# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound6 _audit_creation_date 13-07-08 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title 053SDP12 _chemical_name_systematic '[Rh(dibpe)Br(C6H5)]2[BArF4]2' _chemical_melting_point 'not measured' _refine_special_details ; Rotational disorder of the CF3 groups of the anion was treated by modelling the fluorine atoms over two sites and restraining their geometry. Vibration restraints were used upon the disordered CH2Cl2 solvent molecules and they were treated separately. The occupancy of both molecules were allowed to refine resulting in occupancies of less than unity presumably due to partial evaporation of solvent from the crystal. The second molecule was disordered over two sites pivoting about one chlorine atom and was restrained to maintain sensible geometries, the atomic displacement parameters of the carbon atoms in each site were set to ride with each other. ; _cell_length_a 13.4344(4) _cell_length_b 16.2486(5) _cell_length_c 16.3500(5) _cell_angle_alpha 73.8487(16) _cell_angle_beta 88.5368(15) _cell_angle_gamma 87.5505(11) _cell_volume 3424.70(18) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Rh -1.1178 0.9187 19.2957 0.7515 14.3501 8.2176 4.7343 25.8749 1.2892 98.6062 5.3280 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C112 H114 B2 Br2 Cl0.50 F48 P4 Rh2 # Dc = 2.81 Fooo = 1543.33 Mu = 19.74 M = 2900.90 # Found Formula = C57.13 H59.27 B1 Br1 Cl2.27 F24 P2 Rh1 # Dc = 1.49 FOOO = 1543.33 Mu = 10.68 M = 1537.98 _chemical_formula_sum 'C57.13 H59.27 B1 Br1 Cl2.27 F24 P2 Rh1' _chemical_formula_moiety 'C57.13 H59.27 B1 Br1 Cl2.27 F24 P2 Rh1' _chemical_compound_source 'Lab S10' _chemical_formula_weight 1537.98 _cell_measurement_reflns_used 14578 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.150 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1543.335 _exptl_absorpt_coefficient_mu 1.068 # Sheldrick geometric approximatio 0.81 0.85 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.85 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 27223 _reflns_number_total 15564 _diffrn_reflns_av_R_equivalents 0.066 # Number of reflections with Friedels Law is 15564 # Theoretical number of reflections is about 20774 _diffrn_reflns_theta_min 5.120 _diffrn_reflns_theta_max 27.507 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.856 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min -19 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 2.63 _oxford_diffrn_Wilson_scale 100.63 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.08 _refine_diff_density_max 0.91 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 10296 _refine_ls_number_restraints 569 _refine_ls_number_parameters 886 _oxford_refine_ls_R_factor_ref 0.0826 _refine_ls_wR_factor_ref 0.1498 _refine_ls_goodness_of_fit_ref 0.9485 _refine_ls_shift/su_max 0.0347177 _refine_ls_shift/su_mean 0.0004073 # The values computed with all filters except I/sigma _oxford_reflns_number_all 10296 _refine_ls_R_factor_all 0.0826 _refine_ls_wR_factor_all 0.1498 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7971 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_gt 0.1369 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.06P)^2^ +16.36P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens F1 F 0.4327(4) 0.9732(3) 0.4225(3) 0.0790 1.0000 Uani . . . . . . F2 F 0.5882(3) 0.9417(3) 0.4385(3) 0.0693 1.0000 Uani . . . . . . F3 F 0.4837(4) 0.8425(3) 0.4708(2) 0.0750 1.0000 Uani . . . . . . F4 F 0.5787(5) 1.1215(3) 0.1267(3) 0.0899 1.0000 Uani . . . . . . F5 F 0.5917(4) 1.0465(3) 0.0388(3) 0.0734 1.0000 Uani . . . . . . F6 F 0.4492(4) 1.0871(3) 0.0719(3) 0.0841 1.0000 Uani . . . . . . F10 F 0.2209(3) 0.8262(4) -0.0309(3) 0.0841 1.0000 Uani . . . . . . F11 F 0.1740(5) 0.9227(4) 0.0261(4) 0.1129 1.0000 Uani . . . . . . F12 F 0.0800(3) 0.8188(4) 0.0317(3) 0.1038 1.0000 Uani . . . . . . F13 F 0.3865(4) 0.4293(3) 0.4130(4) 0.0895 1.0000 Uani . . . . . . F14 F 0.4758(4) 0.3830(3) 0.3254(3) 0.0857 1.0000 Uani . . . . . . F15 F 0.5208(5) 0.3595(3) 0.4542(4) 0.1259 1.0000 Uani . . . . . . F16 F 0.8441(4) 0.5992(4) 0.3599(3) 0.1025 1.0000 Uani . . . . . . F17 F 0.7941(4) 0.5284(3) 0.4819(3) 0.0919 1.0000 Uani . . . . . . F18 F 0.7708(4) 0.6628(3) 0.4428(3) 0.0864 1.0000 Uani . . . . . . F19 F 0.8124(4) 0.8467(4) -0.0062(4) 0.1108 1.0000 Uani . . . . . . F20 F 0.8635(3) 0.7293(4) 0.0717(3) 0.0807 1.0000 Uani . . . . . . F21 F 0.8456(4) 0.7408(5) -0.0595(3) 0.1237 1.0000 Uani . . . . . . C1 C 0.1006(4) 1.0232(4) 0.3197(4) 0.0348 1.0000 Uani . . . . . . C2 C 0.1327(5) 1.0535(4) 0.2356(4) 0.0366 1.0000 Uani . . . . . . C3 C 0.2078(5) 1.0111(5) 0.2022(4) 0.0457 1.0000 Uani . . . . . . C4 C 0.2528(5) 0.9378(5) 0.2519(4) 0.0476 1.0000 Uani . . . . . . C5 C 0.2226(5) 0.9060(5) 0.3349(4) 0.0484 1.0000 Uani . . . . . . C6 C 0.1461(5) 0.9478(4) 0.3694(4) 0.0417 1.0000 Uani . . . . . . C7 C -0.0365(5) 1.2557(4) 0.2233(4) 0.0405 1.0000 Uani . . . . . . C8 C -0.0817(5) 1.1870(4) 0.1884(4) 0.0410 1.0000 Uani . . . . . . C9 C 0.0021(5) 1.2743(4) 0.3916(4) 0.0362 1.0000 Uani . . . . . . C10 C 0.0370(5) 1.3684(4) 0.3724(4) 0.0423 1.0000 Uani . . . . . . C11 C 0.0025(6) 1.4025(5) 0.4461(5) 0.0535 1.0000 Uani . . . . . . C12 C -0.0008(7) 1.4265(5) 0.2896(5) 0.0647 1.0000 Uani . . . . . . C13 C 0.1672(4) 1.2303(4) 0.2856(4) 0.0391 1.0000 Uani . . . . . . C14 C 0.2502(5) 1.1861(4) 0.3466(4) 0.0464 1.0000 Uani . . . . . . C15 C 0.2637(5) 1.2281(5) 0.4174(5) 0.0566 1.0000 Uani . . . . . . C16 C 0.3470(5) 1.1866(6) 0.2955(6) 0.0695 1.0000 Uani . . . . . . C17 C -0.1069(5) 1.0083(4) 0.2125(4) 0.0409 1.0000 Uani . . . . . . C18 C -0.1123(5) 0.9131(4) 0.2575(4) 0.0450 1.0000 Uani . . . . . . C19 C -0.0895(8) 0.8633(6) 0.1905(6) 0.0840 1.0000 Uani . . . . . . C20 C -0.2114(6) 0.8862(5) 0.3007(5) 0.0591 1.0000 Uani . . . . . . C21 C -0.2392(4) 1.0988(4) 0.3008(4) 0.0404 1.0000 Uani . . . . . . C22 C -0.2682(4) 1.1732(4) 0.3388(4) 0.0383 1.0000 Uani . . . . . . C23 C -0.2307(5) 1.1560(4) 0.4279(4) 0.0435 1.0000 Uani . . . . . . C24 C -0.3814(5) 1.1873(5) 0.3367(4) 0.0498 1.0000 Uani . . . . . . C25 C 0.5161(4) 0.8221(4) 0.2234(3) 0.0288 1.0000 Uani . . . . . . C26 C 0.5087(4) 0.8301(4) 0.3073(4) 0.0320 1.0000 Uani . . . . . . C27 C 0.5115(4) 0.9100(4) 0.3239(4) 0.0355 1.0000 Uani . . . . . . C28 C 0.5213(4) 0.9840(4) 0.2587(4) 0.0369 1.0000 Uani . . . . . . C29 C 0.5303(4) 0.9779(4) 0.1762(4) 0.0352 1.0000 Uani . . . . . . C30 C 0.5277(4) 0.8983(4) 0.1588(4) 0.0341 1.0000 Uani . . . . . . C31 C 0.5039(5) 0.9158(4) 0.4134(4) 0.0456 1.0000 Uani . . . . . . C32 C 0.5381(6) 1.0571(4) 0.1048(4) 0.0501 1.0000 Uani . . . . . . C33 C 0.5401(4) 0.6484(4) 0.2788(3) 0.0330 1.0000 Uani . . . . . . C34 C 0.6297(5) 0.6529(4) 0.3178(4) 0.0371 1.0000 Uani . . . . . . C35 C 0.6723(5) 0.5838(4) 0.3786(4) 0.0439 1.0000 Uani . . . . . . C36 C 0.6251(6) 0.5068(4) 0.4036(4) 0.0489 1.0000 Uani . . . . . . C37 C 0.5360(6) 0.4999(4) 0.3653(4) 0.0488 1.0000 Uani . . . . . . C38 C 0.4948(5) 0.5692(4) 0.3032(4) 0.0429 1.0000 Uani . . . . . . C39 C 0.7689(6) 0.5941(5) 0.4148(5) 0.0565 1.0000 Uani . . . . . . C40 C 0.4799(7) 0.4182(5) 0.3896(5) 0.0653 1.0000 Uani . . . . . . C41 C 0.3734(4) 0.7346(4) 0.1986(4) 0.0353 1.0000 Uani . . . . . . C42 C 0.3116(5) 0.7031(4) 0.2699(4) 0.0428 1.0000 Uani . . . . . . C43 C 0.2100(4) 0.7130(4) 0.2665(3) 0.0521 1.0000 Uani D . . . . . C44 C 0.1622(5) 0.7531(5) 0.1907(4) 0.0514 1.0000 Uani . . . . . . C45 C 0.2202(5) 0.7871(4) 0.1193(4) 0.0458 1.0000 Uani . . . . . . C46 C 0.3242(5) 0.7783(4) 0.1241(4) 0.0387 1.0000 Uani . . . . . . C47 C 0.1487(2) 0.6782(2) 0.34523(19) 0.0704 1.0000 Uani D . . . . . C48 C 0.1739(6) 0.8381(6) 0.0371(5) 0.0647 1.0000 Uani . . . . . . C49 C 0.5503(4) 0.7226(4) 0.1153(3) 0.0330 1.0000 Uani . . . . . . C50 C 0.6480(5) 0.7467(4) 0.0944(4) 0.0366 1.0000 Uani . . . . . . C51 C 0.6981(5) 0.7351(4) 0.0228(4) 0.0469 1.0000 Uani . . . . . . C52 C 0.6509(5) 0.6991(5) -0.0326(4) 0.0503 1.0000 Uani . . . . . . C53 C 0.5537(4) 0.6734(4) -0.0130(3) 0.0560 1.0000 Uani D . . . . . C54 C 0.5054(5) 0.6848(4) 0.0584(4) 0.0431 1.0000 Uani . . . . . . C55 C 0.8039(6) 0.7608(6) 0.0072(5) 0.0650 1.0000 Uani . . . . . . C56 C 0.4994(3) 0.6394(3) -0.0744(2) 0.0766 1.0000 Uani D . . . . . P1 P 0.03835(11) 1.20939(10) 0.31978(9) 0.0319 1.0000 Uani . . . . . . P2 P -0.10864(11) 1.08764(10) 0.27174(10) 0.0338 1.0000 Uani . . . . . . Rh1 Rh -0.00692(3) 1.07329(3) 0.38251(3) 0.0296 1.0000 Uani . . . . . . Br1 Br -0.08657(4) 0.93559(4) 0.47740(4) 0.0351 1.0000 Uani . . . . . . Cl100 Cl -0.2927(2) 1.40293(19) 0.2361(2) 0.0791 0.7042 Uani D U . . . . B43 B 0.4954(5) 0.7311(4) 0.2041(4) 0.0344 1.0000 Uani . . . . . . F240 F 0.4063(7) 0.6729(8) -0.0891(9) 0.0845 0.2964 Uani D . . 1 2 . F241 F 0.4604(6) 0.6999(4) -0.1374(4) 0.1055 0.7036 Uani D . . 1 1 . F230 F 0.4239(5) 0.5908(5) -0.0387(3) 0.0825 0.7036 Uani D . . 1 1 . F231 F 0.4900(11) 0.5555(4) -0.0485(6) 0.0928 0.2964 Uani D . . 1 2 . F220 F 0.5572(5) 0.5905(5) -0.1111(5) 0.1005 0.7036 Uani D . . 1 1 . F221 F 0.5436(8) 0.6549(10) -0.1504(5) 0.0865 0.2964 Uani D . . 1 2 . C100 C -0.2764(15) 1.5049(5) 0.1724(12) 0.0808 0.4070 Uani D U . 2 2 . C150 C -0.3053(7) 1.5058(10) 0.171(2) 0.0808 0.2972 Uani D U . 2 1 . Cl150 Cl -0.1904(6) 1.5533(5) 0.1565(7) 0.1010 0.2972 Uani D U . 2 1 . Cl101 Cl -0.1849(5) 1.5030(5) 0.0961(4) 0.1067 0.4070 Uani D U . 2 2 . H21 H 0.1034 1.1039 0.2010 0.0428 1.0000 Uiso R . . . . . H31 H 0.2267 1.0326 0.1457 0.0552 1.0000 Uiso R . . . . . H41 H 0.3028 0.9097 0.2298 0.0560 1.0000 Uiso R . . . . . H51 H 0.2532 0.8566 0.3692 0.0569 1.0000 Uiso R . . . . . H61 H 0.1245 0.9250 0.4263 0.0488 1.0000 Uiso R . . . . . H72 H -0.0914 1.2900 0.2380 0.0478 1.0000 Uiso R . . . . . H71 H 0.0050 1.2914 0.1792 0.0474 1.0000 Uiso R . . . . . H81 H -0.1434 1.2099 0.1613 0.0492 1.0000 Uiso R . . . . . H82 H -0.0376 1.1738 0.1458 0.0490 1.0000 Uiso R . . . . . H92 H -0.0702 1.2775 0.3938 0.0441 1.0000 Uiso R . . . . . H91 H 0.0254 1.2428 0.4475 0.0439 1.0000 Uiso R . . . . . H101 H 0.1104 1.3669 0.3703 0.0497 1.0000 Uiso R . . . . . H113 H 0.0240 1.4604 0.4364 0.0788 1.0000 Uiso R . . . . . H112 H -0.0691 1.4024 0.4509 0.0787 1.0000 Uiso R . . . . . H111 H 0.0303 1.3676 0.4984 0.0789 1.0000 Uiso R . . . . . H121 H 0.0203 1.4850 0.2826 0.0949 1.0000 Uiso R . . . . . H122 H -0.0726 1.4254 0.2891 0.0951 1.0000 Uiso R . . . . . H123 H 0.0266 1.4063 0.2428 0.0949 1.0000 Uiso R . . . . . H132 H 0.1746 1.2915 0.2717 0.0458 1.0000 Uiso R . . . . . H131 H 0.1761 1.2125 0.2345 0.0460 1.0000 Uiso R . . . . . H141 H 0.2329 1.1263 0.3725 0.0549 1.0000 Uiso R . . . . . H152 H 0.3178 1.1992 0.4540 0.0831 1.0000 Uiso R . . . . . H151 H 0.2809 1.2872 0.3923 0.0829 1.0000 Uiso R . . . . . H153 H 0.2030 1.2271 0.4514 0.0828 1.0000 Uiso R . . . . . H163 H 0.4001 1.1624 0.3334 0.1040 1.0000 Uiso R . . . . . H162 H 0.3623 1.2448 0.2653 0.1039 1.0000 Uiso R . . . . . H161 H 0.3405 1.1537 0.2550 0.1039 1.0000 Uiso R . . . . . H172 H -0.1608 1.0237 0.1724 0.0490 1.0000 Uiso R . . . . . H171 H -0.0441 1.0152 0.1812 0.0491 1.0000 Uiso R . . . . . H181 H -0.0614 0.8988 0.3010 0.0550 1.0000 Uiso R . . . . . H191 H -0.0888 0.8024 0.2186 0.1269 1.0000 Uiso R . . . . . H192 H -0.0250 0.8789 0.1641 0.1269 1.0000 Uiso R . . . . . H193 H -0.1407 0.8775 0.1474 0.1271 1.0000 Uiso R . . . . . H203 H -0.2107 0.8247 0.3208 0.0870 1.0000 Uiso R . . . . . H202 H -0.2217 0.9098 0.3476 0.0871 1.0000 Uiso R . . . . . H201 H -0.2646 0.9060 0.2602 0.0868 1.0000 Uiso R . . . . . H212 H -0.2762 1.1071 0.2491 0.0478 1.0000 Uiso R . . . . . H211 H -0.2581 1.0461 0.3414 0.0479 1.0000 Uiso R . . . . . H221 H -0.2383 1.2256 0.3029 0.0460 1.0000 Uiso R . . . . . H231 H -0.2470 1.2044 0.4499 0.0648 1.0000 Uiso R . . . . . H233 H -0.1590 1.1469 0.4287 0.0650 1.0000 Uiso R . . . . . H232 H -0.2603 1.1055 0.4646 0.0648 1.0000 Uiso R . . . . . H241 H -0.3973 1.2350 0.3597 0.0739 1.0000 Uiso R . . . . . H243 H -0.4049 1.2016 0.2799 0.0741 1.0000 Uiso R . . . . . H242 H -0.4123 1.1370 0.3706 0.0739 1.0000 Uiso R . . . . . H261 H 0.5011 0.7808 0.3531 0.0377 1.0000 Uiso R . . . . . H281 H 0.5231 1.0371 0.2700 0.0445 1.0000 Uiso R . . . . . H301 H 0.5331 0.8963 0.1030 0.0409 1.0000 Uiso R . . . . . H341 H 0.6627 0.7039 0.3022 0.0438 1.0000 Uiso R . . . . . H361 H 0.6528 0.4611 0.4452 0.0589 1.0000 Uiso R . . . . . H381 H 0.4360 0.5630 0.2784 0.0509 1.0000 Uiso R . . . . . H421 H 0.3410 0.6749 0.3214 0.0498 1.0000 Uiso R . . . . . H441 H 0.0932 0.7570 0.1880 0.0596 1.0000 Uiso R . . . . . H461 H 0.3613 0.8036 0.0746 0.0447 1.0000 Uiso R . . . . . H501 H 0.6819 0.7704 0.1302 0.0438 1.0000 Uiso R . . . . . H521 H 0.6840 0.6910 -0.0807 0.0595 1.0000 Uiso R . . . . . H541 H 0.4408 0.6657 0.0703 0.0515 1.0000 Uiso R . . . . . H1001 H -0.2626 1.5427 0.2068 0.1329 0.4070 Uiso R . . 2 2 . H1002 H -0.3396 1.5214 0.1444 0.1329 0.4070 Uiso R . . 2 2 . H1502 H -0.3540 1.5409 0.1914 0.1330 0.2972 Uiso R . . 2 1 . H1501 H -0.3235 1.5028 0.1149 0.1330 0.2972 Uiso R . . 2 1 . C200 C -0.2258(7) 1.4484(19) -0.1023(9) 0.1441 0.4308 Uani D U . . . . Cl200 Cl -0.1003(6) 1.4198(6) -0.0838(6) 0.1474 0.4308 Uani D U . . . . Cl201 Cl -0.2528(6) 1.5163(6) -0.2027(6) 0.1414 0.4308 Uani D U . . . . F80 F 0.0627(4) 0.7224(4) 0.3471(3) 0.0997 0.8483 Uani D . . 3 2 . F81 F 0.1271(18) 0.7351(6) 0.3883(10) 0.0791 0.1517 Uani D . . 3 1 . F90 F 0.0609(10) 0.6504(17) 0.3302(3) 0.0683 0.1517 Uani D . . 3 1 . F91 F 0.1233(5) 0.5981(3) 0.3561(3) 0.0931 0.8483 Uani D . . 3 2 . F70 F 0.1946(4) 0.6777(4) 0.4167(3) 0.0750 0.8483 Uani D . . 3 2 . F71 F 0.1926(10) 0.6119(12) 0.4011(8) 0.0872 0.1517 Uani D . . 3 1 . H2001 H -0.2509 1.4750 -0.0603 0.1379 0.4308 Uiso R . . . . . H2002 H -0.2603 1.3970 -0.0982 0.1380 0.4308 Uiso 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 F1 0.084(3) 0.101(4) 0.063(3) -0.046(3) 0.002(2) 0.034(3) F2 0.075(3) 0.095(3) 0.047(2) -0.032(2) -0.006(2) -0.018(3) F3 0.131(4) 0.057(3) 0.038(2) -0.014(2) 0.021(2) -0.024(3) F4 0.171(5) 0.043(3) 0.054(3) -0.004(2) -0.017(3) -0.041(3) F5 0.108(4) 0.053(3) 0.051(3) -0.001(2) 0.019(2) -0.018(3) F6 0.090(4) 0.068(3) 0.071(3) 0.018(2) -0.021(3) 0.012(3) F10 0.059(3) 0.146(5) 0.042(2) -0.019(3) -0.008(2) 0.008(3) F11 0.164(6) 0.080(4) 0.085(4) -0.007(3) -0.054(4) 0.031(4) F12 0.045(3) 0.187(6) 0.068(3) -0.017(3) -0.015(2) -0.006(3) F13 0.100(4) 0.054(3) 0.115(4) -0.024(3) 0.045(3) -0.031(3) F14 0.109(4) 0.052(3) 0.106(4) -0.037(3) 0.017(3) -0.026(3) F15 0.172(6) 0.045(3) 0.130(5) 0.037(3) -0.051(4) -0.035(3) F16 0.054(3) 0.172(6) 0.088(4) -0.048(4) 0.002(3) -0.004(3) F17 0.086(4) 0.070(3) 0.100(4) 0.012(3) -0.046(3) 0.004(3) F18 0.087(4) 0.063(3) 0.122(4) -0.045(3) -0.055(3) 0.018(3) F19 0.085(4) 0.110(5) 0.121(5) -0.004(4) 0.019(3) -0.035(4) F20 0.051(3) 0.125(4) 0.069(3) -0.030(3) 0.006(2) -0.015(3) F21 0.067(3) 0.256(8) 0.075(3) -0.090(4) 0.030(3) -0.033(4) C1 0.032(3) 0.038(4) 0.040(3) -0.018(3) 0.001(3) -0.005(3) C2 0.041(4) 0.031(3) 0.038(3) -0.008(3) -0.002(3) -0.002(3) C3 0.039(4) 0.061(5) 0.041(4) -0.020(3) 0.009(3) -0.004(3) C4 0.039(4) 0.059(5) 0.055(4) -0.033(4) 0.003(3) 0.006(3) C5 0.042(4) 0.052(4) 0.056(4) -0.024(3) -0.006(3) 0.010(3) C6 0.039(4) 0.043(4) 0.045(4) -0.017(3) -0.004(3) 0.006(3) C7 0.038(4) 0.042(4) 0.036(3) -0.003(3) -0.005(3) -0.004(3) C8 0.040(4) 0.047(4) 0.034(3) -0.008(3) -0.008(3) 0.007(3) C9 0.036(3) 0.033(3) 0.040(3) -0.009(3) -0.001(3) -0.001(3) C10 0.042(4) 0.036(4) 0.049(4) -0.011(3) 0.002(3) -0.006(3) C11 0.058(5) 0.045(4) 0.063(5) -0.023(4) 0.005(4) -0.005(3) C12 0.089(6) 0.039(4) 0.063(5) -0.007(4) -0.016(4) -0.011(4) C13 0.032(3) 0.040(4) 0.047(4) -0.014(3) 0.004(3) -0.010(3) C14 0.038(4) 0.046(4) 0.053(4) -0.010(3) 0.000(3) -0.009(3) C15 0.049(4) 0.054(5) 0.066(5) -0.013(4) -0.010(4) -0.009(4) C16 0.030(4) 0.080(6) 0.099(6) -0.026(5) 0.011(4) -0.004(4) C17 0.034(3) 0.049(4) 0.046(4) -0.023(3) -0.005(3) -0.002(3) C18 0.038(4) 0.049(4) 0.056(4) -0.027(3) -0.011(3) 0.004(3) C19 0.102(7) 0.069(6) 0.098(7) -0.053(5) 0.006(6) 0.002(5) C20 0.056(5) 0.050(5) 0.071(5) -0.016(4) -0.006(4) -0.004(4) C21 0.035(4) 0.043(4) 0.045(4) -0.015(3) -0.005(3) 0.001(3) C22 0.036(3) 0.032(3) 0.044(4) -0.007(3) 0.001(3) 0.003(3) C23 0.037(4) 0.050(4) 0.047(4) -0.018(3) -0.001(3) -0.006(3) C24 0.036(4) 0.059(5) 0.050(4) -0.010(3) 0.001(3) 0.007(3) C25 0.023(3) 0.032(3) 0.031(3) -0.009(2) -0.003(2) 0.000(2) C26 0.026(3) 0.032(3) 0.035(3) -0.003(3) -0.003(2) -0.002(2) C27 0.034(3) 0.039(4) 0.036(3) -0.014(3) 0.000(3) 0.003(3) C28 0.040(4) 0.032(3) 0.042(4) -0.015(3) 0.000(3) -0.003(3) C29 0.036(3) 0.031(3) 0.038(3) -0.008(3) -0.009(3) -0.001(3) C30 0.043(4) 0.032(3) 0.026(3) -0.006(3) -0.004(3) 0.002(3) C31 0.049(4) 0.048(4) 0.043(4) -0.019(3) 0.002(3) 0.000(3) C32 0.079(5) 0.031(4) 0.041(4) -0.010(3) -0.008(4) -0.007(4) C33 0.039(3) 0.031(3) 0.030(3) -0.010(2) 0.001(3) -0.004(3) C34 0.048(4) 0.029(3) 0.035(3) -0.010(3) 0.004(3) 0.000(3) C35 0.049(4) 0.043(4) 0.042(4) -0.015(3) 0.000(3) 0.003(3) C36 0.071(5) 0.027(4) 0.044(4) -0.005(3) 0.000(3) 0.011(3) C37 0.066(5) 0.030(4) 0.049(4) -0.008(3) 0.005(4) -0.003(3) C38 0.048(4) 0.036(4) 0.045(4) -0.011(3) 0.000(3) -0.003(3) C39 0.062(5) 0.049(5) 0.054(4) -0.008(4) -0.015(4) 0.009(4) C40 0.093(7) 0.029(4) 0.073(5) -0.012(4) 0.006(5) -0.010(4) C41 0.037(3) 0.034(3) 0.036(3) -0.011(3) -0.002(3) -0.004(3) C42 0.043(4) 0.040(4) 0.046(4) -0.012(3) -0.001(3) -0.005(3) C43 0.048(4) 0.056(4) 0.051(3) -0.012(3) 0.007(3) -0.012(3) C44 0.029(4) 0.068(5) 0.058(4) -0.016(4) -0.003(3) -0.016(3) C45 0.039(4) 0.051(4) 0.047(4) -0.012(3) -0.002(3) -0.010(3) C46 0.044(4) 0.041(4) 0.032(3) -0.011(3) 0.002(3) -0.009(3) C47 0.060(3) 0.077(3) 0.064(3) -0.004(3) 0.012(3) -0.014(3) C48 0.041(5) 0.103(7) 0.049(5) -0.017(4) -0.013(3) 0.002(4) C49 0.039(4) 0.026(3) 0.032(3) -0.004(2) -0.006(3) 0.000(3) C50 0.045(4) 0.033(3) 0.031(3) -0.006(3) -0.003(3) 0.000(3) C51 0.055(4) 0.050(4) 0.031(3) -0.004(3) 0.005(3) -0.001(3) C52 0.062(5) 0.058(5) 0.031(3) -0.014(3) 0.007(3) 0.001(4) C53 0.087(5) 0.048(4) 0.039(3) -0.021(3) 0.001(3) -0.004(3) C54 0.046(4) 0.042(4) 0.043(4) -0.015(3) -0.002(3) -0.003(3) C55 0.059(5) 0.081(6) 0.050(5) -0.010(4) 0.018(4) -0.005(5) C56 0.113(4) 0.071(3) 0.054(3) -0.028(3) -0.007(3) -0.016(3) P1 0.0314(8) 0.0325(9) 0.0312(8) -0.0072(6) -0.0014(6) -0.0039(7) P2 0.0295(8) 0.0377(9) 0.0350(8) -0.0110(7) -0.0022(6) -0.0029(7) Rh1 0.0286(3) 0.0298(3) 0.0304(3) -0.00834(19) -0.00055(18) -0.00262(19) Br1 0.0362(4) 0.0335(3) 0.0351(3) -0.0072(3) -0.0042(2) -0.0083(3) Cl100 0.0691(19) 0.0602(18) 0.100(2) -0.0089(16) 0.0056(16) -0.0044(15) B43 0.036(4) 0.032(4) 0.036(4) -0.011(3) -0.002(3) -0.004(3) F240 0.113(7) 0.088(8) 0.063(7) -0.033(6) -0.017(7) -0.023(6) F241 0.169(6) 0.068(4) 0.072(4) 0.002(3) -0.068(4) -0.030(5) F230 0.106(5) 0.098(5) 0.055(4) -0.034(3) 0.000(3) -0.040(4) F231 0.141(9) 0.069(6) 0.074(7) -0.023(6) -0.026(7) -0.027(7) F220 0.136(6) 0.099(5) 0.091(5) -0.066(4) 0.001(4) -0.009(4) F221 0.130(8) 0.090(8) 0.048(6) -0.029(6) 0.000(6) -0.027(7) C100 0.078(4) 0.064(3) 0.090(5) -0.005(3) -0.007(4) 0.001(3) C150 0.078(4) 0.064(3) 0.090(5) -0.005(3) -0.007(4) 0.001(3) Cl150 0.085(5) 0.062(4) 0.127(6) 0.025(4) -0.017(5) -0.004(3) Cl101 0.101(4) 0.109(5) 0.085(4) 0.013(3) 0.006(3) 0.006(4) C200 0.114(5) 0.141(6) 0.184(6) -0.055(5) 0.019(5) -0.025(4) Cl200 0.119(5) 0.146(6) 0.183(6) -0.054(5) 0.016(4) -0.021(4) Cl201 0.106(4) 0.138(5) 0.186(6) -0.053(5) 0.018(4) -0.026(4) F80 0.068(4) 0.117(5) 0.083(4) 0.017(3) 0.032(3) 0.022(3) F81 0.074(9) 0.081(8) 0.074(8) -0.009(6) 0.021(8) -0.015(8) F90 0.054(7) 0.070(9) 0.068(8) 0.001(8) 0.016(7) -0.015(7) F91 0.115(4) 0.078(4) 0.080(4) -0.006(3) 0.026(3) -0.051(4) F70 0.070(3) 0.099(4) 0.051(3) -0.012(3) 0.017(2) -0.024(3) F71 0.069(8) 0.089(8) 0.079(8) 0.016(8) 0.019(8) -0.009(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.15277(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag F1 . C31 . 