####################################################################### # # 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_rovis106_0m _database_code_depnum_ccdc_archive 'CCDC 901682' #TrackingRef '- Rovis106_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H28 Cl F20 N O4 P Rh, C H2 Cl2' _chemical_formula_sum 'C44 H28 Cl3 F20 N O4 P Rh' _chemical_formula_weight 1254.90 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5246(6) _cell_length_b 12.6819(7) _cell_length_c 17.2832(9) _cell_angle_alpha 68.867(2) _cell_angle_beta 84.990(3) _cell_angle_gamma 77.050(3) _cell_volume 2296.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 9951 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 31.26 _exptl_crystal_description Plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not determined' _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 0.709 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7794 _exptl_absorpt_correction_T_max 0.9364 _exptl_absorpt_process_details 'Sheldrick, G. M. (2008) SADABS. University of Gottingen, Germany.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64119 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 33.21 _reflns_number_total 17541 _reflns_number_gt 13133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'APEX2 (Bruker, 2009)' _computing_data_reduction 'APEX2 (Bruker, 2009)' _computing_structure_solution 'XS (Sheldrick, 2008)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_molecular_graphics 'APEX2 (Bruker, 2009)' _computing_publication_material 'APEX2 (Bruker, 2009)' _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^)+(0.0830P)^2^+0.5902P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17541 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1536 _refine_ls_wR_factor_gt 0.1323 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5785(2) 0.6845(2) 0.45634(14) 0.0222(5) Uani 1 1 d . . . H1 H 0.6299 0.6360 0.4285 0.027 Uiso 1 1 calc R . . C2 C 0.5018(3) 0.6309(3) 0.51392(17) 0.0295(6) Uani 1 1 d . . . H2 H 0.5091 0.5497 0.5205 0.035 Uiso 1 1 calc R . . C3 C 0.5884(3) 0.8412(2) 0.53780(16) 0.0237(5) Uani 1 1 d . . . H3 H 0.6332 0.8784 0.5623 0.028 Uiso 1 1 calc R . . C4 C 0.4968(2) 0.7962(2) 0.58908(16) 0.0258(5) Uani 1 1 d . . . H4 H 0.4899 0.8078 0.6425 0.031 Uiso 1 1 calc R . . C5 C 0.3792(3) 0.7928(3) 0.55677(19) 0.0357(7) Uani 1 1 d . . . H5A H 0.3176 0.7981 0.5979 0.043 Uiso 1 1 calc R . . H5B H 0.3580 0.8600 0.5070 0.043 Uiso 1 1 calc R . . C6 C 0.3816(3) 0.6852(4) 0.5370(2) 0.0434(9) Uani 1 1 d . . . H6A H 0.3526 0.6289 0.5850 0.052 Uiso 1 1 calc R . . H6B H 0.3275 0.7050 0.4917 0.052 Uiso 1 1 calc R . . C7 C 0.5479(3) 0.8124(3) 0.40490(16) 0.0300(6) Uani 1 1 d . . . H7A H 0.5836 0.8248 0.3502 0.036 Uiso 1 1 calc R . . H7B H 0.4623 0.8366 0.3981 0.036 Uiso 1 1 calc R . . C8 C 0.5908(3) 0.8863(2) 0.44387(17) 0.0304(6) Uani 1 1 d . . . H8A H 0.6717 0.8923 0.4252 0.036 Uiso 1 1 calc R . . H8B H 0.5415 0.9635 0.4241 0.036 Uiso 1 1 calc R . . C9 C 0.7699(2) 0.78795(19) 0.77470(13) 0.0155(4) Uani 1 1 d . . . C10 C 0.7939(2) 0.6743(2) 0.85236(13) 0.0153(4) Uani 1 1 d . . . H10 H 0.8661 0.6212 0.8444 0.018 Uiso 1 1 calc R . . C11 C 0.6847(2) 0.6179(2) 0.86695(13) 0.0150(4) Uani 1 1 d . . . H11 H 0.6150 0.6756 0.8393 0.018 Uiso 1 1 calc R . . C12 C 0.7100(2) 0.51558(19) 0.83282(13) 0.0149(4) Uani 1 1 d . . . C13 C 0.7407(2) 0.6263(2) 0.99138(13) 0.0188(4) Uani 1 1 d . . . C14 C 0.6617(3) 0.7017(3) 1.03384(17) 0.0275(6) Uani 1 1 d . . . H14A H 0.7099 0.7350 1.0574 0.041 Uiso 1 1 calc R . . H14B H 0.6165 0.6558 1.0770 0.041 Uiso 1 1 calc R . . H14C H 0.6083 0.7622 0.9941 0.041 Uiso 1 1 calc R . . C15 C 0.8284(3) 0.5271(3) 1.04928(17) 0.0285(6) Uani 1 1 d . . . H15A H 0.8814 0.4878 1.0177 0.043 Uiso 1 1 calc R . . H15B H 0.7857 0.4740 1.0889 0.043 Uiso 1 1 calc R . . H15C H 0.8735 0.5567 1.0779 0.043 Uiso 1 1 calc R . . C16 C 0.6032(2) 0.4877(2) 0.80177(13) 0.0166(4) Uani 1 1 d . . . C17 C 0.6272(2) 0.3936(2) 0.77434(14) 0.0193(4) Uani 1 1 d . . . C18 C 0.5415(3) 0.3621(2) 0.74162(15) 0.0230(5) Uani 1 1 d . . . C19 C 0.4255(2) 0.4239(2) 0.73561(15) 0.0232(5) Uani 1 1 d . . . C20 C 0.3984(2) 0.5170(2) 0.76193(14) 0.0213(5) Uani 1 1 d . . . C21 C 0.4850(2) 0.5472(2) 0.79527(14) 0.0189(4) Uani 1 1 d . . . C22 C 0.7721(2) 0.4049(2) 0.90149(13) 0.0165(4) Uani 1 1 d . . . C23 C 0.8924(2) 0.3559(2) 0.90545(14) 0.0192(4) Uani 1 1 d . . . C24 C 0.9409(2) 0.2546(2) 0.96900(17) 0.0258(5) Uani 1 1 d . . . C25 C 0.8685(3) 0.2005(2) 1.03135(17) 0.0300(6) Uani 1 1 d . . . C26 C 0.7483(3) 0.2470(2) 1.02997(16) 0.0272(6) Uani 1 1 d . . . C27 C 0.7021(2) 0.3473(2) 0.96621(15) 0.0214(5) Uani 1 1 d . . . C28 C 0.9140(2) 0.7214(3) 0.55473(16) 0.0272(6) Uani 1 1 d . . . H28A H 0.9194 0.8008 0.5436 0.033 Uiso 1 1 calc R . . H28B H 0.8492 0.7209 0.5226 0.033 Uiso 1 1 calc R . . C29 C 1.0301(3) 0.6530(3) 0.53451(18) 0.0317(6) Uani 1 1 d . . . H29A H 1.0176 0.5878 0.5220 0.038 Uiso 1 1 calc R . . H29B H 1.0702 0.7011 0.4879 0.038 Uiso 1 1 calc R . . C30 C 1.0996(3) 0.6137(3) 0.6129(2) 0.0362(7) Uani 1 1 d . . . H30A H 1.1335 0.6753 0.6163 0.043 Uiso 1 1 calc R . . H30B H 1.1632 0.5476 0.6162 0.043 Uiso 1 1 calc R . . C31 C 1.0075(2) 0.5812(2) 0.68157(16) 0.0250(5) Uani 1 1 d . . . H31A H 1.0015 0.5012 0.6958 0.030 Uiso 1 1 calc R . . H31B H 1.0276 0.5926 0.7309 0.030 Uiso 1 1 calc R . . C32 C 0.8786(2) 0.8368(2) 0.73231(13) 0.0172(4) Uani 1 1 d . . . C33 C 0.8600(2) 0.9307(2) 0.65824(15) 0.0217(5) Uani 1 1 d . . . C34 C 0.9504(3) 0.9836(2) 0.61470(16) 0.0292(6) Uani 1 1 d . . . C35 C 1.0644(3) 0.9443(3) 0.64565(18) 0.0295(6) Uani 1 1 d . . . C36 C 1.0864(2) 0.8532(2) 0.71973(17) 0.0251(5) Uani 1 1 d . . . C37 C 0.9942(2) 0.8012(2) 0.76197(14) 0.0199(5) Uani 1 1 d . . . C38 C 0.6825(2) 0.8818(2) 0.79967(14) 0.0196(5) Uani 1 1 d . . . C39 C 0.5599(2) 0.9127(2) 0.78754(15) 0.0221(5) Uani 1 1 d . . . C40 C 0.4870(3) 0.9957(2) 0.81417(17) 0.0289(6) Uani 1 1 d . . . C41 C 0.5345(3) 1.0504(3) 0.8553(2) 0.0374(8) Uani 1 1 d . . . C42 C 0.6545(3) 1.0227(3) 0.86963(19) 0.0348(7) Uani 1 1 d . . . C43 C 0.7262(3) 0.9403(2) 0.84244(16) 0.0248(5) Uani 1 1 d . . . C44 C -0.0079(4) 0.2612(3) 0.7082(3) 0.0520(10) Uani 1 1 d . . . H44A H -0.0177 0.3023 0.7468 0.062 Uiso 1 1 calc R . . H44B H -0.0676 0.3026 0.6655 0.062 Uiso 1 1 calc R . . Cl1 Cl 0.75653(7) 0.47786(6) 0.58986(4) 0.03050(15) Uani 1 1 d . . . Cl2 Cl -0.03619(16) 0.12895(11) 0.75938(15) 0.1253(8) Uani 1 1 d . . . Cl3 Cl 0.13198(11) 0.26727(15) 0.66151(9) 0.0825(4) Uani 1 1 d . . . F1 F 0.73703(14) 0.32882(13) 0.78025(10) 0.0247(3) Uani 1 1 d . . . F2 F 0.57022(16) 0.27119(15) 0.71672(11) 0.0321(4) Uani 1 1 d . . . F3 F 0.34063(15) 0.39272(16) 0.70617(10) 0.0323(4) Uani 1 1 d . . . F4 F 0.28565(14) 0.57638(16) 0.75747(10) 0.0300(4) Uani 1 1 d . . . F5 F 0.44770(14) 0.63574(14) 0.82260(10) 0.0261(3) Uani 1 1 d . . . F6 F 0.97052(13) 0.40293(14) 0.84843(9) 0.0258(3) Uani 1 1 d . . . F7 F 1.05756(16) 0.21015(16) 0.96802(11) 0.0357(4) Uani 1 1 d . . . F8 F 0.91419(19) 0.10296(16) 1.09243(12) 0.0454(5) Uani 1 1 d . . . F9 F 0.67618(17) 0.19618(16) 1.08989(11) 0.0396(5) Uani 1 1 d . . . F10 F 0.58484(13) 0.38797(14) 0.96854(9) 0.0255(3) Uani 1 1 d . . . F11 F 1.02241(14) 0.71589(14) 0.83486(9) 0.0253(3) Uani 1 1 d . . . F12 F 1.19556(15) 0.81683(16) 0.75178(12) 0.0341(4) Uani 1 1 d . . . F13 F 1.15164(17) 0.99559(17) 0.60464(12) 0.0422(5) Uani 1 1 d . . . F14 F 0.92645(17) 1.07294(16) 0.54348(11) 0.0414(5) Uani 1 1 d . . . F15 F 0.75013(14) 0.97531(14) 0.62615(9) 0.0270(3) Uani 1 1 d . . . F16 F 0.84235(16) 0.91758(15) 0.85886(10) 0.0292(4) Uani 1 1 d . . . F17 F 0.7015(2) 1.07616(19) 0.90947(14) 0.0519(6) Uani 1 1 d . . . F18 F 0.4635(2) 1.13202(18) 0.88026(15) 0.0557(6) Uani 1 1 d . . . F19 F 0.36978(16) 1.02332(16) 0.79875(11) 0.0372(4) Uani 1 1 d . . . F20 F 0.50411(14) 0.86340(14) 0.74940(9) 0.0256(3) Uani 1 1 d . . . N1 N 0.89593(18) 0.66048(18) 0.64494(12) 0.0185(4) Uani 1 1 d . . . O1 O 0.71240(14) 0.76168(14) 0.71482(9) 0.0150(3) Uani 1 1 d . . . O2 O 0.79069(14) 0.54338(14) 0.76347(9) 0.0150(3) Uani 1 1 d . . . O3 O 0.80131(17) 0.69844(15) 0.92503(10) 0.0202(4) Uani 1 1 d . . . O4 O 0.66722(16) 0.58003(15) 0.95381(10) 0.0199(3) Uani 1 1 d . . . P1 P 0.75947(5) 0.65605(5) 0.67899(3) 0.01392(11) Uani 1 1 d . . . Rh1 Rh 0.638240(16) 0.659195(15) 0.583158(10) 0.01550(6) Uani 1 1 d . . . 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 C1 0.0308(13) 0.0203(12) 0.0162(9) -0.0070(9) -0.0040(9) -0.0046(10) C2 0.0348(15) 0.0341(15) 0.0287(13) -0.0157(11) -0.0045(11) -0.0156(13) C3 0.0317(13) 0.0147(11) 0.0253(11) -0.0087(9) -0.0082(10) -0.0001(10) C4 0.0231(12) 0.0278(14) 0.0221(11) -0.0104(10) -0.0046(9) 0.0078(11) C5 0.0202(13) 0.052(2) 0.0298(13) -0.0133(13) -0.0046(11) 0.0027(13) C6 0.0279(15) 0.066(2) 0.0339(15) -0.0075(16) -0.0040(12) -0.0199(16) C7 0.0422(16) 0.0267(14) 0.0183(11) -0.0049(10) -0.0056(11) -0.0049(13) C8 0.0460(17) 0.0181(12) 0.0239(12) -0.0015(9) -0.0032(11) -0.0091(12) C9 0.0205(10) 0.0119(10) 0.0130(8) -0.0028(7) 0.0005(8) -0.0044(8) C10 0.0212(10) 0.0144(10) 0.0118(8) -0.0053(7) 0.0016(7) -0.0062(9) C11 0.0184(10) 0.0138(10) 0.0126(8) -0.0036(7) 0.0021(7) -0.0055(8) C12 0.0166(10) 0.0132(10) 0.0132(8) -0.0029(7) 0.0012(7) -0.0032(8) C13 0.0262(12) 0.0193(11) 0.0125(9) -0.0057(8) 0.0033(8) -0.0091(10) C14 0.0334(14) 0.0286(14) 0.0258(12) -0.0156(11) 0.0085(11) -0.0102(12) C15 0.0320(14) 0.0250(13) 0.0230(11) 0.0001(10) -0.0050(10) -0.0075(11) C16 0.0199(10) 0.0142(10) 0.0146(9) -0.0036(8) 0.0004(8) -0.0040(9) C17 0.0233(11) 0.0153(11) 0.0179(9) -0.0039(8) -0.0018(8) -0.0039(9) C18 0.0336(14) 0.0174(11) 0.0202(10) -0.0072(9) -0.0021(10) -0.0078(10) C19 0.0281(13) 0.0282(13) 0.0166(10) -0.0067(9) -0.0020(9) -0.0137(11) C20 0.0196(11) 0.0252(13) 0.0169(9) -0.0038(9) -0.0007(8) -0.0057(10) C21 0.0213(11) 0.0188(11) 0.0159(9) -0.0052(8) 0.0011(8) -0.0049(9) C22 0.0206(11) 0.0133(10) 0.0146(9) -0.0032(8) -0.0014(8) -0.0035(9) C23 0.0226(11) 0.0166(11) 0.0177(9) -0.0051(8) -0.0002(8) -0.0044(9) C24 0.0254(12) 0.0206(12) 0.0266(12) -0.0042(10) -0.0065(10) 