# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 925034' #TrackingRef '17866_web_deposit_cif_file_0_DavidPowers_1361207103.Cif Files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Rh(I)Rh(III)tfepma2Cl4(CNAd)2 _chemical_melting_point 'Not Measured' _chemical_formula_moiety 'C40 H52 Cl4 F24 N3 O8 P4 Rh2' _chemical_formula_sum 'C40 H52 Cl4 F24 N3 O8 P4 Rh2' _chemical_formula_weight 1644.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.7242(5) _cell_length_b 20.3878(8) _cell_length_c 23.2389(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.4970(10) _cell_angle_gamma 90.00 _cell_volume 5977.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2920 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7017 _exptl_absorpt_correction_T_max 0.8322 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 135954 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 30.03 _reflns_number_total 17477 _reflns_number_gt 12674 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0405P)^2^+19.7337P] 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 17477 _refine_ls_number_parameters 1024 _refine_ls_number_restraints 184 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 1.389999(19) 0.313574(12) 0.274746(11) 0.01754(6) Uani 1 1 d . G . Rh2 Rh 1.37811(2) 0.180673(13) 0.273643(11) 0.02134(6) Uani 1 1 d . G . Cl1 Cl 1.36398(9) 0.05922(5) 0.26684(5) 0.0400(2) Uani 1 1 d . . . Cl2 Cl 1.40542(7) 0.43316(4) 0.27291(4) 0.02711(17) Uani 1 1 d . . . Cl3 Cl 1.41994(7) 0.31433(4) 0.37723(3) 0.02511(16) Uani 1 1 d . . . Cl4 Cl 1.35479(7) 0.31202(4) 0.17286(4) 0.02515(17) Uani 1 1 d . . . P1 P 1.24072(7) 0.18876(4) 0.32676(4) 0.02061(17) Uani 1 1 d . G . P2 P 1.21446(6) 0.32028(4) 0.28345(4) 0.01858(16) Uani 1 1 d . . . P3 P 1.52537(9) 0.17513(6) 0.22612(5) 0.0387(3) Uani 1 1 d U . . P4 P 1.56668(7) 0.30683(5) 0.26711(5) 0.0330(2) Uani 1 1 d U . . N1 N 1.1657(3) 0.25595(16) 0.31645(17) 0.0358(6) Uani 1 1 d . . . N2 N 1.6080(3) 0.23820(16) 0.23832(17) 0.0358(6) Uani 1 1 d U A . N3 N 1.5481(3) 0.15967(16) 0.38137(14) 0.0314(7) Uani 1 1 d . B . N4 N 1.1940(3) 0.17010(15) 0.17198(13) 0.0280(6) Uani 1 1 d . H . O1 O 1.1492(2) 0.13514(12) 0.31157(11) 0.0287(5) Uani 1 1 d . . . O2 O 1.2737(2) 0.17797(13) 0.39444(11) 0.0336(6) Uani 1 1 d . . . O3 O 1.16753(19) 0.38176(12) 0.31431(11) 0.0267(5) Uani 1 1 d . . . O4 O 1.13136(19) 0.32121(12) 0.22537(11) 0.0250(5) Uani 1 1 d . . . O6 O 1.6063(3) 0.11831(15) 0.25090(14) 0.0432(8) Uani 1 1 d . E . O7 O 1.6478(2) 0.30937(18) 0.32663(16) 0.0535(9) Uani 1 1 d DU F . O8 O 1.6230(2) 0.36310(15) 0.23426(13) 0.0371(7) Uani 1 1 d . H . F43 F 0.9600(2) 0.33176(14) 0.14275(14) 0.0629(9) Uani 1 1 d . . . F44 F 0.9459(2) 0.39361(16) 0.21562(14) 0.0587(8) Uani 1 1 d . . . F45 F 0.9797(2) 0.43587(13) 0.13562(13) 0.0528(7) Uani 1 1 d . . . F83 F 1.73386(19) 0.38293(15) 0.14052(12) 0.0482(7) Uani 1 1 d . . . F84 F 1.5917(2) 0.41230(14) 0.08646(11) 0.0453(6) Uani 1 1 d . . . F85 F 1.6064(2) 0.31374(13) 0.12069(15) 0.0558(8) Uani 1 1 d . . . C1 C 1.0532(3) 0.2582(2) 0.3282(2) 0.0383(10) Uani 1 1 d . . . H1A H 1.0064 0.2447 0.2933 0.057 Uiso 1 1 calc R . . H1B H 1.0353 0.3030 0.3388 0.057 Uiso 1 1 calc R . . H1C H 1.0439 0.2284 0.3602 0.057 Uiso 1 1 calc R . . C2 C 1.7313(10) 0.2395(7) 0.2385(10) 0.029(3) Uani 0.46(4) 1 d P A 1 H2A H 1.7648 0.2100 0.2688 0.044 Uiso 0.46(4) 1 calc PR A 1 H2B H 1.7576 0.2842 0.2462 0.044 Uiso 0.46(4) 1 calc PR A 1 H2C H 1.7486 0.2250 0.2007 0.044 Uiso 0.46(4) 1 calc PR A 1 C2A C 1.7078(13) 0.2241(8) 0.2144(10) 0.038(4) Uani 0.54(4) 1 d P A 2 H2A1 H 1.7486 0.2647 0.2129 0.058 Uiso 0.54(4) 1 calc PR A 2 H2A2 H 1.6914 0.2060 0.1752 0.058 Uiso 0.54(4) 1 calc PR A 2 H2A3 H 1.7495 0.1921 0.2393 0.058 Uiso 0.54(4) 1 calc PR A 2 C11 C 1.1567(3) 0.06930(18) 0.33331(18) 0.0341(9) Uani 1 1 d . D . H11A H 1.2244 0.0631 0.3589 0.041 Uiso 1 1 calc R . . H11B H 1.1541 0.0378 0.3008 0.041 Uiso 1 1 calc R . . C12 C 1.0663(4) 0.0582(2) 0.3662(2) 0.0449(11) Uani 1 1 d DU . . C31 C 1.2194(3) 0.42697(18) 0.35544(17) 0.0292(8) Uani 1 1 d . C . H31A H 1.2189 0.4714 0.3382 0.035 Uiso 1 1 calc R . . H31B H 1.2940 0.4135 0.3667 0.035 Uiso 1 1 calc R . . C32 C 1.1624(4) 0.4275(2) 0.4070(2) 0.0459(11) Uani 1 1 d D . . C41 C 1.1169(3) 0.37879(19) 0.19008(18) 0.0312(8) Uani 1 1 d . . . H41A H 1.1556 0.3747 0.1560 0.037 Uiso 1 1 calc R . . H41B H 1.1434 0.4180 0.2126 0.037 Uiso 1 1 calc R . . C42 C 1.0002(3) 0.3846(2) 0.17113(19) 0.0363(9) Uani 1 1 d . . . C81 C 1.5788(3) 0.3998(2) 0.18462(18) 0.0345(7) Uani 1 1 d . . . H81A H 1.5928 0.4471 0.1913 0.041 Uiso 1 1 calc R H . H81B H 1.5012 0.3931 0.1776 0.041 Uiso 1 1 calc R . . C82 C 1.6284(3) 0.3770(2) 0.1333(2) 0.0362(9) Uani 1 1 d . H . C100 C 1.4853(3) 0.17150(17) 0.34365(15) 0.0255(7) Uani 1 1 d . . . C101 C 1.6323(3) 0.1408(2) 0.42658(17) 0.0353(9) Uani 1 1 d . . . C200 C 1.2658(3) 0.18004(17) 0.20589(15) 0.0263(7) Uani 1 1 d . . . C201 C 1.1002(3) 0.14660(18) 0.13500(15) 0.0291(8) Uani 1 1 d . . . C202 C 1.0044(3) 0.1539(2) 0.16848(18) 0.0354(9) Uani 1 1 d . H . H20A H 0.9937 0.2007 0.1776 0.042 Uiso 1 1 calc R . . H20B H 1.0168 0.1292 0.2054 0.042 Uiso 1 1 calc R . . C203 C 0.9060(4) 0.1269(2) 0.1304(2) 0.0428(10) Uani 1 1 d . . . H203 H 0.8426 0.1313 0.1514 0.051 Uiso 1 1 calc R H . C204 C 0.9242(4) 0.0546(2) 0.1175(2) 0.0485(12) Uani 1 1 d . H . H20C H 0.9363 0.0297 0.1544 0.058 Uiso 1 1 calc R . . H20D H 0.8606 0.0364 0.0939 0.058 Uiso 1 1 calc R . . C205 C 1.0192(4) 0.0473(2) 0.0852(2) 0.0482(12) Uani 1 1 d . . . H205 H 1.0296 -0.0001 0.0763 0.058 Uiso 1 1 calc R H . C206 C 1.1187(4) 0.07384(19) 0.12235(19) 0.0374(9) Uani 1 1 d . H . H20E H 1.1811 0.0690 0.1013 0.045 Uiso 1 1 calc R . . H20F H 1.1323 0.0490 0.1592 0.045 Uiso 1 1 calc R . . C207 C 1.0828(4) 0.1864(2) 0.07898(17) 0.0388(10) Uani 1 1 d . H . H20G H 1.1453 0.1826 0.0579 0.047 Uiso 1 1 calc R . . H20H H 1.0725 0.2333 0.0879 0.047 Uiso 1 1 calc R . . C208 C 0.8885(4) 0.1661(2) 0.0739(2) 0.0488(12) Uani 1 1 d . H . H20I H 0.8245 0.1497 0.0493 0.059 Uiso 1 1 calc R . . H20J H 0.8770 0.2128 0.0827 0.059 Uiso 1 1 calc R . . C209 C 1.0017(5) 0.0866(3) 0.0282(2) 0.0600(15) Uani 1 1 d . H . H20K H 0.9391 0.0693 0.0030 0.072 Uiso 1 1 calc R . . H20L H 1.0643 0.0820 0.0073 0.072 Uiso 1 1 calc R . . C210 C 0.9841(4) 0.1596(2) 0.04155(19) 0.0493(12) Uani 1 1 d . . . H210 H 0.9715 0.1848 0.0044 0.059 Uiso 1 1 calc R H . C102 C 1.7412(5) 0.1618(4) 0.4063(3) 0.0376(16) Uani 0.675(10) 1 d P B 1 H10A H 1.7505 0.1393 0.3695 0.045 Uiso 0.675(10) 1 calc PR B 1 H10B H 1.7416 0.2097 0.3993 0.045 Uiso 0.675(10) 1 calc PR B 1 C103 C 1.8324(8) 0.1434(6) 0.4534(5) 0.050(2) Uani 0.675(10) 1 d P B 1 H103 H 1.9017 0.1558 0.4405 0.060 Uiso 0.675(10) 1 calc PR B 1 C104 C 1.8188(8) 0.1796(4) 0.5102(4) 0.054(2) Uani 0.675(10) 1 d P B 1 H10C H 1.8208 0.2276 0.5039 0.065 Uiso 0.675(10) 1 calc PR B 1 H10D H 1.8775 0.1678 0.5407 0.065 Uiso 0.675(10) 1 calc PR B 1 C105 C 1.7118(9) 0.1600(5) 0.5298(4) 0.040(2) Uani 0.675(10) 1 d P B 1 H105 H 1.7038 0.1835 0.5668 0.048 Uiso 0.675(10) 1 calc PR B 1 C106 C 1.6221(7) 0.1805(4) 0.4838(3) 0.0347(17) Uani 0.675(10) 1 d P B 1 H10E H 1.6264 0.2282 0.4762 0.042 Uiso 0.675(10) 1 calc PR B 1 H10F H 1.5530 0.1713 0.4973 0.042 Uiso 0.675(10) 1 calc PR B 1 C107 C 1.6331(7) 0.0702(3) 0.4385(3) 0.0348(16) Uani 0.675(10) 1 d P B 1 H10G H 1.6399 0.0457 0.4024 0.042 Uiso 0.675(10) 1 calc PR B 1 H10H H 1.5653 0.0573 0.4519 0.042 Uiso 0.675(10) 1 calc PR B 1 C108 C 1.8302(8) 0.0693(5) 0.4649(4) 0.049(2) Uani 0.675(10) 1 d P B 1 H10I H 1.8384 0.0450 0.4289 0.059 Uiso 0.675(10) 1 calc PR B 1 H10J H 1.8894 0.0571 0.4949 0.059 Uiso 0.675(10) 1 calc PR B 1 C109 C 1.7089(18) 0.0887(11) 0.5402(9) 0.064(6) Uani 0.675(10) 1 d P B 1 H10K H 1.6396 0.0764 0.5521 0.077 Uiso 0.675(10) 1 calc PR B 1 H10L H 1.7652 0.0765 0.5719 0.077 Uiso 0.675(10) 1 calc PR B 1 C110 C 1.7256(9) 0.0520(4) 0.4852(4) 0.044(2) Uani 0.675(10) 1 d P B 1 H110 H 1.7238 0.0038 0.4927 0.053 Uiso 0.675(10) 1 calc PR B 1 C302 C 1.7193(12) 0.1165(11) 0.3953(7) 0.053(5) Uani 0.325(10) 1 d P B 2 H30A H 1.7468 0.1521 0.3724 0.064 Uiso 0.325(10) 1 calc PR B 2 H30B H 1.6945 0.0800 0.3688 0.064 Uiso 0.325(10) 1 calc PR B 2 C303 C 1.8070(15) 0.0923(16) 0.4446(9) 0.070(8) Uani 0.325(10) 1 d P B 2 H303 H 1.8703 0.0781 0.4265 0.084 Uiso 0.325(10) 1 calc PR B 2 C304 C 1.8379(17) 0.1467(14) 0.4838(13) 0.069(8) Uani 0.325(10) 1 d P B 2 H30C H 1.8646 0.1831 0.4616 0.083 Uiso 0.325(10) 1 calc PR B 2 H30D H 1.8962 0.1324 0.5136 0.083 Uiso 0.325(10) 1 calc PR B 2 C305 C 1.7444(15) 0.1717(12) 0.5143(12) 0.049(6) Uani 0.325(10) 1 d P B 2 H305 H 1.7650 0.2079 0.5425 0.058 Uiso 0.325(10) 1 calc PR B 2 C306 C 1.6560(13) 0.1920(10) 0.4644(9) 0.042(4) Uani 0.325(10) 1 d P B 2 H30E H 1.5916 0.2052 0.4812 0.050 Uiso 0.325(10) 1 calc PR B 2 H30F H 1.6804 0.2300 0.4433 0.050 Uiso 0.325(10) 1 calc PR B 2 C307 C 1.5801(12) 0.0753(7) 0.4522(7) 0.038(4) Uani 0.325(10) 1 d P B 2 H30G H 1.5143 0.0862 0.4687 0.045 Uiso 0.325(10) 1 calc PR B 2 H30H H 1.5640 0.0415 0.4217 0.045 Uiso 0.325(10) 1 calc PR B 2 C308 C 1.7646(17) 0.0341(10) 0.4738(8) 0.048(5) Uani 0.325(10) 1 d P B 2 H30I H 1.7472 -0.0014 0.4450 0.058 Uiso 0.325(10) 1 calc PR B 2 H30J H 1.8196 0.0174 0.5043 0.058 Uiso 0.325(10) 1 calc PR B 2 C309 C 1.698(3) 0.106(2) 0.5446(17) 0.063(14) Uani 0.325(10) 1 d P B 2 H30K H 1.7527 0.0898 0.5755 0.075 Uiso 0.325(10) 1 calc PR B 2 H30L H 1.6349 0.1188 0.5628 0.075 Uiso 0.325(10) 1 calc PR B 2 C310 C 1.6683(16) 0.0517(9) 0.5001(7) 0.046(4) Uani 0.325(10) 1 d P B 2 H310 H 1.6428 0.0125 0.5201 0.055 Uiso 0.325(10) 1 calc PR B 2 F33 F 1.175(5) 0.369(2) 0.4348(17) 0.065(8) Uani 0.48(12) 1 d P C 1 F34 F 1.208(2) 0.4656(15) 0.4536(18) 0.047(5) Uani 0.48(12) 1 d P C 1 F35 F 1.0602(19) 0.4488(14) 0.3893(16) 0.060(5) Uani 0.48(12) 1 d P C 1 F33A F 1.207(3) 0.4744(17) 0.4401(19) 0.058(4) Uani 0.52(12) 1 d PD C 2 F34A F 1.152(6) 0.3692(17) 0.4313(15) 0.064(9) Uani 0.52(12) 1 d PD C 2 F35A F 1.0609(17) 0.439(2) 0.400(2) 0.075(7) Uani 0.52(12) 1 d PD C 2 F13 F 1.0707(13) 0.0976(12) 0.4162(10) 0.051(4) Uani 0.50(9) 1 d P D 1 F14 F 0.9723(17) 0.0642(14) 0.3405(14) 0.048(4) Uani 0.50(9) 1 d PU D 1 F15 F 1.062(2) 0.0009(14) 0.3875(8) 0.062(5) Uani 0.50(9) 1 d P D 1 F13A F 0.9744(18) 0.0662(14) 0.3262(18) 0.055(5) Uani 0.50(9) 1 d PDU D 2 F14A F 1.0765(18) -0.0060(11) 0.3872(9) 0.059(5) Uani 0.50(9) 1 d PD D 2 F15A F 1.060(2) 0.1028(15) 0.4052(18) 0.081(7) Uani 0.50(9) 1 d PD D 2 C61 C 1.6172(8) 0.0587(5) 0.2276(5) 0.041(2) Uani 0.577(6) 1 d P E 1 H61A H 1.6169 0.0628 0.1852 0.049 Uiso 0.577(6) 1 calc PR E 1 H61B H 1.5570 0.0304 0.2347 0.049 Uiso 0.577(6) 1 calc PR E 1 C62 C 1.7211(10) 0.0278(5) 0.2548(5) 0.047(2) Uani 0.577(6) 1 d P E 1 F63 F 1.7325(6) -0.0290(3) 0.2285(3) 0.071(2) Uani 0.577(6) 1 d P E 1 F64 F 1.8018(5) 0.0654(4) 0.2432(3) 0.072(2) Uani 0.577(6) 1 d P E 1 F65 F 1.7292(5) 0.0208(3) 0.3093(2) 0.0634(18) Uani 0.577(6) 1 d P E 1 C61A C 1.5821(11) 0.0435(7) 0.2348(8) 0.042(4) Uani 0.423(6) 1 d P E 2 H61C H 1.5679 0.0180 0.2692 0.050 Uiso 0.423(6) 1 calc PR E 2 H61D H 1.5211 0.0393 0.2039 0.050 Uiso 0.423(6) 1 calc PR E 2 C62A C 1.6843(10) 0.0221(6) 0.2137(8) 0.053(3) Uani 0.423(6) 1 d P E 2 F63A F 1.7686(9) 0.0369(5) 0.2468(6) 0.0700(19) Uani 0.423(6) 1 d P E 2 F64A F 1.6790(7) -0.0433(4) 0.2040(5) 0.0700(19) Uani 0.423(6) 1 d P E 2 F65A F 1.6986(6) 0.0511(4) 0.1632(4) 0.0700(19) Uani 0.423(6) 1 d P E 2 C71 C 1.6505(6) 0.3771(4) 0.3610(4) 0.0345(7) Uani 0.562(5) 1 d PDU F 1 H71A H 1.6593 0.4143 0.3347 0.041 Uiso 0.562(5) 1 calc PR F 1 H71B H 1.5840 0.3834 0.3782 0.041 Uiso 0.562(5) 1 calc PR F 1 C72 C 1.7448(7) 0.3725(4) 0.4084(4) 0.046(2) Uani 0.562(5) 1 d PDU F 1 F73 F 1.7289(5) 0.3301(2) 0.4504(2) 0.0576(17) Uani 0.562(5) 1 d P F 1 F74 F 1.8357(5) 0.3538(4) 0.3901(3) 0.0568(18) Uani 0.562(5) 1 d P F 1 F75 F 1.7628(5) 0.4314(3) 0.4369(3) 0.0602(18) Uani 0.562(5) 1 d P F 1 C71A C 1.6776(7) 0.3611(5) 0.3567(5) 0.0345(7) Uani 0.438(5) 1 d PDU F 2 H71C H 1.6449 0.3612 0.3931 0.041 Uiso 0.438(5) 1 calc PR F 2 H71D H 1.6537 0.4009 0.3344 0.041 Uiso 0.438(5) 1 calc PR F 2 C72A C 1.7966(9) 0.3618(7) 0.3707(6) 0.052(3) Uani 0.438(5) 1 d PDU F 2 F73A F 1.8424(5) 0.3593(4) 0.3238(3) 0.064(2) Uani 0.438(5) 1 d P F 2 F74A F 1.8133(6) 0.4143(5) 0.4003(4) 0.073(3) Uani 0.438(5) 1 d P F 2 F75A F 1.8284(7) 0.3063(6) 0.4004(4) 0.083(3) Uani 0.438(5) 1 d P F 2 C21 C 1.2340(5) 0.2130(2) 0.4386(2) 0.0338(11) Uani 0.821(4) 1 d P G 1 H21A H 1.1555 0.2132 0.4323 0.041 Uiso 0.821(4) 1 calc PR G 1 H21B H 1.2593 0.2589 0.4393 0.041 Uiso 0.821(4) 1 calc PR G 1 C22 C 1.2730(5) 0.1797(3) 0.4940(2) 0.0442(13) Uani 0.821(4) 1 d PU G 1 F23 F 1.3813(4) 0.1878(2) 0.50589(17) 0.0686(7) Uani 0.821(4) 1 d PU G 1 F24 F 1.2555(5) 0.1172(3) 0.49442(18) 0.0686(7) Uani 0.821(4) 1 d PU G 1 F25 F 1.2327(4) 0.2073(2) 0.53759(15) 0.0686(7) Uani 0.821(4) 1 d P G 1 C21A C 1.315(3) 0.2018(12) 0.4442(9) 0.043(7) Uani 0.179(4) 1 d P G 2 H21C H 1.2660 0.2341 0.4578 0.052 Uiso 0.179(4) 1 calc PR G 2 H21D H 1.3818 0.2252 0.4390 0.052 Uiso 0.179(4) 1 calc PR G 2 C22A C 1.343(2) 0.1431(14) 0.4953(11) 0.0442(13) Uani 0.179(4) 1 d P G 2 F23A F 1.3750(17) 0.0930(10) 0.4713(7) 0.0686(7) Uani 0.179(4) 1 d P G 2 F24A F 1.3846(18) 0.1654(10) 0.5338(8) 0.0686(7) Uani 0.179(4) 1 d P G 2 F25A F 1.246(2) 0.1290(13) 0.5114(8) 0.0686(7) Uani 0.179(4) 1 d P G 2 O5 O 1.5032(7) 0.1466(4) 0.1575(3) 0.0421(17) Uani 