1.342(7) yes F2 . C31 . 1.338(8) yes F3 . C31 . 1.329(8) yes F4 . C32 . 1.338(8) yes F5 . C32 . 1.330(8) yes F6 . C32 . 1.338(8) yes F10 . C48 . 1.322(9) yes F11 . C48 . 1.335(10) yes F12 . C48 . 1.324(9) yes F13 . C40 . 1.322(10) yes F14 . C40 . 1.330(9) yes F15 . C40 . 1.324(9) yes F16 . C39 . 1.324(9) yes F17 . C39 . 1.340(8) yes F18 . C39 . 1.321(8) yes F19 . C55 . 1.361(10) yes F20 . C55 . 1.313(9) yes F21 . C55 . 1.326(9) yes C1 . C2 . 1.389(8) yes C1 . C6 . 1.393(9) yes C1 . Rh1 . 2.023(6) yes C2 . C3 . 1.382(8) yes C2 . H21 . 0.934 no C3 . C4 . 1.367(9) yes C3 . H31 . 0.926 no C4 . C5 . 1.369(9) yes C4 . H41 . 0.919 no C5 . C6 . 1.399(9) yes C5 . H51 . 0.928 no C6 . H61 . 0.944 no C7 . C8 . 1.539(9) yes C7 . P1 . 1.850(6) yes C7 . H72 . 0.972 no C7 . H71 . 0.971 no C8 . P2 . 1.843(6) yes C8 . H81 . 0.960 no C8 . H82 . 0.966 no C9 . C10 . 1.562(8) yes C9 . P1 . 1.829(6) yes C9 . H92 . 0.970 no C9 . H91 . 0.967 no C10 . C11 . 1.516(9) yes C10 . C12 . 1.506(9) yes C10 . H101 . 0.985 no C11 . H113 . 0.964 no C11 . H112 . 0.963 no C11 . H111 . 0.959 no C12 . H121 . 0.978 no C12 . H122 . 0.966 no C12 . H123 . 0.971 no C13 . C14 . 1.530(9) yes C13 . P1 . 1.822(6) yes C13 . H132 . 0.965 no C13 . H131 . 0.960 no C14 . C15 . 1.518(9) yes C14 . C16 . 1.526(9) yes C14 . H141 . 0.981 no C15 . H152 . 0.972 no C15 . H151 . 0.969 no C15 . H153 . 0.974 no C16 . H163 . 0.955 no C16 . H162 . 0.966 no C16 . H161 . 0.967 no C17 . C18 . 1.520(9) yes C17 . P2 . 1.815(6) yes C17 . H172 . 0.966 no C17 . H171 . 0.970 no C18 . C19 . 1.550(9) yes C18 . C20 . 1.514(10) yes C18 . H181 . 0.973 no C19 . H191 . 0.968 no C19 . H192 . 0.970 no C19 . H193 . 0.971 no C20 . H203 . 0.960 no C20 . H202 . 0.953 no C20 . H201 . 0.968 no C21 . C22 . 1.537(8) yes C21 . P2 . 1.821(6) yes C21 . H212 . 0.966 no C21 . H211 . 0.965 no C22 . C23 . 1.501(9) yes C22 . C24 . 1.529(8) yes C22 . H221 . 0.984 no C23 . H231 . 0.967 no C23 . H233 . 0.968 no C23 . H232 . 0.966 no C24 . H241 . 0.964 no C24 . H243 . 0.952 no C24 . H242 . 0.956 no C25 . C26 . 1.414(8) yes C25 . C30 . 1.397(8) yes C25 . B43 . 1.633(8) yes C26 . C27 . 1.400(8) yes C26 . H261 . 0.939 no C27 . C28 . 1.376(8) yes C27 . C31 . 1.492(8) yes C28 . C29 . 1.383(8) yes C28 . H281 . 0.933 no C29 . C30 . 1.402(8) yes C29 . C32 . 1.482(9) yes C30 . H301 . 0.923 no C33 . C34 . 1.390(9) yes C33 . C38 . 1.399(9) yes C33 . B43 . 1.647(9) yes C34 . C35 . 1.389(9) yes C34 . H341 . 0.925 no C35 . C36 . 1.381(9) yes C35 . C39 . 1.473(10) yes C36 . C37 . 1.388(10) yes C36 . H361 . 0.928 no C37 . C38 . 1.393(9) yes C37 . C40 . 1.505(10) yes C38 . H381 . 0.920 no C41 . C42 . 1.401(8) yes C41 . C46 . 1.394(8) yes C41 . B43 . 1.642(9) yes C42 . C43 . 1.369(8) yes C42 . H421 . 0.929 no C43 . C44 . 1.388(8) yes C43 . C47 . 1.495(4) yes C44 . C45 . 1.381(9) yes C44 . H441 . 0.928 no C45 . C46 . 1.400(9) yes C45 . C48 . 1.503(10) yes C46 . H461 . 0.940 no C47 . F81 . 1.328(6) yes C47 . F90 . 1.334(6) yes C47 . F71 . 1.330(6) yes C47 . F80 . 1.339(4) yes C47 . F91 . 1.322(4) yes C47 . F70 . 1.332(4) yes C49 . C50 . 1.393(8) yes C49 . C54 . 1.410(8) yes C49 . B43 . 1.648(9) yes C50 . C51 . 1.389(8) yes C50 . H501 . 0.923 no C51 . C52 . 1.386(10) yes C51 . C55 . 1.494(11) yes C52 . C53 . 1.390(9) yes C52 . H521 . 0.933 no C53 . C54 . 1.374(8) yes C53 . C56 . 1.493(4) yes C54 . H541 . 0.932 no C56 . F241 . 1.313(5) yes C56 . F230 . 1.331(5) yes C56 . F220 . 1.335(5) yes C56 . F240 . 1.343(6) yes C56 . F231 . 1.321(6) yes C56 . F221 . 1.327(5) yes P1 . Rh1 . 2.2658(16) yes P2 . Rh1 . 2.2508(16) yes Rh1 . Br1 2_576 2.6062(7) yes Rh1 . Br1 . 2.5974(7) yes Cl100 . C150 . 1.718(8) yes Cl100 . C100 . 1.714(8) yes C100 . Cl101 . 1.734(8) yes C100 . H1001 . 0.967 no C100 . H1002 . 0.966 no C150 . Cl150 . 1.738(8) yes C150 . H1502 . 0.964 no C150 . H1501 . 0.969 no C200 . Cl200 . 1.740(7) yes C200 . Cl201 . 1.742(7) yes C200 . H2001 . 0.955 no C200 . H2002 . 0.959 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . C1 . C6 . 117.6(5) yes C2 . C1 . Rh1 . 128.8(5) yes C6 . C1 . Rh1 . 113.6(4) yes C1 . C2 . C3 . 121.5(6) yes C1 . C2 . H21 . 119.2 no C3 . C2 . H21 . 119.3 no C2 . C3 . C4 . 120.3(6) yes C2 . C3 . H31 . 119.2 no C4 . C3 . H31 . 120.5 no C3 . C4 . C5 . 119.7(6) yes C3 . C4 . H41 . 120.3 no C5 . C4 . H41 . 120.0 no C4 . C5 . C6 . 120.6(6) yes C4 . C5 . H51 . 120.1 no C6 . C5 . H51 . 119.3 no C5 . C6 . C1 . 120.2(6) yes C5 . C6 . H61 . 120.3 no C1 . C6 . H61 . 119.4 no C8 . C7 . P1 . 112.9(4) yes C8 . C7 . H72 . 107.4 no P1 . C7 . H72 . 108.3 no C8 . C7 . H71 . 108.9 no P1 . C7 . H71 . 109.4 no H72 . C7 . H71 . 109.9 no C7 . C8 . P2 . 113.3(4) yes C7 . C8 . H81 . 108.4 no P2 . C8 . H81 . 107.7 no C7 . C8 . H82 . 109.9 no P2 . C8 . H82 . 109.6 no H81 . C8 . H82 . 107.9 no C10 . C9 . P1 . 120.0(4) yes C10 . C9 . H92 . 106.6 no P1 . C9 . H92 . 107.1 no C10 . C9 . H91 . 108.1 no P1 . C9 . H91 . 106.5 no H92 . C9 . H91 . 108.1 no C9 . C10 . C11 . 107.6(5) yes C9 . C10 . C12 . 113.7(5) yes C11 . C10 . C12 . 110.4(6) yes C9 . C10 . H101 . 108.1 no C11 . C10 . H101 . 108.4 no C12 . C10 . H101 . 108.4 no C10 . C11 . H113 . 109.5 no C10 . C11 . H112 . 109.9 no H113 . C11 . H112 . 109.2 no C10 . C11 . H111 . 110.3 no H113 . C11 . H111 . 109.0 no H112 . C11 . H111 . 109.0 no C10 . C12 . H121 . 109.9 no C10 . C12 . H122 . 109.4 no H121 . C12 . H122 . 110.3 no C10 . C12 . H123 . 109.2 no H121 . C12 . H123 . 108.9 no H122 . C12 . H123 . 109.1 no C14 . C13 . P1 . 118.4(4) yes C14 . C13 . H132 . 108.6 no P1 . C13 . H132 . 107.3 no C14 . C13 . H131 . 107.5 no P1 . C13 . H131 . 106.0 no H132 . C13 . H131 . 108.7 no C13 . C14 . C15 . 112.5(6) yes C13 . C14 . C16 . 108.8(6) yes C15 . C14 . C16 . 110.4(6) yes C13 . C14 . H141 . 108.4 no C15 . C14 . H141 . 108.3 no C16 . C14 . H141 . 108.4 no C14 . C15 . H152 . 110.2 no C14 . C15 . H151 . 108.7 no H152 . C15 . H151 . 108.2 no C14 . C15 . H153 . 111.4 no H152 . C15 . H153 . 109.4 no H151 . C15 . H153 . 108.9 no C14 . C16 . H163 . 109.4 no C14 . C16 . H162 . 109.8 no H163 . C16 . H162 . 108.7 no C14 . C16 . H161 . 110.1 no H163 . C16 . H161 . 109.6 no H162 . C16 . H161 . 109.2 no C18 . C17 . P2 . 121.4(4) yes C18 . C17 . H172 . 107.8 no P2 . C17 . H172 . 107.3 no C18 . C17 . H171 . 106.0 no P2 . C17 . H171 . 105.0 no H172 . C17 . H171 . 108.9 no C17 . C18 . C19 . 107.8(6) yes C17 . C18 . C20 . 114.7(6) yes C19 . C18 . C20 . 109.1(6) yes C17 . C18 . H181 . 107.6 no C19 . C18 . H181 . 109.8 no C20 . C18 . H181 . 107.8 no C18 . C19 . H191 . 109.0 no C18 . C19 . H192 . 109.4 no H191 . C19 . H192 . 109.7 no C18 . C19 . H193 . 109.6 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.7 no C18 . C20 . H203 . 108.7 no C18 . C20 . H202 . 110.0 no H203 . C20 . H202 . 109.5 no C18 . C20 . H201 . 109.6 no H203 . C20 . H201 . 109.3 no H202 . C20 . H201 . 109.7 no C22 . C21 . P2 . 116.8(4) yes C22 . C21 . H212 . 107.9 no P2 . C21 . H212 . 106.1 no C22 . C21 . H211 . 108.0 no P2 . C21 . H211 . 108.4 no H212 . C21 . H211 . 109.4 no C21 . C22 . C23 . 111.2(5) yes C21 . C22 . C24 . 109.1(5) yes C23 . C22 . C24 . 110.9(5) yes C21 . C22 . H221 . 108.4 no C23 . C22 . H221 . 108.9 no C24 . C22 . H221 . 108.2 no C22 . C23 . H231 . 110.2 no C22 . C23 . H233 . 110.3 no H231 . C23 . H233 . 108.2 no C22 . C23 . H232 . 110.4 no H231 . C23 . H232 . 109.1 no H233 . C23 . H232 . 108.7 no C22 . C24 . H241 . 107.3 no C22 . C24 . H243 . 111.0 no H241 . C24 . H243 . 108.3 no C22 . C24 . H242 . 109.9 no H241 . C24 . H242 . 110.1 no H243 . C24 . H242 . 110.2 no C26 . C25 . C30 . 116.0(5) yes C26 . C25 . B43 . 120.7(5) yes C30 . C25 . B43 . 122.7(5) yes C25 . C26 . C27 . 121.6(5) yes C25 . C26 . H261 . 119.4 no C27 . C26 . H261 . 119.0 no C26 . C27 . C28 . 121.0(5) yes C26 . C27 . C31 . 120.1(5) yes C28 . C27 . C31 . 118.9(5) yes C27 . C28 . C29 . 118.6(6) yes C27 . C28 . H281 . 120.8 no C29 . C28 . H281 . 120.6 no C28 . C29 . C30 . 120.9(5) yes C28 . C29 . C32 . 119.5(5) yes C30 . C29 . C32 . 119.6(5) yes C29 . C30 . C25 . 121.9(5) yes C29 . C30 . H301 . 118.9 no C25 . C30 . H301 . 119.2 no C27 . C31 . F1 . 111.8(5) yes C27 . C31 . F2 . 112.1(5) yes F1 . C31 . F2 . 105.6(5) yes C27 . C31 . F3 . 114.5(5) yes F1 . C31 . F3 . 106.3(5) yes F2 . C31 . F3 . 105.9(6) yes C29 . C32 . F6 . 112.2(6) yes C29 . C32 . F4 . 113.6(5) yes F6 . C32 . F4 . 106.3(6) yes C29 . C32 . F5 . 113.9(6) yes F6 . C32 . F5 . 104.3(5) yes F4 . C32 . F5 . 105.8(6) yes C34 . C33 . C38 . 116.1(6) yes C34 . C33 . B43 . 120.8(5) yes C38 . C33 . B43 . 123.0(5) yes C33 . C34 . C35 . 122.9(6) yes C33 . C34 . H341 . 118.6 no C35 . C34 . H341 . 118.5 no C34 . C35 . C36 . 120.1(6) yes C34 . C35 . C39 . 118.9(6) yes C36 . C35 . C39 . 121.0(6) yes C35 . C36 . C37 . 118.5(6) yes C35 . C36 . H361 . 120.1 no C37 . C36 . H361 . 121.4 no C36 . C37 . C38 . 120.9(6) yes C36 . C37 . C40 . 121.5(7) yes C38 . C37 . C40 . 117.6(7) yes C33 . C38 . C37 . 121.5(6) yes C33 . C38 . H381 . 119.2 no C37 . C38 . H381 . 119.3 no C35 . C39 . F17 . 112.9(7) yes C35 . C39 . F16 . 113.1(6) yes F17 . C39 . F16 . 105.1(6) yes C35 . C39 . F18 . 113.4(6) yes F17 . C39 . F18 . 104.9(6) yes F16 . C39 . F18 . 106.7(7) yes C37 . C40 . F14 . 112.0(7) yes C37 . C40 . F15 . 112.5(7) yes F14 . C40 . F15 . 106.8(7) yes C37 . C40 . F13 . 113.1(6) yes F14 . C40 . F13 . 106.0(7) yes F15 . C40 . F13 . 105.8(7) yes C42 . C41 . C46 . 115.3(6) yes C42 . C41 . B43 . 122.7(5) yes C46 . C41 . B43 . 121.5(5) yes C41 . C42 . C43 . 122.5(6) yes C41 . C42 . H421 . 118.6 no C43 . C42 . H421 . 118.9 no C42 . C43 . C44 . 121.2(5) yes C42 . C43 . C47 . 119.6(4) yes C44 . C43 . C47 . 119.1(4) yes C43 . C44 . C45 . 118.2(6) yes C43 . C44 . H441 . 121.0 no C45 . C44 . H441 . 120.8 no C44 . C45 . C46 . 119.9(6) yes C44 . C45 . C48 . 121.1(6) yes C46 . C45 . C48 . 118.9(6) yes C45 . C46 . C41 . 122.7(6) yes C45 . C46 . H461 . 117.6 no C41 . C46 . H461 . 119.8 no C43 . C47 . F81 . 113.59(5) yes C43 . C47 . F90 . 113.56(5) yes F81 . C47 . F90 . 105.07(5) yes C43 . C47 . F71 . 113.58(5) yes F81 . C47 . F71 . 105.08(5) yes F90 . C47 . F71 . 105.07(5) yes C43 . C47 . F80 . 113.57(5) yes C43 . C47 . F91 . 113.56(5) yes F80 . C47 . F91 . 105.12(5) yes C43 . C47 . F70 . 113.58(5) yes F80 . C47 . F70 . 105.05(5) yes F91 . C47 . F70 . 105.06(5) yes C45 . C48 . F11 . 113.3(7) yes C45 . C48 . F12 . 112.1(7) yes F11 . C48 . F12 . 106.5(7) yes C45 . C48 . F10 . 113.1(7) yes F11 . C48 . F10 . 104.7(7) yes F12 . C48 . F10 . 106.6(6) yes C50 . C49 . C54 . 114.9(5) yes C50 . C49 . B43 . 122.0(5) yes C54 . C49 . B43 . 123.0(5) yes C49 . C50 . C51 . 123.1(6) yes C49 . C50 . H501 . 118.9 no C51 . C50 . H501 . 118.0 no C50 . C51 . C52 . 120.4(6) yes C50 . C51 . C55 . 119.1(6) yes C52 . C51 . C55 . 120.5(6) yes C51 . C52 . C53 . 118.0(6) yes C51 . C52 . H521 . 121.0 no C53 . C52 . H521 . 121.0 no C52 . C53 . C54 . 120.9(5) yes C52 . C53 . C56 . 118.9(4) yes C54 . C53 . C56 . 120.0(4) yes C49 . C54 . C53 . 122.7(6) yes C49 . C54 . H541 . 118.5 no C53 . C54 . H541 . 118.8 no C51 . C55 . F19 . 111.8(7) yes C51 . C55 . F21 . 113.3(7) yes F19 . C55 . F21 . 107.0(7) yes C51 . C55 . F20 . 115.1(6) yes F19 . C55 . F20 . 101.9(7) yes F21 . C55 . F20 . 106.8(7) yes C53 . C56 . F241 . 113.20(5) yes C53 . C56 . F230 . 113.23(5) yes F241 . C56 . F230 . 105.53(5) yes C53 . C56 . F220 . 113.18(5) yes F241 . C56 . F220 . 105.50(5) yes F230 . C56 . F220 . 105.45(5) yes C53 . C56 . F240 . 113.18(5) yes C53 . C56 . F231 . 113.22(5) yes F240 . C56 . F231 . 105.50(5) yes C53 . C56 . F221 . 113.22(5) yes F240 . C56 . F221 . 105.48(5) yes F231 . C56 . F221 . 105.51(5) yes C7 . P1 . C9 . 104.7(3) yes C7 . P1 . C13 . 105.2(3) yes C9 . P1 . C13 . 108.6(3) yes C7 . P1 . Rh1 . 109.7(2) yes C9 . P1 . Rh1 . 107.8(2) yes C13 . P1 . Rh1 . 119.9(2) yes C8 . P2 . C21 . 105.5(3) yes C8 . P2 . C17 . 102.6(3) yes C21 . P2 . C17 . 104.3(3) yes C8 . P2 . Rh1 . 109.6(2) yes C21 . P2 . Rh1 . 112.3(2) yes C17 . P2 . Rh1 . 121.2(2) yes Br1 2_576 Rh1 . C1 . 99.84(17) yes Br1 2_576 Rh1 . P1 . 93.27(4) yes C1 . Rh1 . P1 . 92.58(18) yes Br1 2_576 Rh1 . P2 . 171.02(5) yes C1 . Rh1 . P2 . 89.09(17) yes P1 . Rh1 . P2 . 87.23(6) yes Br1 2_576 Rh1 . Br1 . 82.20(2) yes C1 . Rh1 . Br1 . 101.47(17) yes P1 . Rh1 . Br1 . 165.77(4) yes P2 . Rh1 . Br1 . 95.16(5) yes Rh1 2_576 Br1 . Rh1 . 97.80(2) yes C49 . B43 . C33 . 104.9(5) yes C49 . B43 . C41 . 112.5(5) yes C33 . B43 . C41 . 113.4(5) yes C49 . B43 . C25 . 112.4(5) yes C33 . B43 . C25 . 112.1(5) yes C41 . B43 . C25 . 101.8(5) yes Cl100 . C100 . Cl101 . 109.63(10) yes Cl100 . C100 . H1001 . 110.1 no Cl101 . C100 . H1001 . 113.5 no Cl100 . C100 . H1002 . 104.2 no Cl101 . C100 . H1002 . 108.9 no H1001 . C100 . H1002 . 110.1 no Cl100 . C150 . Cl150 . 109.66(10) yes Cl100 . C150 . H1502 . 113.4 no Cl150 . C150 . H1502 . 110.3 no Cl100 . C150 . H1501 . 108.2 no Cl150 . C150 . H1501 . 105.1 no H1502 . C150 . H1501 . 109.9 no Cl200 . C200 . Cl201 . 115.45(7) yes Cl200 . C200 . H2001 . 109.3 no Cl201 . C200 . H2001 . 108.6 no Cl200 . C200 . H2002 . 107.6 no Cl201 . C200 . H2002 . 105.6 no H2001 . C200 . H2002 . 110.2 no _iucr_refine_instruction_details_constraints ; # # Punched on 08/07/13 at 11:00:48 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C(100,U'S) C(150,U'S) RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 72,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) RIDE C ( 9,X'S) H ( 92,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 113,X'S) H ( 112,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) H ( 122,X'S) H ( 123,X'S) RIDE C ( 13,X'S) H ( 132,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 152,X'S) H ( 151,X'S) H ( 153,X'S) RIDE C ( 16,X'S) H ( 163,X'S) H ( 162,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 172,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) H ( 192,X'S) H ( 193,X'S) RIDE C ( 20,X'S) H ( 203,X'S) H ( 202,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 212,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) H ( 233,X'S) H ( 232,X'S) RIDE C ( 24,X'S) H ( 241,X'S) H ( 243,X'S) H ( 242,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 46,X'S) H ( 461,X'S) RIDE C ( 50,X'S) H ( 501,X'S) RIDE C ( 52,X'S) H ( 521,X'S) RIDE C ( 54,X'S) H ( 541,X'S) RIDE C ( 100,X'S) H (1001,X'S) H (1002,X'S) RIDE C ( 150,X'S) H (1502,X'S) H (1501,X'S) RIDE C ( 200,X'S) H (2001,X'S) H (2002,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 08/07/13 at 11:00:48 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) SAME C(53) C(56) F(220) F(230) F(241) AND CONT C(53) C(56) F(230) F(241) F(220) AND CONT C(53) C(56) F(241) F(220) F(230) AND CONT C(53) C(56) F(221) F(231) F(240) AND CONT C(53) C(56) F(231) F(240) F(221) AND CONT C(53) C(56) F(240) F(221) F(231) DELU 0.015 C(53) C(56) F(220) F(230) F(241) AND CONT C(53) C(56) F(230) F(241) F(220) AND CONT C(53) C(56) F(241) F(220) F(230) AND CONT C(53) C(56) F(221) F(231) F(240) AND CONT C(53) C(56) F(231) F(240) F(221) AND CONT C(53) C(56) F(240) F(221) F(231) SIMU 0.015 C(53) C(56) F(220) F(230) F(241) AND CONT C(53) C(56) F(230) F(241) F(220) AND CONT C(53) C(56) F(241) F(220) F(230) AND CONT C(53) C(56) F(221) F(231) F(240) AND CONT C(53) C(56) F(231) F(240) F(221) AND CONT C(53) C(56) F(240) F(221) F(231) SAME C(43) C(47) F(71) F(81) F(90) AND CONT C(43) C(47) F(81) F(90) F(71) AND CONT C(43) C(47) F(90) F(71) F(81) AND CONT C(43) C(47) F(70) F(80) F(91) AND CONT C(43) C(47) F(80) F(91) F(70) AND CONT C(43) C(47) F(91) F(70) F(80) DELU 0.015 C(43) C(47) F(71) F(81) F(90) AND CONT C(43) C(47) F(81) F(90) F(71) AND CONT C(43) C(47) F(90) F(71) F(81) AND CONT C(43) C(47) F(70) F(80) F(91) AND CONT C(43) C(47) F(80) F(91) F(70) AND CONT C(43) C(47) F(91) F(70) F(80) SIMU 0.015 C(43) C(47) F(71) F(81) F(90) AND CONT C(43) C(47) F(81) F(90) F(71) AND CONT C(43) C(47) F(90) F(71) F(81) AND CONT C(43) C(47) F(70) F(80) F(91) AND CONT C(43) C(47) F(80) F(91) F(70) AND CONT C(43) C(47) F(91) F(70) F(80) SAME CL(100) C(100) CL(101) AND CONT CL(100) C(150) CL(150) SAME CL(200) C(200) CL(201) AND CONT CL(201) C(200) CL(200) DELU 0.015 CL(100) C(100) CL(101) AND CONT CL(100) C(150) CL(150) DELU 0.015 CL(200) C(200) CL(201) AND CONT CL(201) C(200) CL(200) SIMU 0.01 CL(100) C(100) CL(101) AND CONT CL(100) C(150) CL(150) SIMU 0.005 CL(200) C(200) CL(201) AND CONT CL(201) C(200) CL(200) REM HREST END (DO NOT REMOVE THIS LINE) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = CL(100) TO C(150) VIBR .0, 0.00200 = CL(100) TO C(100) VIBR .0, 0.00200 = C(100) TO CL(101) VIBR .0, 0.00500 = CL(101) TO CL(100) VIBR .0, 0.00200 = C(150) TO CL(150) VIBR .0, 0.00500 = CL(150) TO CL(100) VIBR .0, 0.00200 = C(200) TO CL(200) VIBR .0, 0.00200 = C(200) TO CL(201) VIBR .0, 0.00500 = CL(201) TO CL(200) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.04000 = CL(100) TO C(150) U(IJ) .0, 0.04000 = CL(100) TO C(100) U(IJ) .0, 0.08000 = C(100) TO CL(101) U(IJ) .0, 0.08000 = C(150) TO CL(150) U(IJ) .0, 0.08000 = C(200) TO CL(200) U(IJ) .0, 0.08000 = C(200) TO CL(201) REM THERMSIM END (DO NOT REMOVE THIS LINE) END ; # Manually omitted reflections loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details -3 -2 1 x . -1 4 2 x . # start Validation Reply Form _vrf_PLAT434_compound6 ; PROBLEM: Short Inter HL..HL Contact F17 .. F71 . 2.53 Ang. RESPONSE: The short distance relates to the distance of a Fluorine atom to the minor disorder component (15.2%) of another CF3 group of the disordered anion. ; _vrf_PLAT242_compound6 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C31 etc RESPONSE: The anion contains a significant degree of disorder. See _refine_special_details. