.2143(3) 0.2642(2) 1.07702(17) 0.0389(8) Uani 1 1 d . . . H1A H 0.298(3) 0.238(2) 1.0806(15) 0.047 Uiso 1 1 d . . . H1B H 0.200(3) 0.273(2) 1.1187(16) 0.047 Uiso 1 1 d . . . N1 N 0.1457(2) 0.27741(15) 0.95223(12) 0.0381(6) Uani 1 1 d . . . H1 H 0.0806 0.2948 0.9550 0.046 Uiso 1 1 calc R . . C1 C 0.1540(3) 0.2714(2) 0.89134(15) 0.0499(9) Uani 1 1 d . . . H1C H 0.2196 0.2489 0.8870 0.075 Uiso 1 1 calc R . . H1D H 0.1499 0.3202 0.8745 0.075 Uiso 1 1 calc R . . H1E H 0.0978 0.2413 0.8725 0.075 Uiso 1 1 calc R . . B2 B 0.1566(3) 0.1998(2) 0.98062(16) 0.0355(8) Uani 1 1 d . . . H2A H 0.241(3) 0.1802(19) 0.9810(14) 0.043 Uiso 1 1 d . . . H2B H 0.101(3) 0.161(2) 0.9588(14) 0.043 Uiso 1 1 d . . . N2 N 0.1401(2) 0.20748(15) 1.04347(12) 0.0380(6) Uani 1 1 d . . . H2 H 0.0735 0.2238 1.0436 0.046 Uiso 1 1 calc R . . C2 C 0.1500(3) 0.1344(2) 1.07178(17) 0.0485(9) Uani 1 1 d . . . H2C H 0.2194 0.1154 1.0718 0.073 Uiso 1 1 calc R . . H2D H 0.1002 0.1005 1.0515 0.073 Uiso 1 1 calc R . . H2E H 0.1370 0.1394 1.1106 0.073 Uiso 1 1 calc R . . B3 B 0.2254(3) 0.3331(2) 0.98332(18) 0.0386(8) Uani 1 1 d . . . H3A H 0.310(3) 0.309(2) 0.9839(15) 0.046 Uiso 1 1 d . . . H3B H 0.222(3) 0.387(2) 0.9611(15) 0.046 Uiso 1 1 d . . . N3 N 0.2076(2) 0.33962(15) 1.04615(13) 0.0416(7) Uani 1 1 d . . . H3 H 0.1420 0.3579 1.0462 0.050 Uiso 1 1 calc R . . C3 C 0.2815(3) 0.3923(2) 1.07758(19) 0.0548(10) Uani 1 1 d . . . H3C H 0.2688 0.3959 1.1165 0.082 Uiso 1 1 calc R . . H3D H 0.2727 0.4404 1.0597 0.082 Uiso 1 1 calc R . . H3E H 0.3516 0.3752 1.0771 0.082 Uiso 1 1 calc R . . C4 C 0.5848(2) 0.17339(19) 1.01369(13) 0.0365(7) Uani 1 1 d . A . H4 H 0.6481 0.1587 0.9984 0.044 Uiso 1 1 calc R . . C5 C 0.5399(3) 0.1146(2) 1.04826(16) 0.0457(8) Uani 1 1 d . . . H5A H 0.5057 0.0755 1.0240 0.055 Uiso 1 1 calc R A . H5B H 0.5929 0.0929 1.0770 0.055 Uiso 1 1 calc R . . C6 C 0.4634(3) 0.1593(2) 1.07492(14) 0.0404(8) Uani 1 1 d D A . H6 H 0.428(3) 0.135(2) 1.1035(14) 0.049 Uiso 1 1 d D . . C7 C 0.4982(2) 0.2326(2) 1.07853(14) 0.0409(8) Uani 1 1 d D . . H7 H 0.488(3) 0.2682(18) 1.1080(15) 0.049 Uiso 1 1 d D . . C8 C 0.5983(2) 0.2369(2) 1.05510(15) 0.0440(8) Uani 1 1 d . A . H8A H 0.6580 0.2296 1.0848 0.053 Uiso 1 1 calc R . . H8B H 0.6054 0.2839 1.0359 0.053 Uiso 1 1 calc R . . C9 C 0.4531(4) 0.1311(3) 0.9045(2) 0.0344(12) Uani 0.783(12) 1 d PDU A 1 H9 H 0.4373 0.1577 0.8679 0.041 Uiso 0.783(12) 1 calc PR A 1 C10 C 0.3604(3) 0.0839(3) 0.9106(3) 0.0392(13) Uani 0.783(12) 1 d PU A 1 H10A H 0.3517 0.0466 0.8811 0.059 Uiso 0.783(12) 1 calc PR A 1 H10B H 0.2991 0.1145 0.9071 0.059 Uiso 0.783(12) 1 calc PR A 1 H10C H 0.3709 0.0602 0.9475 0.059 Uiso 0.783(12) 1 calc PR A 1 C11 C 0.5470(7) 0.0836(5) 0.9013(4) 0.0452(18) Uani 0.783(12) 1 d PU A 1 H11A H 0.5628 0.0549 0.9359 0.068 Uiso 0.783(12) 1 calc PR A 1 H11B H 0.6055 0.1148 0.8970 0.068 Uiso 0.783(12) 1 calc PR A 1 H11C H 0.5330 0.0507 0.8690 0.068 Uiso 0.783(12) 1 calc PR A 1 C109 C 0.4466(14) 0.1081(9) 0.9263(10) 0.039(3) Uani 0.217(12) 1 d PDU A 2 H109 H 0.4229 0.0785 0.9568 0.047 Uiso 0.217(12) 1 calc PR A 2 C110 C 0.3571(15) 0.1063(14) 0.8804(11) 0.054(5) Uani 0.217(12) 1 d PU A 2 H11D H 0.3648 0.1445 0.8529 0.081 Uiso 0.217(12) 1 calc PR A 2 H11E H 0.2941 0.1147 0.8963 0.081 Uiso 0.217(12) 1 calc PR A 2 H11F H 0.3536 0.0585 0.8619 0.081 Uiso 0.217(12) 1 calc PR A 2 C111 C 0.541(3) 0.0640(18) 0.9122(14) 0.042(5) Uani 0.217(12) 1 d PU A 2 H11G H 0.5188 0.0158 0.8975 0.063 Uiso 0.217(12) 1 calc PR A 2 H11H H 0.5914 0.0582 0.9463 0.063 Uiso 0.217(12) 1 calc PR A 2 H11I H 0.5727 0.0904 0.8838 0.063 Uiso 0.217(12) 1 calc PR A 2 C12 C 0.5198(3) 0.2808(2) 0.92320(17) 0.0530(10) Uani 1 1 d . A . H12 H 0.5399 0.3187 0.9527 0.064 Uiso 1 1 calc R . . C13 C 0.4364(3) 0.3144(3) 0.8821(2) 0.0652(12) Uani 1 1 d . . . H13A H 0.4626 0.3582 0.8658 0.098 Uiso 1 1 calc R A . H13B H 0.3790 0.3276 0.9015 0.098 Uiso 1 1 calc R . . H13C H 0.4132 0.2793 0.8522 0.098 Uiso 1 1 calc R . . C14 C 0.6167(3) 0.2652(3) 0.89693(18) 0.0591(11) Uani 1 1 d . . . H14A H 0.6000 0.2316 0.8652 0.089 Uiso 1 1 calc R A . H14B H 0.6689 0.2431 0.9252 0.089 Uiso 1 1 calc R . . H14C H 0.6430 0.3110 0.8837 0.089 Uiso 1 1 calc R . . B200 B 0.1367(2) 0.80201(17) 0.76702(13) 0.0240(6) Uani 1 1 d . . . C201 C 0.0883(2) 0.72525(15) 0.73948(11) 0.0250(6) Uani 1 1 d . . . C202 C -0.0027(2) 0.69603(16) 0.75347(12) 0.0274(6) Uani 1 1 d . . . H202 H -0.0347 0.7199 0.7812 0.033 Uiso 1 1 calc R . . C203 C -0.0477(2) 0.63323(16) 0.72808(12) 0.0282(6) Uani 1 1 d . . . C204 C -0.0036(2) 0.59695(16) 0.68753(12) 0.0304(6) Uani 1 1 d . . . H204 H -0.0330 0.5534 0.6709 0.036 Uiso 1 1 calc R . . C205 C 0.0845(2) 0.62569(16) 0.67180(11) 0.0293(6) Uani 1 1 d . . . C206 C 0.1290(2) 0.68877(16) 0.69692(11) 0.0269(6) Uani 1 1 d . . . H206 H 0.1889 0.7076 0.6847 0.032 Uiso 1 1 calc R . . C207 C -0.1455(3) 0.60666(18) 0.74443(15) 0.0403(8) Uani 1 1 d . . . F1 F -0.22347(18) 0.65017(15) 0.72595(15) 0.0863(9) Uani 1 1 d . . . F2 F -0.17211(19) 0.54060(12) 0.72475(11) 0.0658(7) Uani 1 1 d . . . F3 F -0.1425(2) 0.60245(17) 0.79981(10) 0.0799(9) Uani 1 1 d . . . C208 C 0.1351(3) 0.59023(19) 0.62734(14) 0.0419(8) Uani 1 1 d . . . F4 F 0.1374(3) 0.63421(15) 0.58351(9) 0.0890(10) Uani 1 1 d . . . F5 F 0.23261(17) 0.57395(14) 0.64499(10) 0.0624(6) Uani 1 1 d . . . F6 F 0.09107(18) 0.52835(13) 0.60801(10) 0.0663(7) Uani 1 1 d . . . C209 C 0.0665(2) 0.86456(15) 0.73086(11) 0.0256(6) Uani 1 1 d . . . C210 C -0.0250(2) 0.88973(16) 0.74620(12) 0.0296(6) Uani 1 1 d . . . H210 H -0.0435 0.8741 0.7809 0.036 Uiso 1 1 calc R . . C211 C -0.0899(2) 0.93692(18) 0.71247(13) 0.0354(7) Uani 1 1 d . . . C212 C -0.0646(3) 0.96225(18) 0.66214(13) 0.0380(7) Uani 1 1 d . . . H212 H -0.1081 0.9953 0.6394 0.046 Uiso 1 1 calc R . . C213 C 0.0259(2) 0.93806(16) 0.64572(12) 0.0326(7) Uani 1 1 d D B . C214 C 0.0894(2) 0.88991(15) 0.67896(12) 0.0283(6) Uani 1 1 d . . . H214 H 0.1502 0.8735 0.6663 0.034 Uiso 1 1 calc R . . C215 C -0.1911(3) 0.9576(2) 0.72837(16) 0.0521(10) Uani 1 1 d . . . F7 F -0.2138(2) 1.02790(16) 0.71837(12) 0.0796(8) Uani 1 1 d . . . F8 F -0.26713(18) 0.91937(19) 0.70009(13) 0.0888(10) Uani 1 1 d . . . F9 F -0.19504(19) 0.94808(18) 0.78287(10) 0.0814(9) Uani 1 1 d . . . C216 C 0.0530(3) 0.96400(16) 0.59076(14) 0.0428(8) Uani 1 1 d D . . F10 F 0.1371(8) 0.9344(7) 0.5765(5) 0.050(2) Uani 0.52(4) 1 d PDU B 1 F11 F 0.0702(11) 1.0360(3) 0.5911(4) 0.053(2) Uani 0.52(4) 1 d PDU B 1 F12 F -0.0224(8) 0.9520(10) 0.5482(3) 0.066(3) Uani 0.52(4) 1 d PDU B 1 F110 F 0.0434(13) 