0.548(7) 1 d PU H 1 C51 C 1.4564(11) 0.1824(7) 0.1095(6) 0.035(2) Uani 0.548(7) 1 d PDU H 1 H51A H 1.4714 0.2298 0.1145 0.042 Uiso 0.548(7) 1 calc PR H 1 H51B H 1.3787 0.1757 0.1031 0.042 Uiso 0.548(7) 1 calc PR H 1 C52 C 1.5110(11) 0.1529(6) 0.0567(7) 0.081(3) Uani 0.548(7) 1 d PDU H 1 F53 F 1.6141(6) 0.1645(4) 0.0667(3) 0.0757(16) Uani 0.548(7) 1 d PDU H 1 F54 F 1.4724(6) 0.1857(4) 0.0096(3) 0.0757(16) Uani 0.548(7) 1 d PD H 1 F55 F 1.4964(6) 0.0942(4) 0.0472(3) 0.0757(16) Uani 0.548(7) 1 d PDU H 1 O5A O 1.5396(6) 0.1715(4) 0.1610(3) 0.0294(16) Uani 0.452(7) 1 d PU H 2 C51A C 1.4530(15) 0.1653(10) 0.1169(11) 0.074(6) Uani 0.452(7) 1 d PDU H 2 H51C H 1.4005 0.1351 0.1304 0.089 Uiso 0.452(7) 1 calc PR H 2 H51D H 1.4186 0.2087 0.1104 0.089 Uiso 0.452(7) 1 calc PR H 2 C52A C 1.4777(11) 0.1437(7) 0.0672(8) 0.081(3) Uani 0.452(7) 1 d PDU H 2 F53A F 1.3924(9) 0.1361(5) 0.0266(4) 0.112(3) Uani 0.452(7) 1 d PDU H 2 F54A F 1.5417(10) 0.1896(5) 0.0441(4) 0.112(3) Uani 0.452(7) 1 d PDU H 2 F55A F 1.5361(10) 0.0893(6) 0.0683(4) 0.112(3) Uani 0.452(7) 1 d PDU H 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01904(11) 0.01659(12) 0.01667(11) 0.00231(9) 0.00109(8) 0.00260(9) Rh2 0.02818(13) 0.01634(12) 0.01917(12) 0.00093(10) 0.00185(10) 0.00632(10) Cl1 0.0510(6) 0.0174(4) 0.0504(6) -0.0022(4) 0.0025(5) 0.0073(4) Cl2 0.0333(4) 0.0181(4) 0.0305(4) 0.0030(3) 0.0065(3) -0.0013(3) Cl3 0.0330(4) 0.0228(4) 0.0180(3) -0.0007(3) -0.0023(3) -0.0012(3) Cl4 0.0291(4) 0.0270(4) 0.0192(4) 0.0032(3) 0.0029(3) 0.0063(3) P1 0.0246(4) 0.0173(4) 0.0190(4) -0.0003(3) -0.0007(3) -0.0009(3) P2 0.0196(4) 0.0154(4) 0.0205(4) -0.0015(3) 0.0021(3) 0.0019(3) P3 0.0483(6) 0.0370(6) 0.0341(6) 0.0111(5) 0.0182(5) 0.0266(5) P4 0.0202(4) 0.0356(6) 0.0440(6) 0.0214(5) 0.0072(4) 0.0080(4) N1 0.0295(11) 0.0278(12) 0.0541(16) 0.0164(11) 0.0202(11) 0.0106(9) N2 0.0295(11) 0.0278(12) 0.0541(16) 0.0164(11) 0.0202(11) 0.0106(9) N3 0.0377(17) 0.0269(16) 0.0293(17) 0.0013(13) 0.0027(14) 0.0082(13) N4 0.0402(17) 0.0225(15) 0.0206(14) -0.0013(12) 0.0011(13) 0.0056(12) O1 0.0326(13) 0.0209(12) 0.0302(14) 0.0013(10) -0.0047(11) -0.0061(10) O2 0.0489(16) 0.0296(14) 0.0203(12) -0.0014(11) -0.0028(11) 0.0079(12) O3 0.0262(12) 0.0214(12) 0.0329(14) -0.0080(10) 0.0052(10) 0.0042(9) O4 0.0254(11) 0.0202(12) 0.0279(13) 0.0019(10) -0.0021(10) 0.0034(9) O6 0.0517(18) 0.0345(16) 0.0452(18) 0.0069(13) 0.0135(14) 0.0264(14) O7 0.0234(13) 0.069(2) 0.065(2) 0.0408(17) -0.0062(14) -0.0011(14) O8 0.0220(12) 0.0404(16) 0.0497(18) 0.0216(14) 0.0078(12) 0.0055(11) F43 0.0586(18) 0.0386(15) 0.079(2) -0.0097(14) -0.0394(16) 0.0091(13) F44 0.0410(15) 0.070(2) 0.067(2) 0.0073(16) 0.0143(14) 0.0254(14) F45 0.0559(16) 0.0397(15) 0.0568(17) 0.0100(13) -0.0147(13) 0.0210(12) F83 0.0264(12) 0.0700(19) 0.0508(16) 0.0045(14) 0.0152(11) 0.0038(12) F84 0.0468(14) 0.0535(17) 0.0381(14) 0.0092(12) 0.0145(11) 0.0136(12) F85 0.0570(17) 0.0338(15) 0.080(2) -0.0077(14) 0.0209(16) 0.0051(12) C1 0.0242(18) 0.032(2) 0.060(3) 0.0120(19) 0.0129(18) 0.0008(15) C2 0.018(4) 0.029(5) 0.042(8) -0.006(5) 0.007(4) 0.001(3) C2A 0.029(5) 0.039(6) 0.051(8) 0.003(6) 0.016(5) 0.010(4) C11 0.044(2) 0.0191(18) 0.038(2) 0.0020(15) -0.0006(17) -0.0076(15) C12 0.044(2) 0.039(3) 0.050(3) -0.001(2) 0.003(2) -0.0204(19) C31 0.0352(19) 0.0187(17) 0.035(2) -0.0071(14) 0.0078(16) -0.0018(14) C32 0.063(3) 0.035(2) 0.044(3) -0.014(2) 0.023(2) -0.009(2) C41 0.0297(18) 0.029(2) 0.034(2) 0.0108(16) 0.0010(15) 0.0064(14) C42 0.035(2) 0.030(2) 0.040(2) -0.0015(17) -0.0083(17) 0.0100(16) C81 0.0189(14) 0.0399(19) 0.0443(18) 0.0148(15) 0.0034(13) 0.0039(12) C82 0.0272(18) 0.035(2) 0.048(3) 0.0071(18) 0.0099(17) 0.0048(15) C100 0.0391(19) 0.0175(16) 0.0201(16) 0.0006(12) 0.0052(14) 0.0010(13) C101 0.042(2) 0.037(2) 0.0240(18) 0.0031(16) -0.0058(16) 0.0170(17) C200 0.042(2) 0.0160(16) 0.0209(16) -0.0012(13) 0.0055(14) 0.0079(14) C201 0.044(2) 0.0201(17) 0.0205(16) -0.0020(13) -0.0057(15) 0.0029(15) C202 0.045(2) 0.028(2) 0.031(2) -0.0013(16) -0.0016(17) 0.0060(17) C203 0.045(2) 0.034(2) 0.047(3) -0.0027(19) -0.004(2) 0.0025(18) C204 0.056(3) 0.032(2) 0.055(3) -0.006(2) -0.003(2) -0.003(2) C205 0.068(3) 0.027(2) 0.048(3) -0.0152(19) -0.002(2) 0.001(2) C206 0.054(3) 0.0224(19) 0.035(2) -0.0048(16) 0.0020(19) 0.0057(17) C207 0.058(3) 0.031(2) 0.0243(19) 0.0040(16) -0.0038(18) 0.0009(19) C208 0.054(3) 0.042(3) 0.045(3) 0.000(2) -0.016(2) 0.003(2) C209 0.077(4) 0.062(3) 0.037(3) -0.023(2) -0.008(2) -0.007(3) C210 0.071(3) 0.046(3) 0.024(2) 0.0024(18) -0.016(2) 0.001(2) C102 0.040(3) 0.030(4) 0.039(4) 0.002(3) -0.009(3) -0.001(3) C103 0.040(4) 0.049(5) 0.053(6) 0.005(5) -0.022(4) 0.006(3) C104 0.056(6) 0.054(5) 0.042(4) -0.015(4) -0.032(4) 0.018(4) C105 0.046(6) 0.036(6) 0.033(4) -0.002(4) -0.017(4) 0.009(4) C106 0.044(4) 0.029(4) 0.028(4) -0.011(3) -0.011(3) 0.016(3) C107 0.046(4) 0.031(3) 0.027(3) -0.001(2) 0.001(3) 0.004(3) C108 0.062(6) 0.043(5) 0.038(4) -0.003(3) -0.009(4) 0.027(4) C109 0.100(12) 0.063(7) 0.026(8) 0.006(6) -0.007(6) 0.031(6) C110 0.064(6) 0.030(4) 0.035(4) 0.003(3) -0.002(4) 0.021(4) C302 0.041(8) 0.084(15) 0.035(8) 0.018(8) 0.007(6) 0.029(9) C303 0.042(10) 0.12(2) 0.053(12) 0.041(14) 0.017(8) 0.036(12) C304 0.036(9) 0.09(2) 0.072(17) 0.021(17) -0.018(12) 0.021(10) C305 0.024(10) 0.029(9) 0.087(19) 0.009(10) -0.017(9) 0.003(7) C306 0.030(8) 0.048(10) 0.046(11) -0.001(8) 0.002(6) 0.007(6) C307 0.032(7) 0.034(7) 0.040(8) 0.010(6) -0.015(6) -0.007(6) C308 0.056(11) 0.046(11) 0.037(9) -0.001(7) -0.012(7) 0.036(9) C309 0.040(11) 0.14(4) 0.011(8) -0.017(19) -0.003(7) 0.003(17) C310 0.061(11) 0.045(9) 0.029(8) 0.022(7) -0.006(7) 0.005(8) F33 0.090(17) 0.056(9) 0.052(9) 0.003(7) 0.020(8) -0.026(7) F34 0.079(7) 0.042(7) 0.023(8) -0.013(6) 0.022(6) -0.005(6) F35 0.064(8) 0.045(9) 0.080(11) -0.016(7) 0.051(7) 0.010(6) F33A 0.106(8) 0.049(7) 0.026(9) -0.019(6) 0.036(7) -0.030(6) F34A 0.11(3) 0.048(7) 0.041(8) -0.008(6) 0.044(13) -0.028(9) F35A 0.051(7) 0.101(15) 0.079(13) -0.044(12) 0.033(6) -0.018(8) F13 0.037(7) 0.078(8) 0.038(6) -0.003(6) 0.012(5) -0.026(5) F14 0.030(4) 0.060(6) 0.050(9) 0.014(6) -0.007(5) -0.011(4) F15 0.082(10) 0.057(9) 0.049(8) 0.006(7) 0.024(8) -0.036(7) F13A 0.047(5) 0.053(7) 0.062(12) -0.001(7) 0.002(6) -0.029(4) F14A 0.056(6) 0.041(6) 0.070(10) 0.034(7) -0.032(8) -0.029(5) F15A 0.107(13) 0.083(11) 0.064(11) -0.045(9) 0.053(9) -0.070(9) C61 0.037(5) 0.027(5) 0.057(6) -0.007(4) -0.001(4) 0.010(4) C62 0.060(6) 0.042(5) 0.044(5) 0.010(4) 0.031(5) 0.019(4) F63 0.102(5) 0.050(4) 0.060(4) -0.010(3) 0.004(3) 0.054(4) F64 0.038(3) 0.078(5) 0.105(5) 0.032(4) 0.032(3) 0.021(3) F65 0.096(4) 0.050(3) 0.046(3) 0.009(2) 0.015(3) 0.038(3) C61A 0.035(7) 0.015(6) 0.083(10) 0.003(5) 0.036(6) 0.005(4) C62A 0.041(6) 0.033(6) 0.090(12) 0.007(7) 0.025(7) 0.011(5) F63A 0.065(3) 0.041(3) 0.112(5) -0.004(3) 0.042(3) 0.009(2) F64A 0.065(3) 0.041(3) 0.112(5) -0.004(3) 0.042(3) 0.009(2) F65A 0.065(3) 0.041(3) 0.112(5) -0.004(3) 0.042(3) 0.009(2) C71 0.0189(14) 0.0399(19) 0.0443(18) 0.0148(15) 0.0034(13) 0.0039(12) C72 0.043(4) 0.034(4) 0.057(5) 0.012(4) -0.006(4) -0.003(3) F73 0.089(4) 0.037(3) 0.040(3) 0.011(2) -0.016(3) -0.012(3) F74 0.029(3) 0.060(4) 0.075(5) 0.006(4) -0.017(3) 0.006(3) F75 0.071(4) 0.038(3) 0.063(4) -0.006(3) -0.027(3) -0.010(3) C71A 0.0189(14) 0.0399(19) 0.0443(18) 0.0148(15) 0.0034(13) 0.0039(12) C72A 0.030(5) 0.067(9) 0.055(8) 0.024(6) -0.005(5) 0.008(5) F73A 0.026(3) 0.087(6) 0.080(6) 0.009(4) 0.014(3) -0.001(3) F74A 0.047(4) 0.111(8) 0.055(5) -0.006(5) -0.018(4) -0.032(5) F75A 0.060(5) 0.099(8) 0.078(6) 0.038(5) -0.036(4) -0.001(5) C21 0.050(3) 0.025(2) 0.027(2) -0.0020(18) 0.009(2) -0.002(2) C22 0.066(4) 0.041(3) 0.026(2) -0.001(2) 0.009(2) -0.012(3) F23 0.1063(18) 0.0680(16) 0.0340(13) 0.0052(11) 0.0181(12) -0.0080(13) F24 0.1063(18) 0.0680(16) 0.0340(13) 0.0052(11) 0.0181(12) -0.0080(13) F25 0.1063(18) 0.0680(16) 0.0340(13) 0.0052(11) 0.0181(12) -0.0080(13) C21A 0.08(2) 0.030(12) 0.010(9) 0.007(8) -0.013(11) -0.026(13) C22A 0.066(4) 0.041(3) 0.026(2) -0.001(2) 0.009(2) -0.012(3) F23A 0.1063(18) 0.0680(16) 0.0340(13) 0.0052(11) 0.0181(12) -0.0080(13) F24A 0.1063(18) 0.0680(16) 0.0340(13) 0.0052(11) 0.0181(12) -0.0080(13) F25A 0.1063(18) 0.0680(16) 0.0340(13) 0.0052(11) 0.0181(12) -0.0080(13) O5 0.053(5) 0.041(4) 0.035(3) -0.004(3) 0.014(3) 0.012(3) C51 0.035(5) 0.039(5) 0.030(4) -0.005(3) -0.003(3) 0.009(4) C52 0.119(7) 0.072(5) 0.043(4) -0.016(4) -0.019(4) 0.030(5) F53 0.089(3) 0.096(3) 0.043(2) -0.013(2) 0.0105(19) 0.025(2) F54 0.089(3) 0.096(3) 0.043(2) -0.013(2) 0.0105(19) 0.025(2) F55 0.089(3) 0.096(3) 0.043(2) -0.013(2) 0.0105(19) 0.025(2) O5A 0.028(4) 0.034(4) 0.026(3) -0.008(3) 0.003(3) -0.001(3) C51A 0.050(9) 0.104(16) 0.062(8) -0.019(8) -0.019(5) 0.043(9) C52A 0.119(7) 0.072(5) 0.043(4) -0.016(4) -0.019(4) 0.030(5) F53A 0.166(7) 0.108(5) 0.056(4) -0.027(3) -0.012(3) 0.015(4) F54A 0.166(7) 0.108(5) 0.056(4) -0.027(3) -0.012(3) 0.015(4) F55A 0.166(7) 0.108(5) 0.056(4) -0.027(3) -0.012(3) 0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 P2 2.2730(8) . ? Rh1 P4 2.2822(10) . ? Rh1 Cl4 2.3519(9) . ? Rh1 Cl3 2.3624(8) . ? Rh1 Cl2 2.4468(9) . ? Rh1 Rh2 2.7137(4) . ? Rh2 C200 1.983(4) . ? Rh2 C100 1.990(4) . ? Rh2 P1 2.2738(9) . ? Rh2 P3 2.2986(11) . ? Rh2 Cl1 2.4862(10) . ? P1 O2 1.589(3) . ? P1 O1 1.603(3) . ? P1 N1 1.669(3) . ? P2 O3 1.598(2) . ? P2 O4 1.602(2) . ? P2 N1 1.678(3) . ? P3 O5A 1.549(8) . ? P3 O6 1.606(3) . ? P3 N2 1.662(4) . ? P3 O5 1.686(7) . ? P4 O8 1.599(3) . ? P4 O7 1.615(3) . ? P4 N2 1.665(4) . ? N1 C1 1.494(5) . ? N2 C2A 1.479(10) . ? N2 C2 1.568(11) . ? N3 C100 1.133(5) . ? N3 C101 1.451(5) . ? N4 C200 1.144(5) . ? N4 C201 1.458(5) . ? O1 C11 1.433(4) . ? O2 C21A 1.30(2) . ? O2 C21 1.397(5) . ? O3 C31 1.426(4) . ? O4 C41 1.430(4) . ? O6 C61 1.344(10) . ? O6 C61A 1.590(14) . ? O7 C71A 1.295(11) . ? O7 C71 1.593(9) . ? O8 C81 1.427(5) . ? F43 C42 1.329(5) . ? F44 C42 1.329(5) . ? F45 C42 1.337(5) . ? F83 C82 1.336(4) . ? F84 C82 1.336(5) . ? F85 C82 1.345(5) . ? C11 C12 1.479(6) . ? C12 F14 1.27(2) . ? C12 F15 1.27(3) . ? C12 F15A 1.29(2) . ? C12 F14A 1.40(2) . ? C12 F13A 1.41(3) . ? C12 F13 1.41(2) . ? C31 C32 1.480(6) . ? C32 F35A 1.30(2) . ? C32 F33A 1.31(3) . ? C32 F34A 1.33(3) . ? C32 F33 1.36(4) . ? C32 F35 1.38(3) . ? C32 F34 1.39(3) . ? C41 C42 1.497(5) . ? C81 C82 1.494(6) . ? C101 C306 1.37(2) . ? C101 C107 1.466(8) . ? C101 C302 1.487(15) . ? C101 C106 1.577(8) . ? C101 C102 1.582(8) . ? C101 C307 1.638(15) . ? C201 C207 1.525(5) . ? C201 C202 1.536(6) . ? C201 C206 1.536(5) . ? C202 C203 1.539(6) . ? C203 C204 1.527(6) . ? C203 C208 1.527(7) . ? C204 C205 1.512(7) . ? C205 C206 1.536(6) . ? C205 C209 1.538(7) . ? C207 C210 1.532(6) . ? C208 C210 1.517(8) . ? C209 C210 1.542(7) . ? C102 C103 1.535(10) . ? C103 C108 1.534(13) . ? C103 C104 1.540(13) . ? C104 C105 1.543(14) . ? C105 C109 1.48(2) . ? C105 C106 1.517(12) . ? C107 C110 1.537(11) . ? C108 C110 1.510(14) . ? C109 C110 1.52(2) . ? C302 C303 1.57(2) . ? C303 C304 1.46(4) . ? C303 C308 1.50(3) . ? C304 C305 1.55(3) . ? C305 C306 1.56(3) . ? C305 C309 1.65(5) . ? C307 C310 1.550(19) . ? C308 C310 1.48(3) . ? C309 C310 1.53(4) . ? C61 C62 1.525(15) . ? C62 F65 1.265(11) . ? C62 F63 1.326(11) . ? C62 F64 1.337(12) . ? C61A C62A 1.513(17) . ? C62A F63A 1.272(19) . ? C62A F65A 1.348(18) . ? C62A F64A 1.353(15) . ? C71 C72 1.522(10) . ? C72 F74 1.339(11) . ? C72 F73 1.339(10) . ? C72 F75 1.374(10) . ? C71A C72A 1.507(12) . ? C72A F74A 1.275(17) . ? C72A F73A 1.303(16) . ? C72A F75A 1.360(15) . ? C21 C22 1.483(8) . ? C22 F24 1.293(8) . ? C22 F25 1.319(7) . ? C22 F23 1.380(8) . ? C21A C22A 1.69(3) . ? C22A F24A 1.08(3) . ? C22A F23A 1.26(3) . ? C22A F25A 1.36(4) . ? O5 C51 1.399(15) . ? C51 C52 1.60(2) . ? C52 F55 1.226(12) . ? C52 F54 1.322(12) . ? C52 F53 1.323(12) . ? O5A C51A 1.41(2) . ? C51A C52A 1.31(3) . ? C52A F55A 1.333(15) . ? C52A F53A 1.351(14) . ? C52A F54A 1.394(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Rh1 P4 179.36(4) . . ? P2 Rh1 Cl4 91.72(3) . . ? P4 Rh1 Cl4 88.92(4) . . ? P2 Rh1 Cl3 86.62(3) . . ? P4 Rh1 Cl3 92.74(4) . . ? Cl4 Rh1 Cl3 178.27(3) . . ? P2 Rh1 Cl2 91.35(3) . . ? P4 Rh1 Cl2 88.66(4) . . ? Cl4 Rh1 Cl2 90.06(3) . . ? Cl3 Rh1 Cl2 90.48(3) . . ? P2 Rh1 Rh2 90.38(2) . . ? P4 Rh1 Rh2 89.62(3) . . ? Cl4 Rh1 Rh2 88.51(2) . . ? Cl3 Rh1 Rh2 91.00(2) . . ? Cl2 Rh1 Rh2 177.78(2) . . ? C200 Rh2 C100 173.69(15) . . ? C200 Rh2 P1 84.62(11) . . ? C100 Rh2 P1 93.22(11) . . ? C200 Rh2 P3 99.57(11) . . ? C100 Rh2 P3 82.74(11) . . ? P1 Rh2 P3 175.62(4) . . ? C200 Rh2 Cl1 84.51(10) . . ? C100 Rh2 Cl1 89.68(10) . . ? P1 Rh2 Cl1 93.01(4) . . ? P3 Rh2 Cl1 88.69(4) . . ? C200 Rh2 Rh1 92.72(10) . . ? C100 Rh2 Rh1 93.14(10) . . ? P1 Rh2 Rh1 88.18(2) . . ? P3 Rh2 Rh1 90.33(3) . . ? Cl1 Rh2 Rh1 176.87(3) . . ? O2 P1 O1 102.37(15) . . ? O2 P1 N1 109.15(17) . . ? O1 P1 N1 98.21(16) . . ? O2 P1 Rh2 113.86(12) . . ? O1 P1 Rh2 114.78(11) . . ? N1 P1 Rh2 116.57(12) . . ? O3 P2 O4 97.15(13) . . ? O3 P2 N1 103.06(16) . . ? O4 P2 N1 98.73(17) . . ? O3 P2 Rh1 121.07(10) . . ? O4 P2 Rh1 118.29(10) . . ? N1 P2 Rh1 114.81(11) . . ? O5A P3 O6 99.4(3) . . ? O5A P3 N2 93.0(3) . . ? O6 P3 N2 97.76(18) . . ? O5A P3 O5 23.9(3) . . ? O6 P3 O5 96.4(3) . . ? N2 P3 O5 116.9(3) . . ? O5A P3 Rh2 132.7(3) . . ? O6 P3 Rh2 112.84(13) . . ? N2 P3 Rh2 114.66(13) . . ? O5 P3 Rh2 115.1(3) . . ? O8 P4 O7 96.30(16) . . ? O8 