0.0002(10) C25 0.0413(16) 0.0147(12) 0.0249(12) 0.0046(9) -0.0097(11) -0.0037(11) C26 0.0339(14) 0.0207(12) 0.0209(11) 0.0030(9) -0.0024(10) -0.0103(11) C27 0.0246(12) 0.0192(12) 0.0181(10) -0.0013(9) -0.0012(9) -0.0085(10) C28 0.0206(12) 0.0333(15) 0.0211(11) -0.0043(10) 0.0060(9) -0.0034(11) C29 0.0277(14) 0.0375(17) 0.0288(13) -0.0131(12) 0.0088(11) -0.0059(12) C30 0.0195(12) 0.0432(18) 0.0384(15) -0.0101(14) 0.0061(11) -0.0015(12) C31 0.0198(11) 0.0267(13) 0.0241(11) -0.0050(10) -0.0007(9) -0.0024(10) C32 0.0228(11) 0.0154(10) 0.0139(9) -0.0044(8) 0.0018(8) -0.0073(9) C33 0.0276(12) 0.0176(11) 0.0175(10) -0.0022(8) 0.0021(9) -0.0070(10) C34 0.0358(15) 0.0243(13) 0.0219(11) 0.0013(10) 0.0049(11) -0.0125(12) C35 0.0296(14) 0.0290(14) 0.0308(13) -0.0087(11) 0.0118(11) -0.0156(12) C36 0.0213(12) 0.0244(13) 0.0317(13) -0.0109(10) 0.0019(10) -0.0075(10) C37 0.0252(12) 0.0161(11) 0.0184(10) -0.0050(8) -0.0002(9) -0.0059(9) C38 0.0286(12) 0.0140(10) 0.0159(9) -0.0049(8) 0.0062(9) -0.0069(9) C39 0.0294(13) 0.0162(11) 0.0170(9) -0.0040(8) 0.0049(9) -0.0024(10) C40 0.0354(15) 0.0163(12) 0.0276(12) -0.0053(10) 0.0121(11) 0.0007(11) C41 0.056(2) 0.0184(13) 0.0377(15) -0.0166(12) 0.0204(15) -0.0045(13) C42 0.0539(19) 0.0262(15) 0.0324(14) -0.0189(12) 0.0135(14) -0.0155(14) C43 0.0372(14) 0.0184(12) 0.0212(11) -0.0092(9) 0.0049(10) -0.0087(11) C44 0.055(2) 0.038(2) 0.057(2) -0.0131(17) 0.0120(18) -0.0069(18) Cl1 0.0456(4) 0.0180(3) 0.0243(3) -0.0098(2) -0.0057(3) 0.0068(3) Cl2 0.1178(13) 0.0319(6) 0.198(2) -0.0250(9) 0.0731(14) -0.0149(7) Cl3 0.0499(6) 0.1181(12) 0.0853(9) -0.0433(9) 0.0159(6) -0.0224(7) F1 0.0259(8) 0.0189(7) 0.0300(8) -0.0115(6) -0.0059(6) 0.0008(6) F2 0.0436(10) 0.0246(9) 0.0358(9) -0.0173(7) -0.0069(8) -0.0086(8) F3 0.0329(9) 0.0409(10) 0.0307(8) -0.0146(7) -0.0062(7) -0.0173(8) F4 0.0185(7) 0.0419(10) 0.0296(8) -0.0134(7) -0.0023(6) -0.0039(7) F5 0.0209(7) 0.0273(8) 0.0337(8) -0.0179(7) 0.0002(6) -0.0007(6) F6 0.0196(7) 0.0270(8) 0.0234(7) -0.0024(6) -0.0001(6) -0.0012(6) F7 0.0279(9) 0.0312(10) 0.0365(9) -0.0041(7) -0.0100(7) 0.0072(7) F8 0.0510(12) 0.0264(10) 0.0382(10) 0.0125(8) -0.0136(9) -0.0022(9) F9 0.0454(11) 0.0339(10) 0.0272(8) 0.0097(7) 0.0013(8) -0.0189(8) F10 0.0223(7) 0.0283(8) 0.0217(7) -0.0015(6) 0.0022(6) -0.0099(6) F11 0.0255(8) 0.0228(8) 0.0232(7) -0.0003(6) -0.0063(6) -0.0070(6) F12 0.0218(8) 0.0339(10) 0.0458(10) -0.0107(8) -0.0009(7) -0.0095(7) F13 0.0352(10) 0.0400(11) 0.0458(10) -0.0037(8) 0.0145(8) -0.0216(9) F14 0.0460(11) 0.0350(10) 0.0279(8) 0.0107(7) 0.0044(8) -0.0165(9) F15 0.0268(8) 0.0230(8) 0.0231(7) 0.0026(6) -0.0034(6) -0.0059(6) F16 0.0397(9) 0.0284(9) 0.0266(7) -0.0131(7) 0.0016(7) -0.0158(8) F17 0.0755(15) 0.0453(12) 0.0589(13) -0.0425(11) 0.0162(12) -0.0259(12) F18 0.0717(15) 0.0343(11) 0.0685(14) -0.0372(11) 0.0306(12) -0.0050(11) F19 0.0321(9) 0.0270(9) 0.0393(9) -0.0063(7) 0.0127(8) 0.0063(7) F20 0.0232(7) 0.0276(8) 0.0261(7) -0.0134(6) -0.0008(6) 0.0017(6) N1 0.0161(9) 0.0191(10) 0.0156(8) -0.0020(7) 0.0011(7) -0.0017(8) O1 0.0187(7) 0.0132(7) 0.0130(6) -0.0051(6) 0.0004(6) -0.0024(6) O2 0.0173(7) 0.0136(7) 0.0124(6) -0.0028(5) 0.0005(6) -0.0029(6) O3 0.0311(9) 0.0209(9) 0.0117(6) -0.0050(6) 0.0016(6) -0.0136(8) O4 0.0273(9) 0.0218(9) 0.0134(7) -0.0063(6) 0.0051(6) -0.0124(7) P1 0.0163(3) 0.0122(3) 0.0120(2) -0.00375(19) 0.00142(19) -0.0019(2) Rh1 0.01924(9) 0.01334(9) 0.01340(8) -0.00485(6) -0.00007(6) -0.00210(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.365(4) . ? C1 C7 1.518(4) . ? C1 Rh1 2.245(2) . ? C2 C6 1.491(5) . ? C2 Rh1 2.219(3) . ? C3 C4 1.403(4) . ? C3 C8 1.514(4) . ? C3 Rh1 2.110(3) . ? C4 C5 1.524(4) . ? C4 Rh1 2.125(3) . ? C5 C6 1.516(5) . ? C7 C8 1.515(4) . ? C9 O1 1.445(3) . ? C9 C32 1.533(3) . ? C9 C38 1.541(3) . ? C9 C10 1.564(3) . ? C10 O3 1.409(3) . ? C10 C11 1.541(3) . ? C11 O4 1.413(3) . ? C11 C12 1.571(3) . ? C12 O2 1.440(2) . ? C12 C16 1.541(3) . ? C12 C22 1.545(3) . ? C13 O3 1.425(3) . ? C13 O4 1.441(3) . ? C13 C14 1.511(4) . ? C13 C15 1.518(4) . ? C16 C21 1.394(3) . ? C16 C17 1.401(3) . ? C17 F1 1.336(3) . ? C17 C18 1.376(4) . ? C18 F2 1.336(3) . ? C18 C19 1.382(4) . ? C19 F3 1.333(3) . ? C19 C20 1.377(4) . ? C20 F4 1.341(3) . ? C20 C21 1.381(4) . ? C21 F5 1.341(3) . ? C22 C23 1.384(3) . ? C22 C27 1.397(3) . ? C23 F6 1.341(3) . ? C23 C24 1.392(3) . ? C24 F7 1.337(3) . ? C24 C25 1.376(4) . ? C25 F8 1.336(3) . ? C25 C26 1.378(4) . ? C26 F9 1.337(3) . ? C26 C27 1.379(3) . ? C27 F10 1.337(3) . ? C28 N1 1.489(3) . ? C28 C29 1.511(4) . ? C29 C30 1.500(5) . ? C30 C31 1.525(4) . ? C31 N1 1.473(3) . ? C32 C37 1.388(4) . ? C32 C33 1.392(3) . ? C33 F15 1.344(3) . ? C33 C34 1.383(3) . ? C34 F14 1.338(3) . ? C34 C35 1.378(4) . ? C35 F13 1.332(3) . ? C35 C36 1.377(4) . ? C36 F12 1.334(3) . ? C36 C37 1.389(3) . ? C37 F11 1.339(3) . ? C38 C39 1.393(4) . ? C38 C43 1.407(4) . ? C39 F20 1.337(3) . ? C39 C40 1.383(4) . ? C40 F19 1.343(4) . ? C40 C41 1.371(5) . ? C41 F18 1.344(3) . ? C41 C42 1.371(5) . ? C42 F17 1.339(4) . ? C42 C43 1.376(4) . ? C43 F16 1.337(3) . ? C44 Cl2 1.681(4) . ? C44 Cl3 1.743(4) . ? Cl1 Rh1 2.3645(7) . ? N1 P1 1.636(2) . ? O1 P1 1.6390(17) . ? O2 P1 1.6309(16) . ? P1 Rh1 2.2423(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C7 122.2(3) . . ? C2 C1 Rh1 71.18(15) . . ? C7 C1 Rh1 110.13(17) . . ? C1 C2 C6 127.1(3) . . ? C1 C2 Rh1 73.21(16) . . ? C6 C2 Rh1 108.7(2) . . ? C4 C3 C8 126.5(3) . . ? C4 C3 Rh1 71.24(15) . . ? C8 C3 Rh1 109.84(18) . . ? C3 C4 C5 123.8(2) . . ? C3 C4 Rh1 70.06(15) . . ? C5 C4 Rh1 113.3(2) . . ? C6 C5 C4 114.1(3) . . ? C2 C6 C5 114.1(3) . . ? C8 C7 C1 112.7(2) . . ? C3 C8 C7 114.5(2) . . ? O1 C9 C32 107.81(17) . . ? O1 C9 C38 108.55(19) . . ? C32 C9 C38 108.55(18) . . ? O1 C9 C10 106.04(17) . . ? C32 C9 C10 116.94(19) . . ? C38 C9 C10 108.68(17) . . ? O3 C10 C11 104.46(17) . . ? O3 C10 C9 111.13(19) . . ? C11 C10 C9 108.50(19) . . ? O4 C11 C10 104.44(18) . . ? O4 C11 C12 112.39(17) . . ? C10 C11 C12 110.19(18) . . ? O2 C12 C16 106.41(17) . . ? O2 C12 C22 108.60(18) . . ? C16 C12 C22 107.92(18) . . ? O2 C12 C11 107.52(16) . . ? C16 C12 C11 117.72(19) . . ? C22 C12 C11 108.39(18) . . ? O3 C13 O4 106.27(17) . . ? O3 C13 C14 107.8(2) . . ? O4 C13 C14 109.0(2) . . ? O3 C13 C15 110.9(2) . . ? O4 C13 C15 108.9(2) . . ? C14 C13 C15 113.6(2) . . ? C21 C16 C17 115.4(2) . . ? C21 C16 C12 127.8(2) . . ? C17 C16 C12 116.8(2) . . ? F1 C17 C18 116.8(2) . . ? F1 C17 C16 120.1(2) . . ? C18 C17 C16 123.0(2) . . ? F2 C18 C17 120.1(2) . . ? F2 C18 C19 120.2(2) . . ? C17 C18 C19 119.7(2) . . ? F3 C19 C20 120.4(2) . . ? F3 C19 C18 120.6(2) . . ? C20 C19 C18 119.0(2) . . ? F4 C20 C19 119.4(2) . . ? F4 C20 C21 119.9(2) . . ? C19 C20 C21 120.8(2) . . ? F5 C21 C20 115.8(2) . . ? F5 C21 C16 122.1(2) . . ? C20 C21 C16 122.1(2) . . ? C23 C22 C27 115.7(2) . . ? C23 C22 C12 126.0(2) . . ? C27 C22 C12 118.2(2) . . ? F6 C23 C22 122.3(2) . . ? F6 C23 C24 115.4(2) . . ? C22 C23 C24 122.4(2) . . ? F7 C24 C25 120.8(2) . . ? F7 C24 C23 119.3(2) . . ? C25 C24 C23 119.9(3) . . ? F8 C25 C24 120.3(3) . . ? F8 C25 C26 120.1(3) . . ? C24 C25 C26 119.5(2) . . ? F9 C26 C25 120.7(2) . . ? F9 C26 C27 119.8(3) . . ? C25 C26 C27 119.6(2) . . ? F10 C27 C26 116.6(2) . . ? F10 C27 C22 120.5(2) . . ? C26 C27 C22 122.9(2) . . ? N1 C28 C29 104.0(2) . . ? C30 C29 C28 102.7(2) . . ? C29 C30 C31 103.9(2) . . ? N1 C31 C30 103.6(2) . . ? C37 C32 C33 115.5(2) . . ? C37 C32 C9 126.9(2) . . ? C33 C32 C9 117.5(2) . . ? F15 C33 C34 116.7(2) . . ? F15 C33 C32 120.2(2) . . ? C34 C33 C32 123.1(3) . . ? F14 C34 C35 120.5(2) . . ? F14 C34 C33 120.0(3) . . ? C35 C34 C33 119.5(2) . . ? F13 C35 C36 120.6(3) . . ? F13 C35 C34 120.0(3) . . ? C36 C35 C34 119.4(2) . . ? F12 C36 C35 120.0(2) . . ? F12 C36 C37 120.1(2) . . ? C35 C36 C37 119.9(3) . . ? F11 C37 C32 121.3(2) . . ? F11 C37 C36 116.1(2) . . ? C32 C37 C36 122.6(2) . . ? C39 C38 C43 114.7(2) . . ? C39 C38 C9 126.2(2) . . ? C43 C38 C9 119.0(2) . . ? F20 C39 C40 115.2(3) . . ? F20 C39 C38 122.2(2) . . ? C40 C39 C38 122.7(3) . . ? F19 C40 C41 120.2(3) . . ? F19 C40 C39 119.7(3) . . ? C41 C40 C39 120.1(3) . . ? F18 C41 C42 120.3(3) . . ? F18 C41 C40 120.0(3) . . ? C42 C41 C40 119.7(3) . . ? F17 C42 C41 120.0(3) . . ? F17 C42 C43 120.4(3) . . ? C41 C42 C43 119.6(3) . . ? F16 C43 C42 116.3(3) . . ? F16 C43 C38 120.6(2) . . ? C42 C43 C38 123.2(3) . . ? Cl2 C44 Cl3 116.8(2) . . ? C31 N1 C28 109.80(19) . . ? C31 N1 P1 128.56(16) . . ? C28 N1 P1 117.95(17) . . ? C9 O1 P1 127.67(15) . . ? C12 O2 P1 123.75(14) . . ? C10 O3 C13 109.76(17) . . ? C11 O4 C13 110.40(16) . . ? O2 P1 N1 97.71(9) . . ? O2 P1 O1 102.68(8) . . ? N1 P1 O1 108.16(10) . . ? O2 P1 Rh1 120.99(7) . . ? N1 P1 Rh1 112.80(8) . . ? O1 P1 Rh1 112.84(7) . . ? C3 Rh1 C4 38.69(11) . . ? C3 Rh1 C2 95.88(11) . . ? C4 Rh1 C2 81.07(12) . . ? C3 Rh1 P1 93.08(8) . . ? C4 Rh1 P1 99.74(8) . . ? C2 Rh1 P1 166.24(8) . . ? C3 Rh1 C1 81.50(10) . . ? C4 Rh1 C1 89.82(10) . . ? C2 Rh1 C1 35.60(10) . . ? P1 Rh1 C1 157.25(7) . . ? C3 Rh1 Cl1 155.33(8) . . ? C4 Rh1 Cl1 164.91(8) . . ? C2 Rh1 Cl1 89.33(9) . . ? P1 Rh1 Cl1 86.84(2) . . ? C1 Rh1 Cl1 89.08(7) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 33.21 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.036 _refine_diff_density_min -1.839 _refine_diff_density_rms 0.175 data_rovis107a _database_code_depnum_ccdc_archive 'CCDC 901683' #TrackingRef '- Rovis107a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H28 Cl F23 N O7 P Rh S' _chemical_formula_weight 1321.06 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4903(10) _cell_length_b 14.3946(14) _cell_length_c 15.5781(15) _cell_angle_alpha 78.012(3) _cell_angle_beta 84.045(3) _cell_angle_gamma 72.010(4) _cell_volume 2186.