# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_ljh149_2a _database_code_depnum_ccdc_archive 'CCDC 911752' #TrackingRef 'combined.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H39 Cl Ir O3 P, C H2 Cl2' _chemical_formula_sum 'C50 H41 Cl3 Ir O3 P' _chemical_formula_weight 1019.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.3945(2) _cell_length_b 19.2373(5) _cell_length_c 23.8082(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4302.73(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15162 _cell_measurement_theta_min 2.9522 _cell_measurement_theta_max 28.5717 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 3.369 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4314 _exptl_absorpt_correction_T_max 0.5522 _exptl_absorpt_process_details ; 'Fri Nov 11 12:12:35 2011' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube with Enhance optics' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_reflns_number 24836 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 28.63 _reflns_number_total 9076 _reflns_number_gt 8788 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+2.3943P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(4) _chemical_absolute_configuration ad _refine_ls_number_reflns 9076 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0234 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0573 _refine_ls_wR_factor_gt 0.0562 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir Ir 0.767124(13) 0.955114(6) 0.707068(5) 0.01994(4) Uani 1 1 d . . . P P 0.76510(10) 0.98657(4) 0.61717(3) 0.01768(16) Uani 1 1 d . . . Cl Cl 0.56768(9) 0.88684(4) 0.68365(4) 0.02498(18) Uani 1 1 d . . . O1 O 0.8797(2) 1.04621(13) 0.60124(9) 0.0216(5) Uani 1 1 d . . . O2 O 0.6162(2) 1.02403(11) 0.60019(10) 0.0203(5) Uani 1 1 d . . . O3 O 1.1263(3) 0.93968(16) 0.57620(13) 0.0427(7) Uani 1 1 d . . . C1 C 0.8573(4) 1.08558(16) 0.55236(14) 0.0206(7) Uani 1 1 d . . . C2 C 0.9447(4) 1.07115(18) 0.50622(15) 0.0266(8) Uani 1 1 d . . . H2A H 1.0140 1.0352 0.5081 0.032 Uiso 1 1 calc R . . C3 C 0.9290(4) 1.10924(19) 0.45878(16) 0.0293(8) Uani 1 1 d . . . H3A H 0.9909 1.1013 0.4279 0.035 Uiso 1 1 calc R . . C4 C 0.8215(4) 1.16087(18) 0.45452(15) 0.0267(8) Uani 1 1 d . . . C5 C 0.8011(5) 1.1999(2) 0.40449(16) 0.0339(9) Uani 1 1 d . . . H5A H 0.8629 1.1925 0.3735 0.041 Uiso 1 1 calc R . . C6 C 0.6962(5) 1.2472(2) 0.40014(17) 0.0384(10) Uani 1 1 d . . . H6A H 0.6853 1.2732 0.3665 0.046 Uiso 1 1 calc R . . C7 C 0.6025(5) 1.2580(2) 0.44558(17) 0.0351(9) Uani 1 1 d . . . H7A H 0.5273 1.2907 0.4421 0.042 Uiso 1 1 calc R . . C8 C 0.6188(4) 1.2217(2) 0.49474(16) 0.0292(8) Uani 1 1 d . . . H8A H 0.5546 1.2295 0.5249 0.035 Uiso 1 1 calc R . . C9 C 0.7290(4) 1.17315(16) 0.50114(13) 0.0238(7) Uani 1 1 d . . . C10 C 0.7530(4) 1.13552(15) 0.55215(12) 0.0205(6) Uani 1 1 d . . . C11 C 0.6637(4) 1.14565(17) 0.60350(14) 0.0209(7) Uani 1 1 d . . . C12 C 0.6514(4) 1.21079(18) 0.63128(14) 0.0238(7) Uani 1 1 d . . . C13 C 0.7255(4) 1.27087(17) 0.61507(14) 0.0268(7) Uani 1 1 d . . . H13A H 0.7877 1.2688 0.5836 0.032 Uiso 1 1 calc R . . C14 C 0.7105(4) 1.33213(18) 0.64325(16) 0.0311(8) Uani 1 1 d . . . H14A H 0.7598 1.3724 0.6309 0.037 Uiso 1 1 calc R . . C15 C 0.6213(4) 1.33523(19) 0.69089(16) 0.0313(9) Uani 1 1 d . . . H15A H 0.6110 1.3778 0.7107 0.038 Uiso 1 1 calc R . . C16 C 0.5508(4) 1.2784(2) 0.70845(17) 0.0315(8) Uani 1 1 d . . . H16A H 0.4914 1.2815 0.7406 0.038 Uiso 1 1 calc R . . C17 C 0.5630(4) 1.21458(19) 0.68027(15) 0.0251(8) Uani 1 1 d . . . C18 C 0.4920(4) 1.1541(2) 0.69952(15) 0.0295(8) Uani 1 1 d . . . H18A H 0.4312 1.1571 0.7313 0.035 Uiso 1 1 calc R . . C19 C 0.5095(4) 1.0924(2) 0.67353(14) 0.0258(8) Uani 1 1 d . . . H19A H 0.4635 1.0518 0.6873 0.031 Uiso 1 1 calc R . . C20 C 0.5968(4) 1.08905(17) 0.62565(14) 0.0203(7) Uani 1 1 d . . . C21 C 0.7753(4) 0.92657(15) 0.55830(12) 0.0169(6) Uani 1 1 d . . . C22 C 0.6892(4) 0.93910(16) 0.51078(14) 0.0218(7) Uani 1 1 d . . . H22A H 0.6227 0.9763 0.5111 0.026 Uiso 1 1 calc R . . C23 C 0.7015(4) 0.89781(17) 0.46427(14) 0.0231(7) Uani 1 1 d . . . H23A H 0.6427 0.9065 0.4326 0.028 Uiso 1 1 calc R . . C24 C 0.7992(3) 0.84301(17) 0.46259(14) 0.0200(7) Uani 1 1 d . . . C25 C 0.8146(4) 0.80007(19) 0.41399(14) 0.0251(8) Uani 1 1 d . . . H25A H 0.7564 0.8081 0.3820 0.030 Uiso 1 1 calc R . . C26 C 0.9118(4) 0.7478(2) 0.41324(15) 0.0285(8) Uani 1 1 d . . . H26A H 0.9227 0.7205 0.3803 0.034 Uiso 1 1 calc R . . C27 C 0.9958(4) 0.7338(2) 0.46028(16) 0.0314(9) Uani 1 1 d . . . H27A H 1.0617 0.6964 0.4594 0.038 Uiso 1 1 calc R . . C28 C 0.9841(4) 0.7736(2) 0.50764(15) 0.0282(8) Uani 1 1 d . . . H28A H 1.0429 0.7638 0.5391 0.034 Uiso 1 1 calc R . . C29 C 0.8858(4) 0.82910(17) 0.51042(14) 0.0205(7) Uani 1 1 d . . . C30 C 0.8721(3) 0.87259(18) 0.55900(13) 0.0194(7) Uani 1 1 d . . . C31 C 0.9658(4) 0.8565(2) 0.60861(14) 0.0274(8) Uani 1 1 d . . . C32 C 0.9282(4) 0.8011(2) 0.64518(15) 0.0312(9) Uani 1 1 d . . . C33 C 0.8011(5) 0.7627(2) 0.64045(16) 0.0342(9) Uani 1 1 d . . . H33A H 0.7363 0.7741 0.6112 0.041 Uiso 1 1 calc R . . C34 C 0.7677(6) 0.7101(2) 0.67611(17) 0.0470(11) Uani 1 1 d . . . H34A H 0.6800 0.6860 0.6719 0.056 Uiso 1 1 calc R . . C35 C 0.8628(7) 0.6911(3) 0.7194(2) 0.0608(16) Uani 1 1 d . . . H35A H 0.8396 0.6541 0.7442 0.073 Uiso 1 1 calc R . . C36 C 0.9850(7) 0.7250(3) 0.72510(17) 0.0575(16) Uani 1 1 d . . . H36A H 1.0484 0.7117 0.7543 0.069 Uiso 1 1 calc R . . C37 C 1.0244(5) 0.7811(3) 0.68880(16) 0.0441(12) Uani 1 1 d . . . C38 C 1.1519(6) 0.8161(3) 0.69339(18) 0.0550(15) Uani 1 1 d . . . H38A H 1.2168 0.8025 0.7219 0.066 Uiso 1 1 calc R . . C39 C 1.1888(4) 0.8696(3) 0.65859(19) 0.0513(14) Uani 1 1 d . . . H39A H 1.2767 0.8932 0.6635 0.062 Uiso 1 1 calc R . . C40 C 1.0939(4) 0.8897(2) 0.61477(17) 0.0355(9) Uani 1 1 d . . . C48 C 0.7096(4) 0.9493(2) 0.79785(13) 0.0312(8) Uani 1 1 d . . . H48A H 0.6097 0.9342 0.8056 0.037 Uiso 1 1 calc R . . C45 C 0.8613(4) 1.0483(2) 0.73434(15) 0.0274(7) Uani 1 1 d . . . H45A H 0.8668 1.0850 0.7046 0.033 Uiso 1 1 calc R . . C46 C 0.7965(4) 1.07357(19) 0.78917(16) 0.0347(8) Uani 1 1 d . . . H46A H 0.7098 1.1009 0.7807 0.042 Uiso 1 1 calc R . . H46B H 0.8651 1.1049 0.8081 0.042 Uiso 1 1 calc R . . C43 C 1.0366(4) 0.9616(2) 0.78056(16) 0.0381(9) Uani 1 1 d . . . H43A H 1.0434 0.9961 0.8113 0.046 Uiso 1 1 calc R . . H43B H 1.1347 0.9475 0.7705 0.046 Uiso 1 1 calc R . . C47 C 0.7571(5) 1.0141(2) 0.82967(15) 0.0399(9) Uani 1 1 d . . . H47A H 0.8405 1.0026 0.8533 0.048 Uiso 1 1 calc R . . H47B H 0.6793 1.0296 0.8548 0.048 Uiso 1 1 calc R . . C49 C 0.8025(4) 0.8964(2) 0.78636(15) 0.0324(8) Uani 1 1 d . . . H49A H 0.7586 0.8491 0.7869 0.039 Uiso 1 1 calc R . . C44 C 0.9680(4) 0.9964(2) 0.72964(15) 0.0292(8) Uani 1 1 d . . . H44A H 1.0342 1.0032 0.6972 0.035 Uiso 1 1 calc R . . C42 C 0.9566(5) 0.8977(2) 0.80229(17) 0.0409(10) Uani 1 1 d . . . H42A H 1.0031 0.8554 0.7874 0.049 Uiso 1 1 calc R . . H42B H 0.9642 0.8963 0.8438 0.049 Uiso 1 1 calc R . . C41 C 1.2475(6) 0.9819(3) 0.5873(2) 0.0757(17) Uani 1 1 d . . . H41A H 1.2576 1.0168 0.5576 0.114 Uiso 1 1 calc R . . H41B H 1.3330 0.9527 0.5885 0.114 Uiso 1 1 calc R . . H41C H 1.2354 1.0053 0.6236 0.114 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir 0.01964(6) 0.02537(6) 0.01483(6) -0.00418(5) -0.00048(5) -0.00501(5) P 0.0163(4) 0.0198(4) 0.0169(4) -0.0034(3) 0.0012(3) -0.0019(3) Cl 0.0249(4) 0.0304(4) 0.0197(4) 0.0010(3) -0.0029(3) -0.0104(3) O1 0.0207(11) 0.0206(11) 0.0235(12) -0.0015(11) 0.0029(9) -0.0020(11) O2 0.0175(12) 0.0227(12) 0.0208(12) -0.0026(9) 0.0013(9) 0.0005(9) O3 0.0194(13) 0.057(2) 0.0519(18) -0.0211(15) -0.0034(12) -0.0053(12) C1 0.0217(17) 0.0175(16) 0.0225(17) -0.0030(13) 0.0051(13) -0.0053(12) C2 0.0269(19) 0.0220(16) 0.0309(19) -0.0039(15) 0.0121(15) 0.0009(14) C3 0.032(2) 0.0265(18) 0.029(2) -0.0036(16) 0.0166(16) -0.0048(15) C4 0.033(2) 0.0228(17) 0.0242(18) -0.0039(15) 0.0105(15) -0.0039(14) C5 0.043(2) 0.035(2) 0.0233(18) 0.0007(16) 0.0079(16) -0.0071(17) C6 0.050(3) 0.039(2) 0.0254(19) 0.0052(17) 0.0006(18) -0.0025(19) C7 0.045(2) 0.031(2) 0.029(2) 0.0005(17) -0.0053(18) 0.0057(18) C8 0.032(2) 0.033(2) 0.0223(18) -0.0044(16) 0.0039(15) 0.0044(16) C9 0.0269(18) 0.0228(15) 0.0217(16) -0.0043(13) 0.0057(15) -0.0024(15) C10 0.0243(18) 0.0187(14) 0.0186(14) -0.0025(12) 0.0042(13) -0.0011(14) C11 0.0197(17) 0.0233(17) 0.0196(17) -0.0052(14) 0.0014(13) 0.0033(13) C12 0.0235(18) 0.0284(18) 0.0196(17) -0.0060(14) -0.0033(13) 0.0090(14) C13 0.0263(18) 0.0296(17) 0.0244(17) -0.0033(14) -0.0021(15) 0.0039(15) C14 0.033(2) 0.0256(17) 0.034(2) -0.0078(15) -0.0132(16) 0.0051(15) C15 0.034(2) 0.0305(19) 0.029(2) -0.0158(16) -0.0156(15) 0.0141(16) C16 0.0272(18) 0.044(2) 0.0234(17) -0.0165(18) -0.0082(17) 0.0147(15) C17 0.0244(19) 0.0334(19) 0.0176(17) -0.0064(15) -0.0046(14) 0.0095(15) C18 0.0231(17) 0.045(2) 0.0202(18) -0.0038(17) 0.0042(14) 0.0089(15) C19 0.0193(17) 0.038(2) 0.0198(17) -0.0016(15) 0.0038(13) 0.0002(15) C20 0.0172(16) 0.0280(17) 0.0156(16) -0.0078(14) 0.0015(13) 0.0025(13) C21 0.0177(15) 0.0171(13) 0.0160(14) -0.0020(12) 0.0034(12) -0.0026(12) C22 0.0272(18) 0.0188(16) 0.0193(16) 0.0020(13) 0.0004(13) 0.0032(12) C23 0.028(2) 0.0252(17) 0.0160(16) 0.0015(13) -0.0043(13) 0.0019(14) C24 0.0186(17) 0.0238(16) 0.0178(16) -0.0017(13) 0.0000(13) -0.0031(12) C25 0.029(2) 0.0309(19) 0.0152(16) -0.0017(14) -0.0017(13) 0.0013(15) C26 0.033(2) 0.032(2) 0.0202(18) -0.0074(15) 0.0019(15) 0.0004(16) C27 0.029(2) 0.034(2) 0.031(2) -0.0102(17) -0.0005(16) 0.0120(16) C28 0.0256(19) 0.037(2) 0.0222(18) -0.0052(16) -0.0033(14) 0.0069(15) C29 0.0170(17) 0.0247(17) 0.0197(17) -0.0017(14) 0.0014(13) 0.0006(13) C30 0.0129(15) 0.0291(17) 0.0161(15) -0.0023(14) -0.0008(12) 0.0005(13) C31 0.0203(18) 0.042(2) 0.0203(18) -0.0147(16) -0.0040(13) 0.0110(16) C32 0.034(2) 0.044(2) 0.0157(17) -0.0069(16) -0.0061(15) 0.0233(17) C33 0.039(2) 0.042(2) 0.0213(18) 0.0027(16) 0.0017(16) 0.0128(18) C34 0.065(3) 0.042(2) 0.033(2) 0.0077(18) 0.006(2) 0.013(2) C35 0.086(4) 0.060(3) 0.036(3) 0.014(2) 0.009(3) 0.035(3) C36 0.078(4) 0.075(4) 0.019(2) 0.006(2) -0.008(2) 0.051(3) C37 0.045(3) 0.068(3) 0.0187(19) -0.011(2) -0.0119(17) 0.034(2) C38 0.054(3) 0.089(4) 0.022(2) -0.020(2) -0.0191(19) 0.043(3) C39 0.021(2) 0.088(4) 0.044(3) -0.044(3) -0.0163(18) 0.018(2) C40 0.0232(19) 0.052(2) 0.032(2) -0.0186(19) -0.0053(16) 0.0090(17) C48 0.037(2) 0.043(2) 0.0136(15) -0.0010(16) 0.0025(14) -0.0177(17) C45 0.0317(18) 0.0273(17) 0.0231(17) -0.0099(16) 0.0003(14) -0.0106(17) C46 0.038(2) 0.0354(18) 0.0310(19) -0.0185(17) 0.0011(18) -0.0035(15) C43 0.0253(18) 0.060(3) 0.029(2) -0.0174(19) -0.0077(14) -0.0010(19) C47 0.038(2) 0.055(2) 0.0259(18) -0.0197(17) 0.0068(18) -0.013(2) C49 0.041(2) 0.038(2) 0.0185(17) 0.0043(16) -0.0049(16) -0.0069(16) C44 0.0206(18) 0.043(2) 0.0237(18) -0.0130(16) 0.0022(14) -0.0132(16) C42 0.044(2) 0.051(2) 0.027(2) -0.0061(19) -0.0123(18) 0.0090(19) C41 0.037(3) 0.113(5) 0.077(4) -0.027(3) 0.002(3) -0.037(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir P 2.2242(8) . ? Ir Cl 2.3551(8) . ? Ir C48 2.231(3) . ? Ir C45 2.103(3) . ? Ir C49 2.225(4) . ? Ir C44 2.116(4) . ? P O1 1.619(2) . ? P O2 1.625(2) . ? P C21 1.818(3) . ? O1 C1 1.404(4) . ? O2 C20 1.402(4) . ? O3 C40 1.364(5) . ? O3 C41 1.424(5) . ? C1 C2 1.400(5) . ? C1 C10 1.372(5) . ? C2 H2A 0.950 . ? C2 C3 1.354(5) . ? C3 H3A 0.950 . ? C3 C4 1.420(5) . ? C4 C5 1.421(5) . ? C4 C9 1.429(5) . ? C5 H5A 0.950 . ? C5 C6 1.345(6) . ? C6 H6A 0.950 . ? C6 C7 1.410(6) . ? C7 H7A 0.950 . ? C7 C8 1.371(5) . ? C8 H8A 0.950 . ? C8 C9 1.402(5) . ? C9 C10 1.431(4) . ? C10 C11 1.495(4) . ? C11 C12 1.422(5) . ? C11 C20 1.363(5) . ? C12 C13 1.403(5) . ? C12 C17 1.434(5) . ? C13 H13A 0.950 . ? C13 C14 1.363(5) . ? C14 H14A 0.950 . ? C14 C15 1.412(6) . ? C15 H15A 0.950 . ? C15 C16 1.346(6) . ? C16 H16A 0.950 . ? C16 C17 1.403(5) . ? C17 C18 1.417(5) . ? C18 H18A 0.950 . ? C18 C19 1.349(5) . ? C19 H19A 0.950 . ? C19 C20 1.406(5) . ? C21 C22 1.411(4) . ? C21 C30 1.381(4) . ? C22 H22A 0.950 . ? C22 C23 1.368(5) . ? C23 H23A 0.950 . ? C23 C24 1.399(5) . ? C24 C25 1.429(5) . ? C24 C29 1.425(5) . ? C25 H25A 0.950 . ? C25 C26 1.358(5) . ? C26 H26A 0.950 . ? C26 C27 1.397(5) . ? C27 H27A 0.950 . ? C27 C28 1.367(5) . ? C28 H28A 0.950 . ? C28 C29 1.413(5) . ? C29 C30 1.433(5) . ? C30 C31 1.505(5) . ? C31 C32 1.421(6) . ? C31 C40 1.370(6) . ? C32 C33 1.409(6) . ? C32 C37 1.429(5) . ? C33 H33A 0.950 . ? C33 C34 1.358(6) . ? C34 H34A 0.950 . ? C34 C35 1.412(7) . ? C35 H35A 0.950 . ? C35 C36 1.328(9) . ? C36 H36A 0.950 . ? C36 C37 1.431(8) . ? C37 C38 1.378(8) . ? C38 H38A 0.950 . ? C38 C39 1.366(8) . ? C39 H39A 0.950 . ? C39 C40 1.426(6) . ? C48 H48A 1.000 . ? C48 C47 1.525(5) . ? C48 C49 1.368(6) . ? C45 H45A 1.000 . ? C45 C46 1.520(5) . ? C45 C44 1.420(5) . ? C46 H46A 0.990 . ? C46 H46B 0.990 . ? C46 C47 1.542(6) . ? C43 H43A 0.990 . ? C43 H43B 0.990 . ? C43 C44 1.527(6) . ? C43 C42 1.531(6) . ? C47 H47A 0.990 . ? C47 H47B 0.990 . ? C49 H49A 1.000 . ? C49 C42 1.496(6) . ? C44 H44A 1.000 . ? C42 H42A 0.990 . ? C42 H42B 0.990 . ? C41 H41A 0.980 . ? C41 H41B 0.980 . ? C41 H41C 0.980 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P Ir Cl 85.24(3) . . ? P Ir C48 160.73(10) . . ? P Ir C45 93.94(10) . . ? P Ir C49 162.91(11) . . ? P Ir C44 98.63(11) . . ? Cl Ir C48 90.50(9) . . ? Cl Ir C45 152.07(11) . . ? Cl Ir C49 92.11(10) . . ? Cl Ir C44 168.11(11) . . ? C48 Ir C45 81.11(13) . . ? C48 Ir C49 35.77(14) . . ? C48 Ir C44 89.35(13) . . ? C45 Ir C49 96.20(14) . . ? C45 Ir C44 39.34(15) . . ? C49 Ir C44 80.88(15) . . ? Ir P O1 114.37(9) . . ? Ir P O2 111.56(9) . . ? Ir P C21 124.66(10) . . ? O1 P O2 101.54(12) . . ? O1 P C21 103.54(13) . . ? O2 P C21 97.77(14) . . ? P O1 C1 118.5(2) . . ? P O2 C20 113.6(2) . . ? C40 O3 C41 117.1(4) . . ? O1 C1 C2 117.1(3) . . ? O1 C1 C10 119.2(3) . . ? C2 C1 C10 123.7(3) . . ? C1 C2 H2A 120.6 . . ? C1 C2 C3 118.9(3) . . ? H2A C2 C3 120.6 . . ? C2 C3 H3A 119.5 . . ? C2 C3 C4 121.0(3) . . ? H3A C3 C4 119.5 . . ? C3 C4 C5 121.7(3) . . ? C3 C4 C9 119.5(3) . . ? C5 C4 C9 118.8(3) . . ? C4 C5 H5A 119.3 . . ? C4 C5 C6 121.3(4) . . ? H5A C5 C6 119.3 . . ? C5 C6 H6A 120.1 . . ? C5 C6 C7 119.9(4) . . ? H6A C6 C7 120.1 . . ? C6 C7 H7A 119.7 . . ? C6 C7 C8 120.6(4) . . ? H7A C7 C8 119.7 . . ? C7 C8 H8A 119.5 . . ? C7 C8 C9 121.0(4) . . ? H8A C8 C9 119.5 . . ? C4 C9 C8 118.3(3) . . ? C4 C9 C10 118.7(3) . . ? C8 C9 C10 123.0(3) . . ? C1 C10 C9 118.0(3) . . ? C1 C10 C11 119.2(3) . . ? C9 C10 C11 122.7(3) . . ? C10 C11 C12 122.7(3) . . ? C10 C11 C20 118.1(3) . . ? C12 C11 C20 119.1(3) . . ? C11 C12 C13 123.9(3) . . ? C11 C12 C17 118.1(3) . . ? C13 C12 C17 118.0(3) . . ? C12 C13 H13A 119.1 . . ? C12 C13 C14 121.7(3) . . ? H13A C13 C14 119.1 . . ? C13 C14 H14A 120.2 . . ? C13 C14 C15 119.6(4) . . ? H14A C14 C15 120.2 . . ? C14 C15 H15A 119.7 . . ? C14 C15 C16 120.5(3) . . ? H15A C15 C16 119.7 . . ? C15 C16 H16A 119.3 . . ? C15 C16 C17 121.5(4) . . ? H16A C16 C17 119.3 . . ? C12 C17 C16 118.7(4) . . ? C12 C17 C18 119.6(3) . . ? C16 C17 C18 121.7(3) . . ? C17 C18 H18A 119.4 . . ? C17 C18 C19 121.2(3) . . ? H18A C18 C19 119.4 . . ? C18 C19 H19A 120.6 . . ? C18 C19 C20 118.8(3) . . ? H19A C19 C20 120.6 . . ? O2 C20 C11 119.0(3) . . ? O2 C20 C19 117.8(3) . . ? C11 C20 C19 123.1(3) . . ? P C21 C22 118.6(2) . . ? P C21 C30 120.2(2) . . ? C22 C21 C30 121.0(3) . . ? C21 C22 H22A 120.0 . . ? C21 C22 C23 120.1(3) . . ? H22A C22 C23 120.0 . . ? C22 C23 H23A 119.5 . . ? C22 C23 C24 121.1(3) . . ? H23A C23 C24 119.5 . . ? C23 C24 C25 121.7(3) . . ? C23 C24 C29 119.6(3) . . ? C25 C24 C29 118.8(3) . . ? C24 C25 H25A 119.8 . . ? C24 C25 C26 120.4(3) . . ? H25A C25 C26 119.8 . . ? C25 C26 H26A 119.6 . . ? C25 C26 C27 120.8(3) . . ? H26A C26 C27 119.6 . . ? C26 C27 H27A 119.7 . . ? C26 C27 C28 120.5(3) . . ? H27A C27 C28 119.7 . . ? C27 C28 H28A 119.5 . . ? C27 C28 C29 120.9(3) . . ? H28A C28 C29 119.5 . . ? C24 C29 C28 118.5(3) . . ? C24 C29 C30 119.0(3) . . ? C28 C29 C30 122.5(3) . . ? C21 C30 C29 119.2(3) . . ? C21 C30 C31 123.3(3) . . ? C29 C30 C31 117.4(3) . . ? C30 C31 C32 119.3(3) . . ? C30 C31 C40 120.1(4) . . ? C32 C31 C40 120.1(4) . . ? C31 C32 C33 123.7(3) . . ? C31 C32 C37 119.3(4) . . ? C33 C32 C37 116.9(4) . . ? C32 C33 H33A 118.8 . . ? C32 C33 C34 122.5(4) . . ? H33A C33 C34 118.8 . . ? C33 C34 H34A 119.9 . . ? C33 C34 C35 120.2(5) . . ? H34A C34 C35 119.9 . . ? C34 C35 H35A 120.2 . . ? C34 C35 C36 119.6(5) . . ? H35A C35 C36 120.2 . . ? C35 C36 H36A 118.9 . . ? C35 C36 C37 122.2(4) . . ? H36A C36 C37 118.9 . . ? C32 C37 C36 118.6(5) . . ? C32 C37 C38 118.4(5) . . ? C36 C37 C38 123.0(4) . . ? C37 C38 H38A 118.6 . . ? C37 C38 C39 122.7(4) . . ? H38A C38 C39 118.6 . . ? C38 C39 H39A 120.4 . . ? C38 C39 C40 119.3(4) . . ? H39A C39 C40 120.4 . . ? O3 C40 C31 116.9(3) . . ? O3 C40 C39 122.9(4) . . ? C31 C40 C39 120.1(4) . . ? Ir C48 H48A 114.8 . . ? Ir C48 C47 111.7(2) . . ? Ir C48 C49 71.9(2) . . ? H48A C48 C47 114.8 . . ? H48A C48 C49 114.8 . . ? C47 C48 C49 121.4(4) . . ? Ir C45 H45A 113.8 . . ? Ir C45 C46 111.7(2) . . ? Ir C45 C44 70.8(2) . . ? H45A C45 C46 113.8 . . ? H45A C45 C44 113.8 . . ? C46 C45 C44 125.1(3) . . ? C45 C46 H46A 108.9 . . ? C45 C46 H46B 108.9 . . ? C45 C46 C47 113.4(3) . . ? H46A C46 H46B 107.7 . . ? H46A C46 C47 108.9 . . ? H46B C46 C47 108.9 . . ? H43A C43 H43B 107.6 . . ? H43A C43 C44 108.7 . . ? H43A C43 C42 108.7 . . ? H43B C43 C44 108.7 . . ? H43B C43 C42 108.7 . . ? C44 C43 C42 114.4(3) . . ? C48 C47 C46 111.5(3) . . ? C48 C47 H47A 109.3 . . ? C48 C47 H47B 109.3 . . ? C46 C47 H47A 109.3 . . ? C46 C47 H47B 109.3 . . ? H47A C47 H47B 108.0 . . ? Ir C49 C48 72.3(2) . . ? Ir C49 H49A 114.3 . . ? Ir C49 C42 110.6(3) . . ? C48 C49 H49A 114.3 . . ? C48 C49 C42 123.6(4) . . ? H49A C49 C42 114.3 . . ? Ir C44 C45 69.8(2) . . ? Ir C44 C43 114.4(3) . . ? Ir C44 H44A 114.1 . . ? C45 C44 C43 122.9(3) . . ? C45 C44 H44A 114.1 . . ? C43 C44 H44A 114.1 . . ? C43 C42 C49 113.7(3) . . ? C43 C42 H42A 108.8 . . ? C43 C42 H42B 108.8 . . ? C49 C42 H42A 108.8 . . ? C49 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? O3 C41 H41A 109.5 . . ? O3 C41 H41B 109.5 . . ? O3 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl Ir P O1 174.33(10) . . . . ? Cl Ir P O2 59.81(9) . . . . ? Cl Ir P C21 -56.93(14) . . . . ? C48 Ir P O1 96.5(3) . . . . ? C48 Ir P O2 -18.0(3) . . . . ? C48 Ir P C21 -134.7(3) . . . . ? C45 Ir P O1 22.33(14) . . . . ? C45 Ir P O2 -92.20(14) . . . . ? C45 Ir P C21 151.07(17) . . . . ? C49 Ir P O1 -104.0(4) . . . . ? C49 Ir P O2 141.5(4) . . . . ? C49 Ir P C21 24.7(4) . . . . ? C44 Ir P O1 -16.99(15) . . . . ? C44 Ir P O2 -131.51(14) . . . . ? C44 Ir P C21 111.75(17) . . . . ? Ir P O1 C1 -159.22(19) . . . . ? O2 P O1 C1 -38.9(2) . . . . ? C21 P O1 C1 62.1(3) . . . . ? Ir P O2 C20 68.0(2) . . . . ? O1 P O2 C20 -54.2(2) . . . . ? C21 P O2 C20 -159.8(2) . . . . ? P O1 C1 C2 -106.1(3) . . . . ? P O1 C1 C10 74.1(3) . . . . ? O1 C1 C2 C3 -178.3(3) . . . . ? C10 C1 C2 C3 1.6(5) . . . . ? C1 C2 C3 C4 -3.0(6) . . . . ? C2 C3 C4 C5 -178.2(4) . . . . ? C2 C3 C4 C9 0.4(6) . . . . ? C3 C4 C5 C6 177.9(4) . . . . ? C9 C4 C5 C6 -0.8(6) . . . . ? C4 C5 C6 C7 -1.0(6) . . . . ? C5 C6 C7 C8 1.3(6) . . . . ? C6 C7 C8 C9 0.2(6) . . . . ? C7 C8 C9 C4 -1.9(6) . . . . ? C7 C8 C9 C10 178.1(4) . . . . ? C3 C4 C9 C8 -176.5(3) . . . . ? C3 C4 C9 C10 3.5(5) . . . . ? C5 C4 C9 C8 2.2(5) . . . . ? C5 C4 C9 C10 -177.8(3) . . . . ? O1 C1 C10 C9 -177.8(3) . . . . ? O1 C1 C10 C11 -1.4(5) . . . . ? C2 C1 C10 C9 2.4(5) . . . . ? C2 C1 C10 C11 178.8(3) . . . . ? C4 C9 C10 C1 -4.8(5) . . . . ? C4 C9 C10 C11 178.9(3) . . . . ? C8 C9 C10 C1 175.2(3) . . . . ? C8 C9 C10 C11 -1.1(5) . . . . ? C1 C10 C11 C12 123.9(4) . . . . ? C1 C10 C11 C20 -53.2(5) . . . . ? C9 C10 C11 C12 -59.9(5) . . . . ? C9 C10 C11 C20 123.1(4) . . . . ? C10 C11 C12 C13 -2.8(5) . . . . ? C10 C11 C12 C17 -179.9(3) . . . . ? C20 C11 C12 C13 174.2(3) . . . . ? C20 C11 C12 C17 -2.9(5) . . . . ? C11 C12 C13 C14 -179.7(3) . . . . ? C17 C12 C13 C14 -2.6(5) . . . . ? C12 C13 C14 C15 1.7(5) . . . . ? C13 C14 C15 C16 -0.3(5) . . . . ? C14 C15 C16 C17 -0.1(5) . . . . ? C15 C16 C17 C12 -0.8(5) . . . . ? C15 C16 C17 C18 178.2(3) . . . . ? C11 C12 C17 C16 179.4(3) . . . . ? C11 C12 C17 C18 0.4(5) . . . . ? C13 C12 C17 C16 2.1(5) . . . . ? C13 C12 C17 C18 -176.9(3) . . . . ? C12 C17 C18 C19 2.0(5) . . . . ? C16 C17 C18 C19 -177.1(3) . . . . ? C17 C18 C19 C20 -1.7(5) . . . . ? C10 C11 C20 O2 1.1(5) . . . . ? C10 C11 C20 C19 -179.6(3) . . . . ? C12 C11 C20 O2 -176.1(3) . . . . ? C12 C11 C20 C19 3.3(5) . . . . ? P O2 C20 C11 79.9(3) . . . . ? P O2 C20 C19 -99.5(3) . . . . ? C18 C19 C20 O2 178.4(3) . . . . ? C18 C19 C20 C11 -0.9(5) . . . . ? Ir P C21 C22 139.6(2) . . . . ? Ir P C21 C30 -44.4(3) . . . . ? O1 P C21 C22 -87.3(3) . . . . ? O1 P C21 C30 88.6(3) . . . . ? O2 P C21 C22 16.6(3) . . . . ? O2 P C21 C30 -167.4(3) . . . . ? P C21 C22 C23 175.5(3) . . . . ? C30 C21 C22 C23 -0.5(5) . . . . ? C21 C22 C23 C24 -0.4(5) . . . . ? C22 C23 C24 C25 -179.1(3) . . . . ? C22 C23 C24 C29 1.1(5) . . . . ? C23 C24 C25 C26 179.1(3) . . . . ? C29 C24 C25 C26 -1.2(5) . . . . ? C24 C25 C26 C27 1.7(6) . . . . ? C25 C26 C27 C28 -1.5(6) . . . . ? C26 C27 C28 C29 0.8(6) . . . . ? C27 C28 C29 C24 -0.3(6) . . . . ? C27 C28 C29 C30 -179.0(4) . . . . ? C23 C24 C29 C28 -179.8(3) . . . . ? C23 C24 C29 C30 -1.0(5) . . . . ? C25 C24 C29 C28 0.5(5) . . . . ? C25 C24 C29 C30 179.2(3) . . . . ? P C21 C30 C29 -175.3(2) . . . . ? P C21 C30 C31 4.6(5) . . . . ? C22 C21 C30 C29 0.5(5) . . . . ? C22 C21 C30 C31 -179.5(3) . . . . ? C24 C29 C30 C21 0.2(5) . . . . ? C24 C29 C30 C31 -179.7(3) . . . . ? C28 C29 C30 C21 178.9(3) . . . . ? C28 C29 C30 C31 -1.0(5) . . . . ? C21 C30 C31 C32 101.0(4) . . . . ? C21 C30 C31 C40 -86.3(4) . . . . ? C29 C30 C31 C32 -79.0(4) . . . . ? C29 C30 C31 C40 93.6(4) . . . . ? C30 C31 C32 C33 -5.1(5) . . . . ? C30 C31 C32 C37 173.6(3) . . . . ? C40 C31 C32 C33 -177.7(3) . . . . ? C40 C31 C32 C37 1.0(5) . . . . ? C31 C32 C33 C34 -179.8(4) . . . . ? C37 C32 C33 C34 1.6(6) . . . . ? C32 C33 C34 C35 -1.1(6) . . . . ? C33 C34 C35 C36 0.2(7) . . . . ? C34 C35 C36 C37 0.3(7) . . . . ? C31 C32 C37 C36 -179.8(3) . . . . ? C31 C32 C37 C38 -0.8(6) . . . . ? C33 C32 C37 C36 -1.1(5) . . . . ? C33 C32 C37 C38 177.9(4) . . . . ? C35 C36 C37 C32 0.2(7) . . . . ? C35 C36 C37 C38 -178.7(5) . . . . ? C32 C37 C38 C39 1.1(6) . . . . ? C36 C37 C38 C39 180.0(4) . . . . ? C37 C38 C39 C40 -1.4(6) . . . . ? C41 O3 C40 C31 170.1(4) . . . . ? C41 O3 C40 C39 -12.4(6) . . . . ? C30 C31 C40 O3 3.8(5) . . . . ? C30 C31 C40 C39 -173.8(3) . . . . ? C32 C31 C40 O3 176.3(3) . . . . ? C32 C31 C40 C39 -1.2(5) . . . . ? C38 C39 C40 O3 -176.0(4) . . . . ? C38 C39 C40 C31 1.4(6) . . . . ? P Ir C48 C47 -72.8(4) . . . . ? P Ir C48 C49 169.8(2) . . . . ? Cl Ir C48 C47 -149.7(3) . . . . ? Cl Ir C48 C49 92.9(2) . . . . ? C45 Ir C48 C47 3.5(3) . . . . ? C45 Ir C48 C49 -113.8(2) . . . . ? C49 Ir C48 C47 117.4(4) . . . . ? C44 Ir C48 C47 42.1(3) . . . . ? C44 Ir C48 C49 -75.2(2) . . . . ? P Ir C45 C46 140.1(3) . . . . ? P Ir C45 C44 -98.8(2) . . . . ? Cl Ir C45 C46 52.8(4) . . . . ? Cl Ir C45 C44 173.91(18) . . . . ? C48 Ir C45 C46 -21.2(3) . . . . ? C48 Ir C45 C44 99.9(2) . . . . ? C49 Ir C45 C46 -53.7(3) . . . . ? C49 Ir C45 C44 67.4(2) . . . . ? C44 Ir C45 C46 -121.1(4) . . . . ? Ir C45 C46 C47 36.3(4) . . . . ? C44 C45 C46 C47 -44.9(5) . . . . ? Ir C48 C47 C46 14.6(4) . . . . ? C49 C48 C47 C46 96.0(4) . . . . ? C45 C46 C47 C48 -33.1(5) . . . . ? Ir C48 C49 C42 103.4(4) . . . . ? C47 C48 C49 Ir -104.8(3) . . . . ? C47 C48 C49 C42 -1.5(6) . . . . ? P Ir C49 C48 -168.6(3) . . . . ? P Ir C49 C42 71.3(5) . . . . ? Cl Ir C49 C48 -87.9(2) . . . . ? Cl Ir C49 C42 152.0(3) . . . . ? C48 Ir C49 C42 -120.1(4) . . . . ? C45 Ir C49 C48 65.4(2) . . . . ? C45 Ir C49 C42 -54.7(3) . . . . ? C44 Ir C49 C48 101.7(2) . . . . ? C44 Ir C49 C42 -18.4(3) . . . . ? Ir C45 C44 C43 -106.7(3) . . . . ? C46 C45 C44 Ir 103.5(3) . . . . ? C46 C45 C44 C43 -3.2(6) . . . . ? C42 C43 C44 Ir 6.6(4) . . . . ? C42 C43 C44 C45 87.6(4) . . . . ? P Ir C44 C45 85.7(2) . . . . ? P Ir C44 C43 -156.3(3) . . . . ? Cl Ir C44 C45 -166.1(4) . . . . ? Cl Ir C44 C43 -48.1(7) . . . . ? C48 Ir C44 C45 -76.7(2) . . . . ? C48 Ir C44 C43 41.3(3) . . . . ? C45 Ir C44 C43 118.0(4) . . . . ? C49 Ir C44 C45 -111.6(2) . . . . ? C49 Ir C44 C43 6.4(3) . . . . ? Ir C49 C42 C43 27.2(4) . . . . ? C48 C49 C42 C43 -54.8(5) . . . . ? C44 C43 C42 C49 -22.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.857 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.841 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.080 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 -0.236 0.518 0.576 168 30 ' ' 2 -0.265 0.482 0.076 168 30 ' ' 3 0.235 1.018 0.924 168 30 ' ' 4 0.264 0.982 0.424 168 30 ' ' _platon_squeeze_details ; ; # Contents of RES file _computing_special_details ; TITL ljh149 in P2(1)2(1)2(1) CELL 0.71073 9.3945 19.2373 23.8082 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0005 0.0005 0.000 0.000 0.000 LATT -1 SYMM 0.50000-X,-Y, 0.50000+Z SYMM 0.50000+X, 0.50000-Y,-Z SYMM -X, 0.50000+Y, 0.50000-Z SFAC C H O P CL IR UNIT 200 164 12 4 12 4 TEMP -123 ACTA 50 L.S. 8 LIST 1 FMAP 2 PLAN 10 OMIT 0 3 1 OMIT 0 1 4 OMIT 0 0 6 BOND $H CONF SIZE 0.30 0.20 0.20 REM red block REM one DCM squeezed REM EXTI 0.000208 WGHT 0.030100 2.394300 FVAR 2.04239 IR 6 0.767124 0.955114 0.707068 11.00000 0.01964 0.02537 = 0.01483 -0.00418 -0.00048 -0.00501 P 4 0.765100 0.986567 0.617172 11.00000 0.01633 0.01984 = 0.01686 -0.00342 0.00117 -0.00191 CL 5 0.567680 0.886842 0.683647 11.00000 0.02488 0.03038 = 0.01968 0.00100 -0.00289 -0.01039 O1 3 0.879715 1.046215 0.601239 11.00000 0.02074 0.02059 = 0.02352 -0.00151 0.00289 -0.00200 O2 3 0.616162 1.024032 0.600189 11.00000 0.01748 0.02269 = 0.02077 -0.00257 0.00127 0.00054 O3 3 1.126338 0.939675 0.576195 11.00000 0.01939 0.05687 = 0.05191 -0.02115 -0.00337 -0.00533 C1 1 0.857265 1.085583 0.552360 11.00000 0.02166 0.01752 = 0.02248 -0.00299 0.00509 -0.00529 C2 1 0.944746 1.071149 0.506220 11.00000 0.02692 0.02204 = 0.03087 -0.00389 0.01207 0.00086 AFIX 43 H2A 2 1.013982 1.035235 0.508148 11.00000 -1.20000 AFIX 0 C3 1 0.929039 1.109239 0.458780 11.00000 0.03216 0.02650 = 0.02939 -0.00359 0.01661 -0.00481 AFIX 43 H3A 2 0.990906 1.101301 0.427875 11.00000 -1.20000 AFIX 0 C4 1 0.821491 1.160870 0.454522 11.00000 0.03315 0.02277 = 0.02417 -0.00393 0.01046 -0.00393 C5 1 0.801149 1.199901 0.404486 11.00000 0.04325 0.03521 = 0.02331 0.00068 0.00786 -0.00711 AFIX 43 H5A 2 0.862910 1.192451 0.373469 11.00000 -1.20000 AFIX 0 C6 1 0.696234 1.247176 0.400143 11.00000 0.05032 0.03950 = 0.02536 0.00524 0.00058 -0.00253 AFIX 43 H6A 2 0.685295 1.273240 0.366527 11.00000 -1.20000 AFIX 0 C7 1 0.602500 1.257983 0.445581 11.00000 0.04490 0.03105 = 0.02931 0.00053 -0.00527 0.00569 AFIX 43 H7A 2 0.527319 1.290728 0.442106 11.00000 -1.20000 AFIX 0 C8 1 0.618829 1.221677 0.494738 11.00000 0.03227 0.03305 = 0.02229 -0.00435 0.00387 0.00444 AFIX 43 H8A 2 0.554557 1.229519 0.524885 11.00000 -1.20000 AFIX 0 C9 1 0.729029 1.173146 0.501144 11.00000 0.02691 0.02278 = 0.02175 -0.00426 0.00565 -0.00236 C10 1 0.752975 1.135524 0.552145 11.00000 0.02426 0.01868 = 0.01865 -0.00254 0.00418 -0.00106 C11 1 0.663711 1.145645 0.603498 11.00000 0.01965 0.02331 = 0.01960 -0.00518 0.00139 0.00328 C12 1 0.651439 1.210785 0.631275 11.00000 0.02349 0.02844 = 0.01959 -0.00601 -0.00326 0.00901 C13 1 0.725496 1.270871 0.615067 11.00000 0.02634 0.02962 = 0.02438 -0.00334 -0.00214 0.00386 AFIX 43 H13A 2 0.787660 1.268813 0.583639 11.00000 -1.20000 AFIX 0 C14 1 0.710549 1.332125 0.643253 11.00000 0.03340 0.02559 = 0.03419 -0.00781 -0.01323 0.00512 AFIX 43 H14A 2 0.759850 1.372449 0.630917 11.00000 -1.20000 AFIX 0 C15 1 0.621325 1.335228 0.690889 11.00000 0.03436 0.03053 = 0.02890 -0.01581 -0.01564 0.01414 AFIX 43 H15A 2 0.611002 1.377792 0.710709 11.00000 -1.20000 AFIX 0 C16 1 0.550770 1.278355 0.708446 11.00000 0.02725 0.04391 = 0.02338 -0.01650 -0.00823 0.01466 AFIX 43 H16A 2 0.491370 1.281462 0.740641 11.00000 -1.20000 AFIX 0 C17 1 0.562967 1.214583 0.680273 11.00000 0.02438 0.03343 = 0.01758 -0.00642 -0.00459 0.00946 C18 1 0.492049 1.154083 0.699522 11.00000 0.02309 0.04519 = 0.02022 -0.00381 0.00418 0.00886 AFIX 43 H18A 2 0.431160 1.157052 0.731289 11.00000 -1.20000 AFIX 0 C19 1 0.509476 1.092351 0.673532 11.00000 0.01925 0.03841 = 0.01983 -0.00157 0.00380 0.00024 AFIX 43 H19A 2 0.463548 1.051814 0.687349 11.00000 -1.20000 AFIX 0 C20 1 0.596778 1.089050 0.625651 11.00000 0.01719 0.02801 = 0.01563 -0.00779 0.00153 0.00246 C21 1 0.775324 0.926573 0.558297 11.00000 0.01769 0.01714 = 0.01600 -0.00204 0.00336 -0.00265 C22 1 0.689228 0.939101 0.510783 11.00000 0.02717 0.01883 = 0.01930 0.00204 0.00039 0.00324 AFIX 43 H22A 2 0.622653 0.976270 0.511109 11.00000 -1.20000 AFIX 0 C23 1 0.701502 0.897809 0.464273 11.00000 0.02807 0.02525 = 0.01600 0.00145 -0.00434 0.00186 AFIX 43 H23A 2 0.642662 0.906491 0.432589 11.00000 -1.20000 AFIX 0 C24 1 0.799244 0.843013 0.462586 11.00000 0.01856 0.02376 = 0.01776 -0.00168 0.00004 -0.00315 C25 1 0.814569 0.800072 0.413988 11.00000 0.02918 0.03087 = 0.01520 -0.00170 -0.00174 0.00130 AFIX 43 H25A 2 0.756402 0.808122 0.382002 11.00000 -1.20000 AFIX 0 C26 1 0.911752 0.747833 0.413240 11.00000 0.03316 0.03222 = 0.02024 -0.00736 0.00188 0.00037 AFIX 43 H26A 2 0.922692 0.720462 0.380310 11.00000 -1.20000 AFIX 0 C27 1 0.995833 0.733841 0.460283 11.00000 0.02921 0.03362 = 0.03145 -0.01015 -0.00048 0.01196 AFIX 43 H27A 2 1.061685 0.696382 0.459360 11.00000 -1.20000 AFIX 0 C28 1 0.984140 0.773610 0.507641 11.00000 0.02558 0.03683 = 0.02217 -0.00518 -0.00327 0.00694 AFIX 43 H28A 2 1.042935 0.763807 0.539125 11.00000 -1.20000 AFIX 0 C29 1 0.885821 0.829098 0.510423 11.00000 0.01698 0.02470 = 0.01968 -0.00170 0.00145 0.00064 C30 1 0.872124 0.872588 0.559003 11.00000 0.01289 0.02909 = 0.01609 -0.00228 -0.00078 0.00050 C31 1 0.965792 0.856528 0.608607 11.00000 0.02032 0.04156 = 0.02033 -0.01467 -0.00397 0.01103 C32 1 0.928249 0.801088 0.645177 11.00000 0.03398 0.04387 = 0.01567 -0.00689 -0.00608 0.02333 C33 1 0.801091 0.762715 0.640452 11.00000 0.03884 0.04245 = 0.02134 0.00274 0.00169 0.01277 AFIX 43 H33A 2 0.736290 0.774073 0.611227 11.00000 -1.20000 AFIX 0 C34 1 0.767705 0.710113 0.676106 11.00000 0.06544 0.04234 = 0.03313 0.00770 0.00596 0.01293 AFIX 43 H34A 2 0.680049 0.686037 0.671933 11.00000 -1.20000 AFIX 0 C35 1 0.862847 0.691057 0.719382 11.00000 0.08604 0.06045 = 0.03581 0.01441 0.00882 0.03481 AFIX 43 H35A 2 0.839569 0.654148 0.744249 11.00000 -1.20000 AFIX 0 C36 1 0.985005 0.725030 0.725104 11.00000 0.07838 0.07489 = 0.01938 0.00557 -0.00795 0.05125 AFIX 43 H36A 2 1.048394 0.711654 0.754254 11.00000 -1.20000 AFIX 0 C37 1 1.024352 0.781141 0.688805 11.00000 0.04497 0.06845 = 0.01873 -0.01138 -0.01193 0.03357 C38 1 1.151860 0.816116 0.693394 11.00000 0.05359 0.08908 = 0.02240 -0.02010 -0.01908 0.04303 AFIX 43 H38A 2 1.216751 0.802457 0.721938 11.00000 -1.20000 AFIX 0 C39 1 1.188772 0.869613 0.658588 11.00000 0.02144 0.08807 = 0.04436 -0.04437 -0.01627 0.01819 AFIX 43 H39A 2 1.276739 0.893192 0.663528 11.00000 -1.20000 AFIX 0 C40 1 1.093861 0.889676 0.614773 11.00000 0.02322 0.05168 = 0.03173 -0.01860 -0.00526 0.00896 C48 1 0.709631 0.949294 0.797850 11.00000 0.03715 0.04290 = 0.01358 -0.00097 0.00248 -0.01767 AFIX 13 H48A 2 0.609661 0.934216 0.805575 11.00000 -1.20000 AFIX 0 C45 1 0.861298 1.048349 0.734343 11.00000 0.03169 0.02734 = 0.02309 -0.00994 0.00035 -0.01063 AFIX 13 H45A 2 0.866788 1.084962 0.704606 11.00000 -1.20000 AFIX 0 C46 1 0.796510 1.073572 0.789168 11.00000 0.03765 0.03540 = 0.03105 -0.01850 0.00109 -0.00349 AFIX 23 H46A 2 0.709830 1.100896 0.780694 11.00000 -1.20000 H46B 2 0.865067 1.104894 0.808056 11.00000 -1.20000 AFIX 0 C43 1 1.036568 0.961557 0.780558 11.00000 0.02525 0.05964 = 0.02937 -0.01738 -0.00769 -0.00103 AFIX 23 H43A 2 1.043364 0.996060 0.811294 11.00000 -1.20000 H43B 2 1.134668 0.947504 0.770471 11.00000 -1.20000 AFIX 0 C47 1 0.757080 1.014094 0.829673 11.00000 0.03838 0.05540 = 0.02587 -0.01968 0.00684 -0.01271 AFIX 23 H47A 2 0.840538 1.002593 0.853300 11.00000 -1.20000 H47B 2 0.679338 1.029627 0.854784 11.00000 -1.20000 AFIX 0 C49 1 0.802539 0.896399 0.786361 11.00000 0.04061 0.03821 = 0.01847 0.00429 -0.00490 -0.00686 AFIX 13 H49A 2 0.758581 0.849061 0.786893 11.00000 -1.20000 AFIX 0 C44 1 0.967961 0.996357 0.729643 11.00000 0.02065 0.04319 = 0.02367 -0.01298 0.00217 -0.01325 AFIX 13 H44A 2 1.034171 1.003158 0.697217 11.00000 -1.20000 AFIX 0 C42 1 0.956557 0.897687 0.802293 11.00000 0.04408 0.05112 = 0.02745 -0.00606 -0.01230 0.00904 AFIX 23 H42A 2 1.003076 0.855352 0.787393 11.00000 -1.20000 H42B 2 0.964197 0.896342 0.843751 11.00000 -1.20000 AFIX 0 C41 1 1.247520 0.981921 0.587327 11.00000 0.03733 0.11286 = 0.07690 -0.02708 0.00176 -0.03739 AFIX 33 H41A 2 1.257609 1.016774 0.557571 11.00000 -1.50000 H41B 2 1.332970 0.952737 0.588501 11.00000 -1.50000 H41C 2 1.235398 1.005332 0.623571 11.00000 -1.50000 HKLF 4 REM ljh149 in P2(1)2(1)2(1) REM R1 = 0.0218 for 8788 Fo > 4sig(Fo) and 0.0234 for all 9076 data REM 496 parameters refined using 0 restraints END WGHT 0.0297 2.3785 REM Highest difference peak 0.841, deepest hole -0.907, 1-sigma level 0.080 Q1 1 1.3609 0.9979 0.4404 11.00000 0.05 0.84 Q2 1 0.7049 0.9582 0.6635 11.00000 0.05 0.76 Q3 1 0.7374 0.9912 0.6934 11.00000 0.05 0.61 Q4 1 0.8291 0.9568 0.7412 11.00000 0.05 0.59 Q5 1 0.4042 1.0595 0.9005 11.00000 0.05 0.55 Q6 1 0.8277 0.9584 0.6649 11.00000 0.05 0.48 Q7 1 0.6997 0.9572 0.7468 11.00000 0.05 0.46 Q8 1 0.7922 0.8973 0.7291 11.00000 0.05 0.41 Q9 1 0.8648 0.9158 0.7086 11.00000 0.05 0.40 Q10 1 0.7606 1.5024 0.5698 11.00000 0.05 0.37 ; data_ljh97_3a _database_code_depnum_ccdc_archive 'CCDC 911753' #TrackingRef 'combined.