P4 N2 103.08(17) . . ? O7 P4 N2 99.86(19) . . ? O8 P4 Rh1 120.10(10) . . ? O7 P4 Rh1 117.21(14) . . ? N2 P4 Rh1 116.59(13) . . ? C1 N1 P1 122.9(3) . . ? C1 N1 P2 118.7(2) . . ? P1 N1 P2 117.95(19) . . ? C2A N2 C2 25.5(5) . . ? C2A N2 P3 109.9(9) . . ? C2 N2 P3 128.6(6) . . ? C2A N2 P4 130.2(9) . . ? C2 N2 P4 110.6(7) . . ? P3 N2 P4 119.53(19) . . ? C100 N3 C101 175.3(4) . . ? C200 N4 C201 169.4(4) . . ? C11 O1 P1 123.2(2) . . ? C21A O2 C21 45.7(15) . . ? C21A O2 P1 148.4(10) . . ? C21 O2 P1 125.6(3) . . ? C31 O3 P2 129.8(2) . . ? C41 O4 P2 121.0(2) . . ? C61 O6 C61A 20.9(6) . . ? C61 O6 P3 127.0(5) . . ? C61A O6 P3 120.8(7) . . ? C71A O7 C71 15.7(4) . . ? C71A O7 P4 126.7(5) . . ? C71 O7 P4 115.3(3) . . ? C81 O8 P4 127.5(2) . . ? O1 C11 C12 107.8(4) . . ? F14 C12 F15 101(2) . . ? F14 C12 F15A 97.1(19) . . ? F15 C12 F15A 111(2) . . ? F14 C12 F14A 107.0(16) . . ? F15 C12 F14A 8.5(19) . . ? F15A C12 F14A 115(3) . . ? F14 C12 F13A 13(2) . . ? F15 C12 F13A 107(2) . . ? F15A C12 F13A 105.1(19) . . ? F14A C12 F13A 111.8(15) . . ? F14 C12 F13 105.5(17) . . ? F15 C12 F13 101.6(15) . . ? F15A C12 F13 11(3) . . ? F14A C12 F13 104.8(15) . . ? F13A C12 F13 114.8(16) . . ? F14 C12 C11 119.4(16) . . ? F15 C12 C11 114.7(14) . . ? F15A C12 C11 112.1(10) . . ? F14A C12 C11 106.3(12) . . ? F13A C12 C11 106.0(17) . . ? F13 C12 C11 112.9(8) . . ? O3 C31 C32 108.3(3) . . ? F35A C32 F33A 106.8(17) . . ? F35A C32 F34A 93(5) . . ? F33A C32 F34A 118(4) . . ? F35A C32 F33 106(4) . . ? F33A C32 F33 110(3) . . ? F34A C32 F33 13(5) . . ? F35A C32 F35 13(3) . . ? F33A C32 F35 105(2) . . ? F34A C32 F35 105(4) . . ? F33 C32 F35 118(3) . . ? F35A C32 F34 107.8(15) . . ? F33A C32 F34 14.8(15) . . ? F34A C32 F34 103(3) . . ? F33 C32 F34 96(3) . . ? F35 C32 F34 109.6(15) . . ? F35A C32 C31 119(2) . . ? F33A C32 C31 105.2(15) . . ? F34A C32 C31 115.2(16) . . ? F33 C32 C31 109.7(19) . . ? F35 C32 C31 107.6(16) . . ? F34 C32 C31 115.7(18) . . ? O4 C41 C42 106.4(3) . . ? F44 C42 F43 107.1(4) . . ? F44 C42 F45 107.0(3) . . ? F43 C42 F45 107.2(3) . . ? F44 C42 C41 112.2(3) . . ? F43 C42 C41 112.6(3) . . ? F45 C42 C41 110.4(4) . . ? O8 C81 C82 108.7(3) . . ? F84 C82 F83 107.0(3) . . ? F84 C82 F85 107.4(4) . . ? F83 C82 F85 106.9(3) . . ? F84 C82 C81 110.2(3) . . ? F83 C82 C81 113.2(4) . . ? F85 C82 C81 112.0(4) . . ? N3 C100 Rh2 172.6(3) . . ? C306 C101 N3 110.0(8) . . ? C306 C101 C107 129.0(9) . . ? N3 C101 C107 112.6(4) . . ? C306 C101 C302 116.8(11) . . ? N3 C101 C302 105.1(6) . . ? C107 C101 C302 77.2(9) . . ? C306 C101 C106 26.4(7) . . ? N3 C101 C106 109.9(4) . . ? C107 C101 C106 110.2(5) . . ? C302 C101 C106 137.0(9) . . ? C306 C101 C102 81.7(8) . . ? N3 C101 C102 107.7(4) . . ? C107 C101 C102 109.8(5) . . ? C302 C101 C102 37.4(9) . . ? C106 C101 C102 106.4(5) . . ? C306 C101 C307 116.9(10) . . ? N3 C101 C307 100.6(5) . . ? C107 C101 C307 28.8(6) . . ? C302 C101 C307 105.7(10) . . ? C106 C101 C307 91.8(7) . . ? C102 C101 C307 138.0(7) . . ? N4 C200 Rh2 167.4(3) . . ? N4 C201 C207 110.2(3) . . ? N4 C201 C202 108.2(3) . . ? C207 C201 C202 110.1(3) . . ? N4 C201 C206 107.2(3) . . ? C207 C201 C206 111.0(3) . . ? C202 C201 C206 110.0(3) . . ? C201 C202 C203 108.3(3) . . ? C204 C203 C208 110.2(4) . . ? C204 C203 C202 108.9(4) . . ? C208 C203 C202 108.9(4) . . ? C205 C204 C203 110.2(4) . . ? C204 C205 C206 109.8(4) . . ? C204 C205 C209 109.9(4) . . ? C206 C205 C209 108.4(4) . . ? C205 C206 C201 108.2(3) . . ? C201 C207 C210 108.2(4) . . ? C210 C208 C203 110.1(4) . . ? C205 C209 C210 109.8(4) . . ? C208 C210 C207 109.7(4) . . ? C208 C210 C209 109.3(5) . . ? C207 C210 C209 109.2(4) . . ? C103 C102 C101 109.3(6) . . ? C108 C103 C102 109.6(8) . . ? C108 C103 C104 108.4(8) . . ? C102 C103 C104 109.6(7) . . ? C103 C104 C105 109.3(8) . . ? C109 C105 C106 110.8(11) . . ? C109 C105 C104 110.1(12) . . ? C106 C105 C104 109.4(8) . . ? C105 C106 C101 108.4(6) . . ? C101 C107 C110 110.9(6) . . ? C110 C108 C103 108.7(7) . . ? C105 C109 C110 109.7(15) . . ? C108 C110 C109 111.9(12) . . ? C108 C110 C107 110.4(7) . . ? C109 C110 C107 107.3(10) . . ? C101 C302 C303 104.5(12) . . ? C304 C303 C308 113.8(18) . . ? C304 C303 C302 109(2) . . ? C308 C303 C302 108.4(17) . . ? C303 C304 C305 112.1(19) . . ? C304 C305 C306 105.7(19) . . ? C304 C305 C309 105(2) . . ? C306 C305 C309 105.6(17) . . ? C101 C306 C305 110.6(15) . . ? C310 C307 C101 103.0(10) . . ? C310 C308 C303 111.0(15) . . ? C310 C309 C305 112(3) . . ? C308 C310 C309 108(2) . . ? C308 C310 C307 109.8(14) . . ? C309 C310 C307 110.6(19) . . ? O6 C61 C62 109.7(8) . . ? F65 C62 F63 111.2(8) . . ? F65 C62 F64 107.6(11) . . ? F63 C62 F64 105.9(8) . . ? F65 C62 C61 114.5(8) . . ? F63 C62 C61 108.2(10) . . ? F64 C62 C61 109.1(8) . . ? C62A C61A O6 101.9(9) . . ? F63A C62A F65A 102.9(11) . . ? F63A C62A F64A 110.8(11) . . ? F65A C62A F64A 107.3(13) . . ? F63A C62A C61A 115.3(16) . . ? F65A C62A C61A 112.0(11) . . ? F64A C62A C61A 108.2(10) . . ? C72 C71 O7 105.9(6) . . ? F74 C72 F73 105.5(7) . . ? F74 C72 F75 107.8(7) . . ? F73 C72 F75 104.1(7) . . ? F74 C72 C71 114.8(8) . . ? F73 C72 C71 112.7(7) . . ? F75 C72 C71 111.1(7) . . ? O7 C71A C72A 109.9(9) . . ? F74A C72A F73A 115.0(11) . . ? F74A C72A F75A 114.1(12) . . ? F73A C72A F75A 104.8(12) . . ? F74A C72A C71A 102.6(11) . . ? F73A C72A C71A 111.5(10) . . ? F75A C72A C71A 109.1(10) . . ? O2 C21 C22 107.0(4) . . ? F24 C22 F25 109.3(5) . . ? F24 C22 F23 106.6(6) . . ? F25 C22 F23 105.9(5) . . ? F24 C22 C21 114.7(5) . . ? F25 C22 C21 110.6(5) . . ? F23 C22 C21 109.3(5) . . ? O2 C21A C22A 112.4(18) . . ? F24A C22A F23A 124(3) . . ? F24A C22A F25A 103(3) . . ? F23A C22A F25A 108(2) . . ? F24A C22A C21A 109(2) . . ? F23A C22A C21A 108(2) . . ? F25A C22A C21A 104(2) . . ? C51 O5 P3 125.2(8) . . ? O5 C51 C52 103.4(10) . . ? F55 C52 F54 108.2(11) . . ? F55 C52 F53 109.2(12) . . ? F54 C52 F53 108.0(11) . . ? F55 C52 C51 115.6(12) . . ? F54 C52 C51 107.0(10) . . ? F53 C52 C51 108.5(10) . . ? C51A O5A P3 122.4(12) . . ? C52A C51A O5A 114.6(16) . . ? C51A C52A F55A 117.4(13) . . ? C51A C52A F53A 113.0(13) . . ? F55A C52A F53A 108.2(13) . . ? C51A C52A F54A 109.5(13) . . ? F55A C52A F54A 102.3(13) . . ? F53A C52A F54A 105.3(12) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.933 _refine_diff_density_min -1.697 _refine_diff_density_rms 0.114 data_Compound_6 _database_code_depnum_ccdc_archive 'CCDC 925035' #TrackingRef '17866_web_deposit_cif_file_0_DavidPowers_1361207103.Cif Files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H26 Cl2 F25 N3 O8 P4 Rh2' _chemical_formula_weight 1372.09 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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.1595(9) _cell_length_b 10.3860(10) _cell_length_c 12.0283(11) _cell_angle_alpha 73.962(2) _cell_angle_beta 69.0490(10) _cell_angle_gamma 71.477(2) _cell_volume 1104.74(18) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9899 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 30.53 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 670 _exptl_absorpt_coefficient_mu 1.166 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8002 _exptl_absorpt_correction_T_max 0.8923 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25891 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 30.55 _reflns_number_total 12490 _reflns_number_gt 11183 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0363P)^2^+0.4071P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.676(17) _refine_ls_number_reflns 12490 _refine_ls_number_parameters 625 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.15639(2) 1.23117(3) 0.33596(2) 0.01461(7) Uani 1 1 d . . . Rh2 Rh -0.10878(2) 1.18087(2) 0.41426(2) 0.01477(7) Uani 1 1 d . . . P4 P -0.10416(12) 1.11001(11) 0.60987(10) 0.0135(2) Uani 1 1 d . . . P2 P -0.13278(12) 1.25250(11) 0.22452(10) 0.0131(2) Uani 1 1 d . . . P1 P 0.14407(12) 1.31837(11) 0.14305(10) 0.0133(2) Uani 1 1 d . . . P3 P 0.17224(12) 1.17731(12) 0.52775(10) 0.0138(2) Uani 1 1 d . . . Cl1 Cl 0.37288(11) 1.30344(11) 0.27116(8) 0.01839(19) Uani 1 1 d . . . O6 O 0.3235(3) 1.0809(3) 0.5482(3) 0.0148(6) Uani 1 1 d . . . O4 O -0.2818(3) 1.3590(3) 0.2096(3) 0.0176(6) Uani 1 1 d . . . O8 O -0.2371(3) 1.1913(3) 0.7080(3) 0.0183(6) Uani 1 1 d . . . N1 N -0.0041(4) 1.3174(4) 0.1136(3) 0.0157(7) Uani 1 1 d . . . N2 N 0.0463(4) 1.1075(4) 0.6378(3) 0.0183(8) Uani 1 1 d . . . O2 O 0.2781(3) 1.2564(3) 0.0355(3) 0.0179(6) Uani 1 1 d . . . O1 O 0.1420(3) 1.4791(3) 0.0941(3) 0.0163(6) Uani 1 1 d . . . O7 O -0.1151(3) 0.9569(3) 0.6762(3) 0.0162(6) Uani 1 1 d . . . O3 O -0.1363(3) 1.1371(3) 0.1617(3) 0.0179(6) Uani 1 1 d . . . O5 O 0.1607(3) 1.3039(3) 0.5866(3) 0.0175(6) Uani 1 1 d . . . C71 C -0.2446(5) 0.9097(4) 0.7070(4) 0.0166(8) Uani 1 1 d . . . H71A H -0.2443 0.8723 0.6395 0.020 Uiso 1 1 calc R . . H71B H -0.3322 0.9866 0.7243 0.020 Uiso 1 1 calc R . . C11 C 0.2667(5) 1.5343(5) 0.0514(4) 0.0195(9) Uani 1 1 d . . . H11A H 0.3563 1.4610 0.0286 0.023 Uiso 1 1 calc R . . H11B H 0.2725 1.5736 0.1152 0.023 Uiso 1 1 calc R . . C31 C -0.2539(5) 1.0697(4) 0.2110(4) 0.0168(8) Uani 1 1 d . . . H31A H -0.3474 1.1363 0.2398 0.020 Uiso 1 1 calc R . . H31B H -0.2380 0.9941 0.2796 0.020 Uiso 1 1 calc R . . C2 C 0.0577(5) 1.0617(6) 0.7648(4) 0.0250(10) Uani 1 1 d . . . H2A H 0.1147 1.1146 0.7766 0.037 Uiso 1 1 calc R . . H2B H 0.1056 0.9631 0.7778 0.037 Uiso 1 1 calc R . . H2C H -0.0399 1.0778 0.8226 0.037 Uiso 1 1 calc R . . C1 C -0.0181(5) 1.3692(5) -0.0109(4) 0.0213(10) Uani 1 1 d . . . H1A H 0.0413 1.2994 -0.0613 0.032 Uiso 1 1 calc R . . H1B H 0.0153 1.4545 -0.0458 0.032 Uiso 1 1 calc R . . H1C H -0.1200 1.3877 -0.0076 0.032 Uiso 1 1 calc R . . Cl2 Cl -0.35336(9) 1.17046(11) 0.48796(8) 0.01816(19) Uani 1 1 d . . . F33 F -0.2830(3) 1.1117(3) 0.0161(3) 0.0277(6) Uani 1 1 d . . . F53 F 0.3048(3) 1.3265(3) 0.7377(3) 0.0290(7) Uani 1 1 d . . . F52 F 0.1443(3) 1.5098(3) 0.6967(3) 0.0270(6) Uani 1 1 d . . . F73 F -0.3581(3) 0.7454(3) 0.8501(3) 0.0312(7) Uani 1 1 d . . . F13 F 0.3608(3) 1.7050(3) -0.0989(3) 0.0361(8) Uani 1 1 d . . . F32 F -0.1299(3) 0.9252(3) 0.0644(3) 0.0286(6) Uani 1 1 d . . . F51 F 0.3718(3) 1.5027(3) 0.6098(3) 0.0299(7) Uani 1 1 d . . . F23 F 0.3992(4) 0.8976(3) 0.0255(3) 0.0412(8) Uani 1 1 d . . . F83 F -0.3641(4) 1.5468(3) 0.7270(3) 0.0443(9) Uani 1 1 d . . . F63 F 0.3068(4) 0.8050(3) 0.6122(4) 0.0539(10) Uani 1 1 d . . . F42 F -0.4430(5) 1.6014(3) 0.1160(3) 0.0521(10) Uani 1 1 d . . . F31 F -0.3611(3) 0.9444(3) 0.1505(3) 0.0273(6) Uani 1 1 d . . . F62 F 0.4853(4) 0.8402(3) 0.6454(3) 0.0468(9) Uani 1 1 d . . . F43 F -0.2549(4) 1.6332(3) 0.1359(3) 0.0529(10) Uani 1 1 d . . . F22 F 0.3907(4) 1.0609(3) -0.1291(3) 0.0388(7) Uani 1 1 d . . . F21 F 0.1950(3) 1.0399(3) 0.0144(3) 0.0342(7) Uani 1 1 d . . . F12 F 0.2488(4) 1.5949(3) -0.1471(3) 0.0441(9) Uani 1 1 d . . . F72 F -0.2497(4) 0.8478(4) 0.9105(3) 0.0435(9) Uani 1 1 d . . . F41 F -0.4671(4) 1.6999(3) 0.2613(3) 0.0478(9) Uani 1 1 d . . . F82 F -0.1731(4) 1.4003(4) 0.7645(4) 0.0558(10) Uani 1 1 d . . . F61 F 0.5244(4) 0.7449(3) 0.4949(3) 0.0438(8) Uani 1 1 d . . . F11 F 0.1280(3) 1.7431(3) -0.0312(3) 0.0416(8) Uani 1 1 d . . . F71 F -0.1246(3) 0.6959(3) 0.7991(3) 0.0415(8) Uani 1 1 d . . . F81 F -0.3843(4) 1.3722(4) 0.8726(3) 0.0602(12) Uani 1 1 d . . . C52 C 0.2723(5) 1.4297(4) 0.6478(4) 0.0203(9) Uani 1 1 d . . . C22 C 0.3374(5) 1.0300(5) -0.0091(4) 0.0234(10) Uani 1 1 d . . . C82 C -0.3073(6) 1.4130(5) 0.7606(5) 0.0303(12) Uani 1 1 d . . . C81 C -0.3012(5) 1.3329(4) 0.6729(4) 0.0265(10) Uani 1 1 d . . . H81A H -0.4006 1.3437 0.6706 0.032 Uiso 1 1 calc R . . H81B H -0.2432 1.3686 0.5908 0.032 Uiso 1 1 calc R . . C61 C 0.4145(5) 0.9802(4) 0.4762(4) 0.0203(9) Uani 1 1 d . . . H61A H 0.5103 1.0018 0.4329 0.024 Uiso 1 1 calc R . . H61B H 0.3700 0.9795 0.4155 0.024 Uiso 1 1 calc R . . C32 C -0.2541(5) 1.0130(4) 0.1077(4) 0.0189(8) Uani 1 1 d . . . C12 C 0.2510(5) 1.6452(5) -0.0571(4) 0.0235(9) Uani 1 1 d . . . C41 C -0.3613(5) 1.4635(4) 0.2818(4) 0.0210(9) Uani 1 1 d . . . H41A H -0.3073 1.4634 0.3360 0.025 Uiso 1 1 calc R . . H41B H -0.4571 1.4458 0.3324 0.025 Uiso 1 1 calc R . . C21 C 0.3648(5) 1.1185(5) 0.0559(4) 0.0249(10) Uani 1 1 d . . . H21A H 0.3402 1.0802 0.1438 0.030 Uiso 1 1 calc R . . H21B H 0.4689 1.1192 0.0262 0.030 Uiso 1 1 calc R . . C72 C -0.2433(5) 0.7985(5) 0.8178(4) 0.0226(9) Uani 1 1 d . . . C42 C -0.3810(6) 1.5998(5) 0.1983(5) 0.0288(11) Uani 1 1 d . . . C62 C 0.4328(6) 0.8423(5) 0.5581(5) 0.0298(11) Uani 1 1 d . . . C51 C 0.2732(4) 1.3758(4) 0.5443(4) 0.0171(9) Uani 1 1 d . . . H51A H 0.2561 1.4532 0.4773 0.021 Uiso 1 1 calc R . . H51B H 0.3686 1.3125 0.5139 0.021 Uiso 1 1 calc R . . N3 N 0.1487(3) 0.9466(3) 0.3373(3) 0.0178(7) Uani 1 1 d . . . C102 C 0.0508(5) 0.8122(4) 0.2629(4) 0.0219(9) Uani 1 1 d . . . H102 H 0.0769 0.8663 0.1842 0.026 Uiso 1 1 calc R . . C103 C -0.0174(5) 0.7081(5) 0.2829(4) 0.0226(9) Uani 1 1 d . . . H103 H -0.0378 0.6896 0.2184 0.027 Uiso 1 1 calc R . . C101 C 0.0812(4) 0.8376(4) 0.3582(4) 0.0172(8) Uani 1 1 d . . . C100 C 0.0902(4) 1.0660(4) 0.3550(3) 0.0173(7) Uani 1 1 d . . . C104 C -0.0549(4) 0.6321(4) 0.3975(4) 0.0208(8) Uani 1 1 d . . . C106 C 0.0459(5) 0.7559(4) 0.4729(4) 0.0215(9) Uani 1 1 d . . . H106 H 0.0693 0.7712 0.5371 0.026 Uiso 1 1 calc R . . C105 C -0.0233(5) 0.6522(4) 0.4932(4) 0.0224(9) Uani 1 1 d . . . H105 H -0.0483 0.5963 0.5711 0.027 Uiso 1 1 calc R . . F1 F -0.1249(3) 0.5315(3) 0.4174(2) 0.0319(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 Rh1 0.01278(16) 0.02040(17) 0.01293(15) 0.00086(11) -0.00455(13) -0.00960(13) Rh2 0.01145(14) 0.02103(17) 0.01311(15) 0.00055(12) -0.00412(12) -0.00827(12) P4 0.0112(5) 0.0172(5) 0.0128(5) 0.0009(4) -0.0038(4) -0.0074(4) P2 0.0113(5) 0.0172(5) 0.0126(5) -0.0006(4) -0.0045(4) -0.0067(4) P1 0.0120(5) 0.0159(5) 0.0124(5) -0.0007(4) -0.0035(4) -0.0057(4) P3 0.0114(5) 0.0177(5) 0.0135(5) -0.0015(4) -0.0040(4) -0.0061(4) Cl1 0.0142(4) 0.0274(5) 0.0165(4) -0.0009(4) -0.0044(3) -0.0118(4) O6 0.0106(12) 0.0203(15) 0.0177(14) -0.0040(11) -0.0086(11) -0.0040(11) O4 0.0173(14) 0.0190(15) 0.0180(14) -0.0028(11) -0.0057(12) -0.0065(11) O8 0.0160(13) 0.0157(14) 0.0211(14) -0.0022(11) -0.0052(11) -0.0024(11) N1 0.0139(16) 0.0222(19) 0.0136(18) -0.0010(13) -0.0033(14) -0.0105(14) N2 0.0168(18) 0.026(2) 0.0136(18) 0.0031(14) -0.0071(15) -0.0105(15) O2 0.0173(13) 0.0181(14) 0.0187(14) -0.0036(11) -0.0054(11) -0.0043(11) O1 0.0131(12) 0.0170(14) 0.0182(14) 0.0006(10) -0.0040(11) -0.0070(11) O7 0.0132(12) 0.0159(14) 0.0206(14) -0.0021(11) -0.0039(11) -0.0074(10) O3 0.0143(13) 0.0199(15) 0.0209(15) -0.0059(11) -0.0014(11) -0.0086(11) O5 0.0137(13) 0.0187(15) 0.0219(15) -0.0053(11) -0.0034(11) -0.0071(11) C71 0.0155(17) 0.019(2) 0.0184(19) 0.0008(15) -0.0076(15) -0.0088(15) C11 0.0158(18) 0.020(2) 0.023(2) -0.0007(15) -0.0025(16) -0.0106(16) C31 0.0174(18) 0.018(2) 0.0193(19) -0.0066(15) -0.0042(15) -0.0088(15) C2 0.022(2) 0.042(3) 0.014(2) 0.0014(18) -0.0060(18) -0.016(2) C1 0.020(2) 0.032(3) 0.012(2) 0.0023(16) -0.0087(17) -0.0091(18) Cl2 0.0101(4) 0.0272(5) 0.0169(4) -0.0024(4) -0.0031(3) -0.0067(4) F33 0.0319(14) 0.0298(15) 0.0267(14) 0.0026(11) -0.0181(12) -0.0103(12) F53 0.0335(15) 0.0313(15) 0.0247(14) -0.0028(11) -0.0160(12) -0.0047(12) F52 0.0246(13) 0.0315(15) 0.0273(14) -0.0160(11) -0.0068(11) -0.0020(11) F73 0.0352(15) 0.0303(16) 0.0298(14) -0.0017(11) -0.0001(12) -0.0243(12) F13 0.0400(17) 0.0371(18) 0.0318(15) 0.0034(12) -0.0012(13) -0.0294(14) F32 0.0275(14) 0.0313(15) 0.0300(15) -0.0153(12) -0.0120(12) 0.0013(11) F51 0.0285(14) 0.0323(15) 0.0380(16) -0.0135(12) -0.0074(12) -0.0160(12) F23 0.056(2) 0.0181(15) 0.0435(18) -0.0101(12) -0.0191(16) 0.0077(13) F83 0.070(2) 0.0182(14) 0.0482(19) -0.0123(13) -0.0298(18) 0.0039(14) F63 0.058(2) 0.0326(18) 0.061(2) -0.0033(15) 0.0067(18) -0.0295(16) F42 0.074(3) 0.0377(19) 0.043(2) -0.0005(15) -0.0411(19) 0.0100(17) F31 0.0278(13) 0.0261(14) 0.0371(15) -0.0056(11) -0.0132(11) -0.0145(11) F62 0.062(2) 0.0379(19) 0.0372(18) -0.0014(14) -0.0305(17) 0.0048(16) F43 0.061(2) 0.0308(18) 0.055(2) 0.0017(15) 0.0046(18) -0.0281(16) F22 0.0448(17) 0.0419(18) 0.0257(15) -0.0117(13) -0.0075(13) -0.0036(14) F21 0.0311(14) 0.0321(16) 0.0440(17) -0.0093(12) -0.0083(12) -0.0155(12) F12 0.073(2) 0.055(2) 0.0182(14) -0.0002(13) -0.0147(15) -0.0384(18) F72 0.072(2) 0.055(2) 0.0177(14) -0.0009(13) -0.0122(14) -0.0410(18) F41 0.067(2) 0.0208(15) 0.0448(19) -0.0078(13) -0.0088(16) -0.0040(14) F82 0.060(2) 0.044(2) 0.089(3) -0.0256(19) -0.049(2) -0.0051(17) F61 0.0548(19) 0.0217(15) 0.0483(19) -0.0108(13) -0.0154(15) 0.0035(13) F11 0.0372(16) 0.0274(16) 0.0426(18) 0.0083(12) -0.0087(14) -0.0009(12) F71 0.0335(16) 0.0268(16) 0.0495(19) 0.0112(13) -0.0120(14) -0.0038(13) F81 0.080(3) 0.043(2) 0.0238(16) -0.0070(14) 0.0049(17) 0.0079(18) C52 0.0211(19) 0.020(2) 0.024(2) -0.0046(16) -0.0102(17) -0.0059(16) C22 0.025(2) 0.018(2) 0.023(2) -0.0026(16) -0.0072(18) -0.0002(17) C82 0.041(3) 0.020(2) 0.030(3) -0.0092(19) -0.015(2) 0.003(2) C81 0.032(2) 0.019(2) 0.034(2) -0.0054(18) -0.021(2) 0.0003(17) C61 0.0210(19) 0.020(2) 0.0191(19) -0.0021(15) -0.0077(16) -0.0037(16) C32 0.0171(18) 0.017(2) 0.024(2) -0.0039(15) -0.0071(16) -0.0044(15) C12 0.028(2) 0.026(2) 0.018(2) -0.0027(17) -0.0030(17) -0.0148(19) C41 0.0213(19) 0.020(2) 0.020(2) -0.0020(15) -0.0036(16) -0.0072(16) C21 0.023(2) 0.027(2) 0.025(2) -0.0091(18) -0.0109(17) -0.0005(17) C72 0.026(2) 0.023(2) 0.018(2) -0.0019(16) -0.0028(17) -0.0106(18) C42 0.040(3) 0.015(2) 0.028(2) 0.0000(16) -0.008(2) -0.0072(18) C62 0.034(2) 0.024(2) 0.031(2) -0.0088(19) -0.009(2) -0.0039(19) C51 0.0122(16) 0.019(2) 0.0190(19) -0.0077(15) 0.0025(14) -0.0066(15) N3 0.0144(14) 0.0200(17) 0.0209(16) -0.0034(13) -0.0057(12) -0.0064(12) C102 0.0217(19) 0.020(2) 0.025(2) -0.0033(16) -0.0076(16) -0.0064(16) C103 0.025(2) 0.024(2) 0.024(2) -0.0092(17) -0.0077(16) -0.0079(17) C101 0.0159(17) 0.0158(19) 0.0221(18) -0.0094(15) -0.0034(14) -0.0044(14) C100 0.0151(15) 0.024(2) 0.0143(16) -0.0006(13) -0.0044(13) -0.0086(14) C104 0.0174(17) 0.017(2) 0.033(2) -0.0093(17) -0.0059(16) -0.0078(15) C106 0.0237(19) 0.020(2) 0.025(2) -0.0071(16) -0.0054(16) -0.0096(16) C105 0.024(2) 0.022(2) 0.0213(19) 0.0001(16) -0.0080(16) -0.0070(17) F1 0.0383(15) 0.0277(15) 0.0376(15) -0.0044(12) -0.0116(12) -0.0195(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C100 1.963(4) . ? Rh1 P3 2.2707(12) . ? Rh1 P1 2.2792(12) . ? Rh1 Cl1 2.3469(10) . ? Rh1 Rh2 2.6880(4) . ? Rh2 C100 1.981(4) . ? Rh2 P2 2.2730(12) . ? Rh2 P4 2.2759(12) . ? Rh2 Cl2 2.3483(9) . ? P4 O7 1.589(3) . ? P4 O8 1.618(3) . ? P4 N2 1.669(4) . ? P2 O3 1.599(3) . ? P2 O4 1.602(3) . ? P2 N1 1.661(4) . ? P1 O1 1.605(3) . ? P1 O2 1.608(3) . ? P1 N1 1.668(4) . ? P3 O6 1.607(3) . ? P3 O5 1.613(3) . ? P3 N2 1.662(4) . ? O6 C61 1.418(5) . ? O4 C41 1.431(5) . ? O8 C81 1.418(5) . ? N1 C1 1.487(6) . ? N2 C2 1.504(6) . ? O2 C21 1.430(5) . ? O1 C11 1.426(5) . ? O7 C71 1.438(5) . ? O3 C31 1.437(5) . ? O5 C51 1.427(5) . ? C71 C72 1.505(6) . ? C11 C12 1.502(6) . ? C31 C32 1.516(6) . ? F33 C32 1.330(5) . ? F53 C52 1.348(5) . ? F52 C52 1.328(5) . ? F73 C72 1.334(5) . ? F13 C12 1.323(5) . ? F32 C32 1.326(5) . ? F51 C52 1.331(5) . ? F23 C22 1.333(5) . ? F83 C82 1.332(5) . ? F63 C62 1.338(7) . ? F42 C42 1.344(6) . ? F31 C32 1.358(5) . ? F62 C62 1.330(6) . ? F43 C42 1.333(7) . ? F22 C22 1.333(6) . ? F21 C22 1.347(6) . ? F12 C12 1.335(5) . ? F72 C72 1.323(5) . ? F41 C42 1.342(5) . ? F82 C82 1.345(7) . ? F61 C62 1.337(5) . ? F11 C12 1.335(5) . ? F71 C72 1.328(5) . ? F81 C82 1.323(6) . ? C52 C51 1.495(6) . ? C22 C21 1.500(6) . ? C82 C81 1.487(7) . ? C61 C62 1.496(7) . ? C41 C42 1.494(6) . ? N3 C100 1.234(5) . ? N3 C101 1.424(5) . ? C102 C103 1.386(6) . ? C102 C101 1.397(6) . ? C103 C104 1.372(6) . ? C101 C106 1.394(6) . ? C104 F1 1.367(5) . ? C104 C105 1.383(6) . ? C106 C105 1.388(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 C100 Rh1 P3 93.33(11) . . ? C100 Rh1 P1 95.40(11) . . ? P3 Rh1 P1 171.04(4) . . ? C100 Rh1 Cl1 139.81(11) . . ? P3 Rh1 Cl1 88.37(4) . . ? P1 Rh1 Cl1 86.25(4) . . ? C100 Rh1 Rh2 47.33(10) . . ? P3 Rh1 Rh2 91.53(3) . . ? P1 Rh1 Rh2 92.92(3) . . ? Cl1 Rh1 Rh2 172.85(3) . . ? C100 Rh2 P2 92.10(11) . . ? C100 Rh2 P4 91.74(11) . . ? P2 Rh2 P4 175.41(4) . . ? C100 Rh2 Cl2 141.69(11) . . ? P2 Rh2 Cl2 88.66(4) . . ? P4 Rh2 Cl2 86.76(4) . . ? C100 Rh2 Rh1 46.75(11) . . ? P2 Rh2 Rh1 91.52(3) . . ? P4 Rh2 Rh1 92.95(3) . . ? Cl2 Rh2 Rh1 171.55(3) . . ? O7 P4 O8 98.12(16) . . ? O7 P4 N2 97.88(18) . . ? O8 P4 N2 105.38(19) . . ? O7 P4 Rh2 119.25(13) . . ? O8 P4 Rh2 116.00(13) . . ? N2 P4 Rh2 117.07(14) . . ? O3 P2 O4 97.46(17) . . ? O3 P2 N1 98.40(17) . . ? O4 P2 N1 104.41(18) . . ? O3 P2 Rh2 116.51(13) . . ? O4 P2 Rh2 117.38(12) . . ? N1 P2 Rh2 119.04(14) . . ? O1 P1 O2 98.54(16) . . ? O1 P1 N1 98.93(18) . . ? O2 P1 N1 104.95(18) . . ? O1 P1 Rh1 116.56(13) . . ? O2 P1 Rh1 117.32(12) . . ? N1 P1 Rh1 117.41(14) . . ? O6 P3 O5 98.23(17) . . ? O6 P3 N2 104.37(18) . . ? O5 P3 N2 98.90(18) . . ? O6 P3 Rh1 117.00(12) . . ? O5 P3 Rh1 116.60(13) . . ? N2 P3 Rh1 118.42(15) . . ? C61 O6 P3 122.5(3) . . ? C41 O4 P2 123.2(3) . . ? C81 O8 P4 119.4(3) . . ? C1 N1 P2 120.6(3) . . ? C1 N1 P1 120.5(3) . . ? P2 N1 P1 118.9(2) . . ? C2 N2 P3 120.3(3) . . ? C2 N2 P4 120.2(3) . . ? P3 N2 P4 118.9(2) . . ? C21 O2 P1 121.0(3) . . ? C11 O1 P1 124.9(3) . . ? C71 O7 P4 122.9(3) . . ? C31 O3 P2 120.3(2) . . ? C51 O5 P3 121.7(3) . . ? O7 C71 C72 106.1(4) . . ? O1 C11 C12 107.1(4) . . ? O3 C31 C32 105.3(3) . . ? F52 C52 F51 108.3(3) . . ? F52 C52 F53 106.7(4) . . ? F51 C52 F53 107.5(4) . . ? F52 C52 C51 112.9(4) . . ? F51 C52 C51 109.5(4) . . ? F53 C52 C51 111.8(4) . . ? F22 C22 F23 107.5(3) . . ? F22 C22 F21 106.2(4) . . ? F23 C22 F21 107.1(4) . . ? F22 C22 C21 113.2(4) . . ? F23 C22 C21 109.8(4) . . ? F21 C22 C21 112.8(4) . . ? F81 C82 F83 108.2(4) . . ? F81 C82 F82 106.6(5) . . ? F83 C82 F82 107.4(5) . . ? F81 C82 C81 113.4(5) . . ? F83 C82 C81 110.4(4) . . ? F82 C82 C81 110.6(4) . . ? O8 C81 C82 109.7(4) . . ? O6 C61 C62 108.1(4) . . ? F32 C32 F33 108.1(4) . . ? F32 C32 F31 107.9(3) . . ? F33 C32 F31 107.0(4) . . ? F32 C32 C31 113.0(4) . . ? F33 C32 C31 112.8(4) . . ? F31 C32 C31 107.8(4) . . ? F13 C12 F11 107.9(4) . . ? F13 C12 F12 107.6(4) . . ? F11 C12 F12 106.6(4) . . ? F13 C12 C11 110.4(4) . . ? F11 C12 C11 112.1(4) . . ? F12 C12 C11 112.0(4) . . ? O4 C41 C42 108.0(4) . . ? O2 C21 C22 109.8(4) . . ? F72 C72 F71 107.6(4) . . ? F72 C72 F73 107.8(4) . . ? F71 C72 F73 107.8(4) . . ? F72 C72 C71 111.4(4) . . ? F71 C72 C71 112.1(4) . . ? F73 C72 C71 109.9(4) . . ? F43 C42 F41 108.4(4) . . ? F43 C42 F42 106.3(4) . . ? F41 C42 F42 107.3(4) . . ? F43 C42 C41 112.0(4) . . ? F41 C42 C41 110.2(4) . . ? F42 C42 C41 112.4(4) . . ? F62 C62 F61 107.8(4) . . ? F62 C62 F63 107.0(5) . . ? F61 C62 F63 107.3(4) . . ? F62 C62 C61 112.3(4) . . ? F61 C62 C61 110.3(4) . . ? F63 C62 C61 111.9(4) . . ? O5 C51 C52 108.1(3) . . ? C100 N3 C101 128.1(3) . . ? C103 C102 C101 120.1(4) . . ? C104 C103 C102 118.8(4) . . ? C106 C101 C102 119.9(4) . . ? C106 C101 N3 120.4(4) . . ? C102 C101 N3 119.7(4) . . ? N3 C100 Rh1 136.0(3) . . ? N3 C100 Rh2 138.1(3) . . ? Rh1 C100 Rh2 85.92(15) . . ? F1 C104 C103 118.6(4) . . ? F1 C104 C105 118.8(4) . . ? C103 C104 C105 122.7(4) . . ? C105 C106 C101 120.0(4) . . ? C104 C105 C106 118.5(4) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 30.55 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.221 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.108 data_Compound_7 _database_code_depnum_ccdc_archive 'CCDC 925036' #TrackingRef '17866_web_deposit_cif_file_0_DavidPowers_1361207103.Cif Files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H29 Cl2 F24 N3 O9 P4 Rh2' _chemical_formula_weight 1384.12 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0403(8) _cell_length_b 19.3984(13) _cell_length_c 20.6248(14) _cell_angle_alpha 90.00 _cell_angle_beta 106.9610(10) _cell_angle_gamma 90.00 _cell_volume 4607.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9892 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 28.20 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.995 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 1.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7674 _exptl_absorpt_correction_T_max 0.8964 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 79113 _diffrn_reflns_av_R_equivalents 0.0890 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.68 _reflns_number_total 8770 _reflns_number_gt 6365 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0363P)^2^+14.3592P] 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 8770 _refine_ls_number_parameters 745 _refine_ls_number_restraints 1019 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.192 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.36988(3) 0.88761(2) 0.19795(2) 0.01566(11) Uani 1 1 d . . . Rh2 Rh 0.36823(4) 0.75039(2) 0.21173(2) 0.01515(11) Uani 1 1 d . . . P1 P 0.17313(11) 0.89343(7) 0.16217(7) 0.0149(3) Uani 1 1 d . . . P2 P 0.17128(12) 0.74643(7) 0.17739(7) 0.0148(3) Uani 1 1 d . . . P3 P 0.56667(12) 0.89196(7) 0.22908(7) 0.0195(3) Uani 1 1 d D A . P4 P 0.56358(12) 0.74730(7) 0.25771(7) 0.0172(3) Uani 1 1 d . . . Cl1 Cl 0.36172(12) 1.00767(7) 0.21260(8) 0.0278(3) Uani 1 1 d . . . Cl2 Cl 0.36509(12) 0.63579(7) 0.24713(8) 0.0282(3) Uani 1 1 d . . . N1 N 0.1003(4) 0.8193(2) 0.1502(2) 0.0176(10) Uani 1 1 d . . . N2 N 0.6378(4) 0.8181(2) 0.2522(2) 0.0219(10) Uani 1 1 d . . . N3 N 0.3817(4) 0.8082(2) 0.0785(2) 0.0201(10) Uani 1 1 d . . . O1 O 0.1185(3) 0.93632(18) 0.09348(18) 0.0204(8) Uani 1 1 d . . . O2 O 0.1085(3) 0.93241(18) 0.20926(19) 0.0205(8) Uani 1 1 d . . . O3 O 0.1134(3) 0.71588(19) 0.23254(18) 0.0199(8) Uani 1 1 d . . . O4 O 0.1073(3) 0.69796(18) 0.11497(19) 0.0216(9) Uani 1 1 d . . . O5 O 0.6304(4) 0.9462(2) 0.2862(2) 0.0371(10) Uani 1 1 d DU . . O6 O 0.6264(3) 0.9153(2) 0.1731(2) 0.0331(10) Uani 1 1 d DU . . O7 O 0.6096(3) 0.73555(17) 0.33806(19) 0.0208(8) Uani 1 1 d . . . O8 O 0.6355(3) 0.68663(19) 0.23513(19) 0.0226(9) Uani 1 1 d . . . O9 O 0.3625(4) 0.6071(2) -0.1168(2) 0.0358(11) Uani 1 1 d . . . C1 C -0.0295(4) 0.8197(3) 0.1238(3) 0.0248(13) Uani 1 1 d . . . H1A H -0.0541 0.7946 0.0807 0.037 Uiso 1 1 calc R . . H1B H -0.0573 0.8673 0.1168 0.037 Uiso 1 1 calc R . . H1C H -0.0622 0.7972 0.1567 0.037 Uiso 1 1 calc R . . C2 C 0.7672(5) 0.8176(3) 0.2750(3) 0.0310(14) Uani 1 1 d . . . H2A H 0.7946 0.7958 0.3197 0.047 Uiso 1 1 calc R . . H2B H 0.7962 0.8651 0.2778 0.047 Uiso 1 1 calc R . . H2C H 0.7960 0.7916 0.2425 0.047 Uiso 1 1 calc R . . C11 C 0.1746(5) 0.9397(3) 0.0411(3) 0.0225(12) Uani 1 1 d . . . H11A H 0.2551 0.9222 0.0584 0.027 Uiso 1 1 calc R . . H11B H 0.1778 0.9881 0.0266 0.027 Uiso 1 1 calc R . . C12 C 0.1079(6) 