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 945334' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound1 _audit_creation_date 13-07-08 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title 031SDP12 _chemical_name_systematic '[RhdibpeNBD][BArCl4]' _chemical_melting_point 'not measured' _refine_special_details ; On initial refinement, the atoms upon one half of the diphosphine fragment exhibited prolate ellipsoids. Examination of the difference fourier suggested this was due to disorder. Shift limiting restraints were added to aid refinement. One phosphorous atom, its isobutyl substituents and the CH2CH2 bridging atoms were modelled over two sites and the disordered isobutyl substituents were restrained to maintain sensible geometries. The disordered PCH2CH2P atoms were also separately restrained to maintain sensible geometries. The anion was well ordered. ; _cell_length_a 12.0494(3) _cell_length_b 12.4222(3) _cell_length_c 17.4694(4) _cell_angle_alpha 88.3937(9) _cell_angle_beta 89.8872(9) _cell_angle_gamma 86.3926(9) _cell_volume 2608.61(11) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Rh -1.1178 0.9187 19.2957 0.7515 14.3501 8.2176 4.7343 25.8749 1.2892 98.6062 5.3280 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C49 H60 B1 Cl8 P2 Rh1 # Dc = 1.41 Fooo = 1140.00 Mu = 8.31 M = 1108.30 # Found Formula = C49 H60.00 B1 Cl8 P2 Rh1 # Dc = 1.41 FOOO = 1140.00 Mu = 8.31 M = 1108.30 _chemical_formula_sum 'C49 H60.00 B1 Cl8 P2 Rh1' _chemical_formula_moiety 'C49 H60.00 B1 Cl8 P2 Rh1' _chemical_compound_source 'CRL, University of Oxford' _chemical_formula_weight 1108.30 _cell_measurement_reflns_used 10712 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1140.000 _exptl_absorpt_coefficient_mu 0.831 # Sheldrick geometric approximatio 0.91 0.92 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.92 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 20032 _reflns_number_total 11812 _diffrn_reflns_av_R_equivalents 0.038 # Number of reflections with Friedels Law is 11812 # Theoretical number of reflections is about 21676 _diffrn_reflns_theta_min 5.102 _diffrn_reflns_theta_max 27.472 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.824 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 3.00 _oxford_diffrn_Wilson_scale 23.11 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.29 _refine_diff_density_max 1.34 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 10747 _refine_ls_number_restraints 1312 _refine_ls_number_parameters 650 _oxford_refine_ls_R_factor_ref 0.0870 _refine_ls_wR_factor_ref 0.1563 _refine_ls_goodness_of_fit_ref 1.0090 _refine_ls_shift/su_max 0.0333983 _refine_ls_shift/su_mean 0.0007767 # The values computed with all filters except I/sigma _oxford_reflns_number_all 10747 _refine_ls_R_factor_all 0.0870 _refine_ls_wR_factor_all 0.1563 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8238 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_gt 0.1454 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ +14.62P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Cl1 Cl -0.21800(12) 0.57749(10) 0.41159(9) 0.0480 1.0000 Uani . . . . . . Cl2 Cl -0.53183(15) 0.30033(13) 0.47685(11) 0.0682 1.0000 Uani . . . . . . Cl3 Cl -0.29885(11) 0.50929(11) 0.03328(8) 0.0469 1.0000 Uani . . . . . . Cl4 Cl -0.60732(11) 0.22243(12) 0.08783(9) 0.0485 1.0000 Uani . . . . . . Cl5 Cl -0.30299(15) -0.18615(11) 0.16311(10) 0.0613 1.0000 Uani . . . . . . Cl6 Cl -0.21310(18) -0.12338(14) 0.45995(10) 0.0733 1.0000 Uani . . . . . . Cl7 Cl 0.09695(13) 0.15610(14) 0.05532(8) 0.0565 1.0000 Uani . . . . . . Cl8 Cl 0.18759(11) 0.26066(13) 0.34529(9) 0.0538 1.0000 Uani . . . . . . C1 C 0.4574(5) 0.6639(5) 0.2835(4) 0.0487 1.0000 Uani . . . . . . C2 C 0.3875(5) 0.6037(5) 0.3228(3) 0.0506 1.0000 Uani . . . . . . C3 C 0.3822(5) 0.4965(4) 0.2801(4) 0.0484 1.0000 Uani . . . . . . C4 C 0.3255(5) 0.5319(4) 0.2055(4) 0.0454 1.0000 Uani . . . . . . C5 C 0.3952(5) 0.5944(4) 0.1650(3) 0.0436 1.0000 Uani . . . . . . C6 C 0.5000(5) 0.5983(4) 0.2161(3) 0.0454 1.0000 Uani . . . . . . C7 C 0.5031(5) 0.4836(4) 0.2531(3) 0.0438 1.0000 Uani . . . . . . C8 C 0.0806(5) 0.6570(4) 0.1019(3) 0.0481 1.0000 Uani . . . . . . C9 C 0.0310(5) 0.5759(5) 0.1580(4) 0.0526 1.0000 Uani . . . . . . C10 C 0.0205(6) 0.4690(5) 0.1191(5) 0.0675 1.0000 Uani . . . . . . C11 C -0.0801(6) 0.6139(6) 0.1885(5) 0.0756 1.0000 Uani . . . . . . C12 C 0.2205(5) 0.8212(4) 0.0578(3) 0.0428 1.0000 Uani . . . . . . C13 C 0.2989(5) 0.9129(4) 0.0685(3) 0.0393 1.0000 Uani . . . . . . C14 C 0.4098(5) 0.8724(5) 0.1028(4) 0.0499 1.0000 Uani . . . . . . C15 C 0.3151(6) 0.9699(5) -0.0088(3) 0.0520 1.0000 Uani . . . . . . C17 C 0.0511(5) 0.8642(7) 0.2616(4) 0.0371 0.5242(11) Uani D . P 1 1 . C18 C 0.1486(8) 0.7849(6) 0.4074(4) 0.0414 0.5242(11) Uani D . P 1 1 . C19 C 0.0641(6) 0.6994(6) 0.4166(5) 0.0480 0.5242(11) Uani D . P 1 1 . C20 C 0.0282(11) 0.6902(13) 0.5015(7) 0.0549 0.5242(11) Uani D . P 1 1 . C21 C 0.1176(13) 0.5885(7) 0.3925(10) 0.0540 0.5242(11) Uani D . P 1 1 . C22 C 0.2525(6) 0.9542(6) 0.3185(5) 0.0466 0.5242(11) Uani D . P 1 1 . C23 C 0.3778(5) 0.9464(5) 0.3264(4) 0.0511 0.5242(11) Uani D . P 1 1 . C24 C 0.4105(8) 0.8971(9) 0.4058(6) 0.0627 0.5242(11) Uani D . P 1 1 . C25 C 0.4218(7) 1.0603(8) 0.3190(7) 0.0649 0.5242(11) Uani D . P 1 1 . C26 C 0.1221(9) 0.9283(6) 0.2454(5) 0.0500 0.4758(11) Uani D . P 1 2 . C27 C 0.0858(7) 0.7819(7) 0.3721(5) 0.0438 0.4758(11) Uani D . P 1 2 . C28 C 0.1188(6) 0.6881(7) 0.4260(5) 0.0455 0.4758(11) Uani D . P 1 2 . C29 C 0.0419(13) 0.6913(13) 0.4970(7) 0.0482 0.4758(11) Uani D . P 1 2 . C30 C 0.1060(15) 0.5806(7) 0.3850(10) 0.0503 0.4758(11) Uani D . P 1 2 . C31 C 0.2759(7) 0.9138(9) 0.3805(5) 0.0509 0.4758(11) Uani D . P 1 2 . C32 C 0.3962(6) 0.9334(6) 0.3663(5) 0.0552 0.4758(11) Uani D . P 1 2 . C33 C 0.4067(10) 1.0039(11) 0.2928(5) 0.0620 0.4758(11) Uani D . P 1 2 . C34 C 0.4424(8) 0.9935(10) 0.4342(6) 0.0604 0.4758(11) Uani D . P 1 2 . C50 C -0.2484(4) 0.0819(4) 0.2780(3) 0.0323 1.0000 Uani . . . . . . C51 C -0.2302(4) 0.0381(4) 0.3515(3) 0.0388 1.0000 Uani . . . . . . C52 C -0.2362(5) -0.0722(4) 0.3670(3) 0.0455 1.0000 Uani . . . . . . C53 C -0.2580(5) -0.1437(4) 0.3104(3) 0.0460 1.0000 Uani . . . . . . C54 C -0.2744(4) -0.0998(4) 0.2377(3) 0.0405 1.0000 Uani . . . . . . C55 C -0.2693(4) 0.0092(4) 0.2208(3) 0.0364 1.0000 Uani . . . . . . C56 C -0.2759(4) 0.2874(4) 0.3288(3) 0.0293 1.0000 Uani . . . . . . C57 C -0.3683(4) 0.2621(4) 0.3724(3) 0.0356 1.0000 Uani . . . . . . C58 C -0.4116(5) 0.3320(4) 0.4268(3) 0.0409 1.0000 Uani . . . . . . C59 C -0.3657(4) 0.4283(4) 0.4422(3) 0.0355 1.0000 Uani . . . . . . C60 C -0.2753(4) 0.4546(4) 0.3975(3) 0.0331 1.0000 Uani . . . . . . C61 C -0.2310(4) 0.3860(4) 0.3420(3) 0.0311 1.0000 Uani . . . . . . C62 C -0.1001(4) 0.2149(4) 0.2379(3) 0.0298 1.0000 Uani . . . . . . C63 C -0.0203(4) 0.2347(4) 0.2928(3) 0.0338 1.0000 Uani . . . . . . C64 C 0.0917(4) 0.2320(4) 0.2750(3) 0.0370 1.0000 Uani . . . . . . C65 C 0.1310(4) 0.2083(4) 0.2025(3) 0.0391 1.0000 Uani . . . . . . C66 C 0.0521(4) 0.1864(4) 0.1481(3) 0.0387 1.0000 Uani . . . . . . C67 C -0.0607(4) 0.1885(4) 0.1648(3) 0.0349 1.0000 Uani . . . . . . C68 C -0.3093(4) 0.2582(4) 0.1848(3) 0.0273 1.0000 Uani . . . . . . C69 C -0.4130(4) 0.2220(4) 0.1667(3) 0.0315 1.0000 Uani . . . . . . C70 C -0.4783(4) 0.2707(4) 0.1083(3) 0.0354 1.0000 Uani . . . . . . C71 C -0.4444(4) 0.3580(4) 0.0655(3) 0.0335 1.0000 Uani . . . . . . C72 C -0.3421(4) 0.3961(4) 0.0837(3) 0.0321 1.0000 Uani . . . . . . C73 C -0.2757(4) 0.3476(4) 0.1416(3) 0.0301 1.0000 Uani . . . . . . Rh1 Rh 0.28622(3) 0.70080(3) 0.23692(2) 0.0336 1.0000 Uani . . . . . . P1 P 0.16137(11) 0.76059(10) 0.14484(8) 0.0369 1.0000 Uani D . . . . . P2 P 0.1892(5) 0.8244(5) 0.3080(2) 0.0270 0.5242(11) Uani D . P 1 1 . P3 P 0.2011(7) 0.8317(7) 0.3141(3) 0.0505 0.4758(11) Uani D . P 1 2 . B45 B -0.2333(4) 0.2098(4) 0.2580(3) 0.0291 1.0000 Uani . . . . . . H11 H 0.4992 0.7217 0.3056 0.0591 1.0000 Uiso R . . . . . H21 H 0.3714 0.6099 0.3775 0.0614 1.0000 Uiso R . . . . . H31 H 0.3532 0.4350 0.3088 0.0591 1.0000 Uiso R . . . . . H41 H 0.2699 0.4893 0.1813 0.0553 1.0000 Uiso R . . . . . H51 H 0.3961 0.6028 0.1092 0.0534 1.0000 Uiso R . . . . . H61 H 0.5683 0.6193 0.1914 0.0553 1.0000 Uiso R . . . . . H72 H 0.5561 0.4731 0.2950 0.0530 1.0000 Uiso R . . . . . H71 H 0.5164 0.4277 0.2157 0.0527 1.0000 Uiso R . . . . . H82 H 0.0197 0.6937 0.0743 0.0578 1.0000 Uiso R . . . . . H81 H 0.1288 0.6168 0.0664 0.0579 1.0000 Uiso R . . . . . H91 H 0.0823 0.5643 0.2016 0.0629 1.0000 Uiso R . . . . . H103 H -0.0069 0.4165 0.1552 0.1008 1.0000 Uiso R . . . . . H101 H -0.0315 0.4803 0.0768 0.1010 1.0000 Uiso R . . . . . H102 H 0.0922 0.4434 0.0990 0.1009 1.0000 Uiso R . . . . . H111 H -0.1119 0.5543 0.2144 0.1141 1.0000 Uiso R . . . . . H113 H -0.0711 0.6707 0.2233 0.1142 1.0000 Uiso R . . . . . H112 H -0.1268 0.6396 0.1461 0.1140 1.0000 Uiso R . . . . . H122 H 0.1580 0.8512 0.0263 0.0519 1.0000 Uiso R . . . . . H121 H 0.2611 0.7626 0.0312 0.0519 1.0000 Uiso R . . . . . H131 H 0.2625 0.9651 0.1030 0.0480 1.0000 Uiso R . . . . . H141 H 0.4561 0.9308 0.1110 0.0761 1.0000 Uiso R . . . . . H143 H 0.3966 0.8362 0.1507 0.0761 1.0000 Uiso R . . . . . H142 H 0.4465 0.8226 0.0686 0.0758 1.0000 Uiso R . . . . . H152 H 0.3616 1.0302 -0.0036 0.0786 1.0000 Uiso R . . . . . H151 H 0.2440 0.9963 -0.0294 0.0788 1.0000 Uiso R . . . . . H153 H 0.3499 0.9203 -0.0441 0.0789 1.0000 Uiso R . . . . . H172 H 0.0210 0.9334 0.2788 0.0460 0.5242(11) Uiso R . P 1 1 . H171 H 0.0006 0.8094 0.2750 0.0461 0.5242(11) Uiso R . P 1 1 . H181 H 0.1154 0.8489 0.4313 0.0490 0.5242(11) Uiso R . P 1 1 . H182 H 0.2143 0.7592 0.4358 0.0491 0.5242(11) Uiso R . P 1 1 . H191 H 0.0001 0.7190 0.3835 0.0569 0.5242(11) Uiso R . P 1 1 . H202 H -0.0266 0.6378 0.5059 0.0809 0.5242(11) Uiso R . P 1 1 . H201 H -0.0032 0.7581 0.5189 0.0809 0.5242(11) Uiso R . P 1 1 . H203 H 0.0905 0.6678 0.5332 0.0810 0.5242(11) Uiso R . P 1 1 . H212 H 0.0615 0.5380 0.3858 0.0730 0.5242(11) Uiso R . P 1 1 . H213 H 0.1684 0.5604 0.4314 0.0730 0.5242(11) Uiso R . P 1 1 . H211 H 0.1572 0.5967 0.3450 0.0729 0.5242(11) Uiso R . P 1 1 . H221 H 0.2191 0.9903 0.3628 0.0559 0.5242(11) Uiso R . P 1 1 . H222 H 0.2343 0.9981 0.2723 0.0561 0.5242(11) Uiso R . P 1 1 . H231 H 0.4123 0.9011 0.2866 0.0621 0.5242(11) Uiso R . P 1 1 . H243 H 0.4899 0.8975 0.4127 0.0940 0.5242(11) Uiso R . P 1 1 . H241 H 0.3727 0.9401 0.4439 0.0940 0.5242(11) Uiso R . P 1 1 . H242 H 0.3882 0.8243 0.4099 0.0939 0.5242(11) Uiso R . P 1 1 . H251 H 0.5019 1.0549 0.3187 0.0961 0.5242(11) Uiso R . P 1 1 . H253 H 0.3959 1.1013 0.3624 0.0960 0.5242(11) Uiso R . P 1 1 . H252 H 0.3948 1.0956 0.2724 0.0960 0.5242(11) Uiso R . P 1 1 . H262 H 0.0657 0.9692 0.2743 0.0620 0.4758(11) Uiso R . P 1 2 . H261 H 0.1740 0.9768 0.2228 0.0621 0.4758(11) Uiso R . P 1 2 . H271 H 0.0615 0.8425 0.4037 0.0530 0.4758(11) Uiso R . P 1 2 . H272 H 0.0245 0.7624 0.3403 0.0531 0.4758(11) Uiso R . P 1 2 . H281 H 0.1969 0.6905 0.4417 0.0540 0.4758(11) Uiso R . P 1 2 . H292 H 0.0593 0.6298 0.5297 0.0709 0.4758(11) Uiso R . P 1 2 . H291 H 0.0530 0.7552 0.5249 0.0709 0.4758(11) Uiso R . P 1 2 . H293 H -0.0345 0.6912 0.4822 0.0710 0.4758(11) Uiso R . P 1 2 . H302 H 0.1442 0.5209 0.4119 0.0749 0.4758(11) Uiso R . P 1 2 . H303 H 0.0279 0.5699 0.3837 0.0749 0.4758(11) Uiso R . P 1 2 . H301 H 0.1342 0.5849 0.3335 0.0750 0.4758(11) Uiso R . P 1 2 . H311 H 0.2352 0.9844 0.3795 0.0630 0.4758(11) Uiso R . P 1 2 . H312 H 0.2713 0.8808 0.4315 0.0630 0.4758(11) Uiso R . P 1 2 . H321 H 0.4387 0.8636 0.3608 0.0681 0.4758(11) Uiso R . P 1 2 . H332 H 0.4830 1.0194 0.2850 0.0951 0.4758(11) Uiso R . P 1 2 . H333 H 0.3617 1.0703 0.2977 0.0950 0.4758(11) Uiso R . P 1 2 . H331 H 0.3814 0.9665 0.2492 0.0949 0.4758(11) Uiso R . P 1 2 . H343 H 0.5181 1.0091 0.4234 0.0920 0.4758(11) Uiso R . P 1 2 . H341 H 0.3980 1.0597 0.4400 0.0920 0.4758(11) Uiso R . P 1 2 . H342 H 0.4395 0.9499 0.4804 0.0919 0.4758(11) Uiso R . P 1 2 . H511 H -0.2142 0.0838 0.3907 0.0471 1.0000 Uiso R . . . . . H531 H -0.2612 -0.2170 0.3203 0.0560 1.0000 Uiso R . . . . . H551 H -0.2796 0.0346 0.1700 0.0438 1.0000 Uiso R . . . . . H571 H -0.4018 0.1978 0.3645 0.0438 1.0000 Uiso R . . . . . H591 H -0.3933 0.4734 0.4799 0.0440 1.0000 Uiso R . . . . . H611 H -0.1703 0.4057 0.3130 0.0378 1.0000 Uiso R . . . . . H631 H -0.0428 0.2502 0.3426 0.0411 1.0000 Uiso R . . . . . H651 H 0.2064 0.2064 0.1917 0.0478 1.0000 Uiso R . . . . . H671 H -0.1101 0.1729 0.1260 0.0428 1.0000 Uiso R . . . . . H691 H -0.4394 0.1634 0.1948 0.0381 1.0000 Uiso R . . . . . H711 H -0.4885 0.3901 0.0263 0.0406 1.0000 Uiso R . . . . . H731 H -0.2081 0.3758 0.1519 0.0369 1.0000 Uiso R . . . . . C16 C 0.0634(6) 0.8648(9) 0.1862(6) 0.0568 0.4758(11) Uani D . P 1 2 . C161 C 0.0652(7) 0.8704(6) 0.1762(4) 0.0351 0.5242(11) Uani D . P 1 1 . H1611 H 0.0924 0.9400 0.1609 0.0500 0.5242(11) Uiso R . P 1 1 . H1612 H -0.0065 0.8628 0.1525 0.0502 0.5242(11) Uiso R . P 1 1 . H161 H 0.0411 0.9160 0.1450 0.0639 0.4758(11) Uiso R . P 1 2 . H162 H -0.0018 0.8327 0.2078 0.0638 0.4758(11) Uiso R . P 1 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 Cl1 0.0486(8) 0.0339(6) 0.0623(9) -0.0104(6) 0.0016(7) -0.0064(6) Cl2 0.0786(11) 0.0511(8) 0.0777(11) -0.0199(8) 0.0523(10) -0.0203(8) Cl3 0.0432(7) 0.0472(7) 0.0494(8) 0.0208(6) -0.0031(6) -0.0057(6) Cl4 0.0322(7) 0.0587(8) 0.0552(9) 0.0015(7) -0.0041(6) -0.0099(6) Cl5 0.0786(11) 0.0316(7) 0.0743(11) -0.0072(7) -0.0191(9) -0.0045(7) Cl6 0.1127(15) 0.0556(9) 0.0476(9) 0.0235(7) 0.0018(9) 0.0145(9) Cl7 0.0506(8) 0.0778(10) 0.0375(7) 0.0009(7) 0.0138(6) 0.0223(7) Cl8 0.0348(7) 0.0720(10) 0.0547(9) -0.0054(7) -0.0056(6) -0.0031(7) C1 0.039(3) 0.049(3) 0.057(3) -0.017(3) -0.018(3) 0.011(2) C2 0.059(3) 0.057(3) 0.032(3) 0.000(2) -0.005(3) 0.026(3) C3 0.048(3) 0.039(3) 0.056(3) 0.015(2) 0.010(3) 0.007(2) C4 0.042(3) 0.033(3) 0.061(3) -0.011(2) -0.010(3) 0.002(2) C5 0.053(3) 0.044(3) 0.031(3) -0.002(2) 0.006(2) 0.020(2) C6 0.034(3) 0.043(3) 0.059(3) -0.002(2) 0.011(2) 0.000(2) C7 0.045(3) 0.036(3) 0.049(3) -0.002(2) -0.006(2) 0.012(2) C8 0.050(3) 0.045(3) 0.049(3) 0.010(2) -0.012(3) -0.005(2) C9 0.042(3) 0.052(3) 0.063(4) 0.005(3) -0.008(3) -0.005(3) C10 0.052(3) 0.048(3) 0.103(5) 0.002(3) -0.001(4) -0.010(3) C11 0.065(4) 0.067(4) 0.097(5) -0.013(4) 0.007(4) -0.018(3) C12 0.050(3) 0.042(3) 0.036(3) 0.000(2) -0.006(2) 0.001(2) C13 0.050(3) 0.037(3) 0.030(3) 0.002(2) 0.007(2) 0.001(2) C14 0.050(3) 0.051(3) 0.050(3) 0.004(3) 0.002(3) -0.009(3) C15 0.070(3) 0.047(3) 0.037(3) -0.001(2) 0.017(3) 0.009(3) C17 0.032(4) 0.041(4) 0.038(4) 0.004(4) 0.001(4) 0.000(4) C18 0.044(4) 0.046(4) 0.034(4) -0.009(4) 0.003(4) 0.001(4) C19 0.050(4) 0.059(4) 0.035(4) 0.005(4) 0.004(4) -0.004(4) C20 0.054(5) 0.075(6) 0.034(5) 0.012(5) -0.002(5) 0.000(5) C21 0.063(5) 0.055(5) 0.045(5) 0.005(5) 0.002(5) -0.013(5) C22 0.039(4) 0.038(4) 0.063(5) -0.007(4) 0.010(4) -0.003(4) C23 0.038(3) 0.044(4) 0.073(5) -0.014(4) 0.001(4) -0.007(4) C24 0.051(4) 0.067(5) 0.072(5) -0.011(5) -0.002(5) -0.009(5) C25 0.045(4) 0.055(5) 0.098(6) -0.018(5) 0.011(5) -0.017(4) C26 0.049(5) 0.042(5) 0.055(5) 0.017(4) 0.016(5) 0.008(4) C27 0.046(4) 0.045(5) 0.041(5) 0.000(4) 0.009(4) -0.007(4) C28 0.048(4) 0.052(4) 0.035(4) 0.007(4) 0.008(4) 0.000(4) C29 0.043(5) 0.065(6) 0.035(5) 0.008(5) 0.009(5) 0.002(5) C30 0.064(5) 0.045(5) 0.044(6) 0.006(5) 0.006(5) -0.018(5) C31 0.057(4) 0.045(5) 0.051(5) -0.008(4) 0.012(5) -0.007(4) C32 0.058(4) 0.049(4) 0.061(5) -0.017(4) 0.009(4) -0.009(4) C33 0.067(5) 0.060(5) 0.061(5) -0.012(5) 0.003(5) -0.013(5) C34 0.062(5) 0.051(5) 0.070(6) -0.019(5) 0.003(5) -0.011(5) C50 0.029(2) 0.027(2) 0.040(3) 0.0026(19) 0.001(2) 0.0034(18) C51 0.046(3) 0.035(2) 0.034(3) 0.004(2) 0.001(2) 0.008(2) C52 0.055(3) 0.037(3) 0.042(3) 0.012(2) 0.005(3) 0.009(2) C53 0.048(3) 0.028(2) 0.060(3) 0.010(2) 0.005(3) 0.006(2) C54 0.039(3) 0.029(2) 0.053(3) 0.000(2) -0.001(2) 0.001(2) C55 0.037(2) 0.032(2) 0.039(3) 0.002(2) -0.001(2) 0.004(2) C56 0.031(2) 0.029(2) 0.027(2) 0.0038(18) 0.0007(19) 0.0029(18) C57 0.043(3) 0.030(2) 0.034(3) -0.003(2) 0.011(2) -0.006(2) C58 0.047(3) 0.034(3) 0.041(3) -0.001(2) 0.014(2) 0.001(2) C59 0.040(3) 0.034(2) 0.031(2) -0.006(2) 0.005(2) 0.007(2) C60 0.034(2) 0.026(2) 0.038(3) 0.0017(19) -0.004(2) 0.0008(19) C61 0.027(2) 0.032(2) 0.033(2) 0.0009(19) -0.0017(19) 0.0039(19) C62 0.029(2) 0.025(2) 0.034(2) 0.0028(18) 0.0032(19) 0.0074(18) C63 0.031(2) 0.036(2) 0.033(3) 0.001(2) 0.004(2) 0.005(2) C64 0.032(2) 0.033(2) 0.045(3) 0.004(2) 0.000(2) 0.005(2) C65 0.029(2) 0.041(3) 0.045(3) 0.010(2) 0.006(2) 0.007(2) C66 0.037(3) 0.043(3) 0.034(3) 0.001(2) 0.012(2) 0.011(2) C67 0.036(2) 0.032(2) 0.037(3) -0.001(2) 0.006(2) 0.004(2) C68 0.027(2) 0.029(2) 0.025(2) 0.0003(17) 0.0050(18) 0.0028(18) C69 0.035(2) 0.031(2) 0.029(2) -0.0008(19) 0.002(2) -0.0005(19) C70 0.028(2) 0.036(2) 0.042(3) -0.007(2) -0.002(2) 0.0014(19) C71 0.029(2) 0.041(3) 0.030(2) 0.002(2) -0.0026(19) 0.006(2) C72 0.031(2) 0.032(2) 0.033(2) 0.0036(19) 0.002(2) 0.0004(19) C73 0.028(2) 0.031(2) 0.031(2) 0.0019(19) 0.0027(19) -0.0001(18) Rh1 0.0322(2) 0.0311(2) 0.0367(2) -0.00170(15) -0.00091(16) 0.00484(15) P1 0.0370(7) 0.0335(7) 0.0396(7) 0.0055(5) -0.0026(6) 0.0015(5) P2 0.029(2) 0.027(2) 0.023(2) 0.0011(16) 0.0007(16) 0.0050(16) P3 0.048(3) 0.047(3) 0.057(4) -0.006(3) 0.012(3) -0.003(3) B45 0.032(3) 0.025(2) 0.029(3) 0.001(2) 0.003(2) 0.002(2) C16 0.048(5) 0.046(6) 0.073(7) 0.013(6) 0.002(6) 0.018(6) C161 0.030(4) 0.041(5) 0.034(5) 0.008(4) 0.001(4) -0.003(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.21721(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 . C60 . 1.739(5) yes Cl2 . C58 . 1.751(5) yes Cl3 . C72 . 1.746(5) yes Cl4 . C70 . 1.743(5) yes Cl5 . C54 . 1.759(6) yes Cl6 . C52 . 1.744(6) yes Cl7 . C66 . 1.750(5) yes Cl8 . C64 . 1.747(5) yes C1 . C2 . 1.338(9) yes C1 . C6 . 1.521(8) yes C1 . Rh1 . 2.235(5) yes C1 . H11 . 0.990 no C2 . C3 . 1.548(8) yes C2 . Rh1 . 2.217(5) yes C2 . H21 . 0.979 no C3 . C4 . 1.515(8) yes C3 . C7 . 1.530(8) yes C3 . H31 . 0.984 no C4 . C5 . 1.362(8) yes C4 . Rh1 . 2.206(5) yes C4 . H41 . 0.983 no C5 . C6 . 1.551(8) yes C5 . Rh1 . 2.218(5) yes C5 . H51 . 0.978 no C6 . C7 . 1.547(7) yes C6 . H61 . 0.975 no C7 . H72 . 0.973 no C7 . H71 . 0.973 no C8 . C9 . 1.534(8) yes C8 . P1 . 1.839(6) yes C8 . H82 . 0.962 no C8 . H81 . 0.974 no C9 . C10 . 1.521(9) yes C9 . C11 . 1.494(9) yes C9 . H91 . 0.984 no C10 . H103 . 0.967 no C10 . H101 . 0.971 no C10 . H102 . 0.971 no C11 . H111 . 0.956 no C11 . H113 . 0.955 no C11 . H112 . 0.967 no C12 . C13 . 1.541(8) yes C12 . P1 . 1.839(6) yes C12 . H122 . 0.982 no C12 . H121 . 0.979 no C13 . C14 . 1.517(8) yes C13 . C15 . 1.525(7) yes C13 . H131 . 0.980 no C14 . H141 . 0.957 no C14 . H143 . 0.957 no C14 . H142 . 0.959 no C15 . H152 . 0.969 no C15 . H151 . 0.966 no C15 . H153 . 0.962 no C17 . P2 . 1.884(7) yes C17 . H172 . 0.967 no C17 . H171 . 0.967 no C17 . C161 . 1.502(7) yes C18 . C19 . 1.521(6) yes C18 . P2 . 1.865(6) yes C18 . H181 . 0.971 no C18 . H182 . 0.967 no C19 . C20 . 1.547(6) yes C19 . C21 . 1.552(6) yes C19 . H191 . 0.979 no C20 . H202 . 0.957 no C20 . H201 . 0.959 no C20 . H203 . 0.957 no C21 . H212 . 0.960 no C21 . H213 . 0.960 no C21 . H211 . 0.963 no C22 . C23 . 1.513(6) yes C22 . P2 . 1.840(6) yes C22 . H221 . 0.978 no C22 . H222 . 0.979 no C23 . C24 . 1.543(6) yes C23 . C25 . 1.544(6) yes C23 . H231 . 0.981 no C24 . H243 . 