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H39 Cl P O3 Rh, C4 H10 O' _chemical_formula_sum 'C53 H49 Cl O4 P Rh' _chemical_formula_weight 919.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.5919(3) _cell_length_b 19.2348(5) _cell_length_c 23.6141(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4356.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11308 _cell_measurement_theta_min 2.9933 _cell_measurement_theta_max 28.4719 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.537 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8139 _exptl_absorpt_correction_T_max 0.9002 _exptl_absorpt_process_details ; 'Fri Jun 17 15:05:29 2011' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube with Enhance optics' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_reflns_number 25484 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 28.53 _reflns_number_total 9385 _reflns_number_gt 8683 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+2.1824P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(2) _chemical_absolute_configuration ad _refine_ls_number_reflns 9385 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.73025(2) 0.449885(11) 0.789821(8) 0.01955(6) Uani 1 1 d . . . Cl Cl 0.93215(8) 0.38827(4) 0.81801(3) 0.02449(16) Uani 1 1 d . . . P P 0.72283(8) 0.48359(3) 0.87930(3) 0.01713(14) Uani 1 1 d . . . O1 O 0.8652(2) 0.52338(10) 0.89856(8) 0.0193(4) Uani 1 1 d . . . O2 O 0.6079(2) 0.54366(10) 0.89205(8) 0.0197(4) Uani 1 1 d . . . O3 O 0.3719(3) 0.43236(12) 0.91205(10) 0.0367(6) Uani 1 1 d . . . O4 O 0.2373(4) 0.51322(17) 1.0685(2) 0.1123(17) Uani 1 1 d . . . C1 C 0.8865(3) 0.58740(15) 0.87197(11) 0.0195(6) Uani 1 1 d . . . C2 C 0.9779(3) 0.58903(16) 0.82542(12) 0.0245(6) Uani 1 1 d . . . H2A H 1.0242 0.5482 0.8129 0.029 Uiso 1 1 calc R . . C3 C 0.9977(3) 0.65079(16) 0.79897(12) 0.0249(6) Uani 1 1 d . . . H3A H 1.0607 0.6533 0.7680 0.030 Uiso 1 1 calc R . . C4 C 0.9272(3) 0.71131(15) 0.81630(12) 0.0222(6) Uani 1 1 d . . . C5 C 0.9467(3) 0.77570(15) 0.78760(13) 0.0251(6) Uani 1 1 d . . . H5A H 1.0088 0.7781 0.7563 0.030 Uiso 1 1 calc R . . C6 C 0.8776(3) 0.83346(16) 0.80447(13) 0.0281(7) Uani 1 1 d . . . H6A H 0.8923 0.8761 0.7851 0.034 Uiso 1 1 calc R . . C7 C 0.7842(4) 0.83086(15) 0.85042(12) 0.0273(7) Uani 1 1 d . . . H7A H 0.7365 0.8718 0.8619 0.033 Uiso 1 1 calc R . . C8 C 0.7619(4) 0.76999(14) 0.87842(11) 0.0239(6) Uani 1 1 d . . . H8A H 0.6966 0.7685 0.9086 0.029 Uiso 1 1 calc R . . C9 C 0.8348(3) 0.70898(15) 0.86316(11) 0.0208(6) Uani 1 1 d . . . C10 C 0.8177(3) 0.64393(15) 0.89206(11) 0.0206(6) Uani 1 1 d . . . C11 C 0.7238(3) 0.63488(13) 0.94201(11) 0.0202(6) Uani 1 1 d . . . C12 C 0.7404(3) 0.67391(13) 0.99328(11) 0.0206(6) Uani 1 1 d . . . C13 C 0.8488(4) 0.72239(15) 1.00157(12) 0.0256(7) Uani 1 1 d . . . H13A H 0.9139 0.7303 0.9719 0.031 Uiso 1 1 calc R . . C14 C 0.8625(4) 0.75812(16) 1.05099(13) 0.0323(8) Uani 1 1 d . . . H14A H 0.9372 0.7900 1.0557 0.039 Uiso 1 1 calc R . . C15 C 0.7654(4) 0.74772(16) 1.09545(12) 0.0349(8) Uani 1 1 d . . . H15A H 0.7727 0.7739 1.1295 0.042 Uiso 1 1 calc R . . C16 C 0.6628(4) 0.70058(16) 1.08922(13) 0.0303(8) Uani 1 1 d . . . H16A H 0.5995 0.6933 1.1196 0.036 Uiso 1 1 calc R . . C17 C 0.6463(4) 0.66149(15) 1.03889(12) 0.0251(7) Uani 1 1 d . . . C18 C 0.5424(3) 0.61041(15) 1.03338(12) 0.0253(7) Uani 1 1 d . . . H18A H 0.4789 0.6030 1.0636 0.030 Uiso 1 1 calc R . . C19 C 0.5312(3) 0.57126(15) 0.98546(12) 0.0236(6) Uani 1 1 d . . . H19A H 0.4623 0.5360 0.9825 0.028 Uiso 1 1 calc R . . C20 C 0.6238(3) 0.58436(14) 0.94070(11) 0.0187(6) Uani 1 1 d . . . C21 C 0.7100(3) 0.42476(14) 0.93889(10) 0.0190(6) Uani 1 1 d . . . C22 C 0.7890(3) 0.43919(14) 0.98825(11) 0.0212(6) Uani 1 1 d . . . H22A H 0.8495 0.4783 0.9889 0.025 Uiso 1 1 calc R . . C23 C 0.7790(4) 0.39782(15) 1.03463(11) 0.0248(6) Uani 1 1 d . . . H23A H 0.8341 0.4079 1.0670 0.030 Uiso 1 1 calc R . . C24 C 0.6888(3) 0.34048(15) 1.03558(11) 0.0210(6) Uani 1 1 d . . . C25 C 0.6756(4) 0.29753(17) 1.08371(13) 0.0305(8) Uani 1 1 d . . . H25A H 0.7303 0.3070 1.1164 0.037 Uiso 1 1 calc R . . C26 C 0.5859(4) 0.24286(19) 1.08414(13) 0.0344(8) Uani 1 1 d . . . H26A H 0.5772 0.2149 1.1171 0.041 Uiso 1 1 calc R . . C27 C 0.5065(4) 0.22779(18) 1.03601(13) 0.0326(8) Uani 1 1 d . . . H27A H 0.4448 0.1891 1.0364 0.039 Uiso 1 1 calc R . . C28 C 0.5163(4) 0.26753(17) 0.98877(13) 0.0309(8) Uani 1 1 d . . . H28A H 0.4609 0.2565 0.9566 0.037 Uiso 1 1 calc R . . C29 C 0.6079(3) 0.32522(15) 0.98667(12) 0.0220(6) Uani 1 1 d . . . C30 C 0.6215(3) 0.36858(15) 0.93746(11) 0.0204(6) Uani 1 1 d . . . C31 C 0.5367(3) 0.34885(16) 0.88652(12) 0.0239(7) Uani 1 1 d . . . C32 C 0.5805(3) 0.29210(15) 0.85185(12) 0.0241(7) Uani 1 1 d . . . C33 C 0.7083(4) 0.25821(16) 0.85895(12) 0.0292(7) Uani 1 1 d . . . H33A H 0.7692 0.2731 0.8883 0.035 Uiso 1 1 calc R . . C34 C 0.7480(4) 0.20446(16) 0.82497(13) 0.0367(8) Uani 1 1 d . . . H34A H 0.8362 0.1830 0.8305 0.044 Uiso 1 1 calc R . . C35 C 0.6591(4) 0.18072(19) 0.78190(16) 0.0433(9) Uani 1 1 d . . . H35A H 0.6864 0.1429 0.7585 0.052 Uiso 1 1 calc R . . C36 C 0.5354(4) 0.21174(19) 0.77390(13) 0.0387(9) Uani 1 1 d . . . H36A H 0.4763 0.1955 0.7445 0.046 Uiso 1 1 calc R . . C37 C 0.4903(4) 0.26804(17) 0.80813(12) 0.0308(8) Uani 1 1 d . . . C38 C 0.3627(4) 0.30037(19) 0.80056(13) 0.0363(8) Uani 1 1 d . . . H38A H 0.3021 0.2839 0.7717 0.044 Uiso 1 1 calc R . . C39 C 0.3212(4) 0.35473(19) 0.83292(14) 0.0340(8) Uani 1 1 d . . . H39A H 0.2337 0.3763 0.8263 0.041 Uiso 1 1 calc R . . C40 C 0.4094(4) 0.37905(16) 0.87671(13) 0.0278(7) Uani 1 1 d . . . C41 C 0.2506(5) 0.4708(2) 0.89759(19) 0.0601(12) Uani 1 1 d . . . H41A H 0.2347 0.5070 0.9260 0.090 Uiso 1 1 calc R . . H41B H 0.1700 0.4395 0.8965 0.090 Uiso 1 1 calc R . . H41C H 0.2634 0.4923 0.8603 0.090 Uiso 1 1 calc R . . C42 C 0.7059(3) 0.38909(16) 0.70974(12) 0.0311(7) Uani 1 1 d . . . H42A H 0.7531 0.3427 0.7100 0.037 Uiso 1 1 calc R . . C43 C 0.7914(4) 0.44333(18) 0.69808(11) 0.0326(7) Uani 1 1 d . . . H43A H 0.8910 0.4302 0.6914 0.039 Uiso 1 1 calc R . . C44 C 0.7444(4) 0.50653(18) 0.66637(12) 0.0380(8) Uani 1 1 d . . . H44A H 0.6641 0.4941 0.6420 0.046 Uiso 1 1 calc R . . H44B H 0.8208 0.5227 0.6415 0.046 Uiso 1 1 calc R . . C45 C 0.7023(4) 0.56508(16) 0.70576(13) 0.0360(8) Uani 1 1 d . . . H45A H 0.7862 0.5927 0.7153 0.043 Uiso 1 1 calc R . . H45B H 0.6367 0.5961 0.6855 0.043 Uiso 1 1 calc R . . C46 C 0.6345(3) 0.54099(16) 0.75997(13) 0.0272(7) Uani 1 1 d . . . H46A H 0.6252 0.5783 0.7892 0.033 Uiso 1 1 calc R . . C47 C 0.5338(4) 0.48871(16) 0.76412(13) 0.0281(7) Uani 1 1 d . . . H47A H 0.4668 0.4956 0.7961 0.034 Uiso 1 1 calc R . . C48 C 0.4716(3) 0.45109(19) 0.71383(13) 0.0356(7) Uani 1 1 d . . . H48A H 0.4649 0.4841 0.6818 0.043 Uiso 1 1 calc R . . H48B H 0.3757 0.4364 0.7236 0.043 Uiso 1 1 calc R . . C49 C 0.5546(4) 0.38675(18) 0.69437(14) 0.0363(8) Uani 1 1 d . . . H49A H 0.5124 0.3447 0.7115 0.044 Uiso 1 1 calc R . . H49B H 0.5462 0.3824 0.6527 0.044 Uiso 1 1 calc R . . C50 C 0.2812(9) 0.4417(4) 1.0810(4) 0.168(4) Uani 1 1 d . . . H50A H 0.2104 0.4173 1.1041 0.201 Uiso 1 1 calc R . . H50B H 0.2971 0.4152 1.0456 0.201 Uiso 1 1 calc R . . C51 C 0.4009(7) 0.4497(4) 1.1101(6) 0.243(8) Uani 1 1 d . . . H51A H 0.4228 0.4066 1.1303 0.365 Uiso 1 1 calc R . . H51B H 0.3903 0.4877 1.1375 0.365 Uiso 1 1 calc R . . H51C H 0.4767 0.4608 1.0838 0.365 Uiso 1 1 calc R . . C52 C 0.1180(5) 0.5127(3) 1.0435(2) 0.0723(15) Uani 1 1 d . . . H52A H 0.0437 0.4997 1.0706 0.087 Uiso 1 1 calc R . . H52B H 0.1184 0.4784 1.0123 0.087 Uiso 1 1 calc R . . C53 C 0.0904(7) 0.5869(3) 1.0197(2) 0.0807(17) Uani 1 1 d . . . H53A H 0.0019 0.5872 0.9989 0.121 Uiso 1 1 calc R . . H53B H 0.1663 0.6000 0.9940 0.121 Uiso 1 1 calc R . . H53C H 0.0855 0.6202 1.0510 0.121 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh 0.02237(12) 0.02200(10) 0.01427(9) 0.00122(9) -0.00101(8) 0.00473(9) Cl 0.0253(4) 0.0271(4) 0.0211(3) -0.0016(3) -0.0020(3) 0.0084(3) P 0.0181(4) 0.0177(3) 0.0156(3) 0.0013(3) -0.0001(3) 0.0011(3) O1 0.0193(11) 0.0187(9) 0.0197(9) 0.0020(8) 0.0000(8) -0.0008(8) O2 0.0197(11) 0.0187(9) 0.0206(9) -0.0027(9) 0.0008(8) 0.0012(9) O3 0.0252(13) 0.0412(14) 0.0436(13) 0.0032(11) -0.0060(10) 0.0020(10) O4 0.050(2) 0.0553(19) 0.232(5) 0.038(3) -0.014(3) 0.0032(19) C1 0.0199(16) 0.0225(14) 0.0161(13) 0.0016(11) 0.0002(11) -0.0044(12) C2 0.0209(16) 0.0313(16) 0.0212(14) -0.0010(12) 0.0023(12) 0.0009(13) C3 0.0199(15) 0.0358(16) 0.0189(14) 0.0028(13) 0.0052(12) -0.0046(13) C4 0.0227(17) 0.0278(15) 0.0160(13) 0.0040(12) -0.0039(12) -0.0065(13) C5 0.0203(15) 0.0367(16) 0.0184(13) 0.0073(14) -0.0026(13) -0.0119(12) C6 0.0277(18) 0.0288(15) 0.0278(16) 0.0141(13) -0.0110(13) -0.0104(13) C7 0.0315(18) 0.0225(14) 0.0278(14) 0.0053(12) -0.0105(14) -0.0021(13) C8 0.0245(17) 0.0255(13) 0.0215(12) 0.0020(11) -0.0015(13) -0.0022(13) C9 0.0208(16) 0.0232(14) 0.0183(13) 0.0033(12) -0.0031(12) -0.0060(12) C10 0.0225(16) 0.0253(14) 0.0139(12) 0.0010(11) 0.0008(11) -0.0039(12) C11 0.0251(15) 0.0167(12) 0.0188(12) 0.0019(10) 0.0039(12) 0.0006(12) C12 0.0259(18) 0.0171(12) 0.0187(12) 0.0025(10) 0.0038(12) 0.0015(13) C13 0.035(2) 0.0221(14) 0.0195(14) 0.0018(12) 0.0021(13) -0.0033(14) C14 0.043(2) 0.0268(16) 0.0273(16) 0.0008(14) -0.0022(15) -0.0086(15) C15 0.053(2) 0.0321(16) 0.0199(13) -0.0045(12) 0.0007(16) -0.0027(17) C16 0.042(2) 0.0291(16) 0.0196(14) 0.0020(13) 0.0113(14) 0.0084(15) C17 0.0334(19) 0.0212(14) 0.0208(14) 0.0036(12) 0.0051(13) 0.0047(13) C18 0.0283(18) 0.0242(14) 0.0233(14) 0.0024(12) 0.0119(13) 0.0026(13) C19 0.0244(17) 0.0198(14) 0.0265(15) 0.0013(12) 0.0076(13) 0.0011(12) C20 0.0196(15) 0.0190(13) 0.0176(13) 0.0009(11) 0.0032(11) 0.0027(12) C21 0.0223(16) 0.0192(12) 0.0154(12) -0.0003(10) 0.0019(11) 0.0006(12) C22 0.0246(16) 0.0191(13) 0.0201(12) -0.0042(11) -0.0006(11) -0.0028(12) C23 0.0318(17) 0.0290(14) 0.0135(11) -0.0019(11) -0.0036(13) -0.0012(14) C24 0.0206(17) 0.0245(14) 0.0178(13) 0.0000(12) 0.0004(11) -0.0006(12) C25 0.038(2) 0.0363(18) 0.0171(14) 0.0042(13) -0.0021(13) -0.0044(15) C26 0.038(2) 0.0412(19) 0.0237(15) 0.0128(14) -0.0003(15) -0.0079(16) C27 0.031(2) 0.0367(18) 0.0299(16) 0.0112(14) -0.0029(14) -0.0149(15) C28 0.030(2) 0.0398(19) 0.0228(16) 0.0086(14) -0.0043(13) -0.0109(15) C29 0.0222(17) 0.0268(15) 0.0171(13) 0.0043(12) 0.0000(12) -0.0028(13) C30 0.0195(16) 0.0235(14) 0.0183(13) 0.0017(12) -0.0002(11) 0.0002(12) C31 0.0250(18) 0.0288(15) 0.0181(13) 0.0077(12) -0.0054(12) -0.0056(14) C32 0.0256(17) 0.0281(15) 0.0187(13) 0.0048(12) -0.0031(12) -0.0103(13) C33 0.033(2) 0.0293(15) 0.0249(14) 0.0050(13) -0.0052(14) -0.0056(14) C34 0.042(2) 0.0345(16) 0.0336(16) -0.0016(13) 0.0033(16) -0.0019(17) C35 0.054(3) 0.0386(19) 0.038(2) -0.0102(17) 0.0079(18) -0.0092(17) C36 0.047(2) 0.048(2) 0.0214(16) -0.0074(14) -0.0019(15) -0.0197(18) C37 0.0314(19) 0.0406(18) 0.0205(14) 0.0081(13) -0.0068(13) -0.0146(15) C38 0.035(2) 0.051(2) 0.0231(16) 0.0035(15) -0.0095(14) -0.0162(16) C39 0.0211(17) 0.050(2) 0.0313(16) 0.0154(16) -0.0086(13) -0.0048(15) C40 0.0255(18) 0.0289(16) 0.0289(15) 0.0069(13) -0.0010(13) -0.0044(13) C41 0.036(3) 0.075(3) 0.069(3) -0.009(2) -0.006(2) 0.023(2) C42 0.041(2) 0.0388(16) 0.0135(12) -0.0107(14) -0.0066(14) 0.0102(14) C43 0.0380(19) 0.0447(18) 0.0153(13) -0.0012(13) 0.0026(12) 0.0170(17) C44 0.040(2) 0.053(2) 0.0220(14) 0.0116(14) 0.0009(15) 0.0051(18) C45 0.041(2) 0.0370(17) 0.0294(15) 0.0172(15) -0.0027(15) 0.0040(14) C46 0.0319(18) 0.0256(15) 0.0241(14) 0.0053(13) -0.0032(12) 0.0079(14) C47 0.0274(18) 0.0345(16) 0.0224(14) 0.0058(13) -0.0026(13) 0.0105(14) C48 0.0286(17) 0.0492(18) 0.0290(15) 0.0059(18) -0.0072(14) 0.0008(16) C49 0.040(2) 0.0419(19) 0.0267(16) 0.0002(14) -0.0089(14) -0.0014(16) C50 0.124(7) 0.102(5) 0.276(11) 0.135(7) 0.051(8) 0.023(5) C51 0.041(4) 0.129(6) 0.56(2) 0.227(10) -0.081(7) -0.035(4) C52 0.048(3) 0.100(4) 0.068(3) -0.032(3) 0.008(2) -0.022(3) C53 0.086(4) 0.068(3) 0.088(4) -0.015(3) -0.029(3) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh Cl 2.3661(8) . ? Rh P 2.2112(7) . ? Rh C42 2.236(3) . ? Rh C43 2.248(3) . ? Rh C46 2.100(3) . ? Rh C47 2.116(3) . ? P O1 1.630(2) . ? P O2 1.625(2) . ? P C21 1.810(3) . ? O1 C1 1.397(3) . ? O2 C20 1.398(3) . ? O3 C40 1.370(4) . ? O3 C41 1.420(5) . ? O4 C50 1.468(7) . ? O4 C52 1.288(7) . ? C1 C2 1.406(4) . ? C1 C10 1.357(4) . ? C2 H2A 0.950 . ? C2 C3 1.355(4) . ? C3 H3A 0.950 . ? C3 C4 1.407(4) . ? C4 C5 1.424(4) . ? C4 C9 1.419(4) . ? C5 H5A 0.950 . ? C5 C6 1.353(5) . ? C6 H6A 0.950 . ? C6 C7 1.408(5) . ? C7 H7A 0.950 . ? C7 C8 1.361(4) . ? C8 H8A 0.950 . ? C8 C9 1.412(4) . ? C9 C10 1.435(4) . ? C10 C11 1.494(4) . ? C11 C12 1.433(4) . ? C11 C20 1.366(4) . ? C12 C13 1.411(4) . ? C12 C17 1.425(4) . ? C13 H13A 0.950 . ? C13 C14 1.361(4) . ? C14 H14A 0.950 . ? C14 C15 1.418(5) . ? C15 H15A 0.950 . ? C15 C16 1.346(5) . ? C16 H16A 0.950 . ? C16 C17 1.415(4) . ? C17 C18 1.405(4) . ? C18 H18A 0.950 . ? C18 C19 1.363(4) . ? C19 H19A 0.950 . ? C19 C20 1.403(4) . ? C21 C22 1.418(4) . ? C21 C30 1.374(4) . ? C22 H22A 0.950 . ? C22 C23 1.357(4) . ? C23 H23A 0.950 . ? C23 C24 1.402(4) . ? C24 C25 1.411(4) . ? C24 C29 1.422(4) . ? C25 H25A 0.950 . ? C25 C26 1.358(5) . ? C26 H26A 0.950 . ? C26 C27 1.399(5) . ? C27 H27A 0.950 . ? C27 C28 1.356(4) . ? C28 H28A 0.950 . ? C28 C29 1.416(4) . ? C29 C30 1.436(4) . ? C30 C31 1.501(4) . ? C31 C32 1.428(4) . ? C31 C40 1.372(5) . ? C32 C33 1.398(5) . ? C32 C37 1.424(4) . ? C33 H33A 0.950 . ? C33 C34 1.363(4) . ? C34 H34A 0.950 . ? C34 C35 1.404(5) . ? C35 H35A 0.950 . ? C35 C36 1.341(6) . ? C36 H36A 0.950 . ? C36 C37 1.419(5) . ? C37 C38 1.385(5) . ? C38 H38A 0.950 . ? C38 C39 1.355(5) . ? C39 H39A 0.950 . ? C39 C40 1.415(5) . ? C41 H41A 0.980 . ? C41 H41B 0.980 . ? C41 H41C 0.980 . ? C42 H42A 1.000 . ? C42 C43 1.356(5) . ? C42 C49 1.497(5) . ? C43 H43A 1.000 . ? C43 C44 1.498(4) . ? C44 H44A 0.990 . ? C44 H44B 0.990 . ? C44 C45 1.515(5) . ? C45 H45A 0.990 . ? C45 H45B 0.990 . ? C45 C46 1.508(4) . ? C46 H46A 1.000 . ? C46 C47 1.398(5) . ? C47 H47A 1.000 . ? C47 C48 1.513(4) . ? C48 H48A 0.990 . ? C48 H48B 0.990 . ? C48 C49 1.542(5) . ? C49 H49A 0.990 . ? C49 H49B 0.990 . ? C50 H50A 0.990 . ? C50 H50B 0.990 . ? C50 C51 1.348(12) . ? C51 H51A 0.980 . ? C51 H51B 0.980 . ? C51 H51C 0.980 . ? C52 H52A 0.990 . ? C52 H52B 0.990 . ? C52 C53 1.556(7) . ? C53 H53A 0.980 . ? C53 H53B 0.980 . ? C53 H53C 0.980 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl Rh P 84.51(3) . . ? Cl Rh C42 93.53(8) . . ? Cl Rh C43 91.68(8) . . ? Cl Rh C46 150.48(9) . . ? Cl Rh C47 170.55(9) . . ? P Rh C42 163.38(9) . . ? P Rh C43 161.03(10) . . ? P Rh C46 93.56(9) . . ? P Rh C47 98.16(9) . . ? C42 Rh C43 35.20(12) . . ? C42 Rh C46 96.13(12) . . ? C42 Rh C47 81.31(12) . . ? C43 Rh C46 80.65(12) . . ? C43 Rh C47 88.62(12) . . ? C46 Rh C47 38.73(13) . . ? Rh P O1 112.17(8) . . ? Rh P O2 114.04(7) . . ? Rh P C21 124.18(9) . . ? O1 P O2 100.52(10) . . ? O1 P C21 97.68(12) . . ? O2 P C21 104.73(12) . . ? P O1 C1 114.27(18) . . ? P O2 C20 118.47(17) . . ? C40 O3 C41 117.3(3) . . ? C50 O4 C52 109.9(6) . . ? O1 C1 C2 117.5(3) . . ? O1 C1 C10 118.5(2) . . ? C2 C1 C10 123.9(3) . . ? C1 C2 H2A 121.1 . . ? C1 C2 C3 117.8(3) . . ? H2A C2 C3 121.1 . . ? C2 C3 H3A 119.2 . . ? C2 C3 C4 121.6(3) . . ? H3A C3 C4 119.2 . . ? C3 C4 C5 121.2(3) . . ? C3 C4 C9 120.1(3) . . ? C5 C4 C9 118.7(3) . . ? C4 C5 H5A 119.7 . . ? C4 C5 C6 120.6(3) . . ? H5A C5 C6 119.7 . . ? C5 C6 H6A 119.7 . . ? C5 C6 C7 120.6(3) . . ? H6A C6 C7 119.7 . . ? C6 C7 H7A 119.9 . . ? C6 C7 C8 120.3(3) . . ? H7A C7 C8 119.9 . . ? C7 C8 H8A 119.6 . . ? C7 C8 C9 120.9(3) . . ? H8A