1.0349(3) 0.5830(5) 0.053(2) Uani 0.48(4) 1 d PDU B 2 F111 F -0.0014(11) 0.9303(8) 0.5473(3) 0.064(3) Uani 0.48(4) 1 d PDU B 2 F112 F 0.1516(6) 0.9492(9) 0.5858(5) 0.063(3) Uani 0.48(4) 1 d PDU B 2 C217 C 0.1305(2) 0.80742(15) 0.83441(11) 0.0239(6) Uani 1 1 d . . . C218 C 0.1389(2) 0.87497(16) 0.86191(11) 0.0253(6) Uani 1 1 d . . . H218 H 0.1424 0.9180 0.8403 0.030 Uiso 1 1 calc R . . C219 C 0.1424(2) 0.88139(16) 0.91972(11) 0.0259(6) Uani 1 1 d . . . C220 C 0.1372(2) 0.81989(17) 0.95278(12) 0.0283(6) Uani 1 1 d . . . H220 H 0.1385 0.8240 0.9922 0.034 Uiso 1 1 calc R . . C221 C 0.1301(2) 0.75234(17) 0.92659(12) 0.0282(6) Uani 1 1 d D C . C222 C 0.1270(2) 0.74616(16) 0.86857(12) 0.0263(6) Uani 1 1 d . . . H222 H 0.1223 0.6991 0.8519 0.032 Uiso 1 1 calc R . . C223 C 0.1523(2) 0.95409(17) 0.94821(12) 0.0305(6) Uani 1 1 d . . . F13 F 0.07459(16) 0.96703(12) 0.97694(9) 0.0495(5) Uani 1 1 d . . . F14 F 0.23709(15) 0.95893(11) 0.98623(8) 0.0465(5) Uani 1 1 d . . . F15 F 0.15400(16) 1.00937(10) 0.91265(8) 0.0440(5) Uani 1 1 d . . . C224 C 0.1243(2) 0.68608(17) 0.96199(12) 0.0354(7) Uani 1 1 d D . . F16 F 0.1941(3) 0.68331(19) 1.00715(14) 0.0712(13) Uani 0.760(5) 1 d PDU C 1 F17 F 0.0337(2) 0.67440(17) 0.97555(18) 0.0598(11) Uani 0.760(5) 1 d PDU C 1 F18 F 0.1435(3) 0.62228(14) 0.93495(13) 0.0576(10) Uani 0.760(5) 1 d PDU C 1 F116 F 0.0381(7) 0.6503(5) 0.9450(4) 0.070(3) Uani 0.240(5) 1 d PDU C 2 F117 F 0.1998(6) 0.6449(5) 0.9679(5) 0.064(3) Uani 0.240(5) 1 d PDU C 2 F118 F 0.1092(9) 0.7083(4) 1.0154(2) 0.055(3) Uani 0.240(5) 1 d PDU C 2 C225 C 0.2589(2) 0.80971(15) 0.76316(11) 0.0252(6) Uani 1 1 d . . . C226 C 0.3050(2) 0.87718(17) 0.75646(12) 0.0300(6) Uani 1 1 d . . . H226 H 0.2634 0.9196 0.7520 0.036 Uiso 1 1 calc R . . C227 C 0.4101(2) 0.88427(18) 0.75613(13) 0.0351(7) Uani 1 1 d D D . C228 C 0.4734(2) 0.82400(19) 0.76215(13) 0.0369(7) Uani 1 1 d . . . H228 H 0.5447 0.8286 0.7611 0.044 Uiso 1 1 calc R . . C229 C 0.4304(2) 0.75670(18) 0.76979(12) 0.0338(7) Uani 1 1 d D E . C230 C 0.3255(2) 0.74999(17) 0.77088(11) 0.0284(6) Uani 1 1 d . . . H230 H 0.2984 0.7032 0.7771 0.034 Uiso 1 1 calc R . . C231 C 0.4527(2) 0.9578(2) 0.74607(16) 0.0522(10) Uani 1 1 d D . . F19 F 0.5486(3) 0.9648(3) 0.7767(4) 0.077(2) Uani 0.615(17) 1 d PDU D 1 F20 F 0.4646(9) 0.9687(3) 0.6939(2) 0.085(2) Uani 0.615(17) 1 d PDU D 1 F21 F 0.3993(5) 1.0125(3) 0.7614(4) 0.0617(19) Uani 0.615(17) 1 d PDU D 1 F119 F 0.4121(12) 0.9814(6) 0.6929(3) 0.090(3) Uani 0.385(17) 1 d PDU D 2 F120 F 0.4215(10) 1.0082(4) 0.7791(5) 0.061(3) Uani 0.385(17) 1 d PDU D 2 F121 F 0.5500(5) 0.9629(5) 0.7472(7) 0.081(3) Uani 0.385(17) 1 d PDU D 2 C232 C 0.4951(3) 0.6896(2) 0.77366(13) 0.0482(9) Uani 1 1 d D . . F22 F 0.5925(3) 0.7054(3) 0.7991(3) 0.0675(16) Uani 0.681(16) 1 d PDU E 1 F23 F 0.5061(8) 0.6628(4) 0.72452(16) 0.078(2) Uani 0.681(16) 1 d PDU E 1 F24 F 0.4642(5) 0.6380(3) 0.8054(3) 0.0540(15) Uani 0.681(16) 1 d PDU E 1 F122 F 0.4587(11) 0.6442(5) 0.7288(4) 0.061(3) Uani 0.319(16) 1 d PDU E 2 F123 F 0.4863(12) 0.6477(6) 0.8174(4) 0.057(4) Uani 0.319(16) 1 d PDU E 2 F124 F 0.5913(5) 0.6988(6) 0.7704(8) 0.078(3) Uani 0.319(16) 1 d PDU E 2 C801 C 0.3965(15) 0.5538(11) 0.9223(9) 0.133(6) Uani 0.50 1 d PDU . . H80A H 0.3486 0.5598 0.9492 0.199 Uiso 0.50 1 calc PR . . H80B H 0.3588 0.5392 0.8857 0.199 Uiso 0.50 1 calc PR . . H80C H 0.4318 0.6000 0.9183 0.199 Uiso 0.50 1 calc PR . . C802 C 0.4685(12) 0.4999(9) 0.9417(3) 0.121(3) Uani 0.50 1 d PDU . . H80D H 0.4389 0.4515 0.9305 0.145 Uiso 0.50 1 calc PR . . H80E H 0.5295 0.5065 0.9229 0.145 Uiso 0.50 1 calc PR . . C803 C 0.5000 0.5000 1.0000 0.117(2) Uani 1 2 d SDU . . H80F H 0.4383 0.4854 1.0160 0.140 Uiso 0.50 1 calc PR . . H80G H 0.5112 0.5521 1.0098 0.140 Uiso 0.50 1 calc PR . . C804 C 0.5808(9) 0.4635(8) 1.0331(5) 0.113(3) Uani 0.50 1 d PDU . . H80H H 0.5611 0.4118 1.0262 0.135 Uiso 0.50 1 calc PR . . H80I H 0.6377 0.4714 1.0114 0.135 Uiso 0.50 1 calc PR . . C805 C 0.6331(14) 0.4607(10) 1.0884(6) 0.108(4) Uani 0.50 1 d PDU . . H80J H 0.6781 0.5032 1.0954 0.162 Uiso 0.50 1 calc PR . . H80K H 0.6741 0.4160 1.0935 0.162 Uiso 0.50 1 calc PR . . H80L H 0.5835 0.4609 1.1148 0.162 Uiso 0.50 1 calc PR . . 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 0.02147(13) 0.03043(14) 0.02822(13) -0.00103(9) 0.00442(9) 0.00393(9) P1 0.0220(4) 0.0419(4) 0.0300(4) -0.0027(3) 0.0055(3) 0.0030(3) B1 0.0322(19) 0.045(2) 0.042(2) -0.0037(17) 0.0136(16) 0.0030(16) N1 0.0253(13) 0.0409(16) 0.0472(16) 0.0064(12) 0.0032(11) 0.0070(11) C1 0.048(2) 0.056(2) 0.043(2) 0.0089(17) -0.0010(16) 0.0071(18) B2 0.0265(17) 0.0331(18) 0.046(2) 0.0011(16) 0.0025(15) 0.0013(15) N2 0.0246(13) 0.0383(15) 0.0531(17) 0.0039(13) 0.0121(12) 0.0041(11) C2 0.042(2) 0.044(2) 0.062(2) 0.0139(17) 0.0168(17) 0.0012(16) B3 0.0287(18) 0.034(2) 0.054(2) 0.0066(17) 0.0087(16) 0.0054(15) N3 0.0306(14) 0.0352(15) 0.0613(18) -0.0089(13) 0.0138(13) 0.0058(12) C3 0.045(2) 0.046(2) 0.075(3) -0.020(2) 0.0161(19) -0.0026(17) C4 0.0226(15) 0.0481(19) 0.0388(17) -0.0017(14) 0.0045(13) 0.0087(13) C5 0.0348(18) 0.051(2) 0.052(2) 0.0104(17) 0.0068(15) 0.0160(16) C6 0.0316(17) 0.056(2) 0.0336(16) 0.0094(15) 0.0034(13) 0.0123(16) C7 0.0274(16) 0.064(2) 0.0297(16) -0.0100(15) -0.0015(13) 0.0052(15) C8 0.0242(16) 0.063(2) 0.0428(19) -0.0111(17) -0.0015(14) 0.0013(15) C9 0.033(2) 0.044(3) 0.028(2) -0.004(2) 0.0094(19) -0.0005(19) C10 0.035(2) 0.039(3) 0.045(3) -0.010(2) 0.008(2) -0.0012(19) C11 0.039(3) 0.054(5) 0.045(4) -0.008(3) 0.017(3) 0.007(3) C109 0.033(6) 0.053(6) 0.032(6) -0.013(5) 0.010(5) 0.003(5) C110 0.051(7) 0.059(8) 0.053(8) -0.013(7) 0.008(7) 0.001(6) C111 0.046(8) 0.044(9) 0.041(9) -0.006(7) 0.018(7) 0.006(7) C12 0.040(2) 0.070(3) 0.052(2) 0.0152(19) 0.0162(17) -0.0023(18) C13 0.060(3) 0.068(3) 0.072(3) 0.030(2) 0.025(2) 0.004(2) C14 0.039(2) 0.090(3) 0.052(2) 0.006(2) 0.0174(17) -0.012(2) B200 0.0272(16) 0.0212(15) 0.0245(15) -0.0033(12) 0.0067(12) -0.0015(12) C201 0.0283(14) 0.0242(14) 0.0220(13) 0.0008(11) 0.0023(11) -0.0007(11) C202 0.0296(15) 0.0262(14) 0.0269(14) -0.0022(11) 0.0060(11) -0.0005(12) C203 0.0274(15) 0.0271(15) 0.0300(14) 0.0022(12) 0.0037(12) -0.0028(12) C204 0.0377(17) 0.0252(15) 0.0274(14) -0.0041(12) 0.0023(12) -0.0073(13) C205 0.0351(16) 0.0300(15) 0.0225(13) -0.0027(12) 0.0037(12) -0.0021(12) C206 0.0300(15) 0.0289(15) 0.0223(13) 0.0003(11) 0.0057(11) -0.0041(12) C207 0.0391(18) 0.0339(18) 0.050(2) -0.0033(15) 0.0130(15) -0.0086(14) F1 0.0341(12) 0.0659(17) 0.163(3) 0.0278(18) 0.0281(15) 0.0039(12) F2 