0.8970(3) -0.0179(3) 0.0291(14) Uani 1 1 d . . . C21 C 0.0747(5) 1.0030(3) 0.2039(3) 0.0365(14) Uani 1 1 d DU B . H21A H 0.0514 1.0176 0.1558 0.044 Uiso 1 1 calc R . . H21B H 0.1404 1.0323 0.2294 0.044 Uiso 1 1 calc R . . C22 C -0.0226(6) 1.0101(3) 0.2320(4) 0.0418(12) Uani 1 1 d DU . . C31 C 0.1652(5) 0.7295(3) 0.3032(3) 0.0250(13) Uani 1 1 d . . . H31A H 0.2284 0.7638 0.3094 0.030 Uiso 1 1 calc R . . H31B H 0.1983 0.6866 0.3272 0.030 Uiso 1 1 calc R . . C32 C 0.0722(5) 0.7568(3) 0.3307(3) 0.0271(13) Uani 1 1 d . . . C41 C 0.0838(6) 0.6268(3) 0.1206(3) 0.0361(16) Uani 1 1 d . . . H41A H 0.0503 0.6192 0.1585 0.043 Uiso 1 1 calc R . . H41B H 0.1563 0.5996 0.1293 0.043 Uiso 1 1 calc R . . C42 C 0.0000(6) 0.6054(3) 0.0555(3) 0.0366(16) Uani 1 1 d . . . C71 C 0.6222(5) 0.6696(3) 0.3706(3) 0.0260(11) Uani 1 1 d DU . . H71A H 0.6237 0.6327 0.3377 0.031 Uiso 1 1 calc R . . H71B H 0.5565 0.6609 0.3892 0.031 Uiso 1 1 calc R . . C72 C 0.7329(6) 0.6710(4) 0.4257(4) 0.0504(13) Uani 1 1 d DU . . C81 C 0.5980(5) 0.6551(3) 0.1703(3) 0.0252(13) Uani 1 1 d . . . H81A H 0.5218 0.6744 0.1445 0.030 Uiso 1 1 calc R . . H81B H 0.5885 0.6049 0.1756 0.030 Uiso 1 1 calc R . . C82 C 0.6834(6) 0.6672(4) 0.1328(3) 0.0397(17) Uani 1 1 d . . . C100 C 0.3751(4) 0.8117(3) 0.1363(3) 0.0163(11) Uani 1 1 d . . . C101 C 0.3787(5) 0.7542(3) 0.0317(3) 0.0192(11) Uani 1 1 d . . . C102 C 0.4286(6) 0.7651(3) -0.0197(3) 0.0337(15) Uani 1 1 d . . . H102 H 0.4659 0.8077 -0.0225 0.040 Uiso 1 1 calc R . . C103 C 0.4245(6) 0.7141(3) -0.0671(3) 0.0356(16) Uani 1 1 d . . . H103 H 0.4613 0.7213 -0.1014 0.043 Uiso 1 1 calc R . . C104 C 0.3670(5) 0.6526(3) -0.0649(3) 0.0257(13) Uani 1 1 d . . . C105 C 0.3174(5) 0.6412(3) -0.0135(3) 0.0262(13) Uani 1 1 d . . . H105 H 0.2794 0.5988 -0.0111 0.031 Uiso 1 1 calc R . . C106 C 0.3234(5) 0.6923(3) 0.0349(3) 0.0252(13) Uani 1 1 d . . . H106 H 0.2891 0.6846 0.0703 0.030 Uiso 1 1 calc R . . C107 C 0.2983(6) 0.5456(3) -0.1184(4) 0.0413(17) Uani 1 1 d . . . H10A H 0.3344 0.5182 -0.0777 0.062 Uiso 1 1 calc R . . H10B H 0.2977 0.5189 -0.1588 0.062 Uiso 1 1 calc R . . H10C H 0.2185 0.5571 -0.1196 0.062 Uiso 1 1 calc R . . F11 F -0.0008(3) 0.9203(2) -0.04378(19) 0.0440(10) Uani 1 1 d . . . F12 F 0.1577(4) 0.8976(2) -0.06739(18) 0.0458(10) Uani 1 1 d . . . F13 F 0.0991(3) 0.83110(17) -0.00026(18) 0.0363(9) Uani 1 1 d . . . F31 F 0.1136(3) 0.7681(2) 0.39722(18) 0.0412(9) Uani 1 1 d . . . F32 F -0.0165(3) 0.71296(18) 0.32134(18) 0.0344(8) Uani 1 1 d . . . F33 F 0.0288(3) 0.81655(18) 0.30161(19) 0.0369(9) Uani 1 1 d . . . F41 F -0.0297(4) 0.5395(2) 0.0576(2) 0.0652(14) Uani 1 1 d . . . F42 F -0.0972(4) 0.6422(3) 0.0408(3) 0.0746(16) Uani 1 1 d . . . F43 F 0.0418(4) 0.6117(2) 0.0033(2) 0.0592(13) Uani 1 1 d . . . F71 F 0.8220(4) 0.6839(3) 0.4045(4) 0.118(2) Uani 1 1 d DU . . F72 F 0.7307(5) 0.7192(3) 0.4724(2) 0.0899(16) Uani 1 1 d DU . . F73 F 0.7509(4) 0.6103(2) 0.4579(2) 0.0634(12) Uani 1 1 d DU . . F81 F 0.7896(4) 0.6438(3) 0.1673(2) 0.0702(15) Uani 1 1 d . . . F82 F 0.6945(5) 0.7341(2) 0.1216(2) 0.0669(14) Uani 1 1 d . . . F83 F 0.6518(4) 0.6359(2) 0.0728(2) 0.0531(11) Uani 1 1 d . . . C61 C 0.6008(9) 0.9757(5) 0.1321(5) 0.0326(17) Uani 0.620(5) 1 d PDU A 1 H61A H 0.6383 1.0163 0.1587 0.039 Uiso 0.620(5) 1 calc PR A 1 H61B H 0.5158 0.9837 0.1171 0.039 Uiso 0.620(5) 1 calc PR A 1 C62 C 0.6437(11) 0.9672(7) 0.0720(6) 0.0402(18) Uani 0.620(5) 1 d PDU A 1 F61 F 0.7573(5) 0.9548(3) 0.0874(3) 0.0468(16) Uani 0.620(5) 1 d PDU A 1 F62 F 0.5911(6) 0.9167(4) 0.0309(3) 0.0595(19) Uani 0.620(5) 1 d PDU A 1 F63 F 0.6252(6) 1.0257(4) 0.0348(4) 0.063(2) Uani 0.620(5) 1 d PDU A 1 F61A F 0.4801(9) 0.9720(6) 0.0624(6) 0.066(3) Uani 0.380(5) 1 d PDU A 2 C62A C 0.5846(12) 1.0002(6) 0.0907(7) 0.041(2) Uani 0.380(5) 1 d PDU A 2 F62A F 0.5826(11) 1.0666(5) 0.0743(6) 0.061(3) Uani 0.380(5) 1 d PDU A 2 F63A F 0.6607(13) 0.9697(7) 0.0629(6) 0.046(3) Uani 0.380(5) 1 d PDU A 2 C61A C 0.6220(14) 0.9921(6) 0.1648(6) 0.035(2) Uani 0.380(5) 1 d PDU A 2 H61C H 0.5654 1.0130 0.1855 0.042 Uiso 0.380(5) 1 calc PR A 2 H61D H 0.6993 1.0131 0.1852 0.042 Uiso 0.380(5) 1 calc PR A 2 F22 F -0.0654(4) 1.0736(2) 0.2254(2) 0.0568(11) Uani 1 1 d DU B . F21 F -0.0993(7) 0.9624(4) 0.2254(7) 0.063(3) Uani 0.575(15) 1 d PDU B 1 F23 F 0.0301(10) 1.0053(6) 0.3035(4) 0.059(3) Uani 0.575(15) 1 d PDU B 1 F21A F -0.0263(15) 0.9821(7) 0.2848(8) 0.065(3) Uani 0.425(15) 1 d PDU B 2 F23A F -0.1141(8) 0.9799(7) 0.1770(10) 0.083(4) Uani 0.425(15) 1 d PDU B 2 C51 C 0.5883(6) 0.9659(4) 0.3396(3) 0.0355(14) Uani 0.803(6) 1 d PDU C 1 H51A H 0.5135 0.9427 0.3358 0.043 Uiso 0.803(6) 1 calc PR C 1 H51B H 0.5759 1.0164 0.3388 0.043 Uiso 0.803(6) 1 calc PR C 1 C52 C 0.6769(7) 0.9452(4) 0.4035(4) 0.0446(15) Uani 0.803(6) 1 d PDU C 1 F51 F 0.6454(7) 0.9646(4) 0.4580(3) 0.064(2) Uani 0.803(6) 1 d PDU C 1 F52 F 0.7799(5) 0.9749(4) 0.4103(4) 0.066(2) Uani 0.803(6) 1 d PDU C 1 F53 F 0.6958(5) 0.8782(2) 0.4076(3) 0.0564(15) Uani 0.803(6) 1 d PDU C 1 F51A F 0.599(2) 0.9631(16) 0.4572(10) 0.053(5) Uani 0.197(6) 1 d PDU C 2 F52A F 0.7526(18) 0.9877(16) 0.4304(14) 0.053(5) Uani 0.197(6) 1 d PDU C 2 F53A F 0.5904(19) 1.0359(8) 0.3836(10) 0.057(5) Uani 0.197(6) 1 d PDU C 2 C51A C 0.612(2) 0.9220(10) 0.3537(7) 0.044(3) Uani 0.197(6) 1 d PDU C 2 H51C H 0.5299 0.9081 0.3457 0.053 Uiso 0.197(6) 1 calc PR C 2 H51D H 0.6614 0.8814 0.3708 0.053 Uiso 0.197(6) 1 calc PR C 2 C52A C 0.6395(19) 0.9753(10) 0.4031(8) 0.046(3) Uani 0.197(6) 1 d PDU C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0130(2) 0.01203(19) 0.0214(2) -0.00101(17) 0.00412(17) -0.00007(16) Rh2 0.0137(2) 0.01252(19) 0.0202(2) 0.00140(17) 0.00634(16) 0.00094(16) P1 0.0141(7) 0.0129(6) 0.0183(7) 0.0008(5) 0.0055(5) 0.0013(5) P2 0.0142(7) 0.0122(6) 0.0187(7) 0.0006(5) 0.0063(6) -0.0004(5) P3 0.0145(7) 0.0160(7) 0.0279(8) -0.0010(6) 0.0061(6) -0.0022(6) P4 0.0141(7) 0.0159(7) 0.0225(7) 0.0016(6) 0.0066(6) 0.0033(5) Cl1 0.0235(7) 0.0135(6) 0.0459(9) -0.0051(6) 0.0094(7) -0.0018(5) Cl2 0.0242(8) 0.0162(6) 0.0456(9) 0.0093(6) 0.0123(7) 0.0037(6) N1 0.010(2) 0.018(2) 0.022(2) 0.0015(19) 0.0017(19) -0.0005(18) N2 0.012(2) 0.021(2) 0.031(3) 0.003(2) 0.005(2) 0.0017(19) N3 0.021(3) 0.017(2) 0.025(3) 0.0016(19) 0.010(2) 0.0002(19) O1 0.018(2) 0.0199(19) 0.023(2) 0.0048(16) 0.0049(16) 0.0042(16) O2 0.022(2) 0.0167(18) 0.025(2) -0.0003(16) 0.0105(17) 0.0033(15) O3 0.016(2) 0.025(2) 0.019(2) 0.0025(16) 0.0058(16) -0.0031(16) O4 0.027(2) 0.0154(18) 0.022(2) -0.0016(16) 0.0081(17) -0.0048(16) O5 0.021(2) 0.032(2) 0.052(2) -0.016(2) 0.0013(19) -0.0028(18) O6 0.024(2) 0.028(2) 0.053(3) 0.0149(18) 0.019(2) 0.0014(17) O7 0.024(2) 0.0144(18) 0.025(2) 0.0013(15) 0.0088(17) 0.0056(15) O8 0.020(2) 0.025(2) 0.023(2) -0.0004(16) 0.0058(17) 0.0082(16) O9 0.052(3) 0.031(2) 0.031(2) -0.0134(19) 0.022(2) -0.012(2) C1 0.013(3) 0.024(3) 0.036(4) 0.001(3) 0.004(3) -0.002(2) C2 0.011(3) 0.034(3) 0.046(4) 0.004(3) 0.004(3) 0.003(3) C11 0.023(3) 0.024(3) 0.024(3) 0.007(2) 0.011(2) 0.003(2) C12 0.037(4) 0.026(3) 0.023(3) 0.004(2) 0.008(3) 0.001(3) C21 0.042(3) 0.023(3) 0.051(4) 0.002(3) 0.026(3) 0.010(2) C22 0.039(3) 0.031(2) 0.062(3) -0.001(3) 0.023(3) 0.0139(19) C31 0.022(3) 0.034(3) 0.020(3) 0.007(2) 0.009(2) -0.001(2) C32 0.026(3) 0.031(3) 0.027(3) 0.005(3) 0.012(3) -0.001(3) C41 0.051(4) 0.017(3) 0.037(4) -0.005(3) 0.009(3) -0.007(3) C42 0.044(4) 0.028(3) 0.040(4) -0.013(3) 0.016(3) -0.013(3) C71 0.036(2) 0.016(3) 0.027(3) 0.0055(19) 0.012(2) 0.004(2) C72 0.035(3) 0.054(3) 0.056(4) 0.033(2) 0.005(2) 0.011(3) C81 0.025(3) 0.023(3) 0.028(3) -0.002(2) 0.008(3) 0.006(2) C82 0.037(4) 0.053(5) 0.032(4) -0.003(3) 0.013(3) 0.002(3) C100 0.010(3) 0.017(3) 0.023(3) 0.002(2) 0.006(2) -0.002(2) C101 0.023(3) 0.020(3) 0.016(3) -0.002(2) 0.006(2) 0.000(2) C102 0.048(4) 0.027(3) 0.035(4) -0.005(3) 0.026(3) -0.016(3) C103 0.047(4) 0.040(4) 0.031(4) -0.009(3) 0.029(3) -0.011(3) C104 0.027(3) 0.028(3) 0.022(3) -0.005(3) 0.008(3) 0.000(3) C105 0.030(3) 0.022(3) 0.028(3) -0.003(2) 0.010(3) -0.006(2) C106 0.028(3) 0.027(3) 0.023(3) 0.000(2) 0.012(3) -0.002(3) C107 0.053(5) 0.034(4) 0.039(4) -0.016(3) 0.016(3) -0.013(3) F11 0.038(2) 0.046(2) 0.036(2) 0.0015(18) -0.0081(18) 0.0011(18) F12 0.074(3) 0.044(2) 0.024(2) -0.0034(17) 0.023(2) -0.007(2) F13 0.057(2) 0.0216(18) 0.032(2) -0.0032(15) 0.0147(18) -0.0054(16) F31 0.041(2) 0.062(3) 0.024(2) -0.0030(18) 0.0163(17) -0.0004(19) F32 0.0244(19) 0.041(2) 0.044(2) 0.0051(17) 0.0201(17) -0.0005(16) F33 0.039(2) 0.0315(19) 0.044(2) 0.0046(17) 0.0184(18) 0.0090(17) F41 0.096(4) 0.040(2) 0.064(3) -0.026(2) 0.031(3) -0.042(2) F42 0.025(2) 0.075(3) 0.108(4) -0.040(3) -0.005(2) -0.004(2) F43 0.084(3) 0.060(3) 0.043(3) -0.026(2) 0.032(2) -0.032(2) F71 0.027(2) 0.153(5) 0.174(5) 0.122(4) 0.028(3) 0.030(3) F72 0.118(4) 0.059(2) 0.051(3) 0.007(2) -0.041(2) -0.016(3) F73 0.061(3) 0.061(2) 0.062(3) 0.041(2) 0.009(2) 0.018(2) F81 0.028(2) 0.129(5) 0.059(3) -0.017(3) 0.021(2) 0.015(3) F82 0.096(4) 0.066(3) 0.050(3) -0.003(2) 0.039(3) -0.038(3) F83 0.055(3) 0.074(3) 0.038(2) -0.014(2) 0.026(2) 0.003(2) C61 0.032(4) 0.029(4) 0.042(4) 0.011(2) 0.017(3) -0.001(3) C62 0.037(3) 0.044(4) 0.046(4) 0.009(3) 0.022(4) -0.003(4) F61 0.035(3) 0.062(4) 0.051(4) 0.008(3) 0.025(3) -0.006(3) F62 0.055(4) 0.084(4) 0.043(4) -0.010(3) 0.020(3) -0.021(4) F63 0.055(4) 0.079(4) 0.061(4) 0.041(3) 0.026(3) -0.002(3) F61A 0.041(5) 0.067(7) 0.079(7) 0.034(6) 0.002(5) -0.001(4) C62A 0.041(4) 0.031(4) 0.056(4) 0.017(3) 0.021(4) 0.006(4) F62A 0.085(8) 0.035(4) 0.080(7) 0.027(5) 0.050(6) 0.012(4) F63A 0.060(5) 0.043(5) 0.044(5) 0.015(5) 0.028(5) 0.009(5) C61A 0.035(6) 0.026(3) 0.054(4) 0.009(4) 0.030(4) 0.005(5) F22 0.068(3) 0.0386(18) 0.070(3) -0.0013(18) 0.030(2) 0.0325(18) F21 0.031(4) 0.050(3) 0.114(8) 0.001(5) 0.033(4) 0.009(3) F23 0.071(7) 0.061(7) 0.052(3) -0.002(3) 0.030(3) 0.033(4) F21A 0.085(10) 0.038(6) 0.103(6) 0.014(5) 0.074(6) 0.015(6) F23A 0.034(3) 0.051(6) 0.142(9) -0.019(7) -0.008(6) 0.014(5) C51 0.031(3) 0.027(3) 0.042(3) -0.006(3) 0.000(2) 0.002(3) C52 0.047(4) 0.027(3) 0.048(2) 0.001(3) -0.004(3) 0.000(3) F51 0.079(6) 0.056(4) 0.043(2) -0.019(3) -0.007(3) -0.002(4) F52 0.048(3) 0.063(4) 0.063(5) -0.001(3) -0.024(2) -0.019(3) F53 0.084(4) 0.029(2) 0.044(3) 0.007(2) 0.000(3) 0.007(2) F51A 0.052(11) 0.053(10) 0.038(7) -0.007(6) -0.010(7) -0.016(10) F52A 0.050(6) 0.054(9) 0.046(10) -0.019(8) -0.002(6) -0.004(6) F53A 0.074(10) 0.034(6) 0.051(10) -0.005(6) 0.001(9) 0.011(7) C51A 0.041(6) 0.031(5) 0.048(4) -0.005(4) -0.006(5) 0.003(5) C52A 0.047(6) 0.035(5) 0.043(4) -0.004(4) -0.005(5) 0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C100 1.958(5) . ? Rh1 P3 2.2685(15) . ? Rh1 P1 2.2692(14) . ? Rh1 Cl1 2.3542(13) . ? Rh1 Rh2 2.6776(6) . ? Rh2 C100 1.979(5) . ? Rh2 P4 2.2658(14) . ? Rh2 P2 2.2695(14) . ? Rh2 Cl2 2.3438(14) . ? P1 O2 1.600(4) . ? P1 O1 1.609(4) . ? P1 N1 1.666(4) . ? P2 O4 1.599(4) . ? P2 O3 1.610(4) . ? P2 N1 1.662(4) . ? P3 O6 1.594(4) . ? P3 O5 1.598(4) . ? P3 N2 1.665(5) . ? P4 O7 1.603(4) . ? P4 O8 1.609(4) . ? P4 N2 1.661(5) . ? N1 C1 1.497(6) . ? N2 C2 1.491(7) . ? N3 C100 1.220(7) . ? N3 C101 1.417(7) . ? O1 C11 1.433(6) . ? O2 C21 1.424(6) . ? O3 C31 1.432(6) . ? O4 C41 1.421(7) . ? O5 C51 1.394(8) . ? O5 C51A 1.546(16) . ? O6 C61 1.427(9) . ? O6 C61A 1.499(11) . ? O7 C71 1.432(6) . ? O8 C81 1.419(7) . ? O9 C104 1.377(7) . ? O9 C107 1.416(7) . ? C11 C12 1.496(8) . ? C12 F12 1.326(7) . ? C12 F11 1.340(7) . ? C12 F13 1.342(6) . ? C21 C22 1.458(8) . ? C22 F21A 1.229(11) . ? C22 F21 1.287(9) . ? C22 F22 1.327(6) . ? C22 F23 1.429(9) . ? C22 F23A 1.454(11) . ? C31 C32 1.493(8) . ? C32 F31 1.333(7) . ? C32 F32 1.335(7) . ? C32 F33 1.339(7) . ? C41 C42 1.484(9) . ? C42 F43 1.321(8) . ? C42 F42 1.327(8) . ? C42 F41 1.332(7) . ? C71 C72 1.479(9) . ? C72 F71 1.296(8) . ? C72 F73 1.337(7) . ? C72 F72 1.348(8) . ? C81 C82 1.475(9) . ? C82 F83 1.329(8) . ? C82 F82 1.333(8) . ? C82 F81 1.347(8) . ? C101 C102 1.379(8) . ? C101 C106 1.384(8) . ? C102 C103 1.380(8) . ? C103 C104 1.388(8) . ? C104 C105 1.376(8) . ? C105 C106 1.394(8) . ? C61 C62 1.484(13) . ? C62 F62 1.330(13) . ? C62 F61 1.332(12) . ? C62 F63 1.351(12) . ? F61A C62A 1.339(13) . ? C62A F62A 1.330(12) . ? C62A F63A 1.351(13) . ? C62A C61A 1.471(15) . ? C51 C52 1.488(9) . ? C52 F53 1.318(8) . ? C52 F52 1.338(9) . ? C52 F51 1.341(9) . ? F51A C52A 1.364(15) . ? F52A C52A 1.334(15) . ? F53A C52A 1.326(15) . ? C51A C52A 1.420(16) . ? 