C8 C9 119.6 . . ? C4 C9 C8 118.8(3) . . ? C4 C9 C10 118.0(3) . . ? C8 C9 C10 123.2(3) . . ? C1 C10 C9 118.5(3) . . ? C1 C10 C11 118.4(2) . . ? C9 C10 C11 123.1(3) . . ? C10 C11 C12 122.6(3) . . ? C10 C11 C20 119.2(2) . . ? C12 C11 C20 118.0(3) . . ? C11 C12 C13 123.0(3) . . ? C11 C12 C17 118.7(3) . . ? C13 C12 C17 118.2(3) . . ? C12 C13 H13A 119.2 . . ? C12 C13 C14 121.6(3) . . ? H13A C13 C14 119.2 . . ? C13 C14 H14A 120.0 . . ? C13 C14 C15 120.0(3) . . ? H14A C14 C15 120.0 . . ? C14 C15 H15A 120.2 . . ? C14 C15 C16 119.6(3) . . ? H15A C15 C16 120.2 . . ? C15 C16 H16A 118.9 . . ? C15 C16 C17 122.1(3) . . ? H16A C16 C17 118.9 . . ? C12 C17 C16 118.3(3) . . ? C12 C17 C18 119.7(3) . . ? C16 C17 C18 121.9(3) . . ? C17 C18 H18A 119.4 . . ? C17 C18 C19 121.3(3) . . ? H18A C18 C19 119.4 . . ? C18 C19 H19A 120.8 . . ? C18 C19 C20 118.4(3) . . ? H19A C19 C20 120.8 . . ? O2 C20 C11 119.5(2) . . ? O2 C20 C19 116.7(3) . . ? C11 C20 C19 123.7(3) . . ? P C21 C22 118.7(2) . . ? P C21 C30 121.0(2) . . ? C22 C21 C30 120.3(2) . . ? C21 C22 H22A 119.6 . . ? C21 C22 C23 120.7(3) . . ? H22A C22 C23 119.6 . . ? C22 C23 H23A 119.4 . . ? C22 C23 C24 121.2(3) . . ? H23A C23 C24 119.4 . . ? C23 C24 C25 121.9(3) . . ? C23 C24 C29 119.1(3) . . ? C25 C24 C29 119.0(3) . . ? C24 C25 H25A 119.5 . . ? C24 C25 C26 121.1(3) . . ? H25A C25 C26 119.5 . . ? C25 C26 H26A 120.0 . . ? C25 C26 C27 120.0(3) . . ? H26A C26 C27 120.0 . . ? C26 C27 H27A 119.5 . . ? C26 C27 C28 120.9(3) . . ? H27A C27 C28 119.5 . . ? C27 C28 H28A 119.5 . . ? C27 C28 C29 120.9(3) . . ? H28A C28 C29 119.5 . . ? C24 C29 C28 118.1(3) . . ? C24 C29 C30 119.2(3) . . ? C28 C29 C30 122.7(3) . . ? C21 C30 C29 119.5(3) . . ? C21 C30 C31 123.6(2) . . ? C29 C30 C31 116.9(3) . . ? C30 C31 C32 119.6(3) . . ? C30 C31 C40 120.7(3) . . ? C32 C31 C40 119.3(3) . . ? C31 C32 C33 123.1(3) . . ? C31 C32 C37 119.0(3) . . ? C33 C32 C37 117.9(3) . . ? C32 C33 H33A 119.1 . . ? C32 C33 C34 121.9(3) . . ? H33A C33 C34 119.1 . . ? C33 C34 H34A 119.9 . . ? C33 C34 C35 120.2(4) . . ? H34A C34 C35 119.9 . . ? C34 C35 H35A 120.2 . . ? C34 C35 C36 119.7(3) . . ? H35A C35 C36 120.2 . . ? C35 C36 H36A 119.0 . . ? C35 C36 C37 121.9(3) . . ? H36A C36 C37 119.0 . . ? C32 C37 C36 118.4(3) . . ? C32 C37 C38 119.0(3) . . ? C36 C37 C38 122.6(3) . . ? C37 C38 H38A 118.9 . . ? C37 C38 C39 122.2(3) . . ? H38A C38 C39 118.9 . . ? C38 C39 H39A 120.3 . . ? C38 C39 C40 119.5(3) . . ? H39A C39 C40 120.3 . . ? O3 C40 C31 116.6(3) . . ? O3 C40 C39 122.4(3) . . ? C31 C40 C39 121.0(3) . . ? O3 C41 H41A 109.5 . . ? O3 C41 H41B 109.5 . . ? O3 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Rh C42 H42A 114.4 . . ? Rh C42 C43 72.90(17) . . ? Rh C42 C49 108.8(2) . . ? H42A C42 C43 114.4 . . ? H42A C42 C49 114.4 . . ? C43 C42 C49 124.1(3) . . ? Rh C43 C42 71.91(16) . . ? Rh C43 H43A 114.5 . . ? Rh C43 C44 110.9(2) . . ? C42 C43 H43A 114.5 . . ? C42 C43 C44 122.9(3) . . ? H43A C43 C44 114.5 . . ? C43 C44 H44A 109.2 . . ? C43 C44 H44B 109.2 . . ? C43 C44 C45 112.1(2) . . ? H44A C44 H44B 107.9 . . ? H44A C44 C45 109.2 . . ? H44B C44 C45 109.2 . . ? C44 C45 H45A 108.7 . . ? C44 C45 H45B 108.7 . . ? C44 C45 C46 114.0(3) . . ? H45A C45 H45B 107.6 . . ? H45A C45 C46 108.7 . . ? H45B C45 C46 108.7 . . ? Rh C46 C45 110.7(2) . . ? Rh C46 H46A 113.9 . . ? Rh C46 C47 71.26(17) . . ? C45 C46 H46A 113.9 . . ? C45 C46 C47 125.3(3) . . ? H46A C46 C47 113.9 . . ? Rh C47 C46 70.01(18) . . ? Rh C47 H47A 113.7 . . ? Rh C47 C48 114.0(2) . . ? C46 C47 H47A 113.7 . . ? C46 C47 C48 124.2(3) . . ? H47A C47 C48 113.7 . . ? C47 C48 H48A 108.6 . . ? C47 C48 H48B 108.6 . . ? C47 C48 C49 114.5(3) . . ? H48A C48 H48B 107.6 . . ? H48A C48 C49 108.6 . . ? H48B C48 C49 108.6 . . ? C42 C49 C48 113.8(3) . . ? C42 C49 H49A 108.8 . . ? C42 C49 H49B 108.8 . . ? C48 C49 H49A 108.8 . . ? C48 C49 H49B 108.8 . . ? H49A C49 H49B 107.7 . . ? O4 C50 H50A 111.0 . . ? O4 C50 H50B 111.0 . . ? O4 C50 C51 103.9(7) . . ? H50A C50 H50B 109.0 . . ? H50A C50 C51 111.0 . . ? H50B C50 C51 111.0 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O4 C52 H52A 110.1 . . ? O4 C52 H52B 110.1 . . ? O4 C52 C53 108.1(4) . . ? H52A C52 H52B 108.4 . . ? H52A C52 C53 110.1 . . ? H52B C52 C53 110.1 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl Rh P O1 57.68(8) . . . . ? Cl Rh P O2 171.11(9) . . . . ? Cl Rh P C21 -59.13(13) . . . . ? C42 Rh P O1 141.6(3) . . . . ? C42 Rh P O2 -105.0(3) . . . . ? C42 Rh P C21 24.8(3) . . . . ? C43 Rh P O1 -21.4(3) . . . . ? C43 Rh P O2 92.0(3) . . . . ? C43 Rh P C21 -138.2(3) . . . . ? C46 Rh P O1 -92.77(12) . . . . ? C46 Rh P O2 20.66(13) . . . . ? C46 Rh P C21 150.42(15) . . . . ? C47 Rh P O1 -131.45(12) . . . . ? C47 Rh P O2 -18.02(12) . . . . ? C47 Rh P C21 111.74(15) . . . . ? Rh P O1 C1 66.93(18) . . . . ? O2 P O1 C1 -54.61(19) . . . . ? C21 P O1 C1 -161.23(19) . . . . ? Rh P O2 C20 -159.37(17) . . . . ? O1 P O2 C20 -39.2(2) . . . . ? C21 P O2 C20 61.8(2) . . . . ? P O1 C1 C2 -98.9(3) . . . . ? P O1 C1 C10 80.7(3) . . . . ? O1 C1 C2 C3 179.2(3) . . . . ? C10 C1 C2 C3 -0.3(5) . . . . ? C1 C2 C3 C4 -1.5(5) . . . . ? C2 C3 C4 C5 -178.8(3) . . . . ? C2 C3 C4 C9 1.2(5) . . . . ? C3 C4 C5 C6 179.6(3) . . . . ? C9 C4 C5 C6 -0.4(4) . . . . ? C4 C5 C6 C7 -0.6(5) . . . . ? C5 C6 C7 C8 -0.1(5) . . . . ? C6 C7 C8 C9 1.9(5) . . . . ? C7 C8 C9 C4 -2.9(4) . . . . ? C7 C8 C9 C10 178.5(3) . . . . ? C3 C4 C9 C8 -177.9(3) . . . . ? C3 C4 C9 C10 0.8(4) . . . . ? C5 C4 C9 C8 2.1(4) . . . . ? C5 C4 C9 C10 -179.2(3) . . . . ? O1 C1 C10 C9 -177.2(2) . . . . ? O1 C1 C10 C11 0.6(4) . . . . ? C2 C1 C10 C9 2.3(5) . . . . ? C2 C1 C10 C11 -179.9(3) . . . . ? C4 C9 C10 C1 -2.4(4) . . . . ? C4 C9 C10 C11 179.8(3) . . . . ? C8 C9 C10 C1 176.2(3) . . . . ? C8 C9 C10 C11 -1.5(5) . . . . ? C1 C10 C11 C12 123.1(3) . . . . ? C1 C10 C11 C20 -52.4(4) . . . . ? C9 C10 C11 C12 -59.2(4) . . . . ? C9 C10 C11 C20 125.3(3) . . . . ? C10 C11 C12 C13 -2.0(4) . . . . ? C10 C11 C12 C17 -179.6(3) . . . . ? C20 C11 C12 C13 173.5(3) . . . . ? C20 C11 C12 C17 -4.1(4) . . . . ? C11 C12 C13 C14 -179.3(3) . . . . ? C17 C12 C13 C14 -1.7(5) . . . . ? C12 C13 C14 C15 -0.8(5) . . . . ? C13 C14 C15 C16 2.4(5) . . . . ? C14 C15 C16 C17 -1.3(5) . . . . ? C15 C16 C17 C12 -1.2(5) . . . . ? C15 C16 C17 C18 177.5(3) . . . . ? C11 C12 C17 C16 -179.6(3) . . . . ? C11 C12 C17 C18 1.7(4) . . . . ? C13 C12 C17 C16 2.7(4) . . . . ? C13 C12 C17 C18 -176.0(3) . . . . ? C12 C17 C18 C19 1.3(5) . . . . ? C16 C17 C18 C19 -177.4(3) . . . . ? C17 C18 C19 C20 -1.7(4) . . . . ? C10 C11 C20 O2 -2.1(4) . . . . ? C10 C11 C20 C19 179.5(3) . . . . ? C12 C11 C20 O2 -177.8(2) . . . . ? C12 C11 C20 C19 3.8(4) . . . . ? P O2 C20 C11 74.7(3) . . . . ? P O2 C20 C19 -106.8(3) . . . . ? C18 C19 C20 O2 -179.3(3) . . . . ? C18 C19 C20 C11 -0.9(5) . . . . ? Rh P C21 C22 140.03(19) . . . . ? Rh P C21 C30 -42.5(3) . . . . ? O1 P C21 C22 16.5(2) . . . . ? O1 P C21 C30 -166.0(2) . . . . ? O2 P C21 C22 -86.5(2) . . . . ? O2 P C21 C30 91.0(2) . . . . ? P C21 C22 C23 177.8(2) . . . . ? C30 C21 C22 C23 0.3(4) . . . . ? C21 C22 C23 C24 -1.2(5) . . . . ? C22 C23 C24 C25 -179.0(3) . . . . ? C22 C23 C24 C29 0.8(5) . . . . ? C23 C24 C25 C26 178.9(3) . . . . ? C29 C24 C25 C26 -0.9(5) . . . . ? C24 C25 C26 C27 1.0(6) . . . . ? C25 C26 C27 C28 -0.7(6) . . . . ? C26 C27 C28 C29 0.4(6) . . . . ? C27 C28 C29 C24 -0.3(5) . . . . ? C27 C28 C29 C30 179.9(3) . . . . ? C23 C24 C29 C28 -179.3(3) . . . . ? C23 C24 C29 C30 0.5(4) . . . . ? C25 C24 C29 C28 0.5(5) . . . . ? C25 C24 C29 C30 -179.7(3) . . . . ? P C21 C30 C29 -176.4(2) . . . . ? P C21 C30 C31 3.9(4) . . . . ? C22 C21 C30 C29 1.0(4) . . . . ? C22 C21 C30 C31 -178.6(3) . . . . ? C24 C29 C30 C21 -1.4(4) . . . . ? C24 C29 C30 C31 178.3(3) . . . . ? C28 C29 C30 C21 178.4(3) . . . . ? C28 C29 C30 C31 -1.9(5) . . . . ? C21 C30 C31 C32 102.8(3) . . . . ? C21 C30 C31 C40 -85.1(4) . . . . ? C29 C30 C31 C32 -76.9(4) . . . . ? C29 C30 C31 C40 95.3(4) . . . . ? C30 C31 C32 C33 -7.6(4) . . . . ? C30 C31 C32 C37 171.9(3) . . . . ? C40 C31 C32 C33 -179.8(3) . . . . ? C40 C31 C32 C37 -0.4(4) . . . . ? C31 C32 C33 C34 -179.5(3) . . . . ? C37 C32 C33 C34 1.0(5) . . . . ? C32 C33 C34 C35 -1.0(5) . . . . ? C33 C34 C35 C36 0.8(5) . . . . ? C34 C35 C36 C37 -0.5(5) . . . . ? C35 C36 C37 C32 0.5(5) . . . . ? C35 C36 C37 C38 -179.7(3) . . . . ? C31 C32 C37 C36 179.8(3) . . . . ? C31 C32 C37 C38 0.0(4) . . . . ? C33 C32 C37 C36 -0.7(4) . . . . ? C33 C32 C37 C38 179.5(3) . . . . ? C32 C37 C38 C39 0.8(5) . . . . ? C36 C37 C38 C39 -179.1(3) . . . . ? C37 C38 C39 C40 -1.1(5) . . . . ? C41 O3 C40 C31 171.0(3) . . . . ? C41 O3 C40 C39 -10.3(5) . . . . ? C30 C31 C40 O3 6.6(4) . . . . ? C30 C31 C40 C39 -172.1(3) . . . . ? C32 C31 C40 O3 178.8(3) . . . . ? C32 C31 C40 C39 0.1(5) . . . . ? C38 C39 C40 O3 -177.9(3) . . . . ? C38 C39 C40 C31 0.6(5) . . . . ? Cl Rh C42 C43 -87.91(18) . . . . ? Cl Rh C42 C49 151.1(2) . . . . ? P Rh C42 C43 -170.5(2) . . . . ? P Rh C42 C49 68.5(4) . . . . ? C43 Rh C42 C49 -121.0(3) . . . . ? C46 Rh C42 C43 64.2(2) . . . . ? C46 Rh C42 C49 -56.9(2) . . . . ? C47 Rh C42 C43 100.1(2) . . . . ? C47 Rh C42 C49 -21.0(2) . . . . ? Rh C42 C43 C44 -103.7(3) . . . . ? C49 C42 C43 Rh 101.5(3) . . . . ? C49 C42 C43 C44 -2.2(5) . . . . ? Cl Rh C43 C42 93.74(18) . . . . ? Cl Rh C43 C44 -147.1(2) . . . . ? P Rh C43 C42 171.7(2) . . . . ? P Rh C43 C44 -69.2(4) . . . . ? C42 Rh C43 C44 119.2(3) . . . . ? C46 Rh C43 C42 -114.9(2) . . . . ? C46 Rh C43 C44 4.3(3) . . . . ? C47 Rh C43 C42 -76.8(2) . . . . ? C47 Rh C43 C44 42.4(3) . . . . ? Rh C43 C44 C45 14.5(4) . . . . ? C42 C43 C44 C45 96.0(4) . . . . ? C43 C44 C45 C46 -34.5(4) . . . . ? C44 C45 C46 Rh 37.9(3) . . . . ? C44 C45 C46 C47 -43.3(4) . . . . ? Cl Rh C46 C45 54.6(3) . . . . ? Cl Rh C46 C47 176.24(14) . . . . ? P Rh C46 C45 139.8(2) . . . . ? P Rh C46 C47 -98.61(17) . . . . ? C42 Rh C46 C45 -53.8(2) . . . . ? C42 Rh C46 C47 67.86(19) . . . . ? C43 Rh C46 C45 -22.1(2) . . . . ? C43 Rh C46 C47 99.6(2) . . . . ? C47 Rh C46 C45 -121.6(3) . . . . ? Rh C46 C47 C48 -106.1(3) . . . . ? C45 C46 C47 Rh 102.5(3) . . . . ? C45 C46 C47 C48 -3.6(5) . . . . ? Cl Rh C47 C46 -168.7(4) . . . . ? Cl Rh C47 C48 -49.2(7) . . . . ? P Rh C47 C46 85.50(17) . . . . ? P Rh C47 C48 -155.0(2) . . . . ? C42 Rh C47 C46 -111.30(19) . . . . ? C42 Rh C47 C48 8.2(2) . . . . ? C43 Rh C47 C46 -76.71(19) . . . . ? C43 Rh C47 C48 42.8(2) . . . . ? C46 Rh C47 C48 119.5(3) . . . . ? Rh C47 C48 C49 6.1(4) . . . . ? C46 C47 C48 C49 87.5(4) . . . . ? Rh C42 C49 C48 30.2(3) . . . . ? C43 C42 C49 C48 -51.5(4) . . . . ? C47 C48 C49 C42 -25.0(4) . . . . ? C52 O4 C50 C51 -176.0(8) . . . . ? C50 O4 C52 C53 -168.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.745 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.067 # Contents of RES file _computing_special_details ; TITL ljh97 in P2(1)2(1)2(1) CELL 0.71073 9.5919 19.2348 23.6141 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0005 0.0006 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H O P CL RH UNIT 212 196 16 4 4 4 TEMP -123 L.S. 8 BOND $H CONF FMAP 2 PLAN 5 SIZE 0.40 0.20 0.20 ACTA 50 REM EXTI 0.000000 WGHT 0.034300 2.182400 FVAR 0.24702 RH 6 0.730249 0.449885 0.789821 11.00000 0.02237 0.02200 = 0.01427 0.00122 -0.00101 0.00473 CL 5 0.932151 0.388268 0.818008 11.00000 0.02526 0.02712 = 0.02109 -0.00157 -0.00202 0.00845 P 4 0.722833 0.483588 0.879296 11.00000 0.01811 0.01770 = 0.01557 0.00134 -0.00012 0.00115 O1 3 0.865208 0.523384 0.898556 11.00000 0.01933 0.01874 = 0.01973 0.00195 -0.00001 -0.00078 O2 3 0.607918 0.543657 0.892054 11.00000 0.01975 0.01874 = 0.02057 -0.00274 0.00083 0.00115 O3 3 0.371883 0.432356 0.912052 11.00000 0.02519 0.04120 = 0.04357 0.00324 -0.00605 0.00201 O4 3 0.237259 0.513216 1.068548 11.00000 0.04987 0.05526 = 0.23177 0.03807 -0.01363 0.00317 C1 1 0.886534 0.587404 0.871969 11.00000 0.01992 0.02255 = 0.01610 0.00159 0.00024 -0.00437 C2 1 0.977893 0.589026 0.825416 11.00000 0.02089 0.03134 = 0.02117 -0.00097 0.00231 0.00092 AFIX 43 H2A 2 1.024218 0.548163 0.812905 11.00000 -1.20000 AFIX 0 C3 1 0.997713 0.650787 0.798971 11.00000 0.01988 0.03581 = 0.01892 0.00278 0.00518 -0.00456 AFIX 43 H3A 2 1.060706 0.653269 0.767993 11.00000 -1.20000 AFIX 0 C4 1 0.927232 0.711308 0.816300 11.00000 0.02266 0.02784 = 0.01595 0.00398 -0.00395 -0.00649 C5 1 0.946691 0.775704 0.787603 11.00000 0.02025 0.03671 = 0.01842 0.00727 -0.00265 -0.01189 AFIX 43 H5A 2 1.008750 0.778140 0.756313 11.00000 -1.20000 AFIX 0 C6 1 0.877641 0.833460 0.804473 11.00000 0.02767 0.02882 = 0.02783 0.01412 -0.01104 -0.01037 AFIX 43 H6A 2 0.892349 0.876149 0.785143 11.00000 -1.20000 AFIX 0 C7 1 0.784190 0.830858 0.850416 11.00000 0.03150 0.02249 = 0.02778 0.00533 -0.01049 -0.00211 AFIX 43 H7A 2 0.736453 0.871761 0.861924 11.00000 -1.20000 AFIX 0 C8 1 0.761946 0.769988 0.878415 11.00000 0.02451 0.02554 = 0.02151 0.00204 -0.00154 -0.00218 AFIX 43 H8A 2 0.696572 0.768530 0.908614 11.00000 -1.20000 AFIX 0 C9 1 0.834770 0.708982 0.863163 11.00000 0.02075 0.02317 = 0.01834 0.00335 -0.00309 -0.00605 C10 1 0.817748 0.643927 0.892064 11.00000 0.02251 0.02528 = 0.01392 0.00105 0.00081 -0.00388 C11 1 0.723830 0.634880 0.942009 11.00000 0.02511 0.01671 = 0.01875 0.00186 0.00385 0.00062 C12 1 0.740355 0.673907 0.993283 11.00000 0.02594 0.01715 = 0.01875 0.00247 0.00384 0.00148 C13 1 0.848849 0.722391 1.001568 11.00000 0.03524 0.02207 = 0.01948 0.00180 0.00208 -0.00326 AFIX 43 H13A 2 0.913915 0.730280 0.971926 11.00000 -1.20000 AFIX 0 C14 1 0.862530 0.758121 1.050995 11.00000 0.04287 0.02680 = 0.02733 0.00083 -0.00222 -0.00863 AFIX 43 H14A 2 0.937197 0.790049 1.055712 11.00000 -1.20000 AFIX 0 C15 1 0.765404 0.747721 1.095455 11.00000 0.05275 0.03211 = 0.01991 -0.00453 0.00071 -0.00274 AFIX 43 H15A 2 0.772686 0.773872 1.129454 11.00000 -1.20000 AFIX 0 C16 1 0.662804 0.700581 1.089220 11.00000 0.04238 0.02908 = 0.01956 0.00200 0.01134 0.00838 AFIX 43 H16A 2 0.599467 0.693321 1.119578 11.00000 -1.20000 AFIX 0 C17 1 0.646276 0.661491 1.038889 11.00000 0.03335 0.02116 = 0.02080 0.00363 0.00515 0.00469 C18 1 0.542450 0.610414 1.033378 11.00000 0.02832 0.02420 = 0.02334 0.00241 0.01194 0.00256 AFIX 43 H18A 2 0.478850 0.603016 1.063623 11.00000 -1.20000 AFIX 0 C19 1 0.531196 0.571259 0.985464 11.00000 0.02437 0.01982 = 0.02652 0.00126 0.00757 0.00109 AFIX 43 H19A 2 0.462340 0.535950 0.982458 11.00000 -1.20000 AFIX 0 C20 1 0.623756 0.584361 0.940696 11.00000 0.01964 0.01896 = 0.01761 0.00086 0.00318 0.00269 C21 1 0.709995 0.424756 0.938890 11.00000 0.02233 0.01924 = 0.01540 -0.00026 0.00192 0.00062 C22 1 0.788954 0.439192 0.988255 11.00000 0.02456 0.01908 = 0.02006 -0.00424 -0.00061 -0.00280 AFIX 43 H22A 2 0.849522 0.478262 0.988882 11.00000 -1.20000 AFIX 0 C23 1 0.778976 0.397816 1.034627 11.00000 0.03182 0.02899 = 0.01347 -0.00187 -0.00357 -0.00117 AFIX 43 H23A 2 0.834104 0.407890 1.067026 11.00000 -1.20000 AFIX 0 C24 1 0.688799 0.340483 1.035584 11.00000 0.02065 0.02452 = 0.01778 -0.00002 0.00037 -0.00059 C25 1 0.675588 0.297529 1.083711 11.00000 0.03827 0.03630 = 0.01708 0.00420 -0.00210 -0.00438 AFIX 43 H25A 2 0.730283 0.306990 1.116353 11.00000 -1.20000 AFIX 0 C26 1 0.585934 0.242858 1.084140 11.00000 0.03811 0.04125 = 0.02375 0.01285 -0.00032 -0.00787 AFIX 43 H26A 2 0.577200 0.214884 1.117105 11.00000 -1.20000 AFIX 0 C27 1 0.506497 0.227788 1.036014 11.00000 0.03128 0.03668 = 0.02991 0.01116 -0.00289 -0.01487 AFIX 43 H27A 2 0.444813 0.189150 1.036437 11.00000 -1.20000 AFIX 0 C28 1 0.516273 0.267531 0.988773 11.00000 0.03002 0.03984 = 0.02280 0.00862 -0.00431 -0.01086 AFIX 43 H28A 2 0.460917 0.256534 0.956638 11.00000 -1.20000 AFIX 0 C29 1 0.607870 0.325218 0.986666 11.00000 0.02222 0.02676 = 0.01711 0.00434 0.00004 -0.00275 C30 1 0.621496 0.368584 0.937464 11.00000 0.01955 0.02351 = 0.01829 0.00169 -0.00020 0.00022 C31 1 0.536719 0.348847 0.886519 11.00000 0.02495 0.02875 = 0.01812 0.00772 -0.00543 -0.00560 C32 1 0.580547 0.292104 0.851846 11.00000 0.02561 0.02811 = 0.01865 0.00481 -0.00311 -0.01030 C33 1 0.708329 0.258208 0.858949 11.00000 0.03332 0.02928 = 0.02489 0.00495 -0.00520 -0.00560 AFIX 43 H33A 2 0.769192 0.273068 0.888287 11.00000 -1.20000 AFIX 0 C34 1 0.748029 0.204459 0.824974 11.00000 0.04185 0.03452 = 0.03359 -0.00161 0.00334 -0.00193 AFIX 43 H34A 2 0.836188 0.182982 0.830461 11.00000 -1.20000 AFIX 0 C35 1 0.659090 0.180722 0.781898 11.00000 0.05351 0.03855 = 0.03791 -0.01017 0.00791 -0.00919 AFIX 43 H35A 2 0.686361 0.142885 0.758534 11.00000 -1.20000 AFIX 0 C36 1 0.535415 0.211745 