# Electronic Supplementary Material (ESI) for Chemical Science # 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_5883 #TrackingRef '19474_web_deposit_cif_file_0_JohnBrown_1366025934.5883o.cif' _oxford_structure_analysis_title 5883 _ccdc_journal_depnumber ? _computing_structure_solution ; 'SIR92 (Giacovazzo et al, 1992)' ; _chemical_name_systematic ; ((Bicyclo[2.2.1]hepta-2,5-diene)((rac)-bis-2,2'-(diphenylphosphino)-1,1' -binaphthalene)rhodium)((rac)-bis-(1,1'-binaphthalen-2,2'-dioxo)boronate). ; _chemical_melting_point ; Not determined ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 356 30 ' ' 2 0.000 0.500 0.000 357 30 ' ' 3 0.264 0.173 0.433 32 1 ' ' 4 0.264 0.327 0.933 32 1 ' ' 5 0.736 0.673 0.067 32 1 ' ' 6 0.736 0.827 0.567 31 1 ' ' _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 19.3718(2) _cell_length_b 20.1092(2) _cell_length_c 21.5060(2) _cell_angle_alpha 90 _cell_angle_beta 93.7932(3) _cell_angle_gamma 90 _cell_volume 8359.34(14) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 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 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' 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' O 0.0106 0.0060 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' 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' 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' 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 4 # Given Formula = C92 H68 B1 Cl1 O4 P2 Rh1 # Dc = 1.15 Fooo = 3432.00 Mu = 3.22 M = 1448.67 # Found Formula = C95 H74 B1 Cl6 O4 P2 Rh1 # Dc = 1.33 FOOO = 3432.00 Mu = 4.86 M = 1668.01 _chemical_formula_sum 'C95 H74 B1 Cl6 O4 P2 Rh1' _chemical_formula_moiety 'C52 H44 P2 Rh, C40 H24 B O4, 3(C H2 Cl2)' _chemical_compound_source . _chemical_formula_weight 1668.01 _cell_measurement_reflns_used 19378 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour clear_intense_yellow _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3432 _exptl_absorpt_coefficient_mu 0.486 # Sheldrick geometric approximatio 0.87 0.98 _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 0.98 # 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 'Nonius KappaCCD' _diffrn_measurement_device_type 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, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 129861 _reflns_number_total 19014 _diffrn_reflns_av_R_equivalents 0.048 # Number of reflections with Friedels Law is 19014 # Number of reflections without Friedels Law is 19014 # Theoretical number of reflections is about 19162 _diffrn_reflns_theta_min 5.104 _diffrn_reflns_theta_max 27.478 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.478 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -25 _reflns_limit_h_max 25 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _oxford_diffrn_Wilson_B_factor 2.09 _oxford_diffrn_Wilson_scale 23.61 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.48 _refine_diff_density_max 0.78 # 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 19008 _refine_ls_number_restraints 0 _refine_ls_number_parameters 989 _oxford_refine_ls_R_factor_ref 0.0703 _refine_ls_wR_factor_ref 0.1456 _refine_ls_goodness_of_fit_ref 0.9999 _refine_ls_shift/su_max 0.001264 # The values computed from all data _oxford_reflns_number_all 19014 _refine_ls_R_factor_all 0.0703 _refine_ls_wR_factor_all 0.1458 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 14743 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_gt 0.1331 # 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 # none, 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^ +21.54P] ,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 atomsattached 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Rh1 Rh 0.346292(11) 0.497993(11) 0.262889(10) 0.0204 1.0000 Uani . . . . . . . P2 P 0.23929(4) 0.44451(4) 0.24896(3) 0.0196 1.0000 Uani . . . . . . . C3 C 0.20017(14) 0.40491(14) 0.31583(13) 0.0206 1.0000 Uani . . . . . . . C4 C 0.19751(15) 0.33442(15) 0.32040(15) 0.0249 1.0000 Uani . . . . . . . C5 C 0.17503(16) 0.30421(15) 0.37233(15) 0.0272 1.0000 Uani . . . . . . . C6 C 0.15376(15) 0.34208(15) 0.42286(14) 0.0256 1.0000 Uani . . . . . . . C7 C 0.15582(14) 0.41229(15) 0.41915(14) 0.0228 1.0000 Uani . . . . . . . C8 C 0.17926(14) 0.44332(14) 0.36443(13) 0.0208 1.0000 Uani . . . . . . . C9 C 0.18026(14) 0.51777(14) 0.36087(13) 0.0198 1.0000 Uani . . . . . . . C10 C 0.24144(14) 0.55345(14) 0.36309(13) 0.0195 1.0000 Uani . . . . . . . P11 P 0.32617(4) 0.51332(4) 0.36646(3) 0.0205 1.0000 Uani . . . . . . . C12 C 0.38192(15) 0.56497(15) 0.41951(14) 0.0243 1.0000 Uani . . . . . . . C13 C 0.45192(16) 0.54653(17) 0.42741(15) 0.0301 1.0000 Uani . . . . . . . C14 C 0.49629(17) 0.5790(2) 0.47078(17) 0.0374 1.0000 Uani . . . . . . . C15 C 0.47135(19) 0.62903(19) 0.50749(17) 0.0405 1.0000 Uani . . . . . . . C16 C 0.4024(2) 0.64594(18) 0.50169(18) 0.0404 1.0000 Uani . . . . . . . C17 C 0.35763(18) 0.61456(17) 0.45755(16) 0.0333 1.0000 Uani . . . . . . . C18 C 0.32619(14) 0.43871(15) 0.41520(14) 0.0228 1.0000 Uani . . . . . . . C19 C 0.35122(15) 0.37928(15) 0.39295(15) 0.0263 1.0000 Uani . . . . . . . C20 C 0.35639(16) 0.32355(16) 0.43171(17) 0.0315 1.0000 Uani . . . . . . . C21 C 0.33699(16) 0.32740(17) 0.49203(16) 0.0331 1.0000 Uani . . . . . . . C22 C 0.31165(15) 0.38689(17) 0.51446(15) 0.0292 1.0000 Uani . . . . . . . C23 C 0.30698(14) 0.44237(16) 0.47655(14) 0.0249 1.0000 Uani . . . . . . . C24 C 0.24012(15) 0.62341(14) 0.35129(13) 0.0222 1.0000 Uani . . . . . . . C25 C 0.17891(16) 0.65655(15) 0.34240(14) 0.0248 1.0000 Uani . . . . . . . C26 C 0.11485(15) 0.62240(15) 0.34350(13) 0.0226 1.0000 Uani . . . . . . . C27 C 0.11499(14) 0.55216(15) 0.35112(13) 0.0214 1.0000 Uani . . . . . . . C28 C 0.05074(15) 0.51812(15) 0.34808(14) 0.0236 1.0000 Uani . . . . . . . C29 C -0.01052(16) 0.55211(17) 0.33956(14) 0.0277 1.0000 Uani . . . . . . . C30 C -0.01052(16) 0.62204(17) 0.33357(15) 0.0299 1.0000 Uani . . . . . . . C31 C 0.05051(16) 0.65612(16) 0.33535(15) 0.0283 1.0000 Uani . . . . . . . C32 C 0.13693(15) 0.44995(17) 0.47151(14) 0.0269 1.0000 Uani . . . . . . . C33 C 0.11604(17) 0.41842(19) 0.52348(16) 0.0348 1.0000 Uani . . . . . . . C34 C 0.11264(19) 0.3489(2) 0.52640(17) 0.0392 1.0000 Uani . . . . . . . C35 C 0.13118(17) 0.31142(18) 0.47732(16) 0.0343 1.0000 Uani . . . . . . . C36 C 0.17249(15) 0.50267(15) 0.21959(13) 0.0217 1.0000 Uani . . . . . . . C37 C 0.10349(15) 0.48183(16) 0.21103(14) 0.0258 1.0000 Uani . . . . . . . C38 C 0.05301(17) 0.52604(18) 0.18853(15) 0.0326 1.0000 Uani . . . . . . . C39 C 0.07006(19) 0.59151(19) 0.17665(16) 0.0373 1.0000 Uani . . . . . . . C40 C 0.13765(19) 0.61268(17) 0.18593(16) 0.0356 1.0000 Uani . . . . . . . C41 C 0.18903(16) 0.56856(15) 0.20692(14) 0.0267 1.0000 Uani . . . . . . . C42 C 0.23716(15) 0.37868(15) 0.18957(14) 0.0232 1.0000 Uani . . . . . . . C43 C 0.19437(16) 0.38160(17) 0.13531(15) 0.0282 1.0000 Uani . . . . . . . C44 C 0.19434(18) 0.33014(19) 0.09156(17) 0.0385 1.0000 Uani . . . . . . . C45 C 0.23675(18) 0.27571(18) 0.10213(18) 0.0393 1.0000 Uani . . . . . . . C46 C 0.28107(18) 0.27297(17) 0.15521(18) 0.0366 1.0000 Uani . . . . . . . C47 C 0.28185(16) 0.32409(15) 0.19835(16) 0.0294 1.0000 Uani . . . . . . . C48 C 0.40315(17) 0.59325(16) 0.25855(16) 0.0304 1.0000 Uani . . . . . . . C49 C 0.45276(16) 0.54467(17) 0.26595(16) 0.0301 1.0000 Uani . . . . . . . C50 C 0.49563(18) 0.51873(19) 0.21482(19) 0.0391 1.0000 Uani . . . . . . . C51 C 0.46456(18) 0.4563(2) 0.1844(2) 0.0432 1.0000 Uani . . . . . . . C52 C 0.38695(17) 0.45677(17) 0.17636(15) 0.0310 1.0000 Uani . . . . . . . C53 C 0.34480(18) 0.50964(17) 0.15930(15) 0.0312 1.0000 Uani . . . . . . . C54 C 0.3684(2) 0.57908(19) 0.14255(17) 0.0400 1.0000 Uani . . . . . . . C55 C 0.37910(19) 0.62650(18) 0.19834(18) 0.0388 1.0000 Uani . . . . . . . Cl56 Cl 0.32335(12) 1.03392(9) 0.34834(9) 0.1060 1.0000 Uani . . . . . . . C57 C 0.3434(6) 0.9699(6) 0.4019(5) 0.066(2) 0.5000 Uiso . . . . 1 . . Cl58 Cl 0.3047(3) 0.98592(16) 0.46946(16) 0.1045 0.5000 Uani . . . . 1 . . C59 C 0.3531(6) 0.9630(6) 0.3809(6) 0.066(2) 0.5000 Uiso . . . . 2 . . Cl60 Cl 0.4121(2) 0.98380(16) 0.44362(19) 0.1008 0.5000 Uani . . . . 2 . . Cl61 Cl 0.19419(9) 0.14910(9) 0.26481(10) 0.0970 1.0000 Uani . . . . . . . C62 C 0.1476(4) 0.0840(4) 0.2959(3) 0.0968 1.0000 Uani . . . . . . . Cl63 Cl 0.12792(10) 0.09807(12) 0.37243(9) 0.1108 1.0000 Uani . . . . . . . Cl64 Cl 0.37395(7) 0.96752(6) 0.12719(7) 0.0661 1.0000 Uani . . . . . . . C65 C 0.2970(3) 0.9510(2) 0.1617(3) 0.0650 1.0000 Uani . . . . . . . Cl66 Cl 0.23855(7) 1.01753(7) 0.15516(8) 0.0757 1.0000 Uani . . . . . . . O67 O 0.36674(11) 0.84667(11) 0.26130(10) 0.0274 1.0000 Uani . . . . . . . C68 C 0.42377(15) 0.80820(15) 0.25680(14) 0.0241 1.0000 Uani . . . . . . . C69 C 0.45201(17) 0.80434(16) 0.19742(15) 0.0289 1.0000 Uani . . . . . . . C70 C 0.50811(17) 0.76578(17) 0.18901(15) 0.0305 1.0000 Uani . . . . . . . C71 C 0.53762(16) 0.72593(16) 0.23843(14) 0.0266 1.0000 Uani . . . . . . . C72 C 0.51034(15) 0.73060(15) 0.29841(14) 0.0239 1.0000 Uani . . . . . . . C73 C 0.45573(15) 0.77675(15) 0.30834(13) 0.0229 1.0000 Uani . . . . . . . C74 C 0.43167(15) 0.79092(14) 0.37132(14) 0.0233 1.0000 Uani . . . . . . . C75 C 0.47907(16) 0.80994(14) 0.42250(14) 0.0245 1.0000 Uani . . . . . . . C76 C 0.55058(16) 0.82163(15) 0.41585(15) 0.0279 1.0000 Uani . . . . . . . C77 C 0.59425(19) 0.84081(17) 0.46535(17) 0.0367 1.0000 Uani . . . . . . . C78 C 0.5696(2) 0.84796(19) 0.52537(18) 0.0424 1.0000 Uani . . . . . . . C79 C 0.5012(2) 0.83817(18) 0.53344(17) 0.0397 1.0000 Uani . . . . . . . C80 C 0.45433(18) 0.82065(16) 0.48270(15) 0.0307 1.0000 Uani . . . . . . . C81 C 0.38234(19) 0.81505(17) 0.49020(16) 0.0344 1.0000 Uani . . . . . . . C82 C 0.33736(17) 0.80070(17) 0.44070(15) 0.0316 1.0000 Uani . . . . . . . C83 C 0.36155(16) 0.78903(15) 0.38088(14) 0.0256 1.0000 Uani . . . . . . . O84 O 0.31334(11) 0.77248(11) 0.33490(10) 0.0298 1.0000 Uani . . . . . . . B85 B 0.30308(17) 0.81343(18) 0.27891(16) 0.0260 1.0000 Uani . . . . . . . O86 O 0.27445(11) 0.76525(11) 0.23306(10) 0.0275 1.0000 Uani . . . . . . . C87 C 0.23961(16) 0.78668(15) 0.18030(14) 0.0252 1.0000 Uani . . . . . . . C88 C 0.17680(15) 0.81982(14) 0.18176(14) 0.0234 1.0000 Uani . . . . . . . C89 C 0.14700(15) 0.83305(15) 0.24262(14) 0.0239 1.0000 Uani . . . . . . . C90 C 0.07667(15) 0.81713(15) 0.25396(14) 0.0249 1.0000 Uani . . . . . . . C91 C 0.03336(16) 0.77873(16) 0.21217(15) 0.0276 1.0000 Uani . . . . . . . C92 C -0.03342(16) 0.76317(17) 0.22496(16) 0.0330 1.0000 Uani . . . . . . . C93 C -0.06081(16) 0.78581(18) 0.28019(17) 0.0341 1.0000 Uani . . . . . . . C94 C -0.02050(17) 0.82194(17) 0.32194(16) 0.0323 1.0000 Uani . . . . . . . C95 C 0.04889(16) 0.83793(16) 0.31099(15) 0.0284 1.0000 Uani . . . . . . . C96 C 0.09244(18) 0.87178(19) 0.35612(16) 0.0355 1.0000 Uani . . . . . . . C97 C 0.16066(17) 0.88134(18) 0.34715(16) 0.0340 1.0000 Uani . . . . . . . C98 C 0.18858(15) 0.86034(15) 0.29082(15) 0.0259 1.0000 Uani . . . . . . . O99 O 0.25726(11) 0.87123(11) 0.28602(10) 0.0276 1.0000 Uani . . . . . . . C100 C 0.14398(15) 0.84331(15) 0.12376(14) 0.0242 1.0000 Uani . . . . . . . C101 C 0.08396(16) 0.88415(16) 0.12015(14) 0.0266 1.0000 Uani . . . . . . . C102 C 0.05267(17) 0.90347(17) 0.06386(15) 0.0311 1.0000 Uani . . . . . . . C103 C 0.07985(18) 0.88420(18) 0.00756(15) 0.0341 1.0000 Uani . . . . . . . C104 C 0.13874(18) 0.84735(19) 0.00898(16) 0.0357 1.0000 Uani . . . . . . . C105 C 0.17308(16) 0.82655(17) 0.06657(15) 0.0290 1.0000 Uani . . . . . . . C106 C 0.23493(17) 0.78934(18) 0.06765(16) 0.0341 1.0000 Uani . . . . . . . C107 C 0.26782(16) 0.77084(16) 0.12330(15) 0.0303 1.0000 Uani . . . . . . . C108 C 0.53668(15) 0.68627(15) 0.34554(15) 0.0260 1.0000 Uani . . . . . . . C109 C 0.58672(16) 0.64102(16) 0.33430(16) 0.0307 1.0000 Uani . . . . . . . C110 C 0.61542(17) 0.63775(18) 0.27579(17) 0.0351 1.0000 Uani . . . . . . . C111 C 0.59133(17) 0.67963(17) 0.22919(17) 0.0333 1.0000 Uani . . . . . . . H41 H 0.2115 0.3080 0.2877 0.0303 1.0000 Uiso R . . . . . . H51 H 0.1731 0.2576 0.3731 0.0312 1.0000 Uiso R . . . . . . H131 H 0.4695 0.5123 0.4042 0.0355 1.0000 Uiso R . . . . . . H141 H 0.5429 0.5665 0.4745 0.0444 1.0000 Uiso R . . . . . . H151 H 0.5022 0.6517 0.5362 0.0480 1.0000 Uiso R . . . . . . H161 H 0.3843 0.6779 0.5277 0.0495 1.0000 Uiso R . . . . . . H171 H 0.3106 0.6272 0.4523 0.0414 1.0000 Uiso R . . . . . . H191 H 0.3646 0.3767 0.3507 0.0315 1.0000 Uiso R . . . . . . H201 H 0.3724 0.2835 0.4160 0.0361 1.0000 Uiso R . . . . . . H211 H 0.3413 0.2902 0.5189 0.0382 1.0000 Uiso R . . . . . . H221 H 0.2971 0.3900 0.5541 0.0342 1.0000 Uiso R . . . . . . H231 H 0.2912 0.4820 0.4924 0.0302 1.0000 Uiso R . . . . . . H241 H 0.2824 0.6465 0.3507 0.0263 1.0000 Uiso R . . . . . . H251 H 0.1786 0.7024 0.3356 0.0281 1.0000 Uiso R . . . . . . H281 H 0.0497 0.4718 0.3517 0.0277 1.0000 Uiso R . . . . . . H291 H -0.0526 0.5282 0.3377 0.0331 1.0000 Uiso R . . . . . . H301 H -0.0529 0.6452 0.3284 0.0352 1.0000 Uiso R . . . . . . H311 H 0.0496 0.7025 0.3314 0.0328 1.0000 Uiso R . . . . . . H321 H 0.1393 0.4958 0.4701 0.0320 1.0000 Uiso R . . . . . . H331 H 0.1038 0.4436 0.5570 0.0406 1.0000 Uiso R . . . . . . H341 H 0.0971 0.3279 0.5617 0.0462 1.0000 Uiso R . . . . . . H351 H 0.1306 0.2650 0.4800 0.0420 1.0000 Uiso R . . . . . . H371 H 0.0904 0.4382 0.2204 0.0304 1.0000 Uiso R . . . . . . H381 H 0.0080 0.5121 0.1811 0.0387 1.0000 Uiso R . . . . . . H391 H 0.0354 0.6210 0.1633 0.0416 1.0000 Uiso R . . . . . . H401 H 0.1488 0.6571 0.1764 0.0420 1.0000 Uiso R . . . . . . H411 H 0.2343 0.5833 0.2127 0.0325 1.0000 Uiso R . . . . . . H431 H 0.1653 0.4185 0.1286 0.0330 1.0000 Uiso R . . . . . . H441 H 0.1655 0.3325 0.0545 0.0449 1.0000 Uiso R . . . . . . H451 H 0.2353 0.2411 0.0724 0.0482 1.0000 Uiso R . . . . . . H461 H 0.3098 0.2359 0.1613 0.0441 1.0000 Uiso R . . . . . . H471 H 0.3122 0.3222 0.2331 0.0346 1.0000 Uiso R . . . . . . H481 H 0.3970 0.6205 0.2955 0.0359 1.0000 Uiso R . . . . . . H491 H 0.4749 0.5408 0.3072 0.0355 1.0000 Uiso R . . . . . . H501 H 0.5428 0.5093 0.2324 0.0468 1.0000 Uiso R . . . . . . H502 H 0.4982 0.5530 0.1828 0.0472 1.0000 Uiso R . . . . . . H511 H 0.4818 0.4525 0.1433 0.0520 1.0000 Uiso R . . . . . . H512 H 0.4789 0.4172 0.2082 0.0521 1.0000 Uiso R . . . . . . H521 H 0.3667 0.4121 0.1703 0.0367 1.0000 Uiso R . . . . . . H531 H 0.2990 0.4982 0.1398 0.0378 1.0000 Uiso R . . . . . . H541 H 0.4120 0.5748 0.1238 0.0491 1.0000 Uiso R . . . . . . H542 H 0.3335 0.5986 0.1126 0.0487 1.0000 Uiso R . . . . . . H551 H 0.4130 0.6599 0.1882 0.0481 1.0000 Uiso R . . . . . . H552 H 0.3351 0.6486 0.2049 0.0484 1.0000 Uiso R . . . . . . H571 H 0.3926 0.9681 0.4098 0.0772 0.5000 Uiso R . . . 