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 C100 Rh1 P3 89.03(15) . . ? C100 Rh1 P1 93.12(15) . . ? P3 Rh1 P1 174.45(5) . . ? C100 Rh1 Cl1 146.87(16) . . ? P3 Rh1 Cl1 90.35(5) . . ? P1 Rh1 Cl1 85.05(5) . . ? C100 Rh1 Rh2 47.49(15) . . ? P3 Rh1 Rh2 92.66(4) . . ? P1 Rh1 Rh2 92.56(4) . . ? Cl1 Rh1 Rh2 165.45(4) . . ? C100 Rh2 P4 93.93(15) . . ? C100 Rh2 P2 93.13(15) . . ? P4 Rh2 P2 172.87(5) . . ? C100 Rh2 Cl2 145.41(16) . . ? P4 Rh2 Cl2 87.34(5) . . ? P2 Rh2 Cl2 87.41(5) . . ? C100 Rh2 Rh1 46.83(15) . . ? P4 Rh2 Rh1 91.82(4) . . ? P2 Rh2 Rh1 92.29(4) . . ? Cl2 Rh2 Rh1 167.77(4) . . ? O2 P1 O1 98.3(2) . . ? O2 P1 N1 99.8(2) . . ? O1 P1 N1 104.7(2) . . ? O2 P1 Rh1 118.18(15) . . ? O1 P1 Rh1 115.59(15) . . ? N1 P1 Rh1 117.39(16) . . ? O4 P2 O3 98.4(2) . . ? O4 P2 N1 98.6(2) . . ? O3 P2 N1 105.4(2) . . ? O4 P2 Rh2 119.01(15) . . ? O3 P2 Rh2 114.84(14) . . ? N1 P2 Rh2 117.68(16) . . ? O6 P3 O5 97.2(2) . . ? O6 P3 N2 98.5(2) . . ? O5 P3 N2 105.0(2) . . ? O6 P3 Rh1 117.43(17) . . ? O5 P3 Rh1 118.08(17) . . ? N2 P3 Rh1 117.15(17) . . ? O7 P4 O8 98.18(19) . . ? O7 P4 N2 99.1(2) . . ? O8 P4 N2 103.9(2) . . ? O7 P4 Rh2 116.12(15) . . ? O8 P4 Rh2 118.64(15) . . ? N2 P4 Rh2 117.56(17) . . ? C1 N1 P2 120.4(3) . . ? C1 N1 P1 119.9(3) . . ? P2 N1 P1 119.2(3) . . ? C2 N2 P4 120.4(4) . . ? C2 N2 P3 119.9(4) . . ? P4 N2 P3 119.3(3) . . ? C100 N3 C101 135.2(5) . . ? C11 O1 P1 121.8(3) . . ? C21 O2 P1 125.9(3) . . ? C31 O3 P2 120.1(3) . . ? C41 O4 P2 124.5(4) . . ? C51 O5 C51A 35.9(8) . . ? C51 O5 P3 123.7(4) . . ? C51A O5 P3 107.4(7) . . ? C61 O6 C61A 28.5(5) . . ? C61 O6 P3 126.7(5) . . ? C61A O6 P3 110.9(6) . . ? C71 O7 P4 124.7(3) . . ? C81 O8 P4 122.5(3) . . ? C104 O9 C107 117.1(5) . . ? O1 C11 C12 109.2(5) . . ? F12 C12 F11 107.3(5) . . ? F12 C12 F13 107.9(5) . . ? F11 C12 F13 106.5(5) . . ? F12 C12 C11 111.4(5) . . ? F11 C12 C11 111.6(5) . . ? F13 C12 C11 112.0(5) . . ? O2 C21 C22 107.8(5) . . ? F21A C22 F21 64.3(8) . . ? F21A C22 F22 112.7(8) . . ? F21 C22 F22 114.3(6) . . ? F21A C22 F23 34.5(7) . . ? F21 C22 F23 98.7(7) . . ? F22 C22 F23 102.0(6) . . ? F21A C22 F23A 107.4(10) . . ? F21 C22 F23A 43.2(7) . . ? F22 C22 F23A 96.4(7) . . ? F23 C22 F23A 141.8(9) . . ? F21A C22 C21 123.5(8) . . ? F21 C22 C21 121.7(6) . . ? F22 C22 C21 112.4(5) . . ? F23 C22 C21 103.8(6) . . ? F23A C22 C21 99.5(8) . . ? O3 C31 C32 107.5(5) . . ? F31 C32 F32 107.3(5) . . ? F31 C32 F33 107.4(5) . . ? F32 C32 F33 107.2(5) . . ? F31 C32 C31 110.6(5) . . ? F32 C32 C31 112.0(5) . . ? F33 C32 C31 112.0(5) . . ? O4 C41 C42 107.3(5) . . ? F43 C42 F42 106.5(6) . . ? F43 C42 F41 106.5(5) . . ? F42 C42 F41 107.2(6) . . ? F43 C42 C41 113.0(6) . . ? F42 C42 C41 112.2(5) . . ? F41 C42 C41 110.9(6) . . ? O7 C71 C72 107.0(5) . . ? F71 C72 F73 107.9(6) . . ? F71 C72 F72 107.4(7) . . ? F73 C72 F72 106.9(6) . . ? F71 C72 C71 113.1(6) . . ? F73 C72 C71 110.2(6) . . ? F72 C72 C71 111.2(6) . . ? O8 C81 C82 110.3(5) . . ? F83 C82 F82 107.4(6) . . ? F83 C82 F81 108.0(6) . . ? F82 C82 F81 106.9(6) . . ? F83 C82 C81 111.2(6) . . ? F82 C82 C81 111.5(6) . . ? F81 C82 C81 111.6(6) . . ? N3 C100 Rh1 134.4(4) . . ? N3 C100 Rh2 139.9(4) . . ? Rh1 C100 Rh2 85.7(2) . . ? C102 C101 C106 119.5(5) . . ? C102 C101 N3 118.7(5) . . ? C106 C101 N3 121.8(5) . . ? C101 C102 C103 120.1(5) . . ? C102 C103 C104 120.5(6) . . ? C105 C104 O9 124.6(5) . . ? C105 C104 C103 119.7(5) . . ? O9 C104 C103 115.7(5) . . ? C104 C105 C106 119.6(5) . . ? C101 C106 C105 120.6(5) . . ? O6 C61 C62 109.6(8) . . ? F62 C62 F61 106.5(10) . . ? F62 C62 F63 106.7(10) . . ? F61 C62 F63 106.0(9) . . ? F62 C62 C61 113.4(9) . . ? F61 C62 C61 113.9(10) . . ? F63 C62 C61 109.9(10) . . ? F62A C62A F61A 109.9(11) . . ? F62A C62A F63A 106.3(12) . . ? F61A C62A F63A 107.7(13) . . ? F62A C62A C61A 110.2(11) . . ? F61A C62A C61A 111.9(11) . . ? F63A C62A C61A 110.7(11) . . ? C62A C61A O6 102.4(9) . . ? O5 C51 C52 107.1(6) . . ? F53 C52 F52 106.3(7) . . ? F53 C52 F51 108.0(7) . . ? F52 C52 F51 105.7(7) . . ? F53 C52 C51 112.9(6) . . ? F52 C52 C51 112.3(7) . . ? F51 C52 C51 111.2(7) . . ? C52A C51A O5 111.1(13) . . ? F53A C52A F52A 106.1(19) . . ? F53A C52A F51A 99.6(18) . . ? F52A C52A F51A 104.5(17) . . ? F53A C52A C51A 116.0(14) . . ? F52A C52A C51A 115.6(15) . . ? F51A C52A C51A 113.4(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.000 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.119 data_Compound_8 _database_code_depnum_ccdc_archive 'CCDC 925037' #TrackingRef '17866_web_deposit_cif_file_0_DavidPowers_1361207103.Cif Files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H26 Cl4 F25 N3 O8 P4 Rh2' _chemical_formula_weight 1442.99 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' Cl Cl 0.1484 0.1585 '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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P(2)1/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2025(13) _cell_length_b 21.385(2) _cell_length_c 20.398(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.351(2) _cell_angle_gamma 90.00 _cell_volume 5266.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 1.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8995 _exptl_absorpt_correction_T_max 0.8995 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10766 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10766 _reflns_number_gt 8406 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 358 101 ' ' 2 0.000 1.000 0.500 358 101 ' ' _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^)+(0.1028P)^2^+37.7972P] 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 10766 _refine_ls_number_parameters 556 _refine_ls_number_restraints 214 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.2042 _refine_ls_wR_factor_gt 0.1924 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.000 _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 0.4973(8) 0.8933(4) 0.7391(5) 0.0516(10) Uani 1 1 d D . . C2 C 0.5268(7) 0.8335(4) 0.7119(4) 0.0420(18) Uani 1 1 d . B . H2A H 0.5967 0.8176 0.7371 0.050 Uiso 1 1 calc R . . H2B H 0.4677 0.8023 0.7147 0.050 Uiso 1 1 calc R . . C4 C 0.3432(7) 0.7128(5) 0.5883(6) 0.0566(13) Uani 1 1 d D . . H4AA H 0.3838 0.6803 0.6167 0.068 Uiso 0.573(11) 1 calc PR A 1 H4AB H 0.3404 0.7002 0.5414 0.068 Uiso 0.573(11) 1 calc PR A 1 H4BC H 0.3939 0.6789 0.6066 0.068 Uiso 0.427(11) 1 calc PR A 2 H4BD H 0.3225 0.7056 0.5401 0.068 Uiso 0.427(11) 1 calc PR A 2 C5 C 0.4300(7) 0.8840(4) 0.5114(4) 0.0447(13) Uani 1 1 d . . . H5A H 0.4661 0.9217 0.5313 0.067 Uiso 1 1 calc R . . H5B H 0.3643 0.8747 0.5321 0.067 Uiso 1 1 calc R . . H5C H 0.4080 0.8907 0.4638 0.067 Uiso 1 1 calc R . . C10 C 1.0775(6) 0.6460(4) 0.4129(4) 0.0398(17) Uani 1 1 d . . . C11 C 0.9859(6) 0.6873(4) 0.4298(4) 0.0397(17) Uani 1 1 d . . . H11A H 1.0123 0.7311 0.4352 0.048 Uiso 1 1 calc R . . H11B H 0.9224 0.6861 0.3936 0.048 Uiso 1 1 calc R . . C12 C 0.7326(6) 0.5014(3) 0.3908(4) 0.0395(17) Uani 1 1 d . . . C13 C 0.7088(6) 0.5651(3) 0.4185(4) 0.0345(15) Uani 1 1 d . . . H13A H 0.6659 0.5912 0.3837 0.041 Uiso 1 1 calc R . . H13B H 0.6654 0.5605 0.4557 0.041 Uiso 1 1 calc R . . C14 C 0.9345(6) 0.5622(3) 0.5804(4) 0.0345(16) Uani 1 1 d . . . H14A H 1.0070 0.5822 0.5917 0.052 Uiso 1 1 calc R . . H14B H 0.9344 0.5364 0.5407 0.052 Uiso 1 1 calc R . . H14C H 0.9195 0.5358 0.6174 0.052 Uiso 1 1 calc R . . C15 C 0.6499(6) 0.4815(3) 0.6049(4) 0.0328(15) Uani 1 1 d . . . C16 C 0.6328(6) 0.5417(3) 0.6392(4) 0.0333(15) Uani 1 1 d . . . H16A H 0.5844 0.5698 0.6091 0.040 Uiso 1 1 calc R . . H16B H 0.5968 0.5337 0.6789 0.040 Uiso 1 1 calc R . . C17 C 0.9717(9) 0.6693(6) 0.7895(6) 0.0747(9) Uani 1 1 d . . . C18 C 0.8635(9) 0.6524(6) 0.7519(5) 0.0747(9) Uani 1 1 d . . . H18A H 0.8385 0.6115 0.7669 0.090 Uiso 1 1 calc R . . H18B H 0.8073 0.6844 0.7583 0.090 Uiso 1 1 calc R . . C19 C 0.7535(6) 0.7706(3) 0.6467(4) 0.0363(10) Uani 1 1 d . B . C20 C 0.8968(8) 0.8510(5) 0.6896(6) 0.0630(11) Uani 1 1 d . . . C21 C 0.8745(8) 0.8980(5) 0.7304(6) 0.0630(11) Uani 1 1 d . . . H21 H 0.8054 0.8992 0.7466 0.076 Uiso 1 1 calc R . . C22 C 0.9525(8) 0.9442(5) 0.7482(6) 0.0630(11) Uani 1 1 d . . . H22 H 0.9378 0.9774 0.7767 0.076 Uiso 1 1 calc R . . C23 C 1.0490(8) 0.9413(5) 0.7246(6) 0.0630(11) Uani 1 1 d . . . C24 C 1.0749(8) 0.8936(5) 0.6851(6) 0.0630(11) Uani 1 1 d . . . H24 H 1.1449 0.8924 0.6699 0.076 Uiso 1 1 calc R . . C25 C 0.9971(8) 0.8467(5) 0.6673(6) 0.0630(11) Uani 1 1 d . . . H25 H 1.0132 0.8126 0.6404 0.076 Uiso 1 1 calc R . . N1 N 0.5094(6) 0.8298(3) 0.5219(3) 0.0447(13) Uani 1 1 d . . . N2 N 0.8474(4) 0.6109(2) 0.5674(3) 0.0280(12) Uani 1 1 d . . . N3 N 0.8174(5) 0.8055(3) 0.6694(3) 0.0363(10) Uani 1 1 d . . . O1 O 0.9524(4) 0.6656(2) 0.4897(2) 0.0321(11) Uani 1 1 d . . . O2 O 0.8133(4) 0.5931(2) 0.4411(3) 0.0322(11) Uani 1 1 d . . . O3 O 0.8785(4) 0.6493(2) 0.6836(2) 0.0325(11) Uani 1 1 d . . . O4 O 0.7391(4) 0.5705(2) 0.6583(2) 0.0310(10) Uani 1 1 d . . . O5 O 0.6343(6) 0.8757(3) 0.4493(3) 0.0612(18) Uani 1 1 d U . . O7 O 0.5400(4) 0.8439(2) 0.6441(3) 0.0359(11) Uani 1 1 d . . . O8 O 0.3968(4) 0.7723(2) 0.5997(3) 0.0427(13) Uani 1 1 d . A . F1 F 0.5513(4) 0.4550(2) 0.5843(2) 0.0415(10) Uani 1 1 d . . . F2 F 0.7107(4) 0.4402(2) 0.6429(2) 0.0464(11) Uani 1 1 d . . . F3 F 0.6997(4) 0.4900(2) 0.5514(2) 0.0475(11) Uani 1 1 d . . . F4 F 0.9664(5) 0.6713(3) 0.8542(3) 0.0747(9) Uani 1 1 d . . . F5 F 1.0068(5) 0.7252(3) 0.7724(3) 0.0747(9) Uani 1 1 d . . . F6 F 1.0530(5) 0.6300(3) 0.7790(3) 0.0747(9) Uani 1 1 d . . . F7 F 0.6376(4) 0.4717(2) 0.3725(3) 0.0580(14) Uani 1 1 d . . . F8 F 0.7958(4) 0.4671(2) 0.4347(3) 0.0499(12) Uani 1 1 d . . . F9 F 0.7841(4) 0.5059(3) 0.3385(2) 0.0572(13) Uani 1 1 d . . . F10 F 1.0457(5) 0.5861(2) 0.4079(3) 0.0582(14) Uani 1 1 d . . . F11 F 1.1673(4) 0.6475(3) 0.4586(3) 0.0594(14) Uani 1 1 d . . . F12 F 1.1076(4) 0.6636(2) 0.3560(3) 0.0541(13) Uani 1 1 d . . . F13 F 1.1247(5) 0.9865(3) 0.7416(3) 0.083(2) Uani 1 1 d . . . C3 C 0.2285(11) 0.7208(7) 0.6051(8) 0.0566(13) Uani 0.573(11) 1 d PD A 1 F14 F 0.1745(9) 0.6672(5) 0.6004(7) 0.0566(13) Uani 0.573(11) 1 d PD A 1 F15 F 0.1677(8) 0.7591(5) 0.5619(7) 0.0566(13) Uani 0.573(11) 1 d PD A 1 F16 F 0.2262(9) 0.7448(5) 0.6645(6) 0.0566(13) Uani 0.573(11) 1 d PD A 1 C3A C 0.2423(13) 0.7130(9) 0.6215(10) 0.0566(13) Uani 0.427(11) 1 d PD A 2 F14A F 0.1962(12) 0.6572(7) 0.6179(9) 0.0566(13) Uani 0.427(11) 1 d PD A 2 F15A F 0.1689(10) 0.7554(6) 0.5955(9) 0.0566(13) Uani 0.427(11) 1 d PD A 2 F16A F 0.2687(12) 0.7273(7) 0.6849(7) 0.0566(13) Uani 0.427(11) 1 d PD A 2 F17 F 0.486(2) 0.8931(7) 0.8031(6) 0.0516(10) Uani 0.472(16) 1 d PD B 1 F18 F 0.5532(13) 0.9453(5) 0.7302(7) 0.0516(10) Uani 0.472(16) 1 d PD B 1 F19 F 0.3914(10) 0.9050(7) 0.7065(6) 0.0516(10) Uani 0.472(16) 1 d PD B 1 F18A F 0.5895(10) 0.9305(5) 0.7420(6) 0.0516(10) Uani 0.528(16) 1 d PD B 2 F17A F 0.4822(19) 0.8818(6) 0.8028(6) 0.0516(10) Uani 0.528(16) 1 d PD B 2 F19A F 0.4132(10) 0.9273(6) 0.7089(5) 0.0516(10) Uani 0.528(16) 1 d PD B 2 O6 O 0.4760(10) 0.7994(6) 0.4034(6) 0.0386(4) Uani 0.425(6) 1 d PD B 1 C7 C 0.4668(13) 0.7490(8) 0.3575(9) 0.0386(4) Uani 0.425(6) 1 d PD B 1 H7A H 0.5001 0.7096 0.3765 0.046 Uiso 0.425(6) 1 calc PR B 1 H7B H 0.4940 0.7592 0.3154 0.046 Uiso 0.425(6) 1 calc PR B 1 C6 C 0.3483(12) 0.7508(5) 0.3531(5) 0.0386(4) Uani 0.425(6) 1 d PD B 1 F20 F 0.3217(8) 0.7312(5) 0.4159(5) 0.0386(4) Uani 0.425(6) 1 d PD B 1 F21 F 0.2531(8) 0.7830(5) 0.3372(5) 0.0386(4) Uani 0.425(6) 1 d PD B 1 F22 F 0.3101(9) 0.6966(5) 0.3092(5) 0.0386(4) Uani 0.425(6) 1 d PD B 1 O6A O 0.5039(8) 0.8153(4) 0.3930(5) 0.0386(4) Uani 0.575(6) 1 d PD B 2 C7A C 0.4474(10) 0.7649(6) 0.3578(7) 0.0386(4) Uani 0.575(6) 1 d PD B 2 H7AA H 0.4778 0.7258 0.3793 0.046 Uiso 0.575(6) 1 calc PR B 2 H7AB H 0.4679 0.7652 0.3126 0.046 Uiso 0.575(6) 1 calc PR B 2 C6A C 0.3262(10) 0.7602(5) 0.3506(5) 0.0386(4) Uani 0.575(6) 1 d PD B 2 F20A F 0.2963(6) 0.7603(4) 0.4130(4) 0.0386(4) Uani 0.575(6) 1 d PD B 2 F21A F 0.2888(6) 0.8131(3) 0.3288(4) 0.0386(4) Uani 0.575(6) 1 d PD B 2 F22A F 0.2832(6) 0.7152(4) 0.3096(4) 0.0386(4) Uani 0.575(6) 1 d PD B 2 C9A C 0.6887(19) 0.8877(8) 0.3937(12) 0.076(5) Uani 0.76(4) 1 d PDU C 1 H9AA H 0.6766 0.8522 0.3623 0.091 Uiso 0.76(4) 1 calc PR C 1 H9AB H 0.7693 0.8918 0.4083 0.091 Uiso 0.76(4) 1 calc PR C 1 C8A C 0.6463(10) 0.9452(7) 0.3603(6) 0.074(2) Uani 0.76(4) 1 d PDU C 1 F23A F 0.6853(16) 0.9565(7) 0.3040(9) 0.074(4) Uani 0.76(4) 1 d PDU C 1 F24A F 0.5327(9) 0.9450(8) 0.3415(9) 0.088(3) Uani 0.76(4) 1 d PDU C 1 F25A F 0.6611(19) 0.9934(7) 0.4011(7) 0.091(4) Uani 0.76(4) 1 d PDU C 1 C9B C 0.672(7) 0.880(2) 0.378(4) 0.076(5) Uani 0.24(4) 1 d PDU C 2 H9BA H 0.7515 0.8698 0.3796 0.091 Uiso 0.24(4) 1 calc PR C 2 H9BB H 0.6271 0.8523 0.3457 0.091 Uiso 0.24(4) 1 calc PR C 2 C8B C 0.649(2) 0.9461(18) 0.3649(15) 0.074(2) Uani 0.24(4) 1 d PDU C 2 F23B F 0.719(3) 0.965(2) 0.326(2) 0.074(4) Uani 0.24(4) 1 d PDU C 2 F24B F 0.549(3) 0.933(3) 0.325(2) 0.088(3) Uani 0.24(4) 1 d PDU C 2 F25B F 0.616(5) 0.992(3) 0.401(2) 0.091(4) Uani 0.24(4) 1 d PDU C 2 P1 P 0.77812(13) 0.63345(8) 0.62706(9) 0.0260(4) Uani 1 1 d . B . P2 P 0.82818(14) 0.64807(8) 0.49495(9) 0.0275(4) Uani 1 1 d . . . P3 P 0.58054(18) 0.80927(10) 0.46183(10) 0.0411(5) Uani 1 1 d D B . P4 P 0.52054(16) 0.78917(9) 0.59096(11) 0.0386(4) Uani 1 1 d . A . Cl1 Cl 0.84395(17) 0.79701(9) 0.50159(10) 0.0439(4) Uani 1 1 d . . . Cl2 Cl 0.70969(17) 0.72072(9) 0.36340(9) 0.0432(5) Uani 1 1 d . . . Cl3 Cl 0.55278(13) 0.65730(8) 0.50631(9) 0.0349(4) Uani 1 1 d . B . Cl4 Cl 0.57063(14) 0.67718(8) 0.70067(9) 0.0352(4) Uani 1 1 d . B . Rh1 Rh 0.64898(4) 0.71081(2) 0.60252(3) 0.02712(15) Uani 1 1 d . . . Rh2 Rh 0.69818(4) 0.72577(3) 0.48237(3) 0.03018(16) Uani 1 1 d . B . 