0.773903 11.00000 0.04709 0.04760 = 0.02140 -0.00739 -0.00187 -0.01972 AFIX 43 H36A 2 0.476271 0.195548 0.744453 11.00000 -1.20000 AFIX 0 C37 1 0.490323 0.268038 0.808134 11.00000 0.03136 0.04060 = 0.02049 0.00813 -0.00682 -0.01458 C38 1 0.362651 0.300371 0.800559 11.00000 0.03511 0.05074 = 0.02315 0.00352 -0.00950 -0.01619 AFIX 43 H38A 2 0.302097 0.283875 0.771699 11.00000 -1.20000 AFIX 0 C39 1 0.321240 0.354726 0.832921 11.00000 0.02111 0.04965 = 0.03128 0.01544 -0.00864 -0.00484 AFIX 43 H39A 2 0.233713 0.376350 0.826274 11.00000 -1.20000 AFIX 0 C40 1 0.409369 0.379050 0.876710 11.00000 0.02554 0.02894 = 0.02893 0.00690 -0.00101 -0.00442 C41 1 0.250607 0.470751 0.897595 11.00000 0.03597 0.07493 = 0.06947 -0.00859 -0.00612 0.02334 AFIX 33 H41A 2 0.234706 0.507030 0.926008 11.00000 -1.50000 H41B 2 0.170028 0.439458 0.896459 11.00000 -1.50000 H41C 2 0.263364 0.492271 0.860336 11.00000 -1.50000 AFIX 0 C42 1 0.705876 0.389086 0.709744 11.00000 0.04112 0.03878 = 0.01354 -0.01069 -0.00658 0.01018 AFIX 13 H42A 2 0.753058 0.342727 0.710021 11.00000 -1.20000 AFIX 0 C43 1 0.791435 0.443326 0.698084 11.00000 0.03799 0.04466 = 0.01529 -0.00125 0.00263 0.01695 AFIX 13 H43A 2 0.890951 0.430160 0.691429 11.00000 -1.20000 AFIX 0 C44 1 0.744350 0.506531 0.666375 11.00000 0.03951 0.05251 = 0.02200 0.01159 0.00090 0.00509 AFIX 23 H44A 2 0.664085 0.494094 0.642043 11.00000 -1.20000 H44B 2 0.820796 0.522693 0.641472 11.00000 -1.20000 AFIX 0 C45 1 0.702251 0.565083 0.705757 11.00000 0.04146 0.03703 = 0.02936 0.01724 -0.00273 0.00400 AFIX 23 H45A 2 0.786166 0.592659 0.715310 11.00000 -1.20000 H45B 2 0.636705 0.596128 0.685526 11.00000 -1.20000 AFIX 0 C46 1 0.634529 0.540988 0.759966 11.00000 0.03189 0.02560 = 0.02412 0.00534 -0.00320 0.00788 AFIX 13 H46A 2 0.625199 0.578255 0.789248 11.00000 -1.20000 AFIX 0 C47 1 0.533751 0.488713 0.764119 11.00000 0.02739 0.03451 = 0.02238 0.00577 -0.00258 0.01052 AFIX 13 H47A 2 0.466772 0.495571 0.796087 11.00000 -1.20000 AFIX 0 C48 1 0.471567 0.451094 0.713833 11.00000 0.02862 0.04917 = 0.02902 0.00590 -0.00719 0.00078 AFIX 23 H48A 2 0.464876 0.484066 0.681756 11.00000 -1.20000 H48B 2 0.375670 0.436354 0.723638 11.00000 -1.20000 AFIX 0 C49 1 0.554577 0.386745 0.694368 11.00000 0.04037 0.04188 = 0.02671 0.00015 -0.00889 -0.00145 AFIX 23 H49A 2 0.512360 0.344746 0.711492 11.00000 -1.20000 H49B 2 0.546211 0.382394 0.652732 11.00000 -1.20000 AFIX 0 C50 1 0.281200 0.441717 1.080993 11.00000 0.12433 0.10219 = 0.27637 0.13479 0.05133 0.02318 AFIX 23 H50A 2 0.210352 0.417268 1.104076 11.00000 -1.20000 H50B 2 0.297115 0.415200 1.045647 11.00000 -1.20000 AFIX 0 C51 1 0.400936 0.449738 1.110140 11.00000 0.04142 0.12897 = 0.55873 0.22728 -0.08088 -0.03522 AFIX 33 H51A 2 0.422815 0.406551 1.130285 11.00000 -1.50000 H51B 2 0.390309 0.487674 1.137505 11.00000 -1.50000 H51C 2 0.476745 0.460822 1.083823 11.00000 -1.50000 AFIX 0 C52 1 0.117954 0.512738 1.043481 11.00000 0.04844 0.10042 = 0.06812 -0.03243 0.00787 -0.02248 AFIX 23 H52A 2 0.043716 0.499729 1.070611 11.00000 -1.20000 H52B 2 0.118358 0.478380 1.012266 11.00000 -1.20000 AFIX 0 C53 1 0.090368 0.586879 1.019658 11.00000 0.08566 0.06843 = 0.08791 -0.01487 -0.02896 0.02048 AFIX 33 H53A 2 0.001890 0.587170 0.998907 11.00000 -1.50000 H53B 2 0.166293 0.600021 0.994034 11.00000 -1.50000 H53C 2 0.085544 0.620151 1.051027 11.00000 -1.50000 HKLF 4 REM ljh97 in P2(1)2(1)2(1) REM R1 = 0.0330 for 8683 Fo > 4sig(Fo) and 0.0388 for all 9385 data REM 541 parameters refined using 0 restraints END WGHT 0.0343 2.1884 REM Highest difference peak 0.745, deepest hole -0.497, 1-sigma level 0.067 Q1 1 0.7075 0.5445 0.7971 11.00000 0.05 0.75 Q2 1 0.3760 0.4605 1.1613 11.00000 0.05 0.54 Q3 1 0.1249 0.4574 1.0576 11.00000 0.05 0.52 Q4 1 0.3648 0.4137 1.0611 11.00000 0.05 0.48 Q5 1 0.2883 0.4509 1.1075 11.00000 0.05 0.44 ; data_ljh71_4b _database_code_depnum_ccdc_archive 'CCDC 911754' #TrackingRef 'combined.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C82 H54 O6 P2 Rh +, B F4 -, 2 C4 H10 O' _chemical_formula_sum 'C90 H74 B F4 O8 P2 Rh' _chemical_formula_weight 1535.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.0434(4) _cell_length_b 20.3321(6) _cell_length_c 25.7605(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7355.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19157 _cell_measurement_theta_min 1.7133 _cell_measurement_theta_max 62.4304 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3176 _exptl_absorpt_coefficient_mu 2.864 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5981 _exptl_absorpt_correction_T_max 0.8700 _exptl_absorpt_process_details ; 'Thu Jan 13 11:41:54 2011' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'mirror optics' _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_reflns_number 36016 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 7.67 _diffrn_reflns_theta_max 54.24 _reflns_number_total 8935 _reflns_number_gt 8181 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+3.0906P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.037(7) _chemical_absolute_configuration ad _refine_ls_number_reflns 8935 _refine_ls_number_parameters 961 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.87971(3) 0.392397(17) 0.882799(14) 0.02719(12) Uani 1 1 d . . . P1 P 0.76504(10) 0.32976(6) 0.85058(5) 0.0254(3) Uani 1 1 d . . . P2 P 0.78655(10) 0.47381(7) 0.90533(5) 0.0270(3) Uani 1 1 d . . . O1 O 0.7514(2) 0.32899(16) 0.78849(12) 0.0284(8) Uani 1 1 d . . . O2 O 0.6621(2) 0.35661(16) 0.86941(11) 0.0276(8) Uani 1 1 d . . . O3 O 0.6501(3) 0.20032(18) 0.75376(13) 0.0382(9) Uani 1 1 d . . . O4 O 0.7124(2) 0.47714(16) 0.95335(12) 0.0311(8) Uani 1 1 d . . . O5 O 0.7233(2) 0.50211(16) 0.85762(12) 0.0279(8) Uani 1 1 d . . . O6 O 0.9958(3) 0.42062(18) 0.99234(13) 0.0397(9) Uani 1 1 d . . . O7 O 0.3577(8) 0.9008(3) 0.9045(3) 0.149(4) Uani 1 1 d . . . O8 O 1.0403(4) 0.4243(2) 0.60707(16) 0.0761(15) Uani 1 1 d . . . B1 B 0.7012(5) 0.2879(3) 1.0753(2) 0.0399(17) Uani 1 1 d . . . F1 F 0.7661(5) 0.2777(3) 1.03784(18) 0.146(3) Uani 1 1 d . . . F2 F 0.7283(4) 0.3427(3) 1.0993(2) 0.127(2) Uani 1 1 d . . . F3 F 0.6112(4) 0.2944(3) 1.0605(3) 0.175(4) Uani 1 1 d . . . F4 F 0.7038(3) 0.2366(2) 1.10989(18) 0.0810(13) Uani 1 1 d . . . C1 C 0.7236(4) 0.3904(3) 0.76753(17) 0.0296(12) Uani 1 1 d . . . C2 C 0.7954(4) 0.4273(3) 0.74320(19) 0.0342(13) Uani 1 1 d . . . H2A H 0.8588 0.4112 0.7414 0.041 Uiso 1 1 calc R . . C3 C 0.7719(4) 0.4868(3) 0.7223(2) 0.0414(14) Uani 1 1 d . . . H3A H 0.8195 0.5123 0.7055 0.050 Uiso 1 1 calc R . . C4 C 0.6783(4) 0.5109(3) 0.72510(19) 0.0370(14) Uani 1 1 d . . . C5 C 0.6531(5) 0.5744(3) 0.7031(2) 0.0458(16) Uani 1 1 d . . . H5A H 0.6999 0.5994 0.6853 0.055 Uiso 1 1 calc R . . C6 C 0.5639(5) 0.5981(3) 0.7078(2) 0.0461(15) Uani 1 1 d . . . H6A H 0.5480 0.6392 0.6926 0.055 Uiso 1 1 calc R . . C7 C 0.4946(5) 0.5626(3) 0.7350(2) 0.0418(15) Uani 1 1 d . . . H7A H 0.4325 0.5805 0.7388 0.050 Uiso 1 1 calc R . . C8 C 0.5147(4) 0.5023(2) 0.75608(19) 0.0311(12) Uani 1 1 d . . . H8A H 0.4666 0.4794 0.7747 0.037 Uiso 1 1 calc R . . C9 C 0.6060(4) 0.4737(2) 0.75053(17) 0.0314(13) Uani 1 1 d . . . C10 C 0.6308(4) 0.4090(2) 0.77071(16) 0.0255(12) Uani 1 1 d . . . C11 C 0.5589(4) 0.3655(2) 0.79586(18) 0.0271(12) Uani 1 1 d . . . C12 C 0.4683(4) 0.3479(2) 0.77251(18) 0.0271(12) Uani 1 1 d . . . C13 C 0.4425(4) 0.3677(2) 0.7217(2) 0.0342(13) Uani 1 1 d . . . H13A H 0.4874 0.3901 0.7005 0.041 Uiso 1 1 calc R . . C14 C 0.3537(4) 0.3547(3) 0.7030(2) 0.0353(14) Uani 1 1 d . . . H14A H 0.3365 0.3698 0.6694 0.042 Uiso 1 1 calc R . . C15 C 0.2876(4) 0.3195(3) 0.7327(2) 0.0449(15) Uani 1 1 d . . . H15A H 0.2252 0.3123 0.7197 0.054 Uiso 1 1 calc R . . C16 C 0.3118(4) 0.2959(3) 0.7796(2) 0.0380(14) Uani 1 1 d . . . H16A H 0.2669 0.2708 0.7989 0.046 Uiso 1 1 calc R . . C17 C 0.4034(4) 0.3078(3) 0.8007(2) 0.0322(13) Uani 1 1 d . . . C18 C 0.4302(4) 0.2808(3) 0.8488(2) 0.0336(13) Uani 1 1 d . . . H18A H 0.3875 0.2528 0.8670 0.040 Uiso 1 1 calc R . . C19 C 0.5173(4) 0.2947(2) 0.86937(18) 0.0293(12) Uani 1 1 d . . . H19A H 0.5359 0.2752 0.9013 0.035 Uiso 1 1 calc R . . C20 C 0.5799(4) 0.3379(2) 0.84356(18) 0.0258(12) Uani 1 1 d . . . C21 C 0.7605(4) 0.2429(2) 0.86751(18) 0.0279(12) Uani 1 1 d . . . C22 C 0.7389(4) 0.2343(3) 0.92086(19) 0.0315(13) Uani 1 1 d . . . H22A H 0.7317 0.2718 0.9425 0.038 Uiso 1 1 calc R . . C23 C 0.7284(4) 0.1737(3) 0.9414(2) 0.0371(14) Uani 1 1 d . . . H23A H 0.7149 0.1692 0.9773 0.045 Uiso 1 1 calc R . . C24 C 0.7372(4) 0.1169(3) 0.91027(19) 0.0354(13) Uani 1 1 d . . . C25 C 0.7232(5) 0.0528(3) 0.9306(3) 0.0573(18) Uani 1 1 d . . . H25A H 0.7070 0.0474 0.9662 0.069 Uiso 1 1 calc R . . C26 C 0.7326(6) -0.0006(3) 0.8999(3) 0.063(2) Uani 1 1 d . . . H26A H 0.7244 -0.0432 0.9143 0.075 Uiso 1 1 calc R . . C27 C 0.7543(6) 0.0058(3) 0.8470(3) 0.0592(19) Uani 1 1 d . . . H27A H 0.7600 -0.0321 0.8257 0.071 Uiso 1 1 calc R . . C28 C 0.7673(4) 0.0668(3) 0.8263(2) 0.0402(14) Uani 1 1 d . . . H28A H 0.7821 0.0708 0.7905 0.048 Uiso 1 1 calc R . . C29 C 0.7594(4) 0.1246(2) 0.8568(2) 0.0323(13) Uani 1 1 d . . . C30 C 0.7738(3) 0.1889(2) 0.83535(18) 0.0259(12) Uani 1 1 d . . . C31 C 0.8079(4) 0.1931(2) 0.78037(18) 0.0283(12) Uani 1 1 d . . . C32 C 0.9072(4) 0.1873(3) 0.77044(19) 0.0330(13) Uani 1 1 d . . . C33 C 0.9761(4) 0.1775(3) 0.8098(2) 0.0331(13) Uani 1 1 d . . . H33A H 0.9556 0.1740 0.8449 0.040 Uiso 1 1 calc R . . C34 C 1.0709(4) 0.1730(3) 0.7989(2) 0.0405(14) Uani 1 1 d . . . H34A H 1.1153 0.1669 0.8264 0.049 Uiso 1 1 calc R . . C35 C 1.1033(4) 0.1771(3) 0.7476(2) 0.0482(16) Uani 1 1 d . . . H35A H 1.1696 0.1756 0.7403 0.058 Uiso 1 1 calc R . . C36 C 1.0389(5) 0.1834(3) 0.7081(2) 0.0483(16) Uani 1 1 d . . . H36A H 1.0610 0.1845 0.6732 0.058 Uiso 1 1 calc R . . C37 C 0.9400(4) 0.1883(3) 0.7181(2) 0.0399(14) Uani 1 1 d . . . C38 C 0.8720(5) 0.1947(3) 0.6782(2) 0.0489(16) Uani 1 1 d . . . H38A H 0.8928 0.1962 0.6431 0.059 Uiso 1 1 calc R . . C39 C 0.7763(5) 0.1988(3) 0.6886(2) 0.0415(15) Uani 1 1 d . . . H39A H 0.7319 0.2026 0.6610 0.050 Uiso 1 1 calc R . . C40 C 0.7440(4) 0.1976(2) 0.74028(19) 0.0317(13) Uani 1 1 d . . . C41 C 0.5830(4) 0.2140(3) 0.7137(2) 0.0453(15) Uani 1 1 d . . . H41A H 0.5191 0.2170 0.7287 0.068 Uiso 1 1 calc R . . H41B H 0.5845 0.1786 0.6879 0.068 Uiso 1 1 calc R . . H41C H 0.5994 0.2558 0.6970 0.068 Uiso 1 1 calc R . . C42 C 0.6162(4) 0.4600(2) 0.94889(17) 0.0265(11) Uani 1 1 d . . . C43 C 0.5857(4) 0.4056(3) 0.97753(19) 0.0336(14) Uani 1 1 d . . . H43A H 0.6286 0.3824 0.9994 0.040 Uiso 1 1 calc R . . C44 C 0.4925(4) 0.3867(3) 0.9734(2) 0.0367(13) Uani 1 1 d . . . H44A H 0.4705 0.3508 0.9937 0.044 Uiso 1 1 calc R . . C45 C 0.4285(4) 0.4186(3) 0.9400(2) 0.0350(14) Uani 1 1 d . . . C46 C 0.3352(4) 0.3936(3) 0.9292(2) 0.0411(14) Uani 1 1 d . . . H46A H 0.3128 0.3560 0.9474 0.049 Uiso 1 1 calc R . . C47 C 0.2783(4) 0.4229(3) 0.8932(3) 0.0491(17) Uani 1 1 d . . . H47A H 0.2173 0.4049 0.8859 0.059 Uiso 1 1 calc R . . C48 C 0.3085(4) 0.4789(3) 0.8671(2) 0.0430(15) Uani 1 1 d . . . H48A H 0.2676 0.4991 0.8424 0.052 Uiso 1 1 calc R . . C49 C 0.3953(4) 0.5052(3) 0.8764(2) 0.0331(12) Uani 1 1 d . . . H49A H 0.4136 0.5443 0.8587 0.040 Uiso 1 1 calc R . . C50 C 0.4587(4) 0.4760(3) 0.91141(19) 0.0294(13) Uani 1 1 d . . . C51 C 0.5570(4) 0.4989(2) 0.91901(18) 0.0284(12) Uani 1 1 d . . . C52 C 0.5914(3) 0.5607(2) 0.89522(17) 0.0257(12) Uani 1 1 d . . . C53 C 0.5468(4) 0.6231(2) 0.90465(17) 0.0280(12) Uani 1 1 d . . . C54 C 0.4682(4) 0.6304(3) 0.9387(2) 0.0339(13) Uani 1 1 d . . . H54A H 0.4432 0.5930 0.9560 0.041 Uiso 1 1 calc R . . C55 C 0.4280(4) 0.6910(3) 0.9468(2) 0.0398(14) Uani 1 1 d . . . H55A H 0.3761 0.6951 0.9703 0.048 Uiso 1 1 calc R . . C56 C 0.4625(5) 0.7471(3) 0.9209(2) 0.0409(15) Uani 1 1 d . . . H56A H 0.4320 0.7884 0.9256 0.049 Uiso 1 1 calc R . . C57 C 0.5385(4) 0.7422(2) 0.8898(2) 0.0351(13) Uani 1 1 d . . . H57A H 0.5631 0.7808 0.8738 0.042 Uiso 1 1 calc R . . C58 C 0.5833(4) 0.6805(2) 0.8799(2) 0.0339(13) Uani 1 1 d . . . C59 C 0.6623(4) 0.6748(3) 0.8471(2) 0.0353(13) Uani 1 1 d . . . H59A H 0.6858 0.7128 0.8299 0.042 Uiso 1 1 calc R . . C60 C 0.7065(4) 0.6158(3) 0.83927(18) 0.0326(12) Uani 1 1 d . . . H60A H 0.7601 0.6125 0.8169 0.039 Uiso 1 1 calc R . . C61 C 0.6711(4) 0.5605(2) 0.86497(18) 0.0259(12) Uani 1 1 d . . . C62 C 0.8664(4) 0.5394(2) 0.92752(17) 0.0272(12) Uani 1 1 d . . . C63 C 0.8330(4) 0.6011(3) 0.94638(18) 0.0310(12) Uani 1 1 d . . . H63A H 0.7667 0.6097 0.9490 0.037 Uiso 1 1 calc R . . C64 C 0.8977(4) 0.6472(3) 0.96054(18) 0.0339(14) Uani 1 1 d . . . H64A H 0.8753 0.6886 0.9725 0.041 Uiso 1 1 calc R . . C65 C 0.9977(4) 0.6363(3) 0.95822(19) 0.0310(13) Uani 1 1 d . . . C66 C 1.0658(4) 0.6839(3) 0.9730(2) 0.0412(15) Uani 1 1 d . . . H66A H 1.0451 0.7263 0.9837 0.049 Uiso 1 1 calc R . . C67 C 1.1607(5) 0.6699(3) 0.9722(3) 0.0532(17) Uani 1 1 d . . . H67A H 1.2054 0.7028 0.9818 0.064 Uiso 1 1 calc R . . C68 C 1.1931(4) 0.6065(3) 0.9571(2) 0.0482(15) Uani 1 1 d . . . H68A H 1.2592 0.5966 0.9573 0.058 Uiso 1 1 calc R . . C69 C 1.1286(4) 0.5599(3) 0.9424(2) 0.0421(14) Uani 1 1 d . . . H69A H 1.1509 0.5179 0.9319 0.051 Uiso 1 1 calc R . . C70 C 1.0303(4) 0.5723(3) 0.94238(19) 0.0300(13) Uani 1 1 d . . . C71 C 0.9610(4) 0.5251(2) 0.92608(18) 0.0276(12) Uani 1 1 d . . . C72 C 0.9936(4) 0.4594(3) 0.9067(2) 0.0273(12) Uani 1 1 d . . . C73 C 1.0183(4) 0.4524(3) 0.8521(2) 0.0285(12) Uani 1 1 d . . . C74 C 1.0259(4) 0.5056(3) 0.8170(2) 0.0369(14) Uani 1 1 d . . . H74A H 1.0181 0.5494 0.8290 0.044 Uiso 1 1 calc R . . C75 C 1.0443(4) 0.4938(3) 0.7660(2) 0.0452(15) Uani 1 1 d . . . H75A H 1.0495 0.5299 0.7427 0.054 Uiso 1 1 calc R . . C76 C 1.0556(5) 0.4299(3) 0.7470(2) 0.0504(17) Uani 1 1 d . . . H76A H 1.0698 0.4232 0.7113 0.060 Uiso 1 1 calc R . . C77 C 1.0467(4) 0.3779(3) 0.7788(2) 0.0443(16) Uani 1 1 d . . . H77A H 1.0522 0.3348 0.7649 0.053 Uiso 1 1 calc R . . C78 C 1.0295(4) 0.3862(3) 0.8322(2) 0.0354(13) Uani 1 1 d . . . C79 C 1.0181(4) 0.3327(3) 0.8677(2) 0.0377(14) Uani 1 1 d . . . H79A H 1.0118 0.2873 0.8531 0.045 Uiso 1 1 calc R . . C80 C 1.0102(4) 0.3404(3) 0.9213(2) 0.0359(14) Uani 1 1 d . . . H80A H 1.0007 0.3012 0.9442 0.043 Uiso 1 1 calc R . . C81 C 1.0009(4) 0.4054(2) 0.94176(19) 0.0306(12) Uani 1 1 d . . . C82 C 0.9672(5) 0.3684(3) 1.0281(2) 0.0558(18) Uani 1 1 d . . . H82A H 0.9620 0.3864 1.0633 0.084 Uiso 1 1 calc R . . H82B H 1.0149 0.3333 1.0276 0.084 Uiso 1 1 calc R . . H82C H 0.9054 0.3506 1.0173 0.084 Uiso 1 1 calc R . . C83 C 0.2061(15) 0.8426(8) 0.8980(9) 0.263(11) Uani 1 1 d . . . H83A H 0.2433 0.8233 0.8696 0.394 Uiso 1 1 calc R . . H83B H 0.1397 0.8475 0.8870 0.394 Uiso 1 1 calc R . . H83C H 0.2093 0.8137 0.9284 0.394 Uiso 1 1 calc R . . C84 C 0.2491(7) 0.9137(5) 0.9126(4) 0.099(3) Uani 1 1 d . . . H84A H 0.2252 0.9484 0.8890 0.119 Uiso 1 1 calc R . . H84B H 0.2346 0.9259 0.9489 0.119 Uiso 1 1 calc R . . C85 C 0.3891(11) 0.9658(5) 0.9206(3) 0.116(5) Uani 1 1 d . . . H85A H 0.3602 1.0010 0.8993 0.140 Uiso 1 1 calc R . . H85B H 0.3759 0.9741 0.9578 0.140 Uiso 1 1 calc R . . C86 C 0.4896(13) 0.9586(6) 0.9105(4) 0.149(6) Uani 1 1 d . . . H86A H 0.5254 0.9894 0.9323 0.223 Uiso 1 1 calc R . . H86B H 0.5024 0.9680 0.8739 0.223 Uiso 1 1 calc R . . H86C H 0.5093 0.9135 0.9185 0.223 Uiso 1 1 calc R . . C87 C 1.1095(10) 0.3205(4) 0.6142(3) 0.134(5) Uani 1 1 d . . . H87A H 1.1434 0.2861 0.5951 0.201 Uiso 1 1 calc R . . H87B H 1.0557 0.3010 0.6329 0.201 Uiso 1 1 calc R . . H87C H 1.1529 0.3412 0.6391 0.201 Uiso 1 1 calc R . . C88 C 1.0737(8) 0.3707(4) 0.5773(3) 0.098(3) Uani 1 1 d . . . H88A H 1.1255 0.3852 0.5538 0.118 Uiso 1 1 calc R . . H88B H 1.0215 0.3523 0.5559 0.118 Uiso 1 1 calc R . . C89 C 1.0088(6) 0.4781(4) 0.5755(3) 0.065(2) Uani 1 1 d . . . H89A H 0.9539 0.4642 0.5540 0.078 Uiso 1 1 calc R . . H89B H 1.0607 0.4921 0.5520 0.078 Uiso 1 1 calc R . . C90 C 0.9808(6) 0.5332(4) 0.6096(3) 0.075(2) Uani 1 1 d . . . H90A H 0.9536 0.5686 0.5885 0.113 Uiso 1 1 calc R . . H90B H 1.0370 0.5496 0.6281 0.113 Uiso 1 1 calc R . . H90C H 0.9334 0.5179 0.6347 0.113 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0269(2) 0.0217(2) 0.0329(2) -0.00134(17) -0.00076(18) 0.00180(18) P1 0.0291(7) 0.0225(7) 0.0245(6) 0.0003(5) 0.0014(6) 0.0013(6) P2 0.0270(7) 0.0256(7) 0.0284(6) -0.0009(6) -0.0013(6) 0.0009(6) O1 0.031(2) 0.026(2) 0.0284(17) 0.0007(15) 0.0039(15) 0.0030(16) O2 0.0272(19) 0.0273(19) 0.0282(18) -0.0012(14) -0.0019(15) -0.0008(15) O3 0.039(3) 0.039(2) 0.037(2) -0.0038(17) -0.0089(18) -0.0017(17) O4 