# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name ' Andrew Weller' _publ_contact_author_email andrew.weller@chem.ox.ac.uk _publ_author_name A.Weller # Attachment '- Compound2b .cif' data_168abc10 _database_code_depnum_ccdc_archive 'CCDC 801541' #TrackingRef '- Compound2b .cif' #----------------------------------------- # [Rh(dppp)(H3BNMe3)][BArF4].1.25(C6H4F2) #----------------------------------------- # start Validation Reply Form _vrf_PLAT431_168abc10 ; PROBLEM: Short Inter HL..A Contact F5 .. F901 .. 2.41 Ang. RESPONSE: The structure contains a disordered solvent molecule with only partial occupancy (25%) - the short contact occurs with this molecule. ; _vrf_PLAT242_168abc10 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C208 PROBLEM: Check Low Ueq as Compared to Neighbors for C216 RESPONSE: The anion contains a significant degree of disorder. See details in supplementary information or _refine_special_details. ; _vrf_PLAT041_168abc10 ; PROBLEM: Calc. and Reported SumFormula Strings Differ ? RESPONSE: This alert results from the presence of a disordered solvent molecule that lies on a special position in this structure. This response also addresses: PLAT042 and PLAT045. ; _vrf_PLAT301_168abc10 ; PROBLEM: Note: Main Residue Disorder ................... 28.00 Perc. RESPONSE: The structure contains a significant degree of disorder. See details in supplementary information or _refine_special_details. ; _vrf_PLAT605_168abc10 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 153.00 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 'C30 H38 B N P2 Rh, C32 H12 B F24, 1.25(C6 H4 F2)' _chemical_formula_sum 'C69.50 H55 B2 F26.50 N P2 Rh' _chemical_formula_weight 1594.11 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 12.9731(2) _cell_length_b 17.4492(2) _cell_length_c 18.3033(3) _cell_angle_alpha 110.1373(6) _cell_angle_beta 95.3780(7) _cell_angle_gamma 99.4374(7) _cell_volume 3786.61(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15041 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1605 _exptl_absorpt_coefficient_mu 0.372 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.598 _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 26357 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 5.50 _diffrn_reflns_theta_max 26.37 _reflns_number_total 15201 _reflns_number_gt 12968 _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 'SHELXS-86 (Sheldrick, 2008)' _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 shelxs-86 by Patterson interpretation. H1A, H1B, H1C, H11A, H11B and H11C were placed in calculated positions, with the B-H distance free to refine (AFIX 134, the restraint B1-H1A = B1-H1B = B1-H1C = B11-H11A = B11-H11B = B11-H11C was applied) despite the presence of geometrically sensible fourier peaks. Disorder of the amine-borane ligand was treated my modelling it over two sites and restraining its geometry. Disorder of the phosphine ligands was treated by modelling the appropriate substituents over two sites and restraining their geometry - this included the used of rigid body constraints. Disorder of one of the difluorobenzene solvent molecules (occupancy 1) was treated by modelling the fluorine atoms over four sites and restraining the 1,2 and 1,3-C-F bond distances. A rigid body constraint was applied to the arene ring. Disorder of one of the difluorobenzene solvent molecules (occupancy 0.25) was treated by modelling it over two sites - restraints to the 1,2 and 1,3-C-F bond distances were applied as was a rigid body constraint. This molecule lies on a special position. Rotational disorder of the CF3 groups of the anion was treated by modelling the fluorine atoms or 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 0.173 0.220 0.300 152 -5 ' ' 2 -0.173 0.780 0.700 152 -5 ' ' _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^)+(0.0857P)^2^+4.3646P] 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 15201 _refine_ls_number_parameters 1196 _refine_ls_number_restraints 1688 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1541 _refine_ls_wR_factor_gt 0.1455 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.188 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.494839(19) 0.279710(15) 0.208855(15) 0.03173(10) Uani 1 1 d . B . P1 P 0.66544(7) 0.30484(5) 0.25258(5) 0.03399(19) Uani 1 1 d D . . P2 P 0.49611(7) 0.14986(5) 0.13673(5) 0.0351(2) Uani 1 1 d D . . B1 B 0.3745(3) 0.3567(3) 0.2298(3) 0.0442(9) Uani 0.691(12) 1 d PDU A 1 H1A H 0.4639(10) 0.3834(4) 0.2560(4) 0.066 Uiso 0.691(12) 1 calc PRD A 1 H1B H 0.3614(3) 0.2853(7) 0.1940(4) 0.066 Uiso 0.691(12) 1 calc PRD A 1 H1C H 0.3247(5) 0.3680(3) 0.2808(6) 0.066 Uiso 0.691(12) 1 calc PRD A 1 N1 N 0.3384(5) 0.4024(4) 0.1731(4) 0.0523(12) Uani 0.691(12) 1 d PDU A 1 C1 C 0.4128(6) 0.4044(6) 0.1163(5) 0.056(2) Uani 0.691(12) 1 d PDU A 1 H1D H 0.4207 0.3475 0.0871 0.084 Uiso 0.691(12) 1 calc PR A 1 H1E H 0.4820 0.4388 0.1452 0.084 Uiso 0.691(12) 1 calc PR A 1 H1F H 0.3848 0.4282 0.0793 0.084 Uiso 0.691(12) 1 calc PR A 1 C2 C 0.3337(8) 0.4899(4) 0.2228(6) 0.075(2) Uani 0.691(12) 1 d PDU A 1 H2A H 0.4051 0.5211 0.2494 0.113 Uiso 0.691(12) 1 calc PR A 1 H2B H 0.2880 0.4886 0.2622 0.113 Uiso 0.691(12) 1 calc PR A 1 H2C H 0.3048 0.5171 0.1892 0.113 Uiso 0.691(12) 1 calc PR A 1 C3 C 0.2303(5) 0.3578(7) 0.1285(4) 0.069(2) Uani 0.691(12) 1 d PDU A 1 H3A H 0.2064 0.3872 0.0953 0.104 Uiso 0.691(12) 1 calc PR A 1 H3B H 0.1811 0.3563 0.1657 0.104 Uiso 0.691(12) 1 calc PR A 1 H3C H 0.2324 0.3007 0.0952 0.104 Uiso 0.691(12) 1 calc PR A 1 B11 B 0.3745(3) 0.3567(3) 0.2298(3) 0.0442(9) Uani 0.309(12) 1 d PDU A 2 H11A H 0.4621(12) 0.3696(7) 0.2598(6) 0.066 Uiso 0.309(12) 1 calc PRD A 2 H11B H 0.3527(5) 0.2905(8) 0.1804(5) 0.066 Uiso 0.309(12) 1 calc PRD A 2 H11C H 0.3189(3) 0.3600(7) 0.2767(6) 0.066 Uiso 0.309(12) 1 calc PRD A 2 N11 N 0.3606(7) 0.4251(5) 0.1921(6) 0.0523(12) Uani 0.309(12) 1 d PDU A 2 C101 C 0.4333(13) 0.4238(12) 0.1334(9) 0.062(5) Uani 0.309(12) 1 d PDU A 2 H10A H 0.4212 0.3673 0.0936 0.093 Uiso 0.309(12) 1 calc PR A 2 H10B H 0.5069 0.4404 0.1603 0.093 Uiso 0.309(12) 1 calc PR A 2 H10C H 0.4196 0.4628 0.1077 0.093 Uiso 0.309(12) 1 calc PR A 2 C102 C 0.3852(16) 0.5101(5) 0.2555(10) 0.084(5) Uani 0.309(12) 1 d PDU A 2 H10D H 0.4622 0.5305 0.2691 0.126 Uiso 0.309(12) 1 calc PR A 2 H10E H 0.3565 0.5071 0.3023 0.126 Uiso 0.309(12) 1 calc PR A 2 H10F H 0.3532 0.5484 0.2366 0.126 Uiso 0.309(12) 1 calc PR A 2 C103 C 0.2489(9) 0.4073(11) 0.1521(10) 0.066(4) Uani 0.309(12) 1 d PDU A 2 H10G H 0.2348 0.4565 0.1419 0.099 Uiso 0.309(12) 1 calc PR A 2 H10H H 0.2006 0.3939 0.1862 0.099 Uiso 0.309(12) 1 calc PR A 2 H10I H 0.2380 0.3598 0.1021 0.099 Uiso 0.309(12) 1 calc PR A 2 C4 C 0.7518(3) 0.2508(2) 0.1889(2) 0.0412(8) Uani 1 1 d . B . H4A H 0.7563 0.2714 0.1450 0.049 Uiso 1 1 calc R . . H4B H 0.8239 0.2652 0.2196 0.049 Uiso 1 1 calc R . . C5 C 0.7152(3) 0.1559(2) 0.1545(2) 0.0437(8) Uani 1 1 d . . . H5A H 0.7023 0.1356 0.1978 0.052 Uiso 1 1 calc R B . H5B H 0.7723 0.1309 0.1296 0.052 Uiso 1 1 calc R . . C6 C 0.6144(3) 0.1265(2) 0.0934(2) 0.0435(8) Uani 1 1 d . B . H6A H 0.6035 0.0655 0.0650 0.052 Uiso 1 1 calc R . . H6B H 0.6237 0.1536 0.0544 0.052 Uiso 1 1 calc R . . C7 C 0.7199(3) 0.4144(2) 0.2706(2) 0.0405(8) Uani 1 1 d . B . C8 C 0.7135(3) 0.4404(3) 0.2078(3) 0.0490(9) Uani 1 1 d . . . H8 H 0.6860 0.4002 0.1565 0.059 Uiso 1 1 calc R B . C9 C 0.7460(4) 0.5233(3) 0.2169(3) 0.0600(11) Uani 1 1 d . B . H9 H 0.7410 0.5394 0.1723 0.072 Uiso 1 1 calc R . . C10 C 0.7850(4) 0.5812(3) 0.2900(4) 0.0634(13) Uani 1 1 d . . . H10 H 0.8053 0.6384 0.2969 0.076 Uiso 1 1 calc R B . C11 C 0.7950(4) 0.5579(3) 0.3530(4) 0.0753(15) Uani 1 1 d . B . H11 H 0.8245 0.5987 0.4036 0.090 Uiso 1 1 calc R . . C12 C 0.7624(4) 0.4737(3) 0.3447(3) 0.0626(12) Uani 1 1 d . . . H12 H 0.7695 0.4579 0.3894 0.075 Uiso 1 1 calc R B . C13 C 0.6973(3) 0.2936(3) 0.34722(19) 0.0428(13) Uani 0.765(4) 1 d PGDU B 1 C14 C 0.6203(3) 0.3033(3) 0.3956(2) 0.0562(13) Uani 0.765(4) 1 d PGU B 1 H14 H 0.5582 0.3206 0.3813 0.067 Uiso 0.765(4) 1 calc PR B 1 C15 C 0.6339(4) 0.2876(3) 0.4650(2) 0.0700(16) Uani 0.765(4) 1 d PGU B 1 H15 H 0.5812 0.2942 0.4981 0.084 Uiso 0.765(4) 1 calc PR B 1 C16 C 0.7247(4) 0.2622(3) 0.4859(2) 0.0776(19) Uani 0.765(4) 1 d PGU B 1 H16 H 0.7340 0.2514 0.5334 0.093 Uiso 0.765(4) 1 calc PR B 1 C17 C 0.8017(4) 0.2525(3) 0.4375(3) 0.0758(19) Uani 0.765(4) 1 d PGU B 1 H17 H 0.8638 0.2352 0.4518 0.091 Uiso 0.765(4) 1 calc PR B 1 C18 C 0.7881(3) 0.2683(3) 0.3682(3) 0.0582(15) Uani 0.765(4) 1 d PGU B 1 H18 H 0.8408 0.2617 0.3351 0.070 Uiso 0.765(4) 1 calc PR B 1 C113 C 0.6883(13) 0.2770(11) 0.3395(7) 0.049(3) Uani 0.235(4) 1 d PGDU B 2 C114 C 0.6073(10) 0.2363(10) 0.3661(7) 0.057(3) Uani 0.235(4) 1 d PGU B 2 H114 H 0.5363 0.2241 0.3402 0.068 Uiso 0.235(4) 1 calc PR B 2 C115 C 0.6301(12) 0.2136(10) 0.4305(8) 0.072(3) Uani 0.235(4) 1 d PGU B 2 H115 H 0.5748 0.1858 0.4486 0.087 Uiso 0.235(4) 1 calc PR B 2 C116 C 0.7340(14) 0.2314(11) 0.4684(8) 0.072(3) Uani 0.235(4) 1 d PGU B 2 H116 H 0.7496 0.2159 0.5124 0.086 Uiso 0.235(4) 1 calc PR B 2 C117 C 0.8150(10) 0.2721(12) 0.4419(10) 0.074(3) Uani 0.235(4) 1 d PGU B 2 H117 H 0.8860 0.2843 0.4678 0.088 Uiso 0.235(4) 1 calc PR B 2 C118 C 0.7922(11) 0.2948(11) 0.3774(10) 0.058(3) Uani 0.235(4) 1 d PGU B 2 H118 H 0.8476 0.3226 0.3593 0.069 Uiso 0.235(4) 1 calc PR B 2 C19 C 0.3910(3) 0.1134(2) 0.0513(2) 0.0383(7) Uani 1 1 d . B . C20 C 0.4084(4) 0.1312(3) -0.0141(3) 0.0621(12) Uani 1 1 d . . . H20 H 0.4759 0.1609 -0.0158 0.075 Uiso 1 1 calc R B . C21 C 0.3273(4) 0.1059(4) -0.0783(3) 0.0723(14) Uani 1 1 d . B . H21 H 0.3407 0.1171 -0.1241 0.087 Uiso 1 1 calc R . . C22 C 0.2296(4) 0.0655(3) -0.0766(3) 0.0607(12) Uani 1 1 d . . . H22 H 0.1746 0.0491 -0.1204 0.073 Uiso 1 1 calc R B . C23 C 0.2113(4) 0.0487(3) -0.0107(4) 0.0686(14) Uani 1 1 d . B . H23 H 0.1430 0.0207 -0.0087 0.082 Uiso 1 1 calc R . . C24 C 0.2916(3) 0.0721(3) 0.0530(3) 0.0596(11) Uani 1 1 d . . . H24 H 0.2782 0.0595 0.0983 0.071 Uiso 1 1 calc R B . C25 C 0.4741(3) 0.0731(2) 0.1861(2) 0.0390(12) Uani 0.765(4) 1 d PGDU B 1 C26 C 0.4952(4) 0.10025(18) 0.2678(2) 0.0593(14) Uani 0.765(4) 1 d PGU B 1 H26 H 0.5169 0.1582 0.2984 0.071 Uiso 0.765(4) 1 calc PR B 1 C27 C 0.4845(4) 0.0426(3) 0.30491(18) 0.0744(17) Uani 0.765(4) 1 d PGU B 1 H27 H 0.4989 0.0612 0.3608 0.089 Uiso 0.765(4) 1 calc PR B 1 C28 C 0.4528(4) -0.0422(2) 0.2602(3) 0.0654(15) Uani 0.765(4) 1 d PGU B 1 H28 H 0.4454 -0.0816 0.2855 0.078 Uiso 0.765(4) 1 calc PR B 1 C29 C 0.4317(4) -0.06936(17) 0.1784(2) 0.0627(16) Uani 0.765(4) 1 d PGU B 1 H29 H 0.4100 -0.1273 0.1479 0.075 Uiso 0.765(4) 1 calc PR B 1 C30 C 0.4424(4) -0.0117(2) 0.14135(17) 0.0515(13) Uani 0.765(4) 1 d PGU B 1 H30 H 0.4280 -0.0303 0.0855 0.062 Uiso 0.765(4) 1 calc PR B 1 C125 C 0.4544(11) 0.0695(7) 0.1736(8) 0.046(3) Uani 0.235(4) 1 d PGDU B 2 C126 C 0.3895(11) 0.0848(7) 0.2310(8) 0.055(3) Uani 0.235(4) 1 d PGU B 2 H126 H 0.3637 0.1351 0.2465 0.066 Uiso 0.235(4) 1 calc PR B 2 C127 C 0.3622(11) 0.0267(8) 0.2658(8) 0.067(3) Uani 0.235(4) 1 d PGU B 2 H127 H 0.3178 0.0371 0.3051 0.081 Uiso 0.235(4) 1 calc PR B 2 C128 C 0.3998(13) -0.0468(8) 0.2432(9) 0.065(3) Uani 0.235(4) 1 d PGU B 2 H128 H 0.3812 -0.0866 0.2670 0.079 Uiso 0.235(4) 1 calc PR B 2 C129 C 0.4648(13) -0.0621(7) 0.1858(9) 0.061(3) Uani 0.235(4) 1 d PGU B 2 H129 H 0.4905 -0.1123 0.1704 0.073 Uiso 0.235(4) 1 calc PR B 2 C130 C 0.4921(11) -0.0039(9) 0.1510(8) 0.047(3) Uani 0.235(4) 1 d PGU B 2 H130 H 0.5364 -0.0144 0.1118 0.056 Uiso 0.235(4) 1 calc PR B 2 B200 B 0.8560(3) 0.2929(2) 0.7528(2) 0.0284(7) Uani 1 1 d . . . C201 C 0.9053(2) 0.38700(19) 0.75693(19) 0.0282(6) Uani 1 1 d . . . C202 C 0.9495(2) 0.4515(2) 0.8292(2) 0.0311(6) Uani 1 1 d . . . H202 H 0.9503 0.4399 0.8763 0.037 Uiso 1 1 calc R . . C203 C 0.9923(2) 0.5321(2) 0.8342(2) 0.0369(7) Uani 1 1 d D C . C204 C 0.9909(3) 0.5520(2) 0.7670(2) 0.0401(8) Uani 1 1 d . . . H204 H 1.0209 0.6068 0.7702 0.048 Uiso 1 1 calc R . . C205 C 0.9449(3) 0.4906(2) 0.6959(2) 0.0393(8) Uani 1 1 d . . . C206 C 0.9022(2) 0.4099(2) 0.6905(2) 0.0337(7) Uani 1 1 d . . . H206 H 0.8701 0.3692 0.6404 0.040 Uiso 1 1 calc R . . C207 C 1.0405(3) 0.5963(2) 0.9131(2) 0.0504(10) Uani 1 1 d D . . F1 F 1.1344(3) 0.5885(4) 0.9378(3) 0.123(3) Uani 0.829(9) 1 d PDU C 1 F2 F 0.9834(3) 0.5956(3) 0.96835(18) 0.0657(13) Uani 0.829(9) 1 d PDU C 1 F3 F 1.0513(6) 0.6734(2) 0.9131(3) 0.106(2) Uani 0.829(9) 1 d PDU C 1 F101 F 0.9721(10) 0.6363(12) 0.9506(9) 0.091(7) Uani 0.171(9) 1 d PDU C 2 F102 F 1.1184(13) 0.6541(9) 0.9136(7) 0.063(5) Uani 0.171(9) 1 d PDU C 2 F103 F 1.0813(18) 0.5639(7) 0.9626(7) 0.076(6) Uani 0.171(9) 1 d PDU C 2 C208 C 0.9372(4) 0.5097(3) 0.6220(3) 0.0567(11) Uani 1 1 d . . . F4 F 0.9993(3) 0.5807(2) 0.6297(2) 0.0961(11) Uani 1 1 d U . . F5 F 0.8395(3) 0.5125(3) 0.5971(3) 0.1179(16) Uani 1 1 d U . . F6 F 0.9643(4) 0.4520(2) 0.56235(19) 0.0989(12) Uani 1 1 d U . . C209 C 0.7352(2) 0.29487(19) 0.77233(19) 0.0296(6) Uani 