1 . . H572 H 0.3268 0.9276 0.3849 0.0772 0.5000 Uiso R . . . 1 . . H591 H 0.3769 0.9375 0.3502 0.0770 0.5000 Uiso R . . . 2 . . H592 H 0.3151 0.9371 0.3960 0.0770 0.5000 Uiso R . . . 2 . . H622 H 0.1049 0.0779 0.2700 0.1215 1.0000 Uiso R . . . . . . H621 H 0.1765 0.0442 0.2966 0.1214 1.0000 Uiso R . . . . . . H652 H 0.3063 0.9420 0.2054 0.0713 1.0000 Uiso R . . . . . . H651 H 0.2764 0.9124 0.1416 0.0715 1.0000 Uiso R . . . . . . H691 H 0.4309 0.8288 0.1645 0.0347 1.0000 Uiso R . . . . . . H701 H 0.5274 0.7654 0.1506 0.0362 1.0000 Uiso R . . . . . . H761 H 0.5678 0.8162 0.3763 0.0324 1.0000 Uiso R . . . . . . H771 H 0.6409 0.8492 0.4590 0.0430 1.0000 Uiso R . . . . . . H781 H 0.6001 0.8596 0.5604 0.0480 1.0000 Uiso R . . . . . . H791 H 0.4855 0.8427 0.5746 0.0485 1.0000 Uiso R . . . . . . H811 H 0.3656 0.8215 0.5295 0.0401 1.0000 Uiso R . . . . . . H821 H 0.2897 0.7988 0.4458 0.0380 1.0000 Uiso R . . . . . . H911 H 0.0516 0.7630 0.1752 0.0329 1.0000 Uiso R . . . . . . H921 H -0.0621 0.7372 0.1956 0.0393 1.0000 Uiso R . . . . . . H931 H -0.1070 0.7760 0.2885 0.0413 1.0000 Uiso R . . . . . . H941 H -0.0392 0.8371 0.3590 0.0390 1.0000 Uiso R . . . . . . H961 H 0.0727 0.8876 0.3912 0.0402 1.0000 Uiso R . . . . . . H971 H 0.1900 0.9021 0.3771 0.0399 1.0000 Uiso R . . . . . . H1011 H 0.0650 0.8986 0.1567 0.0307 1.0000 Uiso R . . . . . . H1021 H 0.0133 0.9297 0.0627 0.0376 1.0000 Uiso R . . . . . . H1031 H 0.0570 0.8968 -0.0301 0.0404 1.0000 Uiso R . . . . . . H1041 H 0.1562 0.8354 -0.0291 0.0434 1.0000 Uiso R . . . . . . H1061 H 0.2531 0.7770 0.0298 0.0396 1.0000 Uiso R . . . . . . H1071 H 0.3092 0.7465 0.1235 0.0364 1.0000 Uiso R . . . . . . H1081 H 0.5194 0.6875 0.3856 0.0300 1.0000 Uiso R . . . . . . H1091 H 0.6022 0.6108 0.3657 0.0349 1.0000 Uiso R . . . . . . H1101 H 0.6502 0.6079 0.2674 0.0424 1.0000 Uiso R . . . . . . H1111 H 0.6102 0.6781 0.1913 0.0371 1.0000 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 Rh1 0.01970(11) 0.01905(11) 0.02253(12) -0.00001(9) 0.00162(8) -0.00253(8) P2 0.0195(3) 0.0175(3) 0.0217(4) -0.0004(3) 0.0001(3) -0.0003(3) C3 0.0183(13) 0.0199(13) 0.0229(14) 0.0003(11) -0.0030(10) -0.0027(10) C4 0.0256(14) 0.0199(14) 0.0285(15) 0.0000(12) -0.0027(12) -0.0027(11) C5 0.0293(15) 0.0189(14) 0.0324(17) 0.0050(12) -0.0046(12) -0.0041(12) C6 0.0210(13) 0.0260(15) 0.0290(16) 0.0080(12) -0.0057(11) -0.0026(12) C7 0.0167(12) 0.0268(15) 0.0244(15) 0.0044(12) -0.0027(11) -0.0021(11) C8 0.0160(12) 0.0208(14) 0.0249(14) 0.0024(11) -0.0044(10) -0.0021(10) C9 0.0213(13) 0.0203(13) 0.0179(13) 0.0013(10) 0.0016(10) -0.0007(10) C10 0.0219(13) 0.0184(13) 0.0181(13) 0.0007(10) 0.0003(10) 0.0009(10) P11 0.0185(3) 0.0195(3) 0.0234(4) 0.0001(3) -0.0003(3) -0.0014(3) C12 0.0232(14) 0.0220(14) 0.0268(15) 0.0033(11) -0.0040(11) -0.0046(11) C13 0.0244(15) 0.0352(17) 0.0301(16) 0.0071(13) -0.0018(12) -0.0034(13) C14 0.0235(15) 0.049(2) 0.0384(19) 0.0148(16) -0.0079(13) -0.0099(15) C15 0.0424(19) 0.0358(19) 0.040(2) 0.0064(15) -0.0195(16) -0.0165(16) C16 0.050(2) 0.0302(18) 0.039(2) -0.0071(15) -0.0133(16) -0.0038(16) C17 0.0337(17) 0.0285(16) 0.0361(18) -0.0024(14) -0.0107(14) 0.0021(13) C18 0.0167(12) 0.0242(14) 0.0267(15) 0.0023(11) -0.0038(11) -0.0012(11) C19 0.0235(14) 0.0248(15) 0.0306(16) 0.0024(12) 0.0014(12) 0.0002(12) C20 0.0271(15) 0.0233(15) 0.0439(19) 0.0051(13) 0.0007(13) 0.0026(12) C21 0.0260(15) 0.0330(17) 0.0397(19) 0.0143(14) -0.0019(13) -0.0012(13) C22 0.0230(14) 0.0386(18) 0.0255(15) 0.0066(13) -0.0022(12) -0.0023(13) C23 0.0200(13) 0.0278(15) 0.0263(15) -0.0012(12) -0.0024(11) -0.0007(11) C24 0.0239(14) 0.0203(14) 0.0223(14) -0.0008(11) 0.0020(11) -0.0036(11) C25 0.0301(15) 0.0210(14) 0.0234(15) 0.0000(11) 0.0010(12) -0.0005(12) C26 0.0264(14) 0.0228(14) 0.0185(13) 0.0011(11) 0.0012(11) 0.0015(11) C27 0.0211(13) 0.0252(14) 0.0178(13) 0.0015(11) 0.0011(10) 0.0004(11) C28 0.0222(14) 0.0264(15) 0.0223(14) 0.0020(11) 0.0019(11) 0.0008(11) C29 0.0221(14) 0.0339(17) 0.0273(16) 0.0045(13) 0.0023(12) 0.0018(12) C30 0.0228(14) 0.0368(18) 0.0299(16) 0.0062(13) 0.0018(12) 0.0096(13) C31 0.0314(16) 0.0259(15) 0.0279(16) 0.0030(12) 0.0035(12) 0.0076(13) C32 0.0230(14) 0.0311(16) 0.0265(15) 0.0043(12) 0.0007(11) 0.0000(12) C33 0.0318(17) 0.047(2) 0.0266(16) 0.0059(14) 0.0050(13) 0.0026(15) C34 0.0381(18) 0.046(2) 0.0339(19) 0.0178(16) 0.0052(15) -0.0011(16) C35 0.0358(17) 0.0344(18) 0.0326(18) 0.0124(14) 0.0006(14) -0.0036(14) C36 0.0232(13) 0.0233(14) 0.0184(13) -0.0009(11) 0.0006(10) 0.0021(11) C37 0.0252(15) 0.0266(15) 0.0254(15) -0.0035(12) 0.0011(11) 0.0007(12) C38 0.0257(15) 0.0419(19) 0.0298(17) -0.0028(14) -0.0022(12) 0.0047(14) C39 0.0375(18) 0.0397(19) 0.0339(18) 0.0047(15) -0.0045(14) 0.0148(15) C40 0.0443(19) 0.0258(16) 0.0367(18) 0.0085(14) 0.0022(15) 0.0066(14) C41 0.0286(15) 0.0245(15) 0.0269(15) 0.0009(12) 0.0015(12) -0.0004(12) C42 0.0213(13) 0.0214(14) 0.0271(15) -0.0035(11) 0.0032(11) -0.0018(11) C43 0.0245(14) 0.0313(16) 0.0287(16) -0.0058(13) 0.0012(12) 0.0000(12) C44 0.0335(17) 0.048(2) 0.0331(18) -0.0151(16) -0.0013(14) 0.0014(16) C45 0.0349(18) 0.0359(19) 0.048(2) -0.0234(16) 0.0084(15) -0.0018(15) C46 0.0330(17) 0.0273(17) 0.050(2) -0.0087(15) 0.0099(15) 0.0046(14) C47 0.0275(15) 0.0230(15) 0.0377(18) -0.0005(13) 0.0034(13) 0.0018(12) C48 0.0340(17) 0.0230(15) 0.0347(17) -0.0027(13) 0.0069(13) -0.0114(13) C49 0.0239(15) 0.0325(17) 0.0339(17) -0.0038(13) 0.0014(12) -0.0091(13) C50 0.0269(16) 0.042(2) 0.050(2) -0.0075(16) 0.0088(15) -0.0074(14) C51 0.0314(18) 0.043(2) 0.057(2) -0.0177(18) 0.0157(16) -0.0047(16) C52 0.0311(16) 0.0334(17) 0.0296(16) -0.0116(13) 0.0094(13) -0.0067(13) C53 0.0359(17) 0.0368(18) 0.0215(15) -0.0008(13) 0.0072(12) -0.0099(14) C54 0.046(2) 0.041(2) 0.0329(18) 0.0106(15) 0.0051(15) -0.0118(16) C55 0.0385(18) 0.0295(17) 0.049(2) 0.0111(15) 0.0059(16) -0.0080(15) Cl56 0.1630(18) 0.0674(10) 0.0869(11) 0.0179(8) 0.0032(11) -0.0032(11) Cl58 0.179(4) 0.0666(18) 0.0733(19) 0.0069(15) 0.046(2) 0.004(2) Cl60 0.121(3) 0.0626(18) 0.114(3) -0.0089(17) -0.026(2) 0.0015(18) Cl61 0.0854(10) 0.0765(10) 0.1320(15) 0.0004(10) 0.0295(10) 0.0110(8) C62 0.112(5) 0.094(5) 0.084(4) 0.006(4) 0.004(4) -0.016(4) Cl63 0.0960(12) 0.1401(18) 0.0958(13) 0.0095(12) 0.0029(10) -0.0040(12) Cl64 0.0769(8) 0.0408(6) 0.0830(9) 0.0150(6) 0.0239(6) 0.0041(5) C65 0.067(3) 0.048(3) 0.081(3) 0.028(2) 0.007(3) -0.004(2) Cl66 0.0579(7) 0.0646(8) 0.1041(11) 0.0265(7) 0.0029(7) 0.0039(6) O67 0.0252(10) 0.0268(11) 0.0302(11) 0.0095(9) 0.0020(8) 0.0017(9) C68 0.0242(14) 0.0239(14) 0.0242(15) 0.0048(11) 0.0018(11) -0.0022(12) C69 0.0326(16) 0.0315(16) 0.0229(15) 0.0068(12) 0.0028(12) -0.0040(13) C70 0.0321(16) 0.0349(17) 0.0249(15) 0.0019(13) 0.0052(12) -0.0065(14) C71 0.0263(15) 0.0269(15) 0.0266(15) 0.0004(12) 0.0024(12) -0.0038(12) C72 0.0240(14) 0.0224(14) 0.0252(15) 0.0003(11) -0.0007(11) -0.0052(11) C73 0.0218(13) 0.0235(14) 0.0232(15) 0.0026(11) 0.0007(11) -0.0058(11) C74 0.0262(14) 0.0196(14) 0.0241(15) 0.0035(11) 0.0010(11) 0.0005(11) C75 0.0315(15) 0.0185(13) 0.0231(15) 0.0025(11) -0.0013(12) 0.0017(12) C76 0.0311(16) 0.0240(15) 0.0283(16) 0.0009(12) -0.0011(12) 0.0000(12) C77 0.0369(18) 0.0301(17) 0.042(2) -0.0030(15) -0.0071(15) 0.0013(14) C78 0.053(2) 0.0360(19) 0.0357(19) -0.0088(15) -0.0157(16) 0.0075(17) C79 0.054(2) 0.0364(19) 0.0277(18) -0.0054(14) -0.0021(15) 0.0112(17) C80 0.0413(18) 0.0254(16) 0.0252(16) 0.0002(12) -0.0001(13) 0.0064(14) C81 0.0438(19) 0.0351(18) 0.0255(16) 0.0019(13) 0.0105(14) 0.0077(15) C82 0.0320(16) 0.0318(17) 0.0318(17) 0.0071(13) 0.0097(13) 0.0020(13) C83 0.0286(15) 0.0223(14) 0.0260(15) 0.0067(12) 0.0022(12) -0.0010(12) O84 0.0260(11) 0.0334(12) 0.0297(12) 0.0099(9) -0.0007(9) -0.0066(9) B85 0.0232(16) 0.0283(17) 0.0263(17) 0.0028(14) 0.0006(13) 0.0006(13) O86 0.0267(11) 0.0257(11) 0.0294(11) 0.0010(9) -0.0033(9) 0.0044(9) C87 0.0268(15) 0.0212(14) 0.0272(15) 0.0002(12) 0.0002(12) -0.0010(12) C88 0.0262(14) 0.0206(14) 0.0232(14) -0.0013(11) 0.0010(11) 0.0000(11) C89 0.0248(14) 0.0221(14) 0.0245(15) 0.0019(11) 0.0001(11) 0.0033(11) C90 0.0262(14) 0.0234(14) 0.0249(15) 0.0046(12) 0.0008(11) 0.0052(12) C91 0.0274(15) 0.0289(16) 0.0262(16) 0.0034(12) 0.0004(12) 0.0040(12) C92 0.0252(15) 0.0344(18) 0.0384(18) 0.0048(14) -0.0040(13) 0.0021(13) C93 0.0216(15) 0.0378(18) 0.043(2) 0.0090(15) 0.0035(13) 0.0053(13) C94 0.0286(16) 0.0347(18) 0.0342(18) 0.0037(14) 0.0062(13) 0.0100(14) C95 0.0267(15) 0.0288(16) 0.0298(16) 0.0024(13) 0.0032(12) 0.0070(12) C96 0.0362(17) 0.045(2) 0.0258(16) -0.0069(14) 0.0057(13) 0.0053(15) C97 0.0330(17) 0.0403(19) 0.0282(17) -0.0077(14) -0.0006(13) 0.0001(14) C98 0.0246(14) 0.0247(15) 0.0286(16) 0.0018(12) 0.0020(12) 0.0018(12) O99 0.0256(10) 0.0283(11) 0.0287(11) -0.0012(9) -0.0001(8) 0.0007(9) C100 0.0257(14) 0.0225(14) 0.0244(15) -0.0015(11) 0.0020(11) 0.0001(12) C101 0.0282(15) 0.0279(15) 0.0239(15) 0.0011(12) 0.0023(12) 0.0030(12) C102 0.0303(16) 0.0318(17) 0.0308(17) 0.0039(13) -0.0007(13) 0.0056(13) C103 0.0360(17) 0.0402(19) 0.0255(16) 0.0040(14) -0.0031(13) 0.0022(15) C104 0.0365(18) 0.048(2) 0.0233(16) -0.0011(14) 0.0046(13) 0.0007(15) C105 0.0292(15) 0.0329(17) 0.0251(15) -0.0009(13) 0.0037(12) 0.0022(13) C106 0.0338(17) 0.0417(19) 0.0275(17) -0.0045(14) 0.0061(13) 0.0059(15) C107 0.0271(15) 0.0302(16) 0.0338(17) -0.0018(13) 0.0037(13) 0.0067(13) C108 0.0262(15) 0.0231(15) 0.0282(16) -0.0005(12) -0.0018(12) -0.0029(12) C109 0.0301(16) 0.0231(15) 0.0378(18) 0.0008(13) -0.0068(13) -0.0017(13) C110 0.0279(16) 0.0323(17) 0.045(2) -0.0072(15) 0.0010(14) 0.0036(14) C111 0.0295(16) 0.0339(18) 0.0372(18) -0.0055(14) 0.0075(14) -0.0008(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.19184(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 Rh1 . P2 . 2.3369(7) yes Rh1 . P11 . 2.3071(8) yes Rh1 . C48 . 2.215(3) yes Rh1 . C49 . 2.263(3) yes Rh1 . C52 . 2.228(3) yes Rh1 . C53 . 2.238(3) yes P2 . C3 . 1.850(3) yes P2 . C36 . 1.826(3) yes P2 . C42 . 1.838(3) yes C3 . C4 . 1.422(4) yes C3 . C8 . 1.382(4) yes C4 . C5 . 1.368(4) yes C4 . H41 . 0.935 no C5 . C6 . 1.411(5) yes C5 . H51 . 0.938 no C6 . C7 . 1.415(4) yes C6 . C35 . 1.418(4) yes C7 . C8 . 1.432(4) yes C7 . C32 . 1.425(4) yes C8 . C9 . 1.499(4) yes C9 . C10 . 1.384(4) yes C9 . C27 . 1.444(4) yes C10 . P11 . 1.826(3) yes C10 . C24 . 1.429(4) yes P11 . C12 . 1.839(3) yes P11 . C18 . 1.830(3) yes C12 . C13 . 1.405(4) yes C12 . C17 . 1.391(5) yes C13 . C14 . 1.388(5) yes C13 . H131 . 0.928 no C14 . C15 . 1.386(6) yes C14 . H141 . 0.935 no C15 . C16 . 1.375(5) yes C15 . H151 . 0.947 no C16 . C17 . 1.394(5) yes C16 . H161 . 0.935 no C17 . H171 . 0.946 no C18 . C19 . 1.387(4) yes C18 . C23 . 1.396(4) yes C19 . C20 . 1.396(4) yes C19 . H191 . 0.963 no C20 . C21 . 1.376(5) yes C20 . H201 . 0.934 no C21 . C22 . 1.392(5) yes C21 . H211 . 0.944 no C22 . C23 . 1.381(4) yes C22 . H221 . 0.917 no C23 . H231 . 0.926 no C24 . C25 . 1.362(4) yes C24 . H241 . 0.943 no C25 . C26 . 1.420(4) yes C25 . H251 . 0.933 no C26 . C27 . 1.422(4) yes C26 . C31 . 1.420(4) yes C27 . C28 . 1.418(4) yes C28 . C29 . 1.371(4) yes C28 . H281 . 0.935 no C29 . C30 . 1.412(5) yes C29 . H291 . 0.945 no C30 . C31 . 1.365(5) yes C30 . H301 . 0.944 no C31 . H311 . 0.937 no C32 . C33 . 1.369(4) yes C32 . H321 . 0.924 no C33 . C34 . 1.402(5) yes C33 . H331 . 0.925 no C34 . C35 . 1.364(5) yes C34 . H341 . 0.936 no C35 . H351 . 0.936 no C36 . C37 . 1.401(4) yes C36 . C41 . 1.394(4) yes C37 . C38 . 1.385(5) yes C37 . H371 . 0.938 no C38 . C39 . 1.385(5) yes C38 . H381 . 0.919 no C39 . C40 . 1.379(5) yes C39 . H391 . 0.927 no C40 . C41 . 1.386(4) yes C40 . H401 . 0.944 no C41 . H411 . 0.927 no C42 . C43 . 1.387(4) yes C42 . C47 . 1.403(4) yes C43 . C44 . 1.399(5) yes C43 . H431 . 0.938 no C44 . C45 . 1.378(5) yes C44 . H441 . 0.944 no C45 . C46 . 1.383(5) yes C45 . H451 . 0.945 no C46 . C47 . 1.384(5) yes C46 . H461 . 0.935 no C47 . H471 . 0.921 no C48 . C49 . 1.372(5) yes C48 . C55 . 1.504(5) yes C48 . H481 . 0.978 no C49 . C50 . 1.514(5) yes C49 . H491 . 0.962 no C50 . C51 . 1.522(5) yes C50 . H501 . 0.984 no C50 . H502 . 0.979 no C51 . C52 . 1.502(5) yes C51 . H511 . 0.967 no C51 . H512 . 0.970 no C52 . C53 . 1.375(5) yes C52 . H521 . 0.985 no C53 . C54 . 1.520(5) yes C53 . H531 . 0.984 no C54 . C55 . 1.536(5) yes C54 . H541 . 0.964 no C54 . H542 . 0.984 no C55 . H551 . 0.975 no C55 . H552 . 0.979 no Cl56 . C57 . 1.753(13) yes C57 . Cl58 . 1.710(12) yes C57 . H571 . 0.958 no C57 . H572 . 0.972 no C59 . Cl60 . 1.760(12) yes C59 . H591 . 0.977 no C59 . H592 . 0.974 no Cl61 . C62 . 1.749(7) yes C62 . Cl63 . 1.736(7) yes C62 . H622 . 0.974 no C62 . H621 . 0.977 no Cl64 . C65 . 1.740(5) yes C65 . Cl66 . 1.753(5) yes C65 . H652 . 0.962 no C65 . H651 . 0.962 no O67 . C68 . 1.357(4) yes O67 . B85 . 1.474(4) yes C68 . C69 . 1.424(4) yes C68 . C73 . 1.386(4) yes C69 . C70 . 1.357(5) yes C69 . H691 . 0.935 no C70 . C71 . 1.421(4) yes C70 . H701 . 0.929 no C71 . C72 . 1.429(4) yes C71 . C111 . 1.420(5) yes C72 . C73 . 1.434(4) yes C72 . C108 . 1.419(4) yes C73 . C74 . 1.489(4) yes C74 . C75 . 1.438(4) yes C74 . C83 . 1.388(4) yes C75 . C76 . 1.422(4) yes C75 . C80 . 1.426(4) yes C76 . C77 . 1.370(5) yes C76 . H761 . 0.941 no C77 . C78 . 1.413(5) yes C77 . H771 . 0.939 no C78 . C79 . 1.362(6) yes C78 . H781 . 0.955 no C79 . C80 . 1.417(5) yes C79 . H791 . 0.960 no C80 . C81 . 1.419(5) yes C81 . C82 . 1.361(5) yes C81 . H811 . 0.933 no C82 . C83 . 1.418(4) yes C82 . H821 . 0.938 no C83 . O84 . 1.356(4) yes O84 . B85 . 1.461(4) yes B85 . O86 . 1.465(4) yes B85 . O99 . 1.477(4) yes O86 . C87 . 1.352(4) yes C87 . C88 . 1.390(4) yes C87 . C107 . 1.411(4) yes C88 . C89 . 1.489(4) yes C88 . C100 . 1.441(4) yes C89 . C90 . 1.436(4) yes C89 . C98 . 1.384(4) yes C90 . C91 . 1.417(4) yes C90 . C95 . 1.434(4) yes C91 . C92 . 1.376(4) yes C91 . H911 . 0.946 no C92 . C93 . 1.408(5) yes C92 . H921 . 0.967 no C93 . C94 . 1.360(5) yes C93 . H931 . 0.945 no C94 . C95 . 1.417(4) yes C94 . H941 . 0.947 no C95 . C96 . 1.417(5) yes C96 . C97 . 1.362(5) yes C96 . H961 . 0.924 no C97 . C98 . 1.423(4) yes C97 . H971 . 0.929 no C98 . O99 . 1.359(4) yes C100 . C101 . 1.421(4) yes C100 . C105 . 1.427(4) yes C101 . C102 . 1.373(4) yes C101 . H1011 . 0.936 no C102 . C103 . 1.406(5) yes C102 . H1021 . 0.927 no C103 . C104 . 1.359(5) yes C103 . H1031 . 0.931 no C104 . C105 . 1.429(5) yes C104 . H1041 . 0.939 no C105 . C106 . 1.411(5) yes C106 . C107 . 1.369(5) yes C106 . H1061 . 0.942 no C107 . H1071 . 0.940 no C108 . C109 . 1.363(4) yes C108 . H1081 . 0.945 no C109 . C110 . 1.411(5) yes C109 . H1091 . 0.942 no C110 . C111 . 1.367(5) yes C110 . H1101 . 0.929 no C111 . H1111 . 0.916 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 P2 . Rh1 . P11 . 