0.0649(15) 0.0459(13) 0.0946(18) -0.0216(12) 0.0378(13) -0.0306(11) F3 0.0813(18) 0.113(2) 0.0538(14) -0.0131(14) 0.0383(13) -0.0483(16) C208 0.052(2) 0.0410(19) 0.0345(17) -0.0136(15) 0.0134(15) -0.0098(16) F4 0.168(3) 0.0749(18) 0.0339(12) 0.0018(12) 0.0465(16) 0.0124(19) F5 0.0488(13) 0.0799(17) 0.0647(14) -0.0286(12) 0.0282(11) -0.0068(12) F6 0.0646(15) 0.0655(15) 0.0736(15) -0.0478(13) 0.0260(12) -0.0209(12) C209 0.0282(14) 0.0237(14) 0.0251(13) -0.0047(11) 0.0046(11) -0.0034(11) C210 0.0294(15) 0.0314(16) 0.0279(14) -0.0049(12) 0.0039(12) -0.0018(12) C211 0.0322(16) 0.0373(17) 0.0353(16) -0.0100(14) 0.0008(13) 0.0045(13) C212 0.0435(19) 0.0311(17) 0.0360(17) -0.0013(13) -0.0050(14) 0.0062(14) C213 0.0435(18) 0.0247(15) 0.0292(15) -0.0016(12) 0.0036(13) -0.0038(13) C214 0.0301(15) 0.0260(15) 0.0291(14) -0.0021(12) 0.0051(12) -0.0031(12) C215 0.040(2) 0.064(3) 0.050(2) -0.0146(19) -0.0001(16) 0.0173(18) F7 0.0700(17) 0.0778(18) 0.0896(19) -0.0085(15) 0.0079(14) 0.0433(15) F8 0.0327(12) 0.123(2) 0.110(2) -0.051(2) 0.0075(13) -0.0021(14) F9 0.0575(15) 0.135(3) 0.0570(15) 0.0022(15) 0.0240(12) 0.0449(16) C216 0.055(2) 0.0372(19) 0.0351(17) 0.0060(14) 0.0027(16) -0.0021(16) F10 0.068(4) 0.050(4) 0.039(3) 0.005(3) 0.028(3) 0.016(3) F11 0.053(4) 0.051(3) 0.056(4) 0.012(2) 0.010(3) -0.020(3) F12 0.069(4) 0.093(6) 0.031(3) 0.014(3) -0.007(3) -0.030(4) F110 0.070(5) 0.033(3) 0.053(4) 0.017(2) 0.007(3) 0.012(3) F111 0.088(5) 0.072(5) 0.035(3) -0.016(3) 0.015(3) -0.026(4) F112 0.067(4) 0.065(5) 0.060(5) 0.019(4) 0.021(3) -0.010(3) C217 0.0201(13) 0.0263(14) 0.0257(13) -0.0031(11) 0.0039(10) -0.0008(11) C218 0.0223(13) 0.0272(14) 0.0265(14) -0.0005(11) 0.0038(11) 0.0005(11) C219 0.0202(13) 0.0304(15) 0.0270(14) -0.0032(12) 0.0041(11) 0.0043(11) C220 0.0200(13) 0.0408(17) 0.0243(14) 0.0022(12) 0.0045(11) -0.0004(12) C221 0.0183(13) 0.0349(16) 0.0309(15) 0.0041(12) 0.0022(11) -0.0021(12) C222 0.0217(13) 0.0267(14) 0.0303(15) 0.0003(12) 0.0030(11) -0.0014(11) C223 0.0268(15) 0.0374(17) 0.0266(14) -0.0022(13) 0.0016(12) 0.0068(13) F13 0.0464(12) 0.0542(13) 0.0511(12) -0.0178(10) 0.0180(9) 0.0119(10) F14 0.0407(11) 0.0441(11) 0.0478(11) -0.0164(9) -0.0158(9) 0.0102(9) F15 0.0628(13) 0.0298(10) 0.0380(10) -0.0052(8) 0.0027(9) 0.0000(9) C224 0.0319(16) 0.0401(18) 0.0340(16) 0.0089(14) 0.0045(13) -0.0058(14) F16 0.080(2) 0.061(2) 0.059(2) 0.0329(17) -0.0326(18) -0.0285(18) F17 0.0401(16) 0.0453(18) 0.103(3) 0.0294(18) 0.0400(17) 0.0078(13) F18 0.087(2) 0.0339(15) 0.0573(19) 0.0113(13) 0.0283(17) 0.0159(15) F116 0.070(5) 0.065(5) 0.072(5) 0.016(5) 0.001(5) -0.027(4) F117 0.062(5) 0.060(5) 0.075(6) 0.027(5) 0.022(4) 0.012(4) F118 0.089(6) 0.043(4) 0.035(4) 0.014(3) 0.020(4) -0.006(4) C225 0.0270(14) 0.0266(15) 0.0223(13) -0.0051(11) 0.0047(11) 0.0001(11) C226 0.0271(15) 0.0305(15) 0.0342(15) -0.0092(12) 0.0102(12) -0.0011(12) C227 0.0299(16) 0.0377(18) 0.0402(17) -0.0145(14) 0.0133(13) -0.0063(13) C228 0.0251(15) 0.052(2) 0.0344(16) -0.0127(15) 0.0055(12) 0.0027(14) C229 0.0352(17) 0.0437(18) 0.0223(14) -0.0050(13) 0.0037(12) 0.0107(14) C230 0.0331(16) 0.0300(15) 0.0226(14) -0.0018(12) 0.0054(11) 0.0037(12) C231 0.039(2) 0.046(2) 0.077(3) -0.022(2) 0.0293(19) -0.0140(17) F19 0.041(2) 0.073(3) 0.119(5) -0.027(3) 0.021(2) -0.027(2) F20 0.126(5) 0.058(3) 0.085(3) -0.014(2) 0.066(3) -0.039(3) F21 0.040(3) 0.039(2) 0.111(5) -0.019(2) 0.028(3) -0.0126(18) F119 0.100(6) 0.076(5) 0.098(5) 0.019(4) 0.026(4) -0.039(5) F120 0.062(5) 0.048(4) 0.072(5) -0.029(3) 0.011(4) -0.015(3) F121 0.048(4) 0.076(4) 0.130(6) -0.002(5) 0.052(4) -0.016(3) C232 0.048(2) 0.060(2) 0.0371(18) 0.0013(17) 0.0085(16) 0.0231(18) F22 0.039(2) 0.090(3) 0.072(4) 0.004(2) 0.0027(18) 0.0272(18) F23 0.112(4) 0.088(3) 0.0385(19) 0.0023(19) 0.025(2) 0.065(3) F24 0.059(3) 0.045(2) 0.056(3) 0.002(2) 0.004(2) 0.019(2) F122 0.075(6) 0.063(5) 0.046(4) -0.018(4) 0.007(4) 0.044(4) F123 0.079(6) 0.049(5) 0.037(4) -0.007(4) -0.007(4) 0.017(4) F124 0.054(4) 0.082(5) 0.102(7) 0.006(5) 0.028(4) 0.026(4) C801 0.133(7) 0.123(7) 0.141(7) -0.001(5) 0.016(5) 0.008(5) C802 0.119(5) 0.115(5) 0.126(5) -0.006(4) 0.015(4) 0.001(4) C803 0.117(4) 0.110(4) 0.124(4) 0.003(3) 0.023(3) 0.007(3) C804 0.114(4) 0.113(4) 0.111(4) -0.004(4) 0.012(4) 0.005(4) C805 0.108(6) 0.103(6) 0.110(6) -0.001(5) 0.007(5) 0.004(5) _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 C7 2.094(3) . ? Rh1 C6 2.096(3) . ? Rh1 P1 2.2354(8) . ? P1 C4 1.837(3) . ? P1 C9 1.849(4) . ? P1 C12 1.864(4) . ? P1 C109 1.900(10) . ? B1 N3 1.566(5) . ? B1 N2 1.567(5) . ? N1 C1 1.490(5) . ? N1 B3 1.573(5) . ? N1 B2 1.576(5) . ? B2 N2 1.567(5) . ? N2 C2 1.501(4) . ? B3 N3 1.570(5) . ? N3 C3 1.496(5) . ? C4 C8 1.525(5) . ? C4 C5 1.536(5) . ? C5 C6 1.517(5) . ? C6 C7 1.418(5) . ? C7 C8 1.518(5) . ? C9 C10 1.526(8) . ? C9 C11 1.527(10) . ? C109 C110 1.49(3) . ? C109 C111 1.57(4) . ? C12 C13 1.497(6) . ? C12 C14 1.539(5) . ? B200 C225 1.638(4) . ? B200 C217 1.640(4) . ? B200 C209 1.640(4) . ? B200 C201 1.643(4) . ? C201 C206 1.398(4) . ? C201 C202 1.404(4) . ? C202 C203 1.394(4) . ? C203 C204 1.381(4) . ? C203 C207 1.490(4) . ? C204 C205 1.382(4) . ? C205 C206 1.393(4) . ? C205 C208 1.495(4) . ? C207 F1 1.326(4) . ? C207 F2 1.329(4) . ? C207 F3 1.330(4) . ? C208 F6 1.327(4) . ? C208 F5 1.328(4) . ? C208 F4 1.332(4) . ? C209 C210 1.396(4) . ? C209 C214 1.408(4) . ? C210 C211 1.391(4) . ? C211 C212 1.385(5) . ? C211 C215 1.495(5) . ? C212 C213 1.388(5) . ? C213 C214 1.386(4) . ? C213 C216 1.500(4) . ? C215 F8 1.325(5) . ? C215 F9 1.332(5) . ? C215 F7 1.338(5) . ? C216 F110 1.317(5) . ? C216 F111 1.328(6) . ? C216 F10 1.328(5) . ? C216 F12 1.334(5) . ? C216 F11 1.340(6) . ? C216 F112 1.354(6) . ? C217 C222 1.397(4) . ? C217 C218 1.401(4) . ? C218 C219 1.391(4) . ? C219 C220 1.388(4) . ? C219 C223 1.496(4) . ? C220 C221 1.387(4) . ? C221 C222 1.396(4) . ? C221 C224 1.492(4) . ? C223 F15 1.329(4) . ? C223 F14 1.338(3) . ? C223 F13 1.344(4) . ? C224 F117 1.242(6) . ? C224 F17 1.307(4) . ? C224 F16 1.315(4) . ? C224 F116 1.325(6) . ? C224 F18 1.381(4) . ? C224 F118 1.392(6) . ? C225 C226 1.399(4) . ? C225 C230 1.400(4) . ? C226 C227 1.397(4) . ? C227 C228 1.381(5) . ? C227 C231 1.494(5) . ? C228 C229 1.383(5) . ? C229 C230 1.395(4) . ? C229 C232 1.493(5) . ? C231 F121 1.286(6) . ? C231 F20 1.304(5) . ? C231 F21 1.312(5) . ? C231 F120 1.326(6) . ? C231 F19 1.374(5) . ? C231 F119 1.379(6) . ? C232 F124 1.297(6) . ? C232 F23 1.310(4) . ? C232 F24 1.320(5) . ? C232 F123 1.322(6) . ? C232 F22 1.370(5) . ? C232 