1 1 d . . . C210 C 0.7134(2) 0.3195(2) 0.8495(2) 0.0342(7) Uani 1 1 d . . . H210 H 0.7698 0.3330 0.8918 0.041 Uiso 1 1 calc R . . C211 C 0.6116(2) 0.3250(2) 0.8663(2) 0.0400(8) Uani 1 1 d D D . C212 C 0.5275(3) 0.3060(3) 0.8063(2) 0.0452(9) Uani 1 1 d . . . H212 H 0.4578 0.3084 0.8174 0.054 Uiso 1 1 calc R . . C213 C 0.5475(3) 0.2833(2) 0.7292(2) 0.0412(8) Uani 1 1 d D E . C214 C 0.6491(3) 0.2787(2) 0.7131(2) 0.0346(7) Uani 1 1 d . . . H214 H 0.6608 0.2641 0.6600 0.042 Uiso 1 1 calc R . . C215 C 0.5940(3) 0.3519(3) 0.9496(3) 0.0589(12) Uani 1 1 d D . . F7 F 0.6410(7) 0.4284(3) 0.9934(3) 0.079(2) Uani 0.675(15) 1 d PDU D 1 F8 F 0.6375(6) 0.3049(3) 0.9876(2) 0.0712(18) Uani 0.675(15) 1 d PDU D 1 F9 F 0.4947(3) 0.3360(7) 0.9590(3) 0.099(3) Uani 0.675(15) 1 d PDU D 1 F107 F 0.5760(18) 0.2952(6) 0.9789(7) 0.112(5) Uani 0.325(15) 1 d PDU D 2 F108 F 0.5087(9) 0.3903(11) 0.9568(5) 0.085(4) Uani 0.325(15) 1 d PDU D 2 F109 F 0.6713(8) 0.4140(8) 0.9982(6) 0.071(4) Uani 0.325(15) 1 d PDU D 2 C216 C 0.4589(3) 0.2643(3) 0.6632(3) 0.0639(13) Uani 1 1 d D . . F10 F 0.3664(3) 0.2639(7) 0.6825(4) 0.088(2) Uani 0.629(13) 1 d PDU E 1 F11 F 0.4741(6) 0.3157(6) 0.6246(5) 0.109(3) Uani 0.629(13) 1 d PDU E 1 F12 F 0.4536(7) 0.1892(5) 0.6073(5) 0.116(3) Uani 0.629(13) 1 d PDU E 1 F110 F 0.4778(7) 0.2295(11) 0.5934(3) 0.086(4) Uani 0.371(13) 1 d PDU E 2 F111 F 0.3735(7) 0.2155(10) 0.6701(6) 0.096(4) Uani 0.371(13) 1 d PDU E 2 F112 F 0.4258(13) 0.3333(6) 0.6653(10) 0.132(6) Uani 0.371(13) 1 d PDU E 2 C217 C 0.9286(2) 0.26783(19) 0.81622(18) 0.0286(6) Uani 1 1 d . . . C218 C 1.0382(2) 0.2983(2) 0.83636(19) 0.0306(6) Uani 1 1 d . . . H218 H 1.0703 0.3380 0.8160 0.037 Uiso 1 1 calc R . . C219 C 1.1014(3) 0.2728(2) 0.8847(2) 0.0354(7) Uani 1 1 d . . . C220 C 1.0593(3) 0.2153(2) 0.9159(2) 0.0388(7) Uani 1 1 d . . . H220 H 1.1029 0.1981 0.9495 0.047 Uiso 1 1 calc R . . C221 C 0.9514(3) 0.1835(2) 0.8964(2) 0.0417(8) Uani 1 1 d D F . C222 C 0.8878(3) 0.2091(2) 0.8479(2) 0.0358(7) Uani 1 1 d . . . H222 H 0.8139 0.1859 0.8357 0.043 Uiso 1 1 calc R . . C223 C 1.2174(3) 0.3103(3) 0.9029(3) 0.0509(10) Uani 1 1 d . . . F13 F 1.2374(2) 0.39228(17) 0.94489(18) 0.0695(8) Uani 1 1 d U . . F14 F 1.26217(19) 0.3037(2) 0.8394(2) 0.0789(9) Uani 1 1 d U . . F15 F 1.2722(2) 0.2769(2) 0.9456(2) 0.0895(11) Uani 1 1 d U . . C224 C 0.9023(3) 0.1210(3) 0.9280(3) 0.0632(13) Uani 1 1 d D . . F16 F 0.9674(5) 0.0812(7) 0.9511(8) 0.096(3) Uani 0.527(14) 1 d PDU F 1 F17 F 0.8363(7) 0.0542(4) 0.8653(4) 0.085(3) Uani 0.527(14) 1 d PDU F 1 F18 F 0.8378(7) 0.1448(5) 0.9766(5) 0.077(3) Uani 0.527(14) 1 d PDU F 1 F116 F 0.8108(6) 0.1353(7) 0.9519(6) 0.071(3) Uani 0.473(14) 1 d PDU F 2 F117 F 0.9614(6) 0.1310(7) 0.9994(5) 0.080(3) Uani 0.473(14) 1 d PDU F 2 F118 F 0.8908(12) 0.0446(3) 0.8855(6) 0.109(4) Uani 0.473(14) 1 d PDU F 2 C225 C 0.8592(2) 0.2211(2) 0.66788(18) 0.0299(6) Uani 1 1 d . . . C226 C 0.9476(3) 0.2264(2) 0.62960(19) 0.0337(7) Uani 1 1 d . . . H226 H 1.0022 0.2753 0.6510 0.040 Uiso 1 1 calc R . . C227 C 0.9582(3) 0.1628(2) 0.56171(19) 0.0375(7) Uani 1 1 d D G . C228 C 0.8794(3) 0.0907(2) 0.5276(2) 0.0416(8) Uani 1 1 d . G . H228 H 0.8856 0.0475 0.4805 0.050 Uiso 1 1 calc R . . C229 C 0.7930(3) 0.0839(2) 0.5638(2) 0.0436(8) Uani 1 1 d D . . C230 C 0.7833(3) 0.1469(2) 0.6333(2) 0.0365(7) Uani 1 1 d . H . H230 H 0.7231 0.1390 0.6578 0.044 Uiso 1 1 calc R . . C231 C 1.0545(3) 0.1741(2) 0.5241(2) 0.0509(10) Uani 1 1 d D . . F19 F 1.1433(4) 0.1978(8) 0.5765(4) 0.071(3) Uani 0.58(2) 1 d PDU G 1 F20 F 1.0588(7) 0.2395(7) 0.4997(8) 0.084(3) Uani 0.58(2) 1 d PDU G 1 F21 F 1.0634(7) 0.1108(6) 0.4648(5) 0.088(3) Uani 0.58(2) 1 d PDU G 1 F119 F 1.0349(8) 0.1970(13) 0.4630(8) 0.088(4) Uani 0.42(2) 1 d PDU G 2 F120 F 1.0813(9) 0.0995(5) 0.4909(9) 0.081(4) Uani 0.42(2) 1 d PDU G 2 F121 F 1.1376(6) 0.2245(8) 0.5704(6) 0.070(4) Uani 0.42(2) 1 d PDU G 2 C232 C 0.7078(6) 0.0049(4) 0.5330(4) 0.0656(15) Uani 0.543(8) 1 d PDU H 1 F22 F 0.7123(7) -0.0409(5) 0.4599(4) 0.108(4) Uani 0.543(8) 1 d PDU H 1 F23 F 0.7159(6) -0.0417(4) 0.5752(4) 0.100(3) Uani 0.543(8) 1 d PDU H 1 F24 F 0.6140(4) 0.0220(4) 0.5352(6) 0.094(3) Uani 0.543(8) 1 d PDU H 1 C332 C 0.7007(6) 0.0104(5) 0.5220(5) 0.0656(15) Uani 0.457(8) 1 d PDU H 2 F122 F 0.6386(7) -0.0048(6) 0.5699(4) 0.102(4) Uani 0.457(8) 1 d PDU H 2 F123 F 0.6388(6) 0.0183(5) 0.4652(5) 0.092(3) Uani 0.457(8) 1 d PDU H 2 F124 F 0.7336(7) -0.0595(4) 0.4883(6) 0.087(3) Uani 0.457(8) 1 d PDU H 2 C801 C 0.9714(3) 1.0024(2) 0.2899(2) 0.0912(19) Uani 1 1 d GD . . H801 H 1.0421 1.0252 0.2874 0.109 Uiso 0.45 1 calc PR I 2 C802 C 0.8935(3) 1.04868(18) 0.2914(2) 0.0816(16) Uani 1 1 d GD . . H802 H 0.9109 1.1031 0.2900 0.098 Uiso 0.18 1 calc PR J 2 C803 C 0.7900(3) 1.0153(2) 0.2951(2) 0.0848(17) Uani 1 1 d GD . . H803 H 0.7368 1.0469 0.2961 0.102 Uiso 0.55 1 calc PR K 1 C804 C 0.7645(3) 0.9356(2) 0.2972(2) 0.0872(18) Uani 1 1 d GD . . H804 H 0.6938 0.9128 0.2997 0.105 Uiso 0.82 1 calc PR L 1 C805 C 0.8425(4) 0.88935(18) 0.2957(2) 0.095(2) Uani 1 1 d GD . . H805 H 0.8250 0.8349 0.2971 0.114 Uiso 1 1 calc R . . C806 C 0.9459(3) 0.9227(2) 0.2920(2) 0.090(2) Uani 1 1 d GD . . H806 H 0.9992 0.8911 0.2909 0.108 Uiso 1 1 calc R . . F801 F 1.0655(5) 1.0300(4) 0.2854(4) 0.1285(14) Uani 0.55 1 d PDU M 1 F802 F 0.9172(4) 1.1217(3) 0.2874(3) 0.1285(14) Uani 0.82 1 d PDU N 1 F803 F 0.7187(6) 1.0569(5) 0.2965(4) 0.1285(14) Uani 0.45 1 d PDU O 2 F804 F 0.6694(7) 0.9023(11) 0.2994(5) 0.1285(14) Uani 0.18 1 d PDU P 2 C901 C 0.605(2) 0.5199(11) 0.5071(12) 0.086(3) Uani 0.25 1 d PGDU Q -1 C902 C 0.561(2) 0.4776(11) 0.5524(12) 0.078(3) Uani 0.25 1 d PGDU Q -1 C903 C 0.451(2) 0.4526(15) 0.5428(15) 0.085(3) Uani 0.25 1 d PGDU Q -1 H903 H 0.4210 0.4238 0.5738 0.102 Uiso 0.25 1 calc PR Q -1 C904 C 0.387(2) 0.4699(18) 0.4881(17) 0.086(3) Uani 0.25 1 d PGU Q -1 H904 H 0.3119 0.4528 0.4816 0.103 Uiso 0.25 1 calc PR Q -1 C905 C 0.431(2) 0.5121(17) 0.4429(16) 0.078(3) Uani 0.25 1 d PGU Q -1 H905 H 0.3870 0.5238 0.4055 0.094 Uiso 0.25 1 calc PR Q -1 C906 C 0.541(2) 0.5371(14) 0.4524(14) 0.085(3) Uani 0.25 1 d PGDU Q -1 H906 H 0.5711 0.5659 0.4215 0.102 Uiso 0.25 1 calc PR Q -1 F901 F 0.7079(14) 0.5438(11) 0.5160(10) 0.122(4) Uani 0.25 1 d PDU Q -1 F902 F 0.6222(13) 0.4613(11) 0.6035(11) 0.122(4) Uani 0.25 1 d PDU Q -1 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 0.03037(15) 0.02862(15) 0.03403(15) 0.00847(10) 0.00637(10) 0.00624(10) P1 0.0323(4) 0.0318(4) 0.0378(4) 0.0127(3) 0.0047(3) 0.0073(3) P2 0.0357(4) 0.0276(4) 0.0408(5) 0.0103(3) 0.0121(4) 0.0049(3) B1 0.040(2) 0.046(2) 0.045(2) 0.0105(17) 0.0103(17) 0.0158(17) N1 0.046(3) 0.064(3) 0.055(3) 0.023(2) 0.012(2) 0.029(2) C1 0.043(4) 0.082(5) 0.054(4) 0.033(4) 0.009(3) 0.022(4) C2 0.090(5) 0.068(4) 0.083(5) 0.032(4) 0.017(4) 0.046(4) C3 0.040(3) 0.097(6) 0.075(5) 0.035(4) 0.005(3) 0.024(4) B11 0.040(2) 0.046(2) 0.045(2) 0.0105(17) 0.0103(17) 0.0158(17) N11 0.046(3) 0.064(3) 0.055(3) 0.023(2) 0.012(2) 0.029(2) C101 0.054(8) 0.069(8) 0.069(8) 0.031(6) 0.012(6) 0.014(6) C102 0.096(9) 0.068(8) 0.090(9) 0.024(7) 0.005(7) 0.041(7) C103 0.052(6) 0.083(7) 0.072(7) 0.033(6) 0.010(5) 0.030(6) C4 0.0329(17) 0.0382(18) 0.054(2) 0.0163(16) 0.0135(15) 0.0077(14) C5 0.0388(18) 0.0361(18) 0.059(2) 0.0160(17) 0.0159(16) 0.0133(15) C6 0.0427(19) 0.0341(18) 0.050(2) 0.0077(15) 0.0190(16) 0.0071(15) C7 0.0301(16) 0.0335(17) 0.053(2) 0.0106(15) 0.0040(14) 0.0059(13) C8 0.042(2) 0.041(2) 0.064(3) 0.0234(19) 0.0101(18) 0.0004(16) C9 0.050(2) 0.048(2) 0.090(3) 0.036(2) 0.015(2) 0.0060(19) C10 0.048(2) 0.040(2) 0.102(4) 0.027(2) 0.012(2) 0.0073(18) C11 0.076(3) 0.041(2) 0.076(3) -0.008(2) -0.006(3) -0.002(2) C12 0.069(3) 0.042(2) 0.063(3) 0.008(2) -0.002(2) 0.005(2) C13 0.044(2) 0.042(3) 0.042(2) 0.020(2) -0.002(2) 0.002(2) C14 0.058(3) 0.070(3) 0.040(2) 0.021(2) 0.005(2) 0.011(2) C15 0.082(4) 0.080(3) 0.045(3) 0.025(3) 0.010(3) 0.005(3) C16 0.098(4) 0.077(4) 0.054(3) 0.033(3) -0.012(3) 0.003(3) C17 0.081(4) 0.076(4) 0.071(3) 0.034(3) -0.019(3) 0.019(3) C18 0.058(3) 0.057(3) 0.062(3) 0.028(3) -0.007(2) 0.016(2) C113 0.050(5) 0.052(5) 0.045(5) 0.020(4) -0.001(4) 0.012(4) C114 0.061(5) 0.065(5) 0.047(4) 0.025(4) 0.003(4) 0.011(4) C115 0.082(5) 0.077(5) 0.059(5) 0.031(5) 0.002(5) 0.010(5) C116 0.083(5) 0.074(6) 0.062(5) 0.032(5) -0.009(5) 0.019(5) C117 0.077(5) 0.071(5) 0.068(5) 0.027(4) -0.010(5) 0.013(5) C118 0.058(5) 0.054(5) 0.058(5) 0.021(4) -0.004(4) 0.012(4) C19 0.0411(18) 0.0259(15) 0.0432(19) 0.0068(14) 0.0083(15) 0.0064(13) C20 0.054(3) 0.074(3) 0.050(2) 0.021(2) 0.0016(19) -0.001(2) C21 0.071(3) 0.091(4) 0.049(3) 0.026(3) 0.000(2) 0.007(3) C22 0.057(3) 0.044(2) 0.065(3) 0.003(2) -0.009(2) 0.0157(19) C23 0.042(2) 0.058(3) 0.104(4) 0.037(3) -0.008(2) 0.0016(19) C24 0.043(2) 0.059(3) 0.084(3) 0.040(2) 0.003(2) 0.0015(19) C25 0.035(2) 0.036(2) 0.050(3) 0.0207(19) 0.012(2) 0.0062(18) C26 0.066(3) 0.058(3) 0.052(3) 0.028(2) 0.008(2) -0.006(2) C27 0.081(4) 0.080(4) 0.068(3) 0.044(3) 0.008(3) -0.003(3) C28 0.061(3) 0.070(3) 0.087(3) 0.052(3) 0.023(3) 0.014(3) C29 0.070(3) 0.045(3) 0.086(3) 0.033(2) 0.023(3) 0.018(2) C30 0.063(3) 0.040(2) 0.059(3) 0.022(2) 0.016(2) 0.017(2) C125 0.051(5) 0.044(5) 0.049(5) 0.023(4) 0.010(4) 0.011(4) C126 0.062(5) 0.052(5) 0.056(5) 0.026(4) 0.016(4) 0.010(4) C127 0.073(6) 0.067(6) 0.068(6) 0.034(5) 0.020(5) 0.007(5) C128 0.070(6) 0.062(5) 0.077(5) 0.043(4) 0.012(5) 0.010(5) C129 0.066(5) 0.051(5) 0.076(5) 0.033(4) 0.012(4) 0.018(4) C130 0.052(5) 0.039(4) 0.058(4) 0.024(4) 0.009(4) 0.022(4) B200 0.0211(15) 0.0318(17) 0.0297(16) 0.0093(14) 0.0050(12) 0.0022(13) C201 0.0186(13) 0.0298(15) 0.0359(16) 0.0108(12) 0.0069(11) 0.0061(11) C202 0.0234(14) 0.0323(16) 0.0372(16) 0.0113(13) 0.0091(12) 0.0056(12) C203 0.0257(15) 0.0322(16) 0.049(2) 0.0085(15) 0.0112(14) 0.0063(12) C204 0.0320(16) 0.0299(16) 0.061(2) 0.0183(16) 0.0150(15) 0.0060(13) C205 0.0310(16) 0.0398(18) 0.055(2) 0.0238(16) 0.0123(15) 0.0116(14) C206 0.0278(15) 0.0362(17) 0.0382(17) 0.0145(14) 0.0056(13) 0.0074(13) C207 0.040(2) 0.040(2) 0.060(2) 0.0062(18) 0.0107(18) 0.0027(16) F1 0.043(2) 0.150(5) 0.095(3) -0.051(3) -0.024(2) 0.029(3) F2 0.068(2) 0.058(2) 0.0476(17) -0.0021(15) 0.0160(15) -0.0079(17) F3 0.169(6) 0.0358(18) 0.081(3) 0.0013(17) 0.020(3) -0.019(3) F101 0.077(9) 0.086(10) 0.079(9) -0.013(8) 0.025(8) 0.020(8) F102 0.055(8) 0.056(8) 0.051(7) 0.005(6) 0.012(6) -0.028(6) F103 0.097(11) 0.049(7) 0.060(8) 0.014(6) -0.029(8) -0.012(7) C208 0.057(2) 0.060(3) 0.065(3) 0.039(2) 0.011(2) 0.008(2) F4 0.133(3) 0.074(2) 0.090(2) 0.0561(18) 0.017(2) -0.0105(19) F5 0.081(2) 0.183(4) 0.138(3) 0.124(3) 0.001(2) 0.023(2) F6 0.158(4) 0.095(2) 0.0609(18) 0.0453(18) 0.034(2) 0.027(2) C209 0.0234(14) 0.0290(15) 0.0347(16) 0.0101(12) 0.0065(12) 0.0035(11) C210 0.0249(15) 0.0387(17) 0.0358(17) 0.0113(14) 0.0056(12) 0.0025(13) C211 0.0262(16) 0.046(2) 0.0453(19) 0.0136(16) 0.0136(14) 0.0033(14) C212 0.0213(15) 0.059(2) 0.053(2) 0.0170(18) 0.0114(14) 0.0057(15) C213 0.0240(15) 0.050(2) 0.049(2) 0.0187(17) 0.0029(14) 0.0055(14) C214 0.0283(15) 0.0388(17) 0.0359(17) 0.0131(14) 0.0063(13) 0.0054(13) C215 0.037(2) 0.080(3) 0.050(2) 0.012(2) 0.0181(18) 0.005(2) F7 0.098(5) 0.067(3) 0.058(3) 0.004(2) 0.025(3) 0.015(3) F8 0.077(4) 0.098(3) 0.047(2) 0.036(2) 0.024(2) 0.009(3) F9 0.036(2) 0.186(7) 0.063(3) 0.036(4) 0.0249(19) 0.002(3) F107 0.139(11) 0.108(8) 0.095(7) 0.042(6) 0.069(7) -0.002(7) F108 0.063(6) 0.129(10) 0.062(5) 0.015(6) 0.039(4) 0.043(6) F109 0.045(5) 0.104(8) 0.045(5) 0.004(5) 0.012(4) 0.013(5) C216 0.0293(19) 0.093(4) 0.064(3) 0.026(3) -0.0004(18) 0.011(2) F10 0.025(2) 0.158(7) 0.083(4) 0.044(4) 0.003(2) 0.027(3) F11 0.073(4) 0.172(7) 0.094(5) 0.088(5) -0.022(3) -0.005(4) F12 0.083(5) 0.104(5) 0.103(5) -0.012(4) -0.048(4) 0.012(4) F110 0.035(4) 0.165(10) 0.049(4) 0.031(6) -0.001(3) 0.024(6) F111 0.047(5) 0.124(9) 0.086(6) 0.027(6) -0.015(4) -0.028(5) F112 0.117(9) 0.142(8) 0.140(9) 0.052(7) -0.039(7) 0.068(7) C217 0.0251(14) 0.0276(14) 0.0304(15) 0.0071(12) 0.0052(11) 0.0057(11) C218 0.0249(14) 0.0318(15) 0.0348(16) 0.0124(13) 0.0064(12) 0.0036(12) C219 0.0265(15) 0.0352(17) 0.0420(18) 0.0122(14) 0.0031(13) 0.0056(13) C220 0.0312(16) 0.0403(18) 0.0465(19) 0.0190(15) 0.0012(14) 0.0079(14) C221 0.0367(18) 0.0369(18) 0.057(2) 0.0247(17) 0.0084(16) 0.0070(14) C222 0.0251(15) 0.0327(16) 0.0500(19) 0.0178(15) 0.0045(13) 0.0023(12) C223 0.0313(18) 0.057(2) 0.069(3) 0.034(2) -0.0053(17) 0.0042(16) F13 0.0467(13) 0.0584(16) 0.088(2) 0.0261(14) -0.0143(13) -0.0148(11) F14 0.0308(12) 0.108(2) 0.100(2) 0.0401(19) 0.0216(13) 0.0085(13) F15 0.0363(13) 0.099(2) 0.152(3) 0.086(2) -0.0241(16) -0.0024(13) C224 0.042(2) 0.066(3) 0.100(4) 0.057(3) 0.012(2) 0.005(2) F16 0.057(3) 0.095(6) 0.179(8) 0.106(6) 0.013(4) 0.017(4) F17 0.092(5) 0.045(3) 0.127(5) 0.052(3) 0.022(4) -0.005(3) F18 0.091(5) 0.084(4) 0.068(4) 0.046(4) 0.025(4) 0.001(4) F116 0.051(4) 0.102(6) 0.089(6) 0.073(5) 0.014(4) 0.006(4) F117 0.075(4) 0.088(6) 0.095(5) 0.073(5) -0.004(4) -0.008(4) F118 0.170(9) 