88.87(3) yes P2 . Rh1 . C48 . 146.31(9) yes P11 . Rh1 . C48 . 92.37(9) yes P2 . Rh1 . C49 . 173.51(9) yes P11 . Rh1 . C49 . 97.37(9) yes C48 . Rh1 . C49 . 35.67(12) yes P2 . Rh1 . C52 . 94.66(8) yes P11 . Rh1 . C52 . 161.38(10) yes C48 . Rh1 . C52 . 94.72(12) yes C49 . Rh1 . C52 . 78.86(12) yes P2 . Rh1 . C53 . 88.14(9) yes P11 . Rh1 . C53 . 162.75(9) yes C48 . Rh1 . C53 . 80.87(12) yes C49 . Rh1 . C53 . 86.41(12) yes C52 . Rh1 . C53 . 35.87(13) yes Rh1 . P2 . C3 . 120.27(9) yes Rh1 . P2 . C36 . 110.60(10) yes C3 . P2 . C36 . 103.14(13) yes Rh1 . P2 . C42 . 113.54(9) yes C3 . P2 . C42 . 103.81(13) yes C36 . P2 . C42 . 103.78(13) yes P2 . C3 . C4 . 120.1(2) yes P2 . C3 . C8 . 120.2(2) yes C4 . C3 . C8 . 119.4(3) yes C3 . C4 . C5 . 120.9(3) yes C3 . C4 . H41 . 120.0 no C5 . C4 . H41 . 119.1 no C4 . C5 . C6 . 121.0(3) yes C4 . C5 . H51 . 118.3 no C6 . C5 . H51 . 120.7 no C5 . C6 . C7 . 119.0(3) yes C5 . C6 . C35 . 121.6(3) yes C7 . C6 . C35 . 119.5(3) yes C6 . C7 . C8 . 119.5(3) yes C6 . C7 . C32 . 118.4(3) yes C8 . C7 . C32 . 122.0(3) yes C7 . C8 . C3 . 120.2(3) yes C7 . C8 . C9 . 118.9(3) yes C3 . C8 . C9 . 120.9(3) yes C8 . C9 . C10 . 122.0(2) yes C8 . C9 . C27 . 118.1(2) yes C10 . C9 . C27 . 119.8(3) yes C9 . C10 . P11 . 122.5(2) yes C9 . C10 . C24 . 119.9(3) yes P11 . C10 . C24 . 116.6(2) yes C10 . P11 . Rh1 . 103.27(9) yes C10 . P11 . C12 . 105.32(13) yes Rh1 . P11 . C12 . 122.99(10) yes C10 . P11 . C18 . 110.56(13) yes Rh1 . P11 . C18 . 116.73(10) yes C12 . P11 . C18 . 97.45(13) yes P11 . C12 . C13 . 116.6(2) yes P11 . C12 . C17 . 124.2(2) yes C13 . C12 . C17 . 118.6(3) yes C12 . C13 . C14 . 120.5(3) yes C12 . C13 . H131 . 121.0 no C14 . C13 . H131 . 118.5 no C13 . C14 . C15 . 120.0(3) yes C13 . C14 . H141 . 118.9 no C15 . C14 . H141 . 121.1 no C14 . C15 . C16 . 120.0(3) yes C14 . C15 . H151 . 119.5 no C16 . C15 . H151 . 120.5 no C15 . C16 . C17 . 120.4(4) yes C15 . C16 . H161 . 121.1 no C17 . C16 . H161 . 118.5 no C16 . C17 . C12 . 120.4(3) yes C16 . C17 . H171 . 120.8 no C12 . C17 . H171 . 118.9 no P11 . C18 . C19 . 119.7(2) yes P11 . C18 . C23 . 120.5(2) yes C19 . C18 . C23 . 119.5(3) yes C18 . C19 . C20 . 119.9(3) yes C18 . C19 . H191 . 119.6 no C20 . C19 . H191 . 120.5 no C19 . C20 . C21 . 120.3(3) yes C19 . C20 . H201 . 119.2 no C21 . C20 . H201 . 120.5 no C20 . C21 . C22 . 120.0(3) yes C20 . C21 . H211 . 120.8 no C22 . C21 . H211 . 119.2 no C21 . C22 . C23 . 120.0(3) yes C21 . C22 . H221 . 121.2 no C23 . C22 . H221 . 118.8 no C18 . C23 . C22 . 120.3(3) yes C18 . C23 . H231 . 120.6 no C22 . C23 . H231 . 119.1 no C10 . C24 . C25 . 120.8(3) yes C10 . C24 . H241 . 118.8 no C25 . C24 . H241 . 120.5 no C24 . C25 . C26 . 121.0(3) yes C24 . C25 . H251 . 120.1 no C26 . C25 . H251 . 119.0 no C25 . C26 . C27 . 119.2(3) yes C25 . C26 . C31 . 121.9(3) yes C27 . C26 . C31 . 118.9(3) yes C9 . C27 . C26 . 119.2(3) yes C9 . C27 . C28 . 122.2(3) yes C26 . C27 . C28 . 118.6(3) yes C27 . C28 . C29 . 121.0(3) yes C27 . C28 . H281 . 120.0 no C29 . C28 . H281 . 119.0 no C28 . C29 . C30 . 120.2(3) yes C28 . C29 . H291 . 119.3 no C30 . C29 . H291 . 120.5 no C29 . C30 . C31 . 120.2(3) yes C29 . C30 . H301 . 119.7 no C31 . C30 . H301 . 120.1 no C26 . C31 . C30 . 121.0(3) yes C26 . C31 . H311 . 119.9 no C30 . C31 . H311 . 119.1 no C7 . C32 . C33 . 120.3(3) yes C7 . C32 . H321 . 119.2 no C33 . C32 . H321 . 120.5 no C32 . C33 . C34 . 121.1(3) yes C32 . C33 . H331 . 119.2 no C34 . C33 . H331 . 119.7 no C33 . C34 . C35 . 120.0(3) yes C33 . C34 . H341 . 120.3 no C35 . C34 . H341 . 119.6 no C6 . C35 . C34 . 120.7(3) yes C6 . C35 . H351 . 119.4 no C34 . C35 . H351 . 119.9 no P2 . C36 . C37 . 120.1(2) yes P2 . C36 . C41 . 120.6(2) yes C37 . C36 . C41 . 119.2(3) yes C36 . C37 . C38 . 119.9(3) yes C36 . C37 . H371 . 121.4 no C38 . C37 . H371 . 118.7 no C37 . C38 . C39 . 120.2(3) yes C37 . C38 . H381 . 120.4 no C39 . C38 . H381 . 119.4 no C38 . C39 . C40 . 120.2(3) yes C38 . C39 . H391 . 119.2 no C40 . C39 . H391 . 120.6 no C39 . C40 . C41 . 120.3(3) yes C39 . C40 . H401 . 119.3 no C41 . C40 . H401 . 120.4 no C36 . C41 . C40 . 120.2(3) yes C36 . C41 . H411 . 120.4 no C40 . C41 . H411 . 119.4 no P2 . C42 . C43 . 122.6(2) yes P2 . C42 . C47 . 119.0(2) yes C43 . C42 . C47 . 118.4(3) yes C42 . C43 . C44 . 120.5(3) yes C42 . C43 . H431 . 118.9 no C44 . C43 . H431 . 120.5 no C43 . C44 . C45 . 120.2(3) yes C43 . C44 . H441 . 120.3 no C45 . C44 . H441 . 119.5 no C44 . C45 . C46 . 119.9(3) yes C44 . C45 . H451 . 118.8 no C46 . C45 . H451 . 121.3 no C45 . C46 . C47 . 120.1(3) yes C45 . C46 . H461 . 118.6 no C47 . C46 . H461 . 121.2 no C42 . C47 . C46 . 120.8(3) yes C42 . C47 . H471 . 119.8 no C46 . C47 . H471 . 119.5 no Rh1 . C48 . C49 . 74.08(18) yes Rh1 . C48 . C55 . 107.1(2) yes C49 . C48 . C55 . 126.2(3) yes Rh1 . C48 . H481 . 111.2 no C49 . C48 . H481 . 115.2 no C55 . C48 . H481 . 113.8 no Rh1 . C49 . C48 . 70.24(17) yes Rh1 . C49 . C50 . 112.3(2) yes C48 . C49 . C50 . 125.1(3) yes Rh1 . C49 . H491 . 110.0 no C48 . C49 . H491 . 115.4 no C50 . C49 . H491 . 114.2 no C49 . C50 . C51 . 112.1(3) yes C49 . C50 . H501 . 109.2 no C51 . C50 . H501 . 109.7 no C49 . C50 . H502 . 108.9 no C51 . C50 . H502 . 108.4 no H501 . C50 . H502 . 108.4 no C50 . C51 . C52 . 114.1(3) yes C50 . C51 . H511 . 107.9 no C52 . C51 . H511 . 107.4 no C50 . C51 . H512 . 110.4 no C52 . C51 . H512 . 108.4 no H511 . C51 . H512 . 108.4 no C51 . C52 . Rh1 . 108.3(2) yes C51 . C52 . C53 . 127.4(3) yes Rh1 . C52 . C53 . 72.47(18) yes C51 . C52 . H521 . 113.3 no Rh1 . C52 . H521 . 106.9 no C53 . C52 . H521 . 116.4 no Rh1 . C53 . C52 . 71.66(19) yes Rh1 . C53 . C54 . 110.4(2) yes C52 . C53 . C54 . 126.2(3) yes Rh1 . C53 . H531 . 110.6 no C52 . C53 . H531 . 115.8 no C54 . C53 . H531 . 113.0 no C53 . C54 . C55 . 114.4(3) yes C53 . C54 . H541 . 107.6 no C55 . C54 . H541 . 107.7 no C53 . C54 . H542 . 108.5 no C55 . C54 . H542 . 108.4 no H541 . C54 . H542 . 110.1 no C54 . C55 . C48 . 114.5(3) yes C54 . C55 . H551 . 108.1 no C48 . C55 . H551 . 108.9 no C54 . C55 . H552 . 108.6 no C48 . C55 . H552 . 107.5 no H551 . C55 . H552 . 109.0 no Cl56 . C57 . Cl58 . 109.2(7) yes Cl56 . C57 . H571 . 108.7 no Cl58 . C57 . H571 . 110.0 no Cl56 . C57 . H572 . 110.0 no Cl58 . C57 . H572 . 109.3 no H571 . C57 . H572 . 109.5 no Cl56 . C59 . Cl60 . 107.8(7) yes Cl56 . C59 . H591 . 109.2 no Cl60 . C59 . H591 . 109.3 no Cl56 . C59 . H592 . 110.4 no Cl60 . C59 . H592 . 109.8 no H591 . C59 . H592 . 110.2 no Cl61 . C62 . Cl63 . 113.0(4) yes Cl61 . C62 . H622 . 108.3 no Cl63 . C62 . H622 . 109.5 no Cl61 . C62 . H621 . 108.0 no Cl63 . C62 . H621 . 106.3 no H622 . C62 . H621 . 111.7 no Cl64 . C65 . Cl66 . 112.8(2) yes Cl64 . C65 . H652 . 110.0 no Cl66 . C65 . H652 . 107.5 no Cl64 . C65 . H651 . 107.7 no Cl66 . C65 . H651 . 109.5 no H652 . C65 . H651 . 109.4 no C68 . O67 . B85 . 117.3(2) yes O67 . C68 . C69 . 117.2(3) yes O67 . C68 . C73 . 121.7(3) yes C69 . C68 . C73 . 120.9(3) yes C68 . C69 . C70 . 120.6(3) yes C68 . C69 . H691 . 118.4 no C70 . C69 . H691 . 121.0 no C69 . C70 . C71 . 120.6(3) yes C69 . C70 . H701 . 119.7 no C71 . C70 . H701 . 119.7 no C70 . C71 . C72 . 118.9(3) yes C70 . C71 . C111 . 121.8(3) yes C72 . C71 . C111 . 119.2(3) yes C71 . C72 . C73 . 119.8(3) yes C71 . C72 . C108 . 117.8(3) yes C73 . C72 . C108 . 122.3(3) yes C72 . C73 . C68 . 118.1(3) yes C72 . C73 . C74 . 122.5(3) yes C68 . C73 . C74 . 119.3(3) yes C73 . C74 . C75 . 121.7(3) yes C73 . C74 . C83 . 119.9(3) yes C75 . C74 . C83 . 118.4(3) yes C74 . C75 . C76 . 123.0(3) yes C74 . C75 . C80 . 119.9(3) yes C76 . C75 . C80 . 117.0(3) yes C75 . C76 . C77 . 121.6(3) yes C75 . C76 . H761 . 118.5 no C77 . C76 . H761 . 119.9 no C76 . C77 . C78 . 120.7(3) yes C76 . C77 . H771 . 119.2 no C78 . C77 . H771 . 120.1 no C77 . C78 . C79 . 119.5(3) yes C77 . C78 . H781 . 121.2 no C79 . C78 . H781 . 119.4 no C78 . C79 . C80 . 121.1(3) yes C78 . C79 . H791 . 118.4 no C80 . C79 . H791 . 120.5 no C75 . C80 . C79 . 120.0(3) yes C75 . C80 . C81 . 118.9(3) yes C79 . C80 . C81 . 121.1(3) yes C80 . C81 . C82 . 120.7(3) yes C80 . C81 . H811 . 119.7 no C82 . C81 . H811 . 119.6 no C81 . C82 . C83 . 120.8(3) yes C81 . C82 . H821 . 120.0 no C83 . C82 . H821 . 119.2 no C82 . C83 . C74 . 121.0(3) yes C82 . C83 . O84 . 116.7(3) yes C74 . C83 . O84 . 122.2(3) yes C83 . O84 . B85 . 120.8(2) yes O67 . B85 . O84 . 113.4(3) yes O67 . B85 . O86 . 114.4(3) yes O84 . B85 . O86 . 101.9(3) yes O67 . B85 . O99 . 100.9(2) yes O84 . B85 . O99 . 114.1(3) yes O86 . B85 . O99 . 112.8(3) yes B85 . O86 . C87 . 120.0(2) yes O86 . C87 . C88 . 121.6(3) yes O86 . C87 . C107 . 117.2(3) yes C88 . C87 . C107 . 121.2(3) yes C87 . C88 . C89 . 119.8(3) yes C87 . C88 . C100 . 118.3(3) yes C89 . C88 . C100 . 121.8(3) yes C88 . C89 . C90 . 122.5(3) yes C88 . C89 . C98 . 119.3(3) yes C90 . C89 . C98 . 118.2(3) yes C89 . C90 . C91 . 122.8(3) yes C89 . C90 . C95 . 119.6(3) yes C91 . C90 . C95 . 117.5(3) yes C90 . C91 . C92 . 121.5(3) yes C90 . C91 . H911 . 118.4 no C92 . C91 . H911 . 120.1 no C91 . C92 . C93 . 120.4(3) yes C91 . C92 . H921 . 120.0 no C93 . C92 . H921 . 119.5 no C92 . C93 . C94 . 119.8(3) yes C92 . C93 . H931 . 120.5 no C94 . C93 . H931 . 119.7 no C93 . C94 . C95 . 121.4(3) yes C93 . C94 . H941 . 119.5 no C95 . C94 . H941 . 119.1 no C90 . C95 . C94 . 119.3(3) yes C90 . C95 . C96 . 119.1(3) yes C94 . C95 . C96 . 121.6(3) yes C95 . C96 . C97 . 120.7(3) yes C95 . C96 . H961 . 117.6 no C97 . C96 . H961 . 121.7 no C96 . C97 . C98 . 120.4(3) yes C96 . C97 . H971 . 121.3 no C98 . C97 . H971 . 118.3 no C97 . C98 . C89 . 121.4(3) yes C97 . C98 . O99 . 116.5(3) yes C89 . C98 . O99 . 122.1(3) yes C98 . O99 . B85 . 118.6(2) yes C88 . C100 . C101 . 123.3(3) yes C88 . C100 . C105 . 119.4(3) yes C101 . C100 . C105 . 117.2(3) yes C100 . C101 . C102 . 121.6(3) yes C100 . C101 . H1011 . 119.9 no C102 . C101 . H1011 . 118.5 no C101 . C102 . C103 . 120.8(3) yes C101 . C102 . H1021 . 119.9 no C103 . C102 . H1021 . 119.3 no C102 . C103 . C104 . 119.5(3) yes C102 . C103 . H1031 . 119.3 no C104 . C103 . H1031 . 121.2 no C103 . C104 . C105 . 121.4(3) yes C103 . C104 . H1041 . 118.1 no C105 . C104 . H1041 . 120.5 no C104 . C105 . C100 . 119.3(3) yes C104 . C105 . C106 . 121.0(3) yes C100 . C105 . C106 . 119.6(3) yes C105 . C106 . C107 . 120.3(3) yes C105 . C106 . H1061 . 119.4 no C107 . C106 . H1061 . 120.3 no C87 . C107 . C106 . 120.9(3) yes C87 . C107 . H1071 . 119.5 no C106 . C107 . H1071 . 119.6 no C72 . C108 . C109 . 121.3(3) yes C72 . C108 . H1081 . 120.1 no C109 . C108 . H1081 . 118.6 no C108 . C109 . C110 . 121.1(3) yes C108 . C109 . H1091 . 120.0 no C110 . C109 . H1091 . 118.9 no C109 . C110 . C111 . 119.3(3) yes C109 . C110 . H1101 . 122.5 no C111 . C110 . H1101 . 118.2 no C71 . C111 . C110 . 121.3(3) yes C71 . C111 . H1111 . 119.0 no C110 . C111 . H1111 . 119.7 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 C4 . H41 . C47 . 136 0.94 2.45 3.189(5) yes C17 . H171 . C24 . 124 0.95 2.49 3.122(5) yes C43 . H431 . C37 . 126 0.94 2.55 3.193(5) yes C52 . H521 . C47 . 150 0.98 2.52 3.408(5) yes C65 . H652 . O67 . 132 0.96 2.51 3.230(5) yes C65 . H652 . O99 . 137 0.96 2.48 3.255(5) yes _database_code_depnum_ccdc_archive 'CCDC 934111' ####################################################################### # # 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_arc1636 #TrackingRef '19475_web_deposit_cif_file_1_JohnBrown_1366025934.arc1636a.cif' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _ccdc_journal_depnumber ? _chemical_name_systematic ; ((Bicyclo[2.2.1]hepta-2,5-diene)((R)-bis-2,2'-(diphenylphosphino)-1,1' -binaphthalene)rhodium)((S,S)-bis-(1,1'-binaphthalen-2,2'-dioxo)boronate). ; _chemical_melting_point ; Not determined ; _chemical_absolute_configuration ; rm ; _computing_structure_solution ; 'SIR92 (Giacovazzo et al, 1992)' ; _exptl_crystal_thermal_history ; The material was crystallised at ambient temperature. A suitable crystal was cooled rapidly to 150K for single-crystal X-ray diffraction analysis. ; _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_special_details ; Geometric restraints were applied to the disordered solvent. The C-Cl bond lengths were restrained to 1.77(2) \%A, the Cl-C-Cl angles to 112(2) \% and similarity restraints applied to the displacement parameters of directly-bonded pairs of atoms. The hydrogen atoms of the coordinated alkene groups were located in a difference Fourier map and their coordinates and isotropic displacement parameters subsequently refined, subject to restraint of the C-H bond lengths to 1.00(4) \%A and to a similarity restraint between their displacement parameters and those of the parent C atoms. Other hydrogen atoms were positioned geometrically after each cycle of refinement. ; #============================================================= _cell_length_a 15.7224(3) _cell_length_b 20.2138(4) _cell_length_c 25.7426(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8181.2(3) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 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 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' 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' O 0.0106 0.0060 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' 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' 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' _cell_formula_units_Z 4 _chemical_formula_sum 'C98 H80 B Cl6 O5 P2 Rh' _chemical_formula_moiety 'C51 H40 P2 Rh, C40 H24 B O4, C4 H10 O, 3(C H2 Cl2)' _chemical_compound_source 'synthesis as described' _chemical_formula_weight 1726.09 _cell_measurement_reflns_used 86469 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 3560 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.95 _diffrn_measurement_method \w _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 86469 _reflns_number_total 18392 #18424 unique reflections including absences _diffrn_reflns_av_R_equivalents 0.068 _diffrn_reflns_theta_min 5.091 _diffrn_reflns_theta_max 27.406 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.406 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _reflns_limit_h_min -20 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 33 _refine_diff_density_min -0.74 _refine_diff_density_max 0.95 _refine_ls_number_reflns 11955 _refine_ls_number_restraints 42 _refine_ls_number_parameters 1063 #_refine_ls_R_factor_ref 0.0550 _refine_ls_wR_factor_ref 0.0578 _refine_ls_goodness_of_fit_ref 1.0950 #_reflns_number_all 18392 _refine_ls_R_factor_all 0.1012 _refine_ls_wR_factor_all 0.1040 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 11955 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_gt 0.0578 _refine_ls_shift/su_max 0.013974 _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_abs_structure_details 'Flack, 8421 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.920 0.171 0.593 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 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 Rh1 Rh 0.34314(2) 0.581346(19) 0.438484(15) 0.0201 1.0000 Uani . . . . . C1 C 0.3764(4) 0.6641(3) 0.4905(2) 0.0270 1.0000 Uani D U . . . C2 C 0.4125(4) 0.6767(3) 0.4433(3) 0.0316 1.0000 Uani D U . . . C3 C 0.3480(4) 0.7178(3) 0.4124(2) 0.0317 1.0000 Uani . . . . . C4 C 0.2764(4) 0.6669(3) 0.4026(2) 0.0272 1.0000 Uani D U . . . C5 C 0.2401(3) 0.6538(3) 0.4490(2) 0.0253 1.0000 Uani D U . . . C6 C 0.2874(3) 0.6953(3) 0.4905(2) 0.0275 1.0000 Uani . . . . . C7 C 0.3065(4) 0.7585(3) 0.4571(2) 0.0293 1.0000 Uani . . . . . P1 P 0.24803(8) 0.49941(6) 0.41476(5) 0.0202 1.0000 Uani . . . . . P2 P 0.44140(8) 0.50396(7) 0.46449(5) 0.0211 1.0000 Uani . . . . . C8 C 0.2868(3) 0.4171(3) 0.39598(18) 0.0216 1.0000 Uani . . . . . C9 C 0.2799(4) 0.3945(3) 0.3436(2) 0.0262 1.0000 Uani . . . . . C10 C 0.3175(4) 0.3382(3) 0.3270(2) 0.0305 1.0000 Uani . . . . . C11 C 0.3663(3) 0.2991(3) 0.3620(2) 0.0278 1.0000 Uani . . . . . C12 C 0.4094(4) 0.2405(3) 0.3454(2) 0.0382 1.0000 Uani . . . . . C13 C 0.4548(4) 0.2044(3) 0.3795(3) 0.0394 1.0000 Uani . . . . . C14 C 0.4613(4) 0.2238(3) 0.4311(3) 0.0392 1.0000 Uani . . . . . C15 C 0.4209(4) 0.2791(3) 0.4496(2) 0.0313 1.0000 Uani . . . . . C16 C 0.3715(3) 0.3190(3) 0.4148(2) 0.0256 1.0000 Uani . . . . . C17 C 0.3310(3) 0.3781(2) 0.43182(19) 0.0217 1.0000 Uani . . . . . C18 C 0.3336(3) 0.3969(2) 0.48817(17) 0.0209 1.0000 Uani . . . . . C19 C 0.2802(3) 0.3600(3) 0.5236(2) 0.0246 1.0000 Uani . . . . . C20 C 0.2302(4) 0.3046(3) 0.5075(2) 0.0329 1.0000 Uani . . . . . C21 C 0.1803(4) 0.2712(3) 0.5421(2) 0.0375 1.0000 Uani . . . . . C22 C 0.1770(5) 0.2907(3) 0.5946(2) 0.0448 1.0000 Uani . . . . . C23 C 0.2225(4) 0.3420(3) 0.6110(2) 0.0398 1.0000 Uani . . . . . C24 C 0.2754(4) 0.3790(3) 0.5762(2) 0.0311 1.0000 Uani . . . . . C25 C 0.3215(4) 0.4354(3) 0.5926(2) 0.0358 1.0000 Uani . . . . . C26 C 0.3717(3) 0.4694(3) 0.5598(2) 0.0308 1.0000 Uani . . . . . C27 C 0.3819(3) 0.4494(3) 0.50677(19) 0.0240 1.0000 Uani . . . . . C28 C 0.1706(3) 0.4814(2) 0.4651(2) 0.0272 1.0000 Uani . . . . . C29 C 0.1750(4) 0.5118(3) 0.5135(2) 0.0319 1.0000 Uani . . . . . C30 C 0.1145(4) 0.4969(3) 0.5517(2) 0.0449 1.0000 Uani . . . . . C31 C 0.0511(5) 0.4526(4) 0.5414(3) 0.0519 1.0000 Uani . . . . . C32 C 0.0447(4) 0.4223(4) 0.4934(3) 0.0438 1.0000 Uani . . . . . C33 C 0.1062(4) 0.4348(3) 0.4552(2) 0.0339 1.0000 Uani . . . . . C34 C 0.1840(3) 0.5303(2) 0.36075(19) 0.0218 1.0000 Uani . . . . . C35 C 0.0994(3) 0.5501(3) 0.3675(2) 0.0310 1.0000 Uani . . . . . C36 C 0.0556(4) 0.5799(4) 0.3273(2) 0.0434 1.0000 Uani . . . . . C37 C 0.0946(4) 0.5917(4) 0.2792(2) 0.0404 1.0000 Uani . . . . . C38 C 0.1781(3) 0.5733(3) 0.2728(2) 0.0311 1.0000 Uani . . . . . C39 C 0.2230(3) 0.5442(3) 0.3134(2) 0.0249 1.0000 Uani . . . . . C40 C 0.4954(3) 0.4577(2) 0.4135(2) 0.0216 1.0000 Uani . . . . . C41 C 0.4796(3) 0.4741(3) 0.36162(19) 0.0252 1.0000 Uani . . . . . C42 C 0.5295(4) 0.4466(3) 0.3225(2) 0.0322 1.0000 Uani . . . . . C43 C 0.5953(4) 0.4048(3) 0.3344(2) 0.0371 1.0000 Uani . . . . . C44 C 0.6114(4) 0.3876(3) 0.3855(2) 0.0363 1.0000 Uani . . . . . C45 C 0.5617(3) 0.4137(3) 0.4255(2) 0.0295 1.0000 Uani . . . . . C46 C 0.5363(3) 0.5296(3) 0.5017(2) 0.0251 1.0000 Uani . . . . . C47 C 0.5860(3) 0.5778(3) 0.4775(2) 0.0293 1.0000 Uani . . . . . C48 C 0.6633(4) 0.5969(3) 0.4993(2) 0.0366 1.0000 Uani . . . . . C49 C 0.6909(4) 0.5690(3) 0.5452(2) 0.0402 1.0000 Uani . . . . . C50 C 0.6417(4) 0.5218(3) 0.5691(2) 0.0462 1.0000 Uani . . . . . C51 C 0.5648(4) 0.5014(3) 0.5472(2) 0.0352 1.0000 Uani . . . . . B1 B 0.2737(4) 0.6990(3) 0.6518(2) 0.0241 1.0000 Uani . . . . . O1 O 0.3258(2) 0.75667(19) 0.66872(14) 0.0297 1.0000 Uani . . . . . O2 O 0.3240(2) 0.65161(18) 0.62111(14) 0.0257 1.0000 Uani . . . . . O3 O 0.2431(2) 0.66938(18) 0.70074(13) 0.0244 1.0000 Uani . . . . . O4 O 0.2031(2) 0.71882(19) 0.61762(13) 0.0260 1.0000 Uani . . . . . C52 C 0.3743(3) 0.7844(3) 0.6300(2) 0.0245 1.0000 Uani . . . . . C53 C 0.3515(3) 0.8491(3) 0.6134(2) 0.0294 1.0000 Uani . . . . . C54 C 0.3952(3) 0.8776(2) 0.5728(2) 0.0301 1.0000 Uani . . . . . C55 C 0.4607(3) 0.8430(3) 0.54705(19) 0.0266 1.0000 Uani . . . . . C56 C 0.4984(3) 0.8678(3) 0.5009(2) 0.0315 1.0000 Uani . . . . . C57 C 0.5577(4) 0.8317(3) 0.4743(2) 0.0306 1.0000 Uani . . . . . C58 C 0.5823(3) 0.7693(3) 0.4927(2) 0.0322 1.0000 Uani . . . . . C59 C 0.5488(3) 0.7443(3) 0.5382(2) 0.0239 1.0000 Uani . . . . . C60 C 0.4859(3) 0.7796(2) 0.5665(2) 0.0245 1.0000 Uani . . . . . C61 C 0.4437(3) 0.7519(3) 0.6111(2) 0.0240 1.0000 Uani . . . . . C62 C 0.4677(3) 0.6875(3) 0.6333(2) 0.0241 1.0000 Uani . . . . . C63 C 0.5500(3) 0.6729(3) 0.6542(2) 0.0256 1.0000 Uani . . . . . C64 C 0.6157(4) 0.7223(3) 0.6564(2) 0.0294 1.0000 Uani . . . . . C65 C 0.6934(3) 0.7074(3) 0.6780(2) 0.0355 1.0000 Uani . . . . . C66 C 0.7097(4) 0.6440(4) 0.6985(2) 0.0418 1.0000 Uani . . . . . C67 C 0.6478(4) 0.5963(3) 0.6974(2) 0.0347 1.0000 Uani . . . . . C68 C 0.5673(4) 0.6104(3) 0.6763(2) 0.0289 1.0000 Uani . . . . . C69 C 0.5012(4) 0.5618(3) 0.6776(2) 0.0296 1.0000 Uani . . . . . C70 C 0.4211(3) 0.5768(3) 0.6595(2) 0.0277 1.0000 Uani . . . . . C71 C 0.4039(3) 0.6393(3) 0.6376(2) 0.0259 1.0000 Uani . . . . . C72 C 0.1795(3) 0.6237(3) 0.69576(18) 0.0214 1.0000 Uani . . . . . C73 C 0.1993(3) 0.5575(3) 0.70881(19) 0.0232 1.0000 Uani . . . . . C74 C 0.1379(3) 0.5091(3) 0.7051(2) 0.0273 1.0000 Uani . . . . . C75 C 0.0550(3) 0.5240(3) 0.68703(19) 0.0254 1.0000 Uani . . . . . C76 C -0.0076(4) 0.4740(3) 0.6818(2) 0.0316 1.0000 Uani . . . . . C77 C -0.0862(4) 0.4884(3) 0.6614(2) 0.0341 1.0000 Uani . . . . . C78 C -0.1036(4) 0.5533(3) 0.6461(2) 0.0366 1.0000 Uani . . . . . C79 C -0.0455(3) 0.6029(3) 0.6516(2) 0.0283 1.0000 Uani . . . . . C80 C 0.0364(3) 0.5908(3) 0.67335(18) 0.0226 1.0000 Uani . . . . . C81 C 0.0986(3) 0.6415(3) 0.68066(19) 0.0234 1.0000 Uani . . . . . C82 C 0.0813(3) 0.7132(3) 0.6725(2) 0.0234 1.0000 Uani . . . . . C83 C 0.0125(3) 0.7469(3) 0.6984(2) 0.0249 1.0000 Uani . . . . . C84 C -0.0423(3) 0.7161(3) 0.7346(2) 0.0259 1.0000 Uani . . . . . C85 C -0.1082(4) 0.7505(3) 0.7575(2) 0.0332 1.0000 Uani . . . . . C86 C -0.1214(4) 0.8173(3) 0.7458(2) 0.0344 1.0000 Uani . . . . . C87 C -0.0681(4) 0.8490(3) 0.7139(2) 0.0299 1.0000 Uani . . . . . C88 C 0.0015(3) 0.8163(3) 0.6899(2) 0.0263 1.0000 Uani . . . . . C89 C 0.0588(3) 0.8502(3) 0.6564(2) 0.0257 1.0000 Uani . . . . . C90 C 0.1245(3) 0.8173(3) 0.6339(2) 0.0292 1.0000 Uani . . . . . C91 C 0.1368(3) 0.7493(3) 0.64146(19) 0.0241 1.0000 Uani . . . . . C92 C -0.1498(15) 0.3931(11) 0.3345(7) 0.1930 1.0000 Uani . . . . . Cl1 Cl -0.1803(4) 0.3144(4) 0.3533(4) 0.2372 1.0000 Uani . . . . . Cl2 Cl -0.1169(6) 0.4404(4) 0.3829(4) 0.2740 1.0000 Uani . . . . . C93 C 0.0888(8) 0.3025(6) 0.2743(4) 0.0966 1.0000 Uani . . . . . Cl3 Cl 0.0085(3) 0.2450(2) 0.27584(17) 0.1549 1.0000 Uani . . . . . Cl4 Cl 0.0645(2) 0.3766(2) 0.30944(15) 0.1364 1.0000 Uani . . . . . C94 C 0.2848(13) 0.1211(8) 0.2473(7) 0.0794 0.496(10) Uani D U P 1 1 Cl5 Cl 0.2177(5) 0.1276(4) 0.2997(3) 0.1233 0.496(10) Uani D U P 1 1 Cl6 Cl 0.2747(5) 0.0460(2) 0.2123(2) 0.0684 0.496(10) Uani D U P 1 1 C95 C 0.2274(15) 0.1340(12) 0.2501(17) 0.1716 0.504(10) Uani D U P 1 2 Cl7 Cl 0.1268(5) 0.1052(5) 0.2703(4) 0.1515 0.504(10) Uani D U P 1 2 Cl8 Cl 0.2811(10) 0.0633(10) 0.2315(7) 0.1975 0.504(10) Uani D U P 1 2 O5 O 0.1585(6) 0.1588(4) 0.4488(3) 0.1039 1.0000 Uani . . . . . C96 C 0.2364(10) 0.1407(7) 0.4360(7) 0.1345 1.0000 Uani . . . . . C97 C 0.2816(10) 0.1086(7) 0.4870(7) 0.1267 1.0000 Uani . . . . . C98 C 0.1117(13) 0.1890(9) 0.4074(5) 0.1477 1.0000 Uani . . . . . C99 C 0.0230(11) 0.2086(10) 0.4203(6) 0.1686 1.0000 Uani . . . . . H11 H 0.402(3) 0.648(3) 0.5218(16) 0.025(5) 1.0000 Uiso D U . . . H21 H 0.469(2) 0.672(3) 0.433(2) 0.027(5) 1.0000 Uiso D U . . . H41 H 0.257(4) 0.656(3) 0.3661(15) 0.027(5) 1.0000 Uiso D U . . . H51 H 0.186(2) 0.631(2) 0.455(2) 0.020(5) 1.0000 Uiso D U . . . H31 H 0.3698 0.7430 0.3817 0.0381 1.0000 Uiso . . . . . H61 H 0.2588 0.7018 0.5248 0.0330 1.0000 Uiso . . . . . H71 H 0.3467 0.7900 0.4743 0.0352 1.0000 Uiso . . . . . H72 H 0.2540 0.7828 0.4462 0.0352 1.0000 Uiso . . . . . H91 H 0.2459 0.4212 0.3183 0.0315 1.0000 Uiso . . . . . H101 H 0.3110 0.3240 0.2900 0.0367 1.0000 Uiso . . . . . H121 H 0.4057 0.2262 0.3082 0.0459 1.0000 Uiso . . . . . H131 H 0.4841 0.1632 0.3676 0.0473 1.0000 Uiso . . . . . H141 H 0.4965 0.1967 0.4555 0.0470 1.0000 Uiso . . . . . H151 H 0.4259 0.2915 0.4871 0.0375 1.0000 Uiso . . . . . H201 H 0.2317 0.2901 0.4704 0.0394 1.0000 Uiso . . . . . H211 H 0.1458 0.2325 0.5301 0.0450 1.0000 Uiso . . . . . H221 H 0.1403 0.2658 0.6196 0.0537 1.0000 Uiso . . . . . H231 H 0.2197 0.3551 0.6484 0.0478 1.0000 Uiso . . . . . H251 H 0.3165 0.4504 0.6295 0.0430 1.0000 Uiso . . . . . H261 H 0.4026 0.5094 0.5726 0.0369 1.0000 Uiso . . . . . H291 H 0.2214 0.5443 0.5210 0.0383 1.0000 Uiso . . . . . H301 H 0.1177 0.5187 0.5865 0.0538 1.0000 Uiso . . . . . H311 H 0.0086 0.4419 0.5691 0.0623 1.0000 Uiso . . . . . H321 H -0.0036 0.3916 0.4859 0.0525 1.0000 Uiso . . . . . H331 H 0.1044 0.4108 0.4212 0.0406 1.0000 Uiso . . . . . H351 H 0.0705 0.5427 0.4016 0.0371 1.0000 Uiso . . . . . H361 H -0.0050 0.5932 0.3326 0.0520 1.0000 Uiso . . . . . H371 H 0.0623 0.6131 0.2502 0.0485 1.0000 Uiso . . . . . H381 H 0.2069 0.5809 0.2386 0.0373 1.0000 Uiso . . . . . H391 H 0.2844 0.5331 0.3085 0.0299 1.0000 Uiso . . . . . H411 H 0.4326 0.5054 0.3526 0.0303 1.0000 Uiso . . . . . H421 H 0.5173 0.4575 0.2854 0.0387 1.0000 Uiso . . . . . H431 H 0.6318 0.3866 0.3060 0.0445 1.0000 Uiso . . . . . H441 H 0.6589 0.3565 0.3938 0.0436 1.0000 Uiso . . . . . H451 H 0.5733 0.4011 0.4624 0.0354 1.0000 Uiso . . . . . H471 H 0.5662 0.5987 0.4444 0.0352 1.0000 Uiso . . . . . H481 H 0.6990 0.6310 0.4816 0.0439 1.0000 Uiso . . . . . H491 H 0.7462 0.5830 0.5610 0.0482 1.0000 Uiso . . . . . H501 H 0.6611 0.5018 0.6025 0.0554 1.0000 Uiso . . . . . H511 H 0.5303 0.4663 0.5646 0.0423 1.0000 Uiso . . . . . H531 H 0.3043 0.8735 0.6309 0.0352 1.0000 Uiso . . . . . H541 H 0.3802 0.9235 0.5615 0.0361 1.0000 Uiso . . . . . H561 H 0.4813 0.9124 0.4876 0.0378 1.0000 Uiso . . . . . H571 H 0.5836 0.8498 0.4418 0.0367 1.0000 Uiso . . . . . H581 H 0.6245 0.7425 0.4726 0.0387 1.0000 Uiso . . . . . H591 H 0.5691 0.7006 0.5515 0.0287 1.0000 Uiso . . . . . H641 H 0.6049 0.7676 0.6422 0.0352 1.0000 Uiso . . . . . H651 H 0.7388 0.7420 0.6792 0.0425 1.0000 Uiso . . . . . H661 H 0.7667 0.6338 0.7138 0.0502 1.0000 Uiso . . . . . H671 H 0.6599 0.5513 0.7117 0.0417 1.0000 Uiso . . . . . H691 H 0.5132 0.5167 0.6918 0.0355 1.0000 Uiso . . . . . H701 H 0.3748 0.5430 0.6619 0.0332 1.0000 Uiso . . . . . H731 H 0.2579 0.5458 0.7208 0.0279 1.0000 Uiso . . . . . H741 H 0.1521 0.4627 0.7153 0.0328 1.0000 Uiso . . . . . H761 H 0.0055 0.4278 0.6930 0.0379 1.0000 Uiso . . . . . H771 H -0.1302 0.4530 0.6576 0.0409 1.0000 Uiso . . . . . H781 H -0.1605 0.5637 0.6307 0.0440 1.0000 Uiso . . . . . H791 H -0.0607 0.6486 0.6400 0.0339 1.0000 Uiso . . . . . H841 H -0.0332 0.6686 0.7437 0.0310 1.0000 Uiso . . . . . H851 H -0.1467 0.7275 0.7826 0.0399 1.0000 Uiso . . . . . H861 H -0.1708 0.8414 0.7614 0.0412 1.0000 Uiso . . . . . H871 H -0.0776 0.8971 0.7067 0.0359 1.0000 Uiso . . . . . H891 H 0.0505 0.8984 0.6493 0.0309 1.0000 Uiso . . . . . H901 H 0.1652 0.8422 0.6113 0.0350 1.0000 Uiso . . . . . H921 H -0.1997 0.4151 0.3176 0.2316 1.0000 Uiso . . . . . H922 H -0.1025 0.3889 0.3087 0.2316 1.0000 Uiso . . . . . H931 H 0.1409 0.2822 0.2898 0.1159 1.0000 Uiso . . . . . H932 H 0.1001 0.3145 0.2373 0.1159 1.0000 Uiso . . . . . H941 H 0.3447 0.1247 0.2601 0.0953 0.4957 Uiso . . . 1 1 H942 H 0.2726 0.1585 0.2230 0.0953 0.4957 Uiso . . . 1 1 H951 H 0.2576 0.1566 0.2793 0.2059 0.5043 Uiso . . . 1 2 H952 H 0.2216 0.1652 0.2202 0.2059 0.5043 Uiso . . . 1 2 H961 H 0.2695 0.1801 0.4240 0.1613 1.0000 Uiso . . . . . H962 H 0.2341 0.1071 0.4075 0.1613 1.0000 Uiso . . . . . H971 H 0.3408 0.0945 0.4781 0.1521 1.0000 Uiso . . . . . H972 H 0.2836 0.1423 0.5155 0.1521 1.0000 Uiso . . . . . H973 H 0.2482 0.0693 0.4989 0.1521 1.0000 Uiso . . . . . H981 H 0.1432 0.2296 0.3963 0.1772 1.0000 Uiso . . . . . H982 H 0.1095 0.1569 0.3778 0.1772 1.0000 Uiso . . . . . H991 H -0.0043 0.2291 0.3891 0.2023 1.0000 Uiso . . . . . H992 H 0.0237 0.2413 0.4494 0.2023 1.0000 Uiso . . . . . H993 H -0.0100 0.1686 0.4310 0.2023 1.0000 Uiso . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01997(16) 0.01813(16) 0.02209(17) -0.00137(17) -0.00105(17) -0.00012(17) C1 0.030(3) 0.023(3) 0.029(3) -0.003(2) -0.007(2) -0.001(2) C2 0.027(3) 0.025(3) 0.043(3) -0.003(3) 0.003(3) 0.000(2) C3 0.033(3) 0.026(3) 0.036(3) -0.004(2) 0.005(3) -0.002(3) C4 0.031(3) 0.021(3) 0.030(3) -0.004(2) -0.004(2) 0.004(2) C5 0.021(2) 0.023(3) 0.032(3) 0.000(2) -0.002(2) -0.002(2) C6 0.026(3) 0.031(3) 0.025(3) -0.009(2) 0.002(2) 0.003(2) C7 0.028(3) 0.020(3) 0.039(3) -0.007(2) -0.005(2) 0.006(2) P1 0.0221(6) 0.0182(6) 0.0203(6) -0.0008(5) 0.0011(5) -0.0002(5) P2 0.0230(6) 0.0218(7) 0.0185(6) -0.0002(5) -0.0015(5) 0.0000(5) C8 0.021(2) 0.019(2) 0.025(2) 0.003(2) 0.0019(18) -0.003(2) C9 0.031(3) 0.020(2) 0.028(3) 0.000(2) -0.006(2) -0.001(2) C10 0.044(3) 0.024(3) 0.024(3) -0.005(2) -0.001(2) -0.003(2) C11 0.027(3) 0.022(3) 0.034(3) -0.001(2) 0.005(2) -0.002(2) C12 0.048(4) 0.027(3) 0.039(3) -0.002(3) 0.008(3) 0.006(3) C13 0.047(4) 0.023(3) 0.048(4) 0.001(3) 0.001(3) 0.004(3) C14 0.045(3) 0.028(3) 0.045(4) 0.002(3) -0.001(3) 0.012(3) C15 0.034(3) 0.029(3) 0.031(3) 0.000(2) -0.005(2) 0.001(2) C16 0.029(3) 0.022(3) 0.026(3) 0.003(2) -0.001(2) -0.006(2) C17 0.021(2) 0.016(2) 0.028(3) -0.0024(19) 0.000(2) -0.0008(19) C18 0.028(3) 0.019(2) 0.016(2) 0.0010(16) -0.002(2) -0.001(2) C19 0.026(3) 0.022(3) 0.026(3) 0.006(2) -0.001(2) -0.005(2) C20 0.036(3) 0.031(3) 0.032(3) 0.000(2) -0.002(2) -0.003(3) C21 0.040(3) 0.032(3) 0.041(3) 0.001(2) 0.001(3) -0.010(3) C22 0.062(5) 0.042(4) 0.030(3) 0.006(3) 0.010(3) -0.003(3) C23 0.055(4) 0.043(4) 0.022(3) 0.001(3) -0.001(3) -0.011(3) C24 0.040(3) 0.031(3) 0.022(3) 0.001(2) 0.004(2) -0.002(3) C25 0.053(4) 0.037(3) 0.017(2) -0.002(2) 0.003(2) -0.013(3) C26 0.041(3) 0.028(3) 0.023(2) -0.005(2) -0.003(3) -0.011(2) C27 0.032(3) 0.024(3) 0.016(2) 0.004(2) 0.002(2) -0.001(2) C28 0.029(3) 0.023(2) 0.030(3) 0.012(2) 0.002(2) 0.003(2) C29 0.042(4) 0.029(3) 0.025(3) 0.003(2) 0.000(2) 0.012(3) C30 0.057(4) 0.045(4) 0.032(3) 0.011(3) 0.018(3) 0.012(3) C31 0.045(4) 0.049(4) 0.062(5) 0.025(3) 0.029(3) 0.012(3) C32 0.040(3) 0.036(3) 0.055(4) 0.013(3) 0.014(3) -0.001(3) C33 0.032(3) 0.031(3) 0.038(3) 0.001(2) 0.006(2) 0.002(2) C34 0.027(3) 0.019(2) 0.020(2) -0.0013(19) -0.001(2) -0.005(2) C35 0.024(3) 0.040(3) 0.028(3) 0.001(2) 0.001(2) 0.006(2) C36 0.031(3) 0.060(4) 0.039(3) 0.004(3) 0.002(2) 0.017(3) C37 0.038(3) 0.052(4) 0.031(3) 0.005(3) -0.004(2) 0.009(3) C38 0.038(3) 0.032(3) 0.023(2) -0.003(2) -0.002(2) 0.007(3) C39 0.021(3) 0.023(3) 0.031(3) 0.001(2) -0.003(2) 0.000(2) C40 0.023(3) 0.017(2) 0.025(3) -0.0071(19) -0.004(2) -0.003(2) C41 0.031(3) 0.025(3) 0.020(2) 0.001(2) 0.000(2) -0.004(2) C42 0.035(3) 0.040(3) 0.022(3) -0.007(2) 0.000(2) -0.004(3) C43 0.039(3) 0.035(4) 0.037(3) -0.011(3) 0.003(3) 0.001(3) C44 0.040(3) 0.032(3) 0.037(3) -0.008(3) 0.006(3) 0.009(3) C45 0.031(2) 0.020(2) 0.037(3) -0.001(2) -0.007(2) 0.000(2) C46 0.025(3) 0.027(3) 0.023(3) 0.002(2) -0.007(2) 0.001(2) C47 0.026(2) 0.027(3) 0.035(3) 0.002(3) -0.005(2) -0.001(3) C48 0.028(3) 0.030(3) 0.052(3) 0.004(2) -0.003(3) -0.003(3) C49 0.034(3) 0.042(4) 0.045(3) -0.001(3) -0.020(3) -0.002(3) C50 0.046(4) 0.056(4) 0.037(3) 0.001(3) -0.014(3) 0.006(3) C51 0.030(3) 0.040(3) 0.036(3) 0.002(3) -0.004(2) -0.004(3) B1 0.016(3) 0.031(3) 0.025(3) 0.003(3) 0.002(2) 0.003(2) O1 0.031(2) 0.030(2) 0.028(2) -0.0036(15) 0.0050(16) -0.0048(17) O2 0.0211(19) 0.0275(19) 0.0284(19) -0.0039(15) 0.0008(14) -0.0020(15) O3 0.0223(18) 0.030(2) 0.0208(17) -0.0022(15) 0.0009(15) 0.0016(16) O4 0.0219(18) 0.035(2) 0.0208(18) 0.0038(15) 0.0007(14) 0.0014(16) C52 0.016(2) 0.028(3) 0.030(3) 0.000(2) -0.009(2) -0.009(2) C53 0.021(3) 0.026(3) 0.041(3) -0.008(2) 0.000(2) 0.002(2) C54 0.028(3) 0.020(2) 0.042(4) 0.006(2) -0.007(2) -0.006(2) C55 0.031(3) 0.022(3) 0.026(3) -0.003(2) -0.003(2) -0.007(2) C56 0.025(3) 0.031(3) 0.038(3) 0.009(2) -0.005(2) -0.005(2) C57 0.027(3) 0.039(3) 0.026(3) 0.005(2) 0.002(2) -0.004(2) C58 0.022(3) 0.042(3) 0.032(3) -0.006(3) -0.001(2) -0.007(2) C59 0.018(2) 0.028(3) 0.026(3) 0.002(2) -0.004(2) -0.002(2) C60 0.024(2) 0.027(3) 0.023(3) -0.003(2) -0.004(2) -0.005(2) C61 0.024(3) 0.026(3) 0.023(3) 0.001(2) -0.006(2) -0.005(2) C62 0.019(2) 0.027(3) 0.027(3) -0.003(2) 0.002(2) 0.000(2) C63 0.028(3) 0.025(3) 0.024(3) -0.008(2) 0.005(2) -0.002(2) C64 0.025(3) 0.034(3) 0.029(3) 0.000(2) 0.001(2) -0.004(2) C65 0.022(3) 0.051(4) 0.033(3) 0.004(3) 0.001(2) -0.005(3) C66 0.028(3) 0.064(4) 0.034(3) 0.007(3) -0.008(3) 0.009(3) C67 0.027(3) 0.038(3) 0.038(3) 0.004(2) -0.001(3) 0.005(3) C68 0.029(3) 0.034(3) 0.024(3) 0.001(2) 0.000(2) -0.001(2) C69 0.036(3) 0.024(3) 0.029(3) -0.003(2) -0.005(2) 0.003(2) C70 0.025(2) 0.029(3) 0.029(3) 0.001(3) 0.004(2) -0.004(3) C71 0.028(3) 0.030(3) 0.020(2) -0.011(2) 0.001(2) 0.001(2) C72 0.024(3) 0.028(3) 0.012(2) -0.0013(19) 0.0017(18) -0.004(2) C73 0.027(3) 0.028(3) 0.014(2) 0.0022(19) -0.001(2) 0.004(2) C74 0.032(3) 0.028(3) 0.022(2) 0.002(2) 0.001(2) 0.000(2) C75 0.029(3) 0.030(3) 0.017(2) -0.002(2) 0.004(2) -0.003(2) C76 0.040(3) 0.026(3) 0.029(3) -0.005(2) 0.004(2) -0.004(3) C77 0.031(3) 0.033(3) 0.038(3) -0.010(3) 0.003(2) -0.012(3) C78 0.030(3) 0.044(3) 0.035(3) 0.000(3) -0.010(2) 0.000(3) C79 0.023(3) 0.029(3) 0.033(3) -0.004(2) 0.002(2) 0.003(2) C80 0.025(2) 0.026(3) 0.017(2) -0.004(2) 0.0028(19) 0.003(2) C81 0.024(2) 0.030(3) 0.016(2) 0.003(2) 0.004(2) 0.001(2) C82 0.019(2) 0.030(3) 0.021(3) 0.004(2) 0.000(2) -0.001(2) C83 0.023(3) 0.027(3) 0.025(3) -0.001(2) -0.004(2) 0.003(2) C84 0.024(3) 0.027(3) 0.026(3) 0.000(2) 0.007(2) -0.001(2) C85 0.028(3) 0.032(3) 0.040(3) -0.004(3) 0.009(2) 0.003(2) C86 0.034(3) 0.032(3) 0.037(3) -0.010(2) 0.010(3) 0.005(3) C87 0.036(3) 0.026(3) 0.029(3) -0.005(2) 0.002(2) 0.006(2) C88 0.026(3) 0.020(3) 0.033(3) 0.000(2) -0.001(2) 0.005(2) C89 0.030(3) 0.021(2) 0.026(3) 0.001(2) -0.004(2) 0.002(2) C90 0.027(3) 0.035(3) 0.026(3) 0.005(2) -0.003(2) -0.002(2) C91 0.017(3) 0.038(3) 0.017(2) 0.001(2) 0.0000(18) -0.003(2) C92 0.22(2) 0.22(2) 0.134(13) 0.018(13) -0.046(15) -0.120(18) Cl1 0.136(5) 0.221(7) 0.355(10) 0.060(7) 0.040(5) 0.001(4) Cl2 0.277(9) 0.260(9) 0.285(9) -0.105(7) -0.030(7) -0.009(7) C93 0.102(8) 0.123(9) 0.065(6) 0.009(6) -0.002(6) -0.041(7) Cl3 0.162(4) 0.173(4) 0.130(3) 0.033(3) -0.028(3) -0.074(3) Cl4 0.104(2) 0.195(4) 0.110(3) -0.056(3) -0.022(2) -0.011(3) C94 0.111(7) 0.055(5) 0.072(6) -0.014(4) 0.018(5) 0.011(6) Cl5 0.130(6) 0.146(6) 0.094(4) 0.021(4) 0.039(4) 0.052(4) Cl6 0.102(4) 0.034(2) 0.069(3) 0.0075(18) 0.003(3) 0.000(2) C95 0.129(7) 0.200(11) 0.185(11) 0.063(9) 0.021(8) -0.023(7) Cl7 0.114(6) 0.168(8) 0.172(8) 0.024(6) 0.008(5) -0.022(5) Cl8 0.150(8) 0.230(11) 0.212(11) 0.075(9) 0.043(8) 0.009(8) O5 0.101(5) 0.077(4) 0.133(7) -0.018(4) -0.014(6) -0.018(5) C96 0.125(11) 0.100(9) 0.178(15) -0.078(10) 0.088(12) -0.057(9) C97 0.114(10) 0.086(9) 0.181(15) -0.009(9) -0.044(11) -0.015(7) C98 0.211(19) 0.170(16) 0.062(7) -0.009(8) -0.024(10) -0.028(14) C99 0.143(13) 0.25(2) 0.112(11) 0.081(12) 0.080(10) 0.106(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.13988(18) 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 Rh1 . C1 . 2.205(5) yes Rh1 . C2 . 2.219(5) yes Rh1 . C4 . 2.225(5) yes Rh1 . C5 . 2.201(5) yes Rh1 . P1 . 2.3134(14) yes Rh1 . P2 . 2.2983(14) yes C1 . C2 . 1.367(8) yes C1 . C6 . 1.535(8) yes C1 . H11 . 0.95(3) no C2 . C3 . 1.534(9) yes C2 . H21 . 0.93(3) no C3 . C4 . 1.546(8) yes C3 . C7 . 1.559(8) yes C3 . H31 . 1.000 no C4 . C5 . 1.351(8) yes C4 . H41 . 1.01(3) no C5 . C6 . 1.548(7) yes C5 . H51 . 0.98(3) no C6 . C7 . 1.568(8) yes C6 . H61 . 1.000 no C7 . H71 . 1.000 no C7 . H72 . 1.000 no P1 . C8 . 1.838(6) yes P1 . C28 . 1.815(5) yes P1 . C34 . 1.826(5) yes P2 . C27 . 1.810(5) yes P2 . C40 . 1.821(5) yes P2 . C46 . 1.847(5) yes C8 . C9 . 1.428(7) yes C8 . C17 . 1.397(7) yes C9 . C10 . 1.351(8) yes C9 . H91 . 1.000 no C10 . C11 . 1.425(8) yes C10 . H101 . 1.000 no C11 . C12 . 1.430(8) yes C11 . C16 . 1.419(8) yes C12 . C13 . 1.347(9) yes C12 . H121 . 1.000 no C13 . C14 . 1.389(9) yes C13 . H131 . 1.000 no C14 . C15 . 1.370(8) yes C14 . H141 . 1.000 no C15 . C16 . 1.433(8) yes C15 . H151 . 1.000 no C16 . C17 . 1.424(7) yes C17 . C18 . 1.500(7) yes C18 . C19 . 1.447(7) yes C18 . C27 . 1.390(7) yes C19 . C20 . 1.431(8) yes C19 . C24 . 1.409(8) yes C20 . C21 . 1.365(8) yes C20 . H201 . 1.000 no C21 . C22 . 1.409(9) yes C21 . H211 . 1.000 no C22 . C23 . 1.328(9) yes C22 . H221 . 1.000 no C23 . C24 . 1.433(8) yes C23 . H231 . 1.000 no C24 . C25 . 1.415(8) yes C25 . C26 . 1.346(8) yes C25 . H251 . 1.000 no C26 . C27 . 1.432(8) yes C26 . H261 . 1.000 no C28 . C29 . 1.389(8) yes C28 . C33 . 1.407(8) yes C29 . C30 . 1.401(8) yes C29 . H291 . 1.000 no C30 . C31 . 1.365(10) yes C30 . H301 . 1.000 no C31 . C32 . 1.385(11) yes C31 . H311 . 1.000 no C32 . C33 . 1.402(8) yes C32 . H321 . 1.000 no C33 . H331 . 1.000 no C34 . C35 . 1.400(8) yes C34 . C39 . 1.393(7) yes C35 . C36 . 1.381(8) yes C35 . H351 . 1.000 no C36 . C37 . 1.402(8) yes C36 . H361 . 1.000 no C37 . C38 . 1.376(8) yes C37 . H371 . 1.000 no C38 . C39 . 1.392(7) yes C38 . H381 . 1.000 no C39 . H391 . 1.000 no C40 . C41 . 1.399(7) yes C40 . C45 . 1.405(7) yes C41 . C42 . 1.392(8) yes C41 . H411 . 1.000 no C42 . C43 . 1.370(9) yes C42 . H421 . 1.000 no C43 . C44 . 1.382(9) yes C43 . H431 . 1.000 no C44 . C45 . 1.396(8) yes C44 . H441 . 1.000 no C45 . H451 . 1.000 no C46 . C47 . 1.396(8) yes C46 . C51 . 1.378(8) yes C47 . C48 . 1.392(8) yes C47 . H471 . 1.000 no C48 . C49 . 1.379(8) yes C48 . H481 . 1.000 no C49 . C50 . 1.373(9) yes C49 . H491 . 1.000 no C50 . C51 . 1.395(8) yes C50 . H501 . 1.000 no C51 . H511 . 1.000 no B1 . O1 . 1.490(7) yes B1 . O2 . 1.471(7) yes B1 . O3 . 1.476(7) yes B1 . O4 . 1.471(7) yes O1 . C52 . 1.375(6) yes O2 . C71 . 1.350(6) yes O3 . C72 . 1.367(6) yes O4 . C91 . 1.357(6) yes C52 . C53 . 1.421(8) yes C52 . C61 . 1.363(8) yes C53 . C54 . 1.375(8) yes C53 . H531 . 1.000 no C54 . C55 . 1.411(8) yes C54 . H541 . 1.000 no C55 . C56 . 1.418(8) yes C55 . C60 . 1.433(7) yes C56 . C57 . 1.369(8) yes C56 . H561 . 1.000 no C57 . C58 . 1.402(8) yes C57 . H571 . 1.000 no C58 . C59 . 1.380(8) yes C58 . H581 . 1.000 no C59 . C60 . 1.420(7) yes C59 . H591 . 1.000 no C60 . C61 . 1.440(7) yes C61 . C62 . 1.471(7) yes C62 . C63 . 1.431(7) yes C62 . C71 . 1.402(7) yes C63 . C64 . 1.439(8) yes C63 . C68 . 1.413(8) yes C64 . C65 . 1.376(8) yes C64 . H641 . 1.000 no C65 . C66 . 1.409(10) yes C65 . H651 . 1.000 no C66 . C67 . 1.371(9) yes C66 . H661 . 1.000 no C67 . C68 . 1.407(8) yes C67 . H671 . 1.000 no C68 . C69 . 1.429(8) yes C69 . C70 . 1.376(8) yes C69 . H691 . 1.000 no C70 . C71 . 1.411(8) yes C70 . H701 . 1.000 no C72 . C73 . 1.414(7) yes C72 . C81 . 1.379(7) yes C73 . C74 . 1.378(8) yes C73 . H731 . 1.000 no C74 . C75 . 1.416(7) yes C74 . H741 . 1.000 no C75 . C76 . 1.418(8) yes C75 . C80 . 1.426(8) yes C76 . C77 . 1.373(8) yes C76 . H761 . 1.000 no C77 . C78 . 1.396(9) yes C77 . H771 . 1.000 no C78 . C79 . 1.364(8) yes C78 . H781 . 1.000 no C79 . C80 . 1.425(7) yes C79 . H791 . 1.000 no C80 . C81 . 1.429(7) yes C81 . C82 . 1.489(8) yes C82 . C83 . 1.441(7) yes C82 . C91 . 1.389(7) yes C83 . C84 . 1.413(7) yes C83 . C88 . 1.430(7) yes C84 . C85 . 1.379(7) yes C84 . H841 . 1.000 no C85 . C86 . 1.399(8) yes C85 . H851 . 1.000 no C86 . C87 . 1.337(8) yes C86 . H861 . 1.000 no C87 . C88 . 1.421(8) yes C87 . H871 . 1.000 no C88 . C89 . 1.423(8) yes C89 . C90 . 1.359(8) yes C89 . H891 . 1.000 no C90 . C91 . 1.402(8) yes C90 . H901 . 1.000 no C92 . Cl1 . 1.729(19) yes C92 . Cl2 . 1.655(19) yes C92 . H921 . 1.000 no C92 . H922 . 1.000 no C93 . Cl3 . 1.717(11) yes C93 . Cl4 . 1.790(14) yes C93 . H931 . 1.000 no C93 . H932 . 1.000 no C94 . Cl5 . 1.718(14) yes C94 . Cl6 . 1.773(13) yes C94 . H941 . 1.000 no C94 . H942 . 1.000 no C95 . Cl7 . 1.764(17) yes C95 . Cl8 . 1.727(18) yes C95 . H951 . 1.000 no C95 . H952 . 1.000 no O5 . C96 . 1.321(15) yes O5 . C98 . 1.433(17) yes C96 . C97 . 1.63(2) yes C96 . H961 . 1.000 no C96 . H962 . 1.000 no C97 . H971 . 1.000 no C97 . H972 . 1.000 no C97 . H973 . 1.000 no C98 . C99 . 1.49(2) yes C98 . H981 . 1.000 no C98 . H982 . 1.000 no C99 . H991 . 1.000 no C99 . H992 . 1.000 no C99 . H993 . 1.000 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 C1 . Rh1 . C2 . 36.0(2) yes C1 . Rh1 . C4 . 77.0(2) yes C2 . Rh1 . C4 . 65.1(2) yes C1 . Rh1 . C5 . 66.1(2) yes C2 . Rh1 . C5 . 77.1(2) yes C4 . Rh1 . C5 . 35.5(2) yes C1 . Rh1 . P1 . 148.90(15) yes C2 . Rh1 . P1 . 162.66(17) yes C4 . Rh1 . P1 . 98.17(15) yes C5 . Rh1 . P1 . 91.93(14) yes C1 . Rh1 . P2 . 100.37(15) yes C2 . Rh1 . P2 . 104.17(16) yes C4 . Rh1 . P2 . 165.34(15) yes C5 . Rh1 . P2 . 155.77(14) yes P1 . Rh1 . P2 . 91.38(5) yes Rh1 . C1 . C2 . 72.6(3) yes Rh1 . C1 . C6 . 95.5(3) yes C2 . C1 . C6 . 107.6(5) yes Rh1 . C1 . H11 . 111(3) no C2 . C1 . H11 . 130(3) no C6 . C1 . H11 . 121(3) no Rh1 . C2 . C1 . 71.5(3) yes Rh1 . C2 . C3 . 96.7(3) yes C1 . C2 . C3 . 106.7(5) yes Rh1 . C2 . H21 . 111(3) no C1 . C2 . H21 . 129(4) no C3 . C2 . H21 . 123(4) no C2 . C3 . C4 . 101.9(4) yes C2 . C3 . C7 . 100.3(4) yes C4 . C3 . C7 . 99.6(4) yes C2 . C3 . H31 . 117.332 no C4 . C3 . H31 . 117.332 no C7 . C3 . H31 . 117.332 no C3 . C4 . Rh1 . 96.1(3) yes C3 . C4 . C5 . 107.1(5) yes Rh1 . C4 . C5 . 71.3(3) yes C3 . C4 . H41 . 121(3) no Rh1 . C4 . H41 . 111(3) no C5 . C4 . H41 . 131(3) no Rh1 . C5 . C4 . 73.2(3) yes Rh1 . C5 . C6 . 95.3(3) yes C4 . C5 . C6 . 107.6(5) yes Rh1 . C5 . H51 . 110(3) no C4 . C5 . H51 . 127(3) no C6 . C5 . H51 . 124(3) no C1 . C6 . C5 . 102.4(4) yes C1 . C6 . C7 . 99.3(4) yes C5 . C6 . C7 . 98.9(4) yes C1 . C6 . H61 . 117.654 no C5 . C6 . H61 . 117.654 no C7 . C6 . H61 . 117.654 no C3 . C7 . C6 . 93.2(4) yes C3 . C7 . H71 . 113.369 no C6 . C7 . H71 . 113.369 no C3 . C7 . H72 . 113.369 no C6 . C7 . H72 . 113.369 no H71 . C7 . H72 . 109.467 no Rh1 . P1 . C8 . 120.22(16) yes Rh1 . P1 . C28 . 112.84(18) yes C8 . P1 . C28 . 103.3(2) yes Rh1 . P1 . C34 . 108.24(16) yes C8 . P1 . C34 . 107.0(2) yes C28 . P1 . C34 . 104.0(2) yes Rh1 . P2 . C27 . 104.06(18) yes Rh1 . P2 . C40 . 116.93(17) yes C27 . P2 . C40 . 111.1(2) yes Rh1 . P2 . C46 . 120.17(18) yes C27 . P2 . C46 . 106.1(2) yes C40 . P2 . C46 . 98.1(2) yes P1 . C8 . C9 . 120.8(4) yes P1 . C8 . C17 . 120.1(4) yes C9 . C8 . C17 . 118.8(5) yes C8 . C9 . C10 . 122.3(5) yes C8 . C9 . H91 . 118.858 no C10 . C9 . H91 . 118.858 no C9 . C10 . C11 . 120.2(5) yes C9 . C10 . H101 . 119.888 no C11 . C10 . H101 . 119.888 no C10 . C11 . C12 . 121.7(5) yes C10 . C11 . C16 . 118.6(5) yes C12 . C11 . C16 . 119.7(5) yes C11 . C12 . C13 . 120.2(6) yes C11 . C12 . H121 . 119.897 no C13 . C12 . H121 . 119.897 no C12 . C13 . C14 . 120.7(6) yes C12 . C13 . H131 . 119.649 no C14 . C13 . H131 . 119.649 no C13 . C14 . C15 . 121.9(5) yes C13 . C14 . H141 . 119.072 no C15 . C14 . H141 . 119.072 no C14 . C15 . C16 . 119.5(5) yes C14 . C15 . H151 . 120.234 no C16 . C15 . H151 . 120.234 no C15 . C16 . C11 . 118.0(5) yes C15 . C16 . C17 . 121.5(5) yes C11 . C16 . C17 . 120.4(5) yes C16 . C17 . C8 . 119.5(5) yes C16 . C17 . C18 . 119.8(4) yes C8 . C17 . C18 . 120.6(4) yes C17 . C18 . C19 . 117.7(4) yes C17 . C18 . C27 . 122.8(4) yes C19 . C18 . C27 . 119.5(4) yes C18 . C19 . C20 . 122.6(5) yes C18 . C19 . C24 . 119.8(5) yes C20 . C19 . C24 . 117.6(5) yes C19 . C20 . C21 . 120.9(5) yes C19 . C20 . H201 . 119.533 no C21 . C20 . H201 . 119.533 no C20 . C21 . C22 . 120.6(6) yes C20 . C21 . H211 . 119.723 no C22 . C21 . H211 . 119.724 no C21 . C22 . C23 . 120.2(6) yes C21 . C22 . H221 . 119.908 no C23 . C22 . H221 . 119.908 no C22 . C23 . C24 . 121.5(5) yes C22 . C23 . H231 . 119.234 no C24 . C23 . H231 . 119.234 no C23 . C24 . C19 . 119.2(5) yes C23 . C24 . C25 . 122.1(5) yes C19 . C24 . C25 . 118.6(5) yes C24 . C25 . C26 . 121.6(5) yes C24 . C25 . H251 . 119.197 no C26 . C25 . H251 . 119.197 no C25 . C26 . C27 . 121.4(5) yes C25 . C26 . H261 . 119.321 no C27 . C26 . H261 . 119.321 no P2 . C27 . C26 . 117.3(4) yes P2 . C27 . C18 . 122.7(4) yes C26 . C27 . C18 . 118.9(4) yes P1 . C28 . C29 . 121.2(4) yes P1 . C28 . C33 . 119.1(4) yes C29 . C28 . C33 . 119.7(5) yes C28 . C29 . C30 . 120.0(6) yes C28 . C29 . H291 . 120.003 no C30 . C29 . H291 . 120.003 no C29 . C30 . C31 . 120.1(6) yes C29 . C30 . H301 . 119.956 no C31 . C30 . H301 . 119.956 no C30 . C31 . C32 . 121.0(6) yes C30 . C31 . H311 . 119.498 no C32 . C31 . H311 . 119.498 no C31 . C32 . C33 . 119.8(6) yes C31 . C32 . H321 . 120.078 no C33 . C32 . H321 . 120.078 no C28 . C33 . C32 . 119.3(6) yes C28 . C33 . H331 . 120.366 no C32 . C33 . H331 . 120.366 no P1 . C34 . C35 . 121.8(4) yes P1 . C34 . C39 . 119.5(4) yes C35 . C34 . C39 . 117.9(5) yes C34 . C35 . C36 . 120.4(5) yes C34 . C35 . H351 . 119.793 no C36 . C35 . H351 . 119.793 no C35 . C36 . C37 . 121.2(5) yes C35 . C36 . H361 . 