0.964 no C24 . H241 . 0.962 no C24 . H242 . 0.960 no C25 . H251 . 0.964 no C25 . H253 . 0.965 no C25 . H252 . 0.962 no C26 . P3 . 1.888(8) yes C26 . H262 . 0.972 no C26 . H261 . 0.973 no C26 . C16 . 1.520(8) yes C27 . C28 . 1.511(6) yes C27 . P3 . 1.845(6) yes C27 . H271 . 0.976 no C27 . H272 . 0.972 no C28 . C29 . 1.546(6) yes C28 . C30 . 1.550(6) yes C28 . H281 . 0.983 no C29 . H292 . 0.954 no C29 . H291 . 0.959 no C29 . H293 . 0.957 no C30 . H302 . 0.960 no C30 . H303 . 0.959 no C30 . H301 . 0.962 no C31 . C32 . 1.504(6) yes C31 . P3 . 1.839(6) yes C31 . H311 . 0.977 no C31 . H312 . 0.973 no C32 . C33 . 1.543(6) yes C32 . C34 . 1.542(6) yes C32 . H321 . 0.986 no C33 . H332 . 0.961 no C33 . H333 . 0.964 no C33 . H331 . 0.963 no C34 . H343 . 0.962 no C34 . H341 . 0.960 no C34 . H342 . 0.962 no C50 . C51 . 1.393(7) yes C50 . C55 . 1.399(7) yes C50 . B45 . 1.638(7) yes C51 . C52 . 1.395(7) yes C51 . H511 . 0.929 no C52 . C53 . 1.384(8) yes C53 . C54 . 1.377(8) yes C53 . H531 . 0.926 no C54 . C55 . 1.383(7) yes C55 . H551 . 0.940 no C56 . C57 . 1.395(7) yes C56 . C61 . 1.395(7) yes C56 . B45 . 1.650(7) yes C57 . C58 . 1.385(7) yes C57 . H571 . 0.932 no C58 . C59 . 1.382(7) yes C59 . C60 . 1.389(7) yes C59 . H591 . 0.925 no C60 . C61 . 1.392(7) yes C61 . H611 . 0.931 no C62 . C63 . 1.397(7) yes C62 . C67 . 1.402(7) yes C62 . B45 . 1.647(7) yes C63 . C64 . 1.383(7) yes C63 . H631 . 0.934 no C64 . C65 . 1.384(7) yes C65 . C66 . 1.390(8) yes C65 . H651 . 0.927 no C66 . C67 . 1.389(7) yes C67 . H671 . 0.935 no C68 . C69 . 1.395(7) yes C68 . C73 . 1.406(6) yes C68 . B45 . 1.650(7) yes C69 . C70 . 1.390(7) yes C69 . H691 . 0.938 no C70 . C71 . 1.383(7) yes C71 . C72 . 1.388(7) yes C71 . H711 . 0.933 no C72 . C73 . 1.391(7) yes C73 . H731 . 0.927 no Rh1 . P1 . 2.2813(14) yes Rh1 . P2 . 2.267(6) yes Rh1 . P1 . 2.2813(14) yes Rh1 . P3 . 2.329(8) yes P1 . C161 . 1.828(6) yes P1 . C16 . 1.857(7) yes C16 . H161 . 0.974 no C16 . H162 . 0.973 no C161 . H1611 . 0.974 no C161 . H1612 . 0.970 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . C1 . C6 . 107.1(5) yes C2 . C1 . Rh1 . 71.8(3) yes C6 . C1 . Rh1 . 95.8(3) yes C2 . C1 . H11 . 124.6 no C6 . C1 . H11 . 122.9 no Rh1 . C1 . H11 . 120.3 no C1 . C2 . C3 . 106.9(5) yes C1 . C2 . Rh1 . 73.2(3) yes C3 . C2 . Rh1 . 94.7(3) yes C1 . C2 . H21 . 124.7 no C3 . C2 . H21 . 123.0 no Rh1 . C2 . H21 . 120.3 no C2 . C3 . C4 . 103.0(4) yes C2 . C3 . C7 . 99.0(5) yes C4 . C3 . C7 . 100.1(5) yes C2 . C3 . H31 . 117.2 no C4 . C3 . H31 . 117.7 no C7 . C3 . H31 . 116.8 no C3 . C4 . C5 . 108.1(5) yes C3 . C4 . Rh1 . 96.1(3) yes C5 . C4 . Rh1 . 72.5(3) yes C3 . C4 . H41 . 122.4 no C5 . C4 . H41 . 123.3 no Rh1 . C4 . H41 . 121.4 no C4 . C5 . C6 . 105.1(5) yes C4 . C5 . Rh1 . 71.6(3) yes C6 . C5 . Rh1 . 95.6(3) yes C4 . C5 . H51 . 124.7 no C6 . C5 . H51 . 123.8 no Rh1 . C5 . H51 . 121.6 no C5 . C6 . C1 . 103.0(4) yes C5 . C6 . C7 . 99.8(4) yes C1 . C6 . C7 . 99.9(5) yes C5 . C6 . H61 . 117.5 no C1 . C6 . H61 . 117.4 no C7 . C6 . H61 . 116.4 no C6 . C7 . C3 . 93.3(4) yes C6 . C7 . H72 . 113.3 no C3 . C7 . H72 . 113.3 no C6 . C7 . H71 . 112.2 no C3 . C7 . H71 . 113.7 no H72 . C7 . H71 . 110.2 no C9 . C8 . P1 . 116.0(4) yes C9 . C8 . H82 . 107.3 no P1 . C8 . H82 . 107.5 no C9 . C8 . H81 . 108.1 no P1 . C8 . H81 . 108.2 no H82 . C8 . H81 . 109.7 no C8 . C9 . C10 . 109.8(6) yes C8 . C9 . C11 . 113.4(5) yes C10 . C9 . C11 . 109.0(5) yes C8 . C9 . H91 . 107.9 no C10 . C9 . H91 . 108.9 no C11 . C9 . H91 . 107.9 no C9 . C10 . H103 . 109.9 no C9 . C10 . H101 . 108.7 no H103 . C10 . H101 . 109.5 no C9 . C10 . H102 . 109.7 no H103 . C10 . H102 . 110.3 no H101 . C10 . H102 . 108.7 no C9 . C11 . H111 . 108.3 no C9 . C11 . H113 . 109.4 no H111 . C11 . H113 . 110.2 no C9 . C11 . H112 . 108.6 no H111 . C11 . H112 . 110.1 no H113 . C11 . H112 . 110.2 no C13 . C12 . P1 . 117.2(4) yes C13 . C12 . H122 . 106.8 no P1 . C12 . H122 . 107.4 no C13 . C12 . H121 . 108.6 no P1 . C12 . H121 . 106.7 no H122 . C12 . H121 . 110.1 no C12 . C13 . C14 . 112.2(4) yes C12 . C13 . C15 . 108.7(5) yes C14 . C13 . C15 . 110.8(5) yes C12 . C13 . H131 . 108.0 no C14 . C13 . H131 . 108.8 no C15 . C13 . H131 . 108.1 no C13 . C14 . H141 . 111.0 no C13 . C14 . H143 . 108.8 no H141 . C14 . H143 . 109.2 no C13 . C14 . H142 . 109.1 no H141 . C14 . H142 . 109.3 no H143 . C14 . H142 . 109.4 no C13 . C15 . H152 . 110.7 no C13 . C15 . H151 . 109.8 no H152 . C15 . H151 . 108.9 no C13 . C15 . H153 . 110.0 no H152 . C15 . H153 . 108.8 no H151 . C15 . H153 . 108.6 no P2 . C17 . H172 . 111.5 no P2 . C17 . H171 . 107.8 no H172 . C17 . H171 . 109.5 no P2 . C17 . C161 . 109.48(9) yes H172 . C17 . C161 . 108.9 no H171 . C17 . C161 . 109.5 no C19 . C18 . P2 . 117.4(5) yes C19 . C18 . H181 . 105.9 no P2 . C18 . H181 . 107.7 no C19 . C18 . H182 . 107.3 no P2 . C18 . H182 . 109.3 no H181 . C18 . H182 . 109.1 no C18 . C19 . C20 . 109.57(7) yes C18 . C19 . C21 . 109.58(7) yes C20 . C19 . C21 . 108.68(7) yes C18 . C19 . H191 . 109.1 no C20 . C19 . H191 . 111.0 no C21 . C19 . H191 . 108.9 no C19 . C20 . H202 . 108.4 no C19 . C20 . H201 . 111.0 no H202 . C20 . H201 . 109.0 no C19 . C20 . H203 . 110.5 no H202 . C20 . H203 . 109.3 no H201 . C20 . H203 . 108.6 no C19 . C21 . H212 . 110.6 no C19 . C21 . H213 . 109.6 no H212 . C21 . H213 . 108.7 no C19 . C21 . H211 . 110.0 no H212 . C21 . H211 . 108.7 no H213 . C21 . H211 . 109.2 no C23 . C22 . P2 . 115.0(5) yes C23 . C22 . H221 . 109.6 no P2 . C22 . H221 . 108.8 no C23 . C22 . H222 . 107.3 no P2 . C22 . H222 . 107.2 no H221 . C22 . H222 . 108.8 no C22 . C23 . C24 . 109.57(7) yes C22 . C23 . C25 . 109.58(7) yes C24 . C23 . C25 . 108.69(7) yes C22 . C23 . H231 . 110.9 no C24 . C23 . H231 . 109.0 no C25 . C23 . H231 . 109.1 no C23 . C24 . H243 . 109.9 no C23 . C24 . H241 . 107.9 no H243 . C24 . H241 . 110.0 no C23 . C24 . H242 . 109.6 no H243 . C24 . H242 . 109.7 no H241 . C24 . H242 . 109.8 no C23 . C25 . H251 . 109.7 no C23 . C25 . H253 . 108.7 no H251 . C25 . H253 . 109.4 no C23 . C25 . H252 . 109.8 no H251 . C25 . H252 . 109.6 no H253 . C25 . H252 . 109.8 no P3 . C26 . H262 . 108.1 no P3 . C26 . H261 . 108.4 no H262 . C26 . H261 . 109.8 no P3 . C26 . C16 . 109.53(9) yes H262 . C26 . C16 . 108.0 no H261 . C26 . C16 . 112.9 no C28 . C27 . P3 . 114.6(6) yes C28 . C27 . H271 . 107.0 no P3 . C27 . H271 . 104.7 no C28 . C27 . H272 . 109.0 no P3 . C27 . H272 . 111.8 no H271 . C27 . H272 . 109.6 no C27 . C28 . C29 . 109.57(7) yes C27 . C28 . C30 . 109.57(7) yes C29 . C28 . C30 . 108.67(7) yes C27 . C28 . H281 . 110.6 no C29 . C28 . H281 . 110.3 no C30 . C28 . H281 . 108.1 no C28 . C29 . H292 . 110.0 no C28 . C29 . H291 . 109.4 no H292 . C29 . H291 . 108.7 no C28 . C29 . H293 . 110.9 no H292 . C29 . H293 . 108.5 no H291 . C29 . H293 . 109.3 no C28 . C30 . H302 . 111.6 no C28 . C30 . H303 . 106.6 no H302 . C30 . H303 . 109.5 no C28 . C30 . H301 . 110.5 no H302 . C30 . H301 . 109.1 no H303 . C30 . H301 . 109.4 no C32 . C31 . P3 . 119.9(5) yes C32 . C31 . H311 . 106.9 no P3 . C31 . H311 . 105.4 no C32 . C31 . H312 . 107.0 no P3 . C31 . H312 . 107.9 no H311 . C31 . H312 . 109.4 no C31 . C32 . C33 . 109.57(7) yes C31 . C32 . C34 . 109.57(7) yes C33 . C32 . C34 . 108.69(7) yes C31 . C32 . H321 . 109.2 no C33 . C32 . H321 . 110.1 no C34 . C32 . H321 . 109.7 no C32 . C33 . H332 . 109.7 no C32 . C33 . H333 . 109.5 no H332 . C33 . H333 . 109.7 no C32 . C33 . H331 . 110.2 no H332 . C33 . H331 . 108.9 no H333 . C33 . H331 . 108.9 no C32 . C34 . H343 . 108.9 no C32 . C34 . H341 . 108.5 no H343 . C34 . H341 . 109.6 no C32 . C34 . H342 . 110.3 no H343 . C34 . H342 . 109.7 no H341 . C34 . H342 . 109.8 no C51 . C50 . C55 . 116.5(4) yes C51 . C50 . B45 . 121.6(4) yes C55 . C50 . B45 . 121.6(4) yes C50 . C51 . C52 . 121.2(5) yes C50 . C51 . H511 . 118.9 no C52 . C51 . H511 . 120.0 no Cl6 . C52 . C51 . 119.6(4) yes Cl6 . C52 . C53 . 118.3(4) yes C51 . C52 . C53 . 122.1(5) yes C52 . C53 . C54 . 116.2(5) yes C52 . C53 . H531 . 122.3 no C54 . C53 . H531 . 121.4 no Cl5 . C54 . C53 . 118.6(4) yes Cl5 . C54 . C55 . 118.6(4) yes C53 . C54 . C55 . 122.8(5) yes C50 . C55 . C54 . 121.1(5) yes C50 . C55 . H551 . 119.7 no C54 . C55 . H551 . 119.2 no C57 . C56 . C61 . 117.0(4) yes C57 . C56 . B45 . 120.3(4) yes C61 . C56 . B45 . 122.3(4) yes C56 . C57 . C58 . 120.8(5) yes C56 . C57 . H571 . 119.7 no C58 . C57 . H571 . 119.5 no Cl2 . C58 . C57 . 119.3(4) yes Cl2 . C58 . C59 . 117.9(4) yes C57 . C58 . C59 . 122.8(5) yes C58 . C59 . C60 . 116.4(4) yes C58 . C59 . H591 . 122.4 no C60 . C59 . H591 . 121.2 no Cl1 . C60 . C59 . 118.3(4) yes Cl1 . C60 . C61 . 119.8(4) yes C59 . C60 . C61 . 121.8(4) yes C56 . C61 . C60 . 121.2(4) yes C56 . C61 . H611 . 118.9 no C60 . C61 . H611 . 119.9 no C63 . C62 . C67 . 116.7(4) yes C63 . C62 . B45 . 123.0(4) yes C67 . C62 . B45 . 120.0(4) yes C62 . C63 . C64 . 121.5(5) yes C62 . C63 . H631 . 119.4 no C64 . C63 . H631 . 119.0 no Cl8 . C64 . C63 . 119.5(4) yes Cl8 . C64 . C65 . 118.4(4) yes C63 . C64 . C65 . 122.1(5) yes C64 . C65 . C66 . 116.7(5) yes C64 . C65 . H651 . 120.9 no C66 . C65 . H651 . 122.4 no Cl7 . C66 . C65 . 118.7(4) yes Cl7 . C66 . C67 . 119.2(4) yes C65 . C66 . C67 . 122.2(5) yes C62 . C67 . C66 . 120.9(5) yes C62 . C67 . H671 . 120.5 no C66 . C67 . H671 . 118.6 no C69 . C68 . C73 . 116.1(4) yes C69 . C68 . B45 . 123.6(4) yes C73 . C68 . B45 . 120.0(4) yes C68 . C69 . C70 . 121.7(4) yes C68 . C69 . H691 . 118.9 no C70 . C69 . H691 . 119.3 no Cl4 . C70 . C69 . 120.0(4) yes Cl4 . C70 . C71 . 118.1(4) yes C69 . C70 . C71 . 121.9(5) yes C70 . C71 . C72 . 117.1(4) yes C70 . C71 . H711 . 121.4 no C72 . C71 . H711 . 121.5 no Cl3 . C72 . C71 . 118.4(4) yes Cl3 . C72 . C73 . 120.0(4) yes C71 . C72 . C73 . 121.6(4) yes C68 . C73 . C72 . 121.6(4) yes C68 . C73 . H731 . 119.7 no C72 . C73 . H731 . 118.7 no C1 . Rh1 . C5 . 65.4(2) yes C1 . Rh1 . C2 . 35.0(2) yes C5 . Rh1 . C2 . 77.1(2) yes C1 . Rh1 . C4 . 76.4(2) yes C5 . Rh1 . C4 . 35.9(2) yes C2 . Rh1 . C4 . 65.6(2) yes C1 . Rh1 . P1 . 154.05(18) yes C5 . Rh1 . P1 . 98.16(15) yes C2 . Rh1 . P1 . 165.49(18) yes C4 . Rh1 . P1 . 102.43(15) yes C1 . Rh1 . P2 . 111.4(2) yes C5 . Rh1 . P2 . 173.3(2) yes C2 . Rh1 . P2 . 103.7(2) yes C4 . Rh1 . P2 . 150.5(2) yes P1 . Rh1 . P2 . 82.68(14) yes C1 . Rh1 . C5 . 65.4(2) yes C1 . Rh1 . C2 . 35.0(2) yes C5 . Rh1 . C2 . 77.1(2) yes C1 . Rh1 . C4 . 76.4(2) yes C5 . Rh1 . C4 . 35.9(2) yes C2 . Rh1 . C4 . 65.6(2) yes C1 . Rh1 . P1 . 154.05(18) yes C5 . Rh1 . P1 . 98.16(15) yes C2 . Rh1 . P1 . 165.49(18) yes C4 . Rh1 . P1 . 102.43(15) yes C1 . Rh1 . P3 . 106.7(2) yes C5 . Rh1 . P3 . 169.2(2) yes C2 . Rh1 . P3 . 100.8(2) yes C4 . Rh1 . P3 . 152.5(3) yes P1 . Rh1 . P3 . 86.4(2) yes C12 . P1 . C8 . 99.9(3) yes C12 . P1 . Rh1 . 115.88(19) yes C8 . P1 . Rh1 . 116.01(18) yes C12 . P1 . C161 . 101.4(3) yes C8 . P1 . C161 . 108.7(4) yes Rh1 . P1 . C161 . 113.2(2) yes C12 . P1 . C8 . 99.9(3) yes C12 . P1 . Rh1 . 115.88(19) yes C8 . P1 . Rh1 . 116.01(18) yes C12 . P1 . C16 . 107.0(4) yes C8 . P1 . C16 . 108.7(4) yes Rh1 . P1 . C16 . 108.7(3) yes C17 . P2 . C18 . 102.6(5) yes C17 . P2 . C22 . 103.3(5) yes C18 . P2 . C22 . 104.13(7) yes C17 . P2 . Rh1 . 110.3(3) yes C18 . P2 . Rh1 . 118.5(4) yes C22 . P2 . Rh1 . 116.1(4) yes C26 . P3 . C27 . 100.7(6) yes C26 . P3 . C31 . 107.1(6) yes C27 . P3 . C31 . 104.08(7) yes C26 . P3 . Rh1 . 104.8(3) yes C27 . P3 . Rh1 . 113.3(5) yes C31 . P3 . Rh1 . 124.3(5) yes C68 . B45 . C56 . 103.2(3) yes C68 . B45 . C62 . 110.2(4) yes C56 . B45 . C62 . 114.0(4) yes C68 . B45 . C50 . 113.7(4) yes C56 . B45 . C50 . 111.9(4) yes C62 . B45 . C50 . 104.1(4) yes C26 . C16 . P1 . 110.40(9) yes C26 . C16 . H161 . 106.3 no P1 . C16 . H161 . 107.3 no C26 . C16 . H162 . 111.4 no P1 . C16 . H162 . 111.2 no H161 . C16 . H162 . 110.0 no C17 . C161 . P1 . 110.31(9) yes C17 . C161 . H1611 . 109.7 no P1 . C161 . H1611 . 110.4 no C17 . C161 . H1612 . 108.6 no P1 . C161 . H1612 . 108.5 no H1611 . C161 . H1612 . 109.3 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C34 . H241 . C31 . 126.2(9) 1.113 1.664 2.489(10) yes _iucr_refine_instruction_details_constraints ; # # Punched on 08/07/13 at 11:31:52 # #LIST 12 BLOCK SCALE X'S, U'S EQUIV PART(1001,OCC) PART(1002,OCC) WEIGHT -1 PART(1002,OCC) RIDE C ( 1,X'S) H ( 11,X'S) RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 72,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 82,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 103,X'S) H ( 101,X'S) H ( 102,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 113,X'S) H ( 112,X'S) RIDE C ( 12,X'S) H ( 122,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 143,X'S) H ( 142,X'S) RIDE C ( 15,X'S) H ( 152,X'S) H ( 151,X'S) H ( 153,X'S) RIDE C ( 17,X'S) H ( 172,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) H ( 182,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 202,X'S) H ( 201,X'S) H ( 203,X'S) RIDE C ( 21,X'S) H ( 212,X'S) H ( 213,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) H ( 222,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 243,X'S) H ( 241,X'S) H ( 242,X'S) RIDE C ( 25,X'S) H ( 251,X'S) H ( 253,X'S) H ( 252,X'S) RIDE C ( 26,X'S) H ( 262,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) H ( 272,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 292,X'S) H ( 291,X'S) H ( 293,X'S) RIDE C ( 30,X'S) H ( 302,X'S) H ( 303,X'S) H ( 301,X'S) RIDE C ( 31,X'S) H ( 311,X'S) H ( 312,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 332,X'S) H ( 333,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 343,X'S) H ( 341,X'S) H ( 342,X'S) RIDE C ( 51,X'S) H ( 511,X'S) RIDE C ( 53,X'S) H ( 531,X'S) RIDE C ( 55,X'S) H ( 551,X'S) RIDE C ( 57,X'S) H ( 571,X'S) RIDE C ( 59,X'S) H ( 591,X'S) RIDE C ( 61,X'S) H ( 611,X'S) RIDE C ( 63,X'S) H ( 631,X'S) RIDE C ( 65,X'S) H ( 651,X'S) RIDE C ( 67,X'S) H ( 671,X'S) RIDE C ( 69,X'S) H ( 691,X'S) RIDE C ( 71,X'S) H ( 711,X'S) RIDE C ( 73,X'S) H ( 731,X'S) RIDE C ( 16,X'S) H ( 161,X'S) H ( 162,X'S) RIDE C ( 161,X'S) H (1611,X'S) H (1612,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 08/07/13 at 11:31:52 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) REM SHIFTLIMIT START (DO NOT REMOVE THIS LINE) LIMIT 0.01000000 U[ISO] LIMIT 0.01000000 X LIMIT 0.01000000 Y LIMIT 0.01000000 Z LIMIT 0.01000000 U[11] LIMIT 0.01000000 U[22] LIMIT 0.01000000 U[33] LIMIT 0.01000000 U[12] LIMIT 0.01000000 U[13] LIMIT 0.01000000 U[23] LIMIT 0.01000000 OCC REM SHIFTLIMIT END (DO NOT REMOVE THIS LINE) SAME C(18) C(19) C(20) C(21) AND CONT C(18) C(19) C(21) C(20) AND CONT C(22) C(23) C(24) C(25) AND CONT C(22) C(23) C(25) C(24) AND CONT C(27) C(28) C(29) C(30) AND CONT C(27) C(28) C(30) C(29) AND CONT C(31) C(32) C(33) C(34) AND CONT C(31) C(32) C(34) C(33) DELU 0.015 C(18) C(19) C(20) C(21) AND CONT C(18) C(19) C(21) C(20) AND CONT C(22) C(23) C(24) C(25) AND CONT C(22) C(23) C(25) C(24) AND CONT C(27) C(28) C(29) C(30) AND CONT C(27) C(28) C(30) C(29) AND CONT C(31) C(32) C(33) C(34) AND CONT C(31) C(32) C(34) C(33) SIMU 0.015 C(18) C(19) C(20) C(21) AND CONT C(18) C(19) C(21) C(20) AND CONT C(22) C(23) C(24) C(25) AND CONT C(22) C(23) C(25) C(24) AND CONT C(27) C(28) C(29) C(30) AND CONT C(27) C(28) C(30) C(29) AND CONT C(31) C(32) C(33) C(34) AND CONT C(31) C(32) C(34) C(33) SAME P(1) C(16) C(26) P(3) AND CONT P(1) C(161) C(17) P(2) DELU 0.02 P(1) C(16) C(26) P(3) AND CONT P(1) C(161) C(17) P(2) SIMU 0.02 P(1) C(16) C(26) P(3) AND CONT P(1) C(161) C(17) P(2) SAME C(18) P(2) C(22) AND CONT C(22) P(2) C(18) AND CONT C(27) P(3) C(31) AND CONT C(31) P(3) C(27) END ; # Manually omitted reflections loop_ _oxford_refln_omitted_index_h _oxford_refln_omitted_index_k _oxford_refln_omitted_index_l _oxford_refln_omitted_flag _oxford_refln_omitted_details -3 -2 1 x . 2 -12 13 x . 2 1 10 x . _database_code_depnum_ccdc_archive 'CCDC 945335' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound2 _audit_creation_date 12-11-20 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title 045SDP12 _chemical_name_systematic Rh(dibpe)h6-BArCl4 _chemical_melting_point 'not measured' _refine_special_details ; Disorder of one of the isobutyl substituents was treated by modelling the appropriate isobutyl atoms over two sites and restraining their geometry. ; _cell_length_a 12.6148(3) _cell_length_b 12.7474(3) _cell_length_c 16.1361(3) _cell_angle_alpha 101.9704(18) _cell_angle_beta 102.9988(19) _cell_angle_gamma 106.980(2) _cell_volume 2311.91(10) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Rh 0.0927 3.6045 19.2957 0.7515 14.3501 8.2176 4.7343 25.8749 1.2892 98.6062 5.3280 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0090 0.0039 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C42 H52 B1 Cl8 P2 Rh1 # Dc = 1.46 Fooo = 1040.00 Mu = 81.17 M = 1016.16 # Found Formula = C42 H52 B1 Cl8 P2 Rh1 # Dc = 1.46 FOOO = 1040.00 Mu = 81.17 M = 1016.16 _chemical_formula_sum 'C42 H52 B1 Cl8 P2 Rh1' _chemical_formula_moiety 'C42 H52 B1 Cl8 P2 Rh1' _chemical_compound_source 'Lab S10' _chemical_formula_weight 1016.16 _cell_measurement_reflns_used 17407 _cell_measurement_theta_min 4 _cell_measurement_theta_max 76 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'yellow orange' _exptl_crystal_size_min 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.400 _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 8.117 # Sheldrick geometric approximatio 0.20 0.20 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.04 _exptl_absorpt_correction_T_max 0.20 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number . _diffrn_standards_decay_% . _diffrn_ambient_temperature 150(2) _diffrn_reflns_number 23606 _reflns_number_total 9547 _diffrn_reflns_av_R_equivalents 0.027 # Number of reflections with Friedels Law is 9547 # Theoretical number of reflections is about 19387 _diffrn_reflns_theta_min 3.792 _diffrn_reflns_theta_max 76.309 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 74.019 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 2.30 _oxford_diffrn_Wilson_scale 0.08 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.80 _refine_diff_density_max 2.06 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 9509 _refine_ls_number_restraints 108 _refine_ls_number_parameters 523 _oxford_refine_ls_R_factor_ref 0.0395 _refine_ls_wR_factor_ref 0.1050 _refine_ls_goodness_of_fit_ref 1.0037 _refine_ls_shift/su_max 0.0013928 _refine_ls_shift/su_mean 0.0000368 # The values computed with all filters except I/sigma _oxford_reflns_number_all 9509 _refine_ls_R_factor_all 0.0395 _refine_ls_wR_factor_all 0.1050 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9178 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_gt 0.1039 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.08P)^2^ + 1.51P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Cl1 Cl 0.89274(5) 0.32732(5) 0.47923(4) 0.0331 1.0000 Uani . . . . . . Cl2 Cl 1.13754(5) 0.41068(6) 0.24950(4) 0.0385 1.0000 Uani . . . . . . Cl3 Cl 0.96503(7) 1.06652(6) 0.40122(5) 0.0478 1.0000 Uani . . . . . . Cl4 Cl 1.28344(6) 0.86741(7) 0.37215(5) 