0.043(4) 0.136(7) 0.046(4) 0.069(7) 0.025(5) C225 0.0272(14) 0.0318(15) 0.0313(15) 0.0118(13) 0.0036(12) 0.0072(12) C226 0.0276(15) 0.0367(17) 0.0338(16) 0.0085(13) 0.0063(12) 0.0076(13) C227 0.0330(17) 0.0430(19) 0.0340(17) 0.0090(14) 0.0067(13) 0.0117(14) C228 0.046(2) 0.0395(19) 0.0321(17) 0.0033(14) 0.0078(14) 0.0105(15) C229 0.048(2) 0.0324(17) 0.0413(19) 0.0061(15) 0.0047(16) 0.0012(15) C230 0.0356(17) 0.0346(17) 0.0372(17) 0.0108(14) 0.0098(14) 0.0045(13) C231 0.043(2) 0.061(3) 0.045(2) 0.0098(19) 0.0160(17) 0.0154(18) F19 0.034(3) 0.101(6) 0.065(4) 0.013(4) 0.010(2) 0.012(3) F20 0.073(4) 0.103(5) 0.100(6) 0.053(5) 0.053(4) 0.025(4) F21 0.065(4) 0.103(5) 0.055(4) -0.020(3) 0.031(3) -0.002(4) F119 0.072(5) 0.145(9) 0.076(6) 0.061(6) 0.038(4) 0.035(6) F120 0.071(5) 0.072(5) 0.090(7) 0.003(4) 0.044(5) 0.034(4) F121 0.056(5) 0.061(5) 0.069(5) -0.005(4) 0.040(4) -0.007(3) C232 0.067(3) 0.047(2) 0.061(3) 0.001(2) 0.020(2) -0.010(2) F22 0.106(6) 0.089(5) 0.065(4) -0.027(4) 0.024(4) -0.038(4) F23 0.099(5) 0.051(3) 0.139(6) 0.037(3) 0.020(4) -0.021(3) F24 0.044(3) 0.069(4) 0.130(7) 0.006(4) -0.018(4) -0.012(3) C332 0.067(3) 0.047(2) 0.061(3) 0.001(2) 0.020(2) -0.010(2) F122 0.098(6) 0.085(6) 0.073(5) -0.004(4) 0.022(4) -0.048(5) F123 0.071(4) 0.086(5) 0.096(5) 0.036(4) -0.044(4) -0.025(4) F124 0.069(4) 0.037(3) 0.113(7) -0.011(4) -0.021(4) 0.007(3) C801 0.094(5) 0.104(5) 0.065(3) 0.019(3) 0.001(3) 0.028(4) C802 0.107(5) 0.058(3) 0.081(4) 0.031(3) 0.003(3) 0.017(3) C803 0.101(5) 0.097(4) 0.072(3) 0.040(3) 0.014(3) 0.042(4) C804 0.104(5) 0.089(4) 0.064(3) 0.031(3) 0.004(3) 0.007(4) C805 0.131(6) 0.068(4) 0.077(4) 0.020(3) 0.005(4) 0.018(4) C806 0.141(6) 0.064(3) 0.061(3) 0.010(3) 0.010(4) 0.043(4) F801 0.120(3) 0.118(3) 0.164(4) 0.065(3) 0.034(3) 0.035(2) F802 0.120(3) 0.118(3) 0.164(4) 0.065(3) 0.034(3) 0.035(2) F803 0.120(3) 0.118(3) 0.164(4) 0.065(3) 0.034(3) 0.035(2) F804 0.120(3) 0.118(3) 0.164(4) 0.065(3) 0.034(3) 0.035(2) C901 0.086(5) 0.087(5) 0.084(5) 0.031(4) 0.005(4) 0.020(4) C902 0.085(5) 0.085(5) 0.067(4) 0.029(4) 0.005(4) 0.027(4) C903 0.090(5) 0.087(5) 0.081(5) 0.034(4) 0.011(4) 0.025(4) C904 0.086(5) 0.087(5) 0.084(5) 0.031(4) 0.005(4) 0.020(4) C905 0.085(5) 0.085(5) 0.067(4) 0.029(4) 0.005(4) 0.027(4) C906 0.090(5) 0.087(5) 0.081(5) 0.034(4) 0.011(4) 0.025(4) F901 0.120(6) 0.131(6) 0.116(6) 0.051(5) 0.006(5) 0.026(5) F902 0.120(6) 0.131(6) 0.116(6) 0.051(5) 0.006(5) 0.026(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 P2 2.1986(9) . ? Rh1 P1 2.1998(9) . ? P1 C13 1.826(3) . ? P1 C4 1.826(4) . ? P1 C7 1.829(4) . ? P1 C113 1.830(8) . ? P2 C125 1.784(7) . ? P2 C19 1.827(4) . ? P2 C6 1.833(4) . ? P2 C25 1.857(3) . ? B1 N1 1.592(7) . ? B1 H1A 1.1649 . ? B1 H1B 1.1649 . ? B1 H1C 1.1649 . ? N1 C1 1.488(6) . ? N1 C3 1.494(6) . ? N1 C2 1.499(7) . ? C1 H1D 0.9800 . ? C1 H1E 0.9800 . ? C1 H1F 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? N11 C101 1.491(8) . ? N11 C103 1.493(8) . ? N11 C102 1.495(8) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C102 H10D 0.9800 . ? C102 H10E 0.9800 . ? C102 H10F 0.9800 . ? C103 H10G 0.9800 . ? C103 H10H 0.9800 . ? C103 H10I 0.9800 . ? C4 C5 1.528(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.528(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.374(6) . ? C7 C12 1.385(6) . ? C8 C9 1.386(6) . ? C8 H8 0.9500 . ? C9 C10 1.358(7) . ? C9 H9 0.9500 . ? C10 C11 1.351(8) . ? C10 H10 0.9500 . ? C11 C12 1.411(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 H14 0.9500 . ? C15 C16 1.3900 . ? C15 H15 0.9500 . ? C16 C17 1.3900 . ? C16 H16 0.9500 . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C113 C114 1.3900 . ? C113 C118 1.3900 . ? C114 C115 1.3900 . ? C114 H114 0.9500 . ? C115 C116 1.3900 . ? C115 H115 0.9500 . ? C116 C117 1.3900 . ? C116 H116 0.9500 . ? C117 C118 1.3900 . ? C117 H117 0.9500 . ? C118 H118 0.9500 . ? C19 C20 1.366(6) . ? C19 C24 1.379(6) . ? C20 C21 1.394(7) . ? C20 H20 0.9500 . ? C21 C22 1.354(8) . ? C21 H21 0.9500 . ? C22 C23 1.367(8) . ? C22 H22 0.9500 . ? C23 C24 1.386(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C26 H26 0.9500 . ? C27 C28 1.3900 . ? C27 H27 0.9500 . ? C28 C29 1.3900 . ? C28 H28 0.9500 . ? C29 C30 1.3900 . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C125 C126 1.3900 . ? C125 C130 1.3900 . ? C126 C127 1.3900 . ? C126 H126 0.9500 . ? C127 C128 1.3900 . ? C127 H127 0.9500 . ? C128 C129 1.3900 . ? C128 H128 0.9500 . ? C129 C130 1.3900 . ? C129 H129 0.9500 . ? C130 H130 0.9500 . ? B200 C201 1.635(5) . ? B200 C225 1.636(5) . ? B200 C209 1.643(4) . ? B200 C217 1.644(5) . ? C201 C202 1.402(4) . ? C201 C206 1.404(5) . ? C202 C203 1.394(5) . ? C202 H202 0.9500 . ? C203 C204 1.387(5) . ? C203 C207 1.490(5) . ? C204 C205 1.372(5) . ? C204 H204 0.9500 . ? C205 C206 1.391(5) . ? C205 C208 1.501(6) . ? C206 H206 0.9500 . ? C207 F102 1.302(7) . ? C207 F1 1.304(5) . ? C207 F2 1.311(5) . ? C207 F101 1.317(7) . ? C207 F3 1.329(5) . ? C207 F103 1.335(7) . ? C208 F4 1.317(5) . ? C208 F5 1.320(6) . ? C208 F6 1.326(6) . ? C209 C210 1.398(5) . ? C209 C214 1.400(5) . ? C210 C211 1.394(4) . ? C210 H210 0.9500 . ? C211 C212 1.384(5) . ? C211 C215 1.485(5) . ? C212 C213 1.390(5) . ? C212 H212 0.9500 . ? C213 C214 1.386(5) . ? C213 C216 1.493(6) . ? C214 H214 0.9500 . ? C215 F107 1.278(7) . ? C215 F7 1.304(6) . ? C215 F9 1.313(5) . ? C215 F109 1.336(7) . ? C215 F108 1.379(6) . ? C215 F8 1.395(5) . ? C216 F110 1.278(6) . ? C216 F10 1.282(5) . ? C216 F11 1.322(6) . ? C216 F111 1.327(6) . ? C216 F112 1.333(7) . ? C216 F12 1.342(6) . ? C217 C222 1.398(5) . ? C217 C218 1.400(4) . ? C218 C219 1.383(5) . ? C218 H218 0.9500 . ? C219 C220 1.379(5) . ? C219 C223 1.496(5) . ? C220 C221 1.382(5) . ? C220 H220 0.9500 . ? C221 C222 1.388(5) . ? C221 C224 1.485(5) . ? C222 H222 0.9500 . ? C223 F14 1.326(6) . ? C223 F13 1.337(5) . ? C223 F15 1.343(5) . ? C224 F118 1.267(6) . ? C224 F18 1.289(6) . ? C224 F16 1.305(5) . ? C224 F116 1.334(6) . ? C224 F117 1.392(6) . ? C224 F17 1.407(6) . ? C225 C230 1.395(5) . ? C225 C226 1.405(4) . ? C226 C227 1.387(5) . ? C226 H226 0.9500 . ? C227 C228 1.391(5) . ? C227 C231 1.499(5) . ? C228 C229 1.364(5) . ? C228 H228 0.9500 . ? C229 C230 1.399(5) . ? C229 C232 1.513(7) . ? C229 C332 1.521(8) . ? C230 H230 0.9500 . ? C231 F21 1.285(6) . ? C231 F121 1.288(6) . ? C231 F119 1.327(6) . ? C231 F19 1.335(6) . ? C231 F120 1.353(6) . ? C231 F20 1.356(6) . ? C232 F24 1.301(7) . ? C232 F23 1.310(7) . ? C232 F22 1.313(7) . ? C332 F122 1.308(7) . ? C332 F123 1.314(7) . ? C332 F124 1.323(7) . ? C801 C802 1.3900 . ? C801 C806 1.3900 . ? C801 H801 0.9500 . ? C802 C803 1.3900 . ? C802 H802 0.9500 . ? C803 C804 1.3900 . ? C803 H803 0.9500 . ? C804 C805 1.3900 . ? C804 H804 0.9500 . ? C805 C806 1.3900 . ? C805 H805 0.9500 . ? C806 H806 0.9500 . ? C901 F901 1.30(3) . ? C901 C902 1.3900 . ? C901 C906 1.3900 . ? C902 F902 1.31(3) . ? C902 C903 1.3900 . ? C903 C904 1.3900 . ? C903 H903 0.9500 . ? C904 C905 1.3900 . ? C904 H904 0.9500 . ? C905 C906 1.3900 . ? C905 H905 0.9500 . ? C906 H906 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Rh1 P1 91.14(3) . . ? C13 P1 C4 106.07(19) . . ? C13 P1 C7 104.96(19) . . ? C4 P1 C7 102.48(17) . . ? C13 P1 C113 8.6(6) . . ? C4 P1 C113 102.8(6) . . ? C7 P1 C113 113.6(6) . . ? C13 P1 Rh1 114.40(14) . . ? C4 P1 Rh1 119.67(13) . . ? C7 P1 Rh1 107.71(12) . . ? C113 P1 Rh1 110.6(5) . . ? C125 P2 C19 97.0(5) . . ? C125 P2 C6 106.0(4) . . ? C19 P2 C6 103.73(18) . . ? C125 P2 C25 9.5(5) . . ? C19 P2 C25 106.24(17) . . ? C6 P2 C25 101.51(19) . . ? C125 P2 Rh1 119.0(4) . . ? C19 P2 Rh1 108.92(11) . . ? C6 P2 Rh1 119.01(12) . . ? C25 P2 Rh1 116.09(12) . . ? C1 N1 C3 109.3(5) . . ? C1 N1 C2 109.5(5) . . ? C3 N1 C2 108.6(5) . . ? C1 N1 B1 111.7(4) . . ? C3 N1 B1 109.2(4) . . ? C2 N1 B1 108.5(4) . . ? C101 N11 C103 109.2(7) . . ? C101 N11 C102 108.9(7) . . ? C103 N11 C102 109.0(7) . . ? N11 C101 H10A 109.5 . . ? N11 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? N11 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? N11 C102 H10D 109.5 . . ? N11 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? N11 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? N11 C103 H10G 109.5 . . ? N11 C103 H10H 109.5 . . ? H10G C103 H10H 109.5 . . ? N11 C103 H10I 109.5 . . ? H10G C103 H10I 109.5 . . ? H10H C103 H10I 109.5 . . ? C5 C4 P1 114.1(2) . . ? C5 C4 H4A 108.7 . . ? P1 C4 H4A 108.7 . . ? C5 C4 H4B 108.7 . . ? P1 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C4 C5 C6 112.8(3) . . ? C4 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? C4 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C5 C6 P2 113.2(3) . . ? C5 C6 H6A 108.9 . . ? P2 C6 H6A 108.9 . . ? C5 C6 H6B 108.9 . . ? P2 C6 H6B 108.9 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C12 118.1(4) . . ? C8 C7 P1 118.2(3) . . ? C12 C7 P1 123.7(3) . . ? C7 C8 C9 122.1(4) . . ? C7 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C10 C9 C8 119.4(5) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C11 C10 C9 120.3(4) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 121.0(5) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C7 C12 C11 119.1(5) . . ? C7 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 C18 120.0 . . ? C14 C13 P1 116.5(2) . . ? C18 C13 P1 123.2(2) . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C114 C113 C118 120.0 . . ? C114 C113 P1 122.6(9) . . ? C118 C113 P1 117.4(9) . . ? C115 C114 C113 120.0 . . ? C115 C114 H114 120.0 . . ? C113 C114 H114 120.0 . . ? C116 C115 C114 120.0 . . ? C116 C115 H115 120.0 . . ? C114 C115 H115 120.0 . . ? C117 C116 C115 120.0 . . ? C117 C116 H116 120.0 . . ? C115 C116 H116 120.0 . . ? C116 C117 C118 120.0 . . ? C116 C117 H117 120.0 . . ? C118 C117 H117 120.0 . . ? C117 C118 C113 120.0 . . ? C117 C118 H118 120.0 . . ? C113 C118 H118 120.0 . . ? C20 C19 C24 118.8(4) . . ? C20 C19 P2 119.9(3) . . ? C24 C19 P2 121.2(3) . . ? C19 C20 C21 120.0(5) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 121.3(5) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 118.9(4) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C22 C23 C24 120.5(5) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C19 C24 C23 120.5(5) . . ? C19 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C26 C25 C30 120.0 . . ? C26 C25 P2 119.7(2) . . ? C30 C25 P2 120.2(2) . . ? C27 C26 C25 120.0 . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? C126 C125 C130 120.0 . . ? C126 C125 P2 118.2(7) . . ? C130 C125 P2 121.6(7) . . ? C125 C126 C127 120.0 . . ? C125 C126 H126 120.0 . . ? C127 C126 H126 120.0 . . ? C128 C127 C126 120.0 . . ? C128 C127 H127 120.0 . . ? C126 C127 H127 120.0 . . ? C127 C128 C129 120.0 . . ? C127 C128 H128 120.0 . . ? C129 C128 H128 120.0 . . ? C130 C129 C128 120.0 . . ? C130 C129 H129 120.0 . . ? C128 C129 H129 120.0 . . ? C129 C130 C125 120.0 . . ? C129 C130 H130 120.0 . . ? C125 C130 H130 120.0 . . ? C201 B200 C225 112.5(3) . . ? C201 B200 C209 105.4(2) . . ? C225 B200 C209 112.8(2) . . ? C201 B200 C217 110.9(2) . . ? C225 B200 C217 103.3(2) . . ? C209 B200 C217 112.1(3) . . ? C202 C201 C206 115.7(3) . . ? C202 C201 B200 121.0(3) . . ? C206 C201 B200 123.3(3) . . ? C203 C202 C201 122.1(3) . . ? C203 C202 H202 119.0 . . ? C201 C202 H202 119.0 . . ? C204 C203 C202 120.7(3) . . ? C204 C203 C207 120.7(3) . . ? C202 C203 C207 118.6(3) . . ? C205 C204 C203 118.2(3) . . ? C205 C204 H204 120.9 . . ? C203 C204 H204 120.9 . . ? C204 C205 C206 121.4(3) . . ? C204 C205 C208 120.3(3) . . ? C206 C205 C208 118.2(4) . . ? C205 C206 C201 121.9(3) . . ? C205 C206 H206 119.1 . . ? C201 C206 H206 119.1 . . ? F102 C207 F1 65.0(8) . . ? F102 C207 F2 129.0(7) . . ? F1 C207 F2 106.7(4) . . ? F102 C207 F101 105.6(7) . . ? F1 C207 F101 131.7(8) . . ? F2 C207 F101 40.3(11) . . ? F102 C207 F3 43.9(9) . . ? F1 C207 F3 106.6(4) . . ? F2 C207 F3 104.6(4) . . ? F101 C207 F3 67.5(10) . . ? F102 C207 F103 104.0(6) . . ? F1 C207 F103 43.6(9) . . ? F2 C207 F103 67.2(10) . . ? F101 C207 F103 104.1(7) . . ? F3 C207 F103 133.5(6) . . ? F102 C207 C203 115.8(6) . . ? F1 C207 C203 112.8(3) . . ? F2 C207 C203 113.5(3) . . ? F101 C207 C203 113.3(6) . . ? F3 C207 C203 112.1(4) . . ? F103 C207 C203 112.9(6) . . ? F4 C208 F5 107.8(4) . . ? F4 C208 F6 105.4(4) . . ? F5 C208 F6 105.4(5) . . ? F4 C208 C205 113.3(4) . . ? F5 C208 C205 111.9(4) . . ? F6 C208 C205 112.5(4) . . ? C210 C209 C214 115.9(3) . . ? C210 C209 B200 122.1(3) . . ? C214 C209 B200 121.8(3) . . ? C211 C210 C209 122.2(3) . . ? C211 C210 H210 118.9 . . ? C209 C210 H210 118.9 . . ? C212 C211 C210 120.6(3) . . ? C212 C211 C215 120.0(3) . . ? C210 C211 C215 119.4(3) . . ? C211 C212 C213 118.4(3) . . ? C211 C212 H212 120.8 . . ? C213 C212 H212 120.8 . . ? C214 C213 C212 120.6(3) . . ? C214 C213 C216 119.7(3) . . ? C212 C213 C216 119.7(3) . . ? C213 C214 C209 122.4(3) . . ? C213 C214 H214 118.8 . . ? C209 C214 H214 118.8 . . ? F107 C215 F7 121.5(8) . . ? F107 C215 F9 68.1(7) . . ? F7 C215 F9 111.4(5) . . ? F107 C215 F109 108.9(6) . . ? F7 