119.401 no C37 . C36 . H361 . 119.401 no C36 . C37 . C38 . 118.5(5) yes C36 . C37 . H371 . 120.736 no C38 . C37 . H371 . 120.736 no C37 . C38 . C39 . 120.5(5) yes C37 . C38 . H381 . 119.746 no C39 . C38 . H381 . 119.746 no C34 . C39 . C38 . 121.3(5) yes C34 . C39 . H391 . 119.331 no C38 . C39 . H391 . 119.331 no P2 . C40 . C41 . 119.0(4) yes P2 . C40 . C45 . 120.9(4) yes C41 . C40 . C45 . 119.4(5) yes C40 . C41 . C42 . 119.8(5) yes C40 . C41 . H411 . 120.122 no C42 . C41 . H411 . 120.122 no C41 . C42 . C43 . 120.6(5) yes C41 . C42 . H421 . 119.677 no C43 . C42 . H421 . 119.677 no C42 . C43 . C44 . 120.4(5) yes C42 . C43 . H431 . 119.798 no C44 . C43 . H431 . 119.798 no C43 . C44 . C45 . 120.3(5) yes C43 . C44 . H441 . 119.869 no C45 . C44 . H441 . 119.869 no C40 . C45 . C44 . 119.5(5) yes C40 . C45 . H451 . 120.240 no C44 . C45 . H451 . 120.240 no P2 . C46 . C47 . 114.7(4) yes P2 . C46 . C51 . 125.9(4) yes C47 . C46 . C51 . 119.1(5) yes C46 . C47 . C48 . 120.1(5) yes C46 . C47 . H471 . 119.957 no C48 . C47 . H471 . 119.957 no C47 . C48 . C49 . 120.5(5) yes C47 . C48 . H481 . 119.741 no C49 . C48 . H481 . 119.741 no C48 . C49 . C50 . 119.3(5) yes C48 . C49 . H491 . 120.355 no C50 . C49 . H491 . 120.355 no C49 . C50 . C51 . 120.9(6) yes C49 . C50 . H501 . 119.571 no C51 . C50 . H501 . 119.571 no C50 . C51 . C46 . 120.2(5) yes C50 . C51 . H511 . 119.913 no C46 . C51 . H511 . 119.913 no O1 . B1 . O2 . 111.8(4) yes O1 . B1 . O3 . 104.2(4) yes O2 . B1 . O3 . 111.6(4) yes O1 . B1 . O4 . 112.1(5) yes O2 . B1 . O4 . 105.2(4) yes O3 . B1 . O4 . 112.0(4) yes B1 . O1 . C52 . 114.3(4) yes B1 . O2 . C71 . 116.9(4) yes B1 . O3 . C72 . 115.6(4) yes B1 . O4 . C91 . 115.6(4) yes O1 . C52 . C53 . 117.0(5) yes O1 . C52 . C61 . 120.4(5) yes C53 . C52 . C61 . 122.5(5) yes C52 . C53 . C54 . 119.3(5) yes C52 . C53 . H531 . 120.373 no C54 . C53 . H531 . 120.373 no C53 . C54 . C55 . 120.9(5) yes C53 . C54 . H541 . 119.567 no C55 . C54 . H541 . 119.567 no C54 . C55 . C56 . 121.6(5) yes C54 . C55 . C60 . 118.8(5) yes C56 . C55 . C60 . 119.6(5) yes C55 . C56 . C57 . 121.0(5) yes C55 . C56 . H561 . 119.507 no C57 . C56 . H561 . 119.507 no C56 . C57 . C58 . 119.9(5) yes C56 . C57 . H571 . 120.035 no C58 . C57 . H571 . 120.035 no C57 . C58 . C59 . 120.7(5) yes C57 . C58 . H581 . 119.653 no C59 . C58 . H581 . 119.653 no C58 . C59 . C60 . 121.2(5) yes C58 . C59 . H591 . 119.411 no C60 . C59 . H591 . 119.412 no C55 . C60 . C59 . 117.6(5) yes C55 . C60 . C61 . 120.0(5) yes C59 . C60 . C61 . 122.3(5) yes C60 . C61 . C52 . 117.8(5) yes C60 . C61 . C62 . 122.4(5) yes C52 . C61 . C62 . 119.6(5) yes C61 . C62 . C63 . 124.1(5) yes C61 . C62 . C71 . 117.5(5) yes C63 . C62 . C71 . 118.3(5) yes C62 . C63 . C64 . 121.4(5) yes C62 . C63 . C68 . 120.6(5) yes C64 . C63 . C68 . 117.9(5) yes C63 . C64 . C65 . 120.1(5) yes C63 . C64 . H641 . 119.954 no C65 . C64 . H641 . 119.954 no C64 . C65 . C66 . 120.9(5) yes C64 . C65 . H651 . 119.570 no C66 . C65 . H651 . 119.569 no C65 . C66 . C67 . 120.2(5) yes C65 . C66 . H661 . 119.922 no C67 . C66 . H661 . 119.922 no C66 . C67 . C68 . 120.4(5) yes C66 . C67 . H671 . 119.821 no C68 . C67 . H671 . 119.821 no C63 . C68 . C67 . 120.6(5) yes C63 . C68 . C69 . 119.0(5) yes C67 . C68 . C69 . 120.4(5) yes C68 . C69 . C70 . 120.4(5) yes C68 . C69 . H691 . 119.815 no C70 . C69 . H691 . 119.815 no C69 . C70 . C71 . 120.5(5) yes C69 . C70 . H701 . 119.729 no C71 . C70 . H701 . 119.729 no C70 . C71 . C62 . 121.1(5) yes C70 . C71 . O2 . 118.0(5) yes C62 . C71 . O2 . 120.9(5) yes O3 . C72 . C73 . 117.2(4) yes O3 . C72 . C81 . 121.7(5) yes C73 . C72 . C81 . 121.1(5) yes C72 . C73 . C74 . 120.2(5) yes C72 . C73 . H731 . 119.925 no C74 . C73 . H731 . 119.925 no C73 . C74 . C75 . 121.1(5) yes C73 . C74 . H741 . 119.475 no C75 . C74 . H741 . 119.475 no C74 . C75 . C76 . 121.2(5) yes C74 . C75 . C80 . 118.2(5) yes C76 . C75 . C80 . 120.6(5) yes C75 . C76 . C77 . 120.7(5) yes C75 . C76 . H761 . 119.659 no C77 . C76 . H761 . 119.658 no C76 . C77 . C78 . 118.9(5) yes C76 . C77 . H771 . 120.562 no C78 . C77 . H771 . 120.562 no C77 . C78 . C79 . 122.0(5) yes C77 . C78 . H781 . 118.999 no C79 . C78 . H781 . 118.999 no C78 . C79 . C80 . 121.4(5) yes C78 . C79 . H791 . 119.320 no C80 . C79 . H791 . 119.320 no C75 . C80 . C79 . 116.4(5) yes C75 . C80 . C81 . 120.4(5) yes C79 . C80 . C81 . 123.2(5) yes C80 . C81 . C72 . 118.8(5) yes C80 . C81 . C82 . 123.7(5) yes C72 . C81 . C82 . 117.5(5) yes C81 . C82 . C83 . 122.1(5) yes C81 . C82 . C91 . 118.5(5) yes C83 . C82 . C91 . 119.3(5) yes C82 . C83 . C84 . 123.7(5) yes C82 . C83 . C88 . 118.9(5) yes C84 . C83 . C88 . 117.3(5) yes C83 . C84 . C85 . 121.2(5) yes C83 . C84 . H841 . 119.393 no C85 . C84 . H841 . 119.393 no C84 . C85 . C86 . 120.4(5) yes C84 . C85 . H851 . 119.796 no C86 . C85 . H851 . 119.796 no C85 . C86 . C87 . 120.1(5) yes C85 . C86 . H861 . 119.956 no C87 . C86 . H861 . 119.956 no C86 . C87 . C88 . 121.8(5) yes C86 . C87 . H871 . 119.106 no C88 . C87 . H871 . 119.106 no C83 . C88 . C87 . 118.9(5) yes C83 . C88 . C89 . 119.3(5) yes C87 . C88 . C89 . 121.8(5) yes C88 . C89 . C90 . 120.2(5) yes C88 . C89 . H891 . 119.884 no C90 . C89 . H891 . 119.884 no C89 . C90 . C91 . 121.7(5) yes C89 . C90 . H901 . 119.166 no C91 . C90 . H901 . 119.166 no C90 . C91 . C82 . 120.5(5) yes C90 . C91 . O4 . 119.1(5) yes C82 . C91 . O4 . 120.3(5) yes Cl1 . C92 . Cl2 . 114.1(11) yes Cl1 . C92 . H921 . 108.310 no Cl2 . C92 . H921 . 108.310 no Cl1 . C92 . H922 . 108.310 no Cl2 . C92 . H922 . 108.310 no H921 . C92 . H922 . 109.467 no Cl3 . C93 . Cl4 . 113.5(7) yes Cl3 . C93 . H931 . 108.448 no Cl4 . C93 . H931 . 108.448 no Cl3 . C93 . H932 . 108.448 no Cl4 . C93 . H932 . 108.448 no H931 . C93 . H932 . 109.467 no Cl5 . C94 . Cl6 . 114.1(9) yes Cl5 . C94 . H941 . 108.301 no Cl6 . C94 . H941 . 108.300 no Cl5 . C94 . H942 . 108.300 no Cl6 . C94 . H942 . 108.300 no H941 . C94 . H942 . 109.467 no Cl7 . C95 . Cl8 . 104.3(11) yes Cl7 . C95 . H951 . 110.747 no Cl8 . C95 . H951 . 110.747 no Cl7 . C95 . H952 . 110.747 no Cl8 . C95 . H952 . 110.747 no H951 . C95 . H952 . 109.467 no C96 . O5 . C98 . 114.0(15) yes O5 . C96 . C97 . 108.2(13) yes O5 . C96 . H961 . 109.788 no C97 . C96 . H961 . 109.788 no O5 . C96 . H962 . 109.788 no C97 . C96 . H962 . 109.788 no H961 . C96 . H962 . 109.467 no C96 . C97 . H971 . 109.467 no C96 . C97 . H972 . 109.467 no H971 . C97 . H972 . 109.476 no C96 . C97 . H973 . 109.467 no H971 . C97 . H973 . 109.476 no H972 . C97 . H973 . 109.476 no O5 . C98 . C99 . 115.4(13) yes O5 . C98 . H981 . 107.981 no C99 . C98 . H981 . 107.981 no O5 . C98 . H982 . 107.981 no C99 . C98 . H982 . 107.981 no H981 . C98 . H982 . 109.467 no C98 . C99 . H991 . 109.467 no C98 . C99 . H992 . 109.467 no H991 . C99 . H992 . 109.476 no C98 . C99 . H993 . 109.467 no H991 . C99 . H993 . 109.476 no H992 . C99 . H993 . 109.476 no _database_code_depnum_ccdc_archive 'CCDC 934112' ####################################################################### # # 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_arc1456 #TrackingRef '19476_web_deposit_cif_file_2_JohnBrown_1366025934.arc1456a.cif' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _ccdc_journal_depnumber ? _computing_structure_solution ; 'SIR92 (Giacovazzo et al, 1992)' ; _chemical_name_systematic ; ((Bicyclo[2.2.1]hepta-2,5-diene)((R)-bis-2,2'-(diphenylphosphino)-1,1'-binaphthalene)rhodium) ((R,R)-bis-(1,1'-binaphthalen-2,2'-dioxo)boronate). ; _chemical_melting_point ; Not determined ; _chemical_absolute_configuration ; '(R),(R,R)' ; _exptl_crystal_thermal_history ; The material was crystallised at ambient temperature. A suitable crystal was cooled rapidly to 150K for single-crystal X-ray diffraction analysis. ; _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_special_details ; The hydrogen atoms of the coordinated alkene groups were located in a difference Fourier map and their coordinates and isotropic displacement parameters subsequently refined, subject to restraint of the C-H bond lengths to 1.00(4) \%A and to a similarity restraint between their displacement parameters and those of the parent C atoms. Other hydrogen atoms were positioned geometrically after each cycle of refinement. ; #============================================================= _cell_length_a 11.8286(2) _cell_angle_alpha 90 _cell_length_b 25.5279(4) _cell_angle_beta 111.9738(8) _cell_length_c 14.3047(2) _cell_angle_gamma 90 _cell_volume 4005.65(11) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-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 '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_IV_Table_2.2B '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_IV_Table_2.2B '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_IV_Table_2.2B '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_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B '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_IV_Table_2.2B '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_IV_Table_2.2B _cell_formula_units_Z 2 _chemical_formula_sum ' C96 H76 B Cl8 O4 P2 Rh ' _chemical_formula_moiety ' C52 H44 P2 Rh, C40 H24 B O4, 4( C H2 Cl2 ) ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 1752.94 _cell_measurement_reflns_used 38581 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' block ' _exptl_crystal_colour ' orange-yellow ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.24 _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 0.575 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.94 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 38581 _reflns_number_total 16161 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_theta_min 5.118 _diffrn_reflns_theta_max 27.478 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.478 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min -33 _reflns_limit_k_max 29 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _refine_diff_density_min -1.12 _refine_diff_density_max 0.75 _refine_ls_number_reflns 10962 _refine_ls_number_restraints 9 _refine_ls_number_parameters 1026 #_refine_ls_R_factor_ref 0.0432 _refine_ls_wR_factor_ref 0.0464 _refine_ls_goodness_of_fit_ref 1.1097 #_reflns_number_all 16139 _refine_ls_R_factor_all 0.0751 _refine_ls_wR_factor_all 0.0814 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 10962 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_gt 0.0464 _refine_ls_shift/su_max 0.029637 _refine_ls_abs_structure_Flack -0.04(2) _refine_ls_abs_structure_details 'Flack, 6867 Friedel-pairs' _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.294 0.754E-01 0.775E-01 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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 Rh1 Rh 0.14685(3) 0.50026(2) 0.22549(3) 0.0189 1.0000 Uani . . C1 C 0.0633(5) 0.52797(19) 0.0674(4) 0.0295 1.0000 Uani D U C2 C -0.0161(5) 0.5416(2) 0.1116(4) 0.0279 1.0000 Uani D U C3 C -0.0298(5) 0.5976(2) 0.1401(5) 0.0385 1.0000 Uani . . C4 C 0.0433(6) 0.6066(2) 0.2528(5) 0.0375 1.0000 Uani . . C5 C 0.1662(5) 0.5809(2) 0.2907(4) 0.0306 1.0000 Uani D U C6 C 0.2452(5) 0.5773(2) 0.2402(4) 0.0304 1.0000 Uani D U C7 C 0.2255(5) 0.5995(2) 0.1376(4) 0.0325 1.0000 Uani . . C8 C 0.1535(5) 0.5633(2) 0.0484(4) 0.0292 1.0000 Uani . . P1 P 0.08413(10) 0.41616(5) 0.17824(9) 0.0177 1.0000 Uani . . P2 P 0.32409(11) 0.46673(5) 0.34835(9) 0.0180 1.0000 Uani . . C9 C 0.3260(4) 0.39949(17) 0.3954(3) 0.0173 1.0000 Uani . . C10 C 0.3299(4) 0.39090(18) 0.4944(3) 0.0197 1.0000 Uani . . C11 C 0.3144(5) 0.3419(2) 0.5276(4) 0.0266 1.0000 Uani . . C12 C 0.2960(5) 0.29731(19) 0.4636(4) 0.0239 1.0000 Uani . . C13 C 0.2765(6) 0.2475(2) 0.4950(4) 0.0348 1.0000 Uani . . C14 C 0.2580(6) 0.2054(2) 0.4323(4) 0.0364 1.0000 Uani . . C15 C 0.2560(5) 0.21210(19) 0.3352(4) 0.0290 1.0000 Uani . . C16 C 0.2754(4) 0.25962(19) 0.3005(4) 0.0236 1.0000 Uani . . C17 C 0.2949(4) 0.30509(19) 0.3645(3) 0.0182 1.0000 Uani . . C18 C 0.3110(4) 0.35633(18) 0.3311(3) 0.0186 1.0000 Uani . . C19 C 0.3077(4) 0.36347(17) 0.2258(3) 0.0171 1.0000 Uani . . C20 C 0.4099(4) 0.34622(17) 0.2025(4) 0.0183 1.0000 Uani . . C21 C 0.5127(4) 0.32134(19) 0.2753(4) 0.0241 1.0000 Uani . . C22 C 0.6091(5) 0.3053(2) 0.2512(4) 0.0287 1.0000 Uani . . C23 C 0.6086(5) 0.3126(2) 0.1533(4) 0.0288 1.0000 Uani . . C24 C 0.5123(4) 0.3371(2) 0.0829(4) 0.0255 1.0000 Uani . . C25 C 0.4108(4) 0.35473(18) 0.1050(4) 0.0203 1.0000 Uani . . C26 C 0.3135(4) 0.38319(18) 0.0340(3) 0.0209 1.0000 Uani . . C27 C 0.2167(4) 0.39948(19) 0.0564(3) 0.0220 1.0000 Uani . . C28 C 0.2097(4) 0.38746(18) 0.1510(4) 0.0169 1.0000 Uani . . C29 C 0.4487(4) 0.46637(18) 0.3038(4) 0.0209 1.0000 Uani . . C30 C 0.4323(5) 0.48465(18) 0.2071(4) 0.0265 1.0000 Uani . . C31 C 0.5269(5) 0.4832(2) 0.1718(4) 0.0361 1.0000 Uani . . C32 C 0.6387(6) 0.4629(3) 0.2327(5) 0.0456 1.0000 Uani . . C33 C 0.6569(5) 0.4450(2) 0.3278(5) 0.0362 1.0000 Uani . . C34 C 0.5627(5) 0.44625(19) 0.3638(4) 0.0249 1.0000 Uani . . C35 C 0.3778(4) 0.50732(19) 0.4624(3) 0.0171 1.0000 Uani . . C36 C 0.4857(5) 0.5357(2) 0.4909(4) 0.0292 1.0000 Uani . . C37 C 0.5175(5) 0.5693(2) 0.5742(4) 0.0396 1.0000 Uani . . C38 C 0.4432(5) 0.5750(2) 0.6282(4) 0.0337 1.0000 Uani . . C39 C 0.3339(5) 0.5470(2) 0.5995(4) 0.0316 1.0000 Uani . . C40 C 0.3016(5) 0.51408(18) 0.5167(4) 0.0276 1.0000 Uani . . C41 C 0.0440(4) 0.37586(19) 0.2666(4) 0.0192 1.0000 Uani . . C42 C 0.0370(4) 0.3978(2) 0.3518(4) 0.0250 1.0000 Uani . . C43 C -0.0085(5) 0.3695(2) 0.4135(4) 0.0308 1.0000 Uani . . C44 C -0.0476(5) 0.3188(2) 0.3891(5) 0.0327 1.0000 Uani . . C45 C -0.0406(5) 0.2952(2) 0.3026(4) 0.0300 1.0000 Uani . . C46 C 0.0028(5) 0.3237(2) 0.2410(4) 0.0262 1.0000 Uani . . C47 C -0.0571(4) 0.40531(19) 0.0680(3) 0.0211 1.0000 Uani . . C48 C -0.1617(5) 0.4218(2) 0.0839(4) 0.0258 1.0000 Uani . . C49 C -0.2765(4) 0.4137(2) 0.0102(4) 0.0309 1.0000 Uani . . C50 C -0.2885(5) 0.3900(2) -0.0793(4) 0.0291 1.0000 Uani . . C51 C -0.1862(5) 0.3734(2) -0.0948(4) 0.0273 1.0000 Uani . . C52 C -0.0716(4) 0.38113(19) -0.0217(4) 0.0226 1.0000 Uani . . B1 B 0.1850(5) 0.5061(3) 0.8038(4) 0.0247 1.0000 Uani . . O1 O 0.1555(3) 0.55703(13) 0.7509(2) 0.0240 1.0000 Uani . . O2 O 0.2998(3) 0.50857(13) 0.8924(2) 0.0230 1.0000 Uani . . O3 O 0.1900(3) 0.47097(12) 0.7246(2) 0.0229 1.0000 Uani . . O4 O 0.0970(3) 0.48933(12) 0.8473(2) 0.0249 1.0000 Uani . . C53 C 0.1635(4) 0.6007(2) 0.8077(4) 0.0232 1.0000 Uani . . C54 C 0.0546(4) 0.6282(2) 0.7929(4) 0.0284 1.0000 Uani . . C55 C 0.0529(5) 0.6718(2) 0.8475(4) 0.0337 1.0000 Uani . . C56 C 0.1625(5) 0.68891(19) 0.9246(4) 0.0294 1.0000 Uani . . C57 C 0.1621(6) 0.7303(2) 0.9899(5) 0.0365 1.0000 Uani . . C58 C 0.2650(6) 0.7447(2) 1.0689(5) 0.0399 1.0000 Uani . . C59 C 0.3733(5) 0.7176(2) 1.0855(4) 0.0334 1.0000 Uani . . C60 C 0.3789(5) 0.67755(19) 1.0238(4) 0.0289 1.0000 Uani . . C61 C 0.2739(4) 0.66234(18) 0.9393(4) 0.0226 1.0000 Uani . . C62 C 0.2746(4) 0.61903(18) 0.8754(3) 0.0218 1.0000 Uani . . C63 C 0.3899(4) 0.59161(19) 0.8826(3) 0.0212 1.0000 Uani . . C64 C 0.4953(4) 0.61909(19) 0.8826(4) 0.0226 1.0000 Uani . . C65 C 0.4981(5) 0.67409(19) 0.8672(4) 0.0253 1.0000 Uani . . C66 C 0.6018(5) 0.6996(2) 0.8739(4) 0.0305 1.0000 Uani . . C67 C 0.7105(5) 0.6714(2) 0.8935(4) 0.0340 1.0000 Uani . . C68 C 0.7127(5) 0.6185(2) 0.9034(4) 0.0287 1.0000 Uani . . C69 C 0.6051(5) 0.5906(2) 0.8981(4) 0.0256 1.0000 Uani . . C70 C 0.6048(5) 0.5355(2) 0.9058(4) 0.0276 1.0000 Uani . . C71 C 0.5020(4) 0.50951(19) 0.9000(3) 0.0252 1.0000 Uani . . C72 C 0.3943(4) 0.53777(18) 0.8891(3) 0.0207 1.0000 Uani . . C73 C 0.2034(5) 0.4192(2) 0.7487(3) 0.0233 1.0000 Uani . . C74 C 0.3166(4) 0.3959(2) 0.7614(4) 0.0245 1.0000 Uani . . C75 C 0.3375(4) 0.3437(2) 0.7875(4) 0.0272 1.0000 Uani . . C76 C 0.2465(5) 0.31362(19) 0.8057(4) 0.0255 1.0000 Uani . . C77 C 0.2691(5) 0.2608(2) 0.8386(4) 0.0345 1.0000 Uani . . C78 C 0.1839(6) 0.2321(2) 0.8580(5) 0.0405 1.0000 Uani . . C79 C 0.0714(5) 0.2552(2) 0.8488(4) 0.0328 1.0000 Uani . . C80 C 0.0474(5) 0.3064(2) 0.8162(4) 0.0261 1.0000 Uani . . C81 C 0.1315(4) 0.33714(19) 0.7907(3) 0.0215 1.0000 Uani . . C82 C 0.1092(4) 0.39056(19) 0.7593(4) 0.0203 1.0000 Uani . . C83 C -0.0083(4) 0.41788(18) 0.7432(3) 0.0206 1.0000 Uani . . C84 C -0.1247(4) 0.39681(19) 0.6782(4) 0.0246 1.0000 Uani . . C85 C -0.1349(5) 0.3511(2) 0.6166(4) 0.0298 1.0000 Uani . . C86 C -0.2445(5) 0.3291(2) 0.5630(4) 0.0341 1.0000 Uani . . C87 C -0.3526(5) 0.3507(2) 0.5669(4) 0.0374 1.0000 Uani . . C88 C -0.3474(5) 0.3964(2) 0.6201(4) 0.0343 1.0000 Uani . . C89 C -0.2332(5) 0.4207(2) 0.6746(4) 0.0274 1.0000 Uani . . C90 C -0.2284(5) 0.4680(2) 0.7273(4) 0.0316 1.0000 Uani . . C91 C -0.1170(4) 0.49033(18) 0.7814(4) 0.0267 1.0000 Uani . . C92 C -0.0079(4) 0.46549(19) 0.7888(3) 0.0223 1.0000 Uani . . C93 C 0.0459(14) 0.6679(5) 0.5491(8) 0.1237 1.0000 Uani . . Cl1 Cl -0.0194(2) 0.69569(13) 0.4321(2) 0.1064 1.0000 Uani . . Cl2 Cl 0.1976(2) 0.68444(8) 0.61435(19) 0.0787 1.0000 Uani . . C94 C 0.3332(10) 0.6853(4) 0.4321(7) 0.0877 1.0000 Uani . . Cl3 Cl 0.3230(3) 0.71162(10) 0.3192(2) 0.0999 1.0000 Uani . . Cl4 Cl 0.43820(19) 0.71438(8) 0.53821(18) 0.0774 1.0000 Uani . . C95 C 0.6914(7) 0.6030(3) 0.2838(6) 0.0690 1.0000 Uani . . Cl5 Cl 0.5788(2) 0.63755(9) 0.31028(16) 0.0718 1.0000 Uani . . Cl6 Cl 0.66420(17) 0.60049(8) 0.15452(14) 0.0579 1.0000 Uani . . C96 C 0.9238(5) 0.5164(2) 0.5471(4) 0.0367 1.0000 Uani . . Cl7 Cl 0.81130(14) 0.56282(6) 0.54127(12) 0.0442 1.0000 Uani . . Cl8 Cl 0.96281(15) 0.52166(7) 0.43921(12) 0.0486 1.0000 Uani . . H11 H 0.049(4) 0.4945(15) 0.033(3) 0.019(5) 1.0000 Uiso D U H21 H -0.085(4) 0.5217(19) 0.103(4) 0.029(5) 1.0000 Uiso D U H51 H 0.206(4) 0.5723(19) 0.365(3) 0.020(5) 1.0000 Uiso D U H61 H 0.330(3) 0.571(2) 0.284(4) 0.035(5) 1.0000 Uiso D U H31 H 0.0009 0.6218 0.0999 0.0452 1.0000 Uiso . . H32 H -0.1179 0.6051 0.1251 0.0452 1.0000 Uiso . . H41 H 0.0549 0.6451 0.2648 0.0470 1.0000 Uiso . . H42 H -0.0048 0.5923 0.2916 0.0470 1.0000 Uiso . . H71 H 0.1796 0.6332 0.1297 0.0394 1.0000 Uiso . . H72 H 0.3071 0.6066 0.1343 0.0394 1.0000 Uiso . . H81 H 0.1083 0.5859 -0.0111 0.0352 1.0000 Uiso . . H82 H 0.2133 0.5409 0.0324 0.0352 1.0000 Uiso . . H101 H 0.3442 0.4213 0.5415 0.0245 1.0000 Uiso . . H111 H 0.3161 0.3374 0.5975 0.0328 1.0000 Uiso . . H131 H 0.2760 0.2427 0.5643 0.0423 1.0000 Uiso . . H141 H 0.2460 0.1698 0.4562 0.0432 1.0000 Uiso . . H151 H 0.2397 0.1810 0.2894 0.0342 1.0000 Uiso . . H161 H 0.2762 0.2629 0.2311 0.0272 1.0000 Uiso . . H211 H 0.5148 0.3154 0.3450 0.0280 1.0000 Uiso . . H221 H 0.6809 0.2883 0.3039 0.0342 1.0000 Uiso . . H231 H 0.6782 0.2998 0.1359 0.0361 1.0000 Uiso . . H241 H 0.5128 0.3430 0.0139 0.0338 1.0000 Uiso . . H261 H 0.3158 0.3915 -0.0335 0.0276 1.0000 Uiso . . H271 H 0.1500 0.4201 0.0057 0.0260 1.0000 Uiso . . H301 H 0.3512 0.4989 0.1629 0.0346 1.0000 Uiso . . H311 H 0.5143 0.4968 0.1030 0.0484 1.0000 Uiso . . H321 H 0.7067 0.4611 0.2073 0.0617 1.0000 Uiso . . H331 H 0.7385 0.4309 0.3715 0.0440 1.0000 Uiso . . H341 H 0.5766 0.4327 0.4329 0.0305 1.0000 Uiso . . H361 H 0.5403 0.5321 0.4521 0.0353 1.0000 Uiso . . H371 H 0.5955 0.5895 0.5949 0.0464 1.0000 Uiso . . H381 H 0.4675 0.5991 0.6877 0.0397 1.0000 Uiso . . H391 H 0.2795 0.5508 0.6384 0.0389 1.0000 Uiso . . H401 H 0.2224 0.4947 0.4952 0.0338 1.0000 Uiso . . H421 H 0.0650 0.4347 0.3700 0.0309 1.0000 Uiso . . H431 H -0.0128 0.3861 0.4754 0.0400 1.0000 Uiso . . H441 H -0.0810 0.2987 0.4329 0.0424 1.0000 Uiso . . H451 H -0.0668 0.2580 0.2859 0.0362 1.0000 Uiso . . H461 H 0.0052 0.3075 0.1781 0.0302 1.0000 Uiso . . H481 H -0.1535 0.4395 0.1485 0.0316 1.0000 Uiso . . H491 H -0.3507 0.4251 0.0224 0.0365 1.0000 Uiso . . H501 H -0.3711 0.3849 -0.1329 0.0306 1.0000 Uiso . . H511 H -0.1948 0.3556 -0.1594 0.0333 1.0000 Uiso . . H521 H 0.0019 0.3690 -0.0342 0.0268 1.0000 Uiso . . H541 H -0.0235 0.6153 0.7409 0.0342 1.0000 Uiso . . H551 H -0.0248 0.6915 0.8333 0.0412 1.0000 Uiso . . H571 H 0.0843 0.7495 0.9781 0.0457 1.0000 Uiso . . H581 H 0.2628 0.7742 1.1141 0.0511 1.0000 Uiso . . H591 H 0.4486 0.7277 1.1439 0.0420 1.0000 Uiso . . H601 H 0.4577 0.6587 1.0381 0.0346 1.0000 Uiso . . H651 H 0.4211 0.6947 0.8509 0.0315 1.0000 Uiso . . H661 H 0.6008 0.7385 0.8649 0.0373 1.0000 Uiso . . H671 H 0.7870 0.6906 0.9002 0.0411 1.0000 Uiso . . H681 H 0.7897 0.5988 0.9144 0.0345 1.0000 Uiso . . H701 H 0.6809 0.5153 0.9156 0.0331 1.0000 Uiso . . H711 H 0.5022 0.4704 0.9034 0.0288 1.0000 Uiso . . H741 H 0.3819 0.4174 0.7515 0.0311 1.0000 Uiso . . H751 H 0.4164 0.3271 0.7935 0.0314 1.0000 Uiso . . H771 H 0.3494 0.2445 0.8477 0.0409 1.0000 Uiso . . H781 H 0.2005 0.1946 0.8788 0.0486 1.0000 Uiso . . H791 H 0.0098 0.2346 0.8658 0.0399 1.0000 Uiso . . H801 H -0.0322 0.3224 0.8104 0.0313 1.0000 Uiso . . H851 H -0.0592 0.3351 0.6132 0.0360 1.0000 Uiso . . H861 H -0.2488 0.2975 0.5206 0.0399 1.0000 Uiso . . H871 H -0.4326 0.3329 0.5312 0.0417 1.0000 Uiso . . H881 H -0.4244 0.4125 0.6203 0.0396 1.0000 Uiso . . H901 H -0.3053 0.4852 0.7252 0.0383 1.0000 Uiso . . H911 H -0.1138 0.5247 0.8159 0.0318 1.0000 Uiso . . H931 H -0.0018 0.6791 0.5904 0.1551 1.0000 Uiso . . H932 H 0.0408 0.6290 0.5408 0.1551 1.0000 Uiso . . H941 H 0.2511 0.6881 0.4368 0.1062 1.0000 Uiso . . H942 H 0.3558 0.6475 0.4325 0.1062 1.0000 Uiso . . H951 H 0.7717 0.6205 0.3195 0.0736 1.0000 Uiso . . H952 H 0.6945 0.5664 0.3095 0.0736 1.0000 Uiso . . H961 H 0.9980 0.5228 0.6090 0.0433 1.0000 Uiso . . H962 H 0.8919 0.4804 0.5500 0.0433 1.0000 Uiso . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02244(17) 0.01604(16) 0.01854(16) 0.00092(18) 0.00819(13) 0.00138(19) C1 0.041(3) 0.014(3) 0.028(3) 0.003(2) 0.006(2) -0.002(2) C2 0.024(3) 0.028(3) 0.028(3) 0.002(2) 0.006(2) 0.004(2) C3 0.040(3) 0.031(3) 0.042(3) 0.002(3) 0.012(3) 0.016(3) C4 0.050(4) 0.028(3) 0.039(4) 0.005(3) 0.023(3) 0.009(3) C5 0.046(3) 0.021(3) 0.021(3) -0.001(2) 0.008(2) 0.003(2) C6 0.038(3) 0.022(3) 0.029(3) -0.001(2) 0.010(2) -0.002(2) C7 0.041(3) 0.027(3) 0.030(3) 0.007(2) 0.014(3) -0.007(3) C8 0.040(3) 0.025(3) 0.023(3) 0.002(2) 0.012(2) 0.000(2) P1 0.0172(6) 0.0194(6) 0.0171(6) 0.0011(5) 0.0070(5) 0.0010(5) P2 0.0204(6) 0.0184(6) 0.0170(6) -0.0013(5) 0.0090(5) -0.0014(5) C9 0.012(2) 0.018(2) 0.023(2) -0.0012(19) 0.0076(18) -0.0031(17) C10 0.025(2) 0.021(2) 0.015(2) -0.0015(19) 0.0099(19) 0.0006(19) C11 0.032(3) 0.033(3) 0.017(2) 0.002(2) 0.012(2) -0.004(2) C12 0.028(3) 0.019(2) 0.025(3) 0.003(2) 0.011(2) -0.003(2) C13 0.053(4) 0.030(3) 0.023(3) 0.002(2) 0.016(3) -0.009(3) C14 0.050(4) 0.020(3) 0.037(3) 0.007(2) 0.015(3) -0.009(3) C15 0.038(3) 0.020(3) 0.027(3) -0.003(2) 0.010(2) -0.006(2) C16 0.022(2) 0.022(3) 0.023(3) -0.002(2) 0.005(2) -0.001(2) C17 0.016(2) 0.026(2) 0.012(2) -0.0007(19) 0.0041(18) 0.0019(19) C18 0.016(2) 0.023(2) 0.016(2) 0.0023(19) 0.0049(18) 0.0004(19) C19 0.022(2) 0.016(2) 0.016(2) -0.0007(18) 0.0105(19) -0.0050(18) C20 0.014(2) 0.015(2) 0.024(2) -0.0061(19) 0.0049(18) -0.0017(17) C21 0.023(2) 0.025(3) 0.022(3) -0.003(2) 0.006(2) 0.000(2) C22 0.023(3) 0.030(3) 0.033(3) 0.001(2) 0.010(2) 0.001(2) C23 0.022(3) 0.027(3) 0.040(3) -0.003(2) 0.016(2) 0.004(2) C24 0.026(3) 0.030(3) 0.028(3) -0.002(2) 0.019(2) -0.001(2) C25 0.023(2) 0.018(2) 0.022(2) -0.0047(19) 0.0108(19) -0.0033(19) C26 0.028(3) 0.021(2) 0.021(2) -0.004(2) 0.016(2) -0.004(2) C27 0.022(2) 0.026(3) 0.018(2) 0.001(2) 0.0063(19) -0.004(2) C28 0.016(2) 0.016(2) 0.019(2) -0.0060(19) 0.0064(19) -0.0035(18) C29 0.023(2) 0.018(2) 0.025(3) -0.007(2) 0.0119(19) -0.0099(19) C30 0.038(3) 0.025(3) 0.024(2) -0.0014(19) 0.020(2) -0.003(2) C31 0.046(3) 0.036(3) 0.038(3) -0.003(2) 0.030(3) -0.010(2) C32 0.040(4) 0.057(4) 0.058(4) -0.018(3) 0.039(3) -0.011(3) C33 0.026(3) 0.035(3) 0.050(4) -0.012(3) 0.015(3) -0.003(2) C34 0.026(3) 0.023(3) 0.028(3) -0.006(2) 0.012(2) -0.004(2) C35 0.0172(19) 0.019(3) 0.0151(19) 0.0018(19) 0.0057(15) 0.0028(19) C36 0.027(3) 0.034(3) 0.028(3) -0.007(2) 0.011(2) -0.002(2) C37 0.032(3) 0.048(4) 0.035(3) -0.022(3) 0.010(3) -0.014(3) C38 0.043(3) 0.036(3) 0.020(3) -0.007(2) 0.010(2) 0.002(3) C39 0.040(3) 0.034(3) 0.023(3) -0.002(2) 0.015(2) 0.004(2) C40 0.030(3) 0.027(3) 0.027(3) 0.001(2) 0.012(2) 0.004(2) C41 0.017(2) 0.021(3) 0.019(2) 0.001(2) 0.0056(19) 0.0031(19) C42 0.023(2) 0.027(3) 0.028(3) 0.000(2) 0.012(2) 0.000(2) C43 0.030(3) 0.037(3) 0.033(3) 0.001(2) 0.021(2) -0.003(2) C44 0.031(3) 0.029(3) 0.046(3) 0.011(3) 0.023(3) 0.001(2) C45 0.032(3) 0.026(3) 0.033(3) 0.004(2) 0.012(2) -0.003(2) C46 0.025(3) 0.026(3) 0.025(3) 0.000(2) 0.006(2) -0.005(2) C47 0.021(2) 0.025(3) 0.014(2) 0.002(2) 0.0040(18) 0.004(2) C48 0.028(3) 0.028(3) 0.023(3) -0.002(2) 0.011(2) 0.007(2) C49 0.022(2) 0.029(3) 0.040(3) 0.009(2) 0.010(2) 0.006(2) C50 0.024(3) 0.026(3) 0.027(3) -0.001(2) -0.003(2) -0.006(2) C51 0.029(3) 0.031(3) 0.024(3) -0.002(2) 0.011(2) -0.005(2) C52 0.023(2) 0.022(2) 0.022(3) 0.004(2) 0.008(2) 0.000(2) B1 0.024(2) 0.027(3) 0.023(2) -0.001(3) 0.008(2) -0.001(3) O1 0.0295(19) 0.0187(17) 0.0217(18) 0.0024(14) 0.0072(15) 0.0014(15) O2 0.0280(16) 0.0180(19) 0.0218(16) 0.0023(14) 0.0079(13) -0.0015(14) O3 0.0306(18) 0.0206(18) 0.0216(17) 0.0009(14) 0.0143(14) -0.0028(15) O4 0.0268(16) 0.026(2) 0.0220(16) -0.0024(14) 0.0099(13) -0.0037(14) C53 0.024(3) 0.025(3) 0.022(3) 0.005(2) 0.010(2) -0.003(2) C54 0.021(2) 0.034(3) 0.030(3) 0.010(2) 0.010(2) 0.001(2) C55 0.030(3) 0.035(3) 0.038(3) 0.008(3) 0.015(3) 0.012(2) C56 0.040(3) 0.019(2) 0.034(3) 0.007(2) 0.020(3) 0.008(2) C57 0.049(4) 0.024(3) 0.042(3) 0.005(2) 0.022(3) 0.010(2) C58 0.059(4) 0.026(3) 0.042(3) -0.005(3) 0.028(3) 0.005(3) C59 0.036(3) 0.031(3) 0.038(3) -0.004(2) 0.019(3) -0.009(2) C60 0.038(3) 0.019(3) 0.030(3) 0.000(2) 0.013(2) -0.005(2) C61 0.028(3) 0.019(2) 0.021(2) 0.004(2) 0.011(2) 0.001(2) C62 0.028(3) 0.023(3) 0.016(2) 0.0037(19) 0.010(2) 0.003(2) C63 0.024(2) 0.023(2) 0.018(2) 0.002(2) 0.0092(19) 0.003(2) C64 0.021(2) 0.025(3) 0.023(3) 0.001(2) 0.010(2) 0.0000(19) C65 0.027(3) 0.023(3) 0.028(3) 0.006(2) 0.014(2) 0.003(2) C66 0.032(3) 0.029(3) 0.032(3) 0.010(2) 0.014(2) -0.004(2) C67 0.029(3) 0.040(3) 0.034(3) -0.002(3) 0.012(2) -0.006(2) C68 0.028(3) 0.033(3) 0.025(3) -0.002(2) 0.010(2) -0.004(2) C69 0.027(3) 0.033(3) 0.014(2) -0.004(2) 0.004(2) 0.000(2) C70 0.030(3) 0.028(3) 0.025(3) 0.002(2) 0.010(2) 0.009(2) C71 0.028(2) 0.023(3) 0.021(2) 0.001(2) 0.0050(18) -0.002(2) C72 0.023(2) 0.021(2) 0.015(2) 0.0020(18) 0.0031(19) 0.0025(19) C73 0.034(3) 0.024(3) 0.014(2) -0.005(2) 0.012(2) -0.004(2) C74 0.021(2) 0.037(3) 0.020(2) -0.006(2) 0.013(2) -0.004(2) C75 0.022(3) 0.030(3) 0.027(3) -0.006(2) 0.006(2) 0.004(2) C76 0.031(3) 0.024(3) 0.018(2) -0.002(2) 0.005(2) 0.001(2) C77 0.030(3) 0.032(3) 0.040(3) -0.002(2) 0.012(2) 0.005(2) C78 0.049(4) 0.026(3) 0.046(4) 0.007(3) 0.018(3) 0.010(3) C79 0.032(3) 0.032(3) 0.036(3) -0.004(2) 0.014(2) -0.013(2) C80 0.032(3) 0.028(3) 0.018(3) 0.005(2) 0.010(2) 0.004(2) C81 0.029(3) 0.021(2) 0.014(2) -0.0037(19) 0.008(2) -0.005(2) C82 0.020(2) 0.024(2) 0.020(2) -0.003(2) 0.011(2) -0.002(2) C83 0.023(2) 0.021(2) 0.019(2) 0.0038(19) 0.0082(19) -0.0025(19) C84 0.024(2) 0.027(3) 0.023(3) 0.000(2) 0.009(2) -0.004(2) C85 0.028(3) 0.036(3) 0.026(3) 0.002(2) 0.011(2) -0.001(2) C86 0.038(3) 0.038(3) 0.024(3) -0.006(2) 0.009(2) -0.012(3) C87 0.029(3) 0.051(4) 0.024(3) 0.001(3) 0.000(2) -0.011(3) C88 0.024(3) 0.048(3) 0.027(3) 0.005(3) 0.005(2) 0.002(2) C89 0.030(3) 0.030(3) 0.019(2) 0.006(2) 0.006(2) 0.001(2) C90 0.031(3) 0.030(3) 0.035(3) 0.009(2) 0.014(2) 0.011(2) C91 0.034(3) 0.020(3) 0.025(2) -0.002(2) 0.010(2) -0.002(2) C92 0.023(3) 0.024(2) 0.020(2) 0.006(2) 0.0082(19) 0.002(2) C93 0.193(13) 0.105(8) 0.090(8) -0.045(6) 0.072(8) -0.100(9) Cl1 0.0884(17) 0.145(3) 0.0969(19) -0.0692(18) 0.0473(15) -0.0201(17) Cl2 0.1004(17) 0.0550(11) 0.0968(17) 0.0024(11) 0.0554(14) 0.0073(11) C94 0.121(8) 0.084(6) 0.061(6) -0.019(5) 0.037(6) -0.042(6) Cl3 0.157(3) 0.0735(15) 0.0813(16) -0.0095(13) 0.0583(18) -0.0080(16) Cl4 0.0628(12) 0.0608(12) 0.0897(16) -0.0119(11) 0.0068(11) -0.0031(10) C95 0.069(5) 0.070(5) 0.045(4) -0.004(4) -0.005(4) 0.020(4) Cl5 0.0736(13) 0.0725(13) 0.0624(12) -0.0018(10) 0.0174(10) 0.0103(11) Cl6 0.0552(10) 0.0603(11) 0.0578(11) 0.0102(9) 0.0205(8) -0.0035(8) C96 0.034(3) 0.037(3) 0.037(3) 0.008(2) 0.011(2) 0.005(2) Cl7 0.0403(8) 0.0491(9) 0.0456(9) 0.0013(7) 0.0189(7) 0.0086(7) Cl8 0.0455(9) 0.0585(9) 0.0458(9) -0.0018(7) 0.0217(7) 0.0124(7) _refine_ls_extinction_method None 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 Rh1 . C1 . 2.218(5) yes Rh1 . C2 . 2.265(5) yes Rh1 . C5 . 2.237(5) yes Rh1 . C6 . 2.254(5) yes Rh1 . P1 . 2.2893(12) yes Rh1 . P2 . 2.3365(13) yes C1 . C2 . 1.359(8) yes C1 . C8 . 1.497(8) yes C1 . H11 . 0.97(3) no C2 . C3 . 1.513(8) yes C2 . H21 . 0.93(3) no C3 . C4 . 1.534(9) yes C3 . H31 . 1.000 no C3 . H32 . 1.000 no C4 . C5 . 1.499(8) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no C5 . C6 . 1.382(8) yes C5 . H51 . 1.02(3) no C6 . C7 . 1.508(8) yes C6 . H61 . 0.98(3) no C7 . C8 . 1.548(8) yes C7 . H71 . 1.000 no C7 . H72 . 1.000 no C8 . H81 . 1.000 no C8 . H82 . 1.000 no P1 . C28 . 1.825(5) yes P1 . C41 . 1.825(5) yes P1 . C47 . 1.839(5) yes P2 . C9 . 1.840(5) yes P2 . C29 . 1.812(5) yes P2 . C35 . 1.834(4) yes C9 . C10 . 1.418(6) yes C9 . C18 . 1.403(7) yes C10 . C11 . 1.375(7) yes C10 . H101 . 1.000 no C11 . C12 . 1.425(7) yes C11 . H111 . 1.000 no C12 . C13 . 1.397(7) yes C12 . C17 . 1.426(7) yes C13 . C14 . 1.364(8) yes C13 . H131 . 1.000 no C14 . C15 . 1.391(8) yes C14 . H141 . 1.000 no C15 . C16 . 1.363(7) yes C15 . H151 . 