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9116 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 30.28 _exptl_crystal_description Long _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1310 _exptl_absorpt_coefficient_mu 0.692 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8571 _exptl_absorpt_correction_T_max 0.9590 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37196 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.68 _reflns_number_total 8286 _reflns_number_gt 6711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0871P)^2^+2.4671P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8286 _refine_ls_number_parameters 706 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1524 _refine_ls_wR_factor_gt 0.1191 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _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 C1 C 0.4818(5) 0.5209(3) 0.7231(3) 0.0185(9) Uani 1 1 d . . . H1 H 0.3938 0.5663 0.7356 0.022 Uiso 1 1 calc R . . C2 C 0.5763(5) 0.5050(3) 0.7869(3) 0.0182(9) Uani 1 1 d . . . H2 H 0.5413 0.5415 0.8350 0.022 Uiso 1 1 calc R . . C3 C 0.7983(5) 0.4554(3) 0.6656(3) 0.0249(11) Uani 1 1 d . . . H3 H 0.8805 0.4681 0.6368 0.030 Uiso 1 1 calc R . . C4 C 0.7094(5) 0.4541(3) 0.6092(3) 0.0246(11) Uani 1 1 d . . . H4 H 0.7375 0.4658 0.5469 0.030 Uiso 1 1 calc R . . C5 C 0.6143(5) 0.3906(4) 0.6330(4) 0.0304(12) Uani 1 1 d . . . H5A H 0.6532 0.3338 0.6779 0.037 Uiso 1 1 calc R . . H5B H 0.6037 0.3659 0.5816 0.037 Uiso 1 1 calc R . . C6 C 0.8162(5) 0.3971(4) 0.7596(4) 0.0306(12) Uani 1 1 d . . . H6A H 0.8596 0.3274 0.7578 0.037 Uiso 1 1 calc R . . H6B H 0.8750 0.4202 0.7885 0.037 Uiso 1 1 calc R . . C7 C 0.6849(5) 0.4068(4) 0.8138(3) 0.0289(12) Uani 1 1 d . . . H7A H 0.7028 0.3995 0.8750 0.035 Uiso 1 1 calc R . . H7B H 0.6509 0.3527 0.8087 0.035 Uiso 1 1 calc R . . C8 C 0.4768(5) 0.4484(4) 0.6664(3) 0.0273(11) Uani 1 1 d . . . H8A H 0.4228 0.4848 0.6164 0.033 Uiso 1 1 calc R . . H8B H 0.4327 0.4015 0.7002 0.033 Uiso 1 1 calc R . . C9 C 0.6086(4) 0.7477(3) 0.8664(3) 0.0136(9) Uani 1 1 d . . . H9 H 0.6106 0.6802 0.8622 0.016 Uiso 1 1 calc R . . C10 C 0.4658(4) 0.8065(3) 0.8937(3) 0.0139(9) Uani 1 1 d . . . H10 H 0.4602 0.8766 0.8888 0.017 Uiso 1 1 calc R . . C11 C 0.3466(4) 0.7979(3) 0.8468(3) 0.0123(8) Uani 1 1 d . . . C12 C 0.6672(4) 0.7964(3) 0.7811(3) 0.0129(9) Uani 1 1 d . . . C13 C 0.4022(5) 0.9137(3) 0.5739(3) 0.0216(11) Uani 1.027(8) 1 d P . . H13A H 0.4921 0.9201 0.5625 0.026 Uiso 1.027(8) 1 calc PR . . H13B H 0.3500 0.9625 0.6084 0.026 Uiso 1.027(8) 1 calc PR . . C14 C 0.3388(5) 0.7649(3) 0.5660(3) 0.0224(11) Uani 1.027(8) 1 d P . . H14A H 0.2630 0.7475 0.5987 0.027 Uiso 1.027(8) 1 calc PR . . H14B H 0.4015 0.7058 0.5488 0.027 Uiso 1.027(8) 1 calc PR . . C15 C 0.2945(10) 0.8448(5) 0.4882(5) 0.078(3) Uani 1 1 d . . . H15A H 0.3304 0.8191 0.4350 0.094 Uiso 1 1 calc R . . H15B H 0.1974 0.8653 0.4871 0.094 Uiso 1 1 calc R . . C16 C 0.3360(10) 0.9244(5) 0.4898(5) 0.076(3) Uani 1 1 d . . . H16A H 0.2595 0.9837 0.4833 0.091 Uiso 1 1 calc R . . H16B H 0.3988 0.9323 0.4406 0.091 Uiso 1 1 calc R . . C17 C 0.8015(4) 0.7311(3) 0.7453(3) 0.0140(9) Uani 1 1 d . . . C18 C 0.8765(4) 0.6368(3) 0.7862(3) 0.0165(9) Uani 1 1 d . . . C19 C 0.9998(5) 0.5881(3) 0.7510(3) 0.0207(10) Uani 1 1 d . . . C20 C 1.0511(5) 0.6312(4) 0.6741(3) 0.0231(11) Uani 1 1 d . . . C21 C 0.9787(5) 0.7240(4) 0.6313(3) 0.0220(10) Uani 1 1 d . . . C22 C 0.8569(4) 0.7713(3) 0.6670(3) 0.0172(9) Uani 1 1 d . . . C23 C 0.5945(5) 0.7382(4) 1.0161(3) 0.0249(11) Uani 1 1 d . . . C24 C 0.6020(6) 0.8123(6) 1.0674(5) 0.062(2) Uani 1 1 d . . . H24A H 0.5726 0.8778 1.0325 0.093 Uiso 1 1 calc R . . H24B H 0.6929 0.7986 1.0832 0.093 Uiso 1 1 calc R . . H24C H 0.5452 0.8083 1.1196 0.093 Uiso 1 1 calc R . . C25 C 0.6326(6) 0.6319(5) 1.0674(4) 0.055(2) Uani 1 1 d . . . H25A H 0.5804 0.6291 1.1217 0.083 Uiso 1 1 calc R . . H25B H 0.7262 0.6106 1.0794 0.083 Uiso 1 1 calc R . . H25C H 0.6153 0.5890 1.0333 0.083 Uiso 1 1 calc R . . C26 C 0.6879(4) 0.8954(3) 0.7895(3) 0.0126(9) Uani 1 1 d . . . C27 C 0.7974(4) 0.8943(3) 0.8352(3) 0.0158(9) Uani 1 1 d . . . C28 C 0.8223(4) 0.9793(3) 0.8470(3) 0.0169(9) Uani 1 1 d . . . C29 C 0.7385(5) 1.0711(3) 0.8112(3) 0.0177(9) Uani 1 1 d . . . C30 C 0.6324(4) 1.0758(3) 0.7642(3) 0.0161(9) Uani 1 1 d . . . C31 C 0.6069(4) 0.9901(3) 0.7544(3) 0.0132(9) Uani 1 1 d . . . C32 C 0.1611(4) 0.8902(3) 0.7417(3) 0.0165(9) Uani 1 1 d . . . C33 C 0.0725(5) 0.9703(4) 0.6945(3) 0.0227(10) Uani 1 1 d . . . C34 C 0.0726(5) 1.0646(4) 0.6984(3) 0.0262(11) Uani 1 1 d . . . C35 C 0.1618(5) 1.0765(3) 0.7508(3) 0.0241(11) Uani 1 1 d . . . C36 C 0.2514(5) 0.9929(3) 0.7984(3) 0.0205(10) Uani 1 1 d . . . C37 C 0.2574(4) 0.8970(3) 0.7937(3) 0.0143(9) Uani 1 1 d . . . C38 C 0.2482(4) 0.7574(3) 0.9137(3) 0.0152(9) Uani 1 1 d . . . C39 C 0.2126(4) 0.6715(3) 0.9157(3) 0.0166(9) Uani 1 1 d . . . C40 C 0.1142(5) 0.6464(3) 0.9723(3) 0.0192(10) Uani 1 1 d . . . C41 C 0.0456(4) 0.7074(3) 1.0308(3) 0.0173(9) Uani 1 1 d . . . C42 C 0.0785(4) 0.7920(3) 1.0317(3) 0.0173(9) Uani 1 1 d . . . C43 C 0.1782(4) 0.8154(3) 0.9744(3) 0.0145(9) Uani 1 1 d . . . C44 C 0.8636(7) 0.6410(5) 0.4254(4) 0.0419(14) Uani 1 1 d . . . F1 F 0.7906(3) 0.86088(19) 0.62321(16) 0.0211(6) Uani 1 1 d . . . F2 F 1.0265(3) 0.7668(2) 0.55594(19) 0.0325(7) Uani 1 1 d . . . F3 F 1.1702(3) 0.5845(2) 0.6403(2) 0.0329(7) Uani 1 1 d . . . F4 F 1.0690(3) 0.4987(2) 0.7928(2) 0.0303(7) Uani 1 1 d . . . F5 F 0.8346(3) 0.58916(18) 0.86164(17) 0.0225(6) Uani 1 1 d . . . F6 F 0.8882(2) 0.80816(18) 0.86752(16) 0.0179(5) Uani 1 1 d . . . F7 F 0.9280(3) 0.97214(19) 0.89165(17) 0.0221(6) Uani 1 1 d . . . F8 F 0.7614(3) 1.15424(19) 0.82121(19) 0.0273(6) Uani 1 1 d . . . F9 F 0.5514(3) 1.16398(18) 0.72872(17) 0.0223(6) Uani 1 1 d . . . F10 F 0.5010(2) 1.00418(18) 0.70730(16) 0.0181(6) Uani 1 1 d . . . F11 F 0.3289(3) 1.01463(19) 0.85050(17) 0.0237(6) Uani 1 1 d . . . F12 F 0.1625(3) 1.1662(2) 0.7590(2) 0.0326(7) Uani 1 1 d . . . F13 F -0.0155(3) 1.1441(2) 0.6541(2) 0.0395(8) Uani 1 1 d . . . F14 F -0.0172(3) 0.9582(2) 0.64536(19) 0.0322(7) Uani 1 1 d . . . F15 F 0.1495(3) 0.79987(19) 0.73822(17) 0.0224(6) Uani 1 1 d . . . F16 F 0.2051(3) 0.89982(18) 0.97661(16) 0.0198(6) Uani 1 1 d . . . F17 F 0.0111(3) 0.8532(2) 1.08511(17) 0.0247(6) Uani 1 1 d . . . F18 F -0.0529(3) 0.6848(2) 1.08472(18) 0.0257(6) Uani 1 1 d . . . F19 F 0.0822(3) 0.5642(2) 0.97030(19) 0.0292(7) Uani 1 1 d . . . F20 F 0.2700(3) 0.60782(19) 0.86065(19) 0.0276(7) Uani 1 1 d . . . F21 F 0.8886(4) 0.5440(3) 0.4542(3) 0.0531(10) Uani 1 1 d . . . F22 F 0.8554(5) 0.6555(3) 0.3386(2) 0.0734(14) Uani 1 1 d . . . F23 F 0.9664(4) 0.6680(3) 0.4428(3) 0.0715(13) Uani 1 1 d . . . N1 N 0.4049(4) 0.8109(3) 0.6185(2) 0.0166(9) Uani 1.027(8) 1 d P . . O1 O 0.4020(3) 0.7278(2) 0.78859(18) 0.0119(6) Uani 1 1 d . . . O2 O 0.5683(3) 0.8199(2) 0.71578(18) 0.0123(6) Uani 1 1 d . . . O3 O 0.4631(3) 0.7603(3) 0.9843(2) 0.0234(7) Uani 1 1 d . . . O4 O 0.6806(3) 0.7445(2) 0.93910(19) 0.0149(6) Uani 1 1 d . . . O5 O 0.7268(3) 0.6759(2) 0.5631(2) 0.0205(7) Uani 1 1 d . . . O6 O 0.7033(5) 0.8113(3) 0.4477(3) 0.0501(11) Uani 1 1 d . . . O7 O 0.6075(4) 0.6756(4) 0.4469(3) 0.0512(12) Uani 1 1 d . . . P1 P 0.49695(11) 0.74022(8) 0.69908(7) 0.0117(2) Uani 1 1 d . . . Rh1 Rh 0.62588(3) 0.59356(2) 0.66975(2) 0.01421(13) Uani 1 1 d . . . S1 S 0.70728(14) 0.71011(10) 0.47551(9) 0.0335(3) Uani 1 1 d . . . 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 C1 0.020(2) 0.015(2) 0.024(2) -0.0074(19) 0.0042(19) -0.0096(19) C2 0.022(2) 0.012(2) 0.020(2) -0.0016(18) 0.0030(19) -0.0050(19) C3 0.016(2) 0.019(2) 0.040(3) -0.011(2) 0.008(2) -0.004(2) C4 0.027(3) 0.016(2) 0.032(3) -0.014(2) 0.012(2) -0.006(2) C5 0.034(3) 0.024(3) 0.041(3) -0.020(2) 0.005(2) -0.013(2) C6 0.024(3) 0.019(3) 0.043(3) -0.003(2) -0.005(2) 0.001(2) C7 0.032(3) 0.018(3) 0.029(3) 0.003(2) -0.004(2) -0.001(2) C8 0.025(3) 0.027(3) 0.037(3) -0.016(2) 0.002(2) -0.013(2) C9 0.014(2) 0.013(2) 0.015(2) -0.0028(17) -0.0039(17) -0.0038(17) C10 0.015(2) 0.014(2) 0.015(2) -0.0041(17) 0.0014(17) -0.0068(18) C11 0.012(2) 0.010(2) 0.015(2) -0.0040(17) 0.0011(17) -0.0041(17) C12 0.013(2) 0.011(2) 0.015(2) -0.0021(17) -0.0040(17) -0.0030(17) C13 0.026(3) 0.015(2) 0.024(2) 0.0028(19) -0.008(2) -0.008(2) C14 0.025(3) 0.024(3) 0.023(2) -0.0075(19) -0.0059(19) -0.010(2) C15 0.154(8) 0.042(4) 0.055(4) 0.022(3) -0.077(5) -0.050(5) C16 0.143(8) 0.054(4) 0.050(4) 0.032(3) -0.071(5) -0.061(5) C17 0.010(2) 0.014(2) 0.022(2) -0.0075(18) -0.0043(17) -0.0041(17) C18 0.018(2) 0.014(2) 0.018(2) -0.0033(18) -0.0014(18) -0.0055(18) C19 0.014(2) 0.016(2) 0.032(3) -0.006(2) -0.006(2) -0.0016(19) C20 0.014(2) 0.026(3) 0.035(3) -0.016(2) 0.003(2) -0.007(2) C21 0.018(2) 0.031(3) 0.022(2) -0.008(2) 0.0050(19) -0.014(2) C22 0.015(2) 0.014(2) 0.023(2) -0.0027(18) -0.0036(18) -0.0039(18) C23 0.015(2) 0.043(3) 0.017(2) -0.007(2) 0.0000(19) -0.008(2) C24 0.023(3) 0.115(6) 0.065(4) -0.072(5) -0.002(3) -0.009(4) C25 0.027(3) 0.077(5) 0.041(4) 0.039(4) -0.008(3) -0.017(3) C26 0.011(2) 0.014(2) 0.014(2) -0.0037(17) 0.0015(16) -0.0059(17) C27 0.015(2) 0.012(2) 0.017(2) -0.0012(17) -0.0006(18) -0.0020(18) C28 0.017(2) 0.019(2) 0.017(2) -0.0066(18) -0.0013(18) -0.0061(19) C29 0.023(2) 0.012(2) 0.022(2) -0.0067(18) 0.0034(19) -0.0104(19) C30 0.020(2) 0.011(2) 0.014(2) 0.0000(17) 0.0031(18) -0.0025(18) C31 0.012(2) 0.015(2) 0.013(2) -0.0045(17) 0.0000(16) -0.0042(17) C32 0.015(2) 0.016(2) 0.019(2) -0.0034(18) 0.0009(18) -0.0044(18) C33 0.015(2) 0.031(3) 0.022(2) -0.005(2) -0.0023(19) -0.005(2) C34 0.019(2) 0.025(3) 0.024(3) 0.003(2) 0.001(2) 0.001(2) C35 0.030(3) 0.016(2) 0.024(2) -0.003(2) 0.005(2) -0.006(2) C36 0.019(2) 0.023(3) 0.019(2) -0.0065(19) 0.0019(19) -0.006(2) C37 0.012(2) 0.016(2) 0.014(2) -0.0041(17) 0.0021(17) -0.0022(18) C38 0.009(2) 0.018(2) 0.018(2) -0.0021(18) -0.0024(17) -0.0028(18) C39 0.016(2) 0.016(2) 0.016(2) -0.0035(18) 0.0016(18) -0.0028(18) C40 0.021(2) 0.018(2) 0.022(2) -0.0001(19) -0.0018(19) -0.013(2) C41 0.012(2) 0.023(2) 0.016(2) 0.0022(18) -0.0007(17) -0.0079(19) C42 0.015(2) 0.020(2) 0.015(2) -0.0044(18) -0.0021(18) -0.0011(19) C43 0.011(2) 0.017(2) 0.016(2) -0.0022(17) -0.0030(17) -0.0042(18) C44 0.049(4) 0.038(3) 0.042(3) -0.012(3) 0.012(3) -0.019(3) F1 0.0206(14) 0.0190(14) 0.0203(13) 0.0022(11) 0.0023(11) -0.0059(11) F2 0.0247(16) 0.0410(18) 0.0296(16) -0.0055(14) 0.0141(13) -0.0123(14) F3 0.0151(14) 0.0328(17) 0.0488(19) -0.0178(14) 0.0096(13) -0.0012(12) F4 