C215 F109 22.5(7) . . ? F9 C215 F109 126.9(6) . . ? F107 C215 F108 106.8(6) . . ? F7 C215 F108 79.4(6) . . ? F9 C215 F108 41.3(5) . . ? F109 C215 F108 101.1(6) . . ? F107 C215 F8 33.5(8) . . ? F7 C215 F8 103.0(4) . . ? F9 C215 F8 100.7(4) . . ? F109 C215 F8 83.5(7) . . ? F108 C215 F8 134.7(6) . . ? F107 C215 C211 117.1(6) . . ? F7 C215 C211 114.7(4) . . ? F9 C215 C211 114.9(4) . . ? F109 C215 C211 112.6(5) . . ? F108 C215 C211 109.0(5) . . ? F8 C215 C211 110.5(3) . . ? F110 C216 F10 125.1(6) . . ? F110 C216 F11 66.4(6) . . ? F10 C216 F11 107.6(5) . . ? F110 C216 F111 106.3(6) . . ? F10 C216 F111 36.6(6) . . ? F11 C216 F111 133.3(7) . . ? F110 C216 F112 106.8(6) . . ? F10 C216 F112 68.3(7) . . ? F11 C216 F112 45.1(7) . . ? F111 C216 F112 103.6(6) . . ? F110 C216 F12 37.8(6) . . ? F10 C216 F12 106.4(5) . . ? F11 C216 F12 103.1(5) . . ? F111 C216 F12 74.8(6) . . ? F112 C216 F12 135.0(7) . . ? F110 C216 C213 116.6(4) . . ? F10 C216 C213 115.6(4) . . ? F11 C216 C213 112.3(4) . . ? F111 C216 C213 111.6(5) . . ? F112 C216 C213 111.0(5) . . ? F12 C216 C213 111.0(4) . . ? C222 C217 C218 115.3(3) . . ? C222 C217 B200 122.8(3) . . ? C218 C217 B200 121.7(3) . . ? C219 C218 C217 122.3(3) . . ? C219 C218 H218 118.8 . . ? C217 C218 H218 118.8 . . ? C220 C219 C218 121.5(3) . . ? C220 C219 C223 120.9(3) . . ? C218 C219 C223 117.6(3) . . ? C219 C220 C221 117.4(3) . . ? C219 C220 H220 121.3 . . ? C221 C220 H220 121.3 . . ? C220 C221 C222 121.2(3) . . ? C220 C221 C224 119.6(3) . . ? C222 C221 C224 119.2(3) . . ? C221 C222 C217 122.3(3) . . ? C221 C222 H222 118.9 . . ? C217 C222 H222 118.9 . . ? F14 C223 F13 104.7(3) . . ? F14 C223 F15 107.1(4) . . ? F13 C223 F15 105.9(4) . . ? F14 C223 C219 113.8(3) . . ? F13 C223 C219 112.0(3) . . ? F15 C223 C219 112.6(3) . . ? F118 C224 F18 120.3(7) . . ? F118 C224 F16 64.3(5) . . ? F18 C224 F16 113.1(5) . . ? F118 C224 F116 109.4(6) . . ? F18 C224 F116 22.0(6) . . ? F16 C224 F116 128.3(6) . . ? F118 C224 F117 105.5(5) . . ? F18 C224 F117 78.4(6) . . ? F16 C224 F117 44.5(4) . . ? F116 C224 F117 99.8(5) . . ? F118 C224 F17 35.9(5) . . ? F18 C224 F17 102.4(5) . . ? F16 C224 F17 99.8(5) . . ? F116 C224 F17 83.5(6) . . ? F117 C224 F17 136.0(5) . . ? F118 C224 C221 117.5(5) . . ? F18 C224 C221 115.9(5) . . ? F16 C224 C221 115.0(4) . . ? F116 C224 C221 112.5(5) . . ? F117 C224 C221 110.5(4) . . ? F17 C224 C221 108.3(4) . . ? C230 C225 C226 115.3(3) . . ? C230 C225 B200 123.6(3) . . ? C226 C225 B200 120.7(3) . . ? C227 C226 C225 122.4(3) . . ? C227 C226 H226 118.8 . . ? C225 C226 H226 118.8 . . ? C226 C227 C228 120.7(3) . . ? C226 C227 C231 118.9(3) . . ? C228 C227 C231 120.3(3) . . ? C229 C228 C227 117.9(3) . . ? C229 C228 H228 121.0 . . ? C227 C228 H228 121.0 . . ? C228 C229 C230 121.5(3) . . ? C228 C229 C232 120.7(4) . . ? C230 C229 C232 117.7(4) . . ? C228 C229 C332 118.3(4) . . ? C230 C229 C332 119.9(4) . . ? C232 C229 C332 10.0(5) . . ? C225 C230 C229 122.1(3) . . ? C225 C230 H230 119.0 . . ? C229 C230 H230 119.0 . . ? F21 C231 F121 120.4(7) . . ? F21 C231 F119 76.5(6) . . ? F121 C231 F119 108.8(6) . . ? F21 C231 F19 108.3(5) . . ? F121 C231 F19 23.2(7) . . ? F119 C231 F19 127.8(7) . . ? F21 C231 F120 26.8(6) . . ? F121 C231 F120 106.9(5) . . ? F119 C231 F120 102.9(5) . . ? F19 C231 F120 88.4(7) . . ? F21 C231 F20 107.2(5) . . ? F121 C231 F20 79.5(6) . . ? F119 C231 F20 34.7(5) . . ? F19 C231 F20 102.1(5) . . ? F120 C231 F20 130.5(6) . . ? F21 C231 C227 115.9(5) . . ? F121 C231 C227 115.9(5) . . ? F119 C231 C227 111.9(4) . . ? F19 C231 C227 111.5(4) . . ? F120 C231 C227 109.5(5) . . ? F20 C231 C227 110.8(4) . . ? F24 C232 F23 106.6(6) . . ? F24 C232 F22 108.1(6) . . ? F23 C232 F22 107.2(6) . . ? F24 C232 C229 111.1(5) . . ? F23 C232 C229 111.9(5) . . ? F22 C232 C229 111.7(6) . . ? F122 C332 F123 105.8(7) . . ? F122 C332 F124 105.9(7) . . ? F123 C332 F124 105.0(6) . . ? F122 C332 C229 112.8(6) . . ? F123 C332 C229 114.8(6) . . ? F124 C332 C229 111.7(6) . . ? C802 C801 C806 120.0 . . ? C802 C801 H801 120.0 . . ? C806 C801 H801 120.0 . . ? C803 C802 C801 120.0 . . ? C803 C802 H802 120.0 . . ? C801 C802 H802 120.0 . . ? C804 C803 C802 120.0 . . ? C804 C803 H803 120.0 . . ? C802 C803 H803 120.0 . . ? C803 C804 C805 120.0 . . ? C803 C804 H804 120.0 . . ? C805 C804 H804 120.0 . . ? C806 C805 C804 120.0 . . ? C806 C805 H805 120.0 . . ? C804 C805 H805 120.0 . . ? C805 C806 C801 120.0 . . ? C805 C806 H806 120.0 . . ? C801 C806 H806 120.0 . . ? F901 C901 C902 120.3(5) . . ? F901 C901 C906 119.7(5) . . ? C902 C901 C906 120.0 . . ? F902 C902 C903 120.3(5) . . ? F902 C902 C901 119.7(5) . . ? C903 C902 C901 120.0 . . ? C904 C903 C902 120.0 . . ? C904 C903 H903 120.0 . . ? C902 C903 H903 120.0 . . ? C903 C904 C905 120.0 . . ? C903 C904 H904 120.0 . . ? C905 C904 H904 120.0 . . ? C904 C905 C906 120.0 . . ? C904 C905 H905 120.0 . . ? C906 C905 H905 120.0 . . ? C905 C906 C901 120.0 . . ? C905 C906 H906 120.0 . . ? C901 C906 H906 120.0 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.840 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.075 # Attachment '- Compound2d.cif' data_172abc10 _database_code_depnum_ccdc_archive 'CCDC 801542' #TrackingRef '- Compound2d.cif' #---------------------------------------------- # [Rh(Ph2P(CH2)5PPh2)(H3BNMe3)][BArF4].Pentane #---------------------------------------------- # start Validation Reply Form _vrf_PLAT242_172abc10 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C207 PROBLEM: Check Low Ueq as Compared to Neighbors for C232 RESPONSE: The anion contains a significant degree of disorder. See _refine_special_details. ; _vrf_PLAT301_172abc10 ; PROBLEM: Note: Main Residue Disorder ................... 11.00 Perc. RESPONSE: The structure contains a significant degree of disorder. See _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, C32 H42 B N P2 Rh, C5 H12' _chemical_formula_sum 'C69 H66 B2 F24 N P2 Rh' _chemical_formula_weight 1551.70 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 14.94180(10) _cell_length_b 19.2670(2) _cell_length_c 25.1468(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.2143(3) _cell_angle_gamma 90.00 _cell_volume 7237.73(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16824 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description irregular _exptl_crystal_colour violet _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3152 _exptl_absorpt_coefficient_mu 0.382 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.860 _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 28480 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 26.37 _reflns_number_total 14685 _reflns_number_gt 12229 _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 and H1C were located on the Fourier difference map; their isotropic displacement parameters were fixed to ride on the parent atoms. The following restraints were applied: B1-H1A = B1-H1B; H1A-H1C = H1B-H1C. 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^)+(0.0456P)^2^+7.5949P] 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 14685 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 542 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.198 _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 0.278521(14) 0.234527(12) 0.961634(8) 0.02865(8) Uani 1 1 d . . . P1 P 0.30985(5) 0.30550(4) 1.02886(3) 0.02860(16) Uani 1 1 d . . . P2 P 0.38242(5) 0.15535(4) 0.97861(3) 0.03196(17) Uani 1 1 d . . . B1 B 0.1703(2) 0.23780(19) 0.90166(14) 0.0369(7) Uani 1 1 d D . . H1A H 0.177(2) 0.2755(15) 0.9396(11) 0.044 Uiso 1 1 d D . . H1B H 0.2324(19) 0.1984(15) 0.9004(12) 0.044 Uiso 1 1 d D . . H1C H 0.165(2) 0.2671(14) 0.8656(13) 0.044 Uiso 1 1 d D . . N1 N 0.08334(18) 0.19155(16) 0.90756(12) 0.0487(7) Uani 1 1 d . . . C1 C 0.0860(3) 0.1471(3) 0.95592(18) 0.0730(13) Uani 1 1 d . . . H1D H 0.0936 0.1764 0.9876 0.109 Uiso 1 1 calc R . . H1E H 0.1363 0.1147 0.9539 0.109 Uiso 1 1 calc R . . H1F H 0.0299 0.1210 0.9581 0.109 Uiso 1 1 calc R . . C2 C 0.0028(3) 0.2377(3) 0.9097(2) 0.0788(14) Uani 1 1 d . . . H2A H 0.0022 0.2692 0.8791 0.118 Uiso 1 1 calc R . . H2B H 0.0052 0.2649 0.9426 0.118 Uiso 1 1 calc R . . H2C H -0.0516 0.2093 0.9087 0.118 Uiso 1 1 calc R . . C3 C 0.0752(3) 0.1469(2) 0.85944(18) 0.0761(13) Uani 1 1 d . . . H3A H 0.0197 0.1198 0.8609 0.114 Uiso 1 1 calc R . . H3B H 0.1265 0.1153 0.8582 0.114 Uiso 1 1 calc R . . H3C H 0.0739 0.1761 0.8275 0.114 Uiso 1 1 calc R . . C4 C 0.41023(19) 0.30232(17) 1.07235(12) 0.0362(7) Uani 1 1 d . . . H4A H 0.3983 0.3286 1.1053 0.043 Uiso 1 1 calc R . . H4B H 0.4217 0.2535 1.0826 0.043 Uiso 1 1 calc R . . C5 C 0.4946(2) 0.33182(19) 1.04714(13) 0.0432(8) Uani 1 1 d . . . H5A H 0.4846 0.3817 1.0396 0.052 Uiso 1 1 calc R . . H5B H 0.5447 0.3285 1.0734 0.052 Uiso 1 1 calc R . . C6 C 0.5224(2) 0.29617(19) 0.99600(13) 0.0460(8) Uani 1 1 d . . . H6A H 0.5733 0.3219 0.9810 0.055 Uiso 1 1 calc R . . H6B H 0.4720 0.2986 0.9699 0.055 Uiso 1 1 calc R . . C7 C 0.5496(2) 0.2199(2) 1.00335(14) 0.0484(9) Uani 1 1 d . . . H7A H 0.5374 0.2059 1.0404 0.058 Uiso 1 1 calc R . . H7B H 0.6149 0.2159 0.9983 0.058 Uiso 1 1 calc R . . C8 C 0.50139(19) 0.16922(19) 0.96521(13) 0.0438(8) Uani 1 1 d . . . H8A H 0.5325 0.1239 0.9671 0.053 Uiso 1 1 calc R . . H8B H 0.5067 0.1869 0.9285 0.053 Uiso 1 1 calc R . . C9 C 0.21669(18) 0.30573(15) 1.07474(11) 0.0304(6) Uani 1 1 d . . . C10 C 0.2216(2) 0.27451(16) 1.12446(12) 0.0369(7) Uani 1 1 d . . . H10 H 0.2761 0.2540 1.1367 0.044 Uiso 1 1 calc R . . C11 C 0.1467(2) 0.27326(18) 1.15633(13) 0.0457(8) Uani 1 1 d . . . H11 H 0.1501 0.2515 1.1902 0.055 Uiso 1 1 calc R . . C12 C 0.0679(2) 0.30322(18) 1.13919(14) 0.0472(8) Uani 1 1 d . . . H12 H 0.0171 0.3024 1.1613 0.057 Uiso 1 1 calc R . . C13 C 0.0622(2) 0.33445(18) 1.08998(14) 0.0454(8) Uani 1 1 d . . . H13 H 0.0078 0.3555 1.0783 0.054 Uiso 1 1 calc R . . C14 C 0.1359(2) 0.33512(17) 1.05752(12) 0.0380(7) Uani 1 1 d . . . H14 H 0.1314 0.3558 1.0233 0.046 Uiso 1 1 calc R . . C15 C 0.31117(19) 0.39468(15) 1.00397(11) 0.0342(6) Uani 1 1 d . . . C16 C 0.3054(3) 0.45039(18) 1.03881(14) 0.0512(9) Uani 1 1 d . . . H16 H 0.2990 0.4422 1.0758 0.061 Uiso 1 1 calc R . . C17 C 0.3088(3) 0.51800(19) 1.01975(17) 0.0648(11) Uani 1 1 d . . . H17 H 0.3055 0.5559 1.0438 0.078 Uiso 1 1 calc R . . C18 C 0.3171(3) 0.5302(2) 0.96608(17) 0.0618(10) Uani 1 1 d . . . H18 H 0.3192 0.5765 0.9531 0.074 Uiso 1 1 calc R . . C19 C 0.3222(3) 0.4757(2) 0.93150(15) 0.0533(9) Uani 1 1 d . . . H19 H 0.3277 0.4842 0.8945 0.064 Uiso 1 1 calc R . . C20 C 0.3194(2) 0.40780(17) 0.95008(12) 0.0417(7) Uani 1 1 d . . . H20 H 0.3231 0.3702 0.9258 0.050 Uiso 1 1 calc R . . C21 C 0.38096(19) 0.11327(16) 1.04352(12) 0.0348(6) Uani 1 1 d . . . C22 C 0.3052(2) 0.12017(16) 1.07428(12) 0.0351(6) Uani 1 1 d . . . H22 H 0.2571 0.1486 1.0620 0.042 Uiso 1 1 calc R . . C23 C 0.2990(2) 0.08609(18) 1.12268(13) 0.0448(8) Uani 1 1 d . . . H23 H 0.2470 0.0914 1.1434 0.054 Uiso 1 1 calc R . . C24 C 0.3681(3) 0.04457(19) 1.14068(14) 0.0518(9) Uani 1 1 d . . . H24 H 0.3638 0.0209 1.1737 0.062 Uiso 1 1 calc R . . C25 C 0.4438(3) 0.0373(2) 1.11060(15) 0.0581(10) Uani 1 1 d . . . H25 H 0.4916 0.0089 1.1233 0.070 Uiso 1 1 calc R . . C26 C 0.4509(2) 0.0708(2) 1.06240(14) 0.0499(8) Uani 1 1 d . . . H26 H 0.5032 0.0651 1.0420 0.060 Uiso 1 1 calc R . . C27 C 0.35509(19) 0.08427(16) 0.93246(12) 0.0369(7) Uani 1 1 d . . . C28 C 0.3188(2) 0.02232(18) 0.94958(14) 0.0494(8) Uani 1 1 d . . . H28 H 0.3125 0.0141 0.9866 0.059 Uiso 1 1 calc R . . C29 C 0.2914(3) -0.0280(2) 0.91296(17) 0.0645(11) Uani 1 1 d . . . H29 H 0.2665 -0.0704 0.9250 0.077 Uiso 1 1 calc R . . C30 C 0.3003(3) -0.0164(2) 0.85919(17) 0.0633(11) Uani 1 1 d . . . H30 H 0.2808 -0.0505 0.8342 0.076 Uiso 1 1 calc R . . C31 C 0.3374(2) 0.0445(2) 0.84173(14) 0.0521(9) Uani 1 1 d . . . H31 H 0.3443 0.0522 0.8047 0.063 Uiso 1 1 calc R . . C32 C 0.3647(2) 0.09493(19) 0.87800(13) 0.0434(7) Uani 1 1 d . . . H32 H 0.3902 0.1370 0.8657 0.052 Uiso 1 1 calc R . . B200 B 0.1513(2) 0.56074(16) 0.76256(12) 0.0271(6) Uani 1 1 d . . . C201 C 0.13712(17) 0.55229(14) 0.69799(11) 0.0278(6) Uani 1 1 d . . . C202 C 0.08093(18) 0.50283(15) 0.67460(11) 0.0292(6) Uani 1 1 d . . . H202 H 0.0456 0.4744 0.6968 0.035 Uiso 1 1 calc R . . C203 C 0.0749(2) 0.49363(15) 0.61951(11) 0.0351(6) Uani 1 1 d D A . C204 C 0.1264(2) 0.53343(16) 0.58596(12) 0.0383(7) Uani 1 1 d . . . H204 H 0.1224 0.5275 0.5485 0.046 Uiso 1 1 calc R . . C205 C 0.1837(2) 0.58201(16) 0.60843(12) 0.0367(7) Uani 1 1 d D B . C206 C 0.18903(18) 0.59129(15) 0.66289(12) 0.0327(6) Uani 1 1 d . . . H206 H 0.2291 0.6252 0.6771 0.039 Uiso 1 1 calc R . . C207 C 0.0126(2) 0.44014(18) 0.59686(12) 0.0476(8) Uani 1 1 d D . . F1 F -0.0104(3) 0.45132(19) 0.54645(10) 0.0850(12) Uani 0.887(5) 1 d PDU A 1 F2 F -0.06495(19) 0.43764(19) 0.62142(12) 0.0820(11) Uani 0.887(5) 1 d PDU A 1 F3 F 0.0455(3) 0.37713(14) 0.5992(2) 0.1094(16) Uani 0.887(5) 1 d PDU A 1 F101 F -0.0058(15) 0.3901(8) 0.6300(5) 0.071(6) Uani 0.113(5) 1 d PDU A 2 F102 F 0.0444(12) 