F122 1.390(6) . ? C801 C802 1.402(6) . ? C802 C803 1.402(6) . ? C803 C804 1.403(7) . ? C804 C805 1.402(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 C7 Rh1 C6 39.57(15) . . ? C7 Rh1 P1 82.90(10) . . ? C6 Rh1 P1 83.31(10) . . ? C4 P1 C9 110.4(2) . . ? C4 P1 C12 106.48(17) . . ? C9 P1 C12 102.6(3) . . ? C4 P1 C109 98.6(7) . . ? C9 P1 C109 21.2(7) . . ? C12 P1 C109 123.5(8) . . ? C4 P1 Rh1 97.76(10) . . ? C9 P1 Rh1 123.24(17) . . ? C12 P1 Rh1 115.46(14) . . ? C109 P1 Rh1 109.9(7) . . ? N3 B1 N2 110.8(3) . . ? C1 N1 B3 111.8(3) . . ? C1 N1 B2 110.2(3) . . ? B3 N1 B2 111.7(3) . . ? N2 B2 N1 108.7(3) . . ? C2 N2 B1 110.7(3) . . ? C2 N2 B2 110.0(3) . . ? B1 N2 B2 112.9(3) . . ? N3 B3 N1 108.7(3) . . ? C3 N3 B1 110.2(3) . . ? C3 N3 B3 110.7(3) . . ? B1 N3 B3 112.6(3) . . ? C8 C4 C5 101.4(3) . . ? C8 C4 P1 104.4(2) . . ? C5 C4 P1 103.9(2) . . ? C6 C5 C4 100.8(3) . . ? C7 C6 C5 107.9(3) . . ? C7 C6 Rh1 70.16(19) . . ? C5 C6 Rh1 115.4(2) . . ? C6 C7 C8 108.6(3) . . ? C6 C7 Rh1 70.27(18) . . ? C8 C7 Rh1 116.2(2) . . ? C7 C8 C4 100.5(3) . . ? C10 C9 C11 110.7(5) . . ? C10 C9 P1 111.5(4) . . ? C11 C9 P1 112.5(4) . . ? C110 C109 C111 113.4(19) . . ? C110 C109 P1 115.5(15) . . ? C111 C109 P1 115.7(16) . . ? C13 C12 C14 112.3(3) . . ? C13 C12 P1 113.3(3) . . ? C14 C12 P1 112.9(3) . . ? C225 B200 C217 104.4(2) . . ? C225 B200 C209 113.1(2) . . ? C217 B200 C209 111.9(2) . . ? C225 B200 C201 112.2(2) . . ? C217 B200 C201 112.1(2) . . ? C209 B200 C201 103.3(2) . . ? C206 C201 C202 115.6(3) . . ? C206 C201 B200 122.4(2) . . ? C202 C201 B200 121.7(2) . . ? C203 C202 C201 122.3(3) . . ? C204 C203 C202 120.7(3) . . ? C204 C203 C207 120.4(3) . . ? C202 C203 C207 118.9(3) . . ? C203 C204 C205 118.3(3) . . ? C204 C205 C206 121.0(3) . . ? C204 C205 C208 121.2(3) . . ? C206 C205 C208 117.8(3) . . ? C205 C206 C201 122.1(3) . . ? F1 C207 F2 106.2(3) . . ? F1 C207 F3 106.0(3) . . ? F2 C207 F3 105.7(3) . . ? F1 C207 C203 112.1(3) . . ? F2 C207 C203 113.4(3) . . ? F3 C207 C203 112.9(3) . . ? F6 C208 F5 105.8(3) . . ? F6 C208 F4 107.5(3) . . ? F5 C208 F4 104.6(3) . . ? F6 C208 C205 113.7(3) . . ? F5 C208 C205 112.8(3) . . ? F4 C208 C205 111.7(3) . . ? C210 C209 C214 115.9(3) . . ? C210 C209 B200 122.3(2) . . ? C214 C209 B200 121.4(2) . . ? C211 C210 C209 122.3(3) . . ? C212 C211 C210 120.6(3) . . ? C212 C211 C215 118.9(3) . . ? C210 C211 C215 120.4(3) . . ? C211 C212 C213 118.4(3) . . ? C214 C213 C212 120.8(3) . . ? C214 C213 C216 120.4(3) . . ? C212 C213 C216 118.8(3) . . ? C213 C214 C209 122.0(3) . . ? F8 C215 F9 107.3(4) . . ? F8 C215 F7 106.5(3) . . ? F9 C215 F7 105.2(3) . . ? F8 C215 C211 111.9(3) . . ? F9 C215 C211 112.9(3) . . ? F7 C215 C211 112.5(4) . . ? F110 C216 F111 108.6(5) . . ? F110 C216 F10 115.6(7) . . ? F111 C216 F10 88.9(7) . . ? F110 C216 F12 90.6(7) . . ? F111 C216 F12 21.1(7) . . ? F10 C216 F12 107.0(5) . . ? F110 C216 F11 16.3(7) . . ? F111 C216 F11 122.3(7) . . ? F10 C216 F11 104.8(5) . . ? F12 C216 F11 105.9(5) . . ? F110 C216 F112 104.9(5) . . ? F111 C216 F112 104.5(5) . . ? F10 C216 F112 16.4(8) . . ? F12 C216 F112 121.1(7) . . ? F11 C216 F112 91.9(8) . . ? F110 C216 C213 114.0(5) . . ? F111 C216 C213 112.0(5) . . ? F10 C216 C213 114.8(4) . . ? F12 C216 C213 111.9(4) . . ? F11 C216 C213 111.7(4) . . ? F112 C216 C213 112.1(5) . . ? C222 C217 C218 116.1(2) . . ? C222 C217 B200 123.0(2) . . ? C218 C217 B200 120.6(2) . . ? C219 C218 C217 122.4(3) . . ? C220 C219 C218 120.5(3) . . ? C220 C219 C223 118.0(2) . . ? C218 C219 C223 121.5(3) . . ? C221 C220 C219 118.1(3) . . ? C220 C221 C222 121.1(3) . . ? C220 C221 C224 118.2(3) . . ? C222 C221 C224 120.6(3) . . ? C221 C222 C217 121.7(3) . . ? F15 C223 F14 107.2(3) . . ? F15 C223 F13 106.6(2) . . ? F14 C223 F13 105.2(2) . . ? F15 C223 C219 113.2(2) . . ? F14 C223 C219 112.2(2) . . ? F13 C223 C219 111.9(3) . . ? F117 C224 F17 128.5(5) . . ? F117 C224 F16 55.3(5) . . ? F17 C224 F16 110.0(3) . . ? F117 C224 F116 111.9(6) . . ? F17 C224 F116 38.5(5) . . ? F16 C224 F116 134.3(5) . . ? F117 C224 F18 48.5(6) . . ? F17 C224 F18 102.7(3) . . ? F16 C224 F18 101.6(3) . . ? F116 C224 F18 69.2(5) . . ? F117 C224 F118 107.2(5) . . ? F17 C224 F118 63.3(4) . . ? F16 C224 F118 55.1(4) . . ? F116 C224 F118 101.1(5) . . ? F18 C224 F118 138.2(4) . . ? F117 C224 C221 116.8(4) . . ? F17 C224 C221 113.9(3) . . ? F16 C224 C221 114.4(3) . . ? F116 C224 C221 110.1(4) . . ? F18 C224 C221 113.0(2) . . ? F118 C224 C221 108.5(4) . . ? C226 C225 C230 115.5(3) . . ? C226 C225 B200 122.2(3) . . ? C230 C225 B200 122.1(3) . . ? C227 C226 C225 122.3(3) . . ? C228 C227 C226 120.9(3) . . ? C228 C227 C231 120.1(3) . . ? C226 C227 C231 119.0(3) . . ? C227 C228 C229 118.2(3) . . ? C228 C229 C230 120.8(3) . . ? C228 C229 C232 120.0(3) . . ? C230 C229 C232 119.2(3) . . ? C229 C230 C225 122.4(3) . . ? F121 C231 F20 75.1(5) . . ? F121 C231 F21 121.2(6) . . ? F20 C231 F21 107.6(5) . . ? F121 C231 F120 109.7(5) . . ? F20 C231 F120 124.3(6) . . ? F21 C231 F120 21.2(6) . . ? F121 C231 F19 30.9(5) . . ? F20 C231 F19 105.4(4) . . ? F21 C231 F19 105.6(4) . . ? F120 C231 F19 87.6(6) . . ? F121 C231 F119 104.1(5) . . ? F20 C231 F119 31.3(5) . . ? F21 C231 F119 82.6(6) . . ? F120 C231 F119 103.0(5) . . ? F19 C231 F119 131.7(5) . . ? F121 C231 C227 117.5(5) . . ? F20 C231 C227 113.5(3) . . ? F21 C231 C227 114.3(4) . . ? F120 C231 C227 111.9(5) . . ? F19 C231 C227 109.8(4) . . ? F119 C231 C227 109.3(4) . . ? F124 C232 F23 75.5(6) . . ? F124 C232 F24 121.4(7) . . ? F23 C232 F24 109.9(4) . . ? F124 C232 F123 109.2(6) . . ? F23 C232 F123 122.4(6) . . ? F24 C232 F123 18.2(7) . . ? F124 C232 F22 30.2(6) . . ? F23 C232 F22 104.9(4) . . ? F24 C232 F22 104.2(4) . . ? F123 C232 F22 87.6(7) . . ? F124 C232 F122 104.9(5) . . ? F23 C232 F122 31.4(5) . . ? F24 C232 F122 85.3(6) . . ? F123 C232 F122 102.0(6) . . ? F22 C232 F122 131.6(5) . . ? F124 C232 C229 116.6(5) . . ? F23 C232 C229 113.2(3) . . ? F24 C232 C229 113.7(3) . . ? F123 C232 C229 114.2(5) . . ? F22 C232 C229 110.2(3) . . ? F122 C232 C229 108.5(4) . . ? C803 C802 C801 114.6(13) . . ? C802 C803 C804 130.8(8) . . ? C805 C804 C803 141.2(14) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.699 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.067 # Attachment 'C6H5F.cif' data_C6H5F _database_code_depnum_ccdc_archive 'CCDC 767951' #TrackingRef 'C6H5F.cif' #----------------------------- # [Rh(C6H5F)PiPr2(C5H7)]BArF4 #----------------------------- # start Validation Reply Form _vrf_PLAT410_C6H5F ; PROBLEM: Short Intra H...H Contact H11B .. H115 .. 