0.030(2) 0.034(2) 0.0297(18) 0.0037(16) -0.0033(16) 0.0043(17) O5 0.032(2) 0.0263(19) 0.0259(16) -0.0023(14) 0.0027(16) 0.0033(17) O6 0.047(2) 0.034(2) 0.038(2) 0.0068(17) -0.0122(18) -0.0042(18) O7 0.285(12) 0.049(4) 0.114(5) 0.015(3) -0.066(6) -0.018(6) O8 0.133(5) 0.053(3) 0.042(2) 0.003(2) -0.019(3) -0.012(3) B1 0.055(5) 0.038(4) 0.027(3) 0.001(3) -0.010(3) -0.009(3) F1 0.210(7) 0.165(5) 0.063(3) -0.037(3) 0.063(4) -0.089(5) F2 0.119(4) 0.090(3) 0.172(5) -0.075(4) 0.064(4) -0.043(3) F3 0.090(4) 0.137(5) 0.297(8) 0.166(6) -0.113(5) -0.067(4) F4 0.054(2) 0.090(3) 0.099(3) 0.049(3) -0.008(2) 0.000(2) C1 0.035(3) 0.025(3) 0.029(3) 0.005(3) 0.002(2) 0.004(3) C2 0.032(3) 0.036(3) 0.036(3) -0.002(3) 0.004(3) -0.003(3) C3 0.049(4) 0.041(4) 0.034(3) 0.013(3) 0.010(3) -0.006(3) C4 0.050(4) 0.030(3) 0.032(3) -0.003(3) 0.007(3) 0.001(3) C5 0.071(5) 0.028(3) 0.039(3) 0.013(3) 0.004(3) -0.001(3) C6 0.072(5) 0.026(3) 0.040(3) 0.007(3) -0.006(3) 0.005(3) C7 0.047(4) 0.039(4) 0.040(3) -0.004(3) 0.001(3) 0.010(3) C8 0.036(3) 0.021(3) 0.036(3) -0.001(2) -0.006(2) 0.005(2) C9 0.046(4) 0.024(3) 0.023(2) -0.001(2) -0.005(3) -0.001(3) C10 0.028(3) 0.022(3) 0.026(2) 0.000(2) -0.003(2) -0.002(2) C11 0.031(3) 0.023(3) 0.027(3) -0.001(2) 0.005(2) 0.007(2) C12 0.028(3) 0.025(3) 0.028(3) -0.009(2) 0.000(2) 0.009(2) C13 0.039(4) 0.023(3) 0.040(3) -0.004(2) -0.002(3) 0.009(2) C14 0.039(4) 0.030(3) 0.037(3) -0.009(2) -0.013(3) 0.008(3) C15 0.034(3) 0.047(4) 0.054(4) -0.019(3) -0.008(3) 0.010(3) C16 0.036(3) 0.035(3) 0.043(3) -0.007(3) 0.006(3) -0.004(3) C17 0.028(3) 0.033(3) 0.035(3) -0.006(2) 0.004(2) 0.003(2) C18 0.031(3) 0.032(3) 0.038(3) -0.004(3) 0.007(3) -0.002(3) C19 0.034(3) 0.029(3) 0.026(3) 0.003(2) 0.004(2) 0.006(2) C20 0.025(3) 0.024(3) 0.028(3) -0.004(2) 0.000(2) 0.001(2) C21 0.028(3) 0.022(3) 0.033(3) 0.000(2) -0.004(2) 0.002(2) C22 0.039(3) 0.029(3) 0.027(3) -0.002(2) -0.003(2) 0.004(3) C23 0.045(4) 0.035(4) 0.031(3) 0.003(3) -0.005(3) -0.002(3) C24 0.037(3) 0.032(3) 0.037(3) 0.006(3) 0.001(2) 0.001(3) C25 0.079(5) 0.038(4) 0.055(4) 0.007(3) 0.013(4) -0.004(4) C26 0.088(6) 0.028(4) 0.072(5) 0.016(3) 0.021(4) -0.006(4) C27 0.074(5) 0.029(4) 0.074(4) -0.009(3) 0.013(4) -0.007(3) C28 0.043(3) 0.033(4) 0.045(3) -0.005(3) 0.005(3) -0.008(3) C29 0.030(3) 0.024(3) 0.043(3) 0.000(2) 0.004(2) -0.005(2) C30 0.019(3) 0.026(3) 0.033(3) 0.005(2) -0.002(2) -0.002(2) C31 0.036(3) 0.023(3) 0.026(3) -0.005(2) 0.000(3) -0.001(2) C32 0.044(4) 0.024(3) 0.031(3) -0.004(2) 0.007(3) -0.003(2) C33 0.032(3) 0.030(3) 0.038(3) -0.009(2) 0.002(3) -0.004(3) C34 0.033(3) 0.039(3) 0.049(3) -0.016(3) -0.002(3) -0.001(3) C35 0.033(4) 0.047(4) 0.065(4) -0.026(3) 0.013(3) -0.003(3) C36 0.058(4) 0.038(4) 0.049(4) -0.012(3) 0.022(4) -0.008(3) C37 0.046(4) 0.034(3) 0.040(3) -0.004(3) 0.008(3) 0.004(3) C38 0.070(5) 0.047(4) 0.030(3) -0.001(3) 0.014(3) -0.003(4) C39 0.058(4) 0.033(3) 0.033(3) 0.001(2) 0.000(3) -0.003(3) C40 0.037(4) 0.024(3) 0.034(3) -0.002(2) 0.001(3) -0.003(2) C41 0.054(4) 0.037(3) 0.046(3) -0.006(3) -0.013(3) 0.001(3) C42 0.029(3) 0.027(3) 0.024(2) -0.002(2) 0.003(2) 0.005(3) C43 0.044(4) 0.028(3) 0.029(3) 0.000(2) 0.010(2) 0.008(3) C44 0.046(4) 0.024(3) 0.040(3) 0.000(3) 0.014(3) -0.003(3) C45 0.039(3) 0.024(3) 0.042(3) -0.007(3) 0.019(3) -0.001(3) C46 0.040(3) 0.027(3) 0.056(3) -0.006(3) 0.024(3) -0.003(3) C47 0.030(3) 0.031(3) 0.087(5) -0.017(3) 0.010(4) -0.004(3) C48 0.031(3) 0.040(4) 0.058(4) -0.018(3) 0.001(3) 0.008(3) C49 0.027(3) 0.033(3) 0.040(3) -0.007(2) 0.001(3) 0.006(2) C50 0.032(3) 0.023(3) 0.033(3) -0.010(2) 0.009(3) -0.004(3) C51 0.035(3) 0.024(3) 0.027(3) -0.006(2) 0.008(2) 0.001(2) C52 0.032(3) 0.020(3) 0.025(3) 0.001(2) 0.002(2) 0.000(2) C53 0.032(3) 0.027(3) 0.025(2) 0.002(2) -0.006(2) -0.004(2) C54 0.028(3) 0.034(3) 0.041(3) -0.009(2) 0.002(3) 0.001(2) C55 0.033(3) 0.039(4) 0.048(3) -0.020(3) 0.002(3) 0.000(3) C56 0.049(4) 0.028(3) 0.045(3) -0.011(3) -0.008(3) 0.002(3) C57 0.042(3) 0.020(3) 0.042(3) -0.005(2) -0.006(3) 0.002(2) C58 0.038(3) 0.031(3) 0.033(3) -0.001(3) -0.005(3) -0.001(2) C59 0.041(3) 0.025(3) 0.040(3) 0.010(3) 0.005(3) -0.004(3) C60 0.032(3) 0.034(3) 0.032(3) 0.008(3) 0.004(2) -0.006(3) C61 0.028(3) 0.016(3) 0.034(3) -0.002(2) -0.004(2) 0.005(2) C62 0.030(3) 0.026(3) 0.026(2) -0.001(2) -0.001(2) 0.002(2) C63 0.029(3) 0.029(3) 0.035(3) -0.009(3) -0.002(2) 0.001(3) C64 0.044(4) 0.028(3) 0.030(3) -0.006(2) 0.001(3) 0.008(3) C65 0.037(3) 0.027(3) 0.029(3) -0.003(2) 0.001(2) -0.001(3) C66 0.049(4) 0.029(3) 0.045(3) -0.015(3) 0.007(3) 0.001(3) C67 0.039(4) 0.053(4) 0.067(4) -0.029(3) 0.001(3) -0.014(3) C68 0.031(3) 0.047(4) 0.067(4) -0.017(4) 0.006(3) 0.000(3) C69 0.038(4) 0.038(3) 0.051(3) -0.015(3) 0.008(3) -0.003(3) C70 0.033(3) 0.027(3) 0.030(3) -0.007(2) 0.003(2) 0.000(3) C71 0.033(3) 0.023(3) 0.027(2) -0.002(2) 0.003(2) 0.004(3) C72 0.020(3) 0.024(3) 0.038(3) -0.005(2) -0.005(2) 0.003(2) C73 0.022(3) 0.028(3) 0.036(3) -0.005(3) 0.006(2) -0.007(2) C74 0.036(3) 0.035(3) 0.039(3) -0.002(3) 0.003(3) 0.002(3) C75 0.038(4) 0.057(4) 0.041(3) -0.005(3) 0.013(3) -0.010(3) C76 0.053(4) 0.056(4) 0.043(3) -0.013(3) 0.023(3) -0.008(3) C77 0.031(3) 0.049(4) 0.052(4) -0.026(3) 0.004(3) 0.001(3) C78 0.025(3) 0.031(3) 0.050(3) -0.013(3) 0.010(2) 0.000(3) C79 0.026(3) 0.030(3) 0.057(4) -0.011(3) 0.003(3) 0.003(2) C80 0.028(3) 0.025(3) 0.055(4) 0.010(3) -0.005(3) 0.006(3) C81 0.031(3) 0.028(3) 0.033(3) -0.001(2) -0.010(2) -0.002(2) C82 0.070(5) 0.050(4) 0.047(3) 0.009(3) -0.005(3) -0.004(3) C83 0.30(2) 0.151(14) 0.34(3) -0.084(16) -0.07(2) -0.095(16) C84 0.083(6) 0.133(9) 0.082(5) 0.018(5) -0.020(5) 0.048(6) C85 0.217(13) 0.083(7) 0.049(4) 0.006(4) 0.003(7) -0.083(9) C86 0.28(2) 0.096(8) 0.071(6) -0.007(5) 0.040(9) -0.068(11) C87 0.275(15) 0.046(5) 0.081(5) -0.011(4) -0.073(9) 0.001(7) C88 0.170(10) 0.053(5) 0.071(5) -0.002(4) -0.046(6) -0.008(5) C89 0.081(5) 0.064(5) 0.051(4) 0.008(4) 0.001(4) -0.001(4) C90 0.093(6) 0.078(5) 0.055(4) -0.004(4) 0.000(4) 0.011(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 P1 2.2145(14) . ? Rh1 P2 2.1882(14) . ? Rh1 C72 2.189(5) . ? Rh1 C73 2.431(5) . ? Rh1 C78 2.477(5) . ? Rh1 C79 2.324(5) . ? Rh1 C80 2.337(5) . ? Rh1 C81 2.296(5) . ? P1 O1 1.611(3) . ? P1 O2 1.619(4) . ? P1 C21 1.820(5) . ? P2 O4 1.619(4) . ? P2 O5 1.621(3) . ? P2 C62 1.834(5) . ? O1 C1 1.415(6) . ? O2 C20 1.386(6) . ? O3 C40 1.365(7) . ? O3 C41 1.424(6) . ? O4 C42 1.400(6) . ? O5 C61 1.409(6) . ? O6 C81 1.341(6) . ? O6 C82 1.461(7) . ? O7 C84 1.562(12) . ? O7 C85 1.455(10) . ? O8 C88 1.413(10) . ? O8 C89 1.433(8) . ? B1 F1 1.344(9) . ? B1 F2 1.330(8) . ? B1 F3 1.326(9) . ? B1 F4 1.372(8) . ? C1 C2 1.404(7) . ? C1 C10 1.360(7) . ? C2 H2A 0.950 . ? C2 C3 1.366(8) . ? C3 H3A 0.950 . ? C3 C4 1.404(8) . ? C4 C5 1.454(8) . ? C4 C9 1.426(8) . ? C5 H5A 0.950 . ? C5 C6 1.347(9) . ? C6 H6A 0.950 . ? C6 C7 1.400(8) . ? C7 H7A 0.950 . ? C7 C8 1.369(8) . ? C8 H8A 0.950 . ? C8 C9 1.416(8) . ? C9 C10 1.455(7) . ? C10 C11 1.491(7) . ? C11 C12 1.451(7) . ? C11 C20 1.383(7) . ? C12 C13 1.417(7) . ? C12 C17 1.422(7) . ? C13 H13A 0.950 . ? C13 C14 1.362(8) . ? C14 H14A 0.950 . ? C14 C15 1.401(8) . ? C15 H15A 0.950 . ? C15 C16 1.344(8) . ? C16 H16A 0.950 . ? C16 C17 1.417(8) . ? C17 C18 1.407(8) . ? C18 H18A 0.950 . ? C18 C19 1.362(8) . ? C19 H19A 0.950 . ? C19 C20 1.409(7) . ? C21 C22 1.418(7) . ? C21 C30 1.389(7) . ? C22 H22A 0.950 . ? C22 C23 1.348(7) . ? C23 H23A 0.950 . ? C23 C24 1.412(8) . ? C24 C25 1.418(8) . ? C24 C29 1.420(7) . ? C25 H25A 0.950 . ? C25 C26 1.350(9) . ? C26 H26A 0.950 . ? C26 C27 1.402(9) . ? C27 H27A 0.950 . ? C27 C28 1.362(9) . ? C28 H28A 0.950 . ? C28 C29 1.418(7) . ? C29 C30 1.433(7) . ? C30 C31 1.498(7) . ? C31 C32 1.423(8) . ? C31 C40 1.371(7) . ? C32 C33 1.415(8) . ? C32 C37 1.426(8) . ? C33 H33A 0.950 . ? C33 C34 1.364(8) . ? C34 H34A 0.950 . ? C34 C35 1.401(8) . ? C35 H35A 0.950 . ? C35 C36 1.368(9) . ? C36 H36A 0.950 . ? C36 C37 1.417(9) . ? C37 C38 1.409(9) . ? C38 H38A 0.950 . ? C38 C39 1.373(9) . ? C39 H39A 0.950 . ? C39 C40 1.405(8) . ? C41 H41A 0.980 . ? C41 H41B 0.980 . ? C41 H41C 0.980 . ? C42 C43 1.397(7) . ? C42 C51 1.380(7) . ? C43 H43A 0.950 . ? C43 C44 1.368(8) . ? C44 H44A 0.950 . ? C44 C45 1.402(8) . ? C45 C46 1.432(8) . ? C45 C50 1.444(8) . ? C46 H46A 0.950 . ? C46 C47 1.361(8) . ? C47 H47A 0.950 . ? C47 C48 1.389(9) . ? C48 H48A 0.950 . ? C48 C49 1.352(8) . ? C49 H49A 0.950 . ? C49 C50 1.401(7) . ? C50 C51 1.470(8) . ? C51 C52 1.481(7) . ? C52 C53 1.434(7) . ? C52 C61 1.364(7) . ? C53 C54 1.417(7) . ? C53 C58 1.426(7) . ? C54 H54A 0.950 . ? C54 C55 1.370(8) . ? C55 H55A 0.950 . ? C55 C56 1.409(8) . ? C56 H56A 0.950 . ? C56 C57 1.339(8) . ? C57 H57A 0.950 . ? C57 C58 1.427(7) . ? C58 C59 1.399(7) . ? C59 H59A 0.950 . ? C59 C60 1.365(8) . ? C60 H60A 0.950 . ? C60 C61 1.396(7) . ? C62 C63 1.425(7) . ? C62 C71 1.360(7) . ? C63 H63A 0.950 . ? C63 C64 1.356(7) . ? C64 H64A 0.950 . ? C64 C65 1.423(8) . ? C65 C66 1.412(8) . ? C65 C70 1.439(7) . ? C66 H66A 0.950 . ? C66 C67 1.363(9) . ? C67 H67A 0.950 . ? C67 C68 1.423(9) . ? C68 H68A 0.950 . ? C68 C69 1.364(8) . ? C69 H69A 0.950 . ? C69 C70 1.403(8) . ? C70 C71 1.429(7) . ? C71 C72 1.498(7) . ? C72 C73 1.457(7) . ? C72 C81 1.425(7) . ? C73 C74 1.412(8) . ? C73 C78 1.449(8) . ? C74 H74A 0.950 . ? C74 C75 1.361(8) . ? C75 H75A 0.950 . ? C75 C76 1.399(9) . ? C76 H76A 0.950 . ? C76 C77 1.343(9) . ? C77 H77A 0.950 . ? C77 C78 1.409(8) . ? C78 C79 1.431(8) . ? C79 H79A 1.000 . ? C79 C80 1.392(8) . ? C80 H80A 1.000 . ? C80 C81 1.429(8) . ? C82 H82A 0.980 . ? C82 H82B 0.980 . ? C82 H82C 0.980 . ? C83 H83A 0.980 . ? C83 H83B 0.980 . ? C83 H83C 0.980 . ? C83 C84 1.610(16) . ? C84 H84A 0.990 . ? C84 H84B 0.990 . ? C85 H85A 0.990 . ? C85 H85B 0.990 . ? C85 C86 1.443(18) . ? C86 H86A 0.980 . ? C86 H86B 0.980 . ? C86 H86C 0.980 . ? C87 H87A 0.980 . ? C87 H87B 0.980 . ? C87 H87C 0.980 . ? C87 C88 1.484(11) . ? C88 H88A 0.990 . ? C88 H88B 0.990 . ? C89 H89A 0.990 . ? C89 H89B 0.990 . ? C89 C90 1.476(10) . ? C90 H90A 0.980 . ? C90 H90B 0.980 . ? C90 H90C 0.980 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Rh1 P2 95.72(5) . . ? P1 Rh1 C72 174.01(14) . . ? P1 Rh1 C73 138.52(13) . . ? P1 Rh1 C78 113.02(13) . . ? P1 Rh1 C79 104.18(14) . . ? P1 Rh1 C80 117.97(14) . . ? P1 Rh1 C81 148.52(13) . . ? P2 Rh1 C72 83.77(14) . . ? P2 Rh1 C73 100.68(13) . . ? P2 Rh1 C78 133.28(14) . . ? P2 Rh1 C79 159.95(15) . . ? P2 Rh1 C80 134.34(15) . . ? P2 Rh1 C81 100.42(13) . . ? C72 Rh1 C73 36.30(17) . . ? C72 Rh1 C78 63.86(18) . . ? C72 Rh1 C79 76.18(19) . . ? C72 Rh1 C80 65.74(19) . . ? C72 Rh1 C81 36.96(19) . . ? C73 Rh1 C78 34.32(18) . . ? C73 Rh1 C79 62.50(18) . . ? C73 Rh1 C80 74.75(19) . . ? C73 Rh1 C81 64.16(18) . . ? C78 Rh1 C79 34.48(19) . . ? C78 Rh1 C80 62.22(19) . . ? C78 Rh1 C81 74.01(18) . . ? C79 Rh1 C80 34.8(2) . . ? C79 Rh1 C81 63.30(19) . . ? C80 Rh1 C81 35.91(19) . . ? Rh1 P1 O1 117.65(14) . . ? Rh1 P1 O2 110.05(13) . . ? Rh1 P1 C21 119.57(17) . . ? O1 P1 O2 101.22(17) . . ? O1 P1 C21 103.0(2) . . ? O2 P1 C21 103.0(2) . . ? Rh1 P2 O4 128.25(14) . . ? Rh1 P2 O5 113.25(13) . . ? Rh1 P2 C62 105.48(17) . . ? O4 P2 O5 102.25(17) . . ? O4 P2 C62 97.2(2) . . ? O5 P2 C62 108.3(2) . . ? P1 O1 C1 113.8(3) . . ? P1 O2 C20 120.5(3) . . ? C40 O3 C41 117.6(4) . . ? P2 O4 C42 123.2(3) . . ? P2 O5 C61 118.8(3) . . ? C81 O6 C82 117.3(4) . . ? C84 O7 C85 96.0(9) . . ? C88 O8 C89 112.5(5) . . ? F1 B1 F2 105.6(6) . . ? F1 B1 F3 117.1(7) . . ? F1 B1 F4 109.3(6) . . ? F2 B1 F3 108.8(7) . . ? F2 B1 F4 109.2(6) . . ? F3 B1 F4 106.7(6) . . ? O1 C1 C2 116.3(4) . . ? O1 C1 C10 119.2(4) . . ? C2 C1 C10 124.4(5) . . ? C1 C2 H2A 120.8 . . ? C1 C2 C3 118.4(5) . . ? H2A C2 C3 120.8 . . ? C2 C3 H3A 119.5 . . ? C2 C3 C4 121.0(5) . . ? H3A C3 C4 119.5 . . ? C3 C4 C5 121.2(5) . . ? C3 C4 C9 120.4(5) . . ? C5 C4 C9 118.5(5) . . ? C4 C5 H5A 119.7 . . ? C4 C5 C6 120.6(6) . . ? H5A C5 C6 119.7 . . ? C5 C6 H6A 119.8 . . ? C5 C6 C7 120.5(5) . . ? H6A C6 C7 119.8 . . ? C6 C7 H7A 119.5 . . ? C6 C7 C8 121.1(6) . . ? H7A C7 C8 119.5 . . ? C7 C8 H8A 119.5 . . ? C7 C8 C9 121.0(5) . . ? H8A C8 C9 119.5 . . ? C4 C9 C8 118.3(5) . . ? C4 C9 C10 118.2(5) . . ? C8 C9 C10 123.5(5) . . ? C1 C10 C9 117.4(5) . . ? C1 C10 C11 120.6(4) . . ? C9 C10 C11 121.9(5) . . ? C10 C11 C12 124.0(4) . . ? C10 C11 C20 118.8(5) . . ? C12 C11 C20 117.1(5) . . ? C11 C12 C13 122.5(5) . . ? C11 C12 C17 119.5(4) . . ? C13 C12 C17 118.1(5) . . ? C12 C13 H13A 119.8 . . ? C12 C13 C14 120.4(5) . . ? H13A C13 C14 119.8 . . ? C13 C14 H14A 119.6 . . ? C13 C14 C15 120.9(5) . . ? H14A C14 C15 119.6 . . ? C14 C15 H15A 119.8 . . ? C14 C15 C16 120.4(6) . . ? H15A C15 C16 119.8 . . ? C15 C16 H16A 119.6 . . ? C15 C16 C17 120.8(6) . . ? H16A C16 C17 119.6 . . ? C12 C17 C16 119.0(5) . . ? C12 C17 C18 120.1(5) . . ? C16 C17 C18 120.9(5) . . ? C17 C18 H18A 119.9 . . ? C17 C18 C19 120.1(5) . . ? H18A C18 C19 119.9 . . ? C18 C19 H19A 119.8 . . ? C18 C19 C20 120.4(5) . . ? H19A C19 C20 119.8 . . ? O2 C20 C11 119.6(4) . . ? O2 C20 C19 117.7(4) . . ? C11 C20 C19 122.6(5) . . ? P1 C21 C22 111.0(4) . . ? P1 C21 C30 128.3(4) . . ? C22 C21 C30 120.6(5) . . ? C21 C22 H22A 119.5 . . ? C21 C22 C23 121.0(5) . . ? H22A C22 C23 119.5 . . ? C22 C23 H23A 119.5 . . ? C22 C23 C24 121.1(5) . . ? H23A C23 C24 119.5 . . ? C23 C24 C25 122.0(5) . . ? C23 C24 C29 118.6(5) . . ? C25 C24 C29 119.4(5) . . ? C24 C25 H25A 119.7 . . ? C24 C25 C26 120.5(6) . . ? H25A C25 C26 119.7 . . ? C25 C26 H26A 119.4 . . ? C25 C26 C27 121.1(6) . . ? H26A C26 C27 119.4 . . ? C26 C27 H27A 120.2 . . ? C26 C27 C28 119.5(6) . . ? H27A C27 C28 120.2 . . ? C27 C28 H28A 119.1 . . ? C27 C28 C29 121.9(5) . . ? H28A C28 C29 119.1 . . ? C24 C29 C28 117.5(5) . . ? C24 C29 C30 120.4(5) . . ? C28 C29 C30 122.0(5) . . ? C21 C30 C29 118.2(4) . . ? C21 C30 C31 124.2(4) . . ? C29 C30 C31 117.5(4) . . ? C30 C31 C32 118.6(5) . . ? C30 C31 C40 120.5(5) . . ? C32 C31 C40 120.8(5) . . ? C31 C32 C33 123.5(5) . . ? C31 C32 C37 119.0(5) . . ? C33 C32 C37 117.4(5) . . ? C32 C33 H33A 119.0 . . ? C32 C33 C34 121.9(5) . . ? H33A C33 C34 119.0 . . ? C33 C34 H34A 119.7 . . ? C33 C34 C35 120.5(6) . . ? H34A C34 C35 119.7 . . ? C34 C35 H35A 120.2 . . ? C34 C35 C36 119.6(5) . . ? H35A C35 C36 120.2 . . ? C35 C36 H36A 119.3 . . ? C35 C36 C37 121.3(5) . . ? H36A C36 C37 119.3 . . ? C32 C37 C36 119.1(6) . . ? C32 C37 C38 118.2(5) . . ? C36 C37 C38 122.6(5) . . ? C37 C38 H38A 119.2 . . ? C37 C38 C39 121.7(5) . . ? H38A C38 C39 119.2 . . ? C38 C39 H39A 120.0 . . ? C38 C39 C40 120.0(6) . . ? H39A C39 C40 120.0 . . ? O3 C40 C31 116.3(4) . . ? O3 C40 C39 123.5(5) . . ? C31 C40 C39 120.2(5) . . ? O3 C41 H41A 109.5 . . ? O3 C41 H41B 109.5 . . ? O3 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O4 C42 C43 116.7(4) . . ? O4 C42 C51 119.0(4) . . ? C43 C42 C51 124.3(5) . . ? C42 C43 H43A 120.8 . . ? C42 C43 C44 118.3(5) . . ? H43A C43 C44 120.8 . . ? C43 C44 H44A 119.0 . . ? C43 C44 C45 122.1(5) . . ? H44A C44 C45 119.0 . . ? C44 C45 C46 122.8(5) . . ? C44 C45 C50 119.9(5) . . ? C46 C45 C50 117.1(5) . . ? C45 C46 H46A 119.5 . . ? C45 C46 C47 121.0(6) . . ? H46A C46 C47 119.5 . . ? C46 C47 H47A 119.7 . . ? C46 C47 C48 120.6(5) . . ? H47A C47 C48 119.7 . . ? C47 C48 H48A 119.5 . . ? C47 C48 C49 121.0(6) . . ? H48A C48 C49 119.5 . . ? C48 C49 H49A 119.4 . . ? C48 C49 C50 121.2(5) . . ? H49A C49 C50 119.4 . . ? C45 C50 C49 119.0(5) . . ? C45 C50 C51 117.6(5) . . ? C49 C50 C51 123.3(5) . . ? C42 C51 C50 117.3(5) . . ? C42 C51 C52 121.4(5) . . ? C50 C51 C52 121.3(5) . . ? C51 C52 C53 122.6(4) . . ? C51 C52 C61 120.1(4) . . ? C53 C52 C61 117.2(4) . . ? C52 C53 C54 122.5(4) . . ? C52 C53 C58 119.4(5) . . ? C54 C53 C58 118.0(5) . . ? C53 C54 H54A 119.6 . . ? C53 C54 C55 120.8(5) . . ? H54A C54 C55 119.6 . . ? C54 C55 H55A 119.6 . . ? C54 C55 C56 120.9(5) . . ? H55A C55 C56 119.6 . . ? C55 C56 H56A 120.1 . . ? C55 C56 C57 119.9(5) . . ? H56A C56 C57 120.1 . . ? C56 C57 H57A 119.2 . . ? C56 C57 C58 121.6(5) . . ? H57A C57 C58 119.2 . . ? C53 C58 C57 118.8(5) . . ? C53 C58 C59 119.1(5) . . ? C57 C58 C59 122.0(5) . . ? C58 C59 H59A 119.2 . . ? C58 C59 C60 121.5(5) . . ? H59A C59 C60 119.2 . . ? C59 C60 H60A 120.8 . . ? C59 C60 C61 118.4(5) . . ? H60A C60 C61 120.8 . . ? O5 C61 C52 120.5(4) . . ? O5 C61 C60 115.4(4) . . ? C52 C61 C60 124.1(5) . . ? P2 C62 C63 123.0(4) . . ? P2 C62 C71 115.7(4) . . ? C63 C62 C71 121.3(5) . . ? C62 C63 H63A 120.7 . . ? C62 C63 C64 118.7(5) . . ? H63A C63 C64 120.7 . . ? C63 C64 H64A 118.6 . . ? C63 C64 C65 122.8(5) . . ? H64A C64 C65 118.6 . . ? C64 C65 C66 123.4(5) . . ? C64 C65 C70 117.8(5) . . ? C66 C65 C70 118.7(5) . . ? C65 C66 H66A 119.5 . . ? C65 C66 C67 121.0(6) . . ? H66A C66 C67 119.5 . . ? C66 C67 H67A 119.8 . . ? C66 C67 C68 120.4(6) . . ? H67A C67 C68 119.8 . . ? C67 C68 H68A 120.3 . . ? C67 C68 C69 119.5(6) . . ? H68A C68 C69 120.3 . . ? C68 C69 H69A 119.0 . . ? C68 C69 C70 122.0(5) . . ? H69A C69 C70 119.0 . . ? C65 C70 C69 118.3(5) . . ? C65 C70 C71 118.3(5) . . ? C69 C70 C71 123.4(5) . . ? C62 C71 C70 120.9(5) . . ? C62 C71 C72 119.8(5) . . ? C70 C71 C72 119.2(5) . . ? Rh1 C72 C71 115.2(3) . . ? Rh1 C72 C73 80.9(3) . . ? Rh1 C72 C81 75.6(3) . . ? C71 C72 C73 118.7(4) . . ? C71 C72 C81 119.9(4) . . ? C73 C72 C81 121.3(5) . . ? Rh1 C73 C72 62.8(3) . . ? Rh1 C73 C74 130.7(4) . . ? Rh1 C73 C78 74.6(3) . . ? C72 C73 C74 124.2(5) . . ? C72 C73 C78 117.2(5) . . ? C74 C73 C78 118.5(5) . . ? C73 C74 H74A 120.1 . . ? C73 C74 C75 119.8(5) . . ? H74A C74 C75 120.1 . . ? C74 C75 H75A 119.2 . . ? C74 C75 C76 121.6(6) . . ? H75A C75 C76 119.2 . . ? C75 C76 H76A 119.8 . . ? C75 C76 C77 120.5(5) . . ? H76A C76 C77 119.8 . . ? C76 C77 H77A 119.4 . . ? C76 C77 C78 121.2(5) . . ? H77A C77 C78 119.4 . . ? Rh1 C78 C73 71.1(3) . . ? Rh1 C78 C77 131.8(4) . . ? Rh1 C78 C79 66.9(3) . . ? C73 C78 C77 118.3(5) . . ? C73 C78 C79 118.0(5) . . ? C77 C78 C79 123.6(5) . . ? Rh1 C79 C78 78.6(3) . . ? Rh1 C79 H79A 118.1 . . ? Rh1 C79 C80 73.1(3) . . ? C78 C79 H79A 118.1 . . ? C78 C79 C80 123.8(5) . . ? H79A C79 C80 118.1 . . ? Rh1 C80 C79 72.1(3) . . ? Rh1 C80 H80A 120.4 . . ? Rh1 C80 C81 70.5(3) . . ? C79 C80 H80A 120.4 . . ? C79 C80 C81 118.5(5) . . ? H80A C80 C81 120.4 . . ? Rh1 C81 O6 129.0(4) . . ? Rh1 C81 C72 67.4(3) . . ? Rh1 C81 C80 73.6(3) . . ? O6 C81 C72 115.7(4) . . ? O6 C81 C80 125.3(4) . . ? C72 C81 C80 119.0(4) . . ? O6 C82 H82A 109.5 . . ? O6 C82 H82B 109.5 . . ? O6 C82 H82C 109.5 . . ? H82A C82 H82B 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? H83A C83 H83B 109.5 . . ? H83A C83 H83C 109.5 . . ? H83A C83 C84 109.5 . . ? H83B C83 H83C 109.5 . . ? H83B C83 C84 109.5 . . ? H83C C83 C84 109.5 . . ? O7 C84 C83 100.6(10) . . ? O7 C84 H84A 111.7 . . ? O7 C84 H84B 111.7 . . ? C83 C84 H84A 111.7 . . ? C83 C84 H84B 111.7 . . ? H84A C84 H84B 109.4 . . ? O7 C85 H85A 112.0 . . ? O7 C85 H85B 112.0 . . ? O7 C85 C86 98.8(11) . . ? H85A C85 H85B 109.7 . . ? H85A C85 C86 112.0 . . ? H85B C85 C86 112.0 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86B 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? H87A C87 H87B 109.5 . . ? H87A C87 H87C 109.5 . . ? H87A C87 C88 109.5 . . ? H87B C87 H87C 109.5 . . ? H87B C87 C88 109.5 . . ? H87C C87 C88 109.5 . . ? O8 C88 C87 107.1(6) . . ? O8 C88 H88A 110.3 . . ? O8 C88 H88B 110.3 . . ? C87 C88 H88A 110.3 . . ? C87 C88 H88B 110.3 . . ? H88A C88 H88B 108.5 . . ? O8 C89 H89A 109.9 . . ? O8 C89 H89B 109.9 . . ? O8 C89 C90 108.9(5) . . ? H89A C89 H89B 108.3 . . ? H89A C89 C90 109.9 . . ? H89B C89 C90 109.9 . . ? C89 C90 H90A 109.5 . . ? C89 C90 H90B 109.5 . . ? C89 C90 H90C 109.5 . . ? H90A C90 H90B 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Rh1 P1 O1 100.02(15) . . . . ? P2 Rh1 P1 O2 -15.14(13) . . . . ? P2 Rh1 P1 C21 -133.93(19) . . . . ? C72 Rh1 P1 O1 15.2(14) . . . . ? C72 Rh1 P1 O2 -100.0(13) . . . . ? C72 Rh1 P1 C21 141.2(13) . . . . ? C73 Rh1 P1 O1 -13.2(3) . . . . ? C73 Rh1 P1 O2 -128.4(2) . . . . ? C73 Rh1 P1 C21 112.8(3) . . . . ? C78 Rh1 P1 O1 -42.3(2) . . . . ? C78 Rh1 P1 O2 -157.43(19) . . . . ? C78 Rh1 P1 C21 83.8(2) . . . . ? C79 Rh1 P1 O1 -77.5(2) . . . . ? C79 Rh1 P1 O2 167.30(19) . . . . ? C79 Rh1 P1 C21 48.5(2) . . . . ? C80 Rh1 P1 O1 -111.9(2) . . . . ? C80 Rh1 P1 O2 132.9(2) . . . . ? C80 Rh1 P1 C21 14.1(3) . . . . ? C81 Rh1 P1 O1 -139.2(3) . . . . ? C81 Rh1 P1 O2 105.6(3) . . . . ? C81 Rh1 P1 C21 -13.1(3) . . . . ? P1 Rh1 P2 O4 73.72(18) . . . . ? P1 Rh1 P2 O5 -55.53(15) . . . . ? P1 Rh1 P2 C62 -173.74(16) . . . . ? C72 Rh1 P2 O4 -112.3(2) . . . . ? C72 Rh1 P2 O5 118.5(2) . . . . ? C72 Rh1 P2 C62 0.3(2) . . . . ? C73 Rh1 P2 O4 -144.5(2) . . . . ? C73 Rh1 P2 O5 86.20(19) . . . . ? C73 Rh1 P2 C62 -32.0(2) . . . . ? C78 Rh1 P2 O4 -156.9(2) . . . . ? C78 Rh1 P2 O5 73.8(2) . . . . ? C78 Rh1 P2 C62 -44.4(2) . . . . ? C79 Rh1 P2 O4 -113.2(5) . . . . ? C79 Rh1 P2 O5 117.6(4) . . . . ? C79 Rh1 P2 C62 -0.6(5) . . . . ? C80 Rh1 P2 O4 -65.5(3) . . . . ? C80 Rh1 P2 O5 165.3(2) . . . . ? C80 Rh1 P2 C62 47.1(3) . . . . ? C81 Rh1 P2 O4 -79.1(2) . . . . ? C81 Rh1 P2 O5 151.60(19) . . . . ? C81 Rh1 P2 C62 33.4(2) . . . . ? Rh1 P1 O1 C1 -64.4(3) . . . . ? O2 P1 O1 C1 55.5(3) . . . . ? C21 P1 O1 C1 161.8(3) . . . . ? Rh1 P1 O2 C20 161.9(3) . . . . ? O1 P1 O2 C20 36.8(4) . . . . ? C21 P1 O2 C20 -69.5(4) . . . . ? Rh1 P2 O4 C42 -92.4(4) . . . . ? O5 P2 O4 C42 40.8(4) . . . . ? C62 P2 O4 C42 151.3(4) . . . . ? Rh1 P2 O5 C61 -170.7(3) . . . . ? O4 P2 O5 C61 47.7(4) . . . . ? C62 P2 O5 C61 -54.2(4) . . . . ? P1 O1 C1 C2 102.2(4) . . . . ? P1 O1 C1 C10 -79.5(5) . . . . ? O1 C1 C2 C3 179.8(4) . . . . ? C10 C1 C2 C3 1.7(8) . . . . ? C1 C2 C3 C4 0.3(8) . . . . ? C2 C3 C4 C5 179.7(5) . . . . ? C2 C3 C4 C9 0.6(8) . . . . ? C3 C4 C5 C6 -177.4(6) . . . . ? C9 C4 C5 C6 1.6(8) . . . . ? C4 C5 C6 C7 1.4(9) . . . . ? C5 C6 C7 C8 -1.8(8) . . . . ? C6 C7 C8 C9 -0.8(8) . . . . ? C7 C8 C9 C4 3.8(7) . . . . ? C7 C8 C9 C10 -178.1(5) . . . . ? C3 C4 C9 C8 175.0(5) . . . . ? C3 C4 C9 C10 -3.3(7) . . . . ? C5 C4 C9 C8 -4.1(7) . . . . ? C5 C4 C9 C10 177.7(4) . . . . ? O1 C1 C10 C9 177.6(4) . . . . ? O1 C1 C10 C11 -0.1(7) . . . . ? C2 C1 C10 C9 -4.3(7) . . . . ? C2 C1 C10 C11 178.0(5) . . . . ? C4 C9 C10 C1 5.0(6) . . . . ? C4 C9 C10 C11 -177.4(4) . . . . ? C8 C9 C10 C1 -173.2(5) . . . . ? C8 C9 C10 C11 4.5(7) . . . . ? C1 C10 C11 C12 -130.2(5) . . . . ? C1 C10 C11 C20 47.4(7) . . . . ? C9 C10 C11 C12 52.2(6) . . . . ? C9 C10 C11 C20 -130.2(5) . . . . ? C10 C11 C12 C13 3.9(7) . . . . ? C10 C11 C12 C17 -177.8(5) . . . . ? C20 C11 C12 C13 -173.7(5) . . . . ? C20 C11 C12 C17 4.5(7) . . . . ? C11 C12 C13 C14 -174.5(5) . . . . ? C17 C12 C13 C14 7.3(7) . . . . ? C12 C13 C14 C15 -2.5(8) . . . . ? C13 C14 C15 C16 -2.3(8) . . . . ? C14 C15 C16 C17 2.1(8) . . . . ? C15 C16 C17 C12 2.9(8) . . . . ? C15 C16 C17 C18 -177.4(5) . . . . ? C11 C12 C17 C16 174.3(4) . . . . ? C11 C12 C17 C18 -5.5(7) . . . . ? C13 C12 C17 C16 -7.4(7) . . . . ? C13 C12 C17 C18 172.8(5) . . . . ? C12 C17 C18 C19 2.1(7) . . . . ? C16 C17 C18 C19 -177.6(5) . . . . ? C17 C18 C19 C20 2.1(7) . . . . ? C10 C11 C20 O2 6.9(7) . . . . ? C10 C11 C20 C19 -178.2(4) . . . . ? C12 C11 C20 O2 -175.4(4) . . . . ? C12 C11 C20 C19 -0.4(7) . . . . ? P1 O2 C20 C11 -75.4(5) . . . . ? P1 O2 C20 C19 109.4(4) . . . . ? C18 C19 C20 O2 172.1(4) . . . . ? C18 C19 C20 C11 -3.0(7) . . . . ? Rh1 P1 C21 C22 67.3(4) . . . . ? Rh1 P1 C21 C30 -113.8(4) . . . . ? O1 P1 C21 C22 -160.0(4) . . . . ? O1 P1 C21 C30 18.9(5) . . . . ? O2 P1 C21 C22 -55.1(4) . . . . ? O2 P1 C21 C30 123.9(5) . . . . ? P1 C21 C22 C23 177.4(4) . . . . ? C30 C21 C22 C23 -1.6(8) . . . . ? C21 C22 C23 C24 -0.9(9) . . . . ? C22 C23 C24 C25 -177.7(6) . . . . ? C22 C23 C24 C29 1.2(8) . . . . ? C23 C24 C25 C26 -179.7(7) . . . . ? C29 C24 C25 C26 1.3(10) . . . . ? C24 C25 C26 C27 -1.4(12) . . . . ? C25 C26 C27 C28 0.8(12) . . . . ? C26 C27 C28 C29 -0.1(11) . . . . ? C27 C28 C29 C24 0.0(9) . . . . ? C27 C28 C29 C30 179.5(6) . . . . ? C23 C24 C29 C28 -179.6(5) . . . . ? C23 C24 C29 C30 0.9(8) . . . . ? C25 C24 C29 C28 -0.6(8) . . . . ? C25 C24 C29 C30 179.9(5) . . . . ? P1 C21 C30 C29 -175.2(4) . . . . ? P1 C21 C30 C31 8.6(8) . . . . ? C22 C21 C30 C29 3.7(7) . . . . ? C22 C21 C30 C31 -172.5(5) . . . . ? C24 C29 C30 C21 -3.3(8) . . . . ? C24 C29 C30 C31 173.1(5) . . . . ? C28 C29 C30 C21 177.2(5) . . . . ? C28 C29 C30 C31 -6.3(8) . . . . ? C21 C30 C31 C32 92.8(6) . . . . ? C21 C30 C31 C40 -91.9(6) . . . . ? C29 C30 C31 C32 -83.4(6) . . . . ? C29 C30 C31 C40 91.9(6) . . . . ? C30 C31 C32 C33 0.2(8) . . . . ? C30 C31 C32 C37 177.3(5) . . . . ? C40 C31 C32 C33 -175.1(5) . . . . ? C40 C31 C32 C37 2.0(8) . . . . ? C31 C32 C33 C34 -179.2(5) . . . . ? C37 C32 C33 C34 3.7(8) . . . . ? C32 C33 C34 C35 -0.7(9) . . . . ? C33 C34 C35 C36 -2.4(9) . . . . ? C34 C35 C36 C37 2.4(9) . . . . ? C35 C36 C37 C32 0.6(9) . . . . ? C35 C36 C37 C38 -179.9(6) . . . . ? C31 C32 C37 C36 179.2(5) . . . . ? C31 C32 C37 C38 -0.3(8) . . . . ? C33 C32 C37 C36 -3.5(8) . . . . ? C33 C32 C37 C38 176.9(5) . . . . ? C32 C37 C38 C39 -1.0(9) . . . . ? C36 C37 C38 C39 179.5(6) . . . . ? C37 C38 C39 C40 0.8(9) . . . . ? C41 O3 C40 C31 171.6(4) . . . . ? C41 O3 C40 C39 -8.6(7) . . . . ? C30 C31 C40 O3 2.3(7) . . . . ? C30 C31 C40 C39 -177.5(5) . . . . ? C32 C31 C40 O3 177.5(5) . . . . ? C32 C31 C40 C39 -2.2(8) . . . . ? C38 C39 C40 O3 -178.8(5) . . . . ? C38 C39 C40 C31 0.9(8) . . . . ? P2 O4 C42 C43 115.5(4) . . . . ? P2 O4 C42 C51 -67.5(5) . . . . ? O4 C42 C43 C44 -178.8(4) . . . . ? C51 C42 C43 C44 4.4(7) . . . . ? C42 C43 C44 C45 2.4(8) . . . . ? C43 C44 C45 C46 170.3(5) . . . . ? C43 C44 C45 C50 -4.2(8) . . . . ? C44 C45 C46 C47 -174.3(5) . . . . ? C50 C45 C46 C47 0.3(7) . . . . ? C45 C46 C47 C48 -1.7(8) . . . . ? C46 C47 C48 C49 0.7(8) . . . . ? C47 C48 C49 C50 1.8(8) . . . . ? C48 C49 C50 C45 -3.1(7) . . . . ? C48 C49 C50 C51 173.9(5) . . . . ? C44 C45 C50 C49 176.9(5) . . . . ? C44 C45 C50 C51 -0.3(7) . . . . ? C46 C45 C50 C49 2.0(7) . . . . ? C46 C45 C50 C51 -175.1(4) . . . . ? O4 C42 C51 C50 174.6(4) . . . . ? O4 C42 C51 C52 -4.9(6) . . . . ? C43 C42 C51 C50 -8.7(7) . . . . ? C43 C42 C51 C52 171.8(4) . . . . ? C45 C50 C51 C42 6.3(7) . . . . ? C45 C50 C51 C52 -174.2(4) . . . . ? C49 C50 C51 C42 -170.7(4) . . . . ? C49 C50 C51 C52 8.8(7) . . . . ? C42 C51 C52 C53 -123.1(5) . . . . ? C42 C51 C52 C61 53.6(6) . . . . ? C50 C51 C52 C53 57.4(6) . . . . ? C50 C51 C52 C61 -125.9(5) . . . . ? C51 C52 C53 C54 1.9(7) . . . . ? C51 C52 C53 C58 -179.3(4) . . . . ? C61 C52 C53 C54 -174.9(4) . . . . ? C61 C52 C53 C58 3.9(7) . . . . ? C52 C53 C54 C55 179.7(5) . . . . ? C58 C53 C54 C55 0.8(7) . . . . ? C53 C54 C55 C56 1.1(8) . . . . ? C54 C55 C56 C57 -3.1(8) . . . . ? C55 C56 C57 C58 3.1(8) . . . . ? C52 C53 C58 C57 -179.8(5) . . . . ? C52 C53 C58 C59 -0.5(7) . . . . ? C54 C53 C58 C57 -0.9(7) . . . . ? C54 C53 C58 C59 178.4(5) . . . . ? C56 C57 C58 C53 -1.1(8) . . . . ? C56 C57 C58 C59 179.6(5) . . . . ? C53 C58 C59 C60 -1.4(8) . . . . ? C57 C58 C59 C60 177.8(5) . . . . ? C58 C59 C60 C61 -0.1(8) . . . . ? C51 C52 C61 O5 -2.3(7) . . . . ? C51 C52 C61 C60 177.3(5) . . . . ? C53 C52 C61 O5 174.6(4) . . . . ? C53 C52 C61 C60 -5.8(7) . . . . ? C59 C60 C61 O5 -176.4(4) . . . . ? C59 C60 C61 C52 4.0(8) . . . . ? P2 O5 C61 C52 -72.5(5) . . . . ? P2 O5 C61 C60 107.9(4) . . . . ? Rh1 P2 C62 C63 -179.1(4) . . . . ? Rh1 P2 C62 C71 -0.5(4) . . . . ? O4 P2 C62 C63 -46.0(4) . . . . ? O4 P2 C62 C71 132.5(4) . . . . ? O5 P2 C62 C63 59.4(4) . . . . ? O5 P2 C62 C71 -122.0(4) . . . . ? P2 C62 C63 C64 -178.1(4) . . . . ? C71 C62 C63 C64 3.4(7) . . . . ? C62 C63 C64 C65 -1.1(8) . . . . ? C63 C64 C65 C66 -179.7(5) . . . . ? C63 C64 C65 C70 -3.0(8) . . . . ? C64 C65 C66 C67 177.0(6) . . . . ? C70 C65 C66 C67 0.3(9) . . . . ? C65 C66 C67 C68 -1.0(10) . . . . ? C66 C67 C68 C69 1.3(10) . . . . ? C67 C68 C69 C70 -1.0(9) . . . . ? C68 C69 C70 C65 0.3(8) . . . . ? C68 C69 C70 C71 178.6(5) . . . . ? C64 C65 C70 C69 -176.9(5) . . . . ? C64 C65 C70 C71 4.8(7) . . . . ? C66 C65 C70 C69 0.0(7) . . . . ? C66 C65 C70 C71 -178.3(5) . . . . ? P2 C62 C71 C70 180.0(4) . . . . ? P2 C62 C71 C72 0.5(6) . . . . ? C63 C62 C71 C70 -1.5(7) . . . . ? C63 C62 C71 C72 179.1(4) . . . . ? C65 C70 C71 C62 -2.7(7) . . . . ? C65 C70 C71 C72 176.7(4) . . . . ? C69 C70 C71 C62 179.1(5) . . . . ? C69 C70 C71 C72 -1.5(7) . . . . ? C62 C71 C72 Rh1 -0.3(6) . . . . ? C62 C71 C72 C73 93.1(6) . . . . ? C62 C71 C72 C81 -87.7(6) . . . . ? C70 C71 C72 Rh1 -179.7(4) . . . . ? C70 C71 C72 C73 -86.3(6) . . . . ? C70 C71 C72 C81 92.9(6) . . . . ? P1 Rh1 C72 C71 85.4(14) . . . . ? P1 Rh1 C72 C73 -32.1(15) . . . . ? P1 Rh1 C72 C81 -157.9(12) . . . . ? P2 Rh1 C72 C71 0.0(3) . . . . ? P2 Rh1 C72 C73 -117.6(3) . . . . ? P2 Rh1 C72 C81 116.6(3) . . . . ? C73 Rh1 C72 C71 117.6(5) . . . . ? C73 Rh1 C72 C81 -125.8(5) . . . . ? C78 Rh1 C72 C71 145.2(4) . . . . ? C78 Rh1 C72 C73 27.6(3) . . . . ? C78 Rh1 C72 C81 -98.2(3) . . . . ? C79 Rh1 C72 C71 179.6(4) . . . . ? C79 Rh1 C72 C73 62.1(3) . . . . ? C79 Rh1 C72 C81 -63.7(3) . . . . ? C80 Rh1 C72 C71 -145.2(4) . . . . ? C80 Rh1 C72 C73 97.3(3) . . . . ? C80 Rh1 C72 C81 -28.5(3) . . . . ? C81 Rh1 C72 C71 -116.6(5) . . . . ? C81 Rh1 C72 C73 125.8(5) . . . . ? Rh1 C72 C73 C74 122.5(5) . . . . ? Rh1 C72 C73 C78 -53.2(4) . . . . ? C71 C72 C73 Rh1 -113.8(5) . . . . ? C71 C72 C73 C74 8.7(8) . . . . ? C71 C72 C73 C78 -167.0(5) . . . . ? C81 C72 C73 Rh1 66.9(4) . . . . ? C81 C72 C73 C74 -170.6(5) . . . . ? C81 C72 C73 C78 13.8(7) . . . . ? P1 Rh1 C73 C72 175.2(2) . . . . ? P1 Rh1 C73 C74 62.2(5) . . . . ? P1 Rh1 C73 C78 -52.4(4) . . . . ? P2 Rh1 C73 C72 63.7(3) . . . . ? P2 Rh1 C73 C74 -49.3(5) . . . . ? P2 Rh1 C73 C78 -163.9(3) . . . . ? C72 Rh1 C73 C74 -113.0(6) . . . . ? C72 Rh1 C73 C78 132.4(5) . . . . ? C78 Rh1 C73 C72 -132.4(5) . . . . ? C78 Rh1 C73 C74 114.6(6) . . . . ? C79 Rh1 C73 C72 -104.7(3) . . . . ? C79 Rh1 C73 C74 142.3(5) . . . . ? C79 Rh1 C73 C78 27.7(3) . . . . ? C80 Rh1 C73 C72 -69.6(3) . . . . ? C80 Rh1 C73 C74 177.4(5) . . . . ? C80 Rh1 C73 C78 62.8(3) . . . . ? C81 Rh1 C73 C72 -32.8(3) . . . . ? C81 Rh1 C73 C74 -145.8(5) . . . . ? C81 Rh1 C73 C78 99.6(3) . . . . ? Rh1 C73 C74 C75 -94.7(6) . . . . ? C72 C73 C74 C75 -176.4(5) . . . . ? C78 C73 C74 C75 -0.7(8) . . . . ? C73 C74 C75 C76 0.3(9) . . . . ? C74 C75 C76 C77 1.3(10) . . . . ? C75 C76 C77 C78 -2.5(9) . . . . ? C76 C77 C78 Rh1 91.3(7) . . . . ? C76 C77 C78 C73 2.0(8) . . . . ? C76 C77 C78 C79 179.1(6) . . . . ? Rh1 C73 C78 C77 128.0(5) . . . . ? Rh1 C73 C78 C79 -49.3(4) . . . . ? C72 C73 C78 Rh1 47.6(4) . . . . ? C72 C73 C78 C77 175.6(5) . . . . ? C72 C73 C78 C79 -1.7(7) . . . . ? C74 C73 C78 Rh1 -128.4(5) . . . . ? C74 C73 C78 C77 -0.4(7) . . . . ? C74 C73 C78 C79 -177.7(5) . . . . ? P1 Rh1 C78 C73 145.2(3) . . . . ? P1 Rh1 C78 C77 33.7(6) . . . . ? P1 Rh1 C78 C79 -81.5(3) . . . . ? P2 Rh1 C78 C73 21.9(4) . . . . ? P2 Rh1 C78 C77 -89.6(6) . . . . ? P2 Rh1 C78 C79 155.2(3) . . . . ? C72 Rh1 C78 C73 -29.1(3) . . . . ? C72 Rh1 C78 C77 -140.6(6) . . . . ? C72 Rh1 C78 C79 104.2(3) . . . . ? C73 Rh1 C78 C77 -111.5(7) . . . . ? C73 Rh1 C78 C79 133.3(5) . . . . ? C79 Rh1 C78 C73 -133.3(5) . . . . ? C79 Rh1 C78 C77 115.2(7) . . . . ? C80 Rh1 C78 C73 -104.1(3) . . . . ? C80 Rh1 C78 C77 144.4(6) . . . . ? C80 Rh1 C78 C79 29.2(3) . . . . ? C81 Rh1 C78 C73 -67.4(3) . . . . ? C81 Rh1 C78 C77 -178.9(6) . . . . ? C81 Rh1 C78 C79 65.9(3) . . . . ? Rh1 C78 C79 C80 -60.6(5) . . . . ? C73 C78 C79 Rh1 51.2(4) . . . . ? C73 C78 C79 C80 -9.3(8) . . . . ? C77 C78 C79 Rh1 -125.9(5) . . . . ? C77 C78 C79 C80 173.5(6) . . . . ? P1 Rh1 C79 C78 110.2(3) . . . . ? P1 Rh1 C79 C80 -119.0(3) . . . . ? P2 Rh1 C79 C78 -62.8(6) . . . . ? P2 Rh1 C79 C80 68.1(6) . . . . ? C72 Rh1 C79 C78 -63.7(3) . . . . ? C72 Rh1 C79 C80 67.2(4) . . . . ? C73 Rh1 C79 C78 -27.6(3) . . . . ? C73 Rh1 C79 C80 103.3(4) . . . . ? C78 Rh1 C79 C80 130.9(5) . . . . ? C80 Rh1 C79 C78 -130.9(5) . . . . ? C81 Rh1 C79 C78 -100.8(3) . . . . ? C81 Rh1 C79 C80 30.1(3) . . . . ? Rh1 C79 C80 C81 -54.9(5) . . . . ? C78 C79 C80 Rh1 63.2(5) . . . . ? C78 C79 C80 C81 8.2(9) . . . . ? P1 Rh1 C80 C79 73.8(4) . . . . ? P1 Rh1 C80 C81 -155.9(3) . . . . ? P2 Rh1 C80 C79 -153.6(3) . . . . ? P2 Rh1 C80 C81 -23.3(4) . . . . ? C72 Rh1 C80 C79 -101.0(4) . . . . ? C72 Rh1 C80 C81 29.3(3) . . . . ? C73 Rh1 C80 C79 -63.5(3) . . . . ? C73 Rh1 C80 C81 66.8(3) . . . . ? C78 Rh1 C80 C79 -28.9(3) . . . . ? C78 Rh1 C80 C81 101.3(3) . . . . ? C79 Rh1 C80 C81 130.3(5) . . . . ? C81 Rh1 C80 C79 -130.3(5) . . . . ? C82 O6 C81 Rh1 76.6(6) . . . . ? C82 O6 C81 C72 157.5(5) . . . . ? C82 O6 C81 C80 -20.7(8) . . . . ? Rh1 C72 C81 O6 -123.8(4) . . . . ? Rh1 C72 C81 C80 54.5(4) . . . . ? C71 C72 C81 Rh1 111.1(5) . . . . ? C71 C72 C81 O6 -12.8(7) . . . . ? C71 C72 C81 C80 165.6(5) . . . . ? C73 C72 C81 Rh1 -69.7(5) . . . . ? C73 C72 C81 O6 166.5(5) . . . . ? C73 C72 C81 C80 -15.2(8) . . . . ? Rh1 C80 C81 O6 126.6(5) . . . . ? Rh1 C80 C81 C72 -51.6(4) . . . . ? C79 C80 C81 Rh1 55.7(5) . . . . ? C79 C80 C81 O6 -177.7(5) . . . . ? C79 C80 C81 C72 4.1(8) . . . . ? P1 Rh1 C81 O6 -78.8(5) . . . . ? P1 Rh1 C81 C72 175.7(2) . . . . ? P1 Rh1 C81 C80 43.6(4) . . . . ? P2 Rh1 C81 O6 40.8(4) . . . . ? P2 Rh1 C81 C72 -64.7(3) . . . . ? P2 Rh1 C81 C80 163.3(3) . . . . ? C72 Rh1 C81 O6 105.5(5) . . . . ? C72 Rh1 C81 C80 -132.1(4) . . . . ? C73 Rh1 C81 O6 137.7(5) . . . . ? C73 Rh1 C81 C72 32.2(3) . . . . ? C73 Rh1 C81 C80 -99.8(3) . . . . ? C78 Rh1 C81 O6 173.1(5) . . . . ? C78 Rh1 C81 C72 67.6(3) . . . . ? C78 Rh1 C81 C80 -64.5(3) . . . . ? C79 Rh1 C81 O6 -151.6(5) . . . . ? C79 Rh1 C81 C72 102.9(3) . . . . ? C79 Rh1 C81 C80 -29.1(3) . . . . ? C80 Rh1 C81 O6 -122.5(6) . . . . ? C80 Rh1 C81 C72 132.1(4) . . . . ? C85 O7 C84 C83 -177.7(10) . . . . ? C84 O7 C85 C86 -176.2(8) . . . . ? C89 O8 C88 C87 176.6(8) . . . . ? C88 O8 C89 C90 -176.