0.4102(10) 0.5541(6) 0.076(6) Uani 0.113(5) 1 d PDU A 2 F103 F -0.0651(8) 0.4669(8) 0.5818(10) 0.097(7) Uani 0.113(5) 1 d PDU A 2 C208 C 0.2406(2) 0.62560(18) 0.57312(13) 0.0517(9) Uani 1 1 d D . . F4 F 0.2623(5) 0.5995(3) 0.52910(18) 0.094(2) Uani 0.630(7) 1 d PDU B 1 F5 F 0.2107(3) 0.6884(2) 0.5662(3) 0.084(2) Uani 0.630(7) 1 d PDU B 1 F6 F 0.3228(2) 0.6401(3) 0.59757(17) 0.0836(18) Uani 0.630(7) 1 d PDU B 1 F104 F 0.2546(8) 0.6862(3) 0.5882(3) 0.090(3) Uani 0.370(7) 1 d PDU B 2 F105 F 0.3119(4) 0.5935(4) 0.5598(4) 0.084(3) Uani 0.370(7) 1 d PDU B 2 F106 F 0.1952(5) 0.6327(5) 0.5248(2) 0.090(3) Uani 0.370(7) 1 d PDU B 2 C209 C 0.24479(18) 0.51830(14) 0.77567(10) 0.0284(6) Uani 1 1 d . . . C210 C 0.24602(19) 0.44528(15) 0.77390(11) 0.0312(6) Uani 1 1 d . . . H210 H 0.1913 0.4210 0.7680 0.037 Uiso 1 1 calc R . . C211 C 0.3246(2) 0.40767(16) 0.78052(11) 0.0367(7) Uani 1 1 d . . . C212 C 0.4056(2) 0.44110(18) 0.78922(13) 0.0424(8) Uani 1 1 d . . . H212 H 0.4594 0.4154 0.7942 0.051 Uiso 1 1 calc R . . C213 C 0.40636(19) 0.51278(17) 0.79054(12) 0.0398(7) Uani 1 1 d D C . C214 C 0.32738(18) 0.55055(16) 0.78379(11) 0.0330(6) Uani 1 1 d . . . H214 H 0.3300 0.5998 0.7848 0.040 Uiso 1 1 calc R . . C215 C 0.3245(2) 0.33000(18) 0.77720(14) 0.0490(8) Uani 1 1 d . . . F7 F 0.24302(16) 0.30269(11) 0.77037(10) 0.0689(6) Uani 1 1 d U . . F8 F 0.3587(2) 0.29988(13) 0.82032(11) 0.0862(8) Uani 1 1 d U . . F9 F 0.3707(2) 0.30684(12) 0.73602(12) 0.0911(9) Uani 1 1 d U . . C216 C 0.4928(2) 0.5501(2) 0.79993(15) 0.0627(11) Uani 1 1 d D . . F10 F 0.5634(2) 0.5121(2) 0.7982(3) 0.0876(18) Uani 0.678(7) 1 d PDU C 1 F11 F 0.5084(3) 0.5947(3) 0.7576(2) 0.0987(18) Uani 0.678(7) 1 d PDU C 1 F12 F 0.4928(3) 0.5903(4) 0.8402(2) 0.110(3) Uani 0.678(7) 1 d PDU C 1 F110 F 0.4868(6) 0.6151(3) 0.8133(5) 0.076(3) Uani 0.322(7) 1 d PDU C 2 F111 F 0.5353(6) 0.5232(6) 0.8453(4) 0.110(4) Uani 0.322(7) 1 d PDU C 2 F112 F 0.5506(6) 0.5433(7) 0.7646(4) 0.113(4) Uani 0.322(7) 1 d PDU C 2 C217 C 0.06698(18) 0.52955(14) 0.79570(10) 0.0272(5) Uani 1 1 d . . . C218 C -0.02187(18) 0.54450(14) 0.78050(11) 0.0292(6) Uani 1 1 d . . . H218 H -0.0330 0.5686 0.7481 0.035 Uiso 1 1 calc R . . C219 C -0.09390(18) 0.52547(15) 0.81095(11) 0.0321(6) Uani 1 1 d . . . C220 C -0.0804(2) 0.49073(16) 0.85890(12) 0.0359(7) Uani 1 1 d . . . H220 H -0.1296 0.4775 0.8800 0.043 Uiso 1 1 calc R . . C221 C 0.0065(2) 0.47604(15) 0.87493(11) 0.0332(6) Uani 1 1 d . . . C222 C 0.07834(19) 0.49469(14) 0.84407(11) 0.0301(6) Uani 1 1 d . . . H222 H 0.1372 0.4834 0.8562 0.036 Uiso 1 1 calc R . . C223 C -0.1872(2) 0.54039(19) 0.79164(13) 0.0423(7) Uani 1 1 d . . . F13 F -0.22565(14) 0.48604(13) 0.76781(10) 0.0720(7) Uani 1 1 d U . . F14 F -0.24113(13) 0.55949(15) 0.83041(9) 0.0719(7) Uani 1 1 d U . . F15 F -0.19212(13) 0.59221(13) 0.75612(9) 0.0660(6) Uani 1 1 d U . . C224 C 0.0269(3) 0.44113(19) 0.92708(14) 0.0496(8) Uani 1 1 d . . . F16 F -0.04540(16) 0.41558(14) 0.95016(9) 0.0716(7) Uani 1 1 d U . . F17 F 0.08474(18) 0.38870(13) 0.92190(9) 0.0761(7) Uani 1 1 d U . . F18 F 0.06662(17) 0.48387(14) 0.96211(8) 0.0714(7) Uani 1 1 d U . . C225 C 0.15549(17) 0.64195(14) 0.78244(11) 0.0287(6) Uani 1 1 d . . . C226 C 0.12137(18) 0.69766(14) 0.75319(11) 0.0312(6) Uani 1 1 d . . . H226 H 0.1012 0.6899 0.7176 0.037 Uiso 1 1 calc R . . C227 C 0.1157(2) 0.76454(15) 0.77420(13) 0.0359(6) Uani 1 1 d . . . C228 C 0.1448(2) 0.77827(15) 0.82559(13) 0.0391(7) Uani 1 1 d . . . H228 H 0.1417 0.8239 0.8398 0.047 Uiso 1 1 calc R . . C229 C 0.17871(19) 0.72381(15) 0.85604(13) 0.0378(7) Uani 1 1 d D D . C230 C 0.18378(19) 0.65731(15) 0.83490(12) 0.0331(6) Uani 1 1 d . . . H230 H 0.2072 0.6209 0.8566 0.040 Uiso 1 1 calc R . . C231 C 0.0736(2) 0.82040(17) 0.74117(15) 0.0489(8) Uani 1 1 d . . . F19 F -0.01392(16) 0.80943(14) 0.73254(13) 0.0908(9) Uani 1 1 d U . . F20 F 0.10719(18) 0.82493(12) 0.69285(9) 0.0718(7) Uani 1 1 d U . . F21 F 0.0816(2) 0.88324(11) 0.76242(10) 0.0803(8) Uani 1 1 d U . . C232 C 0.2066(2) 0.73676(17) 0.91282(15) 0.0511(9) Uani 1 1 d D . . F22 F 0.2178(5) 0.80133(15) 0.92453(16) 0.1020(18) Uani 0.786(6) 1 d PDU D 1 F23 F 0.2847(2) 0.7062(2) 0.92505(14) 0.0735(12) Uani 0.786(6) 1 d PDU D 1 F24 F 0.1522(3) 0.7079(3) 0.94680(12) 0.110(2) Uani 0.786(6) 1 d PDU D 1 F122 F 0.2272(13) 0.6836(5) 0.9401(4) 0.090(4) Uani 0.214(6) 1 d PDU D 2 F123 F 0.1436(7) 0.7706(8) 0.9384(4) 0.075(4) Uani 0.214(6) 1 d PDU D 2 F124 F 0.2758(9) 0.7798(9) 0.9151(5) 0.112(5) Uani 0.214(6) 1 d PDU D 2 C901 C 0.6755(7) 0.3444(5) 0.8628(3) 0.165(4) Uani 1 1 d . . . H90A H 0.7295 0.3706 0.8540 0.248 Uiso 1 1 calc R . . H90B H 0.6848 0.3207 0.8969 0.248 Uiso 1 1 calc R . . H90C H 0.6247 0.3763 0.8652 0.248 Uiso 1 1 calc R . . C902 C 0.6571(5) 0.2936(4) 0.8216(2) 0.110(2) Uani 1 1 d . . . H90D H 0.6054 0.2652 0.8325 0.132 Uiso 1 1 calc R . . H90E H 0.7094 0.2622 0.8195 0.132 Uiso 1 1 calc R . . C903 C 0.6369(4) 0.3227(3) 0.7663(2) 0.0992(18) Uani 1 1 d . . . H90F H 0.5885 0.3576 0.7687 0.119 Uiso 1 1 calc R . . H90G H 0.6909 0.3467 0.7534 0.119 Uiso 1 1 calc R . . C904 C 0.6095(4) 0.2687(3) 0.7270(2) 0.0953(17) Uani 1 1 d . . . H90H H 0.5590 0.2418 0.7413 0.114 Uiso 1 1 calc R . . H90I H 0.6601 0.2362 0.7220 0.114 Uiso 1 1 calc R . . C905 C 0.5819(4) 0.2986(4) 0.6738(3) 0.111(2) Uani 1 1 d . . . H90J H 0.5318 0.3307 0.6783 0.166 Uiso 1 1 calc R . . H90K H 0.5634 0.2610 0.6497 0.166 Uiso 1 1 calc R . . H90L H 0.6325 0.3235 0.6586 0.166 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02571(12) 0.03223(13) 0.02785(12) -0.00245(9) -0.00308(8) -0.00179(9) P1 0.0272(3) 0.0317(4) 0.0269(3) -0.0013(3) 0.0001(3) -0.0030(3) P2 0.0249(3) 0.0391(4) 0.0319(4) -0.0064(3) -0.0006(3) 0.0012(3) B1 0.0336(17) 0.0404(19) 0.0362(18) -0.0014(15) -0.0088(14) -0.0026(15) N1 0.0415(15) 0.0521(18) 0.0518(17) 0.0029(14) -0.0143(13) -0.0137(13) C1 0.068(3) 0.080(3) 0.071(3) 0.027(2) -0.016(2) -0.038(2) C2 0.0342(19) 0.090(3) 0.111(4) 0.008(3) -0.009(2) -0.004(2) C3 0.085(3) 0.073(3) 0.070(3) -0.015(2) -0.022(2) -0.031(2) C4 0.0299(14) 0.0444(18) 0.0342(15) -0.0059(13) -0.0029(12) -0.0031(13) C5 0.0301(15) 0.0506(19) 0.0489(19) -0.0105(15) -0.0027(13) -0.0088(14) C6 0.0310(16) 0.060(2) 0.0473(19) -0.0083(16) 0.0067(13) -0.0123(15) C7 0.0246(14) 0.069(2) 0.051(2) -0.0176(17) 0.0001(13) -0.0010(15) C8 0.0269(14) 0.059(2) 0.0455(18) -0.0137(16) 0.0045(13) 0.0002(14) C9 0.0304(14) 0.0298(14) 0.0311(14) -0.0019(11) 0.0026(11) -0.0025(12) C10 0.0404(16) 0.0373(17) 0.0332(15) -0.0007(12) 0.0024(12) -0.0003(13) C11 0.057(2) 0.0451(19) 0.0353(16) 0.0046(14) 0.0132(15) -0.0038(16) C12 0.0416(18) 0.0461(19) 0.055(2) -0.0092(16) 0.0202(15) -0.0073(15) C13 0.0344(16) 0.0464(19) 0.056(2) -0.0040(16) 0.0056(14) 0.0032(14) C14 0.0336(15) 0.0425(17) 0.0380(16) 0.0047(13) 0.0006(12) 0.0005(13) C15 0.0344(15) 0.0341(16) 0.0341(15) 0.0002(12) 0.0010(12) -0.0058(12) C16 0.074(2) 0.0389(18) 0.0411(18) -0.0028(14) 0.0077(17) -0.0091(17) C17 0.094(3) 0.0350(19) 0.065(3) -0.0064(18) 0.007(2) -0.011(2) C18 0.076(3) 0.040(2) 0.069(3) 0.0155(19) 0.001(2) -0.0122(19) C19 0.065(2) 0.051(2) 0.0443(19) 0.0137(16) 0.0003(16) -0.0115(18) C20 0.0477(18) 0.0416(18) 0.0358(16) 0.0023(14) 0.0001(13) -0.0090(15) C21 0.0332(15) 0.0366(16) 0.0343(15) -0.0060(12) -0.0070(12) 0.0026(13) C22 0.0347(15) 0.0334(15) 0.0370(16) -0.0009(12) -0.0048(12) 0.0010(12) C23 0.0503(19) 0.0439(19) 0.0400(17) 0.0008(14) -0.0011(14) -0.0059(15) C24 0.071(2) 0.046(2) 0.0375(18) 0.0050(15) -0.0158(17) -0.0004(18) C25 0.061(2) 0.056(2) 0.056(2) 0.0037(18) -0.0223(19) 0.0183(19) C26 0.0426(18) 0.058(2) 0.049(2) -0.0032(16) -0.0086(15) 0.0166(16) C27 0.0309(14) 0.0393(17) 0.0404(16) -0.0088(13) -0.0050(12) 0.0061(13) C28 0.058(2) 0.0446(19) 0.0452(19) -0.0056(15) -0.0056(16) -0.0001(17) C29 0.080(3) 0.045(2) 0.068(3) -0.0091(19) -0.015(2) -0.010(2) C30 0.071(3) 0.057(2) 0.061(2) -0.025(2) -0.021(2) 0.006(2) C31 0.0486(19) 0.067(2) 0.0399(18) -0.0168(17) -0.0081(15) 0.0105(18) C32 0.0384(16) 0.053(2) 0.0388(17) -0.0095(15) -0.0025(13) 0.0050(15) B200 0.0253(14) 0.0262(15) 0.0297(15) 0.0014(12) -0.0024(12) 0.0003(12) C201 0.0253(13) 0.0272(14) 0.0308(14) 0.0025(11) 0.0001(10) 0.0037(11) C202 0.0289(13) 0.0305(14) 0.0283(14) 0.0035(11) 0.0021(11) 0.0010(11) C203 0.0389(16) 0.0350(16) 0.0312(15) -0.0012(12) -0.0015(12) 0.0035(13) C204 0.0461(17) 0.0425(18) 0.0264(14) 0.0032(13) 0.0043(12) 0.0093(14) C205 0.0373(16) 0.0357(16) 0.0375(16) 0.0069(13) 0.0095(12) 0.0066(13) C206 0.0283(14) 0.0308(15) 0.0392(16) 0.0039(12) 0.0034(11) 0.0004(12) C207 0.057(2) 0.052(2) 0.0336(17) -0.0057(15) -0.0037(15) -0.0075(17) F1 0.116(3) 0.102(2) 0.0366(14) 0.0005(14) -0.0245(15) -0.045(2) F2 0.0675(18) 0.115(3) 0.0639(18) -0.0318(17) 0.0081(14) -0.0479(18) F3 0.113(3) 0.0431(16) 0.170(4) -0.027(2) -0.063(3) 0.0033(17) F101 0.087(10) 0.063(9) 0.062(9) -0.011(7) -0.012(8) -0.039(8) F102 0.089(9) 0.067(9) 0.071(9) -0.025(8) 0.002(8) -0.015(8) F103 0.086(10) 0.104(10) 0.098(10) -0.017(9) -0.014(9) -0.015(8) C208 0.054(2) 0.051(2) 0.051(2) 0.0127(17) 0.0196(17) 0.0034(18) F4 0.147(5) 0.083(3) 0.056(3) -0.017(2) 0.063(3) -0.041(4) F5 0.067(3) 0.056(3) 0.130(5) 0.039(3) 0.040(3) 0.003(2) F6 0.054(2) 0.129(4) 0.069(3) 0.028(3) 0.0142(19) -0.033(3) F104 0.139(8) 0.059(5) 0.072(5) -0.010(4) 0.042(5) -0.051(5) F105 0.056(4) 0.088(5) 0.110(7) 0.041(5) 0.048(4) 0.011(4) F106 0.082(5) 0.133(7) 0.057(4) 0.053(4) 0.008(3) -0.031(5) C209 0.0295(13) 0.0316(14) 0.0242(13) -0.0010(11) -0.0008(10) 0.0011(11) C210 0.0301(14) 0.0337(15) 0.0296(14) 0.0001(11) -0.0001(11) 0.0024(12) C211 0.0402(16) 0.0388(17) 0.0310(15) -0.0009(12) 0.0024(12) 0.0092(13) C212 0.0324(16) 0.054(2) 0.0411(17) -0.0042(15) -0.0018(13) 0.0157(14) C213 0.0284(14) 0.052(2) 0.0387(16) -0.0107(14) -0.0004(12) 0.0018(14) C214 0.0299(14) 0.0357(16) 0.0334(15) -0.0040(12) 0.0014(11) -0.0012(12) C215 0.055(2) 0.0405(18) 0.052(2) 0.0012(15) 0.0064(16) 0.0144(16) F7 0.0748(15) 0.0357(11) 0.0960(18) -0.0033(11) -0.0042(13) 0.0032(11) F8 0.114(2) 0.0538(14) 0.0899(18) 0.0218(13) -0.0302(16) 0.0162(14) F9 0.125(2) 0.0460(13) 0.105(2) -0.0092(13) 0.0596(17) 0.0192(14) C216 0.0306(18) 0.075(3) 0.082(3) -0.025(2) -0.0007(18) 0.0000(18) F10 0.0259(16) 0.088(3) 0.149(5) -0.009(3) -0.010(2) 0.0068(17) F11 0.048(2) 0.103(4) 0.145(4) 0.016(3) 0.003(2) -0.031(2) F12 0.061(3) 0.164(6) 0.107(4) -0.088(4) 0.007(3) -0.035(4) F110 0.037(4) 0.064(5) 0.126(8) -0.011(5) -0.028(5) -0.006(3) F111 0.067(5) 0.142(7) 0.118(7) 0.033(6) -0.060(5) -0.030(5) F112 0.075(6) 0.148(8) 0.118(7) -0.044(6) 0.049(6) -0.028(6) C217 0.0293(13) 0.0235(13) 0.0288(13) -0.0032(11) -0.0010(10) 0.0002(11) C218 0.0328(14) 0.0282(14) 0.0264(13) -0.0012(11) -0.0029(11) -0.0002(12) C219 0.0289(14) 0.0343(15) 0.0332(15) -0.0085(12) 0.0017(11) -0.0010(12) C220 0.0368(15) 0.0354(16) 0.0360(16) -0.0049(12) 0.0107(12) -0.0042(13) C221 0.0397(16) 0.0307(15) 0.0291(14) -0.0008(12) 0.0039(12) 0.0020(12) C222 0.0331(14) 0.0273(14) 0.0298(14) -0.0028(11) -0.0005(11) 0.0021(12) C223 0.0318(15) 0.054(2) 0.0411(17) -0.0055(15) 0.0021(13) -0.0021(14) F13 0.0480(12) 0.0712(15) 0.0958(18) -0.0224(13) -0.0255(12) -0.0047(11) F14 0.0374(11) 0.122(2) 0.0568(13) -0.0115(13) 0.0069(9) 0.0195(12) F15 0.0369(10) 0.0858(16) 0.0749(15) 0.0226(13) -0.0085(10) 0.0074(11) C224 0.059(2) 0.051(2) 0.0393(18) 0.0076(15) 0.0124(16) 0.0062(17) F16 0.0710(15) 0.0881(17) 0.0564(13) 0.0325(12) 0.0171(11) -0.0047(13) F17 0.0965(18) 0.0719(16) 0.0606(14) 0.0310(12) 0.0165(12) 0.0386(14) F18 0.0793(16) 0.0993(19) 0.0352(11) 0.0034(11) -0.0057(10) -0.0044(14) C225 0.0224(12) 0.0282(14) 0.0354(15) 0.0003(11) 0.0008(11) -0.0017(11) C226 0.0291(14) 0.0295(15) 0.0349(15) 0.0034(12) -0.0004(11) -0.0022(12) C227 0.0331(15) 0.0274(14) 0.0470(17) 0.0054(13) 0.0001(13) 0.0003(12) C228 0.0360(16) 0.0266(15) 0.0547(19) -0.0066(13) -0.0029(14) 0.0003(12) C229 0.0335(15) 0.0341(16) 0.0453(17) -0.0068(13) -0.0084(13) 0.0004(13) C230 0.0305(14) 0.0301(15) 0.0384(15) 0.0001(12) -0.0061(12) 0.0009(12) C231 0.057(2) 0.0334(17) 0.056(2) 0.0075(15) 0.0011(17) 0.0040(15) F19 0.0567(14) 0.0792(18) 0.136(2) 0.0527(17) -0.0190(15) 0.0123(13) F20 0.1054(19) 0.0546(13) 0.0554(13) 0.0180(11) 0.0036(12) 0.0177(13) F21 0.137(2) 0.0305(11) 0.0724(15) 0.0045(10) -0.0123(15) 0.0165(13) C232 0.056(2) 0.0421(19) 0.054(2) -0.0119(17) -0.0176(17) 0.0041(17) F22 0.184(5) 0.0414(18) 0.078(2) -0.0281(16) -0.059(3) 0.023(2) F23 0.066(2) 0.086(3) 0.067(2) -0.0203(18) -0.0365(17) 0.0204(19) F24 0.089(3) 0.199(5) 0.0407(17) -0.009(2) -0.0051(17) -0.059(3) F122 0.126(9) 0.077(7) 0.066(6) -0.015(6) -0.022(7) 0.010(7) F123 0.086(7) 0.094(8) 0.043(5) -0.026(6) -0.017(5) 0.021(6) F124 0.109(8) 0.121(9) 0.104(8) -0.033(7) -0.045(7) -0.033(7) C901 0.223(10) 0.182(8) 0.090(5) -0.041(5) -0.001(5) 0.061(7) C902 0.131(5) 0.114(5) 0.086(4) -0.003(4) 0.005(4) 0.023(4) C903 0.084(4) 0.106(4) 0.108(4) -0.012(4) 0.012(3) 0.032(3) C904 0.081(3) 0.098(4) 0.107(4) -0.027(3) 0.000(3) 0.010(3) C905 0.101(4) 0.134(6) 