1.74 Ang. RESPONSE: The structure contains a disordered phosphine ligand - the short contact occurs for the minor disordered component (41%) only ; _vrf_PLAT242_C6H5F ; PROBLEM: Check Low Ueq as Compared to Neighbors for C25 PROBLEM: Check Low Ueq as Compared to Neighbors for C32 RESPONSE: The anion contains a significant degree of disorder. See details in supplementary information or _refine_special_details. ; _vrf_PLAT431_C6H5F ; PROBLEM: Short Inter HL..A Contact F3 .. F1B .. 2.57 Ang. RESPONSE: The structure contains a disordered fluorobenzene ligand - the short contact occurs for the minor disordered component (12%) only ; _vrf_PLAT301_C6H5F ; PROBLEM: Note Main Residue Disorder .................... 14.00 Perc. RESPONSE: The structure contains a significant degree of disorder. See details in supplementary information or _refine_special_details. ; # end Validation Reply Form #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic . _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety 'C32 H12 B F24, C17 H26 F P Rh' _chemical_formula_sum 'C49 H38 B F25 P Rh' _chemical_formula_weight 1246.48 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' 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 P2(1)2(1)2(1) 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 12.51030(10) _cell_length_b 19.3211(2) _cell_length_c 20.3470(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4918.13(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6120 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2488 _exptl_absorpt_coefficient_mu 0.511 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.961 _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 'horizonally mounted graphite crystal' _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 9979 _diffrn_reflns_av_R_equivalents 0.078 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9979 _reflns_number_gt 8242 _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 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Solved with sir2004. Alkene protons were located on the Fourier difference map and the 1,2 and 1,3- C-H distances restrained; their isotropic displacement parameters were fixed to ride on the parent atoms. Disorder in the phosphine ligand was treated by modelling the appropriate substituents over two sites and restraining their geometry. Disorder in the fluorobenzene ligand was treated by modelling the fluorine atom over two sites and restraining the 1,2 and 1,3-distances. Rotational disorder in the CF3 groups of the anion was treated by modelling the fluorine atoms over two sites 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^)+(0.0475P)^2^+3.5272P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(2) _refine_ls_number_reflns 9979 _refine_ls_number_parameters 805 _refine_ls_number_restraints 409 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0986 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.90094(2) 1.041932(16) 0.560529(17) 0.02945(9) Uani 1 1 d D . . P1 P 0.98948(9) 0.94068(6) 0.55526(6) 0.0366(3) Uani 1 1 d . B . F1A F 0.6783(3) 1.0909(2) 0.6403(2) 0.0754(12) Uani 0.8791(11) 1 d PDU A 2 F1B F 0.7453(18) 0.9846(9) 0.4433(9) 0.068(7) Uani 0.1209(11) 1 d PDU A 3 C1 C 0.7331(4) 1.0862(3) 0.5856(3) 0.0454(13) Uani 1 1 d D B 1 H1 H 0.6964 1.0877 0.6265 0.055 Uiso 0.1209(11) 1 calc PR A 3 C2 C 0.7178(3) 1.0306(2) 0.5454(3) 0.0490(14) Uani 1 1 d D B 1 H2 H 0.6728 0.9933 0.5578 0.059 Uiso 1 1 calc R B 1 C3 C 0.7728(4) 1.0308(3) 0.4830(3) 0.0528(15) Uani 1 1 d D B 1 H3 H 0.7684 0.9919 0.4547 0.063 Uiso 0.8791(11) 1 calc PR A 2 C4 C 0.8338(4) 1.0898(3) 0.4643(3) 0.0544(15) Uani 1 1 d D B 1 H4 H 0.8647 1.0924 0.4217 0.065 Uiso 1 1 calc R B 1 C5 C 0.8474(4) 1.1429(3) 0.5084(3) 0.0498(13) Uani 1 1 d . B 1 H5 H 0.8902 1.1816 0.4966 0.060 Uiso 1 1 calc R B 1 C6 C 0.8005(4) 1.1409(2) 0.5689(3) 0.0480(13) Uani 1 1 d D B 1 H6 H 0.8139 1.1768 0.5998 0.058 Uiso 1 1 calc R B 1 C7 C 1.0915(4) 0.9595(3) 0.6169(2) 0.0456(11) Uani 1 1 d . . . H7 H 1.1443 0.9215 0.6246 0.055 Uiso 1 1 calc R B . C8 C 1.0268(5) 0.9813(3) 0.6774(3) 0.0563(14) Uani 1 1 d D B . H8A H 0.9706 0.9470 0.6882 0.068 Uiso 1 1 calc R . . H8B H 1.0733 0.9883 0.7162 0.068 Uiso 1 1 calc R . . C9 C 0.9789(5) 1.0494(3) 0.6532(3) 0.0546(13) Uani 1 1 d DU B . H9 H 0.931(3) 1.074(2) 0.6813(17) 0.065 Uiso 1 1 d D . . C10 C 1.0462(5) 1.0762(3) 0.6044(4) 0.0621(16) Uani 1 1 d DU B . H10 H 1.053(3) 1.1238(7) 0.591(2) 0.074 Uiso 1 1 d D . . C11 C 1.1396(4) 1.0278(3) 0.5946(4) 0.0758(19) Uani 1 1 d DU B . H11A H 1.2013 1.0413 0.6223 0.091 Uiso 1 1 calc R . . H11B H 1.1621 1.0261 0.5480 0.091 Uiso 1 1 calc R . . C12 C 0.9035(7) 0.8662(4) 0.5951(4) 0.0360(17) Uani 0.593(8) 1 d PDU B 1 H12 H 0.8594 0.8881 0.6305 0.043 Uiso 0.593(8) 1 calc PR B 1 C13 C 0.9664(10) 0.8086(8) 0.6272(7) 0.054(3) Uani 0.593(8) 1 d PDU B 1 H13A H 0.9175 0.7780 0.6512 0.082 Uiso 0.593(8) 1 calc PR B 1 H13B H 1.0184 0.8284 0.6579 0.082 Uiso 0.593(8) 1 calc PR B 1 H13C H 1.0041 0.7820 0.5934 0.082 Uiso 0.593(8) 1 calc PR B 1 C14 C 0.8237(9) 0.8370(6) 0.5431(6) 0.058(3) Uani 0.593(8) 1 d PDU B 1 H14A H 0.8638 0.8148 0.5075 0.086 Uiso 0.593(8) 1 calc PR B 1 H14B H 0.7805 0.8749 0.5253 0.086 Uiso 0.593(8) 1 calc PR B 1 H14C H 0.7768 0.8028 0.5640 0.086 Uiso 0.593(8) 1 calc PR B 1 C112 C 0.9387(10) 0.8611(6) 0.5615(8) 0.043(3) Uani 0.407(8) 1 d PDU B 2 H112 H 0.9526 0.8396 0.5176 0.052 Uiso 0.407(8) 1 calc PR B 2 C113 C 0.9943(16) 0.8130(14) 0.6103(11) 0.054(3) Uani 0.407(8) 1 d PDU B 2 H11C H 0.9485 0.7729 0.6190 0.082 Uiso 0.407(8) 1 calc PR B 2 H11D H 1.0075 0.8380 0.6514 0.082 Uiso 0.407(8) 1 calc PR B 2 H11E H 1.0624 0.7973 0.5917 0.082 Uiso 0.407(8) 1 calc PR B 2 C114 C 0.8170(12) 0.8574(10) 0.5695(10) 0.058(3) Uani 0.407(8) 1 d PDU B 2 H11F H 0.7943 0.8088 0.5698 0.086 Uiso 0.407(8) 1 calc PR B 2 H11G H 0.7825 0.8816 0.5329 0.086 Uiso 0.407(8) 1 calc PR B 2 H11H H 0.7964 0.8794 0.6111 0.086 Uiso 0.407(8) 1 calc PR B 2 C15 C 1.0352(7) 0.9001(5) 0.4795(4) 0.046(2) Uani 0.593(8) 1 d PDU B 1 H15 H 0.9901 0.8589 0.4687 0.055 Uiso 0.593(8) 1 calc PR B 1 C16 C 1.1643(10) 0.8773(9) 0.4864(11) 0.067(4) Uani 0.593(8) 1 d PDU B 1 H16A H 1.1926 0.8656 0.4429 0.101 Uiso 0.593(8) 1 calc PR B 1 H16B H 1.1703 0.8371 0.5155 0.101 Uiso 0.593(8) 1 calc PR B 1 H16C H 1.2051 0.9160 0.5049 0.101 Uiso 0.593(8) 1 calc PR B 1 C17 C 1.0409(11) 0.9492(8) 0.4213(7) 0.054(3) Uani 0.593(8) 1 d PDU B 1 H17A H 1.0930 0.9858 0.4305 0.081 Uiso 0.593(8) 1 calc PR B 1 H17B H 0.9704 0.9699 