0.0481 1.0000 Uani . . . . . . Cl5 Cl 0.39946(5) 0.61826(6) 0.27266(4) 0.0406 1.0000 Uani . . . . . . Cl6 Cl 0.72821(6) 0.71004(8) 0.58203(4) 0.0497 1.0000 Uani . . . . . . Cl7 Cl 0.81225(7) 0.67774(8) -0.04320(5) 0.0561 1.0000 Uani . . . . . . Cl8 Cl 0.49803(6) 0.31001(6) -0.01422(4) 0.0462 1.0000 Uani . . . . . . C1 C 0.5328(2) 0.1959(2) 0.20742(18) 0.0365 1.0000 Uani . . . . . . C2 C 0.5349(2) 0.2997(2) 0.27554(19) 0.0382 1.0000 Uani . . . . . . C3 C 0.4212(3) 0.3212(3) 0.2448(3) 0.0517 1.0000 Uani . . . . . . C4 C 0.5549(3) 0.2876(3) 0.3691(2) 0.0462 1.0000 Uani . . . . . . C5 C 0.6781(2) 0.0804(2) 0.29668(17) 0.0349 1.0000 Uani . . . . . . C6 C 0.5694(3) -0.0057(2) 0.30482(19) 0.0407 1.0000 Uani . . . . . . C7 C 0.6063(3) -0.0501(3) 0.3831(2) 0.0491 1.0000 Uani . . . . . . C8 C 0.5012(4) -0.1045(3) 0.2209(2) 0.0667 1.0000 Uani . . . . . . C9 C 0.6282(3) 0.0576(2) 0.10669(17) 0.0407 1.0000 Uani . . . . . . C10 C 0.6767(2) 0.1168(2) 0.04289(16) 0.0372 1.0000 Uani . . . . . . C11 C 0.8580(2) 0.3186(2) 0.03452(16) 0.0328 1.0000 Uani . . . . . . C12 C 0.8117(3) 0.2753(3) -0.06803(17) 0.0396 1.0000 Uani . . . . . . C13 C 0.8611(3) 0.3738(3) -0.1046(2) 0.0457 1.0000 Uani . . . . . . C14 C 0.8389(3) 0.1724(3) -0.11076(19) 0.0487 1.0000 Uani . . . . . . C19 C 0.87721(19) 0.51084(19) 0.30166(14) 0.0253 1.0000 Uani . . . . . . C20 C 0.85261(19) 0.4518(2) 0.36448(15) 0.0271 1.0000 Uani . . . . . . C21 C 0.9173(2) 0.3842(2) 0.39312(14) 0.0281 1.0000 Uani . . . . . . C22 C 1.0083(2) 0.3709(2) 0.36105(16) 0.0301 1.0000 Uani . . . . . . C23 C 1.0250(2) 0.4196(2) 0.29227(16) 0.0298 1.0000 Uani . . . . . . C24 C 0.95924(19) 0.48460(19) 0.26125(15) 0.0267 1.0000 Uani . . . . . . C25 C 0.7291(2) 0.6240(2) 0.32743(15) 0.0270 1.0000 Uani . . . . . . C26 C 0.6159(2) 0.6144(2) 0.28338(16) 0.0296 1.0000 Uani . . . . . . C27 C 0.5398(2) 0.6317(2) 0.33054(17) 0.0320 1.0000 Uani . . . . . . C28 C 0.5706(2) 0.6597(2) 0.42200(18) 0.0347 1.0000 Uani . . . . . . C29 C 0.6837(2) 0.6718(2) 0.46584(16) 0.0338 1.0000 Uani . . . . . . C30 C 0.7618(2) 0.6552(2) 0.42089(16) 0.0301 1.0000 Uani . . . . . . C31 C 0.9353(2) 0.7356(2) 0.31538(15) 0.0283 1.0000 Uani . . . . . . C32 C 0.9116(2) 0.8374(2) 0.33766(17) 0.0335 1.0000 Uani . . . . . . C33 C 1.0002(2) 0.9437(2) 0.37149(18) 0.0359 1.0000 Uani . . . . . . C34 C 1.1160(2) 0.9570(2) 0.38363(17) 0.0374 1.0000 Uani . . . . . . C35 C 1.1391(2) 0.8573(2) 0.36033(17) 0.0348 1.0000 Uani . . . . . . C36 C 1.0529(2) 0.7497(2) 0.32773(15) 0.0311 1.0000 Uani . . . . . . C37 C 0.7696(2) 0.5725(2) 0.16902(15) 0.0284 1.0000 Uani . . . . . . C38 C 0.8112(2) 0.6362(2) 0.11500(16) 0.0330 1.0000 Uani . . . . . . C39 C 0.7569(2) 0.5982(3) 0.02302(17) 0.0386 1.0000 Uani . . . . . . C40 C 0.6610(2) 0.4993(3) -0.01839(17) 0.0392 1.0000 Uani . . . . . . C41 C 0.6203(2) 0.4368(2) 0.03535(17) 0.0348 1.0000 Uani . . . . . . C42 C 0.6732(2) 0.4703(2) 0.12645(16) 0.0317 1.0000 Uani . . . . . . P1 P 0.66727(5) 0.16310(5) 0.21650(4) 0.0299 1.0000 Uani . . . . . . P2 P 0.82377(5) 0.22038(5) 0.10226(4) 0.0289 1.0000 Uani . . . . . . Rh1 Rh 0.833490(13) 0.307758(13) 0.240285(10) 0.0248 1.0000 Uani . . . . . . B1 B 0.8262(2) 0.6100(2) 0.27731(16) 0.0259 1.0000 Uani . . . . . . C15 C 0.9305(7) 0.1487(6) 0.0954(7) 0.0287 0.6148 Uani D . . 1 1 . C115 C 0.9220(14) 0.1406(11) 0.0973(12) 0.0474 0.3852 Uani D . . 1 2 . C16 C 0.9373(5) 0.0665(5) 0.1509(4) 0.0458 0.6148 Uani D . . 1 1 . C116 C 0.9653(9) 0.0875(8) 0.1679(6) 0.0467 0.3852 Uani D . . 1 2 . C18 C 0.8650(6) -0.0574(5) 0.0938(6) 0.0732 0.6148 Uani D . . 1 1 . C118 C 0.8792(8) -0.0330(9) 0.1511(8) 0.0608 0.3852 Uani D . . 1 2 . C17 C 1.0639(7) 0.0781(9) 0.1898(5) 0.0630 0.6148 Uani D . . 1 1 . C117 C 1.0852(9) 0.0826(14) 0.1679(9) 0.0593 0.3852 Uani D . . 1 2 . H11 H 0.5133 0.2102 0.1504 0.0439 1.0000 Uiso R . . . . . H12 H 0.4737 0.1283 0.2063 0.0432 1.0000 Uiso R . . . . . H21 H 0.5992 0.3665 0.2778 0.0454 1.0000 Uiso R . . . . . H31 H 0.4198 0.3862 0.2871 0.0776 1.0000 Uiso R . . . . . H32 H 0.4119 0.3356 0.1886 0.0771 1.0000 Uiso R . . . . . H33 H 0.3561 0.2541 0.2381 0.0772 1.0000 Uiso R . . . . . H41 H 0.5595 0.3573 0.4100 0.0696 1.0000 Uiso R . . . . . H42 H 0.6261 0.2713 0.3890 0.0700 1.0000 Uiso R . . . . . H43 H 0.4893 0.2248 0.3706 0.0698 1.0000 Uiso R . . . . . H52 H 0.7320 0.0406 0.2866 0.0422 1.0000 Uiso R . . . . . H51 H 0.7139 0.1386 0.3539 0.0418 1.0000 Uiso R . . . . . H61 H 0.5159 0.0343 0.3175 0.0487 1.0000 Uiso R . . . . . H72 H 0.5390 -0.1018 0.3891 0.0749 1.0000 Uiso R . . . . . H71 H 0.6589 -0.0892 0.3713 0.0751 1.0000 Uiso R . . . . . H73 H 0.6440 0.0137 0.4363 0.0748 1.0000 Uiso R . . . . . H81 H 0.4379 -0.1581 0.2320 0.1039 1.0000 Uiso R . . . . . H82 H 0.5536 -0.1436 0.2057 0.1034 1.0000 Uiso R . . . . . H83 H 0.4704 -0.0773 0.1720 0.1040 1.0000 Uiso R . . . . . H91 H 0.6609 -0.0011 0.1153 0.0493 1.0000 Uiso R . . . . . H92 H 0.5449 0.0222 0.0851 0.0485 1.0000 Uiso R . . . . . H102 H 0.6770 0.0604 -0.0070 0.0441 1.0000 Uiso R . . . . . H101 H 0.6278 0.1587 0.0215 0.0447 1.0000 Uiso R . . . . . H111 H 0.9430 0.3513 0.0521 0.0397 1.0000 Uiso R . . . . . H112 H 0.8260 0.3776 0.0524 0.0398 1.0000 Uiso R . . . . . H121 H 0.7258 0.2540 -0.0865 0.0482 1.0000 Uiso R . . . . . H131 H 0.8275 0.3493 -0.1689 0.0686 1.0000 Uiso R . . . . . H132 H 0.9437 0.3904 -0.0878 0.0683 1.0000 Uiso R . . . . . H133 H 0.8441 0.4405 -0.0783 0.0688 1.0000 Uiso R . . . . . H141 H 0.8133 0.1566 -0.1752 0.0752 1.0000 Uiso R . . . . . H142 H 0.9235 0.1886 -0.0894 0.0747 1.0000 Uiso R . . . . . H143 H 0.7968 0.1061 -0.0953 0.0745 1.0000 Uiso R . . . . . H201 H 0.7901 0.4575 0.3889 0.0332 1.0000 Uiso R . . . . . H221 H 1.0538 0.3268 0.3817 0.0356 1.0000 Uiso R . . . . . H241 H 0.9707 0.5130 0.2120 0.0323 1.0000 Uiso R . . . . . H261 H 0.5907 0.5983 0.2211 0.0361 1.0000 Uiso R . . . . . H281 H 0.5182 0.6695 0.4527 0.0418 1.0000 Uiso R . . . . . H301 H 0.8373 0.6643 0.4529 0.0368 1.0000 Uiso R . . . . . H321 H 0.8334 0.8326 0.3300 0.0400 1.0000 Uiso R . . . . . H341 H 1.1761 1.0300 0.4062 0.0455 1.0000 Uiso R . . . . . H361 H 1.0742 0.6849 0.3150 0.0377 1.0000 Uiso R . . . . . H381 H 0.8770 0.7039 0.1389 0.0394 1.0000 Uiso R . . . . . H401 H 0.6251 0.4764 -0.0806 0.0473 1.0000 Uiso R . . . . . H421 H 0.6433 0.4238 0.1593 0.0381 1.0000 Uiso R . . . . . H151 H 1.0065 0.2114 0.1193 0.0484 0.6148 Uiso R . . 1 1 . H152 H 0.9188 0.1111 0.0335 0.0481 0.6148 Uiso R . . 1 1 . H1151 H 0.9916 0.1930 0.0907 0.0363 0.3852 Uiso R . . 1 2 . H1152 H 0.8827 0.0768 0.0429 0.0362 0.3852 Uiso R . . 1 2 . H161 H 0.9063 0.0835 0.2000 0.0578 0.6148 Uiso R . . 1 1 . H1161 H 0.9664 0.1336 0.2252 0.0521 0.3852 Uiso R . . 1 2 . H181 H 0.8573 -0.1069 0.1321 0.1050 0.6148 Uiso R . . 1 1 . H183 H 0.9047 -0.0813 0.0530 0.1051 0.6148 Uiso R . . 1 1 . H182 H 0.7879 -0.0623 0.0608 0.1047 0.6148 Uiso R . . 1 1 . H1181 H 0.8382 -0.0325 0.1941 0.0852 0.3852 Uiso R . . 1 2 . H1182 H 0.9226 -0.0831 0.1573 0.0851 0.3852 Uiso R . . 1 2 . H1183 H 0.8231 -0.0598 0.0923 0.0853 0.3852 Uiso R . . 1 2 . H171 H 1.0634 0.0172 0.2175 0.0959 0.6148 Uiso R . . 1 1 . H172 H 1.0962 0.0702 0.1411 0.0959 0.6148 Uiso R . . 1 1 . H173 H 1.1071 0.1522 0.2329 0.0961 0.6148 Uiso R . . 1 1 . H1171 H 1.1127 0.0555 0.2177 0.0750 0.3852 Uiso R . . 1 2 . H1172 H 1.1375 0.1579 0.1759 0.0749 0.3852 Uiso R . . 1 2 . H1173 H 1.0821 0.0321 0.1137 0.0750 0.3852 Uiso R . . 1 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 Cl1 0.0372(3) 0.0355(3) 0.0218(2) 0.0093(2) 0.0056(2) 0.0079(2) Cl2 0.0300(3) 0.0466(3) 0.0442(3) 0.0139(3) 0.0180(2) 0.0156(2) Cl3 0.0485(4) 0.0330(3) 0.0571(4) 0.0085(3) 0.0113(3) 0.0143(3) Cl4 0.0269(3) 0.0554(4) 0.0477(4) 0.0017(3) 0.0082(3) 0.0058(3) Cl5 0.0255(3) 0.0522(4) 0.0408(3) 0.0101(3) 0.0063(2) 0.0144(2) Cl6 0.0459(4) 0.0848(5) 0.0249(3) 0.0117(3) 0.0137(3) 0.0333(4) Cl7 0.0583(4) 0.0822(5) 0.0341(3) 0.0308(4) 0.0182(3) 0.0212(4) Cl8 0.0396(3) 0.0473(4) 0.0345(3) -0.0029(3) -0.0035(3) 0.0126(3) C1 0.0239(11) 0.0439(14) 0.0353(13) 0.0122(11) 0.0055(9) 0.0053(10) C2 0.0311(12) 0.0432(14) 0.0416(14) 0.0148(11) 0.0143(10) 0.0112(10) C3 0.0377(15) 0.0621(19) 0.063(2) 0.0249(16) 0.0180(14) 0.0214(14) C4 0.0467(16) 0.0543(17) 0.0418(15) 0.0130(13) 0.0208(13) 0.0194(13) C5 0.0344(12) 0.0358(12) 0.0273(11) 0.0067(9) 0.0060(9) 0.0066(10) C6 0.0392(14) 0.0378(13) 0.0363(13) 0.0103(11) 0.0083(11) 0.0039(11) C7 0.0546(18) 0.0460(16) 0.0392(15) 0.0175(12) 0.0118(13) 0.0057(13) C8 0.073(2) 0.0522(19) 0.0405(17) 0.0127(14) 0.0044(16) -0.0167(17) C9 0.0409(14) 0.0382(13) 0.0273(12) -0.0004(10) 0.0072(10) 0.0011(11) C10 0.0341(12) 0.0415(13) 0.0231(11) 0.0004(10) 0.0042(9) 0.0051(10) C11 0.0368(12) 0.0378(12) 0.0238(11) 0.0082(9) 0.0092(9) 0.0141(10) C12 0.0415(14) 0.0478(15) 0.0270(12) 0.0089(11) 0.0096(10) 0.0142(12) C13 0.0538(17) 0.0552(17) 0.0338(13) 0.0179(12) 0.0178(12) 0.0209(14) C14 0.065(2) 0.0515(17) 0.0301(13) 0.0069(12) 0.0157(13) 0.0236(15) C19 0.0219(10) 0.0276(10) 0.0195(9) 0.0020(8) 0.0031(8) 0.0048(8) C20 0.0237(10) 0.0289(10) 0.0222(10) 0.0031(8) 0.0044(8) 0.0053(8) C21 0.0275(11) 0.0305(11) 0.0197(10) 0.0054(8) 0.0034(8) 0.0051(9) C22 0.0239(10) 0.0334(11) 0.0273(11) 0.0053(9) 0.0029(8) 0.0084(9) C23 0.0249(10) 0.0324(11) 0.0289(11) 0.0045(9) 0.0087(9) 0.0084(9) C24 0.0254(10) 0.0278(10) 0.0224(10) 0.0053(8) 0.0069(8) 0.0051(8) C25 0.0258(10) 0.0286(10) 0.0250(10) 0.0063(8) 0.0077(8) 0.0084(8) C26 0.0271(11) 0.0332(11) 0.0249(10) 0.0059(9) 0.0061(9) 0.0085(9) C27 0.0255(11) 0.0345(12) 0.0339(12) 0.0083(9) 0.0076(9) 0.0103(9) C28 0.0310(12) 0.0431(13) 0.0330(12) 0.0104(10) 0.0143(10) 0.0146(10) C29 0.0362(12) 0.0435(13) 0.0237(11) 0.0086(10) 0.0109(9) 0.0166(10) C30 0.0276(11) 0.0364(12) 0.0252(11) 0.0072(9) 0.0067(9) 0.0120(9) C31 0.0306(11) 0.0316(11) 0.0204(10) 0.0075(8) 0.0072(8) 0.0083(9) C32 0.0313(12) 0.0362(12) 0.0329(12) 0.0115(10) 0.0084(9) 0.0118(10) C33 0.0403(13) 0.0324(12) 0.0328(12) 0.0089(10) 0.0094(10) 0.0114(10) C34 0.0368(13) 0.0351(12) 0.0303(12) 0.0069(10) 0.0060(10) 0.0036(10) C35 0.0277(11) 0.0431(13) 0.0273(11) 0.0067(10) 0.0067(9) 0.0074(10) C36 0.0303(11) 0.0348(12) 0.0240(10) 0.0058(9) 0.0067(9) 0.0088(9) C37 0.0286(11) 0.0378(12) 0.0212(10) 0.0075(9) 0.0080(8) 0.0155(9) C38 0.0303(11) 0.0435(13) 0.0264(11) 0.0109(10) 0.0086(9) 0.0146(10) C39 0.0393(13) 0.0586(16) 0.0278(12) 0.0189(11) 0.0143(10) 0.0240(12) C40 0.0390(13) 0.0586(16) 0.0228(11) 0.0082(11) 0.0073(10) 0.0258(13) C41 0.0311(12) 0.0431(13) 0.0262(11) 0.0017(10) 0.0033(9) 0.0173(10) C42 0.0306(11) 0.0386(12) 0.0245(11) 0.0060(9) 0.0071(9) 0.0135(10) P1 0.0260(3) 0.0323(3) 0.0230(3) 0.0042(2) 0.0046(2) 0.0033(2) P2 0.0285(3) 0.0335(3) 0.0212(3) 0.0042(2) 0.0059(2) 0.0101(2) Rh1 0.02270(10) 0.02839(10) 0.01915(10) 0.00387(7) 0.00481(6) 0.00636(7) B1 0.0241(11) 0.0316(12) 0.0203(11) 0.0065(9) 0.0066(9) 0.0084(9) C15 0.033(3) 0.038(4) 0.030(4) 0.019(3) 0.018(3) 0.021(3) C115 0.057(9) 0.047(7) 0.028(7) -0.002(5) 0.010(6) 0.015(6) C16 0.070(4) 0.054(3) 0.038(3) 0.024(3) 0.028(3) 0.042(3) C116 0.064(5) 0.044(4) 0.034(4) 0.007(3) 0.010(4) 0.030(4) C18 0.092(5) 0.046(3) 0.096(5) 0.022(3) 0.046(4) 0.032(3) C118 0.068(6) 0.056(5) 0.066(6) 0.034(5) 0.016(5) 0.026(4) C17 0.088(5) 0.085(5) 0.038(3) 0.022(3) 0.020(3) 0.060(4) C117 0.067(6) 0.070(6) 0.054(7) 0.023(5) 0.015(5) 0.041(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 3.64(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 . C21 . 1.741(2) yes Cl2 . C23 . 1.734(2) yes Cl3 . C33 . 1.751(3) yes Cl4 . C35 . 1.751(3) yes Cl5 . C27 . 1.746(2) yes Cl6 . C29 . 1.748(2) yes Cl7 . C39 . 1.740(3) yes Cl8 . C41 . 1.755(3) yes C1 . C2 . 1.525(4) yes C1 . P1 . 1.844(3) yes C1 . H11 . 0.966 no C1 . H12 . 0.955 no C2 . C3 . 1.530(4) yes C2 . C4 . 1.522(4) yes C2 . H21 . 0.977 no C3 . H31 . 0.965 no C3 . H32 . 0.952 no C3 . H33 . 0.963 no C4 . H41 . 0.968 no C4 . H42 . 0.980 no C4 . H43 . 0.978 no C5 . C6 . 1.538(4) yes C5 . P1 . 1.836(3) yes C5 . H52 . 0.983 no C5 . H51 . 0.969 no C6 . C7 . 1.522(4) yes C6 . C8 . 1.515(4) yes C6 . H61 . 0.987 no C7 . H72 . 0.949 no C7 . H71 . 0.967 no C7 . H73 . 0.962 no C8 . H81 . 0.966 no C8 . H82 . 0.980 no C8 . H83 . 0.973 no C9 . C10 . 1.530(4) yes C9 . P1 . 1.850(3) yes C9 . H91 . 0.973 no C9 . H92 . 0.960 no C10 . P2 . 1.829(3) yes C10 . H102 . 0.963 no C10 . H101 . 0.980 no C11 . C12 . 1.543(3) yes C11 . P2 . 1.847(3) yes C11 . H111 . 0.978 no C11 . H112 . 0.976 no C12 . C13 . 1.526(4) yes C12 . C14 . 1.519(4) yes C12 . H121 . 0.993 no C13 . H131 . 0.971 no C13 . H132 . 0.962 no C13 . H133 . 0.973 no C14 . H141 . 0.975 no C14 . H142 . 0.988 no C14 . H143 . 0.972 no C19 . C20 . 1.418(3) yes C19 . C24 . 1.422(3) yes C19 . Rh1 . 2.417(2) yes C19 . B1 . 1.653(3) yes C20 . C21 . 1.425(3) yes C20 . Rh1 . 2.333(2) yes C20 . H201 . 0.972 no C21 . C22 . 1.400(3) yes C21 . Rh1 . 2.319(2) yes C22 . C23 . 1.405(3) yes C22 . Rh1 . 2.385(2) yes C22 . H221 . 0.969 no C23 . C24 . 1.419(3) yes C23 . Rh1 . 2.270(2) yes C24 . Rh1 . 2.251(2) yes C24 . H241 . 0.961 no C25 . C26 . 1.403(3) yes C25 . C30 . 1.406(3) yes C25 . B1 . 1.643(3) yes C26 . C27 . 1.389(3) yes C26 . H261 . 0.941 no C27 . C28 . 1.378(4) yes C28 . C29 . 1.390(4) yes C28 . H281 . 0.930 no C29 . C30 . 1.387(3) yes C30 . H301 . 0.936 no C31 . C32 . 1.410(4) yes C31 . C36 . 1.403(3) yes C31 . B1 . 1.661(3) yes C32 . C33 . 1.385(4) yes C32 . H321 . 0.947 no C33 . C34 . 1.383(4) yes C34 . C35 . 1.382(4) yes C34 . H341 . 0.947 no C35 . C36 . 1.383(4) yes C36 . H361 . 0.939 no C37 . C38 . 1.395(3) yes C37 . C42 . 1.406(4) yes C37 . B1 . 1.638(3) yes C38 . C39 . 1.399(4) yes C38 . H381 . 0.939 no C39 . C40 . 1.377(4) yes C40 . C41 . 1.378(4) yes C40 . H401 . 0.945 no C41 . C42 . 1.386(3) yes C42 . H421 . 0.929 no P1 . Rh1 . 2.2429(6) yes P2 . C15 . 1.845(8) yes P2 . Rh1 . 2.2325(6) yes P2 . C115 . 1.822(17) yes C15 . C16 . 1.522(5) yes C15 . H151 . 0.983 no C15 . H152 . 0.972 no C115 . C116 . 1.520(7) yes C115 . H1151 . 0.979 no C115 . H1152 . 0.974 no C16 . C18 . 1.534(6) yes C16 . C17 . 1.528(6) yes C16 . H161 . 0.973 no C116 . C118 . 1.528(6) yes C116 . C117 . 1.532(7) yes C116 . H1161 . 0.982 no C18 . H181 . 0.970 no C18 . H183 . 0.966 no C18 . H182 . 0.975 no C118 . H1181 . 0.955 no C118 . H1182 . 0.961 no C118 . H1183 . 0.969 no C17 . H171 . 0.972 no C17 . H172 . 0.964 no C17 . H173 . 0.965 no C117 . H1171 . 0.972 no C117 . H1172 . 0.956 no C117 . H1173 . 0.958 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . C1 . P1 . 119.06(18) yes C2 . C1 . H11 . 105.9 no P1 . C1 . H11 . 105.4 no C2 . C1 . H12 . 110.1 no P1 . C1 . H12 . 107.0 no H11 . C1 . H12 . 108.9 no C1 . C2 . C3 . 109.1(2) yes C1 . C2 . C4 . 113.2(2) yes C3 . C2 . C4 . 110.7(2) yes C1 . C2 . H21 . 108.1 no C3 . C2 . H21 . 108.4 no C4 . C2 . H21 . 107.2 no C2 . C3 . H31 . 110.9 no C2 . C3 . H32 . 110.9 no H31 . C3 . H32 . 108.5 no C2 . C3 . H33 . 109.7 no H31 . C3 . H33 . 109.4 no H32 . C3 . H33 . 107.5 no C2 . C4 . H41 . 109.8 no C2 . C4 . H42 . 111.7 no H41 . C4 . H42 . 109.6 no C2 . C4 . H43 . 109.8 no H41 . C4 . H43 . 107.7 no H42 . C4 . H43 . 108.3 no C6 . C5 . P1 . 121.63(19) yes C6 . C5 . H52 . 108.3 no P1 . C5 . H52 . 107.9 no C6 . C5 . H51 . 106.0 no P1 . C5 . H51 . 103.9 no H52 . C5 . H51 . 108.4 no C5 . C6 . C7 . 108.7(2) yes C5 . C6 . C8 . 113.7(3) yes C7 . C6 . C8 . 110.6(3) yes C5 . C6 . H61 . 109.0 no C7 . C6 . H61 . 108.0 no C8 . C6 . H61 . 106.6 no C6 . C7 . H72 . 108.8 no C6 . C7 . H71 . 108.6 no H72 . C7 . H71 . 110.0 no C6 . C7 . H73 . 109.0 no H72 . C7 . H73 . 109.7 no H71 . C7 . H73 . 110.6 no C6 . C8 . H81 . 109.4 no C6 . C8 . H82 . 108.0 no H81 . C8 . H82 . 108.6 no C6 . C8 . H83 . 111.1 no H81 . C8 . H83 . 109.6 no H82 . C8 . H83 . 110.1 no C10 . C9 . P1 . 110.15(19) yes C10 . C9 . H91 . 110.3 no P1 . C9 . H91 . 107.9 no C10 . C9 . H92 . 111.9 no P1 . C9 . H92 . 107.8 no H91 . C9 . H92 . 108.5 no C9 . C10 . P2 . 109.42(17) yes C9 . C10 . H102 . 109.8 no P2 . C10 . H102 . 110.9 no C9 . C10 . H101 . 109.2 no P2 . C10 . H101 . 108.1 no H102 . C10 . H101 . 109.3 no C12 . C11 . P2 . 121.05(19) yes C12 . C11 . H111 . 108.1 no P2 . C11 . H111 . 105.6 no C12 . C11 . H112 . 106.0 no P2 . C11 . H112 . 105.3 no H111 . C11 . H112 . 110.7 no C11 . C12 . C13 . 108.6(2) yes C11 . C12 . C14 . 115.4(2) yes C13 . C12 . C14 . 108.9(2) yes C11 . C12 . H121 . 108.4 no C13 . C12 . H121 . 107.3 no C14 . C12 . H121 . 107.9 no C12 . C13 . H131 . 109.3 no C12 . C13 . H132 . 105.4 no H131 . C13 . H132 . 111.1 no C12 . C13 . H133 . 110.3 no H131 . C13 . H133 . 110.2 no H132 . C13 . H133 . 110.4 no C12 . C14 . H141 . 109.1 no C12 . C14 . H142 . 109.8 no H141 . C14 . H142 . 110.1 no C12 . C14 . H143 . 109.0 no H141 . C14 . H143 . 108.9 no H142 . C14 . H143 . 110.0 no C20 . C19 . C24 . 114.8(2) yes C20 . C19 . Rh1 . 69.42(13) yes C24 . C19 . Rh1 . 65.97(12) yes C20 . C19 . B1 . 126.2(2) yes C24 . C19 . B1 . 118.89(19) yes Rh1 . C19 . B1 . 137.67(14) yes C19 . C20 . C21 . 121.8(2) yes C19 . C20 . Rh1 . 75.90(13) yes C21 . C20 . Rh1 . 71.62(13) yes C19 . C20 . H201 . 119.4 no C21 . C20 . H201 . 118.8 no Rh1 . C20 . H201 . 125.1 no Cl1 . C21 . C20 . 119.05(18) yes Cl1 . C21 . C22 . 118.11(18) yes C20 . C21 . C22 . 122.5(2) yes Cl1 . C21 . Rh1 . 130.76(12) yes C20 . C21 . Rh1 . 72.72(13) yes C22 . C21 . Rh1 . 75.29(13) yes C21 . C22 . C23 . 115.7(2) yes C21 . C22 . Rh1 . 70.13(13) yes C23 . C22 . Rh1 . 68.00(13) yes C21 . C22 . H221 . 122.6 no C23 . C22 . H221 . 121.6 no Rh1 . C22 . H221 . 128.7 no Cl2 . C23 . C22 . 119.34(19) yes Cl2 . C23 . C24 . 118.10(18) yes C22 . C23 . C24 . 122.3(2) yes Cl2 . C23 . Rh1 . 129.60(13) yes C22 . C23 . Rh1 . 76.97(14) yes C24 . C23 . Rh1 . 70.99(13) yes C19 . C24 . C23 . 122.0(2) yes C19 . C24 . Rh1 . 78.78(13) yes C23 . C24 . Rh1 . 72.43(13) yes C19 . C24 . H241 . 118.5 no C23 . C24 . H241 . 119.6 no Rh1 . C24 . H241 . 121.6 no C26 . C25 . C30 . 116.5(2) yes C26 . C25 . B1 . 124.2(2) yes C30 . C25 . B1 . 119.1(2) yes C25 . C26 . C27 . 121.0(2) yes C25 . C26 . H261 . 120.3 no C27 . C26 . H261 . 118.7 no Cl5 . C27 . C26 . 119.30(19) yes Cl5 . C27 . C28 . 118.03(19) yes C26 . C27 . C28 . 122.7(2) yes C27 . C28 . C29 . 116.4(2) yes C27 . C28 . H281 . 121.7 no C29 . C28 . H281 . 121.9 no Cl6 . C29 . C28 . 118.29(19) yes Cl6 . C29 . C30 . 119.22(19) yes C28 . C29 . C30 . 122.5(2) yes C25 . C30 . C29 . 120.9(2) yes C25 . C30 . H301 . 119.3 no C29 . C30 . H301 . 119.8 no C32 . C31 . C36 . 115.8(2) yes C32 . C31 . B1 . 119.4(2) yes C36 . C31 . B1 . 124.8(2) yes C31 . C32 . C33 . 121.3(2) yes C31 . C32 . H321 . 119.0 no C33 . C32 . H321 . 119.7 no Cl3 . C33 . C32 . 118.9(2) yes Cl3 . C33 . C34 . 118.4(2) yes C32 . C33 . C34 . 122.7(2) yes C33 . C34 . C35 . 116.1(2) yes C33 . C34 . H341 . 122.3 no C35 . C34 . H341 . 121.7 no Cl4 . C35 . C34 . 118.7(2) yes Cl4 . C35 . C36 . 118.5(2) yes C34 . C35 . C36 . 122.8(2) yes C31 . C36 . C35 . 121.5(2) yes C31 . C36 . H361 . 119.6 no C35 . C36 . H361 . 118.9 no C38 . C37 . C42 . 116.9(2) yes C38 . C37 . B1 . 124.0(2) yes C42 . C37 . B1 . 119.2(2) yes C37 . C38 . C39 . 