0.0229(15) 0.0165(14) 0.0447(18) -0.0051(13) -0.0060(13) 0.0052(12) F5 0.0224(14) 0.0152(13) 0.0244(14) -0.0007(11) -0.0005(11) 0.0003(11) F6 0.0162(13) 0.0125(12) 0.0244(14) -0.0026(10) -0.0056(11) -0.0023(10) F7 0.0180(14) 0.0221(14) 0.0313(15) -0.0093(12) -0.0082(11) -0.0082(11) F8 0.0338(17) 0.0145(14) 0.0390(17) -0.0063(12) -0.0084(13) -0.0117(12) F9 0.0273(15) 0.0112(13) 0.0257(14) -0.0002(11) -0.0055(12) -0.0026(11) F10 0.0153(13) 0.0152(13) 0.0223(13) -0.0011(10) -0.0068(10) -0.0021(10) F11 0.0287(15) 0.0180(14) 0.0276(15) -0.0082(11) -0.0034(12) -0.0081(12) F12 0.0414(18) 0.0144(14) 0.0387(17) -0.0038(12) 0.0004(14) -0.0048(13) F13 0.0371(18) 0.0244(16) 0.0440(19) 0.0065(14) -0.0118(15) 0.0047(14) F14 0.0248(16) 0.0396(18) 0.0300(16) -0.0007(13) -0.0124(13) -0.0066(13) F15 0.0229(14) 0.0208(14) 0.0271(14) -0.0069(11) -0.0047(11) -0.0087(12) F16 0.0219(14) 0.0191(14) 0.0228(14) -0.0104(11) 0.0063(11) -0.0104(11) F17 0.0228(15) 0.0294(15) 0.0240(14) -0.0123(12) 0.0092(11) -0.0094(12) F18 0.0194(14) 0.0337(16) 0.0262(15) -0.0036(12) 0.0069(12) -0.0147(12) F19 0.0326(16) 0.0245(15) 0.0378(17) -0.0095(13) 0.0094(13) -0.0199(13) F20 0.0340(16) 0.0183(14) 0.0360(16) -0.0152(12) 0.0157(13) -0.0146(12) F21 0.057(2) 0.035(2) 0.062(2) -0.0138(17) 0.0197(19) -0.0107(17) F22 0.113(4) 0.061(3) 0.036(2) -0.0156(19) 0.030(2) -0.018(3) F23 0.048(2) 0.076(3) 0.110(4) -0.053(3) 0.035(2) -0.034(2) N1 0.019(2) 0.0150(19) 0.0176(19) -0.0025(15) -0.0036(15) -0.0070(16) O1 0.0127(15) 0.0122(14) 0.0123(14) -0.0050(11) 0.0014(11) -0.0047(12) O2 0.0129(15) 0.0128(15) 0.0126(14) -0.0023(12) -0.0017(12) -0.0056(12) O3 0.0149(16) 0.043(2) 0.0121(15) -0.0029(14) -0.0008(12) -0.0099(15) O4 0.0135(15) 0.0187(16) 0.0130(14) -0.0014(12) -0.0018(12) -0.0060(13) O5 0.0205(17) 0.0109(15) 0.0326(18) -0.0114(14) 0.0249(14) -0.0115(13) O6 0.070(3) 0.032(2) 0.040(2) -0.0033(19) 0.010(2) -0.009(2) O7 0.044(3) 0.073(3) 0.045(3) -0.026(2) -0.006(2) -0.018(2) P1 0.0125(5) 0.0107(5) 0.0129(5) -0.0030(4) 0.0002(4) -0.0045(4) Rh1 0.0147(2) 0.01125(19) 0.01691(19) -0.00488(13) 0.00147(13) -0.00330(14) S1 0.0355(8) 0.0337(8) 0.0319(7) -0.0108(6) 0.0021(6) -0.0091(6) _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 C1 C2 1.412(6) . ? C1 C8 1.516(6) . ? C1 Rh1 2.103(4) . ? C2 C7 1.526(6) . ? C2 Rh1 2.115(4) . ? C3 C4 1.354(7) . ? C3 C6 1.527(7) . ? C3 Rh1 2.244(5) . ? C4 C5 1.520(7) . ? C4 Rh1 2.285(4) . ? C5 C8 1.525(7) . ? C6 C7 1.523(7) . ? C9 O4 1.410(5) . ? C9 C12 1.531(6) . ? C9 C10 1.541(6) . ? C10 O3 1.431(5) . ? C10 C11 1.561(6) . ? C11 O1 1.445(5) . ? C11 C38 1.544(6) . ? C11 C37 1.563(6) . ? C12 O2 1.444(5) . ? C12 C26 1.539(6) . ? C12 C17 1.555(6) . ? C13 N1 1.492(6) . ? C13 C16 1.503(7) . ? C14 N1 1.488(5) . ? C14 C15 1.490(7) . ? C15 C16 1.350(9) . ? C17 C22 1.388(6) . ? C17 C18 1.398(6) . ? C18 F5 1.338(5) . ? C18 C19 1.385(7) . ? C19 F4 1.334(5) . ? C19 C20 1.370(7) . ? C20 F3 1.335(5) . ? C20 C21 1.384(7) . ? C21 F2 1.332(6) . ? C21 C22 1.370(7) . ? C22 F1 1.339(5) . ? C23 O4 1.429(6) . ? C23 O3 1.433(6) . ? C23 C24 1.483(7) . ? C23 C25 1.524(8) . ? C26 C31 1.397(6) . ? C26 C27 1.407(6) . ? C27 F6 1.345(5) . ? C27 C28 1.379(6) . ? C28 F7 1.335(5) . ? C28 C29 1.381(6) . ? C29 F8 1.334(5) . ? C29 C30 1.371(6) . ? C30 F9 1.334(5) . ? C30 C31 1.381(6) . ? C31 F10 1.335(5) . ? C32 F15 1.355(5) . ? C32 C33 1.365(6) . ? C32 C37 1.396(6) . ? C33 F14 1.345(5) . ? C33 C34 1.371(7) . ? C34 F13 1.339(5) . ? C34 C35 1.373(7) . ? C35 F12 1.326(5) . ? C35 C36 1.398(7) . ? C36 F11 1.348(5) . ? C36 C37 1.379(6) . ? C38 C39 1.391(6) . ? C38 C43 1.392(6) . ? C39 F20 1.348(5) . ? C39 C40 1.372(7) . ? C40 F19 1.333(5) . ? C40 C41 1.387(6) . ? C41 F18 1.339(5) . ? C41 C42 1.367(6) . ? C42 F17 1.328(5) . ? C42 C43 1.380(6) . ? C43 F16 1.337(5) . ? C44 F23 1.323(7) . ? C44 F21 1.326(7) . ? C44 F22 1.331(7) . ? C44 S1 1.827(6) . ? N1 P1 1.630(4) . ? O1 P1 1.639(3) . ? O2 P1 1.624(3) . ? O5 S1 1.365(4) . ? O5 Rh1 2.209(3) . ? O6 S1 1.420(4) . ? O7 S1 1.432(4) . ? P1 Rh1 2.2368(11) . ? 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 C2 C1 C8 126.6(4) . . ? C2 C1 Rh1 70.9(3) . . ? C8 C1 Rh1 109.9(3) . . ? C1 C2 C7 124.0(4) . . ? C1 C2 Rh1 70.0(3) . . ? C7 C2 Rh1 113.7(3) . . ? C4 C3 C6 126.1(5) . . ? C4 C3 Rh1 74.2(3) . . ? C6 C3 Rh1 107.2(3) . . ? C3 C4 C5 122.7(5) . . ? C3 C4 Rh1 71.0(3) . . ? C5 C4 Rh1 109.1(3) . . ? C4 C5 C8 112.3(4) . . ? C7 C6 C3 113.5(4) . . ? C6 C7 C2 114.4(4) . . ? C1 C8 C5 113.9(4) . . ? O4 C9 C12 110.9(3) . . ? O4 C9 C10 101.1(3) . . ? C12 C9 C10 114.9(3) . . ? O3 C10 C9 99.1(3) . . ? O3 C10 C11 110.2(3) . . ? C9 C10 C11 117.4(3) . . ? O1 C11 C38 107.9(3) . . ? O1 C11 C10 107.5(3) . . ? C38 C11 C10 111.2(3) . . ? O1 C11 C37 109.2(3) . . ? C38 C11 C37 104.8(3) . . ? C10 C11 C37 115.9(3) . . ? O2 C12 C9 106.5(3) . . ? O2 C12 C26 106.8(3) . . ? C9 C12 C26 111.9(3) . . ? O2 C12 C17 107.9(3) . . ? C9 C12 C17 115.5(3) . . ? C26 C12 C17 107.8(3) . . ? N1 C13 C16 102.1(4) . . ? N1 C14 C15 103.0(4) . . ? C16 C15 C14 111.5(5) . . ? C15 C16 C13 111.9(5) . . ? C22 C17 C18 116.0(4) . . ? C22 C17 C12 117.6(4) . . ? C18 C17 C12 126.4(4) . . ? F5 C18 C19 116.3(4) . . ? F5 C18 C17 122.2(4) . . ? C19 C18 C17 121.4(4) . . ? F4 C19 C20 120.0(4) . . ? F4 C19 C18 119.6(4) . . ? C20 C19 C18 120.5(4) . . ? F3 C20 C19 120.5(4) . . ? F3 C20 C21 119.9(4) . . ? C19 C20 C21 119.5(4) . . ? F2 C21 C22 120.4(4) . . ? F2 C21 C20 120.4(4) . . ? C22 C21 C20 119.2(4) . . ? F1 C22 C21 117.0(4) . . ? F1 C22 C17 119.6(4) . . ? C21 C22 C17 123.3(4) . . ? O4 C23 O3 105.2(3) . . ? O4 C23 C24 108.6(5) . . ? O3 C23 C24 111.7(4) . . ? O4 C23 C25 109.6(4) . . ? O3 C23 C25 107.8(4) . . ? C24 C23 C25 113.6(5) . . ? C31 C26 C27 114.7(4) . . ? C31 C26 C12 125.7(4) . . ? C27 C26 C12 119.5(4) . . ? F6 C27 C28 115.7(4) . . ? F6 C27 C26 120.9(4) . . ? C28 C27 C26 123.4(4) . . ? F7 C28 C27 119.8(4) . . ? F7 C28 C29 120.8(4) . . ? C27 C28 C29 119.4(4) . . ? F8 C29 C30 120.4(4) . . ? F8 C29 C28 120.4(4) . . ? C30 C29 C28 119.3(4) . . ? F9 C30 C29 119.8(4) . . ? F9 C30 C31 119.5(4) . . ? C29 C30 C31 120.7(4) . . ? F10 C31 C30 115.2(4) . . ? F10 C31 C26 122.4(4) . . ? C30 C31 C26 122.4(4) . . ? F15 C32 C33 116.2(4) . . ? F15 C32 C37 119.8(4) . . ? C33 C32 C37 123.9(4) . . ? F14 C33 C32 120.8(4) . . ? F14 C33 C34 119.3(4) . . ? C32 C33 C34 119.9(4) . . ? F13 C34 C33 120.7(5) . . ? F13 C34 C35 120.3(5) . . ? C33 C34 C35 119.0(4) . . ? F12 C35 C34 121.2(4) . . ? F12 C35 C36 119.0(4) . . ? C34 C35 C36 119.8(4) . . ? F11 C36 C37 123.2(4) . . ? F11 C36 C35 114.0(4) . . ? C37 C36 C35 122.8(4) . . ? C36 C37 C32 114.5(4) . . ? C36 C37 C11 127.9(4) . . ? C32 C37 C11 117.3(4) . . ? C39 C38 C43 115.0(4) . . ? C39 C38 C11 126.8(4) . . ? C43 C38 C11 118.0(4) . . ? F20 C39 C40 114.9(4) . . ? F20 C39 C38 122.4(4) . . ? C40 C39 C38 122.7(4) . . ? F19 C40 C39 120.1(4) . . ? F19 C40 C41 119.6(4) . . ? C39 C40 C41 120.2(4) . . ? F18 C41 C42 120.3(4) . . ? F18 C41 C40 120.6(4) . . ? C42 C41 C40 119.1(4) . . ? F17 C42 C41 120.1(4) . . ? F17 C42 C43 120.2(4) . . ? C41 C42 C43 119.6(4) . . ? F16 C43 C42 117.5(4) . . ? F16 C43 C38 119.2(4) . . ? C42 C43 C38 123.4(4) . . ? F23 C44 F21 108.5(6) . . ? F23 C44 F22 108.9(5) . . ? F21 C44 F22 106.4(5) . . ? F23 C44 S1 111.2(4) . . ? F21 C44 S1 111.0(4) . . ? F22 C44 S1 110.7(5) . . ? C14 N1 C13 111.3(3) . . ? C14 N1 P1 118.9(3) . . ? C13 N1 P1 128.0(3) . . ? C11 O1 P1 128.2(3) . . ? C12 O2 P1 122.9(2) . . ? C10 O3 C23 107.8(3) . . ? C9 O4 C23 108.1(3) . . ? S1 O5 Rh1 134.1(2) . . ? O2 P1 N1 97.74(16) . . ? O2 P1 O1 102.56(15) . . ? N1 P1 O1 109.64(17) . . ? O2 P1 Rh1 118.95(12) . . ? N1 P1 Rh1 114.36(13) . . ? O1 P1 Rh1 112.16(11) . . ? C1 Rh1 C2 39.11(17) . . ? C1 Rh1 O5 154.67(16) . . ? C2 Rh1 O5 165.47(16) . . ? C1 Rh1 P1 93.10(12) . . ? C2 Rh1 P1 96.83(12) . . ? O5 Rh1 P1 87.97(8) . . ? C1 Rh1 C3 96.42(18) . . ? C2 Rh1 C3 81.59(18) . . ? O5 Rh1 C3 89.69(15) . . ? P1 Rh1 C3 162.41(13) . . ? C1 Rh1 C4 81.30(17) . . ? C2 Rh1 C4 89.23(17) . . ? O5 Rh1 C4 90.18(15) . . ? P1 Rh1 C4 162.56(14) . . ? C3 Rh1 C4 34.78(18) . . ? O5 S1 O6 113.6(2) . . ? O5 S1 O7 111.1(2) . . ? O6 S1 O7 119.2(3) . . ? O5 S1 C44 102.5(3) . . ? O6 S1 C44 104.4(3) . . ? O7 S1 C44 103.8(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.043 _refine_diff_density_min -1.230 _refine_diff_density_rms 0.257 data_rovis117_0m _database_code_depnum_ccdc_archive 'CCDC 901684' #TrackingRef '- Rovis117_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H33 F20 N O7 P Rh S' _chemical_formula_weight 1305.71 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7155(4) _cell_length_b 12.1131(4) _cell_length_c 18.2303(6) _cell_angle_alpha 70.901(2) _cell_angle_beta 89.025(2) _cell_angle_gamma 83.198(2) _cell_volume 2426.82(14) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 9977 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.35 _exptl_crystal_description Plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not determined' _exptl_crystal_density_diffrn 1.787 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.561 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8538 _exptl_absorpt_correction_T_max 0.9597 _exptl_absorpt_process_details 'Sheldrick, G. M. (2008) SADABS. University of Gottingen, Germany.