0.4139 0.081 Uiso 0.593(8) 1 calc PR B 1 H17C H 1.0629 0.9235 0.3821 0.081 Uiso 0.593(8) 1 calc PR B 1 C115 C 1.0844(9) 0.9412(6) 0.4791(5) 0.039(3) Uani 0.407(8) 1 d PDU B 2 H115 H 1.1379 0.9796 0.4765 0.047 Uiso 0.407(8) 1 calc PR B 2 C116 C 1.1331(17) 0.8596(11) 0.4873(17) 0.067(4) Uani 0.407(8) 1 d PDU B 2 H11I H 1.0867 0.8331 0.5169 0.101 Uiso 0.407(8) 1 calc PR B 2 H11J H 1.2055 0.8616 0.5056 0.101 Uiso 0.407(8) 1 calc PR B 2 H11K H 1.1350 0.8371 0.4442 0.101 Uiso 0.407(8) 1 calc PR B 2 C117 C 1.0118(17) 0.9310(12) 0.4196(10) 0.054(3) Uani 0.407(8) 1 d PDU B 2 H11L H 1.0556 0.9214 0.3807 0.081 Uiso 0.407(8) 1 calc PR B 2 H11M H 0.9698 0.9731 0.4122 0.081 Uiso 0.407(8) 1 calc PR B 2 H11N H 0.9635 0.8920 0.4276 0.081 Uiso 0.407(8) 1 calc PR B 2 B1 B 0.6223(3) 0.7050(2) 0.7734(2) 0.0233(9) Uani 1 1 d . . . C18 C 0.5345(3) 0.7252(2) 0.7165(2) 0.0252(9) Uani 1 1 d . . . C19 C 0.4317(3) 0.6959(2) 0.7168(2) 0.0261(9) Uani 1 1 d . . . H19 H 0.4136 0.6646 0.7511 0.031 Uiso 1 1 calc R . . C20 C 0.3559(3) 0.7104(2) 0.6696(2) 0.0294(9) Uani 1 1 d . . . C21 C 0.3798(3) 0.7555(2) 0.6184(2) 0.0346(10) Uani 1 1 d . . . H21 H 0.3276 0.7662 0.5861 0.042 Uiso 1 1 calc R . . C22 C 0.4793(4) 0.7841(2) 0.6154(2) 0.0346(10) Uani 1 1 d . . . C23 C 0.5568(3) 0.7684(2) 0.6632(2) 0.0302(9) Uani 1 1 d . . . H23 H 0.6263 0.7878 0.6592 0.036 Uiso 1 1 calc R . . C24 C 0.2477(4) 0.6773(3) 0.6718(2) 0.0402(11) Uani 1 1 d . . . F2 F 0.1701(2) 0.7210(2) 0.6583(2) 0.0895(13) Uani 1 1 d U . . F3 F 0.2391(3) 0.6264(2) 0.62654(18) 0.0787(11) Uani 1 1 d U . . F4 F 0.2246(2) 0.64758(16) 0.72851(15) 0.0510(7) Uani 1 1 d U . . C25 C 0.5067(4) 0.8333(3) 0.5621(3) 0.0541(14) Uani 1 1 d . . . F5 F 0.4216(3) 0.8602(3) 0.5340(3) 0.146(2) Uani 1 1 d U . . F6 F 0.5656(4) 0.8022(2) 0.51441(16) 0.0975(15) Uani 1 1 d U . . F7 F 0.5662(3) 0.88590(16) 0.58066(16) 0.0639(9) Uani 1 1 d U . . C26 C 0.6744(3) 0.6311(2) 0.74829(19) 0.0244(8) Uani 1 1 d . . . C27 C 0.6293(3) 0.5665(2) 0.7618(2) 0.0275(9) Uani 1 1 d . . . H27 H 0.5673 0.5644 0.7887 0.033 Uiso 1 1 calc R . . C28 C 0.6719(3) 0.5051(2) 0.7375(2) 0.0284(9) Uani 1 1 d . . . C29 C 0.7611(4) 0.5060(2) 0.6975(2) 0.0311(9) Uani 1 1 d . . . H29 H 0.7905 0.4641 0.6809 0.037 Uiso 1 1 calc R . . C30 C 0.8070(3) 0.5695(2) 0.68221(19) 0.0276(9) Uani 1 1 d . C . C31 C 0.7637(3) 0.6304(2) 0.70670(19) 0.0262(8) Uani 1 1 d . . . H31 H 0.7958 0.6732 0.6949 0.031 Uiso 1 1 calc R . . C32 C 0.6246(4) 0.4370(2) 0.7544(3) 0.0439(12) Uani 1 1 d . . . F8 F 0.5666(4) 0.4109(2) 0.7047(2) 0.1029(15) Uani 1 1 d U . . F9 F 0.6917(3) 0.3892(2) 0.7659(3) 0.128(2) Uani 1 1 d U . . F10 F 0.5534(4) 0.43938(18) 0.8011(2) 0.1138(18) Uani 1 1 d U . . C33 C 0.9052(5) 0.5717(3) 0.6407(3) 0.0495(13) Uani 1 1 d . . . F11 F 0.9780(5) 0.5238(4) 0.6575(3) 0.0758(19) Uani 0.714(6) 1 d PDU C 1 F12 F 0.8817(4) 0.5542(3) 0.57732(19) 0.0724(16) Uani 0.714(6) 1 d PDU C 1 F13 F 0.9476(5) 0.6320(3) 0.6349(4) 0.085(2) Uani 0.714(6) 1 d PDU C 1 F111 F 0.9073(13) 0.6179(9) 0.5977(7) 0.081(3) Uani 0.286(6) 1 d PDU C 2 F112 F 0.9904(9) 0.6039(7) 0.6837(7) 0.065(3) Uani 0.286(6) 1 d PDU C 2 F113 F 0.9520(16) 0.5150(10) 0.6313(9) 0.077(4) Uani 0.286(6) 1 d PDU C 2 C34 C 0.5629(3) 0.6997(2) 0.84478(19) 0.0234(8) Uani 1 1 d . . . C35 C 0.4847(3) 0.7482(2) 0.8632(2) 0.0251(8) Uani 1 1 d . . . H35 H 0.4657 0.7833 0.8327 0.030 Uiso 1 1 calc R . . C36 C 0.4344(3) 0.7472(2) 0.92360(19) 0.0262(9) Uani 1 1 d . . . C37 C 0.4565(3) 0.6955(2) 0.9687(2) 0.0282(9) Uani 1 1 d . . . H37 H 0.4193 0.6932 1.0094 0.034 Uiso 1 1 calc R . . C38 C 0.5345(3) 0.6472(2) 0.95303(18) 0.0253(8) Uani 1 1 d . . . C39 C 0.5877(3) 0.6501(2) 0.89244(19) 0.0262(8) Uani 1 1 d . . . H39 H 0.6425 0.6174 0.8835 0.031 Uiso 1 1 calc R . . C40 C 0.3532(3) 0.8018(2) 0.9394(2) 0.0311(9) Uani 1 1 d . . . F17 F 0.4914(3) 0.58563(17) 1.04934(16) 0.0673(10) Uani 1 1 d U . . F18 F 0.6565(2) 0.59145(17) 1.02292(17) 0.0648(10) Uani 1 1 d U . . F19 F 0.5501(3) 0.52805(14) 0.96939(14) 0.0563(8) Uani 1 1 d U . . C41 C 0.5591(3) 0.5890(2) 0.9986(2) 0.0297(9) Uani 1 1 d . . . F14 F 0.2752(2) 0.80449(16) 0.89478(15) 0.0543(8) Uani 1 1 d U . . F15 F 0.3961(2) 0.86459(12) 0.94125(16) 0.0543(7) Uani 1 1 d U . . F16 F 0.3044(3) 0.79167(17) 0.99691(15) 0.0632(9) Uani 1 1 d U . . C42 C 0.7148(3) 0.76466(19) 0.78296(18) 0.0238(8) Uani 1 1 d . . . C43 C 0.6912(3) 0.8354(2) 0.7760(2) 0.0287(9) Uani 1 1 d . . . H43 H 0.6207 0.8486 0.7641 0.034 Uiso 1 1 calc R . . C44 C 0.7680(3) 0.8872(2) 0.7860(2) 0.0302(9) Uani 1 1 d . D . C45 C 0.8709(3) 0.8698(2) 0.8031(2) 0.0325(10) Uani 1 1 d . . . H45 H 0.9234 0.9046 0.8097 0.039 Uiso 1 1 calc R . . C46 C 0.8967(3) 0.8005(2) 0.81051(18) 0.0265(8) Uani 1 1 d . . . C47 C 0.8197(3) 0.7494(2) 0.80176(19) 0.0270(9) Uani 1 1 d . . . H47 H 0.8390 0.7024 0.8088 0.032 Uiso 1 1 calc R . . C48 C 0.7374(4) 0.9602(3) 0.7751(3) 0.0425(11) Uani 1 1 d . . . F20 F 0.6467(9) 0.9806(10) 0.8050(7) 0.051(3) Uani 0.591(16) 1 d PDU D 1 F21 F 0.7279(9) 0.9735(5) 0.7153(5) 0.067(2) Uani 0.591(16) 1 d PDU D 1 F22 F 0.8169(6) 1.0026(3) 0.8004(7) 0.066(2) Uani 0.591(16) 1 d PDU D 1 F120 F 0.8127(8) 1.0034(5) 0.7599(9) 0.062(3) Uani 0.409(16) 1 d PDU D 2 F121 F 0.6720(14) 0.9821(14) 0.8190(9) 0.052(4) Uani 0.409(16) 1 d PDU D 2 F122 F 0.6782(12) 0.9685(7) 0.7124(7) 0.060(3) Uani 0.409(16) 1 d PDU D 2 C49 C 1.0090(4) 0.7796(2) 0.8265(2) 0.0368(11) Uani 1 1 d . . . F23 F 1.0802(2) 0.82995(17) 0.81489(19) 0.0707(10) Uani 1 1 d U . . F24 F 1.0221(2) 0.76123(17) 0.88935(14) 0.0551(8) Uani 1 1 d U . . F25 F 1.0414(2) 0.72512(17) 0.79185(15) 0.0571(8) Uani 1 1 d U . . 