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 0.064(2) 0.027(3) 0.0635(19) -0.0073(17) 0.0088(17) 0.014(2) C2 0.056(5) 0.034(4) 0.038(4) -0.001(3) 0.011(3) 0.005(4) C4 0.036(2) 0.053(2) 0.082(4) -0.013(2) 0.012(2) -0.0018(16) C5 0.044(3) 0.037(3) 0.052(3) 0.000(2) 0.005(2) 0.023(2) C10 0.037(4) 0.037(4) 0.048(4) 0.005(3) 0.013(3) 0.003(3) C11 0.032(4) 0.027(4) 0.060(5) 0.007(3) 0.010(3) 0.001(3) C12 0.033(4) 0.026(4) 0.062(5) -0.010(3) 0.014(3) 0.001(3) C13 0.027(4) 0.027(4) 0.048(4) -0.005(3) 0.003(3) 0.005(3) C14 0.023(3) 0.029(4) 0.052(4) 0.005(3) 0.005(3) 0.010(3) C15 0.030(4) 0.024(3) 0.045(4) 0.000(3) 0.007(3) -0.003(3) C16 0.027(3) 0.025(4) 0.050(4) -0.004(3) 0.010(3) -0.007(3) C17 0.0558(19) 0.090(2) 0.0730(19) -0.0230(18) -0.0104(15) 0.0057(17) C18 0.0558(19) 0.090(2) 0.0730(19) -0.0230(18) -0.0104(15) 0.0057(17) C19 0.026(2) 0.023(2) 0.058(3) 0.003(2) -0.001(2) 0.0001(17) C20 0.043(2) 0.055(2) 0.092(3) -0.026(2) 0.017(2) -0.0180(18) C21 0.043(2) 0.055(2) 0.092(3) -0.026(2) 0.017(2) -0.0180(18) C22 0.043(2) 0.055(2) 0.092(3) -0.026(2) 0.017(2) -0.0180(18) C23 0.043(2) 0.055(2) 0.092(3) -0.026(2) 0.017(2) -0.0180(18) C24 0.043(2) 0.055(2) 0.092(3) -0.026(2) 0.017(2) -0.0180(18) C25 0.043(2) 0.055(2) 0.092(3) -0.026(2) 0.017(2) -0.0180(18) N1 0.044(3) 0.037(3) 0.052(3) 0.000(2) 0.005(2) 0.023(2) N2 0.019(3) 0.015(3) 0.050(3) 0.001(2) 0.006(2) 0.005(2) N3 0.026(2) 0.023(2) 0.058(3) 0.003(2) -0.001(2) 0.0001(17) O1 0.020(2) 0.026(2) 0.051(3) 0.001(2) 0.007(2) -0.0009(19) O2 0.019(2) 0.027(3) 0.050(3) -0.006(2) 0.004(2) 0.0009(18) O3 0.019(2) 0.032(3) 0.045(3) 0.001(2) -0.0011(19) -0.0031(19) O4 0.022(2) 0.021(2) 0.050(3) -0.002(2) 0.006(2) -0.0029(18) O5 0.075(4) 0.040(3) 0.076(4) 0.020(3) 0.037(3) 0.030(3) O7 0.037(3) 0.023(3) 0.049(3) -0.001(2) 0.010(2) 0.002(2) O8 0.026(3) 0.026(3) 0.076(4) -0.005(2) 0.006(2) 0.008(2) F1 0.037(2) 0.033(2) 0.054(3) -0.0061(19) 0.0058(19) -0.0133(19) F2 0.043(3) 0.028(2) 0.070(3) 0.004(2) 0.010(2) 0.0041(19) F3 0.056(3) 0.036(3) 0.057(3) -0.009(2) 0.029(2) -0.010(2) F4 0.0558(19) 0.090(2) 0.0730(19) -0.0230(18) -0.0104(15) 0.0057(17) F5 0.0558(19) 0.090(2) 0.0730(19) -0.0230(18) -0.0104(15) 0.0057(17) F6 0.0558(19) 0.090(2) 0.0730(19) -0.0230(18) -0.0104(15) 0.0057(17) F7 0.035(3) 0.043(3) 0.096(4) -0.027(3) 0.009(2) -0.007(2) F8 0.044(3) 0.028(2) 0.079(3) -0.002(2) 0.012(2) 0.012(2) F9 0.064(3) 0.057(3) 0.056(3) -0.020(2) 0.027(3) -0.006(3) F10 0.070(4) 0.031(3) 0.081(4) -0.004(2) 0.035(3) 0.005(2) F11 0.032(2) 0.083(4) 0.062(3) 0.007(3) 0.004(2) 0.011(3) F12 0.052(3) 0.057(3) 0.059(3) 0.008(2) 0.025(2) 0.005(2) F13 0.068(4) 0.080(4) 0.096(5) -0.013(4) -0.001(3) -0.046(4) C3 0.036(2) 0.053(2) 0.082(4) -0.013(2) 0.012(2) -0.0018(16) F14 0.036(2) 0.053(2) 0.082(4) -0.013(2) 0.012(2) -0.0018(16) F15 0.036(2) 0.053(2) 0.082(4) -0.013(2) 0.012(2) -0.0018(16) F16 0.036(2) 0.053(2) 0.082(4) -0.013(2) 0.012(2) -0.0018(16) C3A 0.036(2) 0.053(2) 0.082(4) -0.013(2) 0.012(2) -0.0018(16) F14A 0.036(2) 0.053(2) 0.082(4) -0.013(2) 0.012(2) -0.0018(16) F15A 0.036(2) 0.053(2) 0.082(4) -0.013(2) 0.012(2) -0.0018(16) F16A 0.036(2) 0.053(2) 0.082(4) -0.013(2) 0.012(2) -0.0018(16) F17 0.064(2) 0.027(3) 0.0635(19) -0.0073(17) 0.0088(17) 0.014(2) F18 0.064(2) 0.027(3) 0.0635(19) -0.0073(17) 0.0088(17) 0.014(2) F19 0.064(2) 0.027(3) 0.0635(19) -0.0073(17) 0.0088(17) 0.014(2) F18A 0.064(2) 0.027(3) 0.0635(19) -0.0073(17) 0.0088(17) 0.014(2) F17A 0.064(2) 0.027(3) 0.0635(19) -0.0073(17) 0.0088(17) 0.014(2) F19A 0.064(2) 0.027(3) 0.0635(19) -0.0073(17) 0.0088(17) 0.014(2) O6 0.0275(8) 0.0274(9) 0.0604(10) -0.0018(7) 0.0048(7) 0.0080(6) C7 0.0275(8) 0.0274(9) 0.0604(10) -0.0018(7) 0.0048(7) 0.0080(6) C6 0.0275(8) 0.0274(9) 0.0604(10) -0.0018(7) 0.0048(7) 0.0080(6) F20 0.0275(8) 0.0274(9) 0.0604(10) -0.0018(7) 0.0048(7) 0.0080(6) F21 0.0275(8) 0.0274(9) 0.0604(10) -0.0018(7) 0.0048(7) 0.0080(6) F22 0.0275(8) 0.0274(9) 0.0604(10) -0.0018(7) 0.0048(7) 0.0080(6) O6A 0.0275(8) 0.0274(9) 0.0604(10) -0.0018(7) 0.0048(7) 0.0080(6) C7A 0.0275(8) 0.0274(9) 0.0604(10) -0.0018(7) 0.0048(7) 0.0080(6) C6A 0.0275(8) 0.0274(9) 0.0604(10) -0.0018(7) 0.0048(7) 0.0080(6) F20A 0.0275(8) 0.0274(9) 0.0604(10) -0.0018(7) 0.0048(7) 0.0080(6) F21A 0.0275(8) 0.0274(9) 0.0604(10) -0.0018(7) 0.0048(7) 0.0080(6) F22A 0.0275(8) 0.0274(9) 0.0604(10) -0.0018(7) 0.0048(7) 0.0080(6) C9A 0.097(8) 0.055(5) 0.089(9) 0.031(6) 0.058(7) 0.037(6) C8A 0.095(6) 0.051(5) 0.088(6) 0.027(4) 0.055(5) 0.033(5) F23A 0.096(8) 0.059(5) 0.075(7) 0.021(5) 0.043(7) 0.022(5) F24A 0.093(5) 0.078(8) 0.102(8) 0.036(5) 0.049(4) 0.033(4) F25A 0.144(11) 0.052(4) 0.089(5) 0.014(3) 0.057(7) 0.031(7) C9B 0.097(8) 0.055(5) 0.089(9) 0.031(6) 0.058(7) 0.037(6) C8B 0.095(6) 0.051(5) 0.088(6) 0.027(4) 0.055(5) 0.033(5) F23B 0.096(8) 0.059(5) 0.075(7) 0.021(5) 0.043(7) 0.022(5) F24B 0.093(5) 0.078(8) 0.102(8) 0.036(5) 0.049(4) 0.033(4) F25B 0.144(11) 0.052(4) 0.089(5) 0.014(3) 0.057(7) 0.031(7) P1 0.0179(8) 0.0186(8) 0.0407(9) -0.0009(7) 0.0020(6) 0.0002(6) P2 0.0213(8) 0.0191(8) 0.0417(9) -0.0019(7) 0.0031(7) 0.0015(6) P3 0.0456(12) 0.0356(11) 0.0401(10) -0.0025(8) 0.0000(8) 0.0207(9) P4 0.0275(8) 0.0274(9) 0.0604(10) -0.0018(7) 0.0048(7) 0.0080(6) Cl1 0.0472(11) 0.0287(9) 0.0572(11) -0.0011(8) 0.0124(9) -0.0023(8) Cl2 0.0488(11) 0.0392(10) 0.0400(10) -0.0025(8) 0.0008(8) 0.0172(8) Cl3 0.0207(8) 0.0309(9) 0.0516(10) -0.0144(7) 0.0003(7) 0.0027(6) Cl4 0.0318(9) 0.0265(9) 0.0486(10) -0.0026(7) 0.0102(7) 0.0037(7) Rh1 0.0201(3) 0.0194(3) 0.0410(3) -0.0044(2) 0.0013(2) 0.00167(19) Rh2 0.0269(3) 0.0234(3) 0.0388(3) -0.0029(2) 0.0001(2) 0.0070(2) _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 F18 1.331(14) . ? C1 F19A 1.332(13) . ? C1 F17 1.334(15) . ? C1 F17A 1.362(14) . ? C1 F18A 1.372(13) . ? C1 F19 1.387(14) . ? C1 C2 1.460(11) . ? C2 O7 1.433(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C4 O8 1.434(10) . ? C4 C3A 1.490(17) . ? C4 C3 1.498(15) . ? C4 H4AA 0.9900 . ? C4 H4AB 0.9900 . ? C4 H4BC 0.9900 . ? C4 H4BD 0.9900 . ? C5 N1 1.506(9) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C10 F12 1.321(9) . ? C10 F11 1.333(9) . ? C10 F10 1.337(9) . ? C10 C11 1.504(10) . ? C11 O1 1.423(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 F8 1.317(10) . ? C12 F9 1.318(9) . ? C12 F7 1.327(9) . ? C12 C13 1.519(10) . ? C13 O2 1.424(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N2 1.485(8) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 F2 1.328(8) . ? C15 F3 1.336(8) . ? C15 F1 1.341(8) . ? C15 C16 1.495(10) . ? C16 O4 1.437(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 F4 1.331(13) . ? C17 F5 1.335(15) . ? C17 F6 1.341(13) . ? C17 C18 1.472(15) . ? C18 O3 1.434(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 N3 1.129(9) . ? C19 Rh1 1.934(7) . ? C20 C21 1.358(13) . ? C20 C25 1.369(13) . ? C20 N3 1.392(11) . ? C21 C22 1.384(12) . ? C21 H21 0.9500 . ? C22 C23 1.336(13) . ? C22 H22 0.9500 . ? C23 F13 1.347(10) . ? C23 C24 1.367(13) . ? C24 C25 1.392(12) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? N1 P4 1.643(7) . ? N1 P3 1.661(7) . ? N2 P1 1.651(6) . ? N2 P2 1.664(6) . ? O1 P2 1.580(5) . ? O2 P2 1.601(5) . ? O3 P1 1.592(5) . ? O4 P1 1.593(5) . ? O5 C9A 1.419(15) . ? O5 C9B 1.59(5) . ? O5 P3 1.601(7) . ? O7 P4 1.590(5) . ? O8 P4 1.587(5) . ? C3 F14 1.317(14) . ? C3 F16 1.319(15) . ? C3 F15 1.346(16) . ? C3A F14A 1.317(16) . ? C3A F16A 1.322(18) . ? C3A F15A 1.329(18) . ? O6 C7 1.420(16) . ? O6 P3 1.629(11) . ? C7 C6 1.44(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C6 F21 1.348(13) . ? C6 F20 1.429(12) . ? C6 F22 1.497(12) . ? O6A C7A 1.419(13) . ? O6A P3 1.574(9) . ? C7A C6A 1.468(16) . ? C7A H7AA 0.9900 . ? C7A H7AB 0.9900 . ? C6A F21A 1.274(11) . ? C6A F22A 1.332(11) . ? C6A F20A 1.374(11) . ? C9A C8A 1.464(16) . ? C9A H9AA 0.9900 . ? C9A H9AB 0.9900 . ? C8A F25A 1.321(12) . ? C8A F23A 1.328(12) . ? C8A F24A 1.384(15) . ? C9B C8B 1.47(2) . ? C9B H9BA 0.9900 . ? C9B H9BB 0.9900 . ? C8B F23B 1.315(16) . ? C8B F25B 1.322(17) . ? C8B F24B 1.38(2) . ? P1 Rh1 2.2893(17) . ? P2 Rh2 2.2858(17) . ? P3 Rh2 2.2913(19) . ? P4 Rh1 2.2833(19) . ? Cl1 Rh2 2.331(2) . ? Cl2 Rh2 2.454(2) . ? Cl3 Rh2 2.4046(19) . ? Cl3 Rh1 2.4228(17) . ? Cl4 Rh1 2.4486(19) . ? Rh1 Rh2 2.6260(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F18 C1 F19A 81.8(8) . . ? F18 C1 F17 105.3(11) . . ? F19A C1 F17 105.8(13) . . ? F18 C1 F17A 115.1(11) . . ? F19A C1 F17A 109.8(12) . . ? F17 C1 F17A 10.4(11) . . ? F18 C1 F18A 24.3(6) . . ? F19A C1 F18A 106.1(9) . . ? F17 C1 F18A 99.1(12) . . ? F17A C1 F18A 106.6(12) . . ? F18 C1 F19 104.2(9) . . ? F19A C1 F19 23.0(6) . . ? F17 C1 F19 104.4(14) . . ? F17A C1 F19 104.1(13) . . ? F18A C1 F19 128.2(9) . . ? F18 C1 C2 121.4(10) . . ? F19A C1 C2 121.2(9) . . ? F17 C1 C2 115.7(10) . . ? F17A C1 C2 106.1(9) . . ? F18A C1 C2 106.2(9) . . ? F19 C1 C2 103.9(9) . . ? O7 C2 C1 107.4(7) . . ? O7 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? O7 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? O8 C4 C3A 108.1(10) . . ? O8 C4 C3 106.3(9) . . ? C3A C4 C3 15.0(9) . . ? O8 C4 H4AA 110.5 . . ? C3A C4 H4AA 96.4 . . ? C3 C4 H4AA 110.5 . . ? O8 C4 H4AB 110.5 . . ? C3A C4 H4AB 121.7 . . ? C3 C4 H4AB 110.5 . . ? H4AA C4 H4AB 108.7 . . ? O8 C4 H4BC 110.1 . . ? C3A C4 H4BC 110.1 . . ? C3 C4 H4BC 123.4 . . ? H4AA C4 H4BC 15.0 . . ? H4AB C4 H4BC 95.6 . . ? O8 C4 H4BD 110.1 . . ? C3A C4 H4BD 110.1 . . ? C3 C4 H4BD 97.6 . . ? H4AA C4 H4BD 120.4 . . ? H4AB C4 H4BD 14.2 . . ? H4BC C4 H4BD 108.4 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? F12 C10 F11 107.7(6) . . ? F12 C10 F10 108.7(7) . . ? F11 C10 F10 106.0(7) . . ? F12 C10 C11 110.1(6) . . ? F11 C10 C11 112.9(7) . . ? F10 C10 C11 111.3(6) . . ? O1 C11 C10 108.7(6) . . ? O1 C11 H11A 109.9 . . ? C10 C11 H11A 109.9 . . ? O1 C11 H11B 109.9 . . ? C10 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? F8 C12 F9 106.9(6) . . ? F8 C12 F7 109.1(7) . . ? F9 C12 F7 107.9(7) . . ? F8 C12 C13 111.7(7) . . ? F9 C12 C13 112.1(6) . . ? F7 C12 C13 109.1(6) . . ? O2 C13 C12 106.7(6) . . ? O2 C13 H13A 110.4 . . ? C12 C13 H13A 110.4 . . ? O2 C13 H13B 110.4 . . ? C12 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? F2 C15 F3 106.7(6) . . ? F2 C15 F1 107.6(6) . . ? F3 C15 F1 107.2(6) . . ? F2 C15 C16 113.7(6) . . ? F3 C15 C16 112.1(6) . . ? F1 C15 C16 109.3(6) . . ? O4 C16 C15 108.3(5) . . ? O4 C16 H16A 110.0 . . ? C15 C16 H16A 110.0 . . ? O4 C16 H16B 110.0 . . ? C15 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? F4 C17 F5 107.0(9) . . ? F4 C17 F6 108.7(9) . . ? F5 C17 F6 104.2(10) . . ? F4 C17 C18 110.8(10) . . ? F5 C17 C18 112.4(11) . . ? F6 C17 C18 113.2(10) . . ? O3 C18 C17 106.6(10) . . ? O3 C18 H18A 110.4 . . ? C17 C18 H18A 110.4 . . ? O3 C18 H18B 110.4 . . ? C17 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? N3 C19 Rh1 176.1(8) . . ? C21 C20 C25 121.4(9) . . ? C21 C20 N3 120.4(8) . . ? C25 C20 N3 118.2(8) . . ? C20 C21 C22 119.9(9) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 118.7(9) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 F13 118.8(9) . . ? C22 C23 C24 122.6(9) . . ? F13 C23 C24 118.6(9) . . ? C23 C24 C25 119.0(9) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C20 C25 C24 118.3(9) . . ? C20 C25 H25 120.9 . . ? C24 C25 H25 120.9 . . ? C5 N1 P4 120.0(5) . . ? C5 N1 P3 119.5(5) . . ? P4 N1 P3 120.4(4) . . ? C14 N2 P1 120.2(5) . . ? C14 N2 P2 119.9(5) . . ? P1 N2 P2 119.6(3) . . ? C19 N3 C20 173.0(9) . . ? C11 O1 P2 122.2(5) . . ? C13 O2 P2 122.5(4) . . ? C18 O3 P1 121.3(5) . . ? C16 O4 P1 124.3(5) . . ? C9A O5 C9B 13(4) . . ? C9A O5 P3 122.5(10) . . ? C9B O5 P3 112(3) . . ? C2 O7 P4 121.1(5) . . ? C4 O8 P4 127.0(5) . . ? F14 C3 F16 109.2(13) . . ? F14 C3 F15 105.0(11) . . ? F16 C3 F15 106.3(11) . . ? F14 C3 C4 111.0(11) . . ? F16 C3 C4 113.6(11) . . ? F15 C3 C4 111.3(12) . . ? F14A C3A F16A 107.8(15) . . ? F14A C3A F15A 109.8(14) . . ? F16A C3A F15A 106.7(14) . . ? F14A C3A C4 110.2(14) . . ? F16A C3A C4 110.2(14) . . ? F15A C3A C4 112.0(15) . . ? C7 O6 P3 124.0(11) . . ? O6 C7 C6 90.2(10) . . ? O6 C7 H7A 113.6 . . ? C6 C7 H7A 113.6 . . ? O6 C7 H7B 113.6 . . ? C6 C7 H7B 113.6 . . ? H7A C7 H7B 110.9 . . ? F21 C6 F20 93.7(10) . . ? F21 C6 C7 148.6(13) . . ? F20 C6 C7 107.0(11) . . ? F21 C6 F22 94.0(9) . . ? F20 C6 F22 102.5(10) . . ? C7 C6 F22 103.9(10) . . ? C7A O6A P3 124.8(9) . . ? O6A C7A C6A 120.8(10) . . ? O6A C7A H7AA 107.1 . . ? C6A C7A H7AA 107.1 . . ? O6A C7A H7AB 107.1 . . ? C6A C7A H7AB 107.1 . . ? H7AA C7A H7AB 106.8 . . ? F21A C6A F22A 109.5(9) . . ? F21A C6A F20A 101.0(8) . . ? F22A C6A F20A 116.7(10) . . ? F21A C6A C7A 106.2(10) . . ? F22A C6A C7A 114.3(9) . . ? F20A C6A C7A 107.8(9) . . ? O5 C9A C8A 110.5(12) . . ? O5 C9A H9AA 109.6 . . ? C8A C9A H9AA 109.6 . . ? O5 C9A H9AB 109.6 . . ? C8A C9A H9AB 109.6 . . ? H9AA C9A H9AB 108.1 . . ? F25A C8A F23A 111.8(11) . . ? F25A C8A F24A 102.5(11) . . ? F23A C8A F24A 103.4(10) . . ? F25A C8A C9A 110.8(18) . . ? F23A C8A C9A 114.1(12) . . ? F24A C8A C9A 113.4(15) . . ? C8B C9B O5 98(3) . . ? C8B C9B H9BA 112.1 . . ? O5 C9B H9BA 112.1 . . ? C8B C9B H9BB 112.1 . . ? O5 C9B H9BB 112.1 . . ? H9BA C9B H9BB 109.7 . . ? F23B C8B F25B 112(3) . . ? F23B C8B F24B 108(3) . . ? F25B C8B F24B 100(2) . . ? F23B C8B C9B 107(3) . . ? F25B C8B C9B 133(4) . . ? F24B C8B C9B 92(6) . . ? O3 P1 O4 97.7(3) . . ? O3 P1 N2 100.0(3) . . ? O4 P1 N2 105.3(3) . . ? O3 P1 Rh1 115.9(2) . . ? O4 P1 Rh1 117.55(18) . . ? N2 P1 Rh1 117.4(2) . . ? O1 P2 O2 98.2(3) . . ? O1 P2 N2 99.2(3) . . ? O2 P2 N2 104.3(3) . . ? O1 P2 Rh2 118.5(2) . . ? O2 P2 Rh2 116.65(19) . . ? N2 P2 Rh2 116.9(2) . . ? O6A P3 O5 89.4(5) . . ? O6A P3 O6 19.5(5) . . ? O5 P3 O6 107.1(6) . . ? O6A P3 N1 109.3(4) . . ? O5 P3 N1 98.8(3) . . ? O6 P3 N1 97.9(5) . . ? O6A P3 Rh2 120.1(4) . . ? O5 P3 Rh2 117.4(3) . . ? O6 P3 Rh2 115.9(5) . . ? N1 P3 Rh2 116.8(2) . . ? O8 P4 O7 98.1(3) . . ? O8 P4 N1 104.8(3) . . ? O7 P4 N1 100.4(3) . . ? O8 P4 Rh1 118.1(2) . . ? O7 P4 Rh1 116.0(2) . . ? N1 P4 Rh1 116.5(2) . . ? Rh2 Cl3 Rh1 65.91(5) . . ? C19 Rh1 P4 87.7(2) . . ? C19 Rh1 P1 89.4(2) . . ? P4 Rh1 P1 173.37(8) . . ? C19 Rh1 Cl3 154.0(2) . . ? P4 Rh1 Cl3 91.06(7) . . ? P1 Rh1 Cl3 94.19(6) . . ? C19 Rh1 Cl4 97.0(2) . . ? P4 Rh1 Cl4 87.49(7) . . ? P1 Rh1 Cl4 86.97(6) . . ? Cl3 Rh1 Cl4 108.83(7) . . ? C19 Rh1 Rh2 97.5(2) . . ? P4 Rh1 Rh2 93.48(6) . . ? P1 Rh1 Rh2 92.79(5) . . ? Cl3 Rh1 Rh2 56.71(5) . . ? Cl4 Rh1 Rh2 165.51(5) . . ? P2 Rh2 P3 173.29(8) . . ? P2 Rh2 Cl1 87.48(7) . . ? P3 Rh2 Cl1 87.94(8) . . ? P2 Rh2 Cl3 93.16(6) . . ? P3 Rh2 Cl3 92.90(8) . . ? Cl1 Rh2 Cl3 158.62(7) . . ? P2 Rh2 Cl2 86.59(6) . . ? P3 Rh2 Cl2 88.72(7) . . ? Cl1 Rh2 Cl2 92.47(8) . . ? Cl3 Rh2 Cl2 108.90(7) . . ? P2 Rh2 Rh1 93.19(5) . . ? P3 Rh2 Rh1 92.50(6) . . ? Cl1 Rh2 Rh1 101.24(6) . . ? Cl3 Rh2 Rh1 57.38(5) . . ? Cl2 Rh2 Rh1 166.26(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.734 _refine_diff_density_min -2.431 _refine_diff_density_rms 0.169 data_Compound_9 _database_code_depnum_ccdc_archive 'CCDC 925038' #TrackingRef '17866_web_deposit_cif_file_0_DavidPowers_1361207103.Cif Files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H37 Cl4 F24 N3 O9 P4 Rh2' _chemical_formula_weight 1547.16 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' Cl Cl 0.1484 0.1585 '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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7825(5) _cell_length_b 15.2029(8) _cell_length_c 18.7253(9) _cell_angle_alpha 87.9830(10) _cell_angle_beta 80.0650(10) _cell_angle_gamma 73.2230(10) _cell_volume 2894.