120.2(3) yes C37 . C38 . H381 . 121.2 no C39 . C38 . H381 . 118.6 no Cl7 . C39 . C38 . 119.3(2) yes Cl7 . C39 . C40 . 117.8(2) yes C38 . C39 . C40 . 122.9(3) yes C39 . C40 . C41 . 116.7(2) yes C39 . C40 . H401 . 121.1 no C41 . C40 . H401 . 122.2 no Cl8 . C41 . C40 . 118.4(2) yes Cl8 . C41 . C42 . 119.4(2) yes C40 . C41 . C42 . 122.1(3) yes C37 . C42 . C41 . 121.2(2) yes C37 . C42 . H421 . 120.2 no C41 . C42 . H421 . 118.6 no C9 . P1 . C1 . 101.02(13) yes C9 . P1 . C5 . 104.81(13) yes C1 . P1 . C5 . 107.98(12) yes C9 . P1 . Rh1 . 110.34(9) yes C1 . P1 . Rh1 . 118.07(9) yes C5 . P1 . Rh1 . 113.19(8) yes C11 . P2 . C10 . 106.77(12) yes C11 . P2 . Rh1 . 114.10(8) yes C10 . P2 . Rh1 . 109.97(9) yes C11 . P2 . C15 . 101.1(3) yes C10 . P2 . C15 . 109.6(3) yes Rh1 . P2 . C15 . 114.8(3) yes C11 . P2 . C10 . 106.77(12) yes C11 . P2 . Rh1 . 114.10(8) yes C10 . P2 . Rh1 . 109.97(9) yes C11 . P2 . C115 . 105.0(5) yes C10 . P2 . C115 . 106.4(5) yes Rh1 . P2 . C115 . 114.0(6) yes C21 . Rh1 . C20 . 35.66(8) yes C21 . Rh1 . C23 . 62.31(8) yes C20 . Rh1 . C23 . 74.23(8) yes C21 . Rh1 . C24 . 74.69(8) yes C20 . Rh1 . C24 . 62.91(8) yes C23 . Rh1 . C24 . 36.58(9) yes C21 . Rh1 . C22 . 34.59(8) yes C20 . Rh1 . C22 . 63.30(8) yes C23 . Rh1 . C22 . 35.02(9) yes C24 . Rh1 . C22 . 64.42(8) yes C21 . Rh1 . C19 . 63.22(8) yes C20 . Rh1 . C19 . 34.68(8) yes C23 . Rh1 . C19 . 63.93(8) yes C24 . Rh1 . C19 . 35.25(8) yes C22 . Rh1 . C19 . 75.02(8) yes C21 . Rh1 . P1 . 106.97(6) yes C20 . Rh1 . P1 . 106.98(6) yes C23 . Rh1 . P1 . 160.65(7) yes C24 . Rh1 . P1 . 160.99(6) yes C22 . Rh1 . P1 . 127.52(6) yes C21 . Rh1 . P2 . 155.50(6) yes C20 . Rh1 . P2 . 160.38(6) yes C23 . Rh1 . P2 . 99.43(6) yes C24 . Rh1 . P2 . 100.77(6) yes C22 . Rh1 . P2 . 121.48(6) yes C19 . Rh1 . P1 . 127.87(6) yes C19 . Rh1 . P2 . 125.80(6) yes P1 . Rh1 . P2 . 85.23(2) yes C31 . B1 . C19 . 108.46(18) yes C31 . B1 . C25 . 106.51(18) yes C19 . B1 . C25 . 111.42(18) yes C31 . B1 . C37 . 111.91(19) yes C19 . B1 . C37 . 107.57(18) yes C25 . B1 . C37 . 111.00(18) yes P2 . C15 . C16 . 117.3(6) yes P2 . C15 . H151 . 104.7 no C16 . C15 . H151 . 105.6 no P2 . C15 . H152 . 109.5 no C16 . C15 . H152 . 110.5 no H151 . C15 . H152 . 108.9 no P2 . C115 . C116 . 125.3(11) yes P2 . C115 . H1151 . 105.4 no C116 . C115 . H1151 . 106.0 no P2 . C115 . H1152 . 105.2 no C116 . C115 . H1152 . 105.1 no H1151 . C115 . H1152 . 109.2 no C15 . C16 . C18 . 110.24(7) yes C15 . C16 . C17 . 110.24(7) yes C18 . C16 . C17 . 109.96(7) yes C15 . C16 . H161 . 110.5 no C18 . C16 . H161 . 107.7 no C17 . C16 . H161 . 108.1 no C115 . C116 . C118 . 110.25(7) yes C115 . C116 . C117 . 110.25(7) yes C118 . C116 . C117 . 109.97(7) yes C115 . C116 . H1161 . 107.4 no C118 . C116 . H1161 . 106.3 no C117 . C116 . H1161 . 112.6 no C16 . C18 . H181 . 109.3 no C16 . C18 . H183 . 108.7 no H181 . C18 . H183 . 109.3 no C16 . C18 . H182 . 110.2 no H181 . C18 . H182 . 109.5 no H183 . C18 . H182 . 109.9 no C116 . C118 . H1181 . 109.7 no C116 . C118 . H1182 . 108.1 no H1181 . C118 . H1182 . 108.9 no C116 . C118 . H1183 . 110.9 no H1181 . C118 . H1183 . 108.6 no H1182 . C118 . H1183 . 110.6 no C16 . C17 . H171 . 107.5 no C16 . C17 . H172 . 107.2 no H171 . C17 . H172 . 111.4 no C16 . C17 . H173 . 110.3 no H171 . C17 . H173 . 110.6 no H172 . C17 . H173 . 109.8 no C116 . C117 . H1171 . 107.4 no C116 . C117 . H1172 . 109.3 no H1171 . C117 . H1172 . 109.5 no C116 . C117 . H1173 . 112.0 no H1171 . C117 . H1173 . 109.6 no H1172 . C117 . H1173 . 109.0 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C36 . H361 . C24 . 131.11(8) 0.939 2.393 3.092(6) yes _iucr_refine_instruction_details_constraints ; # # Punched on 20/11/12 at 13:49:04 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) H ( 33,X'S) RIDE C ( 4,X'S) H ( 41,X'S) H ( 42,X'S) H ( 43,X'S) RIDE C ( 5,X'S) H ( 52,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 72,X'S) H ( 71,X'S) H ( 73,X'S) RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) H ( 83,X'S) RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) RIDE C ( 10,X'S) H ( 102,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) H ( 132,X'S) H ( 133,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) RIDE C ( 115,X'S) H (1151,X'S) H (1152,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 116,X'S) H (1161,X'S) RIDE C ( 18,X'S) H ( 181,X'S) H ( 183,X'S) H ( 182,X'S) RIDE C ( 118,X'S) H (1181,X'S) H (1182,X'S) H (1183,X'S) RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) H ( 173,X'S) RIDE C ( 117,X'S) H (1171,X'S) H (1172,X'S) H (1173,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 20/11/12 at 13:49:04 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) SAME C(15) C(16) C(17) C(18) AND CONT C(15) C(16) C(18) C(17) AND CONT C(115) C(116) C(117) C(118) AND CONT C(115) C(116) C(118) C(117) DELU 0.02 C(15) C(16) C(17) C(18) AND CONT C(15) C(16) C(18) C(17) AND CONT C(115) C(116) C(117) C(118) AND CONT C(115) C(116) C(118) C(117) SIMU 0.02 C(15) C(16) C(17) C(18) AND CONT C(15) C(16) C(18) C(17) AND CONT C(115) C(116) C(117) C(118) AND CONT C(115) C(116) C(118) C(117) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 945336' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound3 _audit_creation_date 13-03-18 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title 051SDP12 _chemical_name_systematic '[Rh(dibpe)Cl{C6ClH3(B(ArCl)3)}]2' _chemical_melting_point 'not measured' _refine_special_details ; Several molecules of dichloromethane were present in the structure, some of which refined with an occupancy less than unity, consistent with the crystals cracking when withdrawn from the solvent as dichloromethane evaporated. The solvent molecules were restrained together to maintain sensible geometries and in two cases the molecule was modelled over two sites (one of which occurs across a symmetry plane). A final disordered solvent molecule could not be adequately modelled and so was treated using the SQUEEZE algorithm leaving a void from which the electron density was removed. Analysis of the residual electron density at the end of the refinement suggests a minor component is present and unaccounted for with small amounts of electron density occuring nearby some of the rhodium, chlorine and phosphorus atoms in one half of the molecule. This component is very small and could not be modelled,the origin of this is unknown, although partial oxidation of one phosphourus could lead to a distortion that could explain this. ; 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 0.187 0.647 0.162 13 0 ' ' 2 0.500 0.000 1.000 117 36 ' ' 3 0.813 0.353 0.838 13 0 ' ' _platon_squeeze_details ; The discrete Fourier transform of the void region were treated as contributions to the A and B parts of the calculated structure factors. ; _cell_length_a 13.2301(3) _cell_length_b 17.4742(5) _cell_length_c 23.2939(5) _cell_angle_alpha 78.048(2) _cell_angle_beta 88.4952(19) _cell_angle_gamma 77.569(2) _cell_volume 5144.0(2) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Rh 0.0927 3.6045 19.2957 0.7515 14.3501 8.2176 4.7343 25.8749 1.2892 98.6062 5.3280 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0090 0.0039 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C84 H104 B2 Cl16 O1 P4 Rh2 # Dc = 1.32 Fooo = 2340.61 Mu = 73.08 M = 2052.35 # Found Formula = C87.10 H110.21 B2 Cl22.21 P4 Rh2 # Dc = 1.48 FOOO = 2340.61 Mu = 88.13 M = 2295.84 _chemical_formula_sum 'C87.1 H110.2 B2 Cl22.2 P4 Rh2' _chemical_formula_moiety 'C84 H104 B2 Cl16 P4 Rh2, 3.10(C H2 Cl2)' _chemical_compound_source 'CRL, Universtity of Oxford' _chemical_formula_weight 2295.84 _cell_measurement_reflns_used 27687 _cell_measurement_theta_min 3 _cell_measurement_theta_max 76 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_min 0.035 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_max 0.217 _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2340.614 _exptl_absorpt_coefficient_mu 8.813 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 2 0 0.0200 0.0005 2.0010 0.0024 -0.1588 -0.0872 -0.0351 0 -2 0 0.0150 -0.0005 -2.0010 -0.0024 0.1588 0.0872 0.0351 1 0 -1 0.1000 1.0000 0.0010 -1.0005 0.0511 -0.0185 -0.1246 -1 0 1 0.0900 -1.0000 -0.0010 1.0005 -0.0511 0.0185 0.1246 0 0 -1 0.0900 -0.0002 0.0008 -1.0002 0.0215 -0.0617 -0.0175 0 0 1 0.0900 0.0002 -0.0008 1.0002 -0.0215 0.0617 0.0175 1 1 2 0.1100 1.0008 0.9993 2.0013 -0.0928 0.1230 -0.0897 -1 -1 -3 0.1000 -1.0010 -0.9985 -3.0015 0.1144 -0.1847 0.0723 3 2 1 0.1000 3.0013 2.0011 1.0017 -0.0916 0.1041 -0.3391 _exptl_absorpt_correction_T_min 0.327 _exptl_absorpt_correction_T_max 0.781 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 54944 _reflns_number_total 21352 _diffrn_reflns_av_R_equivalents 0.028 # Number of reflections with Friedels Law is 21352 # Theoretical number of reflections is about 43331 _diffrn_reflns_theta_min 3.421 _diffrn_reflns_theta_max 76.668 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 74.368 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min -21 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _oxford_diffrn_Wilson_B_factor 2.27 _oxford_diffrn_Wilson_scale 0.33 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.75 _refine_diff_density_max 3.17 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 21268 _refine_ls_number_restraints 170 _refine_ls_number_parameters 1110 _oxford_refine_ls_R_factor_ref 0.0585 _refine_ls_wR_factor_ref 0.1381 _refine_ls_goodness_of_fit_ref 0.9822 _refine_ls_shift/su_max 0.0163011 _refine_ls_shift/su_mean 0.0001459 # The values computed with all filters except I/sigma _oxford_reflns_number_all 21268 _refine_ls_R_factor_all 0.0585 _refine_ls_wR_factor_all 0.1381 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 18963 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_gt 0.1351 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +16.61P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Cl1 Cl 0.22191(7) 0.48339(5) 0.81817(4) 0.0264 1.0000 Uani . . . . . . C1 C -0.0033(4) 0.5191(3) 0.9087(2) 0.0447 1.0000 Uani . . . . . . P1 P 0.12948(7) 0.66970(5) 0.84235(4) 0.0243 1.0000 Uani . . . . . . Rh1 Rh 0.208104(19) 0.622129(15) 0.766098(11) 0.0213 1.0000 Uani . . . . . . B1 B 0.4871(3) 0.7693(2) 0.86813(17) 0.0229 1.0000 Uani . . . . . . Cl2 Cl 0.27147(7) 0.55919(5) 0.68147(4) 0.0271 1.0000 Uani . . . . . . C2 C -0.1542(3) 0.5960(3) 0.8435(2) 0.0472 1.0000 Uani . . . . . . P2 P 0.17897(8) 0.74895(6) 0.71567(4) 0.0273 1.0000 Uani . . . . . . Rh2 Rh 0.286126(19) 0.418415(16) 0.735247(12) 0.0246 1.0000 Uani . . . . . . B2 B 0.0487(3) 0.2378(2) 0.63056(16) 0.0224 1.0000 Uani . . . . . . Cl3 Cl 0.62940(7) 0.49074(6) 0.80182(6) 0.0420 1.0000 Uani . . . . . . C3 C -0.0372(3) 0.5798(3) 0.85145(19) 0.0339 1.0000 Uani . . . . . . P3 P 0.39667(8) 0.35589(7) 0.67769(5) 0.0364 1.0000 Uani . . . . . . Cl4 Cl 0.15744(9) 1.00099(6) 0.78909(5) 0.0415 1.0000 Uani . . . . . . C4 C -0.0061(3) 0.6600(2) 0.84911(18) 0.0310 1.0000 Uani . . . . . . P4 P 0.32874(8) 0.30356(6) 0.80075(5) 0.0347 1.0000 Uani . . . . . . Cl5 Cl 0.20776(9) 0.88482(7) 1.02063(5) 0.0467 1.0000 Uani . . . . . . C5 C 0.1099(5) 0.7201(3) 0.9764(2) 0.0529 1.0000 Uani . . . . . . Cl6 Cl 0.70772(14) 0.83573(11) 0.67430(6) 0.0740 1.0000 Uani . . . . . . C6 C 0.2205(4) 0.5867(4) 1.0208(2) 0.0533 1.0000 Uani . . . . . . Cl7 Cl 0.61597(9) 1.04408(6) 0.81863(6) 0.0467 1.0000 Uani . . . . . . C7 C 0.1452(3) 0.6338(3) 0.97109(18) 0.0366 1.0000 Uani . . . . . . Cl8 Cl 0.84198(8) 0.70215(8) 0.99431(5) 0.0439 1.0000 Uani . . . . . . C8 C 0.1989(3) 0.6253(2) 0.91226(17) 0.0304 1.0000 Uani . . . . . . Cl9 Cl 0.54467(8) 0.53730(6) 1.06143(4) 0.0383 1.0000 Uani . . . . . . C9 C 0.1135(3) 0.7793(2) 0.82840(18) 0.0313 1.0000 Uani . . . . . . Cl10 Cl -0.13698(8) 0.47765(8) 0.72931(7) 0.0586 1.0000 Uani . . . . . . C10 C 0.1093(4) 0.8155(2) 0.76254(19) 0.0382 1.0000 Uani . . . . . . Cl11 Cl -0.00583(11) 0.46362(6) 0.43435(4) 0.0467 1.0000 Uani . . . . . . C11 C 0.0045(3) 0.6481(3) 0.6910(2) 0.0383 1.0000 Uani . . . . . . Cl12 Cl -0.28358(11) 0.27940(10) 0.48760(6) 0.0633 1.0000 Uani . . . . . . C12 C -0.0740(4) 0.7595(3) 0.6077(2) 0.0450 1.0000 Uani . . . . . . Cl13 Cl -0.08726(9) -0.03359(6) 0.66026(5) 0.0452 1.0000 Uani . . . . . . C13 C -0.0101(3) 0.7373(3) 0.66475(19) 0.0346 1.0000 Uani . . . . . . Cl14 Cl -0.14109(14) 0.13622(11) 0.83089(6) 0.0707 1.0000 Uani . . . . . . C14 C 0.0939(3) 0.7621(2) 0.65263(18) 0.0330 1.0000 Uani . . . . . . Cl15 Cl 0.34697(15) 0.16072(15) 0.47693(7) 0.0997 1.0000 Uani . . . . . . C15 C 0.2938(4) 0.7830(3) 0.6842(2) 0.0420 1.0000 Uani . . . . . . Cl16 Cl 0.40545(8) 0.03924(6) 0.70807(5) 0.0439 1.0000 Uani . . . . . . C16 C 0.2809(5) 0.8547(3) 0.6318(2) 0.0507 1.0000 Uani . . . . . . C17 C 0.2177(5) 0.9309(3) 0.6456(2) 0.0536 1.0000 Uani . . . . . . C18 C 0.3894(5) 0.8652(4) 0.6126(3) 0.0725 1.0000 Uani . . . . . . C19 C 0.3784(6) 0.4928(4) 0.5490(3) 0.0725 1.0000 Uani . . . . . . C20 C 0.3113(5) 0.4289(4) 0.5646(3) 0.0621 1.0000 Uani . . . . . . C21 C 0.2799(6) 0.4098(5) 0.5061(3) 0.0835 1.0000 Uani . . . . . . C22 C 0.3687(4) 0.3545(4) 0.6027(2) 0.0570 1.0000 Uani . . . . . . C23 C 0.6881(5) 0.3020(4) 0.7022(3) 0.0733 1.0000 Uani . . . . . . C24 C 0.6673(4) 0.4164(4) 0.6180(3) 0.0671 1.0000 Uani . . . . . . C25 C 0.6143(4) 0.3553(3) 0.6536(2) 0.0477 1.0000 Uani . . . . . . C26 C 0.5133(3) 0.3974(3) 0.6798(2) 0.0426 1.0000 Uani . . . . . . C27 C 0.4377(4) 0.2468(3) 0.7128(2) 0.0460 1.0000 Uani . . . . . . C28 C 0.3728(4) 0.2212(3) 0.7640(2) 0.0416 1.0000 Uani . . . . . . C29 C 0.6179(4) 0.2810(3) 0.8811(2) 0.0507 1.0000 Uani . . . . . . C30 C 0.4970(4) 0.1893(3) 0.9129(2) 0.0524 1.0000 Uani . . . . . . C31 C 0.5293(4) 0.2482(3) 0.8622(2) 0.0416 1.0000 Uani . . . . . . C32 C 0.4397(3) 0.3193(3) 0.8392(2) 0.0379 1.0000 Uani . . . . . . C33 C 0.1703(8) 0.1550(4) 0.8636(4) 0.0943 1.0000 Uani . . . . . . C34 C 0.0448(5) 0.2832(6) 0.8621(3) 0.0837 1.0000 Uani . . . . . . C35 C 0.1467(4) 0.2449(3) 0.8397(2) 0.0489 1.0000 Uani . . . . . . C36 C 0.2331(4) 0.2801(3) 0.8566(2) 0.0445 1.0000 Uani . . . . . . C37 C 0.3479(3) 0.6317(2) 0.79420(15) 0.0232 1.0000 Uani . . . . . . C38 C 0.4293(3) 0.5682(2) 0.78925(16) 0.0259 1.0000 Uani . . . . . . C39 C 0.5269(3) 0.5706(2) 0.80836(17) 0.0275 1.0000 Uani . . . . . . C40 C 0.5455(3) 0.6321(2) 0.83246(16) 0.0265 1.0000 Uani . . . . . . C41 C 0.4649(3) 0.6971(2) 0.83762(15) 0.0230 1.0000 Uani . . . . . . C42 C 0.3672(3) 0.6948(2) 0.81724(15) 0.0222 1.0000 Uani . . . . . . C43 C 0.5507(3) 0.8280(2) 0.82411(16) 0.0247 1.0000 Uani . . . . . . C44 C 0.5571(3) 0.9018(2) 0.83723(17) 0.0292 1.0000 Uani . . . . . . C45 C 0.6089(3) 0.9530(2) 0.80041(19) 0.0322 1.0000 Uani . . . . . . C46 C 0.6566(3) 0.9348(3) 0.75013(19) 0.0382 1.0000 Uani . . . . . . C47 C 0.6500(4) 0.8622(3) 0.73801(19) 0.0415 1.0000 Uani . . . . . . C48 C 0.5982(3) 0.8097(3) 0.77341(18) 0.0332 1.0000 Uani . . . . . . C49 C 0.5581(3) 0.7222(2) 0.92711(15) 0.0235 1.0000 Uani . . . . . . C50 C 0.6561(3) 0.7345(2) 0.93781(16) 0.0269 1.0000 Uani . . . . . . C51 C 0.7176(3) 0.6868(3) 0.98457(17) 0.0303 1.0000 Uani . . . . . . C52 C 0.6860(3) 0.6252(2) 1.02329(17) 0.0312 1.0000 Uani . . . . . . C53 C 0.5873(3) 0.6140(2) 1.01333(16) 0.0288 1.0000 Uani . . . . . . C54 C 0.5249(3) 0.6602(2) 0.96686(16) 0.0260 1.0000 Uani . . . . . . C55 C 0.3783(3) 0.8277(2) 0.88350(16) 0.0246 1.0000 Uani . . . . . . C56 C 0.3412(3) 0.8291(2) 0.94028(16) 0.0280 1.0000 Uani . . . . . . C57 C 0.2514(3) 0.8835(3) 0.94917(17) 0.0325 1.0000 Uani . . . . . . C58 C 0.1938(3) 0.9373(2) 0.90411(18) 0.0325 1.0000 Uani . . . . . . C59 C 0.2298(3) 0.9357(2) 0.84800(17) 0.0297 1.0000 Uani . . . . . . C60 C 0.3201(3) 0.8834(2) 0.83747(16) 0.0268 1.0000 Uani . . . . . . C61 C 0.1603(3) 0.3861(2) 0.70862(15) 0.0231 1.0000 Uani . . . . . . C62 C 0.0703(3) 0.4353(2) 0.72303(18) 0.0291 1.0000 Uani . . . . . . C63 C -0.0231(3) 0.4204(2) 0.70767(19) 0.0324 1.0000 Uani . . . . . . C64 C -0.0287(3) 0.3609(2) 0.67806(17) 0.0276 1.0000 Uani . . . . . . C65 C 0.0612(3) 0.3096(2) 0.66391(15) 0.0226 1.0000 Uani . . . . . . C66 C 0.1560(3) 0.3241(2) 0.68015(15) 0.0232 1.0000 Uani . . . . . . C67 C -0.0078(3) 0.1727(2) 0.67362(16) 0.0243 1.0000 Uani . . . . . . C68 C -0.0458(3) 0.1801(2) 0.72890(17) 0.0309 1.0000 Uani . . . . . . C69 C -0.0951(3) 0.1234(3) 0.76189(18) 0.0377 1.0000 Uani . . . . . . C70 C -0.1088(3) 0.0573(3) 0.74195(19) 0.0369 1.0000 Uani . . . . . . C71 C -0.0700(3) 0.0490(2) 0.68773(18) 0.0321 1.0000 Uani . . . . . . C72 C -0.0195(3) 0.1038(2) 0.65402(17) 0.0280 1.0000 Uani . . . . . . C73 C -0.0223(3) 0.2825(2) 0.57115(16) 0.0255 1.0000 Uani . . . . . . C74 C -0.1134(3) 0.2625(2) 0.55608(17) 0.0311 1.0000 Uani . . . . . . C75 C -0.1690(3) 0.3048(3) 0.50506(19) 0.0368 1.0000 Uani . . . . . . C76 C -0.1379(4) 0.3669(3) 0.46724(18) 0.0384 1.0000 Uani . . . . . . C77 C -0.0483(4) 0.3869(2) 0.48229(17) 0.0341 1.0000 Uani . . . . . . C78 C 0.0081(3) 0.3466(2) 0.53285(16) 0.0301 1.0000 Uani . . . . . . C79 C 0.1627(3) 0.1885(2) 0.61451(16) 0.0257 1.0000 Uani . . . . . . C80 C 0.2285(3) 0.1401(2) 0.66043(17) 0.0268 1.0000 Uani . . . . . . C81 C 0.3263(3) 0.0988(2) 0.64954(19) 0.0320 1.0000 Uani . . . . . . C82 C 0.3650(4) 0.1030(3) 0.5936(2) 0.0446 1.0000 Uani . . . . . . C83 C 0.3003(4) 0.1511(3) 0.5484(2) 0.0506 1.0000 Uani . . . . . . C84 C 0.2020(3) 0.1927(3) 0.55769(18) 0.0378 1.0000 Uani . . . . . . C201 C 0.8297(3) 0.9254(5) 0.9258(3) 0.0862 1.0000 Uani D . . . . . Cl202 Cl 0.93819(14) 0.91212(11) 0.97026(9) 0.0827 1.0000 Uani D . . . . . Cl203 Cl 0.85110(11) 0.87810(9) 0.86682(7) 0.0655 1.0000 Uani D . . . . . C204 C 0.5821(5) 0.6729(7) 0.6547(6) 0.1146 0.6678 Uani D . . . . . Cl205 Cl 0.7085(3) 0.6297(2) 0.6506(3) 0.1396 0.6678 Uani D . . . . . Cl206 Cl 0.49976(16) 0.63928(16) 0.61439(15) 0.0822 0.6678 Uani D . . . . . C207 C 0.6681(11) 0.1080(4) 0.5628(3) 0.0815 0.650(5) Uani D . P 1 1 . Cl208 Cl 0.6563(2) 0.01193(16) 0.55954(14) 0.0796 0.650(5) Uani D . P 1 1 . Cl209 Cl 0.6502(6) 0.1306(3) 0.6320(3) 0.0790 0.650(5) Uani D . P 1 1 . C210 C 0.7003(14) 0.0717(15) 0.5845(8) 0.1192 0.350(5) Uani D . P 1 2 . Cl211 Cl 0.6652(15) 0.1261(10) 0.6381(5) 0.1211 0.350(5) Uani D . P 1 2 . Cl212 Cl 0.6122(6) 0.0931(5) 0.5275(3) 0.1198 0.350(5) Uani D . P 1 2 . C213 C 0.9314(10) 0.9788(7) 0.4975(6) 0.0716 0.435(4) Uani D . P 2 -1 . Cl214 Cl 0.9304(9) 1.0797(8) 0.4873(7) 0.0708 0.435(4) Uani D . P 2 -1 . Cl215 Cl 1.0537(11) 0.9172(7) 0.5036(7) 0.0738 0.435(4) Uani D . P 2 -1 . H11 H 0.0708 0.5098 0.9149 0.0666 1.0000 Uiso R . . . . . H12 H -0.0371 0.5385 0.9414 0.0667 1.0000 Uiso R . . . . . H13 H -0.0210 0.4692 0.9066 0.0669 1.0000 Uiso R . . . . . H21 H -0.1716 0.6327 0.8068 0.0697 1.0000 Uiso R . . . . . H22 H -0.1858 0.6194 0.8752 0.0697 1.0000 Uiso R . . . . . H23 H -0.1743 0.5464 0.8432 0.0699 1.0000 Uiso R . . . . . H31 H -0.0055 0.5578 0.8182 0.0396 1.0000 Uiso R . . . . . H41 H -0.0313 0.6792 0.8844 0.0365 1.0000 Uiso R . . . . . H42 H -0.0418 0.6971 0.8151 0.0371 1.0000 Uiso R . . . . . H51 H 0.0570 0.7477 0.9465 0.0790 1.0000 Uiso R . . . . . H52 H 0.0836 0.7224 1.0153 0.0789 1.0000 Uiso R . . . . . H53 H 0.1686 0.7447 0.9706 0.0789 1.0000 Uiso R . . . . . H61 H 0.2389 0.5323 1.0172 0.0788 1.0000 Uiso R . . . . . H62 H 0.1900 0.5906 1.0582 0.0786 1.0000 Uiso R . . . . . H63 H 0.2804 0.6091 1.0175 0.0788 1.0000 Uiso R . . . . . H71 H 0.0844 0.6093 0.9733 0.0441 1.0000 Uiso R . . . . . H81 H 0.2599 0.6481 0.9112 0.0360 1.0000 Uiso R . . . . . H82 H 0.2204 0.5687 0.9135 0.0359 1.0000 Uiso R . . . . . H91 H 0.1707 0.7918 0.8475 0.0383 1.0000 Uiso R . . . . . H92 H 0.0490 0.8002 0.8457 0.0375 1.0000 Uiso R . . . . . H101 H 0.1390 0.8615 0.7567 0.0465 1.0000 Uiso R . . . . . H102 H 0.0378 0.8305 0.7504 0.0460 1.0000 Uiso R . . . . . H111 H 0.0451 0.6343 0.7271 0.0567 1.0000 Uiso R . . . . . H112 H -0.0621 0.6353 0.6987 0.0568 1.0000 Uiso R . . . . . H113 H 0.0398 0.6186 0.6636 0.0570 1.0000 Uiso R . . . . . H121 H -0.0892 0.8163 0.5933 0.0667 1.0000 Uiso R . . . . . H122 H -0.1375 0.7416 0.6139 0.0668 1.0000 Uiso R . . . . . H123 H -0.0369 0.7347 0.5777 0.0670 1.0000 Uiso R . . . . . H131 H -0.0479 0.7672 0.6922 0.0410 1.0000 Uiso R . . . . . H141 H 0.0808 0.8179 0.6335 0.0388 1.0000 Uiso R . . . . . H142 H 0.1328 0.7301 0.6269 0.0384 1.0000 Uiso R . . . . . H151 H 0.3277 0.7977 0.7152 0.0498 1.0000 Uiso R . . . . . H152 H 0.3398 0.7380 0.6721 0.0496 1.0000 Uiso R . . . . . H161 H 0.2474 0.8414 0.5988 0.0610 1.0000 Uiso R . . . . . H171 H 0.2159 0.9742 0.6122 0.0801 1.0000 Uiso R . . . . . H172 H 0.2482 0.9424 0.6792 0.0798 1.0000 Uiso R . . . . . H173 H 0.1473 0.9239 0.6548 0.0799 1.0000 Uiso R . . . . . H181 H 0.3855 0.9115 0.5814 0.1089 1.0000 Uiso R . . . . . H182 H 0.4262 0.8713 0.6458 0.1088 1.0000 Uiso R . . . . . H183 H 0.4254 0.8183 0.5994 0.1085 1.0000 Uiso R . . . . . H191 H 0.3961 0.5092 0.5850 0.1092 1.0000 Uiso R . . . . . H192 H 0.3409 0.5394 0.5198 0.1091 1.0000 Uiso R . . . . . H193 H 0.4433 0.4681 0.5320 0.1090 1.0000 Uiso R . . . . . H201 H 0.2484 0.4501 0.5846 0.0748 1.0000 Uiso R . . . . . H211 H 0.2435 0.3663 0.5140 0.1261 1.0000 Uiso R . . . . . H212 H 0.2359 0.4563 0.4821 0.1261 1.0000 Uiso R . . . . . H213 H 0.3431 0.3942 0.4856 0.1259 1.0000 Uiso R . . . . . H221 H 0.4353 0.3367 0.5837 0.0694 1.0000 Uiso R . . . . . H222 H 0.3254 0.3143 0.6042 0.0693 1.0000 Uiso R . . . . . H231 H 0.6557 0.2609 0.7258 0.1101 1.0000 Uiso R . . . . . H232 H 0.7075 0.3352 0.7269 0.1103 1.0000 Uiso R . . . . . H233 H 0.7500 0.2753 0.6851 0.1101 1.0000 Uiso R . . . . . H241 H 0.6206 0.4512 0.5876 0.1010 1.0000 Uiso R . . . . . H242 H 0.6855 0.4483 0.6440 0.1012 1.0000 Uiso R . . . . . H243 H 0.7295 0.3899 0.6009 0.1009 1.0000 Uiso R . . . . . H251 H 0.5969 0.3223 0.6274 0.0572 1.0000 Uiso R . . . . . H261 H 0.5278 0.4002 0.7203 0.0513 1.0000 Uiso R . . . . . H262 H 0.4975 0.4516 0.6554 0.0515 1.0000 Uiso R . . . . . H271 H 0.5087 0.2364 0.7257 0.0550 1.0000 Uiso R . . . . . H272 H 0.4319 0.2193 0.6817 0.0558 1.0000 Uiso R . . . . . H281 H 0.4141 0.1756 0.7912 0.0502 1.0000 Uiso R . . . . . H282 H 0.3121 0.2053 0.7506 0.0500 1.0000 Uiso R . . . . . H291 H 0.6423 0.3148 0.8469 0.0762 1.0000 Uiso R . . . . . H292 H 0.5940 0.3122 0.9108 0.0757 1.0000 Uiso R . . . . . H293 H 0.6731 0.2363 0.8974 0.0760 1.0000 Uiso R . . . . . H301 H 0.4400 0.1708 0.9002 0.0776 1.0000 Uiso R . . . . . H302 H 0.4748 0.2166 0.9446 0.0777 1.0000 Uiso R . . . . . H303 H 0.5536 0.1449 0.9266 0.0781 1.0000 Uiso R . . . . . H311 H 0.5538 0.2211 0.8299 0.0495 1.0000 Uiso R . . . . . H321 H 0.4108 0.3401 0.8726 0.0453 1.0000 Uiso R . . . . . H322 H 0.4687 0.3592 0.8122 0.0452 1.0000 Uiso R . . . . . H331 H 0.2401 0.1330 0.8525 0.1422 1.0000 Uiso R . . . . . H332 H 0.1665 0.1460 0.9060 0.1419 1.0000 Uiso R . . . . . H333 H 0.1209 0.1307 0.8485 0.1420 1.0000 Uiso R . . . . . H341 H 0.0358 0.3404 0.8494 0.1261 1.0000 Uiso R . . . . . H342 H 0.0479 0.2688 0.9045 0.1259 1.0000 Uiso R . . . . . H343 H -0.0113 0.2652 0.8471 0.1260 1.0000 Uiso R . . . . . H351 H 0.1416 0.2542 0.7967 0.0593 1.0000 Uiso R . . . . . H361 H 0.2019 0.3303 0.8701 0.0546 1.0000 Uiso R . . . . . H362 H 0.2717 0.2412 0.8894 0.0541 1.0000 Uiso R . . . . . H381 H 0.4192 0.5256 0.7739 0.0311 1.0000 Uiso R . . . . . H401 H 0.6120 0.6303 0.8461 0.0320 1.0000 Uiso R . . . . . H421 H 0.3127 0.7377 0.8194 0.0271 1.0000 Uiso R . . . . . H441 H 0.5265 0.9168 0.8706 0.0348 1.0000 Uiso R . . . . . H461 H 0.6910 0.9705 0.7254 0.0456 1.0000 Uiso R . . . . . H481 H 0.5960 0.7619 0.7632 0.0395 1.0000 Uiso R . . . . . H501 H 0.6809 0.7752 0.9130 0.0318 1.0000 Uiso R . . . . . H521 H 0.7281 0.5928 1.0543 0.0372 1.0000 Uiso R . . . . . H541 H 0.4605 0.6497 0.9615 0.0309 1.0000 Uiso R . . . . . H561 H 0.3773 0.7934 0.9725 0.0338 1.0000 Uiso R . . . . . H581 H 0.1332 0.9723 0.9112 0.0392 1.0000 Uiso R . . . . . H601 H 0.3424 0.8860 0.7993 0.0318 1.0000 Uiso R . . . . . H621 H 0.0727 0.4762 0.7419 0.0348 1.0000 Uiso R . . . . . H641 H -0.0933 0.3547 0.6674 0.0330 1.0000 Uiso R . . . . . H661 H 0.2178 0.2913 0.6717 0.0278 1.0000 Uiso R . . . . . H681 H -0.0385 0.2241 0.7438 0.0366 1.0000 Uiso R . . . . . H701 H -0.1426 0.0198 0.7640 0.0440 1.0000 Uiso R . . . . . H721 H 0.0074 0.0949 0.6183 0.0328 1.0000 Uiso R . . . . . H741 H -0.1379 0.2205 0.5802 0.0369 1.0000 Uiso R . . . . . H761 H -0.1757 0.3941 0.4339 0.0460 1.0000 Uiso R . . . . . H781 H 0.0676 0.3623 0.5412 0.0359 1.0000 Uiso R . . . . . H801 H 0.2059 0.1359 0.6989 0.0317 1.0000 Uiso R . . . . . H821 H 0.4307 0.0756 0.5867 0.0529 1.0000 Uiso R . . . . . H841 H 0.1620 0.2234 0.5253 0.0450 1.0000 Uiso R . . . . . H2011 H 0.8073 0.9826 0.9101 0.1042 1.0000 Uiso R . . . . . H2012 H 0.7741 0.9056 0.9500 0.1044 1.0000 Uiso R . . . . . H2041 H 0.5688 0.6547 0.6953 0.1373 0.6678 Uiso R . . . . . H2042 H 0.5738 0.7300 0.6446 0.1370 0.6678 Uiso R . . . . . H2071 H 0.6152 0.1465 0.5370 0.0981 0.650(5) Uiso R . P 1 1 . H2072 H 0.7371 0.1142 0.5500 0.0979 0.650(5) Uiso R . P 1 1 . H2101 H 0.7654 0.0826 0.5684 0.1430 0.350(5) Uiso R . P 1 2 . H2102 H 0.7097 0.0156 0.6028 0.1430 0.350(5) Uiso R . P 1 2 . H2131 H 0.8944 0.9641 0.5326 0.0860 0.435(4) Uiso R . P 2 -1 . H2132 H 0.8957 0.9709 0.4646 0.0859 0.435(4) Uiso R . P 2 -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 Cl1 0.0280(4) 0.0256(4) 0.0254(4) -0.0019(3) -0.0023(3) -0.0086(3) C1 0.047(3) 0.048(3) 0.046(3) -0.008(2) 0.007(2) -0.026(2) P1 0.0212(4) 0.0277(4) 0.0258(4) -0.0063(3) 0.0019(3) -0.0087(3) Rh1 0.02021(12) 0.02329(13) 0.02187(13) -0.00379(9) -0.00170(9) -0.00833(9) B1 0.0210(17) 0.0257(18) 0.0228(18) -0.0029(14) -0.0019(14) -0.0084(14) Cl2 0.0314(4) 0.0286(4) 0.0222(4) -0.0049(3) 0.0003(3) -0.0089(3) C2 0.029(2) 0.065(3) 0.058(3) -0.027(2) 0.007(2) -0.020(2) P2 0.0309(5) 0.0252(4) 0.0256(4) -0.0006(3) -0.0034(4) -0.0100(4) Rh2 0.01958(13) 0.02519(13) 0.03083(14) -0.00717(10) -0.00180(10) -0.00685(9) B2 0.0254(18) 0.0243(18) 0.0180(17) -0.0025(14) -0.0024(14) -0.0077(15) Cl3 0.0236(4) 0.0377(5) 0.0690(7) -0.0245(5) -0.0006(4) -0.0029(4) C3 0.0277(19) 0.042(2) 0.039(2) -0.0148(17) 0.0084(16) -0.0170(16) P3 0.0298(5) 0.0466(6) 0.0394(6) -0.0180(5) 0.0077(4) -0.0142(4) Cl4 0.0457(6) 0.0341(5) 0.0372(5) -0.0011(4) -0.0117(4) 0.0035(4) C4 0.0241(17) 0.035(2) 0.036(2) -0.0094(16) 0.0015(15) -0.0094(15) P4 0.0344(5) 0.0310(5) 0.0365(5) -0.0022(4) -0.0062(4) -0.0061(4) Cl5 0.0482(6) 0.0545(6) 0.0304(5) -0.0097(4) 0.0074(4) 0.0045(5) C5 0.063(3) 0.058(3) 0.044(3) -0.022(2) 0.019(2) -0.019(3) Cl6 0.0904(11) 0.1046(12) 0.0506(7) -0.0352(8) 0.0414(7) -0.0586(10) C6 0.053(3) 0.077(4) 0.029(2) -0.008(2) 0.001(2) -0.015(3) Cl7 0.0474(6) 0.0294(5) 0.0661(7) -0.0071(5) 0.0014(5) -0.0172(4) C7 0.038(2) 0.048(2) 0.0277(19) -0.0087(17) 0.0052(16) -0.0197(19) Cl8 0.0268(4) 0.0714(7) 0.0345(5) -0.0052(5) -0.0059(4) -0.0174(5) C8 0.0275(18) 0.036(2) 0.0292(19) -0.0075(15) 0.0016(15) -0.0102(15) Cl9 0.0476(5) 0.0339(5) 0.0318(5) 0.0036(4) -0.0034(4) -0.0147(4) C9 0.0315(19) 0.0290(18) 0.036(2) -0.0089(15) 0.0034(16) -0.0099(15) Cl10 0.0219(4) 0.0643(7) 0.1068(11) -0.0576(8) 0.0075(5) -0.0086(5) C10 0.051(3) 0.0249(18) 0.037(2) -0.0062(16) -0.0072(19) -0.0042(17) Cl11 0.0754(8) 0.0359(5) 0.0278(5) 0.0051(4) -0.0072(5) -0.0202(5) C11 0.036(2) 0.042(2) 0.041(2) -0.0090(18) -0.0051(17) -0.0155(18) Cl12 0.0526(7) 0.0850(10) 0.0552(7) 0.0002(7) -0.0260(6) -0.0318(7) C12 0.041(2) 0.048(3) 0.045(3) -0.010(2) -0.014(2) -0.002(2) Cl13 0.0540(6) 0.0311(5) 0.0567(6) -0.0098(4) -0.0012(5) -0.0210(4) C13 0.032(2) 0.037(2) 0.035(2) -0.0087(17) -0.0070(16) -0.0063(16) Cl14 0.1002(11) 0.0959(11) 0.0409(6) -0.0275(7) 0.0353(7) -0.0657(10) C14 0.038(2) 0.0300(19) 0.0299(19) -0.0011(15) -0.0070(16) -0.0101(16) Cl15 0.0832(11) 0.1419(18) 0.0428(7) -0.0081(9) 0.0264(8) 0.0302(11) C15 0.043(2) 0.045(2) 0.040(2) -0.0007(19) 0.0000(19) -0.022(2) Cl16 0.0373(5) 0.0357(5) 0.0533(6) -0.0041(4) -0.0159(4) 0.0010(4) C16 0.068(3) 0.048(3) 0.040(2) -0.001(2) 0.004(2) -0.029(2) C17 0.071(4) 0.044(3) 0.048(3) -0.001(2) 0.002(2) -0.026(3) C18 0.075(4) 0.067(4) 0.077(4) 0.001(3) 0.024(3) -0.035(3) C19 0.074(4) 0.073(4) 0.063(4) -0.001(3) 0.005(3) -0.013(3) C20 0.050(3) 0.078(4) 0.054(3) -0.013(3) 0.004(2) -0.005(3) C21 0.089(5) 0.106(6) 0.052(4) 0.007(4) -0.006(3) -0.036(4) C22 0.052(3) 0.087(4) 0.041(3) -0.021(3) 0.010(2) -0.028(3) C23 0.042(3) 0.080(4) 0.086(5) 0.004(4) 0.001(3) -0.007(3) C24 0.037(3) 0.094(5) 0.064(4) -0.006(3) 0.013(2) -0.014(3) C25 0.032(2) 0.060(3) 0.054(3) -0.021(2) 0.009(2) -0.009(2) C26 0.031(2) 0.052(3) 0.050(3) -0.019(2) 0.0072(19) -0.0136(19) C27 0.041(2) 0.035(2) 0.067(3) -0.023(2) 0.012(2) -0.0078(18) C28 0.049(3) 0.033(2) 0.043(2) -0.0110(18) -0.010(2) -0.0045(18) C29 0.042(3) 0.049(3) 0.054(3) -0.005(2) -0.016(2) -0.001(2) C30 0.059(3) 0.040(2) 0.053(3) 0.001(2) -0.016(2) -0.007(2) C31 0.043(2) 0.037(2) 0.041(2) -0.0077(18) -0.0113(19) -0.0008(18) C32 0.040(2) 0.034(2) 0.038(2) -0.0060(17) -0.0084(18) -0.0039(17) C33 0.141(8) 0.054(4) 0.098(6) -0.007(4) 0.010(5) -0.053(5) C34 0.059(4) 0.138(7) 0.069(4) -0.050(5) 0.000(3) -0.027(4) C35 0.056(3) 0.060(3) 0.037(2) -0.009(2) 0.003(2) -0.026(2) C36 0.052(3) 0.047(3) 0.036(2) -0.0062(19) 0.002(2) -0.016(2) C37 0.0193(15) 0.0281(17) 0.0229(16) -0.0030(13) -0.0010(12) -0.0088(13) C38 0.0252(17) 0.0286(17) 0.0280(17) -0.0087(14) 0.0008(14) -0.0117(14) C39 0.0224(17) 0.0275(18) 0.0324(19) -0.0054(14) 0.0011(14) -0.0058(14) C40 0.0187(16) 0.0312(18) 0.0307(18) -0.0058(14) -0.0020(13) -0.0083(14) C41 0.0213(16) 0.0265(17) 0.0221(16) -0.0035(13) 0.0002(13) -0.0085(13) C42 0.0203(15) 0.0234(16) 0.0232(16) -0.0024(13) -0.0008(12) -0.0073(13) C43 0.0199(16) 0.0293(17) 0.0248(17) -0.0024(14) -0.0031(13) -0.0080(13) C44 0.0276(18) 0.0304(19) 0.0311(19) -0.0057(15) 0.0000(15) -0.0096(15) C45 0.0288(18) 0.0271(18) 0.040(2) -0.0007(16) -0.0057(16) -0.0094(15) C46 0.033(2) 0.043(2) 0.038(2) 0.0056(18) 0.0001(17) -0.0188(18) C47 0.040(2) 0.059(3) 0.030(2) -0.0101(19) 0.0094(17) -0.021(2) C48 0.035(2) 0.039(2) 0.0302(19) -0.0079(16) 0.0038(16) -0.0165(17) C49 0.0230(16) 0.0261(17) 0.0230(16) -0.0069(13) 0.0007(13) -0.0071(13) C50 0.0264(17) 0.0320(18) 0.0240(17) -0.0058(14) 0.0005(14) -0.0096(14) C51 0.0237(17) 0.041(2) 0.0277(18) -0.0091(16) -0.0028(14) -0.0074(15) C52 0.0309(19) 0.037(2) 0.0236(17) -0.0045(15) -0.0051(14) -0.0026(15) C53 0.0330(19) 0.0288(18) 0.0244(17) -0.0035(14) 0.0004(14) -0.0081(15) C54 0.0255(17) 0.0287(18) 0.0253(17) -0.0052(14) -0.0007(14) -0.0094(14) C55 0.0236(16) 0.0264(17) 0.0267(17) -0.0062(14) -0.0002(13) -0.0107(13) C56 0.0291(18) 0.0293(18) 0.0256(17) -0.0045(14) -0.0021(14) -0.0068(14) C57 0.033(2) 0.036(2) 0.0277(19) -0.0071(16) 0.0034(15) -0.0060(16) C58 0.0310(19) 0.0281(18) 0.037(2) -0.0081(16) -0.0003(16) -0.0024(15) C59 0.0334(19) 0.0239(17) 0.0299(19) -0.0011(14) -0.0079(15) -0.0055(14) C60 0.0303(18) 0.0272(17) 0.0237(17) -0.0034(14) 0.0003(14) -0.0096(14) C61 0.0186(15) 0.0256(16) 0.0254(16) -0.0016(13) -0.0039(13) -0.0085(13) C62 0.0251(18) 0.0289(18) 0.037(2) -0.0132(15) 0.0002(15) -0.0085(14) C63 0.0212(17) 0.034(2) 0.045(2) -0.0152(17) 0.0004(15) -0.0058(15) C64 0.0226(17) 0.0290(18) 0.0337(19) -0.0072(15) -0.0027(14) -0.0096(14) C65 0.0243(16) 0.0236(16) 0.0194(15) -0.0003(12) -0.0012(12) -0.0080(13) C66 0.0211(16) 0.0253(16) 0.0227(16) -0.0030(13) -0.0008(13) -0.0058(13) C67 0.0227(16) 0.0241(16) 0.0257(17) -0.0016(13) -0.0035(13) -0.0069(13) C68 0.0332(19) 0.034(2) 0.0297(19) -0.0074(15) 0.0006(15) -0.0166(16) C69 0.040(2) 0.049(2) 0.0284(19) -0.0049(17) 0.0063(17) -0.0214(19) C70 0.038(2) 0.038(2) 0.037(2) 0.0010(17) -0.0001(17) -0.0209(18) C71 0.034(2) 0.0262(18) 0.038(2) -0.0039(15) -0.0030(16) -0.0127(15) C72 0.0316(19) 0.0265(17) 0.0261(17) -0.0033(14) 0.0003(14) -0.0086(14) C73 0.0290(18) 0.0242(16) 0.0229(16) -0.0048(13) -0.0030(14) -0.0050(14) C74 0.034(2) 0.0335(19) 0.0280(18) -0.0049(15) -0.0055(15) -0.0117(16) C75 0.035(2) 0.042(2) 0.033(2) -0.0057(17) -0.0111(17) -0.0107(18) C76 0.046(2) 0.039(2) 0.0269(19) -0.0025(16) -0.0123(17) -0.0042(18) C77 0.052(2) 0.0267(18) 0.0236(18) -0.0019(14) -0.0038(17) -0.0102(17) C78 0.039(2) 0.0270(18) 0.0251(18) -0.0035(14) -0.0041(15) -0.0103(15) C79 0.0278(17) 0.0255(17) 0.0252(17) -0.0032(13) -0.0010(14) -0.0105(14) C80 0.0290(18) 0.0239(17) 0.0279(18) -0.0034(14) -0.0011(14) -0.0079(14) C81 0.0306(19) 0.0249(18) 0.040(2) -0.0046(15) -0.0048(16) -0.0064(15) C82 0.034(2) 0.044(2) 0.052(3) -0.012(2) 0.0065(19) 0.0019(18) C83 0.050(3) 0.062(3) 0.035(2) -0.010(2) 0.009(2) -0.001(2) C84 0.039(2) 0.044(2) 0.0266(19) -0.0053(17) 0.0003(16) -0.0016(18) C201 0.070(3) 0.079(3) 0.101(4) -0.016(3) -0.012(3) 0.003(3) Cl202 0.0681(10) 0.0693(10) 0.1040(13) -0.0183(9) -0.0169(9) 0.0024(8) Cl203 0.0463(7) 0.0625(8) 0.0770(9) 0.0005(7) 0.0007(6) -0.0028(6) C204 0.077(4) 0.084(4) 0.192(5) -0.041(4) -0.035(4) -0.021(4) Cl205 0.085(2) 0.0707(17) 0.259(5) -0.023(2) -0.085(3) -0.0092(15) Cl206 0.0410(10) 0.0744(15) 0.147(3) -0.0479(16) 0.0050(12) -0.0225(10) C207 0.093(4) 0.063(4) 0.094(4) -0.024(4) 0.015(4) -0.024(4) Cl208 0.0826(18) 0.0586(14) 0.098(2) -0.0173(13) 0.0095(14) -0.0158(12) Cl209 0.087(3) 0.0588(19) 0.092(3) -0.025(2) 0.019(2) -0.0100(19) C210 0.101(6) 0.132(7) 0.104(6) 0.024(5) -0.015(5) -0.023(6) Cl211 0.096(6) 0.124(7) 0.107(6) 0.031(5) -0.005(5) 0.004(5) Cl212 0.109(5) 0.143(6) 0.104(5) 0.019(4) -0.016(4) -0.059(4) C213 0.104(5) 0.066(4) 0.034(4) -0.008(4) -0.017(4) 0.004(4) Cl214 0.089(3) 0.073(3) 0.037(5) 0.001(3) -0.018(3) 0.001(3) Cl215 0.121(6) 0.055(2) 0.037(4) -0.010(2) -0.020(3) 0.004(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.707(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 . Rh1 . 2.4464(8) yes Cl1 . Rh2 . 2.4796(9) yes C1 . C3 . 1.531(6) yes C1 . H11 . 0.968 no C1 . H12 . 0.959 no C1 . H13 . 0.963 no P1 . Rh1 . 2.2518(9) yes P1 . C4 . 1.837(4) yes P1 . C8 . 1.829(4) yes P1 . C9 . 1.840(4) yes Rh1 . Cl2 . 2.4924(9) yes Rh1 . P2 . 2.2399(9) yes Rh1 . C37 . 2.030(3) yes B1 . C41 . 1.651(5) yes B1 . C43 . 1.644(5) yes B1 . C49 . 1.647(5) yes B1 . C55 . 1.654(5) yes Cl2 . Rh2 . 2.4878(9) yes C2 . C3 . 1.521(6) yes C2 . H21 . 0.957 no C2 . H22 . 0.961 no C2 . H23 . 0.961 no P2 . C10 . 1.845(4) yes P2 . C14 . 1.820(4) yes P2 . C15 . 1.830(4) yes Rh2 . P3 . 2.2239(11) yes Rh2 . P4 . 2.2279(11) yes Rh2 . C61 . 2.020(3) yes B2 . C65 . 1.644(5) yes B2 . C67 . 1.647(5) yes B2 . C73 . 1.646(5) yes B2 . C79 . 1.645(5) yes Cl3 . C39 . 1.753(4) yes C3 . C4 . 1.534(5) yes C3 . H31 . 0.979 no P3 . C22 . 1.802(5) yes P3 . C26 . 1.847(5) yes P3 . C27 . 1.879(5) yes Cl4 . C59 . 1.747(4) yes C4 . H41 . 0.975 no C4 . H42 . 0.973 no P4 . C28 . 1.806(5) yes P4 . C32 . 1.838(4) yes P4 . C36 . 1.837(5) yes Cl5 . C57 . 1.750(4) yes C5 . C7 . 1.510(7) yes C5 . H51 . 0.974 no C5 . H52 . 0.969 no C5 . H53 . 0.958 no Cl6 . C47 . 1.753(5) yes C6 . C7 . 1.524(7) yes C6 . H61 . 0.951 no C6 . H62 . 0.959 no C6 . H63 . 0.950 no Cl7 . C45 . 1.751(4) yes C7 . C8 . 1.547(5) yes C7 . H71 . 0.984 no Cl8 . C51 . 1.752(4) yes C8 . H81 . 0.972 no C8 . H82 . 0.962 no Cl9 . C53 . 1.744(4) yes C9 . C10 . 1.531(6) yes C9 . H91 . 0.974 no C9 . H92 . 0.966 no Cl10 . C63 . 1.744(4) yes C10 . H101 . 0.953 no C10 . H102 . 0.959 no Cl11 . C77 . 1.741(4) yes C11 . C13 . 1.525(6) yes C11 . H111 . 0.967 no C11 . H112 . 0.959 no C11 . H113 . 0.952 no Cl12 . C75 . 1.748(4) yes C12 . C13 . 1.528(6) yes C12 . H121 . 0.958 no C12 . H122 . 0.956 no C12 . H123 . 0.966 no Cl13 . C71 . 1.755(4) yes C13 . C14 . 1.531(6) yes C13 . H131 . 0.969 no Cl14 . C69 . 1.745(4) yes C14 . H141 . 0.965 no C14 . H142 . 0.966 no Cl15 . C83 . 1.747(5) yes C15 . C16 . 1.541(6) yes C15 . H151 . 0.965 no C15 . H152 . 0.973 no Cl16 . C81 . 1.748(4) yes C16 . C17 . 1.504(8) yes C16 . C18 . 1.528(8) yes C16 . H161 . 0.988 no C17 . H171 . 0.962 no C17 . H172 . 0.965 no C17 . H173 . 0.979 no C18 . H181 . 0.964 no C18 . H182 . 0.960 no C18 . H183 . 0.961 no C19 . C20 . 1.553(9) yes C19 . H191 . 0.989 no C19 . H192 . 0.992 no C19 . H193 . 0.987 no C20 . C21 . 1.554(9) yes C20 . C22 . 1.478(9) yes C20 . H201 . 0.983 no C21 . H211 . 0.970 no C21 . H212 . 0.968 no C21 . H213 . 0.967 no C22 . H221 . 0.994 no C22 . H222 . 0.991 no C23 . C25 . 1.527(8) yes C23 . H231 . 0.979 no C23 . H232 . 0.973 no C23 . H233 . 0.971 no C24 . C25 . 1.499(8) yes C24 . H241 . 0.969 no C24 . H242 . 0.968 no C24 . H243 . 0.972 no C25 . C26 . 1.555(6) yes C25 . H251 . 0.984 no C26 . H261 . 0.980 no C26 . H262 . 0.981 no C27 . C28 . 1.500(7) yes C27 . H271 . 0.961 no C27 . H272 . 0.964 no C28 . H281 . 0.977 no C28 . H282 . 0.982 no C29 . C31 . 1.522(7) yes C29 . H291 . 0.980 no C29 . H292 . 0.974 no C29 . H293 . 0.966 no C30 . C31 . 1.516(7) yes C30 . H301 . 0.957 no C30 . H302 . 0.964 no C30 . H303 . 0.961 no C31 . C32 . 1.535(6) yes C31 . H311 . 0.982 no C32 . H321 . 0.963 no C32 . H322 . 0.975 no C33 . C35 . 1.519(9) yes C33 . H331 . 0.971 no C33 . H332 . 0.969 no C33 . H333 . 0.962 no C34 . C35 . 1.502(9) yes C34 . H341 . 0.963 no C34 . H342 . 0.966 no C34 . H343 . 0.966 no C35 . C36 . 1.507(7) yes C35 . H351 . 0.982 no C36 . H361 . 0.995 no C36 . H362 . 0.982 no C37 . C38 . 1.392(5) yes C37 . C42 . 1.393(5) yes C38 . C39 . 1.389(5) yes C38 . H381 . 0.924 no C39 . C40 . 1.379(5) yes C40 . C41 . 1.403(5) yes C40 . H401 . 0.935 no C41 . C42 . 1.401(5) yes C42 . H421 . 0.931 no C43 . C44 . 1.405(5) yes C43 . C48 . 1.387(5) yes C44 . C45 . 1.386(5) yes C44 . H441 . 0.928 no C45 . C46 . 1.379(6) yes C46 . C47 . 1.376(7) yes C46 . H461 . 0.943 no C47 . C48 . 1.386(6) yes C48 . H481 . 0.921 no C49 . C50 . 1.395(5) yes C49 . C54 . 1.412(5) yes C50 . C51 . 1.386(5) yes C50 . H501 . 0.931 no C51 . C52 . 1.384(6) yes C52 . C53 . 1.394(6) yes C52 . H521 . 0.932 no C53 . C54 . 1.379(5) yes C54 . H541 . 0.926 no C55 . C56 . 1.402(5) yes C55 . C60 . 1.406(5) yes C56 . C57 . 1.393(5) yes C56 . H561 . 0.937 no C57 . C58 . 1.376(6) yes C58 . C59 . 1.383(6) yes C58 . H581 . 0.932 no C59 . C60 . 1.389(5) yes C60 . H601 . 0.924 no C61 . C62 . 