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36213 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 26.52 _reflns_number_total 9971 _reflns_number_gt 7073 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'APEX2 (Bruker, 2009)' _computing_data_reduction 'APEX2 (Bruker, 2009)' _computing_structure_solution 'XS (Sheldrick, 2008)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_molecular_graphics 'APEX2 (Bruker, 2009)' _computing_publication_material 'APEX2 (Bruker, 2009)' _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^)+(0.0771P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9971 _refine_ls_number_parameters 733 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1451 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 C1 C 0.9955(4) 0.8455(4) 0.5518(3) 0.0315(11) Uani 1 1 d . . . H1 H 0.9925 0.9226 0.5587 0.038 Uiso 1 1 calc R . . C2 C 0.9206(4) 0.8425(4) 0.4954(3) 0.0326(11) Uani 1 1 d . . . H2 H 0.8736 0.9173 0.4690 0.039 Uiso 1 1 calc R . . C3 C 0.9865(4) 0.6004(4) 0.6177(2) 0.0288(10) Uani 1 1 d . . . H3 H 0.9905 0.5355 0.6671 0.035 Uiso 1 1 calc R . . C4 C 0.8957(4) 0.6007(4) 0.5686(3) 0.0333(11) Uani 1 1 d . . . H4 H 0.8493 0.5357 0.5898 0.040 Uiso 1 1 calc R . . C5 C 0.8938(4) 0.6495(4) 0.4805(3) 0.0413(12) Uani 1 1 d . . . H5A H 0.8147 0.6629 0.4619 0.050 Uiso 1 1 calc R . . H5B H 0.9344 0.5908 0.4609 0.050 Uiso 1 1 calc R . . C6 C 0.9476(5) 0.7642(5) 0.4471(3) 0.0420(13) Uani 1 1 d . . . H6A H 1.0303 0.7465 0.4452 0.050 Uiso 1 1 calc R . . H6B H 0.9185 0.8048 0.3945 0.050 Uiso 1 1 calc R . . C7 C 1.1032(4) 0.6404(4) 0.5907(3) 0.0397(12) Uani 1 1 d . . . H7A H 1.1610 0.5957 0.6301 0.048 Uiso 1 1 calc R . . H7B H 1.1222 0.6222 0.5436 0.048 Uiso 1 1 calc R . . C8 C 1.1091(4) 0.7704(4) 0.5751(3) 0.0358(11) Uani 1 1 d . . . H8A H 1.1383 0.7810 0.6216 0.043 Uiso 1 1 calc R . . H8B H 1.1634 0.7973 0.5342 0.043 Uiso 1 1 calc R . . C9 C 0.7958(3) 0.6393(3) 0.8449(2) 0.0183(8) Uani 1 1 d . . . C10 C 0.8051(3) 0.5016(3) 0.8765(2) 0.0186(8) Uani 1 1 d . . . H10 H 0.8676 0.4685 0.8507 0.022 Uiso 1 1 calc R . . C11 C 0.6914(3) 0.4585(3) 0.8627(2) 0.0192(9) Uani 1 1 d . . . H11 H 0.6269 0.5207 0.8559 0.023 Uiso 1 1 calc R . . C12 C 0.7028(3) 0.4175(3) 0.7902(2) 0.0204(9) Uani 1 1 d . . . C13 C 0.7459(4) 0.3732(3) 0.9927(2) 0.0242(9) Uani 1 1 d . . . C14 C 0.6685(4) 0.4193(4) 1.0454(3) 0.0371(12) Uani 1 1 d . . . H14A H 0.6204 0.4885 1.0151 0.056 Uiso 1 1 calc R . . H14B H 0.7144 0.4387 1.0816 0.056 Uiso 1 1 calc R . . H14C H 0.6214 0.3603 1.0733 0.056 Uiso 1 1 calc R . . C15 C 0.8130(4) 0.2543(3) 1.0323(3) 0.0334(11) Uani 1 1 d . . . H15A H 0.7607 0.1970 1.0527 0.050 Uiso 1 1 calc R . . H15B H 0.8595 0.2586 1.0739 0.050 Uiso 1 1 calc R . . H15C H 0.8616 0.2318 0.9954 0.050 Uiso 1 1 calc R . . C16 C 0.5996(4) 1.0401(3) 0.6383(2) 0.0272(10) Uani 1 1 d . . . C17 C 0.6073(4) 1.0656(4) 0.7070(3) 0.0360(11) Uani 1 1 d . . . H17 H 0.6785 1.0721 0.7259 0.043 Uiso 1 1 calc R . . C18 C 0.5093(4) 1.0811(4) 0.7467(3) 0.0409(12) Uani 1 1 d . . . H18 H 0.5154 1.0947 0.7937 0.049 Uiso 1 1 calc R . . C19 C 0.4013(4) 1.0768(4) 0.7181(3) 0.0364(11) Uani 1 1 d . . . C20 C 0.3948(4) 1.0554(4) 0.6485(3) 0.0391(12) Uani 1 1 d . . . H20 H 0.3231 1.0541 0.6279 0.047 Uiso 1 1 calc R . . C21 C 0.4916(4) 1.0360(4) 0.6090(3) 0.0330(11) Uani 1 1 d . . . H21 H 0.4852 1.0201 0.5628 0.040 Uiso 1 1 calc R . . C22 C 0.2962(5) 1.0933(5) 0.7623(3) 0.0536(15) Uani 1 1 d . . . H22A H 0.2293 1.1066 0.7295 0.080 Uiso 1 1 calc R . . H22B H 0.2994 1.1599 0.7794 0.080 Uiso 1 1 calc R . . H22C H 0.2922 1.0241 0.8066 0.080 Uiso 1 1 calc R . . C23 C 0.9072(3) 0.6931(3) 0.8169(2) 0.0209(9) Uani 1 1 d . . . C24 C 0.9007(4) 0.8167(3) 0.7898(2) 0.0228(9) Uani 1 1 d . . . C25 C 0.9936(4) 0.8761(3) 0.7603(2) 0.0269(10) Uani 1 1 d . . . C26 C 1.0979(4) 0.8147(4) 0.7568(2) 0.0282(10) Uani 1 1 d . . . C27 C 1.1093(4) 0.6940(4) 0.7832(2) 0.0274(10) Uani 1 1 d . . . C28 C 1.0152(4) 0.6352(3) 0.8133(2) 0.0244(9) Uani 1 1 d . . . C29 C 0.7445(3) 0.6876(3) 0.9080(2) 0.0192(9) Uani 1 1 d . . . C30 C 0.6311(3) 0.7337(3) 0.9111(2) 0.0219(9) Uani 1 1 d . . . C31 C 0.5911(4) 0.7751(4) 0.9702(2) 0.0260(10) Uani 1 1 d . . . C32 C 0.6646(4) 0.7711(3) 1.0290(2) 0.0277(10) Uani 1 1 d . . . C33 C 0.7771(4) 0.7260(4) 1.0286(2) 0.0266(10) Uani 1 1 d . . . C34 C 0.8153(4) 0.6855(3) 0.9689(2) 0.0226(9) Uani 1 1 d . . . C35 C 0.7766(4) 0.2964(3) 0.8133(2) 0.0226(9) Uani 1 1 d . . . C36 C 0.8931(4) 0.2760(3) 0.8022(2) 0.0260(10) Uani 1 1 d . . . C37 C 0.9546(4) 0.1659(4) 0.8316(3) 0.0314(10) Uani 1 1 d . . . C38 C 0.9008(4) 0.0709(4) 0.8741(3) 0.0361(11) Uani 1 1 d . . . C39 C 0.7858(4) 0.0868(4) 0.8856(3) 0.0328(11) Uani 1 1 d . . . C40 C 0.7252(4) 0.1968(4) 0.8559(2) 0.0277(10) Uani 1 1 d . . . C41 C 0.5900(4) 0.4088(3) 0.7514(2) 0.0212(9) Uani 1 1 d . . . C42 C 0.5962(4) 0.3875(4) 0.6803(3) 0.0282(10) Uani 1 1 d . . . C43 C 0.5001(4) 0.3757(4) 0.6423(3) 0.0351(11) Uani 1 1 d . . . C44 C 0.3952(4) 0.3829(4) 0.6736(3) 0.0352(12) Uani 1 1 d . . . C45 C 0.3852(4) 0.4014(4) 0.7441(3) 0.0300(10) Uani 1 1 d . . . C46 C 0.4809(4) 0.4143(3) 0.7818(2) 0.0239(9) Uani 1 1 d . . . C47 C 0.5788(4) 0.7086(4) 0.5831(2) 0.0353(11) Uani 1 1 d . . . H47A H 0.6219 0.6524 0.5624 0.042 Uiso 1 1 calc R . . H47B H 0.5979 0.7869 0.5548 0.042 Uiso 1 1 calc R . . C48 C 0.4530(4) 0.7033(5) 0.5785(3) 0.0405(12) Uani 1 1 d . . . H48A H 0.4207 0.7554 0.5289 0.049 Uiso 1 1 calc R . . H48B H 0.4376 0.6238 0.5848 0.049 Uiso 1 1 calc R . . C49 C 0.4034(4) 0.7417(4) 0.6430(3) 0.0332(11) Uani 1 1 d . . . H49A H 0.3392 0.6988 0.6648 0.040 Uiso 1 1 calc R . . H49B H 0.3762 0.8251 0.6243 0.040 Uiso 1 1 calc R . . C50 C 0.4991(3) 0.7160(4) 0.7043(2) 0.0229(9) Uani 1 1 d . . . H50A H 0.5090 0.7859 0.7172 0.027 Uiso 1 1 calc R . . H50B H 0.4825 0.6541 0.7512 0.027 Uiso 1 1 calc R . . F1 F 0.55167(19) 0.7395(2) 0.85729(13) 0.0296(6) Uani 1 1 d . . . F2 F 0.4813(2) 0.8215(2) 0.96872(14) 0.0353(6) Uani 1 1 d . . . F3 F 0.6264(2) 0.8131(2) 1.08562(14) 0.0370(6) Uani 1 1 d . . . F4 F 0.8511(2) 0.7237(2) 1.08429(14) 0.0375(6) Uani 1 1 d . . . F5 F 0.9269(2) 0.6428(2) 0.97191(13) 0.0283(6) Uani 1 1 d . . . F6 F 0.8016(2) 0.88108(19) 0.79386(14) 0.0292(6) Uani 1 1 d . . . F7 F 0.9812(2) 0.9940(2) 0.73585(15) 0.0381(7) Uani 1 1 d . . . F8 F 1.1884(2) 0.8716(2) 0.72893(16) 0.0422(7) Uani 1 1 d . . . F9 F 1.2113(2) 0.6333(2) 0.78064(15) 0.0380(6) Uani 1 1 d . . . F10 F 1.0377(2) 0.5175(2) 0.84060(15) 0.0331(6) Uani 1 1 d . . . F11 F 0.6991(2) 0.3755(2) 0.64799(14) 0.0355(6) Uani 1 1 d . . . F12 F 0.5119(3) 0.3567(3) 0.57374(16) 0.0523(8) Uani 1 1 d . . . F13 F 0.3018(3) 0.3714(3) 0.63746(18) 0.0550(9) Uani 1 1 d . . . F14 F 0.2821(2) 0.4058(2) 0.77677(17) 0.0402(7) Uani 1 1 d . . . F15 F 0.4644(2) 0.4294(2) 0.85093(13) 0.0284(6) Uani 1 1 d . . . F16 F 0.6125(2) 0.20428(19) 0.87116(14) 0.0307(6) Uani 1 1 d . . . F17 F 0.7315(3) -0.0046(2) 0.92648(17) 0.0464(7) Uani 1 1 d . . . F18 F 0.9611(3) -0.0360(2) 0.90336(17) 0.0488(8) Uani 1 1 d . . . F19 F 1.0677(2) 0.1518(2) 0.81812(17) 0.0442(7) Uani 1 1 d . . . F20 F 0.9548(2) 0.3624(2) 0.76209(15) 0.0344(6) Uani 1 1 d . . . N1 N 0.6022(3) 0.6783(3) 0.66699(18) 0.0223(8) Uani 1 1 d . . . O1 O 0.7647(3) 0.8838(2) 0.63615(17) 0.0351(8) Uani 1 1 d . . . O2 O 0.6922(3) 1.0208(3) 0.51267(18) 0.0407(8) Uani 1 1 d . . . O3 O 0.8068(3) 1.0843(3) 0.5986(2) 0.0444(9) Uani 1 1 d . . . O4 O 0.7644(2) 0.5019(2) 0.73342(15) 0.0201(6) Uani 1 1 d . . . O5 O 0.7160(2) 0.6791(2) 0.77904(14) 0.0180(6) Uani 1 1 d . . . O6 O 0.6794(2) 0.3630(2) 0.93053(15) 0.0228(6) Uani 1 1 d . . . O7 O 0.8242(2) 0.4566(2) 0.95762(15) 0.0246(7) Uani 1 1 d . . . P1 P 0.73465(9) 0.64463(9) 0.70042(6) 0.0189(2) Uani 1 1 d . . . Rh1 Rh 0.85771(3) 0.73928(3) 0.613542(18) 0.02159(11) Uani 1 1 d . . . S1 S 0.72537(10) 1.00848(9) 0.59056(6) 0.0288(3) Uani 1 1 d . . . 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 C1 0.028(2) 0.024(2) 0.036(3) 0.0003(19) 0.013(2) -0.0086(19) C2 0.034(3) 0.027(2) 0.027(2) 0.0035(19) 0.009(2) -0.001(2) C3 0.031(3) 0.025(2) 0.026(2) -0.0042(19) 0.006(2) 0.0028(19) C4 0.031(3) 0.034(3) 0.043(3) -0.023(2) 0.012(2) -0.010(2) C5 0.041(3) 0.055(3) 0.039(3) -0.030(3) 0.001(2) -0.007(3) C6 0.045(3) 0.057(3) 0.021(2) -0.009(2) 0.007(2) -0.007(3) C7 0.024(3) 0.045(3) 0.045(3) -0.009(2) 0.005(2) -0.001(2) C8 0.025(2) 0.048(3) 0.035(3) -0.013(2) 0.004(2) -0.010(2) C9 0.017(2) 0.0164(19) 0.021(2) -0.0054(16) -0.0023(16) -0.0028(16) C10 0.020(2) 0.0151(18) 0.022(2) -0.0073(16) -0.0022(17) -0.0023(16) C11 0.022(2) 0.0141(18) 0.021(2) -0.0034(16) -0.0018(17) -0.0049(16) C12 0.021(2) 0.0180(19) 0.021(2) -0.0045(17) 0.0003(17) -0.0063(17) C13 0.031(2) 0.021(2) 0.020(2) -0.0042(17) -0.0019(18) -0.0090(18) C14 0.039(3) 0.045(3) 0.035(3) -0.021(2) 0.008(2) -0.013(2) C15 0.045(3) 0.019(2) 0.030(3) 0.0008(19) -0.010(2) -0.007(2) C16 0.033(3) 0.018(2) 0.030(2) -0.0066(18) 0.004(2) -0.0029(18) C17 0.030(3) 0.030(2) 0.053(3) -0.021(2) -0.001(2) -0.004(2) C18 0.046(3) 0.037(3) 0.050(3) -0.030(2) 0.004(3) -0.002(2) C19 0.035(3) 0.034(3) 0.050(3) -0.026(2) 0.008(2) -0.010(2) C20 0.032(3) 0.043(3) 0.051(3) -0.023(2) -0.002(2) -0.010(2) C21 0.036(3) 0.032(2) 0.034(3) -0.015(2) 0.003(2) -0.007(2) C22 0.040(3) 0.063(4) 0.074(4) -0.043(3) 0.016(3) -0.014(3) C23 0.021(2) 0.023(2) 0.020(2) -0.0074(17) -0.0006(17) -0.0060(17) C24 0.026(2) 0.019(2) 0.025(2) -0.0081(17) 0.0018(18) -0.0045(18) C25 0.035(3) 0.021(2) 0.026(2) -0.0064(18) 0.001(2) -0.0104(19) C26 0.031(3) 0.033(2) 0.027(2) -0.015(2) 0.005(2) -0.016(2) C27 0.024(2) 0.037(3) 0.026(2) -0.016(2) 0.0015(19) -0.007(2) C28 0.027(2) 0.019(2) 0.028(2) -0.0072(18) -0.0028(19) -0.0055(18) C29 0.024(2) 0.0123(18) 0.022(2) -0.0060(16) 0.0038(17) -0.0039(16) C30 0.023(2) 0.021(2) 0.021(2) -0.0048(17) -0.0001(17) -0.0046(17) C31 0.028(2) 0.024(2) 0.026(2) -0.0081(18) 0.0080(19) -0.0059(19) C32 0.041(3) 0.019(2) 0.028(2) -0.0125(18) 0.008(2) -0.009(2) C33 0.036(3) 0.026(2) 0.020(2) -0.0086(18) -0.0046(19) -0.009(2) C34 0.023(2) 0.0167(19) 0.028(2) -0.0065(17) 0.0011(18) -0.0020(17) C35 0.026(2) 0.019(2) 0.024(2) -0.0094(17) -0.0046(18) 0.0000(17) C36 0.033(3) 0.017(2) 0.030(2) -0.0095(18) 0.001(2) -0.0069(18) C37 0.030(3) 0.026(2) 0.041(3) -0.018(2) 0.000(2) 0.0036(19) C38 0.049(3) 0.019(2) 0.039(3) -0.009(2) -0.007(2) 0.004(2) C39 0.047(3) 0.017(2) 0.034(3) -0.0057(19) -0.001(2) -0.009(2) C40 0.031(3) 0.024(2) 0.030(2) -0.0126(19) -0.002(2) -0.0029(19) C41 0.027(2) 0.0123(18) 0.024(2) -0.0041(16) -0.0041(18) -0.0049(17) C42 0.034(3) 0.024(2) 0.030(2) -0.0120(19) -0.001(2) -0.0037(19) C43 0.052(3) 0.032(2) 0.029(3) -0.019(2) -0.011(2) -0.005(2) C44 0.038(3) 0.029(2) 0.041(3) -0.014(2) -0.018(2) -0.001(2) C45 0.028(3) 0.019(2) 0.041(3) -0.006(2) -0.005(2) -0.0023(19) C46 0.027(2) 0.0149(19) 0.030(2) -0.0075(17) -0.0032(19) -0.0033(17) C47 0.031(3) 0.049(3) 0.024(2) -0.010(2) -0.002(2) -0.001(2) C48 0.031(3) 0.052(3) 0.036(3) -0.014(2) -0.007(2) 