1.000 no C16 . C17 . 1.443(7) yes C16 . H161 . 1.000 no C17 . C18 . 1.429(7) yes C18 . C19 . 1.504(6) yes C19 . C20 . 1.438(6) yes C19 . C28 . 1.391(7) yes C20 . C21 . 1.421(7) yes C20 . C25 . 1.416(7) yes C21 . C22 . 1.371(7) yes C21 . H211 . 1.000 no C22 . C23 . 1.411(8) yes C22 . H221 . 1.000 no C23 . C24 . 1.359(7) yes C23 . H231 . 1.000 no C24 . C25 . 1.424(7) yes C24 . H241 . 1.000 no C25 . C26 . 1.418(7) yes C26 . C27 . 1.363(7) yes C26 . H261 . 1.000 no C27 . C28 . 1.419(7) yes C27 . H271 . 1.000 no C29 . C30 . 1.402(7) yes C29 . C34 . 1.397(7) yes C30 . C31 . 1.389(7) yes C30 . H301 . 1.000 no C31 . C32 . 1.385(9) yes C31 . H311 . 1.000 no C32 . C33 . 1.373(9) yes C32 . H321 . 1.000 no C33 . C34 . 1.392(8) yes C33 . H331 . 1.000 no C34 . H341 . 1.000 no C35 . C36 . 1.389(7) yes C35 . C40 . 1.404(6) yes C36 . C37 . 1.401(8) yes C36 . H361 . 1.000 no C37 . C38 . 1.377(8) yes C37 . H371 . 1.000 no C38 . C39 . 1.398(8) yes C38 . H381 . 1.000 no C39 . C40 . 1.385(7) yes C39 . H391 . 1.000 no C40 . H401 . 1.000 no C41 . C42 . 1.371(7) yes C41 . C46 . 1.418(7) yes C42 . C43 . 1.394(7) yes C42 . H421 . 1.000 no C43 . C44 . 1.376(8) yes C43 . H431 . 1.000 no C44 . C45 . 1.406(8) yes C44 . H441 . 1.000 no C45 . C46 . 1.382(7) yes C45 . H451 . 1.000 no C46 . H461 . 1.000 no C47 . C48 . 1.404(7) yes C47 . C52 . 1.376(7) yes C48 . C49 . 1.388(7) yes C48 . H481 . 1.000 no C49 . C50 . 1.375(8) yes C49 . H491 . 1.000 no C50 . C51 . 1.377(8) yes C50 . H501 . 1.000 no C51 . C52 . 1.382(7) yes C51 . H511 . 1.000 no C52 . H521 . 1.000 no B1 . O1 . 1.479(7) yes B1 . O2 . 1.472(6) yes B1 . O3 . 1.463(7) yes B1 . O4 . 1.463(6) yes O1 . C53 . 1.361(6) yes O2 . C72 . 1.358(6) yes O3 . C73 . 1.360(6) yes O4 . C92 . 1.354(6) yes C53 . C54 . 1.411(7) yes C53 . C62 . 1.390(7) yes C54 . C55 . 1.365(8) yes C54 . H541 . 1.000 no C55 . C56 . 1.421(8) yes C55 . H551 . 1.000 no C56 . C57 . 1.411(8) yes C56 . C61 . 1.426(7) yes C57 . C58 . 1.365(9) yes C57 . H571 . 1.000 no C58 . C59 . 1.395(8) yes C58 . H581 . 1.000 no C59 . C60 . 1.368(8) yes C59 . H591 . 1.000 no C60 . C61 . 1.424(7) yes C60 . H601 . 1.000 no C61 . C62 . 1.437(7) yes C62 . C63 . 1.501(7) yes C63 . C64 . 1.431(7) yes C63 . C72 . 1.377(7) yes C64 . C65 . 1.423(7) yes C64 . C69 . 1.431(7) yes C65 . C66 . 1.361(7) yes C65 . H651 . 1.000 no C66 . C67 . 1.408(8) yes C66 . H661 . 1.000 no C67 . C68 . 1.358(8) yes C67 . H671 . 1.000 no C68 . C69 . 1.435(8) yes C68 . H681 . 1.000 no C69 . C70 . 1.413(7) yes C70 . C71 . 1.359(7) yes C70 . H701 . 1.000 no C71 . C72 . 1.421(7) yes C71 . H711 . 1.000 no C73 . C74 . 1.413(7) yes C73 . C82 . 1.388(7) yes C74 . C75 . 1.381(7) yes C74 . H741 . 1.000 no C75 . C76 . 1.423(7) yes C75 . H751 . 1.000 no C76 . C77 . 1.420(7) yes C76 . C81 . 1.427(7) yes C77 . C78 . 1.356(8) yes C77 . H771 . 1.000 no C78 . C79 . 1.416(8) yes C78 . H781 . 1.000 no C79 . C80 . 1.382(8) yes C79 . H791 . 1.000 no C80 . C81 . 1.419(7) yes C80 . H801 . 1.000 no C81 . C82 . 1.429(7) yes C82 . C83 . 1.494(7) yes C83 . C84 . 1.446(7) yes C83 . C92 . 1.379(7) yes C84 . C85 . 1.441(7) yes C84 . C89 . 1.404(7) yes C85 . C86 . 1.357(7) yes C85 . H851 . 1.000 no C86 . C87 . 1.412(8) yes C86 . H861 . 1.000 no C87 . C88 . 1.382(9) yes C87 . H871 . 1.000 no C88 . C89 . 1.425(7) yes C88 . H881 . 1.000 no C89 . C90 . 1.414(8) yes C90 . C91 . 1.377(7) yes C90 . H901 . 1.000 no C91 . C92 . 1.406(7) yes C91 . H911 . 1.000 no C93 . Cl1 . 1.713(13) yes C93 . Cl2 . 1.737(13) yes C93 . H931 . 1.000 no C93 . H932 . 1.000 no C94 . Cl3 . 1.712(10) yes C94 . Cl4 . 1.728(9) yes C94 . H941 . 1.000 no C94 . H942 . 1.000 no C95 . Cl5 . 1.752(9) yes C95 . Cl6 . 1.756(8) yes C95 . H951 . 1.000 no C95 . H952 . 1.000 no C96 . Cl7 . 1.761(6) yes C96 . Cl8 . 1.774(6) yes C96 . H961 . 1.000 no C96 . H962 . 1.000 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 C1 . Rh1 . C2 . 35.3(2) yes C1 . Rh1 . C5 . 93.95(19) yes C2 . Rh1 . C5 . 78.3(2) yes C1 . Rh1 . C6 . 80.46(19) yes C2 . Rh1 . C6 . 86.0(2) yes C5 . Rh1 . C6 . 35.8(2) yes C1 . Rh1 . P1 . 91.52(13) yes C2 . Rh1 . P1 . 97.48(14) yes C5 . Rh1 . P1 . 163.28(15) yes C6 . Rh1 . P1 . 160.82(15) yes C1 . Rh1 . P2 . 144.66(15) yes C2 . Rh1 . P2 . 173.71(14) yes C5 . Rh1 . P2 . 95.77(14) yes C6 . Rh1 . P2 . 87.88(15) yes P1 . Rh1 . P2 . 88.80(4) yes Rh1 . C1 . C2 . 74.3(3) yes Rh1 . C1 . C8 . 107.5(3) yes C2 . C1 . C8 . 126.4(5) yes Rh1 . C1 . H11 . 99(3) no C2 . C1 . H11 . 116(3) no C8 . C1 . H11 . 116(3) no Rh1 . C2 . C1 . 70.5(3) yes Rh1 . C2 . C3 . 113.3(4) yes C1 . C2 . C3 . 122.0(5) yes Rh1 . C2 . H21 . 108(3) no C1 . C2 . H21 . 122(3) no C3 . C2 . H21 . 112(3) no C2 . C3 . C4 . 110.4(5) yes C2 . C3 . H31 . 109.237 no C4 . C3 . H31 . 109.237 no C2 . C3 . H32 . 109.237 no C4 . C3 . H32 . 109.237 no H31 . C3 . H32 . 109.466 no C3 . C4 . C5 . 113.8(5) yes C3 . C4 . H41 . 108.368 no C5 . C4 . H41 . 108.368 no C3 . C4 . H42 . 108.368 no C5 . C4 . H42 . 108.368 no H41 . C4 . H42 . 109.467 no Rh1 . C5 . C4 . 108.5(4) yes Rh1 . C5 . C6 . 72.7(3) yes C4 . C5 . C6 . 126.4(5) yes Rh1 . C5 . H51 . 100(3) no C4 . C5 . H51 . 119(3) no C6 . C5 . H51 . 113(3) no Rh1 . C6 . C5 . 71.4(3) yes Rh1 . C6 . C7 . 110.6(4) yes C5 . C6 . C7 . 126.6(5) yes Rh1 . C6 . H61 . 106(3) no C5 . C6 . H61 . 114(3) no C7 . C6 . H61 . 116(3) no C6 . C7 . C8 . 114.5(4) yes C6 . C7 . H71 . 108.209 no C8 . C7 . H71 . 108.209 no C6 . C7 . H72 . 108.209 no C8 . C7 . H72 . 108.208 no H71 . C7 . H72 . 109.466 no C1 . C8 . C7 . 114.8(4) yes C1 . C8 . H81 . 108.117 no C7 . C8 . H81 . 108.116 no C1 . C8 . H82 . 108.116 no C7 . C8 . H82 . 108.116 no H81 . C8 . H82 . 109.467 no Rh1 . P1 . C28 . 103.87(15) yes Rh1 . P1 . C41 . 117.62(16) yes C28 . P1 . C41 . 111.4(2) yes Rh1 . P1 . C47 . 118.97(16) yes C28 . P1 . C47 . 107.9(2) yes C41 . P1 . C47 . 97.0(2) yes Rh1 . P2 . C9 . 120.10(15) yes Rh1 . P2 . C29 . 110.88(17) yes C9 . P2 . C29 . 102.9(2) yes Rh1 . P2 . C35 . 112.14(14) yes C9 . P2 . C35 . 104.4(2) yes C29 . P2 . C35 . 105.0(2) yes P2 . C9 . C10 . 120.0(3) yes P2 . C9 . C18 . 120.8(3) yes C10 . C9 . C18 . 118.8(4) yes C9 . C10 . C11 . 121.8(4) yes C9 . C10 . H101 . 119.097 no C11 . C10 . H101 . 119.096 no C10 . C11 . C12 . 120.9(4) yes C10 . C11 . H111 . 119.561 no C12 . C11 . H111 . 119.561 no C11 . C12 . C13 . 121.6(5) yes C11 . C12 . C17 . 118.0(4) yes C13 . C12 . C17 . 120.4(5) yes C12 . C13 . C14 . 120.7(5) yes C12 . C13 . H131 . 119.652 no C14 . C13 . H131 . 119.652 no C13 . C14 . C15 . 119.9(5) yes C13 . C14 . H141 . 120.039 no C15 . C14 . H141 . 120.039 no C14 . C15 . C16 . 122.1(5) yes C14 . C15 . H151 . 118.953 no C16 . C15 . H151 . 118.953 no C15 . C16 . C17 . 119.6(5) yes C15 . C16 . H161 . 120.219 no C17 . C16 . H161 . 120.218 no C12 . C17 . C16 . 117.3(4) yes C12 . C17 . C18 . 120.4(4) yes C16 . C17 . C18 . 122.3(4) yes C9 . C18 . C17 . 120.0(4) yes C9 . C18 . C19 . 120.7(4) yes C17 . C18 . C19 . 119.3(4) yes C18 . C19 . C20 . 119.1(4) yes C18 . C19 . C28 . 121.7(4) yes C20 . C19 . C28 . 119.1(4) yes C19 . C20 . C21 . 122.0(4) yes C19 . C20 . C25 . 119.9(4) yes C21 . C20 . C25 . 118.0(4) yes C20 . C21 . C22 . 120.9(5) yes C20 . C21 . H211 . 119.530 no C22 . C21 . H211 . 119.530 no C21 . C22 . C23 . 121.0(5) yes C21 . C22 . H221 . 119.509 no C23 . C22 . H221 . 119.509 no C22 . C23 . C24 . 119.2(4) yes C22 . C23 . H231 . 120.400 no C24 . C23 . H231 . 120.400 no C23 . C24 . C25 . 121.6(5) yes C23 . C24 . H241 . 119.217 no C25 . C24 . H241 . 119.217 no C20 . C25 . C24 . 119.3(4) yes C20 . C25 . C26 . 118.7(4) yes C24 . C25 . C26 . 122.0(4) yes C25 . C26 . C27 . 121.1(4) yes C25 . C26 . H261 . 119.438 no C27 . C26 . H261 . 119.438 no C26 . C27 . C28 . 120.7(4) yes C26 . C27 . H271 . 119.629 no C28 . C27 . H271 . 119.629 no P1 . C28 . C19 . 121.5(4) yes P1 . C28 . C27 . 117.4(4) yes C19 . C28 . C27 . 120.0(4) yes P2 . C29 . C30 . 121.0(4) yes P2 . C29 . C34 . 120.7(4) yes C30 . C29 . C34 . 118.3(4) yes C29 . C30 . C31 . 121.1(5) yes C29 . C30 . H301 . 119.435 no C31 . C30 . H301 . 119.435 no C30 . C31 . C32 . 119.3(5) yes C30 . C31 . H311 . 120.331 no C32 . C31 . H311 . 120.330 no C31 . C32 . C33 . 120.5(5) yes C31 . C32 . H321 . 119.763 no C33 . C32 . H321 . 119.763 no C32 . C33 . C34 . 120.6(5) yes C32 . C33 . H331 . 119.714 no C34 . C33 . H331 . 119.716 no C29 . C34 . C33 . 120.2(5) yes C29 . C34 . H341 . 119.911 no C33 . C34 . H341 . 119.911 no P2 . C35 . C36 . 121.9(3) yes P2 . C35 . C40 . 118.8(3) yes C36 . C35 . C40 . 119.0(4) yes C35 . C36 . C37 . 119.5(5) yes C35 . C36 . H361 . 120.241 no C37 . C36 . H361 . 120.241 no C36 . C37 . C38 . 121.2(5) yes C36 . C37 . H371 . 119.411 no C38 . C37 . H371 . 119.410 no C37 . C38 . C39 . 119.7(5) yes C37 . C38 . H381 . 120.153 no C39 . C38 . H381 . 120.153 no C38 . C39 . C40 . 119.4(5) yes C38 . C39 . H391 . 120.317 no C40 . C39 . H391 . 120.316 no C35 . C40 . C39 . 121.3(5) yes C35 . C40 . H401 . 119.370 no C39 . C40 . H401 . 119.370 no P1 . C41 . C42 . 120.2(4) yes P1 . C41 . C46 . 120.2(4) yes C42 . C41 . C46 . 118.9(5) yes C41 . C42 . C43 . 121.1(5) yes C41 . C42 . H421 . 119.434 no C43 . C42 . H421 . 119.433 no C42 . C43 . C44 . 119.9(5) yes C42 . C43 . H431 . 120.025 no C44 . C43 . H431 . 120.025 no C43 . C44 . C45 . 120.2(5) yes C43 . C44 . H441 . 119.917 no C45 . C44 . H441 . 119.917 no C44 . C45 . C46 . 119.5(5) yes C44 . C45 . H451 . 120.232 no C46 . C45 . H451 . 120.231 no C41 . C46 . C45 . 120.2(5) yes C41 . C46 . H461 . 119.881 no C45 . C46 . H461 . 119.881 no P1 . C47 . C48 . 112.9(3) yes P1 . C47 . C52 . 128.6(4) yes C48 . C47 . C52 . 118.4(4) yes C47 . C48 . C49 . 120.3(5) yes C47 . C48 . H481 . 119.862 no C49 . C48 . H481 . 119.862 no C48 . C49 . C50 . 120.2(5) yes C48 . C49 . H491 . 119.887 no C50 . C49 . H491 . 119.887 no C49 . C50 . C51 . 119.7(5) yes C49 . C50 . H501 . 120.161 no C51 . C50 . H501 . 120.160 no C50 . C51 . C52 . 120.4(5) yes C50 . C51 . H511 . 119.781 no C52 . C51 . H511 . 119.781 no C47 . C52 . C51 . 121.0(5) yes C47 . C52 . H521 . 119.511 no C51 . C52 . H521 . 119.510 no O1 . B1 . O2 . 111.6(4) yes O1 . B1 . O3 . 102.3(4) yes O2 . B1 . O3 . 113.7(4) yes O1 . B1 . O4 . 113.9(4) yes O2 . B1 . O4 . 102.8(4) yes O3 . B1 . O4 . 113.0(4) yes B1 . O1 . C53 . 117.6(4) yes B1 . O2 . C72 . 120.0(4) yes B1 . O3 . C73 . 115.7(4) yes B1 . O4 . C92 . 120.2(4) yes O1 . C53 . C54 . 117.5(4) yes O1 . C53 . C62 . 121.8(4) yes C54 . C53 . C62 . 120.6(5) yes C53 . C54 . C55 . 121.9(5) yes C53 . C54 . H541 . 119.049 no C55 . C54 . H541 . 119.049 no C54 . C55 . C56 . 119.3(5) yes C54 . C55 . H551 . 120.333 no C56 . C55 . H551 . 120.334 no C55 . C56 . C57 . 121.0(5) yes C55 . C56 . C61 . 119.6(5) yes C57 . C56 . C61 . 119.4(5) yes C56 . C57 . C58 . 121.7(5) yes C56 . C57 . H571 . 119.131 no C58 . C57 . H571 . 119.132 no C57 . C58 . C59 . 119.0(5) yes C57 . C58 . H581 . 120.495 no C59 . C58 . H581 . 120.494 no C58 . C59 . C60 . 121.5(5) yes C58 . C59 . H591 . 119.228 no C60 . C59 . H591 . 119.228 no C59 . C60 . C61 . 120.9(5) yes C59 . C60 . H601 . 119.544 no C61 . C60 . H601 . 119.543 no C56 . C61 . C60 . 117.4(5) yes C56 . C61 . C62 . 119.8(4) yes C60 . C61 . C62 . 122.6(4) yes C53 . C62 . C61 . 118.2(4) yes C53 . C62 . C63 . 119.3(4) yes C61 . C62 . C63 . 122.4(4) yes C62 . C63 . C64 . 122.7(4) yes C62 . C63 . C72 . 118.7(4) yes C64 . C63 . C72 . 118.6(4) yes C63 . C64 . C65 . 123.7(4) yes C63 . C64 . C69 . 119.4(4) yes C65 . C64 . C69 . 116.9(4) yes C64 . C65 . C66 . 122.3(5) yes C64 . C65 . H651 . 118.854 no C66 . C65 . H651 . 118.854 no C65 . C66 . C67 . 120.1(5) yes C65 . C66 . H661 . 119.950 no C67 . C66 . H661 . 119.950 no C66 . C67 . C68 . 120.6(5) yes C66 . C67 . H671 . 119.678 no C68 . C67 . H671 . 119.678 no C67 . C68 . C69 . 120.4(5) yes C67 . C68 . H681 . 119.806 no C69 . C68 . H681 . 119.805 no C64 . C69 . C68 . 119.5(5) yes C64 . C69 . C70 . 119.3(5) yes C68 . C69 . C70 . 121.2(5) yes C69 . C70 . C71 . 120.6(5) yes C69 . C70 . H701 . 119.700 no C71 . C70 . H701 . 119.700 no C70 . C71 . C72 . 120.3(5) yes C70 . C71 . H711 . 119.868 no C72 . C71 . H711 . 119.868 no O2 . C72 . C63 . 122.6(4) yes O2 . C72 . C71 . 115.6(4) yes C63 . C72 . C71 . 121.6(4) yes O3 . C73 . C74 . 117.2(4) yes O3 . C73 . C82 . 121.2(4) yes C74 . C73 . C82 . 121.7(5) yes C73 . C74 . C75 . 120.4(4) yes C73 . C74 . H741 . 119.786 no C75 . C74 . H741 . 119.787 no C74 . C75 . C76 . 119.9(4) yes C74 . C75 . H751 . 120.033 no C76 . C75 . H751 . 120.033 no C75 . C76 . C77 . 120.8(5) yes C75 . C76 . C81 . 119.2(4) yes C77 . C76 . C81 . 120.0(5) yes C76 . C77 . C78 . 121.2(5) yes C76 . C77 . H771 . 119.375 no C78 . C77 . H771 . 119.376 no C77 . C78 . C79 . 120.1(5) yes C77 . C78 . H781 . 119.972 no C79 . C78 . H781 . 119.972 no C78 . C79 . C80 . 119.5(5) yes C78 . C79 . H791 . 120.248 no C80 . C79 . H791 . 120.248 no C79 . C80 . C81 . 122.3(5) yes C79 . C80 . H801 . 118.826 no C81 . C80 . H801 . 118.826 no C76 . C81 . C80 . 116.7(4) yes C76 . C81 . C82 . 120.2(4) yes C80 . C81 . C82 . 122.9(4) yes C73 . C82 . C81 . 118.4(4) yes C73 . C82 . C83 . 118.4(4) yes C81 . C82 . C83 . 123.1(4) yes C82 . C83 . C84 . 122.2(4) yes C82 . C83 . C92 . 120.0(4) yes C84 . C83 . C92 . 117.8(4) yes C83 . C84 . C85 . 122.4(4) yes C83 . C84 . C89 . 120.0(4) yes C85 . C84 . C89 . 117.6(4) yes C84 . C85 . C86 . 121.5(5) yes C84 . C85 . H851 . 119.228 no C86 . C85 . H851 . 119.228 no C85 . C86 . C87 . 120.4(5) yes C85 . C86 . H861 . 119.810 no C87 . C86 . H861 . 119.810 no C86 . C87 . C88 . 119.8(5) yes C86 . C87 . H871 . 120.115 no C88 . C87 . H871 . 120.116 no C87 . C88 . C89 . 120.4(5) yes C87 . C88 . H881 . 119.780 no C89 . C88 . H881 . 119.780 no C84 . C89 . C88 . 119.9(5) yes C84 . C89 . C90 . 119.8(5) yes C88 . C89 . C90 . 120.3(5) yes C89 . C90 . C91 . 119.6(5) yes C89 . C90 . H901 . 120.221 no C91 . C90 . H901 . 120.221 no C90 . C91 . C92 . 120.9(4) yes C90 . C91 . H911 . 119.548 no C92 . C91 . H911 . 119.548 no O4 . C92 . C83 . 122.0(4) yes O4 . C92 . C91 . 116.6(4) yes C83 . C92 . C91 . 121.4(4) yes Cl1 . C93 . Cl2 . 115.0(6) yes Cl1 . C93 . H931 . 108.074 no Cl2 . C93 . H931 . 108.087 no Cl1 . C93 . H932 . 108.082 no Cl2 . C93 . H932 . 108.094 no H931 . C93 . H932 . 109.466 no Cl3 . C94 . Cl4 . 115.7(5) yes Cl3 . C94 . H941 . 107.898 no Cl4 . C94 . H941 . 107.898 no Cl3 . C94 . H942 . 107.899 no Cl4 . C94 . H942 . 107.899 no H941 . C94 . H942 . 109.468 no Cl5 . C95 . Cl6 . 113.1(4) yes Cl5 . C95 . H951 . 108.570 no Cl6 . C95 . H951 . 108.570 no Cl5 . C95 . H952 . 108.569 no Cl6 . C95 . H952 . 108.569 no H951 . C95 . H952 . 109.466 no Cl7 . C96 . Cl8 . 110.2(3) yes Cl7 . C96 . H961 . 109.282 no Cl8 . C96 . H961 . 109.283 no Cl7 . C96 . H962 . 109.282 no Cl8 . C96 . H962 . 109.283 no H961 . C96 . H962 . 109.467 no _database_code_depnum_ccdc_archive 'CCDC 934113'