0.097(4) -0.004(4) -0.006(3) 0.003(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 B1 2.189(3) . ? Rh1 P2 2.2116(8) . ? Rh1 P1 2.2166(7) . ? P1 C9 1.827(3) . ? P1 C15 1.829(3) . ? P1 C4 1.839(3) . ? P2 C21 1.823(3) . ? P2 C27 1.836(3) . ? P2 C8 1.836(3) . ? B1 N1 1.585(4) . ? N1 C1 1.487(5) . ? N1 C3 1.488(5) . ? N1 C2 1.498(5) . ? C4 C5 1.532(4) . ? C5 C6 1.523(5) . ? C6 C7 1.535(5) . ? C7 C8 1.538(4) . ? C9 C10 1.388(4) . ? C9 C14 1.394(4) . ? C10 C11 1.390(4) . ? C11 C12 1.373(5) . ? C12 C13 1.377(5) . ? C13 C14 1.385(4) . ? C15 C20 1.387(4) . ? C15 C16 1.389(4) . ? C16 C17 1.389(5) . ? C17 C18 1.378(6) . ? C18 C19 1.367(6) . ? C19 C20 1.390(5) . ? C21 C22 1.390(4) . ? C21 C26 1.402(4) . ? C22 C23 1.388(4) . ? C23 C24 1.375(5) . ? C24 C25 1.381(6) . ? C25 C26 1.379(5) . ? C27 C28 1.383(5) . ? C27 C32 1.395(4) . ? C28 C29 1.393(5) . ? C29 C30 1.380(6) . ? C30 C31 1.374(6) . ? C31 C32 1.388(5) . ? B200 C217 1.640(4) . ? B200 C201 1.641(4) . ? B200 C225 1.643(4) . ? B200 C209 1.646(4) . ? C201 C202 1.392(4) . ? C201 C206 1.405(4) . ? C202 C203 1.398(4) . ? C203 C204 1.385(4) . ? C203 C207 1.494(5) . ? C204 C205 1.381(4) . ? C205 C206 1.382(4) . ? C205 C208 1.500(4) . ? C207 F101 1.306(7) . ? C207 F3 1.311(4) . ? C207 F103 1.318(7) . ? C207 F102 1.318(7) . ? C207 F1 1.324(4) . ? C207 F2 1.325(4) . ? C208 F104 1.245(6) . ? C208 F4 1.265(4) . ? C208 F105 1.282(5) . ? C208 F5 1.300(5) . ? C208 F106 1.386(6) . ? C208 F6 1.390(5) . ? C209 C214 1.393(4) . ? C209 C210 1.408(4) . ? C210 C211 1.387(4) . ? C211 C212 1.384(5) . ? C211 C215 1.499(5) . ? C212 C213 1.381(5) . ? C213 C214 1.394(4) . ? C213 C216 1.493(5) . ? C215 F8 1.323(4) . ? C215 F9 1.334(4) . ? C215 F7 1.334(4) . ? C216 F112 1.259(6) . ? C216 F12 1.275(5) . ? C216 F10 1.286(4) . ? C216 F110 1.300(6) . ? C216 F11 1.392(5) . ? C216 F111 1.395(6) . ? C217 C222 1.397(4) . ? C217 C218 1.404(4) . ? C218 C219 1.383(4) . ? C219 C220 1.390(4) . ? C219 C223 1.495(4) . ? C220 C221 1.381(4) . ? C221 C222 1.385(4) . ? C221 C224 1.499(4) . ? C223 F14 1.330(4) . ? C223 F13 1.331(4) . ? C223 F15 1.341(4) . ? C224 F16 1.331(4) . ? C224 F18 1.336(4) . ? C224 F17 1.338(4) . ? C225 C226 1.392(4) . ? C225 C230 1.408(4) . ? C226 C227 1.396(4) . ? C227 C228 1.380(4) . ? C227 C231 1.491(4) . ? C228 C229 1.388(4) . ? C229 C230 1.390(4) . ? C229 C232 1.500(5) . ? C231 F20 1.327(4) . ? C231 F21 1.328(4) . ? C231 F19 1.338(4) . ? C232 F122 1.267(6) . ? C232 F22 1.289(4) . ? C232 F24 1.316(5) . ? C232 F123 1.324(6) . ? C232 F124 1.325(7) . ? C232 F23 1.336(4) . ? C901 C902 1.446(9) . ? C902 C903 1.525(8) . ? C903 C904 1.488(8) . ? C904 C905 1.507(8) . ? 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 B1 Rh1 P2 131.17(10) . . ? B1 Rh1 P1 130.45(10) . . ? P2 Rh1 P1 98.18(3) . . ? C9 P1 C15 103.16(13) . . ? C9 P1 C4 104.32(13) . . ? C15 P1 C4 102.72(14) . . ? C9 P1 Rh1 109.38(9) . . ? C15 P1 Rh1 108.80(10) . . ? C4 P1 Rh1 126.13(11) . . ? C21 P2 C27 103.15(14) . . ? C21 P2 C8 105.02(15) . . ? C27 P2 C8 101.30(14) . . ? C21 P2 Rh1 117.25(10) . . ? C27 P2 Rh1 104.29(10) . . ? C8 P2 Rh1 122.86(13) . . ? N1 B1 Rh1 121.0(2) . . ? C1 N1 C3 109.4(3) . . ? C1 N1 C2 108.7(4) . . ? C3 N1 C2 108.7(3) . . ? C1 N1 B1 113.1(3) . . ? C3 N1 B1 107.6(3) . . ? C2 N1 B1 109.3(3) . . ? C5 C4 P1 114.2(2) . . ? C6 C5 C4 115.0(3) . . ? C5 C6 C7 114.0(3) . . ? C6 C7 C8 114.4(3) . . ? C7 C8 P2 114.9(2) . . ? C10 C9 C14 119.0(3) . . ? C10 C9 P1 122.8(2) . . ? C14 C9 P1 118.1(2) . . ? C9 C10 C11 119.9(3) . . ? C12 C11 C10 120.5(3) . . ? C11 C12 C13 120.1(3) . . ? C12 C13 C14 120.0(3) . . ? C13 C14 C9 120.5(3) . . ? C20 C15 C16 118.9(3) . . ? C20 C15 P1 120.5(2) . . ? C16 C15 P1 120.6(2) . . ? C15 C16 C17 120.2(3) . . ? C18 C17 C16 120.2(4) . . ? C19 C18 C17 120.0(3) . . ? C18 C19 C20 120.4(3) . . ? C15 C20 C19 120.3(3) . . ? C22 C21 C26 118.5(3) . . ? C22 C21 P2 118.7(2) . . ? C26 C21 P2 122.6(2) . . ? C23 C22 C21 120.9(3) . . ? C24 C23 C22 120.0(3) . . ? C23 C24 C25 119.8(3) . . ? C26 C25 C24 120.9(3) . . ? C25 C26 C21 119.9(3) . . ? C28 C27 C32 118.8(3) . . ? C28 C27 P2 122.0(2) . . ? C32 C27 P2 119.0(3) . . ? C27 C28 C29 120.5(3) . . ? C30 C29 C28 120.1(4) . . ? C31 C30 C29 120.0(3) . . ? C30 C31 C32 120.2(3) . . ? C31 C32 C27 120.5(3) . . ? C217 B200 C201 112.4(2) . . ? C217 B200 C225 102.6(2) . . ? C201 B200 C225 113.5(2) . . ? C217 B200 C209 112.0(2) . . ? C201 B200 C209 103.9(2) . . ? C225 B200 C209 112.7(2) . . ? C202 C201 C206 115.9(3) . . ? C202 C201 B200 123.4(2) . . ? C206 C201 B200 120.5(2) . . ? C201 C202 C203 122.1(3) . . ? C204 C203 C202 120.6(3) . . ? C204 C203 C207 120.0(3) . . ? C202 C203 C207 119.5(3) . . ? C205 C204 C203 118.3(3) . . ? C204 C205 C206 121.0(3) . . ? C204 C205 C208 119.5(3) . . ? C206 C205 C208 119.5(3) . . ? C205 C206 C201 122.2(3) . . ? F101 C207 F3 51.0(10) . . ? F101 C207 F103 106.1(7) . . ? F3 C207 F103 134.6(7) . . ? F101 C207 F102 106.3(7) . . ? F3 C207 F102 59.3(10) . . ? F103 C207 F102 105.5(7) . . ? F101 C207 F1 132.6(7) . . ? F3 C207 F1 106.5(3) . . ? F103 C207 F1 56.8(11) . . ? F102 C207 F1 51.8(11) . . ? F101 C207 F2 58.6(11) . . ? F3 C207 F2 106.0(3) . . ? F103 C207 F2 51.4(11) . . ? F102 C207 F2 134.3(7) . . ? F1 C207 F2 103.9(3) . . ? F101 C207 C203 113.8(6) . . ? F3 C207 C203 113.0(3) . . ? F103 C207 C203 112.2(6) . . ? F102 C207 C203 112.4(6) . . ? F1 C207 C203 113.6(3) . . ? F2 C207 C203 113.0(3) . . ? F104 C208 F4 126.6(5) . . ? F104 C208 F105 113.4(5) . . ? F4 C208 F105 49.4(4) . . ? F104 C208 F5 39.0(5) . . ? F4 C208 F5 110.3(4) . . ? F105 C208 F5 134.3(5) . . ? F104 C208 F106 104.5(5) . . ? F4 C208 F106 53.3(4) . . ? F105 C208 F106 102.2(5) . . ? F5 C208 F106 68.3(5) . . ? F104 C208 F6 62.3(5) . . ? F4 C208 F6 103.1(4) . . ? F105 C208 F6 58.8(5) . . ? F5 C208 F6 99.8(4) . . ? F106 C208 F6 141.2(4) . . ? F104 C208 C205 116.0(4) . . ? F4 C208 C205 117.0(3) . . ? F105 C208 C205 111.7(4) . . ? F5 C208 C205 113.8(3) . . ? F106 C208 C205 107.6(3) . . ? F6 C208 C205 111.0(3) . . ? C214 C209 C210 116.0(3) . . ? C214 C209 B200 123.6(3) . . ? C210 C209 B200 120.1(2) . . ? C211 C210 C209 122.0(3) . . ? C212 C211 C210 120.7(3) . . ? C212 C211 C215 118.2(3) . . ? C210 C211 C215 121.0(3) . . ? C213 C212 C211 118.4(3) . . ? C212 C213 C214 120.8(3) . . ? C212 C213 C216 119.5(3) . . ? C214 C213 C216 119.7(3) . . ? C209 C214 C213 122.0(3) . . ? F8 C215 F9 107.0(3) . . ? F8 C215 F7 105.5(3) . . ? F9 C215 F7 104.7(3) . . ? F8 C215 C211 113.1(3) . . ? F9 C215 C211 112.2(3) . . ? F7 C215 C211 113.6(3) . . ? F112 C216 F12 129.5(6) . . ? F112 C216 F10 48.8(6) . . ? F12 C216 F10 112.7(4) . . ? F112 C216 F110 109.5(6) . . ? F12 C216 F110 37.7(4) . . ? F10 C216 F110 128.2(5) . . ? F112 C216 F11 52.8(7) . . ? F12 C216 F11 103.6(4) . . ? F10 C216 F11 100.1(4) . . ? F110 C216 F11 67.4(5) . . ? F112 C216 F111 103.4(6) . . ? F12 C216 F111 65.4(5) . . ? F10 C216 F111 57.1(5) . . ? F110 C216 F111 100.4(5) . . ? F11 C216 F111 140.8(5) . . ? F112 C216 C213 116.3(5) . . ? F12 C216 C213 113.8(3) . . ? F10 C216 C213 115.4(3) . . ? F110 C216 C213 116.1(4) . . ? F11 C216 C213 109.6(3) . . ? F111 C216 C213 109.2(4) . . ? C222 C217 C218 115.6(2) . . ? C222 C217 B200 122.6(2) . . ? C218 C217 B200 121.3(2) . . ? C219 C218 C217 122.5(3) . . ? C218 C219 C220 120.5(3) . . ? C218 C219 C223 120.0(3) . . ? C220 C219 C223 119.4(3) . . ? C221 C220 C219 118.0(3) . . ? C220 C221 C222 121.2(3) . . ? C220 C221 C224 121.3(3) . . ? C222 C221 C224 117.4(3) . . ? C221 C222 C217 122.1(3) . . ? F14 C223 F13 106.6(3) . . ? F14 C223 F15 104.9(3) . . ? F13 C223 F15 105.6(3) . . ? F14 C223 C219 113.0(3) . . ? F13 C223 C219 112.7(3) . . ? F15 C223 C219 113.4(3) . . ? F16 C224 F18 107.1(3) . . ? F16 C224 F17 107.2(3) . . ? F18 C224 F17 104.5(3) . . ? F16 C224 C221 113.3(3) . . ? F18 C224 C221 112.3(3) . . ? F17 C224 C221 111.9(3) . . ? C226 C225 C230 115.6(3) . . ? C226 C225 B200 124.2(2) . . ? C230 C225 B200 119.6(2) . . ? C225 C226 C227 122.4(3) . . ? C228 C227 C226 120.7(3) . . ? C228 C227 C231 120.3(3) . . ? C226 C227 C231 118.9(3) . . ? C227 C228 C229 118.4(3) . . ? C228 C229 C230 120.5(3) . . ? C228 C229 C232 119.4(3) . . ? C230 C229 C232 120.1(3) . . ? C229 C230 C225 122.3(3) . . ? F20 C231 F21 106.0(3) . . ? F20 C231 F19 104.4(3) . . ? F21 C231 F19 106.8(3) . . ? F20 C231 C227 113.2(3) . . ? F21 C231 C227 113.6(3) . . ? F19 C231 C227 112.1(3) . . ? F122 C232 F22 128.9(6) . . ? F122 C232 F24 56.8(7) . . ? F22 C232 F24 109.8(4) . . ? F122 C232 F123 107.6(6) . . ? F22 C232 F123 60.2(6) . . ? F24 C232 F123 55.7(7) . . ? F122 C232 F124 107.6(6) . . ? F22 C232 F124 44.7(7) . . ? F24 C232 F124 136.8(6) . . ? F123 C232 F124 103.5(6) . . ? F122 C232 F23 47.0(8) . . ? F22 C232 F23 105.4(3) . . ? F24 C232 F23 102.3(4) . . ? F123 C232 F23 137.0(5) . . ? F124 C232 F23 65.8(8) . . ? F122 C232 C229 116.1(5) . . ? F22 C232 C229 114.2(3) . . ? F24 C232 C229 112.6(3) . . ? F123 C232 C229 111.0(4) . . ? F124 C232 C229 110.3(6) . . ? F23 C232 C229 111.7(3) . . ? C901 C902 C903 115.7(6) . . ? C904 C903 C902 113.3(6) . . ? C903 C904 C905 112.9(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.663 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.056 data_142abc09 _database_code_depnum_ccdc_archive 'CCDC 801544' #TrackingRef '- Compound 1b.cif' #------------------------ # [Rh(dppp)(C6H5F)]BArF4 #------------------------ # start Validation Reply Form _vrf_PLAT242_142abc09 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C223 RESPONSE: The anion contains a significant degree of disorder. See details in supplementary information or _refine_special_details. ; _vrf_PLAT431_142abc09 ; PROBLEM: Short Inter HL..A Contact F106 .. F1C .. 2.50 Ang. RESPONSE: The structure contains a disordered anion and fluorobenzene lignad - the short contact occurs between disordered components (7%). ; _vrf_PLAT301_142abc09 ; 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, C33 H31 F P2 Rh' _chemical_formula_sum 'C65 H43 B F25 P2 Rh' _chemical_formula_weight 1474.65 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5134(2) _cell_length_b 13.5513(2) _cell_length_c 19.5061(4) _cell_angle_alpha 105.8393(7) _cell_angle_beta 94.3128(7) _cell_angle_gamma 94.6952(9) _cell_volume 3154.98(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9658 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 0.436 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.879 _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 19313 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 5.14 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12382 _reflns_number_gt 10432 _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. Disorder of the fluorobenzene ligand was treated by modelling the flourine atom over three sites and restraining the 1,2- and 1,3- C-F distances. A planarity restraint was also applied about each disordered fluorine atom. 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^)+(0.0425P)^2^+4.3628P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 12382 _refine_ls_number_parameters 1005 _refine_ls_number_restraints 654 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1145 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.198 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.72169(2) 0.307122(19) 0.782743(14) 0.02917(9) Uani 1 1 d . . . P1 P 0.85262(7) 0.35917(6) 0.87259(4) 0.02800(18) Uani 1 1 d . A . P2 P 0.83389(7) 0.34703(7) 0.70817(5) 0.03120(19) Uani 1 1 d . A . C1 C 0.5559(2) 0.3360(3) 0.8278(2) 0.0512(10) Uani 1 1 d D A 1 H1 H 0.5375 0.3905 0.8658 0.061 Uiso 0.50 1 calc PR A 1 C2 C 0.5901(3) 0.2481(3) 0.8431(2) 0.0477(10) Uani 1 1 d D A 1 H2 H 0.6032 0.2468 0.8914 0.057 Uiso 0.90 1 calc PR A 1 C3 C 0.6052(3) 0.1620(3) 0.7874(2) 0.0499(10) Uani 1 1 d D A 1 H3 H 0.6238 0.1001 0.7970 0.060 Uiso 1 1 calc R A 1 C4 C 0.5923(2) 0.1694(3) 0.7183(2) 0.0521(11) Uani 1 1 d D A 1 H4 H 0.5992 0.1105 0.6797 0.063 Uiso 0.60 1 calc PR A 1 C5 C 0.5695(3) 0.2609(3) 0.7033(2) 0.0511(10) Uani 1 1 d D A 1 H5 H 0.5684 0.2663 0.6557 0.061 Uiso 1 1 calc R A 1 C6 C 0.5479(3) 0.3458(3) 0.7596(2) 0.0520(10) Uani 1 1 d D A 1 H6 H 0.5286 0.4076 0.7504 0.062 Uiso 1 1 calc R A 1 F1A F 0.5293(5) 0.4055(5) 0.8793(3) 0.101(2) Uani 0.50 1 d PDU B 2 F1B F 0.5996(6) 0.0916(5) 0.6662(4) 0.101(3) Uani 0.40 1 d PDU C 2 F1C F 0.6062(9) 0.2464(7) 0.9074(5) 0.071(7) Uani 0.10 1 d PDU D 2 C7 C 0.9454(3) 0.4714(3) 0.87473(19) 0.0361(8) Uani 1 1 d . . . H7A H 0.9043 0.5321 0.8805 0.043 Uiso 1 1 calc R A . H7B H 0.9989 0.4855 0.9172 0.043 Uiso 1 1 calc R . . C8 C 1.0055(3) 0.4595(3) 0.8082(2) 0.0391(8) Uani 1 1 d . A . H8A H 1.0642 0.5166 0.8177 0.047 Uiso 1 1 calc R . . H8B H 1.0387 0.3939 0.7984 0.047 Uiso 1 1 calc R . . C9 C 0.9323(3) 0.4601(3) 0.7424(2) 0.0402(8) Uani 1 1 d . . . H9A H 0.9777 0.4656 0.7039 0.048 Uiso 1 1 calc R A . H9B H 0.8933 0.5223 0.7544 0.048 Uiso 1 1 calc R . . C10 C 0.7963(3) 0.3997(2) 0.95817(18) 0.0310(7) Uani 1 1 d . . . C11 C 0.7424(3) 0.4885(3) 0.9737(2) 0.0438(9) Uani 1 1 d . A . H11 H 0.7387 0.5285 0.9407 