0.003(2) C49 0.025(2) 0.044(3) 0.028(2) -0.009(2) -0.002(2) -0.002(2) C50 0.016(2) 0.025(2) 0.023(2) -0.0022(17) -0.0001(17) 0.0016(17) F1 0.0206(13) 0.0438(15) 0.0278(13) -0.0174(12) -0.0009(11) -0.0008(11) F2 0.0311(15) 0.0412(15) 0.0368(15) -0.0194(13) 0.0085(12) 0.0016(12) F3 0.0477(17) 0.0398(15) 0.0329(15) -0.0251(12) 0.0067(13) -0.0054(13) F4 0.0450(17) 0.0428(15) 0.0309(14) -0.0189(12) -0.0065(12) -0.0094(13) F5 0.0263(14) 0.0320(13) 0.0285(13) -0.0117(11) -0.0048(11) -0.0048(11) F6 0.0313(14) 0.0183(12) 0.0369(14) -0.0081(11) 0.0050(11) -0.0022(11) F7 0.0506(17) 0.0219(13) 0.0439(16) -0.0094(12) 0.0068(13) -0.0173(12) F8 0.0372(16) 0.0463(16) 0.0523(17) -0.0220(14) 0.0172(13) -0.0267(13) F9 0.0209(14) 0.0438(16) 0.0493(17) -0.0167(13) 0.0050(12) -0.0001(12) F10 0.0233(13) 0.0220(12) 0.0503(16) -0.0080(12) 0.0018(12) 0.0007(10) F11 0.0461(17) 0.0385(15) 0.0286(14) -0.0192(12) 0.0063(12) -0.0081(13) F12 0.072(2) 0.0568(18) 0.0376(17) -0.0281(15) -0.0150(15) -0.0079(16) F13 0.0475(19) 0.0570(18) 0.069(2) -0.0304(16) -0.0301(16) -0.0053(15) F14 0.0240(14) 0.0381(15) 0.0628(19) -0.0213(14) -0.0053(13) -0.0055(12) F15 0.0264(13) 0.0353(13) 0.0286(14) -0.0152(11) 0.0034(11) -0.0104(11) F16 0.0297(14) 0.0234(12) 0.0389(15) -0.0085(11) 0.0030(11) -0.0087(11) F17 0.0567(19) 0.0188(13) 0.0581(19) -0.0037(13) 0.0061(15) -0.0085(13) F18 0.0564(19) 0.0189(13) 0.063(2) -0.0086(13) -0.0052(16) 0.0146(13) F19 0.0329(16) 0.0367(15) 0.064(2) -0.0217(14) 0.0012(14) 0.0069(13) F20 0.0293(14) 0.0247(13) 0.0471(16) -0.0099(12) 0.0075(12) -0.0014(11) N1 0.0208(18) 0.0259(18) 0.0188(18) -0.0058(15) 0.0002(14) -0.0014(15) O1 0.046(2) 0.0205(15) 0.0301(17) -0.0004(13) 0.0084(15) 0.0071(14) O2 0.047(2) 0.0383(19) 0.0298(18) -0.0044(15) -0.0006(16) 0.0042(16) O3 0.042(2) 0.0406(19) 0.054(2) -0.0158(17) 0.0084(17) -0.0184(17) O4 0.0224(15) 0.0162(13) 0.0217(15) -0.0055(11) 0.0031(12) -0.0044(11) O5 0.0181(14) 0.0161(13) 0.0179(14) -0.0038(11) -0.0030(11) 0.0012(11) O6 0.0279(16) 0.0208(14) 0.0193(15) -0.0040(12) -0.0022(12) -0.0085(12) O7 0.0316(17) 0.0195(14) 0.0217(15) -0.0024(12) -0.0056(13) -0.0104(13) P1 0.0190(5) 0.0179(5) 0.0187(5) -0.0045(4) 0.0011(4) -0.0022(4) Rh1 0.02064(19) 0.02029(18) 0.02196(19) -0.00432(13) 0.00238(13) -0.00281(13) S1 0.0309(6) 0.0204(5) 0.0295(6) -0.0012(5) 0.0029(5) -0.0009(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 C1 C2 1.376(6) . ? C1 C8 1.503(6) . ? C1 Rh1 2.239(4) . ? C2 C6 1.496(6) . ? C2 Rh1 2.269(4) . ? C3 C4 1.401(6) . ? C3 C7 1.525(6) . ? C3 Rh1 2.105(4) . ? C4 C5 1.517(6) . ? C4 Rh1 2.098(4) . ? C5 C6 1.529(7) . ? C7 C8 1.515(7) . ? C9 O5 1.449(4) . ? C9 C23 1.534(5) . ? C9 C29 1.535(5) . ? C9 C10 1.567(5) . ? C10 O7 1.410(4) . ? C10 C11 1.541(5) . ? C11 O6 1.409(4) . ? C11 C12 1.556(5) . ? C12 O4 1.447(4) . ? C12 C41 1.540(5) . ? C12 C35 1.545(5) . ? C13 O7 1.431(5) . ? C13 O6 1.433(5) . ? C13 C14 1.503(6) . ? C13 C15 1.512(6) . ? C16 C17 1.390(6) . ? C16 C21 1.394(6) . ? C16 S1 1.765(4) . ? C17 C18 1.374(7) . ? C18 C19 1.390(7) . ? C19 C20 1.381(7) . ? C19 C22 1.490(7) . ? C20 C21 1.370(7) . ? C23 C28 1.384(6) . ? C23 C24 1.407(5) . ? C24 F6 1.335(5) . ? C24 C25 1.380(6) . ? C25 F7 1.340(5) . ? C25 C26 1.365(6) . ? C26 F8 1.335(5) . ? C26 C27 1.372(6) . ? C27 F9 1.335(5) . ? C27 C28 1.391(6) . ? C28 F10 1.342(4) . ? C29 C30 1.387(6) . ? C29 C34 1.390(6) . ? C30 F1 1.342(4) . ? C30 C31 1.383(6) . ? C31 F2 1.338(5) . ? C31 C32 1.372(6) . ? C32 F3 1.341(5) . ? C32 C33 1.367(6) . ? C33 F4 1.338(5) . ? C33 C34 1.379(6) . ? C34 F5 1.343(5) . ? C35 C36 1.380(6) . ? C35 C40 1.402(6) . ? C36 F20 1.346(4) . ? C36 C37 1.380(6) . ? C37 F19 1.345(5) . ? C37 C38 1.376(6) . ? C38 F18 1.344(5) . ? C38 C39 1.360(7) . ? C39 F17 1.340(5) . ? C39 C40 1.375(6) . ? C40 F16 1.343(5) . ? C41 C46 1.387(6) . ? C41 C42 1.401(6) . ? C42 F11 1.347(5) . ? C42 C43 1.377(6) . ? C43 F12 1.345(5) . ? C43 C44 1.351(7) . ? C44 F13 1.332(5) . ? C44 C45 1.376(6) . ? C45 F14 1.340(5) . ? C45 C46 1.376(6) . ? C46 F15 1.339(5) . ? C47 N1 1.474(5) . ? C47 C48 1.487(6) . ? C48 C49 1.485(6) . ? C49 C50 1.529(6) . ? C50 N1 1.475(5) . ? N1 P1 1.632(3) . ? O1 S1 1.487(3) . ? O1 Rh1 2.104(3) . ? O2 S1 1.434(3) . ? O3 S1 1.441(3) . ? O4 P1 1.629(3) . ? O5 P1 1.624(3) . ? P1 Rh1 2.2421(10) . ? 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 C2 C1 C8 125.9(4) . . ? C2 C1 Rh1 73.4(2) . . ? C8 C1 Rh1 107.8(3) . . ? C1 C2 C6 122.1(4) . . ? C1 C2 Rh1 71.0(2) . . ? C6 C2 Rh1 110.6(3) . . ? C4 C3 C7 125.0(4) . . ? C4 C3 Rh1 70.3(3) . . ? C7 C3 Rh1 113.8(3) . . ? C3 C4 C5 125.8(4) . . ? C3 C4 Rh1 70.8(2) . . ? C5 C4 Rh1 109.5(3) . . ? C4 C5 C6 114.5(4) . . ? C2 C6 C5 111.1(4) . . ? C8 C7 C3 114.3(4) . . ? C1 C8 C7 113.9(4) . . ? O5 C9 C23 106.8(3) . . ? O5 C9 C29 108.1(3) . . ? C23 C9 C29 109.1(3) . . ? O5 C9 C10 107.2(3) . . ? C23 C9 C10 116.5(3) . . ? C29 C9 C10 108.8(3) . . ? O7 C10 C11 104.9(3) . . ? O7 C10 C9 112.0(3) . . ? C11 C10 C9 110.9(3) . . ? O6 C11 C10 104.0(3) . . ? O6 C11 C12 110.9(3) . . ? C10 C11 C12 109.0(3) . . ? O4 C12 C41 107.9(3) . . ? O4 C12 C35 108.4(3) . . ? C41 C12 C35 108.7(3) . . ? O4 C12 C11 106.4(3) . . ? C41 C12 C11 116.6(3) . . ? C35 C12 C11 108.4(3) . . ? O7 C13 O6 106.4(3) . . ? O7 C13 C14 109.1(3) . . ? O6 C13 C14 109.9(4) . . ? O7 C13 C15 109.3(4) . . ? O6 C13 C15 107.4(3) . . ? C14 C13 C15 114.4(4) . . ? C17 C16 C21 119.3(4) . . ? C17 C16 S1 120.3(3) . . ? C21 C16 S1 120.4(3) . . ? C18 C17 C16 119.7(4) . . ? C17 C18 C19 121.4(5) . . ? C20 C19 C18 118.1(5) . . ? C20 C19 C22 121.4(4) . . ? C18 C19 C22 120.5(5) . . ? C21 C20 C19 121.6(4) . . ? C20 C21 C16 119.9(4) . . ? C28 C23 C24 114.7(4) . . ? C28 C23 C9 128.0(3) . . ? C24 C23 C9 117.2(4) . . ? F6 C24 C25 117.4(3) . . ? F6 C24 C23 119.5(3) . . ? C25 C24 C23 123.0(4) . . ? F7 C25 C26 120.3(4) . . ? F7 C25 C24 119.8(4) . . ? C26 C25 C24 120.0(4) . . ? F8 C26 C25 120.3(4) . . ? F8 C26 C27 120.3(4) . . ? C25 C26 C27 119.4(4) . . ? F9 C27 C26 119.8(4) . . ? F9 C27 C28 120.1(4) . . ? C26 C27 C28 120.1(4) . . ? F10 C28 C23 122.3(3) . . ? F10 C28 C27 114.8(4) . . ? C23 C28 C27 122.8(4) . . ? C30 C29 C34 115.1(4) . . ? C30 C29 C9 126.0(3) . . ? C34 C29 C9 118.9(4) . . ? F1 C30 C31 115.2(4) . . ? F1 C30 C29 122.2(4) . . ? C31 C30 C29 122.6(4) . . ? F2 C31 C32 120.2(4) . . ? F2 C31 C30 119.8(4) . . ? C32 C31 C30 120.0(4) . . ? F3 C32 C33 120.5(4) . . ? F3 C32 C31 120.0(4) . . ? C33 C32 C31 119.4(4) . . ? F4 C33 C32 120.5(4) . . ? F4 C33 C34 119.8(4) . . ? C32 C33 C34 119.7(4) . . ? F5 C34 C33 116.5(4) . . ? F5 C34 C29 120.2(4) . . ? C33 C34 C29 123.2(4) . . ? C36 C35 C40 115.1(4) . . ? C36 C35 C12 126.4(4) . . ? C40 C35 C12 118.3(4) . . ? F20 C36 C37 115.2(4) . . ? F20 C36 C35 122.3(4) . . ? C37 C36 C35 122.5(4) . . ? F19 C37 C38 120.1(4) . . ? F19 C37 C36 119.5(4) . . ? C38 C37 C36 120.4(4) . . ? F18 C38 C39 120.6(4) . . ? F18 C38 C37 120.3(5) . . ? C39 C38 C37 119.1(4) . . ? F17 C39 C38 120.1(4) . . ? F17 C39 C40 119.8(4) . . ? C38 C39 C40 120.1(4) . . ? F16 C40 C39 115.9(4) . . ? F16 C40 C35 121.3(4) . . ? C39 C40 C35 122.8(4) . . ? C46 C41 C42 115.4(4) . . ? C46 C41 C12 126.3(4) . . ? C42 C41 C12 118.2(4) . . ? F11 C42 C43 118.0(4) . . ? F11 C42 C41 119.7(4) . . ? C43 C42 C41 122.3(4) . . ? F12 C43 C44 120.4(4) . . ? F12 C43 C42 119.2(5) . . ? C44 C43 C42 120.4(4) . . ? F13 C44 C43 120.9(4) . . ? F13 C44 C45 119.6(5) . . ? C43 C44 C45 119.4(4) . . ? F14 C45 C46 119.6(4) . . ? F14 C45 C44 120.1(4) . . ? C46 C45 C44 120.3(4) . . ? F15 C46 C45 116.6(4) . . ? F15 C46 C41 121.1(3) . . ? C45 C46 C41 122.2(4) . . ? N1 C47 C48 103.4(4) . . ? C49 C48 C47 105.4(4) . . ? C48 C49 C50 106.9(4) . . ? N1 C50 C49 104.0(3) . . ? C47 N1 C50 109.5(3) . . ? C47 N1 P1 119.7(3) . . ? C50 N1 P1 128.5(3) . . ? S1 O1 Rh1 136.05(19) . . ? C12 O4 P1 128.1(2) . . ? C9 O5 P1 124.5(2) . . ? C11 O6 C13 109.5(3) . . ? C10 O7 C13 110.3(3) . . ? O5 P1 O4 103.02(14) . . ? O5 P1 N1 98.25(16) . . ? O4 P1 N1 109.15(16) . . ? O5 P1 Rh1 117.86(10) . . ? O4 P1 Rh1 115.15(11) . . ? N1 P1 Rh1 111.79(12) . . ? C4 Rh1 O1 159.38(16) . . ? C4 Rh1 C3 38.94(17) . . ? O1 Rh1 C3 161.58(15) . . ? C4 Rh1 C1 96.45(17) . . ? O1 Rh1 C1 92.95(15) . . ? C3 Rh1 C1 81.22(16) . . ? C4 Rh1 P1 93.91(12) . . ? O1 Rh1 P1 80.50(8) . . ? C3 Rh1 P1 101.05(12) . . ? C1 Rh1 P1 165.74(13) . . ? C4 Rh1 C2 81.08(17) . . ? O1 Rh1 C2 96.39(14) . . ? C3 Rh1 C2 89.00(16) . . ? C1 Rh1 C2 35.55(16) . . ? P1 Rh1 C2 157.25(13) . . ? O2 S1 O3 116.2(2) . . ? O2 S1 O1 111.50(19) . . ? O3 S1 O1 110.6(2) . . ? O2 S1 C16 107.4(2) . . ? O3 S1 C16 107.2(2) . . ? O1 S1 C16 102.97(18) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.52 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.740 _refine_diff_density_min -1.029 _refine_diff_density_rms 0.215 data_rovis141r_0m-sr _database_code_depnum_ccdc_archive 'CCDC 901685' #TrackingRef '- rovis141r_0m-sr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H52 Co F20 N2 O7 P' _chemical_formula_weight 1310.88 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4123(5) _cell_length_b 14.8876(6) _cell_length_c 16.7728(7) _cell_angle_alpha 94.268(2) _cell_angle_beta 90.340(2) _cell_angle_gamma 97.344(2) _cell_volume 3312.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7211 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 20.59 _exptl_crystal_description Plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not determined' _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.385 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8137 _exptl_absorpt_correction_T_max 0.9795 _exptl_absorpt_process_details 'Sheldrick, G. M. (2008) SADABS. University of Gottingen, Germany.