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 54.24 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.798 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.057 # Contents of RES file _computing_special_details ; TITL ljh71 in P2(1)2(1)2(1) CELL 1.54178 14.0434 20.3321 25.7605 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0006 0.0006 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H B O F P RH UNIT 360 296 4 32 16 8 4 TEMP -123 L.S. 8 BOND $H CONF SIZE 0.20 0.05 0.05 FMAP 2 PLAN 5 SHEL 5.8 0.95 ACTA REM EXTI 0.000000 WGHT 0.062500 3.090600 FVAR 1.03509 RH1 7 0.879706 0.392397 0.882799 11.00000 0.02692 0.02172 = 0.03292 -0.00134 -0.00076 0.00180 P1 6 0.765041 0.329756 0.850579 11.00000 0.02915 0.02247 = 0.02450 0.00025 0.00136 0.00128 P2 6 0.786552 0.473809 0.905326 11.00000 0.02695 0.02564 = 0.02842 -0.00088 -0.00134 0.00090 O1 4 0.751406 0.328988 0.788486 11.00000 0.03127 0.02553 = 0.02841 0.00069 0.00387 0.00299 O2 4 0.662122 0.356611 0.869406 11.00000 0.02717 0.02730 = 0.02824 -0.00123 -0.00188 -0.00078 O3 4 0.650120 0.200318 0.753762 11.00000 0.03887 0.03920 = 0.03657 -0.00378 -0.00886 -0.00173 O4 4 0.712389 0.477143 0.953352 11.00000 0.03006 0.03362 = 0.02965 0.00368 -0.00329 0.00427 O5 4 0.723349 0.502107 0.857619 11.00000 0.03161 0.02626 = 0.02588 -0.00232 0.00273 0.00326 O6 4 0.995805 0.420621 0.992336 11.00000 0.04720 0.03409 = 0.03768 0.00682 -0.01224 -0.00418 O7 4 0.357702 0.900756 0.904494 11.00000 0.28521 0.04893 = 0.11419 0.01531 -0.06559 -0.01838 O8 4 1.040346 0.424298 0.607073 11.00000 0.13334 0.05299 = 0.04210 0.00331 -0.01858 -0.01177 B1 3 0.701156 0.287888 1.075302 11.00000 0.05493 0.03808 = 0.02657 0.00100 -0.00969 -0.00853 F1 5 0.766062 0.277668 1.037837 11.00000 0.20968 0.16487 = 0.06282 -0.03668 0.06280 -0.08948 F2 5 0.728258 0.342735 1.099254 11.00000 0.11885 0.08993 = 0.17241 -0.07474 0.06378 -0.04332 F3 5 0.611182 0.294370 1.060521 11.00000 0.08981 0.13706 = 0.29707 0.16610 -0.11347 -0.06708 F4 5 0.703801 0.236588 1.109890 11.00000 0.05416 0.08961 = 0.09911 0.04875 -0.00796 -0.00010 C1 1 0.723614 0.390363 0.767530 11.00000 0.03459 0.02544 = 0.02866 0.00513 0.00160 0.00362 C2 1 0.795400 0.427267 0.743204 11.00000 0.03155 0.03565 = 0.03551 -0.00197 0.00429 -0.00259 AFIX 43 H2A 2 0.858832 0.411200 0.741357 11.00000 -1.20000 AFIX 0 C3 1 0.771882 0.486807 0.722259 11.00000 0.04942 0.04102 = 0.03378 0.01278 0.01024 -0.00626 AFIX 43 H3A 2 0.819531 0.512307 0.705522 11.00000 -1.20000 AFIX 0 C4 1 0.678344 0.510868 0.725103 11.00000 0.04978 0.02973 = 0.03160 -0.00286 0.00711 0.00050 C5 1 0.653109 0.574396 0.703114 11.00000 0.07070 0.02780 = 0.03894 0.01273 0.00389 -0.00141 AFIX 43 H5A 2 0.699924 0.599412 0.685259 11.00000 -1.20000 AFIX 0 C6 1 0.563926 0.598096 0.707835 11.00000 0.07182 0.02637 = 0.03998 0.00677 -0.00555 0.00456 AFIX 43 H6A 2 0.548000 0.639219 0.692631 11.00000 -1.20000 AFIX 0 C7 1 0.494567 0.562560 0.734983 11.00000 0.04684 0.03871 = 0.03993 -0.00434 0.00073 0.00969 AFIX 43 H7A 2 0.432527 0.580536 0.738834 11.00000 -1.20000 AFIX 0 C8 1 0.514662 0.502321 0.756080 11.00000 0.03605 0.02094 = 0.03617 -0.00107 -0.00638 0.00505 AFIX 43 H8A 2 0.466619 0.479421 0.774717 11.00000 -1.20000 AFIX 0 C9 1 0.605989 0.473657 0.750527 11.00000 0.04648 0.02446 = 0.02317 -0.00071 -0.00508 -0.00074 C10 1 0.630784 0.409048 0.770709 11.00000 0.02819 0.02246 = 0.02590 0.00039 -0.00292 -0.00228 C11 1 0.558858 0.365501 0.795861 11.00000 0.03127 0.02307 = 0.02700 -0.00088 0.00498 0.00667 C12 1 0.468317 0.347887 0.772514 11.00000 0.02814 0.02529 = 0.02800 -0.00936 -0.00031 0.00868 C13 1 0.442517 0.367683 0.721682 11.00000 0.03913 0.02330 = 0.04013 -0.00447 -0.00167 0.00893 AFIX 43 H13A 2 0.487386 0.390117 0.700513 11.00000 -1.20000 AFIX 0 C14 1 0.353728 0.354721 0.703003 11.00000 0.03861 0.03023 = 0.03700 -0.00860 -0.01275 0.00787 AFIX 43 H14A 2 0.336459 0.369759 0.669380 11.00000 -1.20000 AFIX 0 C15 1 0.287551 0.319503 0.732726 11.00000 0.03388 0.04658 = 0.05419 -0.01895 -0.00816 0.00962 AFIX 43 H15A 2 0.225163 0.312294 0.719654 11.00000 -1.20000 AFIX 0 C16 1 0.311786 0.295854 0.779619 11.00000 0.03597 0.03504 = 0.04304 -0.00694 0.00648 -0.00382 AFIX 43 H16A 2 0.266940 0.270814 0.798899 11.00000 -1.20000 AFIX 0 C17 1 0.403417 0.307807 0.800669 11.00000 0.02848 0.03335 = 0.03470 -0.00640 0.00400 0.00324 C18 1 0.430209 0.280822 0.848805 11.00000 0.03086 0.03161 = 0.03820 -0.00434 0.00690 -0.00232 AFIX 43 H18A 2 0.387509 0.252848 0.866988 11.00000 -1.20000 AFIX 0 C19 1 0.517262 0.294742 0.869371 11.00000 0.03353 0.02875 = 0.02560 0.00340 0.00391 0.00597 AFIX 43 H19A 2 0.535863 0.275239 0.901311 11.00000 -1.20000 AFIX 0 C20 1 0.579910 0.337903 0.843556 11.00000 0.02542 0.02360 = 0.02850 -0.00420 0.00048 0.00074 C21 1 0.760537 0.242914 0.867510 11.00000 0.02822 0.02236 = 0.03307 -0.00006 -0.00448 0.00228 C22 1 0.738911 0.234326 0.920858 11.00000 0.03867 0.02914 = 0.02658 -0.00200 -0.00287 0.00413 AFIX 43 H22A 2 0.731711 0.271845 0.942484 11.00000 -1.20000 AFIX 0 C23 1 0.728408 0.173738 0.941369 11.00000 0.04511 0.03512 = 0.03120 0.00299 -0.00525 -0.00169 AFIX 43 H23A 2 0.714856 0.169237 0.977324 11.00000 -1.20000 AFIX 0 C24 1 0.737226 0.116883 0.910271 11.00000 0.03714 0.03189 = 0.03715 0.00574 0.00145 0.00113 C25 1 0.723176 0.052832 0.930625 11.00000 0.07888 0.03830 = 0.05487 0.00693 0.01345 -0.00425 AFIX 43 H25A 2 0.706998 0.047425 0.966178 11.00000 -1.20000 AFIX 0 C26 1 0.732613 -0.000556 0.899864 11.00000 0.08767 0.02787 = 0.07197 0.01619 0.02145 -0.00597 AFIX 43 H26A 2 0.724390 -0.043170 0.914309 11.00000 -1.20000 AFIX 0 C27 1 0.754334 0.005815 0.846981 11.00000 0.07430 0.02905 = 0.07415 -0.00895 0.01253 -0.00654 AFIX 43 H27A 2 0.759955 -0.032147 0.825700 11.00000 -1.20000 AFIX 0 C28 1 0.767314 0.066828 0.826349 11.00000 0.04252 0.03330 = 0.04463 -0.00457 0.00510 -0.00842 AFIX 43 H28A 2 0.782111 0.070778 0.790499 11.00000 -1.20000 AFIX 0 C29 1 0.759378 0.124619 0.856841 11.00000 0.02973 0.02417 = 0.04288 -0.00038 0.00361 -0.00502 C30 1 0.773800 0.188864 0.835349 11.00000 0.01858 0.02629 = 0.03275 0.00488 -0.00191 -0.00162 C31 1 0.807916 0.193060 0.780370 11.00000 0.03641 0.02284 = 0.02554 -0.00458 -0.00025 -0.00097 C32 1 0.907239 0.187279 0.770444 11.00000 0.04386 0.02410 = 0.03111 -0.00398 0.00693 -0.00268 C33 1 0.976058 0.177523 0.809841 11.00000 0.03183 0.02992 = 0.03767 -0.00947 0.00249 -0.00392 AFIX 43 H33A 2 0.955618 0.174045 0.844889 11.00000 -1.20000 AFIX 0 C34 1 1.070887 0.172971 0.798940 11.00000 0.03334 0.03878 = 0.04927 -0.01586 -0.00198 -0.00106 AFIX 43 H34A 2 1.115269 0.166939 0.826361 11.00000 -1.20000 AFIX 0 C35 1 1.103316 0.177123 0.747629 11.00000 0.03287 0.04669 = 0.06502 -0.02607 0.01293 -0.00348 AFIX 43 H35A 2 1.169589 0.175585 0.740332 11.00000 -1.20000 AFIX 0 C36 1 1.038928 0.183408 0.708090 11.00000 0.05785 0.03825 = 0.04886 -0.01230 0.02249 -0.00756 AFIX 43 H36A 2 1.061013 0.184505 0.673243 11.00000 -1.20000 AFIX 0 C37 1 0.939986 0.188313 0.718063 11.00000 0.04636 0.03362 = 0.03977 -0.00428 0.00766 0.00403 C38 1 0.871956 0.194699 0.678152 11.00000 0.07009 0.04703 = 0.02970 -0.00071 0.01397 -0.00257 AFIX 43 H38A 2 0.892834 0.196174 0.643094 11.00000 -1.20000 AFIX 0 C39 1 0.776274 0.198844 0.688643 11.00000 0.05824 0.03281 = 0.03338 0.00055 -0.00039 -0.00334 AFIX 43 H39A 2 0.731856 0.202578 0.660985 11.00000 -1.20000 AFIX 0 C40 1 0.744040 0.197565 0.740276 11.00000 0.03671 0.02410 = 0.03420 -0.00180 0.00051 -0.00286 C41 1 0.583028 0.213986 0.713731 11.00000 0.05370 0.03668 = 0.04556 -0.00626 -0.01321 0.00127 AFIX 137 H41A 2 0.519051 0.217035 0.728732 11.00000 -1.50000 H41B 2 0.584516 0.178566 0.687943 11.00000 -1.50000 H41C 2 0.599353 0.255762 0.696973 11.00000 -1.50000 AFIX 0 C42 1 0.616156 0.460025 0.948889 11.00000 0.02850 0.02747 = 0.02355 -0.00152 0.00339 0.00464 C43 1 0.585673 0.405638 0.977525 11.00000 0.04394 0.02821 = 0.02863 -0.00043 0.01049 0.00849 AFIX 43 H43A 2 0.628554 0.382380 0.999355 11.00000 -1.20000 AFIX 0 C44 1 0.492496 0.386689 0.973354 11.00000 0.04646 0.02394 = 0.03967 -0.00049 0.01429 -0.00258 AFIX 43 H44A 2 0.470474 0.350805 0.993694 11.00000 -1.20000 AFIX 0 C45 1 0.428506 0.418561 0.940010 11.00000 0.03941 0.02390 = 0.04174 -0.00700 0.01944 -0.00125 C46 1 0.335237 0.393603 0.929205 11.00000 0.03983 0.02700 = 0.05639 -0.00617 0.02382 -0.00293 AFIX 43 H46A 2 0.312783 0.356039 0.947404 11.00000 -1.20000 AFIX 0 C47 1 0.278277 0.422901 0.893248 11.00000 0.02976 0.03067 = 0.08695 -0.01722 0.00993 -0.00448 AFIX 43 H47A 2 0.217320 0.404881 0.885937 11.00000 -1.20000 AFIX 0 C48 1 0.308513 0.478936 0.867142 11.00000 0.03057 0.04022 = 0.05834 -0.01828 0.00078 0.00822 AFIX 43 H48A 2 0.267588 0.499061 0.842445 11.00000 -1.20000 AFIX 0 C49 1 0.395286 0.505249 0.876354 11.00000 0.02677 0.03272 = 0.03986 -0.00713 0.00100 0.00571 AFIX 43 H49A 2 0.413596 0.544297 0.858733 11.00000 -1.20000 AFIX 0 C50 1 0.458711 0.475986 0.911413 11.00000 0.03195 0.02271 = 0.03348 -0.00996 0.00861 -0.00364 C51 1 0.557000 0.498855 0.919014 11.00000 0.03462 0.02363 = 0.02690 -0.00603 0.00757 0.00145 C52 1 0.591373 0.560740 0.895218 11.00000 0.03164 0.02041 = 0.02518 0.00142 0.00226 -0.00027 C53 1 0.546841 0.623065 0.904649 11.00000 0.03191 0.02733 = 0.02473 0.00167 -0.00554 -0.00398 C54 1 0.468244 0.630447 0.938670 11.00000 0.02757 0.03359 = 0.04054 -0.00942 0.00170 0.00083 AFIX 43 H54A 2 0.443202 0.593017 0.956015 11.00000 -1.20000 AFIX 0 C55 1 0.427965 0.690955 0.946830 11.00000 0.03304 0.03852 = 0.04781 -0.01969 0.00169 -0.00018 AFIX 43 H55A 2 0.376059 0.695074 0.970255 11.00000 -1.20000 AFIX 0 C56 1 0.462495 0.747127 0.920949 11.00000 0.04892 0.02835 = 0.04547 -0.01141 -0.00834 0.00219 AFIX 43 H56A 2 0.431951 0.788397 0.925606 11.00000 -1.20000 AFIX 0 C57 1 0.538467 0.742243 0.889762 11.00000 0.04249 0.02037 = 0.04244 -0.00471 -0.00588 0.00233 AFIX 43 H57A 2 0.563126 0.780797 0.873847 11.00000 -1.20000 AFIX 0 C58 1 0.583268 0.680492 0.879869 11.00000 0.03807 0.03053 = 0.03316 -0.00125 -0.00509 -0.00089 C59 1 0.662329 0.674792 0.847114 11.00000 0.04089 0.02468 = 0.04033 0.00986 0.00495 -0.00360 AFIX 43 H59A 2 0.685793 0.712832 0.829941 11.00000 -1.20000 AFIX 0 C60 1 0.706512 0.615814 0.839275 11.00000 0.03184 0.03383 = 0.03211 0.00778 0.00398 -0.00565 AFIX 43 H60A 2 0.760053 0.612469 0.816890 11.00000 -1.20000 AFIX 0 C61 1 0.671063 0.560539 0.864968 11.00000 0.02754 0.01613 = 0.03390 -0.00203 -0.00367 0.00459 C62 1 0.866442 0.539387 0.927524 11.00000 0.02981 0.02639 = 0.02551 -0.00104 -0.00082 0.00201 C63 1 0.832989 0.601079 0.946384 11.00000 0.02893 0.02936 = 0.03458 -0.00933 -0.00231 0.00126 AFIX 43 H63A 2 0.766679 0.609713 0.948991 11.00000 -1.20000 AFIX 0 C64 1 0.897712 0.647235 0.960541 11.00000 0.04365 0.02796 = 0.03016 -0.00556 0.00141 0.00773 AFIX 43 H64A 2 0.875317 0.688627 0.972526 11.00000 -1.20000 AFIX 0 C65 1 0.997704 0.636330 0.958216 11.00000 0.03712 0.02712 = 0.02886 -0.00291 0.00050 -0.00147 C66 1 1.065759 0.683871 0.973024 11.00000 0.04920 0.02941 = 0.04494 -0.01549 0.00654 0.00059 AFIX 43 H66A 2 1.045071 0.726252 0.983697 11.00000 -1.20000 AFIX 0 C67 1 1.160655 0.669918 0.972247 11.00000 0.03918 0.05316 = 0.06726 -0.02873 0.00060 -0.01407 AFIX 43 H67A 2 1.205412 0.702774 0.981848 11.00000 -1.20000 AFIX 0 C68 1 1.193131 0.606460 0.957150 11.00000 0.03128 0.04669 = 0.06663 -0.01682 0.00589 -0.00028 AFIX 43 H68A 2 1.259244 0.596566 0.957328 11.00000 -1.20000 AFIX 0 C69 1 1.128588 0.559943 0.942418 11.00000 0.03756 0.03809 = 0.05071 -0.01497 0.00751 -0.00330 AFIX 43 H69A 2 1.150864 0.517902 0.931857 11.00000 -1.20000 AFIX 0 C70 1 1.030323 0.572285 0.942384 11.00000 0.03289 0.02689 = 0.03023 -0.00685 0.00266 -0.00004 C71 1 0.961021 0.525120 0.926082 11.00000 0.03300 0.02290 = 0.02704 -0.00160 0.00296 0.00369 C72 1 0.993578 0.459375 0.906718 11.00000 0.01993 0.02367 = 0.03834 -0.00458 -0.00454 0.00309 C73 1 1.018347 0.452438 0.852062 11.00000 0.02171 0.02803 = 0.03580 -0.00504 0.00641 -0.00676 C74 1 1.025871 0.505573 0.817025 11.00000 0.03644 0.03498 = 0.03941 -0.00233 0.00333 0.00190 AFIX 43 H74A 2 1.018116 0.549422 0.829041 11.00000 -1.20000 AFIX 0 C75 1 1.044264 0.493820 0.765984 11.00000 0.03844 0.05651 = 0.04057 -0.00470 0.01327 -0.01017 AFIX 43 H75A 2 1.049493 0.529906 0.742732 11.00000 -1.20000 AFIX 0 C76 1 1.055649 0.429872 0.746957 11.00000 0.05309 0.05558 = 0.04254 -0.01306 0.02292 -0.00781 AFIX 43 H76A 2 1.069778 0.423153 0.711284 11.00000 -1.20000 AFIX 0 C77 1 1.046747 0.377916 0.778759 11.00000 0.03130 0.04925 = 0.05235 -0.02637 0.00394 0.00079 AFIX 43 H77A 2 1.052206 0.334758 0.764945 11.00000 -1.20000 AFIX 0 C78 1 1.029462 0.386202 0.832231 11.00000 0.02510 0.03122 = 0.04975 -0.01254 0.01040 0.00010 C79 1 1.018089 0.332673 0.867733 11.00000 0.02564 0.02999 = 0.05743 -0.01148 0.00319 0.00298 AFIX 13 H79A 2 1.011757 0.287330 0.853097 11.00000 -1.20000 AFIX 0 C80 1 1.010224 0.340390 0.921260 11.00000 0.02780 0.02505 = 0.05485 0.01040 -0.00470 0.00602 AFIX 13 H80A 2 1.000694 0.301239 0.944175 11.00000 -1.20000 AFIX 0 C81 1 1.000875 0.405358 0.941757 11.00000 0.03124 0.02756 = 0.03310 -0.00108 -0.01000 -0.00198 C82 1 0.967167 0.368448 1.028069 11.00000 0.06968 0.05045 = 0.04730 0.00935 -0.00521 -0.00439 AFIX 137 H82A 2 0.961952 0.386383 1.063266 11.00000 -1.50000 H82B 2 1.014937 0.333316 1.027619 11.00000 -1.50000 H82C 2 0.905403 0.350647 1.017293 11.00000 -1.50000 AFIX 0 C83 1 0.206128 0.842595 0.897963 11.00000 0.30031 0.15109 = 0.33697 -0.08395 -0.07123 -0.09468 AFIX 137 H83A 2 0.243305 0.823345 0.869578 11.00000 -1.50000 H83B 2 0.139657 0.847452 0.887033 11.00000 -1.50000 H83C 2 0.209296 0.813735 0.928384 11.00000 -1.50000 AFIX 0 C84 1 0.249056 0.913663 0.912576 11.00000 0.08328 0.13279 = 0.08205 0.01814 -0.02036 0.04771 AFIX 23 H84A 2 0.225156 0.948364 0.888974 11.00000 -1.20000 H84B 2 0.234560 0.925863 0.948932 11.00000 -1.20000 AFIX 0 C85 1 0.389113 0.965810 0.920617 11.00000 0.21665 0.08323 = 0.04949 0.00630 0.00278 -0.08330 AFIX 23 H85A 2 0.360190 1.001036 0.899279 11.00000 -1.20000 H85B 2 0.375929 0.974130 0.957795 11.00000 -1.20000 AFIX 0 C86 1 0.489619 0.958593 0.910516 11.00000 0.27849 0.09629 = 0.07131 -0.00665 0.03973 -0.06790 AFIX 137 H86A 2 0.525410 0.989369 0.932346 11.00000 -1.50000 H86B 2 0.502426 0.968049 0.873872 11.00000 -1.50000 H86C 2 0.509292 0.913460 0.918470 11.00000 -1.50000 AFIX 0 C87 1 1.109483 0.320489 0.614235 11.00000 0.27470 0.04579 = 0.08058 -0.01050 -0.07282 0.00149 AFIX 137 H87A 2 1.143423 0.286058 0.595094 11.00000 -1.50000 H87B 2 1.055682 0.300984 0.632944 11.00000 -1.50000 H87C 2 1.152949 0.341249 0.639081 11.00000 -1.50000 AFIX 0 C88 1 1.073733 0.370734 0.577263 11.00000 0.16988 0.05302 = 0.07136 -0.00248 -0.04568 -0.00755 AFIX 23 H88A 2 1.125540 0.385170 0.553823 11.00000 -1.20000 H88B 2 1.021486 0.352343 0.555933 11.00000 -1.20000 AFIX 0 C89 1 1.008828 0.478058 0.575491 11.00000 0.08103 0.06423 = 0.05077 0.00786 0.00101 -0.00084 AFIX 23 H89A 2 0.953898 0.464191 0.554033 11.00000 -1.20000 H89B 2 1.060726 0.492126 0.551972 11.00000 -1.20000 AFIX 0 C90 1 0.980841 0.533152 0.609553 11.00000 0.09290 0.07760 = 0.05488 -0.00403 -0.00040 0.01058 AFIX 137 H90A 2 0.953575 0.568609 0.588502 11.00000 -1.50000 H90B 2 1.036985 0.549555 0.628069 11.00000 -1.50000 H90C 2 0.933384 0.517867 0.634700 11.00000 -1.50000 HKLF 4 REM ljh71 in P2(1)2(1)2(1) REM R1 = 0.0401 for 8181 Fo > 4sig(Fo) and 0.0461 for all 8935 data REM 961 parameters refined using 0 restraints END WGHT 0.0625 3.2349 REM Highest difference peak 0.798, deepest hole -0.501, 1-sigma level 0.057 Q1 1 0.3233 0.8817 0.8773 11.00000 0.05 0.80 Q2 1 0.4310 0.8894 0.8944 11.00000 0.05 0.73 Q3 1 0.6017 0.3017 1.0784 11.00000 0.05 0.62 Q4 1 0.7035 0.2191 1.0669 11.00000 0.05 0.51 Q5 1 0.6374 0.2678 1.0357 11.00000 0.05 0.48 ; #===END