0.053 Uiso 1 1 calc R . . C12 C 0.6945(4) 0.5183(3) 1.0366(2) 0.0539(11) Uani 1 1 d . . . H12 H 0.6589 0.5792 1.0468 0.065 Uiso 1 1 calc R A . C13 C 0.6981(3) 0.4605(3) 1.0848(2) 0.0500(10) Uani 1 1 d . A . H13 H 0.6648 0.4810 1.1279 0.060 Uiso 1 1 calc R . . C14 C 0.7505(3) 0.3724(3) 1.0699(2) 0.0468(9) Uani 1 1 d . . . H14 H 0.7531 0.3322 1.1029 0.056 Uiso 1 1 calc R A . C15 C 0.7994(3) 0.3422(3) 1.0073(2) 0.0380(8) Uani 1 1 d . A . H15 H 0.8354 0.2816 0.9977 0.046 Uiso 1 1 calc R . . C16 C 0.9416(3) 0.2640(2) 0.88476(18) 0.0309(7) Uani 1 1 d . . . C17 C 1.0341(3) 0.2915(3) 0.9328(2) 0.0383(8) Uani 1 1 d . A . H17 H 1.0521 0.3614 0.9599 0.046 Uiso 1 1 calc R . . C18 C 1.1004(3) 0.2178(3) 0.9414(2) 0.0441(9) Uani 1 1 d . . . H18 H 1.1633 0.2373 0.9744 0.053 Uiso 1 1 calc R A . C19 C 1.0752(3) 0.1166(3) 0.9023(2) 0.0473(10) Uani 1 1 d . A . H19 H 1.1215 0.0664 0.9076 0.057 Uiso 1 1 calc R . . C20 C 0.9836(4) 0.0880(3) 0.8556(3) 0.0513(10) Uani 1 1 d . . . H20 H 0.9658 0.0178 0.8291 0.062 Uiso 1 1 calc R A . C21 C 0.9164(3) 0.1614(3) 0.8468(2) 0.0415(8) Uani 1 1 d . A . H21 H 0.8527 0.1409 0.8145 0.050 Uiso 1 1 calc R . . C22 C 0.7577(3) 0.3797(3) 0.63527(19) 0.0382(8) Uani 1 1 d . . . C23 C 0.7415(4) 0.3150(4) 0.5670(2) 0.0533(11) Uani 1 1 d . A . H23 H 0.7746 0.2528 0.5555 0.064 Uiso 1 1 calc R . . C24 C 0.6767(4) 0.3400(5) 0.5142(2) 0.0726(15) Uani 1 1 d . . . H24 H 0.6648 0.2941 0.4672 0.087 Uiso 1 1 calc R A . C25 C 0.6300(4) 0.4302(5) 0.5298(3) 0.0713(15) Uani 1 1 d . A . H25 H 0.5863 0.4472 0.4935 0.086 Uiso 1 1 calc R . . C26 C 0.6461(4) 0.4959(4) 0.5973(3) 0.0666(13) Uani 1 1 d . . . H26 H 0.6140 0.5588 0.6080 0.080 Uiso 1 1 calc R A . C27 C 0.7095(4) 0.4710(3) 0.6505(2) 0.0529(10) Uani 1 1 d . A . H27 H 0.7200 0.5168 0.6975 0.063 Uiso 1 1 calc R . . C28 C 0.9117(3) 0.2445(3) 0.66378(19) 0.0341(7) Uani 1 1 d . . . C29 C 0.8813(3) 0.1438(3) 0.6636(2) 0.0474(9) Uani 1 1 d . A . H29 H 0.8213 0.1294 0.6878 0.057 Uiso 1 1 calc R . . C30 C 0.9371(4) 0.0639(3) 0.6289(2) 0.0551(11) Uani 1 1 d . . . H30 H 0.9153 -0.0047 0.6294 0.066 Uiso 1 1 calc R A . C31 C 1.0237(3) 0.0833(3) 0.5937(2) 0.0490(10) Uani 1 1 d . A . H31 H 1.0620 0.0284 0.5698 0.059 Uiso 1 1 calc R . . C32 C 1.0548(3) 0.1828(4) 0.5933(2) 0.0529(10) Uani 1 1 d . . . H32 H 1.1149 0.1964 0.5690 0.063 Uiso 1 1 calc R A . C33 C 0.9999(3) 0.2629(3) 0.6278(2) 0.0466(9) Uani 1 1 d . A . H33 H 1.0223 0.3312 0.6270 0.056 Uiso 1 1 calc R . . B200 B 0.3293(3) 0.8512(3) 0.75559(19) 0.0267(7) Uani 1 1 d . . . C201 C 0.2677(2) 0.8652(2) 0.82925(17) 0.0271(6) Uani 1 1 d . . . C202 C 0.3188(3) 0.9137(2) 0.89780(17) 0.0285(7) Uani 1 1 d . . . H202 H 0.3929 0.9388 0.9029 0.034 Uiso 1 1 calc R . . C203 C 0.2644(3) 0.9264(2) 0.95898(17) 0.0283(7) Uani 1 1 d D E . C204 C 0.1562(3) 0.8933(2) 0.95468(18) 0.0300(7) Uani 1 1 d . . . H204 H 0.1191 0.9029 0.9964 0.036 Uiso 1 1 calc R . . C205 C 0.1035(2) 0.8453(2) 0.88682(18) 0.0288(7) Uani 1 1 d . . . C206 C 0.1582(3) 0.8315(2) 0.82646(17) 0.0288(7) Uani 1 1 d . . . H206 H 0.1198 0.7977 0.7811 0.035 Uiso 1 1 calc R . . C207 C 0.3255(3) 0.9763(3) 1.03030(19) 0.0421(9) Uani 1 1 d D . . F101 F -0.07083(18) 0.87143(19) 0.92223(15) 0.0576(6) Uani 1 1 d U . . F102 F -0.02876(19) 0.71806(17) 0.89724(16) 0.0593(7) Uani 1 1 d U . . F103 F -0.05970(19) 0.7906(3) 0.81378(14) 0.0863(11) Uani 1 1 d U . . C208 C -0.0129(3) 0.8066(3) 0.8798(2) 0.0393(8) Uani 1 1 d . . . F104 F 0.2659(4) 1.0070(8) 1.0828(3) 0.078(2) Uani 0.680(18) 1 d PDU E 1 F105 F 0.3941(6) 1.0568(5) 1.0311(3) 0.0624(18) Uani 0.680(18) 1 d PDU E 1 F106 F 0.3896(7) 0.9115(5) 1.0501(4) 0.076(2) Uani 0.680(18) 1 d PDU E 1 F204 F 0.4176(7) 0.9420(14) 1.0410(6) 0.068(4) Uani 0.320(18) 1 d PDU E 2 F205 F 0.2696(9) 0.9630(14) 1.0834(4) 0.065(4) Uani 0.320(18) 1 d PDU E 2 F206 F 0.3442(18) 1.0772(5) 1.0418(7) 0.089(4) Uani 0.320(18) 1 d PDU E 2 C209 C 0.3200(2) 0.9525(3) 0.72584(17) 0.0288(7) Uani 1 1 d . . . C210 C 0.3322(3) 0.9480(3) 0.65414(18) 0.0337(7) Uani 1 1 d . . . H210 H 0.3444 0.8840 0.6223 0.040 Uiso 1 1 calc R . . C211 C 0.3271(3) 1.0332(3) 0.62753(19) 0.0367(8) Uani 1 1 d D F . C212 C 0.3074(3) 1.1273(3) 0.6716(2) 0.0381(8) Uani 1 1 d . . . H212 H 0.3030 1.1856 0.6537 0.046 Uiso 1 1 calc R . . C213 C 0.2943(3) 1.1340(3) 0.74240(19) 0.0338(7) Uani 1 1 d . . . C214 C 0.3006(2) 1.0486(2) 0.76900(18) 0.0295(7) Uani 1 1 d . . . H214 H 0.2915 1.0562 0.8180 0.035 Uiso 1 1 calc R . . C215 C 0.3403(3) 1.0242(3) 0.5508(2) 0.0536(11) Uani 1 1 d D . . F107 F 0.3703(11) 1.1060(5) 0.5354(4) 0.107(3) Uani 0.518(12) 1 d PDU F 1 F108 F 0.4066(7) 0.9540(7) 0.5243(4) 0.073(2) Uani 0.518(12) 1 d PDU F 1 F109 F 0.2471(5) 0.9809(10) 0.5098(3) 0.090(3) Uani 0.518(12) 1 d PDU F 1 F207 F 0.3552(10) 0.9349(5) 0.5117(4) 0.080(3) Uani 0.482(12) 1 d PDU F 2 F208 F 0.2617(7) 1.0602(11) 0.5185(4) 0.086(3) Uani 0.482(12) 1 d PDU F 2 F209 F 0.4270(7) 1.0880(7) 0.5457(4) 0.088(3) Uani 0.482(12) 1 d PDU F 2 C216 C 0.2676(3) 1.2329(3) 0.7905(2) 0.0438(9) Uani 1 1 d . . . F110 F 0.3083(2) 1.31605(18) 0.77209(17) 0.0671(8) Uani 1 1 d U . . F111 F 0.3046(2) 1.24684(18) 0.85864(13) 0.0559(6) Uani 1 1 d U . . F112 F 0.16093(18) 1.23825(18) 0.78920(14) 0.0537(6) Uani 1 1 d U . . C217 C 0.4558(2) 0.8314(2) 0.76940(17) 0.0269(6) Uani 1 1 d . . . C218 C 0.4884(3) 0.7729(2) 0.81501(18) 0.0314(7) Uani 1 1 d . . . H218 H 0.4378 0.7522 0.8437 0.038 Uiso 1 1 calc R . . C219 C 0.5923(3) 0.7443(2) 0.81954(19) 0.0336(7) Uani 1 1 d D G . C220 C 0.6691(3) 0.7736(3) 0.7795(2) 0.0363(8) Uani 1 1 d . . . H220 H 0.7398 0.7534 0.7822 0.044 Uiso 1 1 calc R . . C221 C 0.6395(3) 0.8333(2) 0.73531(19) 0.0345(7) Uani 1 1 d D H . C222 C 0.5355(3) 0.8617(2) 0.73076(18) 0.0302(7) Uani 1 1 d . . . H222 H 0.5181 0.9033 0.7003 0.036 Uiso 1 1 calc R . . C223 C 0.6216(3) 0.6787(3) 0.8668(2) 0.0472(10) Uani 1 1 d D . . F113 F 0.5992(10) 0.5815(3) 0.8351(4) 0.110(3) Uani 0.529(8) 1 d PDU G 1 F114 F 0.5670(6) 0.6951(6) 0.9239(4) 0.083(2) Uani 0.529(8) 1 d PDU G 1 F115 F 0.7214(4) 0.6956(7) 0.8941(5) 0.090(3) Uani 0.529(8) 1 d PDU G 1 F213 F 0.6502(11) 0.7274(5) 0.9327(3) 0.106(3) Uani 0.471(8) 1 d PDU G 2 F214 F 0.7048(6) 0.6251(7) 0.8456(5) 0.081(3) Uani 0.471(8) 1 d PDU G 2 F215 F 0.5471(5) 0.6049(6) 0.8662(6) 0.086(3) Uani 0.471(8) 1 d PDU G 2 C224 C 0.7205(3) 0.8677(3) 0.6924(2) 0.0507(10) Uani 1 1 d D . . F116 F 0.7970(4) 0.8079(4) 0.6782(4) 0.087(2) Uani 0.682(7) 1 d PDU H 1 F117 F 0.7752(5) 0.9590(4) 0.7317(3) 0.097(2) Uani 0.682(7) 1 d PDU H 1 F118 F 0.6819(3) 0.8866(6) 0.6350(3) 0.092(2) Uani 0.682(7) 1 d PDU H 1 F216 F 0.7066(9) 0.9537(7) 0.6767(7) 0.081(3) Uani 0.318(7) 1 d PDU H 2 F217 F 0.7138(10) 0.7993(8) 0.6253(4) 0.095(4) Uani 0.318(7) 1 d PDU H 2 F218 F 0.8208(4) 0.8716(11) 0.7149(6) 0.081(3) Uani 0.318(7) 1 d PDU H 2 C225 C 0.2686(3) 0.7485(3) 0.69551(17) 0.0304(7) Uani 1 1 d . . . C226 C 0.1715(3) 0.7535(3) 0.65658(18) 0.0364(8) Uani 1 1 d . . . H226 H 0.1454 0.8187 0.6614 0.044 Uiso 1 1 calc R . . C227 C 0.1122(3) 0.6660(3) 0.6111(2) 0.0445(9) Uani 1 1 d . . . C228 C 0.1487(3) 0.5700(3) 0.6015(2) 0.0503(10) Uani 1 1 d . . . H228 H 0.1080 0.5100 0.5705 0.060 Uiso 1 1 calc R . . C229 C 0.2454(3) 0.5630(3) 0.6379(2) 0.0421(8) Uani 1 1 d D I . C230 C 0.3038(3) 0.6505(3) 0.68438(18) 0.0347(7) Uani 1 1 d . . . H230 H 0.3696 0.6435 0.7094 0.042 Uiso 1 1 calc R . . C231 C 0.0068(4) 0.6748(4) 0.5723(3) 0.0655(13) Uani 1 1 d . . . F119 F 0.0073(3) 0.6381(3) 0.50174(16) 0.0834(9) Uani 1 1 d U . . F120 F -0.0177(3) 0.7706(3) 0.5822(2) 0.1101(14) Uani 1 1 d U . . F121 F -0.0735(3) 0.6212(4) 0.5888(2) 0.1273(16) Uani 1 1 d U . . C232 C 0.2870(3) 0.4604(3) 0.6288(2) 0.0610(12) Uani 1 1 d D . . F122 F 0.3897(3) 0.4627(3) 0.6298(4) 0.094(2) Uani 0.719(8) 1 d PDU I 1 F123 F 0.2455(5) 0.3919(3) 0.5682(3) 0.098(2) Uani 0.719(8) 1 d PDU I 1 F124 F 0.2541(7) 0.4169(5) 0.6779(4) 0.124(2) Uani 0.719(8) 1 d PDU I 1 F222 F 0.2180(7) 0.3853(6) 0.6287(9) 0.086(4) Uani 0.281(8) 1 d PDU I 2 F223 F 0.3641(10) 0.4610(7) 0.6807(7) 0.081(4) Uani 0.281(8) 1 d PDU I 2 F224 F 0.3358(14) 0.4284(9) 0.5697(6) 0.106(5) Uani 0.281(8) 1 d PDU I 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 0.02760(15) 0.02873(14) 0.03097(15) 0.00887(11) 0.00106(10) 0.00189(10) P1 0.0310(4) 0.0225(4) 0.0300(4) 0.0072(3) 0.0000(3) 0.0031(3) P2 0.0316(4) 0.0320(4) 0.0318(4) 0.0125(4) 0.0025(3) 0.0025(3) C1 0.035(2) 0.058(3) 0.056(3) 0.004(2) 0.0170(19) 0.0093(18) C2 0.034(2) 0.065(3) 0.051(2) 0.029(2) 0.0096(17) -0.0023(18) C3 0.037(2) 0.040(2) 0.073(3) 0.020(2) -0.0002(19) -0.0058(16) C4 0.036(2) 0.047(2) 0.057(3) -0.007(2) -0.0025(18) -0.0108(17) C5 0.0304(19) 0.075(3) 0.046(2) 0.021(2) -0.0099(17) -0.0122(19) C6 0.030(2) 0.058(3) 0.074(3) 0.029(2) -0.0027(19) 0.0055(17) F1A 0.084(4) 0.090(4) 0.109(5) -0.010(4) 0.029(4) 0.013(4) F1B 0.086(5) 0.097(6) 0.096(6) -0.007(5) 0.009(5) -0.009(4) F1C 0.090(12) 0.074(11) 0.055(11) 0.035(9) 0.010(9) -0.015(9) C7 0.0392(19) 0.0270(16) 0.0385(19) 0.0067(14) -0.0036(15) -0.0021(14) C8 0.0334(19) 0.0351(18) 0.047(2) 0.0124(16) -0.0002(16) -0.0054(14) C9 0.045(2) 0.0346(18) 0.043(2) 0.0160(16) 0.0039(16) -0.0019(15) C10 0.0334(17) 0.0259(15) 0.0309(17) 0.0038(13) -0.0001(13) 0.0049(13) C11 0.058(2) 0.0317(18) 0.043(2) 0.0086(16) 0.0086(18) 0.0146(17) C12 0.066(3) 0.039(2) 0.054(3) 0.0024(19) 0.015(2) 0.0185(19) C13 0.052(2) 0.052(2) 0.040(2) 0.0010(18) 0.0136(18) 0.0075(19) C14 0.050(2) 0.050(2) 0.045(2) 0.0181(19) 0.0128(18) 0.0096(18) C15 0.040(2) 0.0360(18) 0.041(2) 0.0131(16) 0.0086(16) 0.0101(15) C16 0.0325(17) 0.0298(16) 0.0325(17) 0.0102(14) 0.0058(14) 0.0075(13) C17 0.0370(19) 0.042(2) 0.0363(19) 0.0099(16) 0.0031(15) 0.0103(15) C18 0.036(2) 0.062(3) 0.041(2) 0.0226(19) 0.0048(16) 0.0161(18) C19 0.048(2) 0.049(2) 0.058(3) 0.030(2) 0.0137(19) 0.0227(18) C20 0.059(3) 0.0308(19) 0.068(3) 0.0176(19) 0.007(2) 0.0133(17) C21 0.043(2) 0.0315(18) 0.050(2) 0.0125(16) -0.0004(17) 0.0065(15) C22 0.0374(19) 0.047(2) 0.0366(19) 0.0206(17) 0.0046(15) 0.0096(16) C23 0.053(3) 0.069(3) 0.039(2) 0.012(2) 0.0016(18) 0.025(2) C24 0.074(3) 0.110(4) 0.035(2) 0.015(3) -0.001(2) 0.041(3) C25 0.066(3) 0.114(4) 0.053(3) 0.045(3) 0.008(2) 0.043(3) C26 0.071(3) 0.073(3) 0.070(3) 0.037(3) 0.003(3) 0.033(3) C27 0.059(3) 0.052(2) 0.051(2) 0.017(2) 0.000(2) 0.018(2) C28 0.0289(17) 0.0418(19) 0.0332(18) 0.0140(15) -0.0006(14) 0.0045(14) C29 0.050(2) 0.042(2) 0.053(2) 0.0139(18) 0.0202(19) 0.0063(17) C30 0.064(3) 0.042(2) 0.061(3) 0.010(2) 0.023(2) 0.0128(19) C31 0.041(2) 0.057(3) 0.048(2) 0.0096(19) 0.0096(18) 0.0153(18) C32 0.039(2) 0.067(3) 0.056(3) 0.019(2) 0.0169(19) 0.012(2) C33 0.039(2) 0.052(2) 0.056(2) 0.025(2) 0.0128(18) 0.0057(17) B200 0.0231(17) 0.0310(18) 0.0250(17) 0.0064(14) 0.0004(13) 0.0047(14) C201 0.0249(15) 0.0256(15) 0.0307(17) 0.0091(13) -0.0011(13) 0.0021(12) C202 0.0253(16) 0.0282(16) 0.0297(16) 0.0060(13) -0.0006(13) 0.0001(12) C203 0.0310(17) 0.0274(16) 0.0259(16) 0.0076(13) -0.0004(13) 0.0026(12) C204 0.0324(17) 0.0298(16) 0.0307(17) 0.0126(14) 0.0049(13) 0.0050(13) C205 0.0241(16) 0.0306(16) 0.0342(17) 0.0138(14) 0.0020(13) 0.0019(12) C206 0.0255(16) 0.0331(17) 0.0273(16) 0.0098(13) -0.0027(13) 0.0003(12) C207 0.043(2) 0.049(2) 0.0291(18) 0.0051(16) 0.0021(16) -0.0038(17) F101 0.0333(12) 0.0589(14) 0.0888(19) 0.0276(13) 0.0229(12) 0.0126(10) F102 0.0429(13) 0.0412(12) 0.096(2) 0.0234(13) 0.0145(13) -0.0073(10) F103 0.0288(13) 0.178(3) 0.0492(15) 0.0396(18) -0.0084(11) -0.0236(16) C208 0.0279(18) 0.053(2) 0.040(2) 0.0187(17) 0.0028(15) 0.0011(15) F104 0.051(3) 0.114(5) 0.040(3) -0.025(3) 0.012(2) -0.005(3) F105 0.065(3) 0.066(3) 0.039(2) -0.0013(19) -0.004(2) -0.029(2) F106 0.088(4) 0.073(3) 0.060(3) 0.020(2) -0.037(3) 0.005(3) F204 0.028(4) 0.117(8) 0.042(5) -0.002(5) -0.007(3) 0.001(5) F205 0.069(6) 0.102(8) 0.018(4) 0.018(5) 0.001(4) -0.025(5) F206 0.126(9) 0.057(5) 0.062(6) -0.006(4) -0.009(6) -0.024(6) C209 0.0206(15) 0.0380(17) 0.0285(16) 0.0100(14) 0.0013(12) 0.0053(12) C210 0.0280(17) 0.0432(19) 0.0294(17) 0.0085(15) 0.0025(13) 0.0078(14) C211 0.0281(17) 0.054(2) 0.0339(18) 0.0205(16) 0.0067(14) 0.0085(15) C212 0.0295(18) 0.047(2) 0.047(2) 0.0254(17) 0.0083(15) 0.0111(15) C213 0.0230(16) 0.0384(18) 0.043(2) 0.0145(15) 0.0079(14) 0.0070(13) C214 0.0248(16) 0.0353(17) 0.0300(17) 0.0107(14) 0.0048(13) 0.0059(13) C215 0.050(3) 0.080(3) 0.039(2) 0.023(2) 0.0134(19) 0.022(2) F107 0.179(8) 0.096(5) 0.071(4) 0.062(4) 0.031(5) 0.008(5) F108 0.071(5) 0.111(6) 0.051(4) 0.029(3) 0.036(3) 0.037(4) F109 0.070(4) 0.159(8) 0.035(3) 0.018(4) 0.000(3) 0.018(4) F207 0.126(7) 0.073(4) 0.038(3) 0.015(3) 0.017(4) -0.004(4) F208 0.082(5) 0.157(8) 0.043(3) 0.051(4) 0.017(3) 0.060(5) F209 0.083(5) 0.127(6) 0.051(4) 0.025(4) 0.029(4) -0.025(4) C216 0.042(2) 0.0364(19) 0.059(3) 0.0199(18) 0.0160(19) 0.0111(16) F110 0.0761(18) 0.0385(13) 0.097(2) 0.0269(13) 0.0385(16) 0.0120(12) F111 0.0656(16) 0.0422(13) 0.0519(15) -0.0013(11) 0.0017(12) 0.0127(11) F112 0.0420(13) 0.0591(14) 0.0681(16) 0.0220(12) 0.0203(11) 0.0244(11) C217 