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 0.02451(14) 0.02957(16) 0.03428(16) 0.00305(15) -0.00156(15) 0.00055(14) P1 0.0357(5) 0.0452(7) 0.0289(6) -0.0032(5) -0.0044(5) 0.0153(5) F1A 0.073(3) 0.081(3) 0.072(3) 0.016(2) 0.019(2) 0.032(2) F1B 0.064(10) 0.059(10) 0.081(11) -0.001(9) -0.013(9) 0.008(8) C1 0.031(2) 0.048(3) 0.058(3) 0.003(2) 0.011(2) 0.015(2) C2 0.020(2) 0.034(3) 0.093(4) 0.016(3) -0.012(2) -0.0013(18) C3 0.052(3) 0.045(3) 0.061(3) -0.015(3) -0.036(3) 0.015(2) C4 0.054(3) 0.067(4) 0.042(3) 0.021(3) -0.007(2) 0.013(3) C5 0.043(3) 0.037(3) 0.070(4) 0.012(3) 0.000(3) 0.005(2) C6 0.038(2) 0.029(2) 0.076(4) -0.001(3) -0.007(3) 0.0079(19) C7 0.035(2) 0.046(3) 0.056(3) 0.008(2) -0.011(2) 0.007(3) C8 0.074(4) 0.060(3) 0.035(3) -0.004(2) -0.023(3) 0.015(3) C9 0.065(3) 0.042(3) 0.057(3) -0.015(3) -0.023(3) 0.009(3) C10 0.044(3) 0.044(3) 0.098(4) 0.005(3) -0.032(3) -0.011(2) C11 0.034(3) 0.071(4) 0.123(5) 0.025(4) -0.025(3) -0.013(3) C12 0.042(4) 0.026(3) 0.039(4) -0.001(3) 0.012(4) 0.000(3) C13 0.075(7) 0.042(4) 0.046(7) 0.018(5) 0.009(5) 0.006(5) C14 0.046(3) 0.054(6) 0.073(7) -0.008(5) 0.000(5) -0.006(4) C112 0.051(6) 0.031(5) 0.047(6) 0.000(6) 0.001(6) -0.010(4) C113 0.075(7) 0.042(4) 0.046(7) 0.018(5) 0.009(5) 0.006(5) C114 0.046(3) 0.054(6) 0.073(7) -0.008(5) 0.000(5) -0.006(4) C15 0.046(5) 0.055(5) 0.037(4) -0.001(4) 0.009(4) 0.004(4) C16 0.047(7) 0.091(7) 0.065(4) -0.010(6) 0.015(6) 0.034(6) C17 0.063(7) 0.065(7) 0.035(3) 0.008(4) 0.020(4) -0.001(5) C115 0.027(5) 0.052(6) 0.039(5) -0.006(5) 0.010(4) -0.004(5) C116 0.047(7) 0.091(7) 0.065(4) -0.010(6) 0.015(6) 0.034(6) C117 0.063(7) 0.065(7) 0.035(3) 0.008(4) 0.020(4) -0.001(5) B1 0.021(2) 0.019(2) 0.030(2) 0.0004(18) 0.0004(17) -0.0003(16) C18 0.026(2) 0.024(2) 0.025(2) 0.0022(16) 0.0008(16) 0.0025(16) C19 0.028(2) 0.022(2) 0.029(2) 0.0015(17) 0.0000(16) -0.0003(15) C20 0.0267(19) 0.030(2) 0.032(2) 0.0011(18) -0.0031(17) 0.0007(17) C21 0.036(3) 0.030(2) 0.038(2) 0.0047(19) -0.0093(18) 0.0023(18) C22 0.038(2) 0.036(2) 0.030(2) 0.0138(19) -0.0008(19) 0.000(2) C23 0.026(2) 0.035(2) 0.029(2) 0.0078(18) -0.0015(17) -0.0037(17) C24 0.030(2) 0.041(3) 0.049(3) 0.005(2) -0.008(2) -0.005(2) F2 0.0323(16) 0.086(3) 0.150(4) 0.057(2) -0.0133(19) 0.0021(16) F3 0.079(2) 0.089(3) 0.068(2) -0.020(2) -0.0038(18) -0.047(2) F4 0.0355(15) 0.0602(18) 0.0572(18) 0.0134(15) 0.0022(13) -0.0133(13) C25 0.044(3) 0.072(4) 0.047(3) 0.026(3) -0.017(3) -0.012(2) F5 0.074(3) 0.197(5) 0.165(4) 0.154(4) -0.042(3) -0.032(3) F6 0.167(4) 0.089(3) 0.0365(18) 0.0034(17) 0.025(2) -0.044(3) F7 0.082(2) 0.0444(17) 0.065(2) 0.0253(14) 0.0099(16) -0.0108(15) C26 0.027(2) 0.022(2) 0.024(2) 0.0024(16) -0.0058(16) 0.0019(16) C27 0.027(2) 0.025(2) 0.031(2) -0.0006(17) -0.0022(16) -0.0014(15) C28 0.032(2) 0.022(2) 0.031(2) -0.0030(17) -0.0082(18) -0.0048(17) C29 0.040(2) 0.022(2) 0.031(2) -0.0079(17) -0.0057(19) 0.0050(17) C30 0.029(2) 0.030(2) 0.023(2) -0.0022(17) -0.0016(16) -0.0018(17) C31 0.031(2) 0.027(2) 0.0208(19) 0.0021(16) 0.0006(16) 0.0025(16) C32 0.052(3) 0.021(2) 0.059(3) -0.004(2) 0.003(2) -0.008(2) F8 0.126(4) 0.074(3) 0.108(3) -0.021(2) -0.008(3) -0.060(2) F9 0.078(3) 0.051(2) 0.253(6) 0.073(3) -0.010(3) -0.005(2) F10 0.180(4) 0.043(2) 0.118(3) -0.013(2) 0.085(3) -0.040(2) C33 0.066(3) 0.033(3) 0.049(3) 0.000(2) 0.023(3) 0.006(3) F11 0.056(3) 0.104(4) 0.067(4) 0.019(3) 0.021(3) 0.032(3) F12 0.092(3) 0.088(3) 0.037(2) -0.011(2) 0.032(2) 0.003(3) F13 0.084(4) 0.060(3) 0.112(5) -0.035(3) 0.057(4) -0.025(3) F111 0.080(6) 0.100(6) 0.064(6) 0.018(5) 0.029(5) -0.005(5) F112 0.043(5) 0.082(6) 0.069(5) -0.020(5) 0.023(4) -0.020(4) F113 0.079(6) 0.082(6) 0.071(6) -0.024(5) 0.029(5) 0.014(5) C34 0.0213(18) 0.020(2) 0.029(2) 0.0010(16) -0.0014(15) -0.0029(14) C35 0.0254(19) 0.021(2) 0.029(2) -0.0013(16) -0.0017(16) -0.0018(16) C36 0.0248(19) 0.025(2) 0.028(2) -0.0047(16) -0.0020(15) 0.0020(15) C37 0.029(2) 0.031(2) 0.025(2) -0.0005(17) 0.0021(17) -0.0041(17) C38 0.030(2) 0.0235(19) 0.023(2) 0.0024(16) -0.0015(16) -0.0037(16) C39 0.024(2) 0.026(2) 0.029(2) 0.0013(16) -0.0015(17) -0.0032(17) C40 0.0324(19) 0.029(2) 0.032(2) -0.005(2) 0.002(2) 0.0022(16) F17 0.082(2) 0.065(2) 0.055(2) 0.0353(16) 0.0271(17) 0.0251(16) F18 0.0524(17) 0.061(2) 0.081(2) 0.0374(17) -0.0383(17) -0.0195(15) F19 0.092(2) 0.0283(16) 0.0490(16) 0.0068(12) -0.0217(15) -0.0049(14) C41 0.032(2) 0.032(2) 0.025(2) 0.0008(18) -0.0040(17) -0.0005(17) F14 0.0371(15) 0.0587(19) 0.067(2) -0.0191(15) -0.0171(14) 0.0202(13) F15 0.0459(14) 0.0279(13) 0.089(2) -0.0159(14) 0.0061(19) -0.0001(12) F16 0.072(2) 0.064(2) 0.0539(19) 0.0090(15) 0.0303(16) 0.0301(17) C42 0.028(2) 0.0207(19) 0.023(2) 0.0014(16) 0.0000(16) 0.0004(16) C43 0.025(2) 0.024(2) 0.037(2) -0.0006(18) 0.0032(17) 0.0013(17) C44 0.035(2) 0.022(2) 0.034(2) -0.0027(18) 0.0049(18) 0.0029(17) C45 0.033(2) 0.030(2) 0.035(2) -0.0068(19) 0.0059(17) -0.0076(17) C46 0.0276(19) 0.030(2) 0.0215(19) -0.0019(15) -0.0016(18) -0.0032(19) C47 0.033(2) 0.022(2) 0.026(2) -0.0034(17) -0.0018(17) 0.0024(17) C48 0.039(2) 0.031(2) 0.057(3) 0.006(3) 0.009(2) -0.003(2) F20 0.044(4) 0.039(3) 0.069(6) -0.003(4) -0.001(4) 0.024(4) F21 0.081(5) 0.052(4) 0.070(4) 0.025(3) 0.011(4) 0.015(4) F22 0.061(3) 0.025(3) 0.113(7) -0.006(4) -0.016(4) -0.010(2) F120 0.052(4) 0.031(4) 0.102(6) 0.016(5) 0.010(5) -0.003(3) F121 0.056(7) 0.041(5) 0.059(7) 0.008(5) 0.008(6) 0.025(6) F122 0.072(7) 0.039(4) 0.070(5) 0.020(4) -0.016(5) 0.005(5) C49 0.038(2) 0.036(3) 0.036(3) 0.001(2) -0.001(2) -0.003(2) F23 0.0361(16) 0.062(2) 0.114(3) 0.0237(19) -0.0147(17) -0.0175(14) F24 0.0518(17) 0.075(2) 0.0384(16) 0.0045(15) -0.0114(13) 0.0217(16) F25 0.0367(15) 0.075(2) 0.0593(19) -0.0200(16) -0.0007(13) 0.0165(14) _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 C9 2.127(5) . ? Rh1 C10 2.131(5) . ? Rh1 P1 2.2507(11) . ? Rh1 C3 2.259(4) . ? Rh1 C6 2.294(4) . ? Rh1 C5 2.319(5) . ? Rh1 C2 2.322(4) . ? Rh1 C4 2.323(5) . ? Rh1 C1 2.324(4) . ? P1 C112 1.668(11) . ? P1 C15 1.821(8) . ? P1 C7 1.825(5) . ? P1 C115 1.952(11) . ? P1 C12 1.972(8) . ? C1 C2 1.364(7) . ? C1 C6 1.394(7) . ? C2 C3 1.443(8) . ? C3 C4 1.422(8) . ? C4 C5 1.374(8) . ? C5 C6 1.365(8) . ? C7 C11 1.520(8) . ? C7 C8 1.533(7) . ? C8 C9 1.529(7) . ? C9 C10 1.401(9) . ? C10 C11 1.509(8) . ? C12 C13 1.511(12) . ? C12 C14 1.560(11) . ? C112 C113 1.528(15) . ? C112 C114 1.533(15) . ? C15 C17 1.518(12) . ? C15 C16 1.680(12) . ? C115 C117 1.526(16) . ? C115 C116 1.698(17) . ? B1 C34 1.634(6) . ? B1 C18 1.643(6) . ? B1 C42 1.644(5) . ? B1 C26 1.652(6) . ? C18 C23 1.397(6) . ? C18 C19 1.405(5) . ? C19 C20 1.378(6) . ? C20 C21 1.390(6) . ? C20 C24 1.498(6) . ? C21 C22 1.363(6) . ? C22 C23 1.407(6) . ? C22 C25 1.484(7) . ? C24 F2 1.316(5) . ? C24 F4 1.320(6) . ? C24 F3 1.351(6) . ? C25 F7 1.315(6) . ? C25 F5 1.315(6) . ? C25 F6 1.358(7) . ? C26 C27 1.397(6) . ? C26 C31 1.402(5) . ? C27 C28 1.391(6) . ? C28 C29 1.381(6) . ? C28 C32 1.483(6) . ? C29 C30 1.390(6) . ? C30 C31 1.389(6) . ? C30 C33 1.492(7) . ? C32 F9 1.269(6) . ? C32 F10 1.302(6) . ? C32 F8 1.344(6) . ? C33 F111 1.250(14) . ? C33 F113 1.256(19) . ? C33 F13 1.284(7) . ? C33 F11 1.343(8) . ? C33 F12 1.366(7) . ? C33 F112 1.512(14) . ? C34 C39 1.398(5) . ? C34 C35 1.406(5) . ? C35 C36 1.381(5) . ? C36 C37 1.385(6) . ? C36 C40 1.499(5) . ? C37 C38 1.388(6) . ? C38 C39 1.402(5) . ? C38 C41 1.489(6) . ? C40 F15 1.328(5) . ? C40 F14 1.333(5) . ? C40 F16 1.335(5) . ? F17 C41 1.337(5) . ? F18 C41 1.316(5) . ? F19 C41 1.323(5) . ? C42 C47 1.399(6) . ? C42 C43 1.405(5) . ? C43 C44 1.403(6) . ? C44 C45 1.375(6) . ? C44 C48 1.478(6) . ? C45 C46 1.386(6) . ? C46 C47 1.391(6) . ? C46 C49 1.498(6) . ? C48 F21 1.250(11) . ? C48 F121 1.28(2) . ? C48 F120 1.295(11) . ? C48 F20 1.346(13) . ? C48 F22 1.387(9) . ? C48 F122 1.484(14) . ? C49 F25 1.330(5) . ? C49 F24 1.337(5) . ? C49 F23 1.340(5) . ? 