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48968 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 26.45 _reflns_number_total 13496 _reflns_number_gt 6729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'APEX2 (Bruker, 2009)' _computing_data_reduction 'APEX2 (Bruker, 2009)' _computing_structure_solution 'XS (Sheldrick, 2008)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_molecular_graphics 'APEX2 (Bruker, 2009)' _computing_publication_material 'APEX2 (Bruker, 2009)' _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. ; 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 -0.005 0.000 0.500 663 162 ' ' _platon_squeeze_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13496 _refine_ls_number_parameters 772 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1172 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1645 _refine_ls_wR_factor_gt 0.1458 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_restrained_S_all 0.934 _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 C1 C 0.1347(3) 0.3478(2) 0.4123(2) 0.0634(10) Uani 1 1 d . . . C2 C 0.2441(3) 0.2324(2) 0.5031(2) 0.0605(10) Uani 1 1 d . . . C3 C 0.3367(3) 0.3303(2) 0.3786(2) 0.0654(10) Uani 1 1 d . . . C4 C 0.1574(2) 0.1869(2) 0.18425(18) 0.0450(8) Uani 1 1 d . . . C5 C 0.2393(2) 0.1244(2) 0.16998(17) 0.0448(8) Uani 1 1 d . . . H5 H 0.2065 0.0614 0.1656 0.054 Uiso 1 1 calc R . . C6 C 0.3280(2) 0.1306(2) 0.22991(18) 0.0446(8) Uani 1 1 d . . . H6 H 0.3401 0.1925 0.2555 0.053 Uiso 1 1 calc R . . C7 C 0.3085(2) 0.0620(2) 0.29590(18) 0.0432(8) Uani 1 1 d . . . C8 C 0.3808(3) 0.1090(2) 0.0982(2) 0.0596(9) Uani 1 1 d . . . C9 C 0.4583(3) 0.1708(3) 0.0529(2) 0.0839(13) Uani 1 1 d . . . H9A H 0.4361 0.1712 -0.0016 0.126 Uiso 1 1 calc R . . H9B H 0.5222 0.1482 0.0540 0.126 Uiso 1 1 calc R . . H9C H 0.4650 0.2314 0.0779 0.126 Uiso 1 1 calc R . . C10 C 0.3709(3) 0.0097(3) 0.0644(2) 0.0756(12) Uani 1 1 d . . . H10A H 0.3192 -0.0255 0.0922 0.113 Uiso 1 1 calc R . . H10B H 0.4336 -0.0136 0.0712 0.113 Uiso 1 1 calc R . . H10C H 0.3536 0.0062 0.0085 0.113 Uiso 1 1 calc R . . C11 C 0.1846(3) 0.2913(2) 0.19506(18) 0.0490(8) Uani 1 1 d . . . C12 C 0.1070(3) 0.3420(2) 0.2136(2) 0.0608(10) Uani 1 1 d . . . C13 C 0.1207(4) 0.4354(3) 0.2260(3) 0.0786(12) Uani 1 1 d . . . C14 C 0.2139(4) 0.4818(2) 0.2205(3) 0.0850(13) Uani 1 1 d . . . C15 C 0.2920(3) 0.4355(3) 0.2008(2) 0.0733(11) Uani 1 1 d . . . C16 C 0.2786(3) 0.3421(2) 0.1897(2) 0.0558(9) Uani 1 1 d . . . C17 C 0.0825(3) 0.1642(2) 0.1123(2) 0.0506(8) Uani 1 1 d . . . C18 C 0.0890(3) 0.2108(3) 0.0446(2) 0.0709(11) Uani 1 1 d . . . C19 C 0.0217(4) 0.1922(3) -0.0188(3) 0.0918(15) Uani 1 1 d . . . C20 C -0.0560(4) 0.1253(4) -0.0148(3) 0.0904(15) Uani 1 1 d . . . C21 C -0.0634(3) 0.0754(3) 0.0475(3) 0.0752(12) Uani 1 1 d . . . C22 C 0.0063(3) 0.0936(3) 0.1092(2) 0.0611(10) Uani 1 1 d . . . C23 C 0.3739(2) 0.0846(2) 0.37207(18) 0.0431(8) Uani 1 1 d . . . C24 C 0.4556(3) 0.1497(2) 0.3850(2) 0.0536(9) Uani 1 1 d . . . C25 C 0.5051(3) 0.1677(2) 0.4569(2) 0.0604(10) Uani 1 1 d . . . C26 C 0.4742(3) 0.1197(3) 0.5200(2) 0.0640(10) Uani 1 1 d . . . C27 C 0.3948(3) 0.0525(2) 0.5113(2) 0.0578(9) Uani 1 1 d . . . C28 C 0.3473(2) 0.0358(2) 0.4376(2) 0.0507(8) Uani 1 1 d . . . C29 C 0.3219(2) -0.0340(2) 0.26174(18) 0.0474(8) Uani 1 1 d . . . C30 C 0.2449(3) -0.1025(2) 0.23854(19) 0.0509(8) Uani 1 1 d . . . C31 C 0.2622(3) -0.1861(2) 0.2057(2) 0.0648(10) Uani 1 1 d . . . C32 C 0.3580(4) -0.2053(3) 0.1947(3) 0.0805(13) Uani 1 1 d . . . C33 C 0.4373(3) -0.1404(3) 0.2179(3) 0.0764(12) Uani 1 1 d . . . C34 C 0.4185(3) -0.0580(2) 0.2508(2) 0.0578(9) Uani 1 1 d . . . C35 C -0.0136(3) 0.1495(3) 0.4340(3) 0.0894(14) Uani 1 1 d . . . H35A H -0.0213 0.2071 0.4128 0.107 Uiso 1 1 calc R . . H35B H 0.0124 0.1611 0.4883 0.107 Uiso 1 1 calc R . . C36 C -0.1098(4) 0.0916(4) 0.4325(4) 0.145(3) Uani 1 1 d . . . H36A H -0.1285 0.0776 0.4863 0.174 Uiso 1 1 calc R . . H36B H -0.1617 0.1228 0.4104 0.174 Uiso 1 1 calc R . . C37 C -0.1009(4) 0.0104(4) 0.3846(4) 0.145(3) Uani 1 1 d . . . H37A H -0.1476 0.0047 0.3396 0.174 Uiso 1 1 calc R . . H37B H -0.1177 -0.0414 0.4160 0.174 Uiso 1 1 calc R . . C38 C 0.0026(3) 0.0113(2) 0.3551(2) 0.0669(10) Uani 1 1 d . . . H38A H 0.0030 0.0041 0.2972 0.080 Uiso 1 1 calc R . . H38B H 0.0346 -0.0370 0.3762 0.080 Uiso 1 1 calc R . . C39 C 0.4645(5) 0.6448(4) 0.3510(4) 0.157(3) Uani 1 1 d . . . H39A H 0.5069 0.6827 0.3177 0.235 Uiso 1 1 calc R . . H39B H 0.4253 0.6817 0.3843 0.235 Uiso 1 1 calc R . . H39C H 0.4203 0.6013 0.3179 0.235 Uiso 1 1 calc R . . C40 C 0.5267(3) 0.5971(3) 0.4012(3) 0.0912(14) Uani 1 1 d . . . H40A H 0.4836 0.5515 0.4277 0.109 Uiso 1 1 calc R . . H40B H 0.5601 0.6401 0.4422 0.109 Uiso 1 1 calc R . . C41 C 0.6051(3) 0.5517(3) 0.3546(3) 0.0878(13) Uani 1 1 d . . . H41A H 0.5714 0.5050 0.3168 0.105 Uiso 1 1 calc R . . H41B H 0.6441 0.5964 0.3242 0.105 Uiso 1 1 calc R . . C42 C 0.6737(3) 0.5105(3) 0.4048(3) 0.0774(12) Uani 1 1 d . . . H42A H 0.6332 0.4675 0.4359 0.093 Uiso 1 1 calc R . . H42B H 0.7063 0.5581 0.4423 0.093 Uiso 1 1 calc R . . C43 C 0.8287(3) 0.4400(3) 0.4275(3) 0.0843(13) Uani 1 1 d . . . H43A H 0.8837 0.4155 0.3998 0.101 Uiso 1 1 calc R . . H43B H 0.8564 0.4962 0.4571 0.101 Uiso 1 1 calc R . . C44 C 0.7878(4) 0.3750(3) 0.4855(3) 0.0988(15) Uani 1 1 d . . . H44A H 0.7308 0.3982 0.5114 0.119 Uiso 1 1 calc R . . H44B H 0.7629 0.3179 0.4561 0.119 Uiso 1 1 calc R . . C45 C 0.8584(4) 0.3563(4) 0.5483(3) 0.1104(17) Uani 1 1 d . . . H45A H 0.8783 0.4122 0.5812 0.132 Uiso 1 1 calc R . . H45B H 0.9184 0.3386 0.5227 0.132 Uiso 1 1 calc R . . C46 C 0.7054(3) 0.3759(3) 0.3187(3) 0.0850(13) Uani 1 1 d . . . H46A H 0.6629 0.3412 0.3551 0.102 Uiso 1 1 calc R . . H46B H 0.6616 0.3941 0.2783 0.102 Uiso 1 1 calc R . . C47 C 0.8192(4) 0.2849(4) 0.6013(3) 0.1233(19) Uani 1 1 d . . . H47A H 0.7675 0.3061 0.6342 0.185 Uiso 1 1 calc R . . H47B H 0.8729 0.2712 0.6346 0.185 Uiso 1 1 calc R . . H47C H 0.7919 0.2311 0.5693 0.185 Uiso 1 1 calc R . . C48 C 0.7704(4) 0.3147(3) 0.2787(3) 0.1021(15) Uani 1 1 d . . . H48A H 0.8165 0.2979 0.3182 0.122 Uiso 1 1 calc R . . H48B H 0.8103 0.3475 0.2396 0.122 Uiso 1 1 calc R . . C49 C 0.7164(5) 0.2306(4) 0.2381(4) 0.149(3) Uani 1 1 d . . . H49A H 0.6825 0.1961 0.2791 0.179 Uiso 1 1 calc R . . H49B H 0.6643 0.2487 0.2046 0.179 Uiso 1 1 calc R . . C50 C 0.8127(3) 0.5216(3) 0.3064(3) 0.0831(13) Uani 1 1 d . . . H50A H 0.8669 0.4900 0.2853 0.100 Uiso 1 1 calc R . . H50B H 0.7676 0.5267 0.2619 0.100 Uiso 1 1 calc R . . C51 C 0.8563(4) 0.6143(3) 0.3357(3) 0.0905(14) Uani 1 1 d . . . H51A H 0.8038 0.6449 0.3611 0.109 Uiso 1 1 calc R . . H51B H 0.9069 0.6099 0.3763 0.109 Uiso 1 1 calc R . . C52 C 0.7691(6) 0.1695(5) 0.1896(5) 0.207(4) Uani 1 1 d . . . H52A H 0.7895 0.1965 0.1411 0.311 Uiso 1 1 calc R . . H52B H 0.7257 0.1137 0.1769 0.311 Uiso 1 1 calc R . . H52C H 0.8274 0.1573 0.2183 0.311 Uiso 1 1 calc R . . C53 C 0.9021(4) 0.6702(3) 0.2746(4) 0.132(2) Uani 1 1 d . . . H53A H 0.9620 0.6446 0.2570 0.159 Uiso 1 1 calc R . . H53B H 0.8558 0.6629 0.2292 0.159 Uiso 1 1 calc R . . C54 C 0.9303(5) 0.7652(4) 0.2919(4) 0.156(3) Uani 1 1 d . . . H54A H 0.8711 0.7951 0.2957 0.233 Uiso 1 1 calc R . . H54B H 0.9719 0.7889 0.2500 0.233 Uiso 1 1 calc R . . H54C H 0.9670 0.7754 0.3418 0.233 Uiso 1 1 calc R . . Co1 Co 0.22374(3) 0.27368(3) 0.41022(3) 0.05119(16) Uani 1 1 d . . . F1 F 0.01183(15) 0.30143(14) 0.21807(14) 0.0769(6) Uani 1 1 d . . . F2 F 0.0416(2) 0.47920(16) 0.24302(19) 0.1136(9) Uani 1 1 d . . . F3 F 0.2280(2) 0.57259(15) 0.2326(2) 0.1296(11) Uani 1 1 d . . . F4 F 0.38551(19) 0.48019(15) 0.19357(16) 0.1010(8) Uani 1 1 d . . . F5 F 0.36095(15) 0.30398(13) 0.17114(12) 0.0673(6) Uani 1 1 d . . . F6 F 0.1656(2) 0.27863(17) 0.03667(13) 0.0964(8) Uani 1 1 d . . . F7 F 0.0338(3) 0.2436(2) -0.08174(17) 0.1474(13) Uani 1 1 d . . . F8 F -0.1230(2) 0.1084(2) -0.07585(17) 0.1322(11) Uani 1 1 d . . . F9 F -0.1388(2) 0.00663(19) 0.04959(16) 0.1117(9) Uani 1 1 d . . . F10 F -0.00775(19) 0.03592(16) 0.16750(14) 0.0938(8) Uani 1 1 d . . . F11 F 0.49292(15) 0.19856(14) 0.32500(12) 0.0713(6) Uani 1 1 d . . . F12 F 0.58473(17) 0.23209(16) 0.46533(15) 0.0952(8) Uani 1 1 d . . . F13 F 0.52323(19) 0.13612(16) 0.59118(13) 0.0924(8) Uani 1 1 d . . . F14 F 0.36446(17) 0.00356(16) 0.57230(12) 0.0790(6) Uani 1 1 d . . . F15 F 0.27180(15) -0.03385(13) 0.43152(11) 0.0638(5) Uani 1 1 d . . . F16 F 0.14845(15) -0.09062(12) 0.24478(12) 0.0648(5) Uani 1 1 d . . . F17 F 0.18416(19) -0.24905(13) 0.18341(14) 0.0891(7) Uani 1 1 d . . . F18 F 0.3754(2) -0.28662(16) 0.16030(18) 0.1180(10) Uani 1 1 d . . . F19 F 0.53169(19) -0.15824(17) 0.20674(17) 0.1083(9) Uani 1 1 d . . . F20 F 0.49962(15) 0.00196(14) 0.27231(13) 0.0720(6) Uani 1 1 d . . . N1 N 0.05431(19) 0.10160(18) 0.38500(15) 0.0521(7) Uani 1 1 d . . . N2 N 0.7549(2) 0.46196(19) 0.36574(18) 0.0598(8) Uani 1 1 d . . . O1 O 0.0742(2) 0.3977(2) 0.4140(2) 0.0972(10) Uani 1 1 d . . . O2 O 0.2590(2) 0.2062(2) 0.56455(18) 0.0909(9) Uani 1 1 d . . . O3 O 0.4117(2) 0.3728(2) 0.3621(2) 0.1045(11) Uani 1 1 d . . . O4 O 0.20740(14) 0.06261(12) 0.31979(11) 0.0411(5) Uani 1 1 d . . . O5 O 0.10214(14) 0.16015(13) 0.25294(12) 0.0435(5) Uani 1 1 d . . . O6 O 0.28640(17) 0.14168(15) 0.09655(12) 0.0561(6) Uani 1 1 d . . . O7 O 0.41020(16) 0.11490(15) 0.18076(13) 0.0554(6) Uani 1 1 d . . . P1 P 0.15332(6) 0.15521(5) 0.34366(5) 0.0426(2) Uani 1 1 d . . . 