1.387(5) yes C61 . C66 . 1.393(5) yes C62 . C63 . 1.386(5) yes C62 . H621 . 0.920 no C63 . C64 . 1.377(5) yes C64 . C65 . 1.403(5) yes C64 . H641 . 0.930 no C65 . C66 . 1.408(5) yes C66 . H661 . 0.934 no C67 . C68 . 1.391(5) yes C67 . C72 . 1.412(5) yes C68 . C69 . 1.391(5) yes C68 . H681 . 0.932 no C69 . C70 . 1.377(6) yes C70 . C71 . 1.375(6) yes C70 . H701 . 0.932 no C71 . C72 . 1.384(5) yes C72 . H721 . 0.926 no C73 . C74 . 1.399(5) yes C73 . C78 . 1.404(5) yes C74 . C75 . 1.396(6) yes C74 . H741 . 0.938 no C75 . C76 . 1.378(6) yes C76 . C77 . 1.380(6) yes C76 . H761 . 0.919 no C77 . C78 . 1.384(5) yes C78 . H781 . 0.926 no C79 . C80 . 1.404(5) yes C79 . C84 . 1.402(5) yes C80 . C81 . 1.385(5) yes C80 . H801 . 0.931 no C81 . C82 . 1.381(6) yes C82 . C83 . 1.385(7) yes C82 . H821 . 0.926 no C83 . C84 . 1.383(7) yes C84 . H841 . 0.931 no C201 . Cl202 . 1.738(4) yes C201 . Cl203 . 1.732(4) yes C201 . H2011 . 0.973 no C201 . H2012 . 0.995 no C204 . Cl205 . 1.690(5) yes C204 . Cl206 . 1.723(5) yes C204 . H2041 . 0.958 no C204 . H2042 . 0.960 no C207 . Cl208 . 1.736(5) yes C207 . Cl209 . 1.735(5) yes C207 . H2071 . 0.978 no C207 . H2072 . 0.975 no C210 . Cl211 . 1.716(7) yes C210 . Cl212 . 1.718(7) yes C210 . H2101 . 0.971 no C210 . H2102 . 0.968 no C213 . Cl214 . 1.727(6) yes C213 . Cl215 . 1.731(5) yes C213 . H2131 . 0.960 no C213 . H2132 . 0.959 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Rh1 . Cl1 . Rh2 . 97.38(3) yes C3 . C1 . H11 . 110.8 no C3 . C1 . H12 . 110.4 no H11 . C1 . H12 . 108.5 no C3 . C1 . H13 . 109.2 no H11 . C1 . H13 . 108.6 no H12 . C1 . H13 . 109.4 no Rh1 . P1 . C4 . 112.73(13) yes Rh1 . P1 . C8 . 113.21(13) yes C4 . P1 . C8 . 110.01(18) yes Rh1 . P1 . C9 . 109.96(13) yes C4 . P1 . C9 . 100.88(18) yes C8 . P1 . C9 . 109.32(19) yes Cl1 . Rh1 . P1 . 91.90(3) yes Cl1 . Rh1 . Cl2 . 83.61(3) yes P1 . Rh1 . Cl2 . 170.94(3) yes Cl1 . Rh1 . P2 . 174.11(3) yes P1 . Rh1 . P2 . 87.52(4) yes Cl2 . Rh1 . P2 . 96.13(3) yes Cl1 . Rh1 . C37 . 95.29(10) yes P1 . Rh1 . C37 . 91.07(10) yes Cl2 . Rh1 . C37 . 97.16(10) yes P2 . Rh1 . C37 . 90.58(10) yes C41 . B1 . C43 . 111.6(3) yes C41 . B1 . C49 . 104.6(3) yes C43 . B1 . C49 . 110.1(3) yes C41 . B1 . C55 . 111.8(3) yes C43 . B1 . C55 . 106.1(3) yes C49 . B1 . C55 . 112.7(3) yes Rh1 . Cl2 . Rh2 . 95.98(3) yes C3 . C2 . H21 . 107.2 no C3 . C2 . H22 . 108.5 no H21 . C2 . H22 . 110.4 no C3 . C2 . H23 . 108.9 no H21 . C2 . H23 . 110.6 no H22 . C2 . H23 . 111.1 no Rh1 . P2 . C10 . 109.04(14) yes Rh1 . P2 . C14 . 110.55(13) yes C10 . P2 . C14 . 106.0(2) yes Rh1 . P2 . C15 . 115.26(16) yes C10 . P2 . C15 . 111.3(2) yes C14 . P2 . C15 . 104.2(2) yes Cl2 . Rh2 . Cl1 . 83.03(3) yes Cl2 . Rh2 . P3 . 99.50(4) yes Cl1 . Rh2 . P3 . 159.45(4) yes Cl2 . Rh2 . P4 . 163.12(4) yes Cl1 . Rh2 . P4 . 87.46(4) yes P3 . Rh2 . P4 . 84.69(4) yes Cl2 . Rh2 . C61 . 104.50(10) yes Cl1 . Rh2 . C61 . 103.51(11) yes P3 . Rh2 . C61 . 95.64(11) yes P4 . Rh2 . C61 . 91.25(10) yes C65 . B2 . C67 . 110.5(3) yes C65 . B2 . C73 . 105.8(3) yes C67 . B2 . C73 . 111.2(3) yes C65 . B2 . C79 . 110.6(3) yes C67 . B2 . C79 . 107.0(3) yes C73 . B2 . C79 . 111.7(3) yes C1 . C3 . C2 . 110.0(4) yes C1 . C3 . C4 . 113.1(4) yes C2 . C3 . C4 . 108.2(4) yes C1 . C3 . H31 . 109.4 no C2 . C3 . H31 . 108.1 no C4 . C3 . H31 . 107.9 no Rh2 . P3 . C22 . 124.2(2) yes Rh2 . P3 . C26 . 104.09(15) yes C22 . P3 . C26 . 108.9(2) yes Rh2 . P3 . C27 . 109.68(16) yes C22 . P3 . C27 . 103.4(3) yes C26 . P3 . C27 . 105.3(2) yes C3 . C4 . P1 . 121.9(3) yes C3 . C4 . H41 . 107.9 no P1 . C4 . H41 . 106.1 no C3 . C4 . H42 . 106.6 no P1 . C4 . H42 . 105.1 no H41 . C4 . H42 . 108.9 no Rh2 . P4 . C28 . 110.30(16) yes Rh2 . P4 . C32 . 101.69(15) yes C28 . P4 . C32 . 108.6(2) yes Rh2 . P4 . C36 . 117.48(17) yes C28 . P4 . C36 . 110.9(2) yes C32 . P4 . C36 . 107.1(2) yes C7 . C5 . H51 . 109.6 no C7 . C5 . H52 . 109.6 no H51 . C5 . H52 . 110.9 no C7 . C5 . H53 . 108.1 no H51 . C5 . H53 . 109.6 no H52 . C5 . H53 . 108.9 no C7 . C6 . H61 . 109.0 no C7 . C6 . H62 . 110.6 no H61 . C6 . H62 . 110.2 no C7 . C6 . H63 . 108.2 no H61 . C6 . H63 . 109.9 no H62 . C6 . H63 . 108.9 no C6 . C7 . C5 . 111.0(4) yes C6 . C7 . C8 . 108.1(4) yes C5 . C7 . C8 . 112.4(4) yes C6 . C7 . H71 . 108.5 no C5 . C7 . H71 . 108.8 no C8 . C7 . H71 . 107.9 no C7 . C8 . P1 . 120.7(3) yes C7 . C8 . H81 . 107.1 no P1 . C8 . H81 . 106.7 no C7 . C8 . H82 . 106.2 no P1 . C8 . H82 . 106.8 no H81 . C8 . H82 . 109.0 no P1 . C9 . C10 . 111.4(3) yes P1 . C9 . H91 . 108.5 no C10 . C9 . H91 . 110.7 no P1 . C9 . H92 . 107.1 no C10 . C9 . H92 . 109.3 no H91 . C9 . H92 . 109.7 no C9 . C10 . P2 . 115.6(3) yes C9 . C10 . H101 . 108.0 no P2 . C10 . H101 . 107.4 no C9 . C10 . H102 . 107.4 no P2 . C10 . H102 . 108.2 no H101 . C10 . H102 . 110.3 no C13 . C11 . H111 . 110.4 no C13 . C11 . H112 . 109.0 no H111 . C11 . H112 . 109.8 no C13 . C11 . H113 . 108.9 no H111 . C11 . H113 . 109.1 no H112 . C11 . H113 . 109.7 no C13 . C12 . H121 . 110.7 no C13 . C12 . H122 . 110.3 no H121 . C12 . H122 . 109.0 no C13 . C12 . H123 . 111.0 no H121 . C12 . H123 . 107.9 no H122 . C12 . H123 . 107.8 no C12 . C13 . C11 . 110.7(4) yes C12 . C13 . C14 . 109.1(4) yes C11 . C13 . C14 . 111.5(3) yes C12 . C13 . H131 . 107.7 no C11 . C13 . H131 . 108.7 no C14 . C13 . H131 . 109.0 no C13 . C14 . P2 . 116.9(3) yes C13 . C14 . H141 . 108.5 no P2 . C14 . H141 . 107.5 no C13 . C14 . H142 . 108.6 no P2 . C14 . H142 . 105.6 no H141 . C14 . H142 . 109.5 no P2 . C15 . C16 . 119.4(4) yes P2 . C15 . H151 . 107.0 no C16 . C15 . H151 . 106.4 no P2 . C15 . H152 . 107.9 no C16 . C15 . H152 . 107.2 no H151 . C15 . H152 . 108.6 no C15 . C16 . C17 . 113.3(4) yes C15 . C16 . C18 . 107.4(5) yes C17 . C16 . C18 . 110.6(5) yes C15 . C16 . H161 . 108.7 no C17 . C16 . H161 . 109.1 no C18 . C16 . H161 . 107.6 no C16 . C17 . H171 . 109.6 no C16 . C17 . H172 . 109.1 no H171 . C17 . H172 . 110.3 no C16 . C17 . H173 . 108.9 no H171 . C17 . H173 . 109.6 no H172 . C17 . H173 . 109.3 no C16 . C18 . H181 . 110.6 no C16 . C18 . H182 . 108.6 no H181 . C18 . H182 . 109.9 no C16 . C18 . H183 . 109.2 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.0 no C20 . C19 . H191 . 110.0 no C20 . C19 . H192 . 109.8 no H191 . C19 . H192 . 111.3 no C20 . C19 . H193 . 107.8 no H191 . C19 . H193 . 108.3 no H192 . C19 . H193 . 109.5 no C19 . C20 . C21 . 107.6(5) yes C19 . C20 . C22 . 111.7(5) yes C21 . C20 . C22 . 109.3(6) yes C19 . C20 . H201 . 110.0 no C21 . C20 . H201 . 109.1 no C22 . C20 . H201 . 109.0 no C20 . C21 . H211 . 110.2 no C20 . C21 . H212 . 111.0 no H211 . C21 . H212 . 109.0 no C20 . C21 . H213 . 107.2 no H211 . C21 . H213 . 109.8 no H212 . C21 . H213 . 109.6 no C20 . C22 . P3 . 118.7(5) yes C20 . C22 . H221 . 108.1 no P3 . C22 . H221 . 108.0 no C20 . C22 . H222 . 106.0 no P3 . C22 . H222 . 106.4 no H221 . C22 . H222 . 109.4 no C25 . C23 . H231 . 111.0 no C25 . C23 . H232 . 108.8 no H231 . C23 . H232 . 110.0 no C25 . C23 . H233 . 109.9 no H231 . C23 . H233 . 108.2 no H232 . C23 . H233 . 108.9 no C25 . C24 . H241 . 109.8 no C25 . C24 . H242 . 107.9 no H241 . C24 . H242 . 108.7 no C25 . C24 . H243 . 110.0 no H241 . C24 . H243 . 110.5 no H242 . C24 . H243 . 109.8 no C23 . C25 . C24 . 109.3(5) yes C23 . C25 . C26 . 110.9(5) yes C24 . C25 . C26 . 110.2(5) yes C23 . C25 . H251 . 109.2 no C24 . C25 . H251 . 107.9 no C26 . C25 . H251 . 109.4 no C25 . C26 . P3 . 117.8(3) yes C25 . C26 . H261 . 108.8 no P3 . C26 . H261 . 109.5 no C25 . C26 . H262 . 104.2 no P3 . C26 . H262 . 106.6 no H261 . C26 . H262 . 109.6 no P3 . C27 . C28 . 113.3(3) yes P3 . C27 . H271 . 108.4 no C28 . C27 . H271 . 109.3 no P3 . C27 . H272 . 104.4 no C28 . C27 . H272 . 111.3 no H271 . C27 . H272 . 110.1 no C27 . C28 . P4 . 109.5(3) yes C27 . C28 . H281 . 109.2 no P4 . C28 . H281 . 110.0 no C27 . C28 . H282 . 110.4 no P4 . C28 . H282 . 108.7 no H281 . C28 . H282 . 109.0 no C31 . C29 . H291 . 109.2 no C31 . C29 . H292 . 109.5 no H291 . C29 . H292 . 110.0 no C31 . C29 . H293 . 108.3 no H291 . C29 . H293 . 110.1 no H292 . C29 . H293 . 109.6 no C31 . C30 . H301 . 108.7 no C31 . C30 . H302 . 108.7 no H301 . C30 . H302 . 108.8 no C31 . C30 . H303 . 111.0 no H301 . C30 . H303 . 110.4 no H302 . C30 . H303 . 109.2 no C29 . C31 . C30 . 110.4(4) yes C29 . C31 . C32 . 108.2(4) yes C30 . C31 . C32 . 111.9(4) yes C29 . C31 . H311 . 107.8 no C30 . C31 . H311 . 109.8 no C32 . C31 . H311 . 108.7 no C31 . C32 . P4 . 119.9(3) yes C31 . C32 . H321 . 107.1 no P4 . C32 . H321 . 105.1 no C31 . C32 . H322 . 107.4 no P4 . C32 . H322 . 106.6 no H321 . C32 . H322 . 110.5 no C35 . C33 . H331 . 108.2 no C35 . C33 . H332 . 108.1 no H331 . C33 . H332 . 109.6 no C35 . C33 . H333 . 110.6 no H331 . C33 . H333 . 110.9 no H332 . C33 . H333 . 109.5 no C35 . C34 . H341 . 107.9 no C35 . C34 . H342 . 107.9 no H341 . C34 . H342 . 110.1 no C35 . C34 . H343 . 110.6 no H341 . C34 . H343 . 110.1 no H342 . C34 . H343 . 110.3 no C33 . C35 . C34 . 110.3(6) yes C33 . C35 . C36 . 109.7(5) yes C34 . C35 . C36 . 111.0(5) yes C33 . C35 . H351 . 108.2 no C34 . C35 . H351 . 108.5 no C36 . C35 . H351 . 109.1 no C35 . C36 . P4 . 118.0(3) yes C35 . C36 . H361 . 108.2 no P4 . C36 . H361 . 107.6 no C35 . C36 . H362 . 107.2 no P4 . C36 . H362 . 106.5 no H361 . C36 . H362 . 109.1 no Rh1 . C37 . C38 . 114.8(3) yes Rh1 . C37 . C42 . 125.8(3) yes C38 . C37 . C42 . 119.4(3) yes C37 . C38 . C39 . 117.7(3) yes C37 . C38 . H381 . 121.5 no C39 . C38 . H381 . 120.8 no Cl3 . C39 . C38 . 117.6(3) yes Cl3 . C39 . C40 . 119.5(3) yes C38 . C39 . C40 . 122.9(3) yes C39 . C40 . C41 . 120.5(3) yes C39 . C40 . H401 . 119.9 no C41 . C40 . H401 . 119.6 no B1 . C41 . C40 . 120.2(3) yes B1 . C41 . C42 . 123.6(3) yes C40 . C41 . C42 . 116.2(3) yes C41 . C42 . C37 . 123.3(3) yes C41 . C42 . H421 . 117.8 no C37 . C42 . H421 . 118.9 no B1 . C43 . C44 . 119.3(3) yes B1 . C43 . C48 . 123.7(3) yes C44 . C43 . C48 . 117.0(3) yes C43 . C44 . C45 . 120.5(4) yes C43 . C44 . H441 . 120.2 no C45 . C44 . H441 . 119.3 no Cl7 . C45 . C44 . 119.1(3) yes Cl7 . C45 . C46 . 118.3(3) yes C44 . C45 . C46 . 122.6(4) yes C45 . C46 . C47 . 116.2(4) yes C45 . C46 . H461 . 121.5 no C47 . C46 . H461 . 122.2 no Cl6 . C47 . C46 . 118.6(3) yes Cl6 . C47 . C48 . 118.5(4) yes C46 . C47 . C48 . 122.9(4) yes C43 . C48 . C47 . 120.7(4) yes C43 . C48 . H481 . 119.9 no C47 . C48 . H481 . 119.3 no B1 . C49 . C50 . 123.5(3) yes B1 . C49 . C54 . 119.6(3) yes C50 . C49 . C54 . 116.5(3) yes C49 . C50 . C51 . 121.1(3) yes C49 . C50 . H501 . 119.6 no C51 . C50 . H501 . 119.4 no Cl8 . C51 . C50 . 119.2(3) yes Cl8 . C51 . C52 . 118.0(3) yes C50 . C51 . C52 . 122.7(4) yes C51 . C52 . C53 . 116.2(3) yes C51 . C52 . H521 . 122.3 no C53 . C52 . H521 . 121.5 no Cl9 . C53 . C52 . 117.5(3) yes Cl9 . C53 . C54 . 120.2(3) yes C52 . C53 . C54 . 122.3(4) yes C49 . C54 . C53 . 121.2(3) yes C49 . C54 . H541 . 119.7 no C53 . C54 . H541 . 119.1 no B1 . C55 . C56 . 124.6(3) yes B1 . C55 . C60 . 119.0(3) yes C56 . C55 . C60 . 116.4(3) yes C55 . C56 . C57 . 120.5(4) yes C55 . C56 . H561 . 119.8 no C57 . C56 . H561 . 119.7 no Cl5 . C57 . C56 . 119.5(3) yes Cl5 . C57 . C58 . 117.3(3) yes C56 . C57 . C58 . 123.2(4) yes C57 . C58 . C59 . 116.4(4) yes C57 . C58 . H581 . 121.5 no C59 . C58 . H581 . 122.1 no Cl4 . C59 . C58 . 118.2(3) yes Cl4 . C59 . C60 . 119.7(3) yes C58 . C59 . C60 . 122.1(4) yes C55 . C60 . C59 . 121.5(3) yes C55 . C60 . H601 . 119.7 no C59 . C60 . H601 . 118.8 no Rh2 . C61 . C62 . 110.5(3) yes Rh2 . C61 . C66 . 128.7(3) yes C62 . C61 . C66 . 120.8(3) yes C61 . C62 . C63 . 117.4(3) yes C61 . C62 . H621 . 121.2 no C63 . C62 . H621 . 121.4 no Cl10 . C63 . C62 . 118.0(3) yes Cl10 . C63 . C64 . 119.4(3) yes C62 . C63 . C64 . 122.5(4) yes C63 . C64 . C65 . 121.1(3) yes C63 . C64 . H641 . 119.2 no C65 . C64 . H641 . 119.7 no B2 . C65 . C64 . 118.5(3) yes B2 . C65 . C66 . 125.2(3) yes C64 . C65 . C66 . 116.3(3) yes C65 . C66 . C61 . 121.8(3) yes C65 . C66 . H661 . 119.3 no C61 . C66 . H661 . 118.9 no B2 . C67 . C68 . 124.8(3) yes B2 . C67 . C72 . 118.9(3) yes C68 . C67 . C72 . 116.3(3) yes C67 . C68 . C69 . 121.2(4) yes C67 . C68 . H681 . 119.1 no C69 . C68 . H681 . 119.6 no Cl14 . C69 . C68 . 118.9(3) yes Cl14 . C69 . C70 . 118.9(3) yes C68 . C69 . C70 . 122.2(4) yes C69 . C70 . C71 . 116.8(4) yes C69 . C70 . H701 . 122.0 no C71 . C70 . H701 . 121.2 no Cl13 . C71 . C70 . 118.3(3) yes Cl13 . C71 . C72 . 119.2(3) yes C70 . C71 . C72 . 122.5(4) yes C67 . C72 . C71 . 120.9(4) yes C67 . C72 . H721 . 119.7 no C71 . C72 . H721 . 119.5 no B2 . C73 . C74 . 124.6(3) yes B2 . C73 . C78 . 118.8(3) yes C74 . C73 . C78 . 116.5(3) yes C73 . C74 . C75 . 120.3(4) yes C73 . C74 . H741 . 120.3 no C75 . C74 . H741 . 119.4 no Cl12 . C75 . C74 . 119.5(3) yes Cl12 . C75 . C76 . 117.7(3) yes C74 . C75 . C76 . 122.9(4) yes C75 . C76 . C77 . 116.8(4) yes C75 . C76 . H761 . 121.5 no C77 . C76 . H761 . 121.7 no Cl11 . C77 . C76 . 117.7(3) yes Cl11 . C77 . C78 . 120.6(3) yes C76 . C77 . C78 . 121.8(4) yes C73 . C78 . C77 . 121.7(4) yes C73 . C78 . H781 . 119.7 no C77 . C78 . H781 . 118.6 no B2 . C79 . C80 . 118.8(3) yes B2 . C79 . C84 . 124.7(3) yes C80 . C79 . C84 . 116.4(4) yes C79 . C80 . C81 . 121.2(4) yes C79 . C80 . H801 . 119.4 no C81 . C80 . H801 . 119.4 no Cl16 . C81 . C80 . 119.7(3) yes Cl16 . C81 . C82 . 118.0(3) yes C80 . C81 . C82 . 122.4(4) yes C81 . C82 . C83 . 116.3(4) yes C81 . C82 . H821 . 121.9 no C83 . C82 . H821 . 121.8 no Cl15 . C83 . C82 . 118.1(4) yes Cl15 . C83 . C84 . 119.1(4) yes C82 . C83 . C84 . 122.7(4) yes C79 . C84 . C83 . 120.9(4) yes C79 . C84 . H841 . 120.5 no C83 . C84 . H841 . 118.5 no Cl202 . C201 . Cl203 . 114.54(7) yes Cl202 . C201 . H2011 . 107.3 no Cl203 . C201 . H2011 . 107.6 no Cl202 . C201 . H2012 . 108.9 no Cl203 . C201 . H2012 . 108.8 no H2011 . C201 . H2012 . 109.6 no Cl205 . C204 . Cl206 . 114.50(7) yes Cl205 . C204 . H2041 . 101.7 no Cl206 . C204 . H2041 . 107.3 no Cl205 . C204 . H2042 . 109.0 no Cl206 . C204 . H2042 . 112.2 no H2041 . C204 . H2042 . 111.8 no Cl208 . C207 . Cl209 . 114.56(7) yes Cl208 . C207 . H2071 . 108.6 no Cl209 . C207 . H2071 . 106.5 no Cl208 . C207 . H2072 . 108.4 no Cl209 . C207 . H2072 . 108.3 no H2071 . C207 . H2072 . 110.5 no Cl211 . C210 . Cl212 . 114.52(7) yes Cl211 . C210 . H2101 . 108.2 no Cl212 . C210 . H2101 . 107.9 no Cl211 . C210 . H2102 . 107.8 no Cl212 . C210 . H2102 . 108.7 no H2101 . C210 . H2102 . 109.6 no Cl214 . C213 . Cl215 . 114.54(7) yes Cl214 . C213 . H2131 . 107.9 no Cl215 . C213 . H2131 . 108.7 no Cl214 . C213 . H2132 . 107.7 no Cl215 . C213 . H2132 . 108.7 no H2131 . C213 . H2132 . 109.2 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C42 . H421 . C9 . 143.87 0.931 2.594 3.390(7) yes C68 . H681 . C64 . 123.14 0.932 2.584 3.191(7) yes _iucr_refine_instruction_details_constraints ; # # Punched on 18/03/13 at 18:18:39 # #LIST 12 BLOCK SCALE X'S, U'S EQUIV PART(1001,OCC) PART(1002,OCC) WEIGHT -1 PART(1002,OCC) EQUIV PART(-2001,OCC) RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S) RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) H ( 42,X'S) RIDE C ( 5,X'S) H ( 51,X'S) H ( 52,X'S) H ( 53,X'S) RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) H ( 63,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) RIDE C ( 10,X'S) H ( 101,X'S) H ( 102,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) RIDE C ( 12,X'S) H ( 121,X'S) H ( 122,X'S) H ( 123,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) H ( 173,X'S) RIDE C ( 18,X'S) H ( 181,X'S) H ( 182,X'S) H ( 183,X'S) RIDE C ( 19,X'S) H ( 191,X'S) H ( 192,X'S) H ( 193,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) H ( 212,X'S) H ( 213,X'S) RIDE C ( 22,X'S) H ( 221,X'S) H ( 222,X'S) RIDE C ( 23,X'S) H ( 231,X'S) H ( 232,X'S) H ( 233,X'S) RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S) H ( 243,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) H ( 262,X'S) RIDE C ( 27,X'S) H ( 271,X'S) H ( 272,X'S) RIDE C ( 28,X'S) H ( 281,X'S) H ( 282,X'S) RIDE C ( 29,X'S) H ( 291,X'S) H ( 292,X'S) H ( 293,X'S) RIDE C ( 30,X'S) H ( 301,X'S) H ( 302,X'S) H ( 303,X'S) RIDE C ( 31,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 321,X'S) H ( 322,X'S) RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S) H ( 333,X'S) RIDE C ( 34,X'S) H ( 341,X'S) H ( 342,X'S) H ( 343,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) H ( 362,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 46,X'S) H ( 461,X'S) RIDE C ( 48,X'S) H ( 481,X'S) RIDE C ( 50,X'S) H ( 501,X'S) RIDE C ( 52,X'S) H ( 521,X'S) RIDE C ( 54,X'S) H ( 541,X'S) RIDE C ( 56,X'S) H ( 561,X'S) RIDE C ( 58,X'S) H ( 581,X'S) RIDE C ( 60,X'S) H ( 601,X'S) RIDE C ( 62,X'S) H ( 621,X'S) RIDE C ( 64,X'S) H ( 641,X'S) RIDE C ( 66,X'S) H ( 661,X'S) RIDE C ( 68,X'S) H ( 681,X'S) RIDE C ( 70,X'S) H ( 701,X'S) RIDE C ( 72,X'S) H ( 721,X'S) RIDE C ( 74,X'S) H ( 741,X'S) RIDE C ( 76,X'S) H ( 761,X'S) RIDE C ( 78,X'S) H ( 781,X'S) RIDE C ( 80,X'S) H ( 801,X'S) RIDE C ( 82,X'S) H ( 821,X'S) RIDE C ( 84,X'S) H ( 841,X'S) RIDE C ( 201,X'S) H (2011,X'S) H (2012,X'S) RIDE C ( 204,X'S) H (2041,X'S) H (2042,X'S) RIDE C ( 207,X'S) H (2071,X'S) H (2072,X'S) RIDE C ( 210,X'S) H (2101,X'S) H (2102,X'S) RIDE C ( 213,X'S) H (2131,X'S) H (2132,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 18/03/13 at 18:18:39 # #LIST 16 SAME C(201) CL(202) CL(203) AND CONT C(201) CL(203) CL(202) AND CONT C(204) CL(205) CL(206) AND CONT C(204) CL(206) CL(205) AND CONT C(207) CL(208) CL(209) AND CONT C(207) CL(209) CL(208) AND CONT C(210) CL(211) CL(212) AND CONT C(210) CL(212) CL(211) AND CONT C(213) CL(214) CL(215) AND CONT C(213) CL(215) CL(214) SIMU 0.01 C(201) CL(202) CL(203) AND CONT C(201) CL(203) CL(202) AND CONT C(204) CL(205) CL(206) AND CONT C(204) CL(206) CL(205) AND CONT C(207) CL(208) CL(209) AND CONT C(207) CL(209) CL(208) AND CONT C(210) CL(211) CL(212) AND CONT C(210) CL(212) CL(211) AND CONT C(213) CL(214) CL(215) AND CONT C(213) CL(215) CL(214) DELU 0.01 C(201) CL(202) CL(203) AND CONT C(201) CL(203) CL(202) AND CONT C(204) CL(205) CL(206) AND CONT C(204) CL(206) CL(205) AND CONT C(207) CL(208) CL(209) AND CONT C(207) CL(209) CL(208) AND CONT C(210) CL(211) CL(212) AND CONT C(210) CL(212) CL(211) AND CONT C(213) CL(214) CL(215) AND CONT C(213) CL(215) CL(214) END ; # start Validation Reply Form _vrf_PLAT220_Compound3 ; PROBLEM: Large Non-Solvent C/Cl Ueq(max)/Ueq(min) ...4.2/3.8 Ratio RESPONSE: The large molecule contains isopropyl and C6H3Cl2 groups which have larger thermal ellipsoids than the central atoms due to greater degrees of freedom. ; _vrf_PLAT222_Compound3 ; PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) ..5.2 Ratio RESPONSE: The large molecule contains isopropyl and C6H3Cl2 groups which have larger thermal ellipsoids than the central atoms due to greater degrees of freedom. ; _vrf_PLAT242_Compound3 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C35 RESPONSE: C35 is bonded to two methyl groups which show larger thermal ellipsoids due to slight disorder ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 945337'