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 C9 Rh1 C10 38.4(3) . . ? C9 Rh1 P1 82.87(15) . . ? C10 Rh1 P1 82.56(16) . . ? C9 Rh1 C3 161.9(2) . . ? C10 Rh1 C3 158.0(2) . . ? P1 Rh1 C3 103.51(13) . . ? C9 Rh1 C6 97.4(2) . . ? C10 Rh1 C6 100.2(2) . . ? P1 Rh1 C6 175.92(13) . . ? C3 Rh1 C6 75.09(19) . . ? C9 Rh1 C5 118.7(2) . . ? C10 Rh1 C5 100.1(2) . . ? P1 Rh1 C5 148.37(15) . . ? C3 Rh1 C5 63.6(2) . . ? C6 Rh1 C5 34.41(19) . . ? C9 Rh1 C2 125.2(2) . . ? C10 Rh1 C2 157.9(2) . . ? P1 Rh1 C2 113.43(12) . . ? C3 Rh1 C2 36.7(2) . . ? C6 Rh1 C2 63.13(17) . . ? C5 Rh1 C2 74.54(18) . . ? C9 Rh1 C4 152.3(2) . . ? C10 Rh1 C4 122.5(2) . . ? P1 Rh1 C4 118.93(15) . . ? C3 Rh1 C4 36.1(2) . . ? C6 Rh1 C4 62.2(2) . . ? C5 Rh1 C4 34.4(2) . . ? C2 Rh1 C4 64.43(19) . . ? C9 Rh1 C1 101.2(2) . . ? C10 Rh1 C1 124.4(2) . . ? P1 Rh1 C1 140.81(14) . . ? C3 Rh1 C1 63.1(2) . . ? C6 Rh1 C1 35.13(17) . . ? C5 Rh1 C1 61.97(19) . . ? C2 Rh1 C1 34.14(18) . . ? C4 Rh1 C1 73.3(2) . . ? C112 P1 C15 77.7(7) . . ? C112 P1 C7 113.4(5) . . ? C15 P1 C7 116.6(3) . . ? C112 P1 C115 107.3(7) . . ? C15 P1 C115 30.6(4) . . ? C7 P1 C115 96.8(4) . . ? C112 P1 C12 24.3(5) . . ? C15 P1 C12 101.9(4) . . ? C7 P1 C12 104.1(3) . . ? C115 P1 C12 131.5(4) . . ? C112 P1 Rh1 127.6(5) . . ? C15 P1 Rh1 124.7(3) . . ? C7 P1 Rh1 97.96(17) . . ? C115 P1 Rh1 109.4(4) . . ? C12 P1 Rh1 110.3(3) . . ? C2 C1 C6 122.4(5) . . ? C2 C1 Rh1 72.8(3) . . ? C6 C1 Rh1 71.3(3) . . ? C1 C2 C3 117.3(4) . . ? C1 C2 Rh1 73.0(3) . . ? C3 C2 Rh1 69.3(2) . . ? C4 C3 C2 119.6(5) . . ? C4 C3 Rh1 74.4(3) . . ? C2 C3 Rh1 74.0(3) . . ? C5 C4 C3 119.3(5) . . ? C5 C4 Rh1 72.6(3) . . ? C3 C4 Rh1 69.5(3) . . ? C6 C5 C4 121.0(5) . . ? C6 C5 Rh1 71.8(3) . . ? C4 C5 Rh1 72.9(3) . . ? C5 C6 C1 120.1(5) . . ? C5 C6 Rh1 73.8(3) . . ? C1 C6 Rh1 73.6(3) . . ? C11 C7 C8 102.1(5) . . ? C11 C7 P1 104.2(4) . . ? C8 C7 P1 103.7(3) . . ? C9 C8 C7 100.6(4) . . ? C10 C9 C8 108.1(5) . . ? C10 C9 Rh1 70.9(3) . . ? C8 C9 Rh1 114.0(3) . . ? C9 C10 C11 109.2(5) . . ? C9 C10 Rh1 70.7(3) . . ? C11 C10 Rh1 114.4(4) . . ? C10 C11 C7 101.1(5) . . ? C13 C12 C14 111.1(9) . . ? C13 C12 P1 115.5(7) . . ? C14 C12 P1 109.5(7) . . ? C113 C112 C114 110.7(13) . . ? C113 C112 P1 115.9(13) . . ? C114 C112 P1 115.4(11) . . ? C17 C15 C16 100.6(9) . . ? C17 C15 P1 113.9(9) . . ? C16 C15 P1 110.1(10) . . ? C117 C115 C116 99.9(14) . . ? C117 C115 P1 105.5(12) . . ? C116 C115 P1 97.7(13) . . ? C34 B1 C18 109.7(3) . . ? C34 B1 C42 105.0(3) . . ? C18 B1 C42 112.8(3) . . ? C34 B1 C26 113.6(3) . . ? C18 B1 C26 104.6(3) . . ? C42 B1 C26 111.4(3) . . ? C23 C18 C19 115.3(4) . . ? C23 C18 B1 123.7(3) . . ? C19 C18 B1 120.9(3) . . ? C20 C19 C18 123.0(4) . . ? C19 C20 C21 120.1(4) . . ? C19 C20 C24 120.9(4) . . ? C21 C20 C24 119.0(4) . . ? C22 C21 C20 118.9(4) . . ? C21 C22 C23 120.8(4) . . ? C21 C22 C25 120.3(4) . . ? C23 C22 C25 119.0(4) . . ? C18 C23 C22 121.8(4) . . ? F2 C24 F4 107.4(4) . . ? F2 C24 F3 105.4(4) . . ? F4 C24 F3 105.2(4) . . ? F2 C24 C20 112.7(4) . . ? F4 C24 C20 114.2(4) . . ? F3 C24 C20 111.3(4) . . ? F7 C25 F5 106.2(5) . . ? F7 C25 F6 103.9(4) . . ? F5 C25 F6 107.7(6) . . ? F7 C25 C22 114.6(5) . . ? F5 C25 C22 112.6(4) . . ? F6 C25 C22 111.3(5) . . ? C27 C26 C31 115.6(4) . . ? C27 C26 B1 123.6(3) . . ? C31 C26 B1 120.6(3) . . ? C28 C27 C26 122.5(4) . . ? C29 C28 C27 120.6(4) . . ? C29 C28 C32 118.1(4) . . ? C27 C28 C32 121.4(4) . . ? C28 C29 C30 118.4(4) . . ? C31 C30 C29 120.5(4) . . ? C31 C30 C33 119.9(4) . . ? C29 C30 C33 119.5(4) . . ? C30 C31 C26 122.3(4) . . ? F9 C32 F10 110.1(5) . . ? F9 C32 F8 102.8(5) . . ? F10 C32 F8 101.2(4) . . ? F9 C32 C28 115.1(4) . . ? F10 C32 C28 114.3(4) . . ? F8 C32 C28 111.9(4) . . ? F111 C33 F113 120.4(12) . . ? F111 C33 F13 44.0(8) . . ? F113 C33 F13 125.7(11) . . ? F111 C33 F11 131.0(9) . . ? F113 C33 F11 28.6(8) . . ? F13 C33 F11 111.6(7) . . ? F111 C33 F12 61.3(9) . . ? F113 C33 F12 75.0(9) . . ? F13 C33 F12 103.1(5) . . ? F11 C33 F12 102.4(5) . . ? F111 C33 C30 115.8(8) . . ? F113 C33 C30 116.4(10) . . ? F13 C33 C30 114.8(4) . . ? F11 C33 C30 113.2(5) . . ? F12 C33 C30 110.5(5) . . ? F111 C33 F112 95.6(11) . . ? F113 C33 F112 96.8(11) . . ? F13 C33 F112 52.4(6) . . ? F11 C33 F112 70.0(7) . . ? F12 C33 F112 143.1(6) . . ? C30 C33 F112 105.4(5) . . ? C39 C34 C35 115.3(4) . . ? C39 C34 B1 124.0(3) . . ? C35 C34 B1 120.7(3) . . ? C36 C35 C34 123.1(4) . . ? C35 C36 C37 120.6(4) . . ? C35 C36 C40 119.3(4) . . ? C37 C36 C40 120.1(4) . . ? C36 C37 C38 118.2(4) . . ? C37 C38 C39 120.6(4) . . ? C37 C38 C41 120.6(4) . . ? C39 C38 C41 118.7(4) . . ? C34 C39 C38 122.1(4) . . ? F15 C40 F14 106.2(3) . . ? F15 C40 F16 107.0(4) . . ? F14 C40 F16 105.6(3) . . ? F15 C40 C36 112.0(3) . . ? F14 C40 C36 112.2(3) . . ? F16 C40 C36 113.2(3) . . ? F18 C41 F19 106.3(4) . . ? F18 C41 F17 107.3(4) . . ? F19 C41 F17 104.4(4) . . ? F18 C41 C38 113.5(4) . . ? F19 C41 C38 112.0(3) . . ? F17 C41 C38 112.8(3) . . ? C47 C42 C43 115.4(4) . . ? C47 C42 B1 123.0(3) . . ? C43 C42 B1 121.5(3) . . ? C44 C43 C42 122.4(4) . . ? C45 C44 C43 120.2(4) . . ? C45 C44 C48 120.9(4) . . ? C43 C44 C48 118.8(4) . . ? C44 C45 C46 118.9(4) . . ? C45 C46 C47 120.7(4) . . ? C45 C46 C49 120.1(4) . . ? C47 C46 C49 119.1(4) . . ? C46 C47 C42 122.3(4) . . ? F21 C48 F121 123.3(10) . . ? F21 C48 F120 72.8(7) . . ? F121 C48 F120 114.7(13) . . ? F21 C48 F20 107.4(7) . . ? F121 C48 F20 18.5(12) . . ? F120 C48 F20 122.2(10) . . ? F21 C48 F22 107.9(7) . . ? F121 C48 F22 90.3(11) . . ? F120 C48 F22 35.6(5) . . ? F20 C48 F22 105.4(8) . . ? F21 C48 C44 111.5(6) . . ? F121 C48 C44 112.1(12) . . ? F120 C48 C44 117.5(6) . . ? F20 C48 C44 115.4(8) . . ? F22 C48 C44 108.8(5) . . ? F21 C48 F122 24.9(6) . . ? F121 C48 F122 104.1(9) . . ? F120 C48 F122 95.0(8) . . ? F20 C48 F122 86.3(8) . . ? F22 C48 F122 127.8(7) . . ? C44 C48 F122 111.2(7) . . ? F25 C49 F24 105.1(4) . . ? F25 C49 F23 106.2(4) . . ? F24 C49 F23 106.3(4) . . ? F25 C49 C46 112.5(4) . . ? F24 C49 C46 113.2(4) . . ? F23 C49 C46 112.9(4) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.683 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.067