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 C1 0.068(3) 0.058(2) 0.062(2) -0.0119(18) 0.011(2) 0.004(2) C2 0.062(2) 0.060(2) 0.058(3) -0.0119(19) 0.002(2) 0.0118(18) C3 0.066(3) 0.056(2) 0.068(3) -0.0130(18) -0.001(2) -0.002(2) C4 0.0428(19) 0.0469(18) 0.0449(19) -0.0006(15) -0.0001(16) 0.0067(15) C5 0.051(2) 0.0470(18) 0.0361(18) -0.0006(14) 0.0051(15) 0.0058(15) C6 0.0358(18) 0.0483(18) 0.050(2) -0.0041(15) 0.0081(15) 0.0096(14) C7 0.0353(18) 0.0478(18) 0.0459(19) 0.0001(15) 0.0021(15) 0.0049(14) C8 0.054(2) 0.073(2) 0.054(2) 0.0026(18) 0.0121(18) 0.0177(19) C9 0.083(3) 0.091(3) 0.080(3) 0.012(2) 0.033(2) 0.015(2) C10 0.087(3) 0.078(3) 0.065(3) -0.012(2) 0.015(2) 0.029(2) C11 0.054(2) 0.0504(19) 0.0426(19) 0.0028(15) 0.0052(16) 0.0072(17) C12 0.063(3) 0.050(2) 0.069(3) 0.0025(18) 0.009(2) 0.0086(19) C13 0.089(3) 0.056(3) 0.095(3) 0.003(2) 0.025(3) 0.029(2) C14 0.100(4) 0.036(2) 0.119(4) 0.001(2) 0.023(3) 0.009(2) C15 0.084(3) 0.052(2) 0.079(3) 0.004(2) 0.012(2) -0.012(2) C16 0.062(2) 0.053(2) 0.053(2) 0.0046(16) 0.0083(18) 0.0076(18) C17 0.055(2) 0.051(2) 0.047(2) 0.0013(16) -0.0023(17) 0.0143(17) C18 0.078(3) 0.069(3) 0.065(3) 0.006(2) -0.006(2) 0.006(2) C19 0.117(4) 0.106(4) 0.055(3) 0.018(3) -0.026(3) 0.015(3) C20 0.096(4) 0.106(4) 0.068(3) -0.014(3) -0.042(3) 0.020(3) C21 0.072(3) 0.074(3) 0.076(3) -0.011(2) -0.017(2) 0.007(2) C22 0.069(3) 0.061(2) 0.052(2) -0.0008(19) -0.015(2) 0.007(2) C23 0.0383(18) 0.0465(18) 0.0444(19) 0.0025(15) -0.0004(15) 0.0054(14) C24 0.045(2) 0.058(2) 0.057(2) 0.0052(18) -0.0027(18) 0.0011(17) C25 0.046(2) 0.064(2) 0.067(3) -0.003(2) -0.0139(19) -0.0037(18) C26 0.063(3) 0.073(3) 0.056(2) -0.011(2) -0.023(2) 0.016(2) C27 0.059(2) 0.064(2) 0.052(2) 0.0048(19) -0.0036(19) 0.0162(19) C28 0.043(2) 0.0496(19) 0.058(2) -0.0013(17) -0.0019(17) 0.0049(16) C29 0.048(2) 0.0471(18) 0.048(2) 0.0022(15) -0.0007(16) 0.0097(16) C30 0.055(2) 0.049(2) 0.050(2) 0.0053(16) 0.0002(17) 0.0130(17) C31 0.082(3) 0.043(2) 0.069(3) 0.0022(18) -0.009(2) 0.009(2) C32 0.109(4) 0.053(2) 0.083(3) -0.010(2) -0.003(3) 0.035(3) C33 0.075(3) 0.074(3) 0.087(3) -0.001(2) 0.005(2) 0.035(2) C34 0.055(2) 0.063(2) 0.057(2) -0.0002(18) -0.0036(18) 0.0161(19) C35 0.072(3) 0.081(3) 0.112(4) -0.007(3) 0.041(3) 0.002(2) C36 0.067(4) 0.135(5) 0.222(7) -0.019(5) 0.054(4) -0.013(3) C37 0.058(3) 0.087(4) 0.277(8) -0.033(4) 0.047(4) -0.017(3) C38 0.054(2) 0.060(2) 0.080(3) 0.0046(19) 0.009(2) -0.0150(18) C39 0.139(5) 0.150(5) 0.191(7) -0.044(5) -0.056(5) 0.088(5) C40 0.073(3) 0.081(3) 0.117(4) -0.020(3) 0.009(3) 0.013(2) C41 0.058(3) 0.086(3) 0.118(4) 0.001(3) -0.004(3) 0.010(2) C42 0.062(3) 0.078(3) 0.091(3) 0.004(2) 0.017(2) 0.008(2) C43 0.074(3) 0.089(3) 0.088(3) -0.007(3) -0.003(3) 0.013(2) C44 0.095(4) 0.108(4) 0.091(3) 0.018(3) -0.003(3) 0.000(3) C45 0.110(4) 0.110(4) 0.113(4) 0.015(3) -0.025(3) 0.017(3) C46 0.082(3) 0.087(3) 0.084(3) -0.018(2) 0.001(2) 0.015(2) C47 0.136(5) 0.132(5) 0.110(4) 0.040(4) -0.005(4) 0.030(4) C48 0.105(4) 0.083(3) 0.117(4) -0.023(3) -0.004(3) 0.025(3) C49 0.155(6) 0.103(4) 0.179(6) -0.060(4) 0.050(5) 0.014(4) C50 0.064(3) 0.087(3) 0.096(3) -0.005(3) 0.016(2) 0.011(2) C51 0.086(3) 0.079(3) 0.104(4) -0.003(3) 0.020(3) 0.001(3) C52 0.209(8) 0.152(6) 0.250(9) -0.096(6) 0.023(7) 0.044(6) C53 0.130(5) 0.066(3) 0.193(6) 0.003(3) 0.061(4) -0.018(3) C54 0.161(6) 0.103(5) 0.197(7) 0.007(4) 0.072(5) -0.006(4) Co1 0.0518(3) 0.0483(3) 0.0498(3) -0.0096(2) 0.0023(2) 0.0001(2) F1 0.0498(13) 0.0695(13) 0.1138(18) 0.0043(12) 0.0066(12) 0.0186(11) F2 0.105(2) 0.0717(16) 0.173(3) 0.0070(16) 0.0298(18) 0.0455(15) F3 0.148(3) 0.0422(14) 0.196(3) 0.0006(16) 0.030(2) 0.0082(15) F4 0.0944(19) 0.0608(14) 0.139(2) 0.0038(14) 0.0163(16) -0.0210(13) F5 0.0534(13) 0.0605(12) 0.0865(15) 0.0039(10) 0.0184(11) 0.0020(10) F6 0.121(2) 0.1011(18) 0.0629(15) 0.0235(13) -0.0049(14) -0.0111(16) F7 0.214(4) 0.154(3) 0.0736(19) 0.0396(19) -0.042(2) 0.003(3) F8 0.143(3) 0.154(3) 0.098(2) -0.0088(18) -0.064(2) 0.023(2) F9 0.095(2) 0.116(2) 0.111(2) -0.0182(16) -0.0363(16) -0.0223(17) F10 0.110(2) 0.0797(15) 0.0807(16) 0.0079(13) -0.0313(14) -0.0287(14) F11 0.0527(13) 0.0805(14) 0.0753(15) 0.0155(12) -0.0034(11) -0.0174(11) F12 0.0728(16) 0.0984(17) 0.1037(18) 0.0032(14) -0.0327(13) -0.0266(14) F13 0.1027(18) 0.1019(17) 0.0688(15) -0.0068(12) -0.0408(14) 0.0088(14) F14 0.0848(16) 0.0979(16) 0.0571(13) 0.0214(12) -0.0039(12) 0.0136(13) F15 0.0597(13) 0.0670(12) 0.0621(13) 0.0176(10) -0.0049(10) -0.0085(10) F16 0.0570(13) 0.0547(11) 0.0779(14) -0.0110(10) -0.0053(10) -0.0018(10) F17 0.1110(19) 0.0464(12) 0.1047(18) -0.0101(11) -0.0134(15) -0.0004(12) F18 0.145(3) 0.0655(15) 0.147(2) -0.0263(15) -0.0007(19) 0.0474(16) F19 0.0849(19) 0.1014(19) 0.145(2) -0.0168(16) 0.0058(16) 0.0526(15) F20 0.0474(12) 0.0791(14) 0.0899(15) -0.0082(12) -0.0002(11) 0.0178(11) N1 0.0427(16) 0.0552(16) 0.0548(17) -0.0069(13) 0.0155(13) -0.0017(13) N2 0.0467(18) 0.0654(19) 0.0651(19) -0.0032(15) 0.0058(15) 0.0030(15) O1 0.088(2) 0.080(2) 0.127(3) -0.0054(18) 0.0141(19) 0.0323(18) O2 0.122(3) 0.100(2) 0.0573(18) 0.0060(16) 0.0016(17) 0.0381(19) O3 0.080(2) 0.089(2) 0.131(3) -0.0060(19) 0.0214(19) -0.0324(18) O4 0.0339(12) 0.0401(11) 0.0482(12) -0.0016(9) 0.0041(9) 0.0030(9) O5 0.0367(12) 0.0501(12) 0.0429(12) -0.0006(9) 0.0014(10) 0.0043(9) O6 0.0599(15) 0.0689(15) 0.0424(13) 0.0039(11) 0.0104(11) 0.0186(12) O7 0.0451(14) 0.0690(15) 0.0531(15) 0.0025(11) 0.0108(11) 0.0118(11) P1 0.0378(5) 0.0446(5) 0.0434(5) -0.0032(4) 0.0041(4) 0.0011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.167(4) . ? C1 Co1 1.726(4) . ? C2 O2 1.153(4) . ? C2 Co1 1.750(4) . ? C3 O3 1.164(4) . ? C3 Co1 1.743(4) . ? C4 O5 1.427(4) . ? C4 C5 1.537(4) . ? C4 C11 1.548(4) . ? C4 C17 1.555(4) . ? C5 O6 1.413(3) . ? C5 C6 1.542(4) . ? C6 O7 1.414(3) . ? C6 C7 1.562(4) . ? C7 O4 1.417(3) . ? C7 C29 1.532(4) . ? C7 C23 1.537(4) . ? C8 O6 1.415(4) . ? C8 O7 1.430(4) . ? C8 C10 1.532(5) . ? C8 C9 1.541(5) . ? C11 C12 1.386(5) . ? C11 C16 1.392(5) . ? C12 F1 1.346(4) . ? C12 C13 1.378(5) . ? C13 F2 1.337(4) . ? C13 C14 1.355(6) . ? C14 F3 1.341(4) . ? C14 C15 1.355(6) . ? C15 F4 1.354(4) . ? C15 C16 1.376(5) . ? C16 F5 1.333(4) . ? C17 C22 1.367(5) . ? C17 C18 1.371(5) . ? C18 F6 1.360(4) . ? C18 C19 1.379(6) . ? C19 F7 1.349(5) . ? C19 C20 1.350(6) . ? C20 C21 1.325(6) . ? C20 F8 1.346(5) . ? C21 F9 1.347(4) . ? C21 C22 1.379(5) . ? C22 F10 1.348(4) . ? C23 C24 1.372(4) . ? C23 C28 1.386(4) . ? C24 F11 1.346(4) . ? C24 C25 1.366(5) . ? C25 F12 1.341(4) . ? C25 C26 1.357(5) . ? C26 F13 1.350(4) . ? C26 C27 1.364(5) . ? C27 F14 1.336(4) . ? C27 C28 1.377(5) . ? C28 F15 1.352(3) . ? C29 C30 1.388(4) . ? C29 C34 1.397(5) . ? C30 F16 1.332(4) . ? C30 C31 1.371(5) . ? C31 F17 1.343(4) . ? C31 C32 1.363(6) . ? C32 F18 1.350(4) . ? C32 C33 1.377(6) . ? C33 F19 1.338(4) . ? C33 C34 1.361(5) . ? C34 F20 1.345(4) . ? C35 N1 1.449(5) . ? C35 C36 1.456(6) . ? C36 C37 1.419(7) . ? C37 C38 1.475(6) . ? C38 N1 1.482(4) . ? C39 C40 1.465(7) . ? C40 C41 1.513(6) . ? C41 C42 1.464(6) . ? C42 N2 1.509(5) . ? C43 C44 1.481(6) . ? C43 N2 1.511(5) . ? C44 C45 1.477(6) . ? C45 C47 1.484(6) . ? C46 C48 1.470(6) . ? C46 N2 1.526(5) . ? C48 C49 1.480(6) . ? C49 C52 1.432(7) . ? C50 C51 1.476(5) . ? C50 N2 1.532(5) . ? C51 C53 1.458(6) . ? C53 C54 1.423(6) . ? Co1 P1 2.1254(8) . ? N1 P1 1.644(3) . ? O4 P1 1.663(2) . ? O5 P1 1.676(2) . ? 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 O1 C1 Co1 179.6(4) . . ? O2 C2 Co1 178.9(4) . . ? O3 C3 Co1 175.0(3) . . ? O5 C4 C5 108.3(2) . . ? O5 C4 C11 107.0(2) . . ? C5 C4 C11 121.0(3) . . ? O5 C4 C17 105.7(2) . . ? C5 C4 C17 105.9(2) . . ? C11 C4 C17 108.1(3) . . ? O6 C5 C4 109.3(2) . . ? O6 C5 C6 103.7(2) . . ? C4 C5 C6 119.7(2) . . ? O7 C6 C5 103.4(2) . . ? O7 C6 C7 113.4(3) . . ? C5 C6 C7 112.7(2) . . ? O4 C7 C29 108.7(2) . . ? O4 C7 C23 106.5(2) . . ? C29 C7 C23 108.6(3) . . ? O4 C7 C6 107.1(2) . . ? C29 C7 C6 110.2(2) . . ? C23 C7 C6 115.5(2) . . ? O6 C8 O7 105.6(2) . . ? O6 C8 C10 110.3(3) . . ? O7 C8 C10 109.6(3) . . ? O6 C8 C9 109.8(3) . . ? O7 C8 C9 109.0(3) . . ? C10 C8 C9 112.3(3) . . ? C12 C11 C16 114.7(3) . . ? C12 C11 C4 117.0(3) . . ? C16 C11 C4 128.2(3) . . ? F1 C12 C13 116.1(4) . . ? F1 C12 C11 120.7(3) . . ? C13 C12 C11 123.2(4) . . ? F2 C13 C14 120.7(4) . . ? F2 C13 C12 119.4(4) . . ? C14 C13 C12 119.9(4) . . ? F3 C14 C15 120.5(4) . . ? F3 C14 C13 120.2(4) . . ? C15 C14 C13 119.2(4) . . ? F4 C15 C14 120.5(4) . . ? F4 C15 C16 118.6(4) . . ? C14 C15 C16 120.9(4) . . ? F5 C16 C15 115.6(3) . . ? F5 C16 C11 122.3(3) . . ? C15 C16 C11 122.1(4) . . ? C22 C17 C18 113.6(3) . . ? C22 C17 C4 123.1(3) . . ? C18 C17 C4 123.3(3) . . ? F6 C18 C17 120.2(3) . . ? F6 C18 C19 116.3(4) . . ? C17 C18 C19 123.5(4) . . ? F7 C19 C20 122.1(4) . . ? F7 C19 C18 118.6(5) . . ? C20 C19 C18 119.3(4) . . ? C21 C20 F8 120.8(5) . . ? C21 C20 C19 119.8(4) . . ? F8 C20 C19 119.4(5) . . ? C20 C21 F9 119.5(4) . . ? C20 C21 C22 119.9(4) . . ? F9 C21 C22 120.6(4) . . ? F10 C22 C17 122.4(3) . . ? F10 C22 C21 113.9(4) . . ? C17 C22 C21 123.7(4) . . ? C24 C23 C28 114.4(3) . . ? C24 C23 C7 128.1(3) . . ? C28 C23 C7 117.5(3) . . ? F11 C24 C25 116.2(3) . . ? F11 C24 C23 120.5(3) . . ? C25 C24 C23 123.2(3) . . ? F12 C25 C26 119.8(3) . . ? F12 C25 C24 120.2(4) . . ? C26 C25 C24 120.1(3) . . ? F13 C26 C25 120.6(4) . . ? F13 C26 C27 119.3(4) . . ? C25 C26 C27 120.1(3) . . ? F14 C27 C26 120.9(3) . . ? F14 C27 C28 120.8(3) . . ? C26 C27 C28 118.3(3) . . ? F15 C28 C27 115.7(3) . . ? F15 C28 C23 120.3(3) . . ? C27 C28 C23 124.0(3) . . ? C30 C29 C34 114.5(3) . . ? C30 C29 C7 125.8(3) . . ? C34 C29 C7 119.8(3) . . ? F16 C30 C31 115.2(3) . . ? F16 C30 C29 122.0(3) . . ? C31 C30 C29 122.8(3) . . ? F17 C31 C32 119.9(3) . . ? F17 C31 C30 119.8(4) . . ? C32 C31 C30 120.3(4) . . ? F18 C32 C31 120.5(4) . . ? F18 C32 C33 120.1(4) . . ? C31 C32 C33 119.4(4) . . ? F19 C33 C34 120.8(4) . . ? F19 C33 C32 119.8(4) . . ? C34 C33 C32 119.4(4) . . ? F20 C34 C33 116.1(3) . . ? F20 C34 C29 120.3(3) . . ? C33 C34 C29 123.6(4) . . ? N1 C35 C36 107.1(4) . . ? C37 C36 C35 108.6(4) . . ? C36 C37 C38 110.3(4) . . ? C37 C38 N1 104.3(3) . . ? C39 C40 C41 113.0(5) . . ? C42 C41 C40 113.7(4) . . ? C41 C42 N2 119.2(4) . . ? C44 C43 N2 115.9(4) . . ? C45 C44 C43 116.2(4) . . ? C44 C45 C47 115.5(5) . . ? C48 C46 N2 118.4(4) . . ? C46 C48 C49 114.8(4) . . ? C52 C49 C48 120.8(6) . . ? C51 C50 N2 117.9(3) . . ? C53 C51 C50 115.0(4) . . ? C54 C53 C51 120.4(5) . . ? C1 Co1 C3 108.34(18) . . ? C1 Co1 C2 113.38(17) . . ? C3 Co1 C2 108.66(18) . . ? C1 Co1 P1 104.31(12) . . ? C3 Co1 P1 120.39(11) . . ? C2 Co1 P1 101.83(11) . . ? C35 N1 C38 109.6(3) . . ? C35 N1 P1 121.9(2) . . ? C38 N1 P1 124.7(2) . . ? C42 N2 C43 110.8(3) . . ? C42 N2 C46 108.6(3) . . ? C43 N2 C46 111.2(3) . . ? C42 N2 C50 110.3(3) . . ? C43 N2 C50 108.3(3) . . ? C46 N2 C50 107.6(3) . . ? C7 O4 P1 125.24(17) . . ? C4 O5 P1 124.50(18) . . ? C5 O6 C8 107.5(2) . . ? C6 O7 C8 110.4(2) . . ? N1 P1 O4 95.44(12) . . ? N1 P1 O5 97.57(12) . . ? O4 P1 O5 95.50(10) . . ? N1 P1 Co1 115.64(10) . . ? O4 P1 Co1 124.99(8) . . ? O5 P1 Co1 121.56(8) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.535 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.072