0.0256(16) 0.0240(15) 0.0263(16) 0.0014(12) -0.0034(12) 0.0003(12) C218 0.0277(17) 0.0306(16) 0.0335(18) 0.0072(14) -0.0007(13) -0.0001(13) C219 0.0291(17) 0.0263(16) 0.0422(19) 0.0079(14) -0.0064(14) 0.0004(13) C220 0.0242(16) 0.0285(17) 0.053(2) 0.0069(15) -0.0030(15) 0.0030(13) C221 0.0259(17) 0.0285(16) 0.045(2) 0.0055(15) 0.0025(14) -0.0004(13) C222 0.0270(16) 0.0260(15) 0.0355(18) 0.0059(13) -0.0002(13) 0.0021(12) C223 0.041(2) 0.044(2) 0.059(3) 0.023(2) -0.0087(19) 0.0052(17) F113 0.181(8) 0.036(3) 0.106(5) 0.021(3) -0.030(5) 0.015(4) F114 0.087(5) 0.116(5) 0.082(4) 0.077(4) 0.022(4) 0.044(4) F115 0.040(3) 0.136(6) 0.119(6) 0.090(5) -0.026(3) -0.006(3) F213 0.167(8) 0.082(5) 0.069(4) 0.027(4) -0.035(5) 0.033(5) F214 0.082(5) 0.098(5) 0.096(5) 0.061(4) 0.031(4) 0.065(4) F215 0.054(4) 0.083(5) 0.145(7) 0.084(5) -0.014(4) -0.008(3) C224 0.032(2) 0.054(2) 0.073(3) 0.025(2) 0.015(2) 0.0100(17) F116 0.068(3) 0.095(4) 0.125(5) 0.050(3) 0.061(3) 0.043(3) F117 0.094(4) 0.081(3) 0.100(4) 0.011(3) 0.032(3) -0.051(3) F118 0.051(3) 0.174(6) 0.071(3) 0.072(4) 0.013(2) 0.000(3) F216 0.070(6) 0.070(6) 0.124(8) 0.049(5) 0.054(6) 0.017(5) F217 0.099(7) 0.106(7) 0.078(6) 0.020(5) 0.046(5) -0.020(6) F218 0.037(4) 0.118(8) 0.090(7) 0.036(6) 0.013(4) -0.008(5) C225 0.0244(16) 0.0396(18) 0.0250(16) 0.0066(14) 0.0013(12) 0.0008(13) C226 0.0316(18) 0.0421(19) 0.0297(18) 0.0016(15) -0.0021(14) 0.0040(14) C227 0.034(2) 0.055(2) 0.034(2) -0.0002(17) -0.0079(15) -0.0001(16) C228 0.047(2) 0.048(2) 0.043(2) -0.0025(18) -0.0079(18) -0.0079(18) C229 0.046(2) 0.0343(19) 0.041(2) 0.0056(16) -0.0023(17) -0.0024(16) C230 0.0327(18) 0.0363(18) 0.0332(18) 0.0094(15) -0.0027(14) -0.0010(14) C231 0.053(3) 0.065(3) 0.057(3) -0.011(2) -0.022(2) 0.001(2) F119 0.081(2) 0.098(2) 0.0592(18) 0.0166(16) -0.0326(15) -0.0025(17) F120 0.081(2) 0.089(2) 0.127(3) -0.012(2) -0.063(2) 0.0262(18) F121 0.0395(17) 0.217(5) 0.143(3) 0.098(3) -0.0204(19) -0.022(2) C232 0.067(3) 0.040(2) 0.068(3) 0.010(2) -0.011(2) -0.004(2) F122 0.056(3) 0.042(2) 0.167(6) 0.004(3) -0.011(3) 0.0110(18) F123 0.113(4) 0.040(2) 0.111(4) -0.018(2) -0.039(3) 0.014(2) F124 0.181(6) 0.081(4) 0.134(5) 0.069(4) 0.017(5) 0.023(4) F222 0.069(6) 0.050(5) 0.133(9) 0.028(6) -0.011(6) -0.013(4) F223 0.087(7) 0.038(5) 0.107(8) 0.012(5) -0.029(6) 0.017(5) F224 0.131(9) 0.079(7) 0.113(8) 0.021(6) 0.041(7) 0.041(7) _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 P1 2.2266(9) . ? Rh1 P2 2.2343(9) . ? Rh1 C5 2.292(4) . ? Rh1 C2 2.307(3) . ? Rh1 C6 2.318(4) . ? Rh1 C1 2.335(3) . ? Rh1 C4 2.367(3) . ? Rh1 C3 2.377(4) . ? P1 C16 1.822(3) . ? P1 C10 1.823(3) . ? P1 C7 1.826(3) . ? P2 C9 1.822(4) . ? P2 C28 1.822(4) . ? P2 C22 1.827(4) . ? C1 C6 1.369(6) . ? C1 C2 1.396(6) . ? C2 C3 1.397(6) . ? C3 C4 1.378(6) . ? C4 C5 1.396(6) . ? C5 C6 1.417(6) . ? C7 C8 1.525(5) . ? C8 C9 1.522(5) . ? C10 C15 1.390(5) . ? C10 C11 1.400(5) . ? C11 C12 1.381(6) . ? C12 C13 1.379(6) . ? C13 C14 1.381(6) . ? C14 C15 1.384(5) . ? C16 C21 1.383(5) . ? C16 C17 1.389(5) . ? C17 C18 1.385(5) . ? C18 C19 1.372(6) . ? C19 C20 1.369(6) . ? C20 C21 1.391(5) . ? C22 C23 1.371(6) . ? C22 C27 1.389(5) . ? C23 C24 1.393(6) . ? C24 C25 1.368(7) . ? C25 C26 1.363(7) . ? C26 C27 1.389(6) . ? C28 C29 1.385(5) . ? C28 C33 1.393(5) . ? C29 C30 1.384(5) . ? C30 C31 1.370(6) . ? C31 C32 1.375(6) . ? C32 C33 1.377(6) . ? B200 C209 1.639(5) . ? B200 C225 1.640(5) . ? B200 C217 1.641(5) . ? B200 C201 1.654(5) . ? C201 C202 1.397(4) . ? C201 C206 1.401(4) . ? C202 C203 1.395(4) . ? C203 C204 1.380(5) . ? C203 C207 1.490(5) . ? C204 C205 1.392(5) . ? C205 C206 1.383(4) . ? C205 C208 1.491(5) . ? C207 F204 1.301(7) . ? C207 F104 1.308(5) . ? C207 F206 1.322(6) . ? C207 F105 1.328(5) . ? C207 F205 1.335(6) . ? C207 F106 1.348(5) . ? F101 C208 1.334(4) . ? F102 C208 1.337(4) . ? F103 C208 1.326(4) . ? C209 C214 1.395(5) . ? C209 C210 1.403(5) . ? C210 C211 1.393(5) . ? C211 C212 1.383(5) . ? C211 C215 1.491(5) . ? C212 C213 1.383(5) . ? C213 C214 1.397(5) . ? C213 C216 1.491(5) . ? C215 F107 1.261(6) . ? C215 F207 1.280(6) . ? C215 F208 1.324(5) . ? C215 F108 1.337(6) . ? C215 F109 1.355(6) . ? C215 F209 1.358(6) . ? C216 F111 1.332(5) . ? C216 F112 1.341(4) . ? C216 F110 1.346(4) . ? C217 C222 1.396(5) . ? C217 C218 1.403(5) . ? C218 C219 1.390(5) . ? C219 C220 1.383(5) . ? C219 C223 1.491(5) . ? C220 C221 1.384(5) . ? C221 C222 1.390(4) . ? C221 C224 1.485(5) . ? C223 F213 1.283(6) . ? C223 F113 1.290(5) . ? C223 F115 1.297(5) . ? C223 F215 1.307(5) . ? C223 F114 1.328(5) . ? C223 F214 1.344(5) . ? C224 F118 1.284(5) . ? C224 F218 1.291(6) . ? C224 F116 1.302(5) . ? C224 F216 1.304(6) . ? C224 F117 1.361(5) . ? C224 F217 1.375(6) . ? C225 C230 1.400(5) . ? C225 C226 1.400(5) . ? C226 C227 1.388(5) . ? C227 C228 1.383(6) . ? C227 C231 1.500(6) . ? C228 C229 1.381(6) . ? C229 C230 1.390(5) . ? C229 C232 1.495(6) . ? C231 F121 1.303(6) . ? C231 F120 1.324(6) . ? C231 F119 1.330(6) . ? C232 F222 1.279(6) . ? C232 F122 1.282(5) . ? C232 F123 1.325(5) . ? C232 F124 1.327(5) . ? C232 F224 1.328(7) . ? C232 F223 1.344(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Rh1 P2 90.07(3) . . ? P1 Rh1 C5 171.32(11) . . ? P2 Rh1 C5 97.48(11) . . ? P1 Rh1 C2 98.61(11) . . ? P2 Rh1 C2 170.61(11) . . ? C5 Rh1 C2 74.16(15) . . ? P1 Rh1 C6 136.59(12) . . ? P2 Rh1 C6 112.64(11) . . ? C5 Rh1 C6 35.80(15) . . ? C2 Rh1 C6 63.00(15) . . ? P1 Rh1 C1 109.18(10) . . ? P2 Rh1 C1 144.14(12) . . ? C5 Rh1 C1 62.15(15) . . ? C2 Rh1 C1 35.00(15) . . ? C6 Rh1 C1 34.22(15) . . ? P1 Rh1 C4 145.15(12) . . ? P2 Rh1 C4 109.52(11) . . ? C5 Rh1 C4 34.83(16) . . ? C2 Rh1 C4 61.17(15) . . ? C6 Rh1 C4 62.48(15) . . ? C1 Rh1 C4 71.52(13) . . ? P1 Rh1 C3 114.13(11) . . ? P2 Rh1 C3 137.50(11) . . ? C5 Rh1 C3 62.54(15) . . ? C2 Rh1 C3 34.65(15) . . ? C6 Rh1 C3 73.98(15) . . ? C1 Rh1 C3 61.82(14) . . ? C4 Rh1 C3 33.76(15) . . ? C16 P1 C10 103.87(15) . . ? C16 P1 C7 103.59(16) . . ? C10 P1 C7 102.50(16) . . ? C16 P1 Rh1 116.89(12) . . ? C10 P1 Rh1 110.60(11) . . ? C7 P1 Rh1 117.60(12) . . ? C9 P2 C28 104.73(17) . . ? C9 P2 C22 101.72(17) . . ? C28 P2 C22 104.79(16) . . ? C9 P2 Rh1 118.30(13) . . ? C28 P2 Rh1 115.71(12) . . ? C22 P2 Rh1 109.93(12) . . ? C6 C1 C2 121.9(4) . . ? C6 C1 Rh1 72.2(2) . . ? C2 C1 Rh1 71.44(19) . . ? C1 C2 C3 120.2(4) . . ? C1 C2 Rh1 73.56(19) . . ? C3 C2 Rh1 75.4(2) . . ? C4 C3 C2 118.1(4) . . ? C4 C3 Rh1 72.7(2) . . ? C2 C3 Rh1 69.9(2) . . ? C3 C4 C5 121.9(4) . . ? C3 C4 Rh1 73.5(2) . . ? C5 C4 Rh1 69.6(2) . . ? C4 C5 C6 119.5(4) . . ? C4 C5 Rh1 75.5(2) . . ? C6 C5 Rh1 73.1(2) . . ? C1 C6 C5 118.0(4) . . ? C1 C6 Rh1 73.6(2) . . ? C5 C6 Rh1 71.1(2) . . ? C8 C7 P1 114.3(2) . . ? C9 C8 C7 112.6(3) . . ? C8 C9 P2 114.7(2) . . ? C15 C10 C11 118.2(3) . . ? C15 C10 P1 122.3(2) . . ? C11 C10 P1 119.3(3) . . ? C12 C11 C10 120.6(4) . . ? C13 C12 C11 120.5(4) . . ? C12 C13 C14 119.5(4) . . ? C13 C14 C15 120.4(4) . . ? C14 C15 C10 120.7(3) . . ? C21 C16 C17 118.5(3) . . ? C21 C16 P1 119.9(3) . . ? C17 C16 P1 121.6(3) . . ? C18 C17 C16 120.6(4) . . ? C19 C18 C17 120.2(4) . . ? C20 C19 C18 120.0(3) . . ? C19 C20 C21 120.3(4) . . ? C16 C21 C20 120.4(4) . . ? C23 C22 C27 118.7(4) . . ? C23 C22 P2 122.4(3) . . ? C27 C22 P2 118.8(3) . . ? C22 C23 C24 120.4(4) . . ? C25 C24 C23 120.3(5) . . ? C26 C25 C24 120.0(4) . . ? C25 C26 C27 120.1(4) . . ? C26 C27 C22 120.5(4) . . ? C29 C28 C33 118.0(3) . . ? C29 C28 P2 119.6(3) . . ? C33 C28 P2 122.4(3) . . ? C30 C29 C28 121.0(4) . . ? C31 C30 C29 120.2(4) . . ? C30 C31 C32 119.5(4) . . ? C31 C32 C33 120.7(4) . . ? C32 C33 C28 120.5(4) . . ? C209 B200 C225 109.4(3) . . ? C209 B200 C217 110.9(3) . . ? C225 B200 C217 107.5(2) . . ? C209 B200 C201 109.9(2) . . ? C225 B200 C201 107.5(3) . . ? C217 B200 C201 111.4(3) . . ? C202 C201 C206 115.2(3) . . ? C202 C201 B200 123.2(3) . . ? C206 C201 B200 121.5(3) . . ? C203 C202 C201 122.1(3) . . ? C204 C203 C202 121.5(3) . . ? C204 C203 C207 119.7(3) . . ? C202 C203 C207 118.8(3) . . ? C203 C204 C205 117.4(3) . . ? C206 C205 C204 120.9(3) . . ? C206 C205 C208 119.9(3) . . ? C204 C205 C208 119.2(3) . . ? C205 C206 C201 122.9(3) . . ? F204 C207 F104 121.1(7) . . ? F204 C207 F206 107.3(6) . . ? F104 C207 F206 80.4(7) . . ? F204 C207 F105 78.6(7) . . ? F104 C207 F105 106.9(4) . . ? F206 C207 F105 31.8(8) . . ? F204 C207 F205 105.2(6) . . ? F104 C207 F205 26.4(6) . . ? F206 C207 F205 105.7(6) . . ? F105 C207 F205 127.5(6) . . ? F204 C207 F106 25.7(7) . . ? F104 C207 F106 106.1(4) . . ? F206 C207 F106 128.5(7) . . ? F105 C207 F106 103.2(4) . . ? F205 C207 F106 84.2(7) . . ? F204 C207 C203 115.2(5) . . ? F104 C207 C203 115.0(4) . . ? F206 C207 C203 111.5(5) . . ? F105 C207 C203 113.6(3) . . ? F205 C207 C203 111.4(5) . . ? F106 C207 C203 111.1(4) . . ? F103 C208 F101 105.7(3) . . ? F103 C208 F102 107.4(3) . . ? F101 C208 F102 105.1(3) . . ? F103 C208 C205 112.4(3) . . ? F101 C208 C205 113.4(3) . . ? F102 C208 C205 112.4(3) . . ? C214 C209 C210 115.2(3) . . ? C214 C209 B200 123.3(3) . . ? C210 C209 B200 121.5(3) . . ? C211 C210 C209 122.9(3) . . ? C212 C211 C210 120.5(3) . . ? C212 C211 C215 118.7(3) . . ? C210 C211 C215 120.8(3) . . ? C211 C212 C213 117.9(3) . . ? C212 C213 C214 121.3(3) . . ? C212 C213 C216 119.3(3) . . ? C214 C213 C216 119.3(3) . . ? C209 C214 C213 122.1(3) . . ? F107 C215 F207 122.4(6) . . ? F107 C215 F208 66.7(5) . . ? F207 C215 F208 109.0(5) . . ? F107 C215 F108 108.0(5) . . ? F207 C215 F108 29.8(5) . . ? F208 C215 F108 130.8(5) . . ? F107 C215 F109 108.2(5) . . ? F207 C215 F109 71.3(5) . . ? F208 C215 F109 45.7(4) . . ? F108 C215 F109 100.5(5) . . ? F107 C215 F209 35.3(5) . . ? F207 C215 F209 105.4(5) . . ? F208 C215 F209 101.2(5) . . ? F108 C215 F209 80.5(5) . . ? F109 C215 F209 136.2(5) . . ? F107 C215 C211 117.0(5) . . ? F207 C215 C211 116.4(5) . . ? F208 C215 C211 113.3(4) . . ? F108 C215 C211 111.9(4) . . ? F109 C215 C211 109.8(4) . . ? F209 C215 C211 110.1(4) . . ? F111 C216 F112 106.6(3) . . ? F111 C216 F110 106.4(3) . . ? F112 C216 F110 105.8(3) . . ? F111 C216 C213 112.6(3) . . ? F112 C216 C213 112.1(3) . . ? F110 C216 C213 112.7(3) . . ? C222 C217 C218 115.6(3) . . ? C222 C217 B200 122.1(3) . . ? C218 C217 B200 122.0(3) . . ? C219 C218 C217 122.1(3) . . ? C220 C219 C218 121.1(3) . . ? C220 C219 C223 118.9(3) . . ? C218 C219 C223 120.0(3) . . ? C219 C220 C221 117.9(3) . . ? C220 C221 C222 121.0(3) . . ? C220 C221 C224 119.4(3) . . ? C222 C221 C224 119.7(3) . . ? C221 C222 C217 122.4(3) . . ? F213 C223 F113 131.3(6) . . ? F213 C223 F115 57.4(5) . . ? F113 C223 F115 108.9(5) . . ? F213 C223 F215 106.8(5) . . ? F113 C223 F215 42.3(4) . . ? F115 C223 F215 130.3(5) . . ? F213 C223 F114 48.7(5) . . ? F113 C223 F114 104.5(5) . . ? F115 C223 F114 103.4(5) . . ? F215 C223 F114 64.6(5) . . ? F213 C223 F214 104.6(5) . . ? F113 C223 F214 63.1(5) . . ? F115 C223 F214 51.0(4) . . ? F215 C223 F214 101.5(5) . . ? F114 C223 F214 134.6(5) . . ? F213 C223 C219 115.4(4) . . ? F113 C223 C219 112.5(4) . . ? F115 C223 C219 114.4(4) . . ? F215 C223 C219 114.6(4) . . ? F114 C223 C219 112.4(3) . . ? F214 C223 C219 112.5(4) . . ? F118 C224 F218 127.2(6) . . ? F118 C224 F116 109.9(4) . . ? F218 C224 F116 43.8(5) . . ? F118 C224 F216 47.8(5) . . ? F218 C224 F216 107.6(6) . . ? F116 C224 F216 130.0(5) . . ? F118 C224 F117 104.2(4) . . ? F218 C224 F117 60.0(6) . . ? F116 C224 F117 102.7(4) . . ? F216 C224 F117 58.6(6) . . ? F118 C224 F217 55.9(5) . . ? F218 C224 F217 102.3(6) . . ? F116 C224 F217 62.3(6) . . ? F216 C224 F217 101.3(6) . . ? F117 C224 F217 140.3(5) . . ? F118 C224 C221 115.5(3) . . ? F218 C224 C221 117.3(5) . . ? F116 C224 C221 113.9(4) . . ? F216 C224 C221 116.1(4) . . ? F117 C224 C221 109.4(3) . . ? F217 C224 C221 110.3(4) . . ? C230 C225 C226 116.0(3) . . ? C230 C225 B200 123.1(3) . . ? C226 C225 B200 120.6(3) . . ? C227 C226 C225 122.0(3) . . ? C228 C227 C226 120.7(4) . . ? C228 C227 C231 119.3(4) . . ? C226 C227 C231 120.0(4) . . ? C229 C228 C227 118.6(4) . . ? C228 C229 C230 120.6(4) . . ? C228 C229 C232 119.9(3) . . ? C230 C229 C232 119.5(3) . . ? C229 C230 C225 122.0(3) . . ? F121 C231 F120 108.2(5) . . ? F121 C231 F119 105.4(4) . . ? F120 C231 F119 104.6(5) . . ? F121 C231 C227 112.3(5) . . ? F120 C231 C227 114.4(4) . . ? F119 C231 C227 111.4(4) . . ? F222 C232 F122 128.8(6) . . ? F222 C232 F123 58.8(6) . . ? F122 C232 F123 106.9(4) . . ? F222 C232 F124 44.7(6) . . ? F122 C232 F124 109.3(5) . . ? F123 C232 F124 102.3(4) . . ? F222 C232 F224 105.8(6) . . ? F122 C232 F224 57.5(7) . . ? F123 C232 F224 53.4(7) . . ? F124 C232 F224 134.6(7) . . ? F222 C232 F223 104.0(6) . . ? F122 C232 F223 48.1(6) . . ? F123 C232 F223 134.6(6) . . ? F124 C232 F223 65.6(6) . . ? F224 C232 F223 102.6(6) . . ? F222 C232 C229 116.4(5) . . ? F122 C232 C229 114.4(4) . . ? F123 C232 C229 112.4(4) . . ? F124 C232 C229 110.8(4) . . ? F224 C232 C229 114.0(5) . . ? F223 C232 C229 112.7(5) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.622 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.066