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 0.990 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8266 _exptl_absorpt_correction_T_max 0.9075 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 74141 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 28.32 _reflns_number_total 14427 _reflns_number_gt 12029 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0783P)^2^+11.7463P] 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 14427 _refine_ls_number_parameters 771 _refine_ls_number_restraints 502 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1598 _refine_ls_wR_factor_gt 0.1486 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.041 _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 -0.0233(5) 0.4345(3) 0.7885(3) 0.0397(11) Uani 1 1 d . . . H1A H 0.0663 0.4139 0.7611 0.059 Uiso 1 1 calc R . . H1B H -0.0687 0.3880 0.7843 0.059 Uiso 1 1 calc R . . H1C H -0.0199 0.4433 0.8397 0.059 Uiso 1 1 calc R . . C2 C -0.4741(5) 0.9812(3) 0.6063(3) 0.0391(11) Uani 1 1 d . . . H2A H -0.5200 1.0246 0.6463 0.059 Uiso 1 1 calc R . . H2B H -0.5382 0.9699 0.5792 0.059 Uiso 1 1 calc R . . H2C H -0.4124 1.0071 0.5739 0.059 Uiso 1 1 calc R . . C3 C -0.4258(5) 0.5129(3) 0.8696(3) 0.0336(10) Uani 1 1 d . . . H3A H -0.4720 0.5085 0.8291 0.040 Uiso 1 1 calc R . . H3B H -0.4824 0.5637 0.9025 0.040 Uiso 1 1 calc R . . C4 C -0.3984(6) 0.4244(4) 0.9098(3) 0.0432(12) Uani 1 1 d . . . C5 C -0.2792(5) 0.4416(3) 0.6522(3) 0.0352(10) Uani 1 1 d . . . H5A H -0.2849 0.4995 0.6253 0.042 Uiso 1 1 calc R . . H5B H -0.3575 0.4217 0.6484 0.042 Uiso 1 1 calc R . . C6 C -0.1565(6) 0.3691(3) 0.6213(3) 0.0435(12) Uani 1 1 d . . . C7 C 0.1310(5) 0.5467(3) 0.6077(2) 0.0348(10) Uani 1 1 d . F . H7A H 0.1345 0.6070 0.5872 0.042 Uiso 1 1 calc R . . H7B H 0.0578 0.5301 0.5916 0.042 Uiso 1 1 calc R . . C8 C 0.2585(5) 0.4748(4) 0.5838(3) 0.0363(10) Uani 1 1 d . . . C9 C 0.1314(4) 0.6558(3) 0.8100(3) 0.0310(9) Uani 1 1 d . F . H9A H 0.0924 0.7229 0.8060 0.037 Uiso 1 1 calc R . . H9B H 0.2064 0.6349 0.7698 0.037 Uiso 1 1 calc R . . C10 C 0.1759(5) 0.6341(3) 0.8812(3) 0.0396(11) Uani 1 1 d D . . C11 C -0.5092(8) 0.7318(4) 0.5468(4) 0.0599(18) Uani 1 1 d U D . H11A H -0.5269 0.6755 0.5688 0.072 Uiso 1 1 calc R . . H11B H -0.4136 0.7182 0.5291 0.072 Uiso 1 1 calc R . . C12 C -0.5810(6) 0.7602(4) 0.4872(3) 0.0506(13) Uani 1 1 d U . . C15 C -0.1674(5) 0.9946(3) 0.7182(3) 0.0420(11) Uani 1 1 d U C . H15A H -0.0818 0.9545 0.6939 0.050 Uiso 1 1 calc R . . H15B H -0.1708 0.9886 0.7713 0.050 Uiso 1 1 calc R . . C16 C -0.1798(6) 1.0899(4) 0.6977(4) 0.0517(13) Uani 1 1 d DU . . C17 C -0.1041(6) 0.8523(4) 0.5164(3) 0.0416(11) Uani 1 1 d DU . . H17A H -0.0941 0.7874 0.5301 0.050 Uiso 0.778(5) 1 calc PR A 1 H17B H -0.0152 0.8605 0.5032 0.050 Uiso 0.778(5) 1 calc PR A 1 H17C H -0.1396 0.7998 0.5124 0.050 Uiso 0.222(5) 1 calc PR A 2 H17D H -0.0095 0.8290 0.5196 0.050 Uiso 0.222(5) 1 calc PR A 2 C19B C -0.2446(10) 0.8610(6) 0.9146(5) 0.0256(18) Uani 0.436(4) 1 d PU B 2 C20A C -0.6055(10) 0.8021(7) 0.9840(5) 0.047(2) Uani 0.564(4) 1 d PU B 1 H20A H -0.6675 0.7762 0.9691 0.056 Uiso 0.564(4) 1 calc PR B 1 C19A C -0.4889(8) 0.8011(5) 0.9373(4) 0.0269(15) Uani 0.564(4) 1 d PU B 1 C20B C -0.1682(13) 0.9067(9) 0.9436(6) 0.043(3) Uani 0.436(4) 1 d PU B 2 H20B H -0.0848 0.9083 0.9180 0.051 Uiso 0.436(4) 1 calc PR B 2 C21A C -0.6288(11) 0.8411(8) 1.0517(5) 0.054(3) Uani 0.564(4) 1 d PU B 1 H21A H -0.7062 0.8406 1.0845 0.065 Uiso 0.564(4) 1 calc PR B 1 C21B C -0.2184(14) 0.9492(10) 1.0106(7) 0.049(3) Uani 0.436(4) 1 d PU B 2 H21B H -0.1730 0.9858 1.0293 0.059 Uiso 0.436(4) 1 calc PR B 2 C22A C -0.5391(8) 0.8820(6) 1.0729(4) 0.0298(15) Uani 0.564(4) 1 d PU B 1 C22B C -0.3343(11) 0.9393(8) 1.0509(6) 0.036(2) Uani 0.436(4) 1 d PU B 2 C23B C -0.428(4) 0.878(4) 1.029(2) 0.039(3) Uani 0.436(4) 1 d PU B 1 H23B H -0.3635 0.9000 1.0454 0.047 Uiso 0.436(4) 1 calc PR B 1 C23A C -0.410(3) 0.891(3) 1.0222(15) 0.039(3) Uani 0.564(4) 1 d PU B 2 H23A H -0.4925 0.8876 1.0478 0.047 Uiso 0.564(4) 1 calc PR B 2 C24A C -0.4030(11) 0.8417(11) 0.9583(7) 0.0424(18) Uani 0.564(4) 1 d PU B 1 H24A H -0.3271 0.8453 0.9254 0.051 Uiso 0.564(4) 1 calc PR B 1 C24B C -0.3566(15) 0.8486(16) 0.9543(10) 0.0424(18) Uani 0.436(4) 1 d PU B 2 H24B H -0.3994 0.8103 0.9354 0.051 Uiso 0.436(4) 1 calc PR B 2 C29A C -0.479(2) 0.9620(18) 1.1665(11) 0.037(3) Uani 0.564(4) 1 d PU B 1 H29A H -0.4695 1.0143 1.1364 0.056 Uiso 0.564(4) 1 calc PR B 1 H29B H -0.3938 0.9156 1.1636 0.056 Uiso 0.564(4) 1 calc PR B 1 H29C H -0.5129 0.9828 1.2170 0.056 Uiso 0.564(4) 1 calc PR B 1 C29B C -0.488(4) 0.968(3) 1.1583(19) 0.048(2) Uani 0.436(4) 1 d PU B 2 H29D H -0.5611 0.9917 1.1314 0.073 Uiso 0.436(4) 1 calc PR B 2 H29E H -0.5085 1.0000 1.2050 0.073 Uiso 0.436(4) 1 calc PR B 2 H29F H -0.4761 0.9018 1.1665 0.073 Uiso 0.436(4) 1 calc PR B 2 C30A C -0.4244(14) 0.7339(14) 0.8104(11) 0.025(2) Uani 0.564(4) 1 d P B 1 C30B C -0.1797(17) 0.7901(10) 0.7868(9) 0.025(2) Uani 0.436(4) 1 d P B 2 N1 N -0.4006(4) 0.8933(3) 0.6359(2) 0.0291(8) Uani 1 1 d . . . N2 N -0.0959(4) 0.5231(2) 0.7588(2) 0.0287(7) Uani 1 1 d . . . N3A N -0.4626(6) 0.7615(4) 0.8681(4) 0.0259(13) Uani 0.564(4) 1 d P B 1 N3B N -0.1996(9) 0.8214(6) 0.8435(7) 0.0272(18) Uani 0.436(4) 1 d P B 2 O1 O -0.3035(3) 0.5299(2) 0.84239(17) 0.0307(7) Uani 1 1 d . . . O2 O -0.2742(3) 0.4559(2) 0.72680(17) 0.0291(6) Uani 1 1 d . . . O3 O 0.0355(3) 0.6085(2) 0.80742(16) 0.0275(6) Uani 1 1 d . . . O4 O 0.1131(3) 0.5503(2) 0.68480(17) 0.0315(7) Uani 1 1 d . . . O5 O -0.6002(4) 0.8780(3) 0.7168(3) 0.0591(6) Uani 1 1 d U B . O6 O -0.5517(4) 0.8054(2) 0.5998(2) 0.0478(10) Uani 1 1 d . . . O7 O -0.2721(3) 0.9670(2) 0.69733(18) 0.0301(6) Uani 1 1 d . . . O8 O -0.1757(3) 0.9109(2) 0.57629(18) 0.0330(7) Uani 1 1 d . A . O9A O -0.5737(6) 0.9211(5) 1.1400(3) 0.0386(15) Uani 0.564(4) 1 d PU B 1 O9B O -0.3704(10) 0.9809(7) 1.1172(5) 0.048(2) Uani 0.436(4) 1 d PU B 2 F1 F -0.1047(6) 1.1265(7) 0.7312(6) 0.055(2) Uani 0.784(7) 1 d PDU C 1 F2 F -0.2962(5) 1.1478(3) 0.7109(4) 0.0638(15) Uani 0.784(7) 1 d PDU C 1 F3 F -0.1431(6) 1.0924(4) 0.6234(3) 0.0656(14) Uani 0.784(7) 1 d PDU C 1 F2A F -0.2924(17) 1.1315(12) 0.7496(12) 0.0638(15) Uani 0.216(7) 1 d PDU C 2 F1A F -0.076(3) 1.111(3) 0.716(3) 0.055(2) Uani 0.216(7) 1 d PDU C 2 F3A F -0.231(2) 1.1448(13) 0.6469(10) 0.0656(14) Uani 0.216(7) 1 d PDU C 2 C18 C -0.1731(7) 0.8738(6) 0.4539(4) 0.0477(17) Uani 0.778(5) 1 d PDU A 1 F4 F -0.1065(5) 0.8225(5) 0.3960(2) 0.0681(15) Uani 0.778(5) 1 d PU A 1 F5 F -0.1979(6) 0.9615(6) 0.4347(4) 0.0715(17) Uani 0.778(5) 1 d PU A 1 F6 F -0.2918(4) 0.8555(4) 0.4701(2) 0.0588(12) Uani 0.778(5) 1 d PU A 1 C18A C -0.127(3) 0.9166(19) 0.4552(12) 0.0477(17) Uani 0.222(5) 1 d PD A 2 F5A F -0.244(2) 0.974(3) 0.4481(17) 0.0715(17) Uani 0.222(5) 1 d PDU A 2 F4A F -0.0513(16) 0.9704(15) 0.4599(8) 0.0681(15) Uani 0.222(5) 1 d PD A 2 F6A F -0.0705(17) 0.8680(15) 0.3929(9) 0.0588(12) Uani 0.222(5) 1 d PDU A 2 F7 F -0.5664(6) 0.8292(4) 0.4498(3) 0.0576(8) Uani 0.689(6) 1 d PU D 1 F8 F -0.5513(10) 0.6975(6) 0.4365(5) 0.0576(8) Uani 0.689(6) 1 d PU D 1 F9 F -0.7150(6) 0.7848(5) 0.5101(3) 0.0576(8) Uani 0.689(6) 1 d PU D 1 F7A F -0.6572(13) 0.8443(9) 0.4806(6) 0.0576(8) Uani 0.311(6) 1 d PU D 2 F9A F -0.7021(13) 0.7443(10) 0.5273(7) 0.0576(8) Uani 0.311(6) 1 d PU D 2 F8A F -0.563(2) 0.6799(14) 0.4445(12) 0.0576(8) Uani 0.311(6) 1 d PU D 2 C13 C -0.7130(5) 0.8470(4) 0.7423(4) 0.0591(6) Uani 1 1 d U . . H13A H -0.6856 0.7869 0.7661 0.071 Uiso 0.399(5) 1 calc PR E 1 H13B H -0.7543 0.8385 0.7008 0.071 Uiso 0.399(5) 1 calc PR E 1 H13C H -0.6974 0.8051 0.7836 0.071 Uiso 0.601(5) 1 calc PR E 2 H13D H -0.7329 0.8138 0.7032 0.071 Uiso 0.601(5) 1 calc PR E 2 C14 C -0.8086(16) 0.9134(12) 0.7940(12) 0.0591(6) Uani 0.399(5) 1 d PU E 1 F10 F -0.8414(9) 1.0005(6) 0.7756(6) 0.0591(6) Uani 0.399(5) 1 d PDU E 1 F11 F -0.7539(8) 0.8878(6) 0.8506(6) 0.0591(6) Uani 0.399(5) 1 d PDU E 1 F12 F -0.9245(12) 0.8881(7) 0.8021(9) 0.0591(6) Uani 0.399(5) 1 d PDU E 1 C14A C -0.8205(11) 0.9282(8) 0.7649(8) 0.0591(6) Uani 0.601(5) 1 d PU E 2 F12A F -0.9265(8) 0.9103(4) 0.8002(6) 0.0591(6) Uani 0.601(5) 1 d PU E 2 F10A F -0.8567(5) 0.9779(4) 0.7051(4) 0.0591(6) Uani 0.601(5) 1 d PU E 2 F11A F -0.7964(6) 0.9876(4) 0.8054(4) 0.0591(6) Uani 0.601(5) 1 d PU E 2 F13 F -0.3349(4) 0.4268(3) 0.96447(19) 0.0595(9) Uani 1 1 d . . . F14 F -0.5111(4) 0.4070(3) 0.93788(19) 0.0604(10) Uani 1 1 d . . . F15 F -0.3252(4) 0.3539(2) 0.8677(2) 0.0600(10) Uani 1 1 d . . . F16 F -0.1391(5) 0.2938(2) 0.6593(2) 0.0773(13) Uani 1 1 d . . . F17 F -0.1610(4) 0.3471(2) 0.55417(19) 0.0605(10) Uani 1 1 d . . . F18 F -0.0502(4) 0.3986(3) 0.6178(2) 0.0659(11) Uani 1 1 d . . . F19 F 0.2553(4) 0.3920(2) 0.6060(2) 0.0548(9) Uani 1 1 d . . . F20 F 0.2849(3) 0.4705(2) 0.51084(17) 0.0494(8) Uani 1 1 d . . . F21 F 0.3589(3) 0.4919(3) 0.6057(2) 0.0624(11) Uani 1 1 d . . . F22 F 0.192(4) 0.560(2) 0.910(2) 0.055(2) Uani 0.17(3) 1 d PD F 1 F23 F 0.264(5) 0.662(4) 0.896(3) 0.0462(14) Uani 0.17(3) 1 d PD F 1 F24 F 0.079(4) 0.681(3) 0.9240(19) 0.0632(17) Uani 0.17(3) 1 d PD F 1 F24A F 0.0798(7) 0.6540(7) 0.9386(4) 0.0632(17) Uani 0.83(3) 1 d PD F 2 F22A F 0.2427(11) 0.5431(4) 0.8842(6) 0.055(2) Uani 0.83(3) 1 d PD F 2 F23A F 0.2643(9) 0.6809(7) 0.8871(6) 0.0462(14) Uani 0.83(3) 1 d PD F 2 P1 P -0.02154(10) 0.60356(7) 0.73517(6) 0.0222(2) Uani 1 1 d . B . P2 P -0.25594(10) 0.54654(7) 0.75909(6) 0.0235(2) Uani 1 1 d . . . P3 P -0.24824(10) 0.87752(7) 0.64953(6) 0.0240(2) Uani 1 1 d . A . P4 P -0.47761(11) 0.81492(7) 0.66428(6) 0.0271(2) Uani 1 1 d . B . Cl1A Cl -0.1637(3) 0.80746(17) 0.80317(17) 0.0252(5) Uani 0.564(4) 1 d P B 1 Cl1B Cl -0.4567(4) 0.7352(5) 0.8231(4) 0.0308(10) Uani 0.436(4) 1 d P B 2 Cl2 Cl 0.06239(10) 0.77237(7) 0.64869(6) 0.0289(2) Uani 1 1 d . B . Cl3 Cl -0.19678(10) 0.65521(7) 0.59877(5) 0.02486(19) Uani 1 1 d . B . Cl4 Cl -0.53604(10) 0.61715(7) 0.70242(6) 0.0313(2) Uani 1 1 d . . . Rh1 Rh -0.14406(3) 0.73739(2) 0.692280(16) 0.02001(8) Uani 1 1 d . . . Rh2 Rh -0.35702(3) 0.68295(2) 0.710267(17) 0.02186(9) Uani 1 1 d . B . C1S C -0.4411(7) 0.6637(5) 1.2454(4) 0.0610(6) Uani 1 1 d . . . H1SA H -0.4008 0.5999 1.2580 0.091 Uiso 1 1 calc R . . H1SB H -0.4960 0.6648 1.2086 0.091 Uiso 1 1 calc R . . H1SC H -0.4957 0.6975 1.2888 0.091 Uiso 1 1 calc R . . C2S C -0.3329(7) 0.7090(5) 1.2155(4) 0.0610(6) Uani 1 1 d . . . C3S C -0.2889(7) 0.7599(5) 1.2605(4) 0.0610(6) Uani 1 1 d . . . H3S H -0.3287 0.7702 1.3101 0.073 Uiso 1 1 calc R . . C4S C -0.1870(7) 0.7951(5) 1.2325(4) 0.0610(6) Uani 1 1 d . . . H4S H -0.1554 0.8296 1.2628 0.073 Uiso 1 1 calc R . . C5S C -0.1310(7) 0.7806(5) 1.1610(4) 0.0610(6) Uani 1 1 d . . . H5S H -0.0607 0.8052 1.1420 0.073 Uiso 1 1 calc R . . C6S C -0.1750(7) 0.7311(5) 1.1167(4) 0.0610(6) Uani 1 1 d . . . H6S H -0.1362 0.7218 1.0670 0.073 Uiso 1 1 calc R . . C7S C -0.2731(7) 0.6960(5) 1.1440(4) 0.0610(6) Uani 1 1 d . . . H7S H -0.3024 0.6609 1.1131 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.036(2) 0.026(2) 0.056(3) 0.012(2) -0.017(2) -0.0028(19) C2 0.034(2) 0.031(2) 0.050(3) 0.012(2) -0.015(2) -0.0015(19) C3 0.033(2) 0.041(3) 0.027(2) 0.0071(18) -0.0038(17) -0.0126(19) C4 0.052(3) 0.047(3) 0.033(2) 0.009(2) -0.005(2) -0.020(2) C5 0.044(3) 0.031(2) 0.032(2) -0.0043(18) -0.008(2) -0.013(2) C6 0.052(3) 0.026(2) 0.048(3) -0.006(2) -0.002(2) -0.007(2) C7 0.037(2) 0.032(2) 0.026(2) -0.0031(17) 0.0026(18) -0.0001(19) C8 0.030(2) 0.040(3) 0.038(2) -0.011(2) -0.0009(19) -0.0093(19) C9 0.025(2) 0.036(2) 0.035(2) 0.0052(18) -0.0086(17) -0.0119(18) C10 0.045(3) 0.044(3) 0.039(3) 0.004(2) -0.017(2) -0.021(2) C11 0.090(5) 0.035(3) 0.062(4) -0.002(2) -0.052(4) -0.008(3) C12 0.045(3) 0.058(3) 0.035(3) 0.003(2) -0.007(2) 0.006(3) C15 0.041(3) 0.028(2) 0.058(3) -0.006(2) -0.016(2) -0.0061(19) C16 0.060(3) 0.039(3) 0.067(4) 0.012(3) -0.026(3) -0.025(2) C17 0.047(3) 0.043(3) 0.028(2) 0.004(2) 0.002(2) -0.008(2) C19B 0.034(5) 0.023(4) 0.018(4) -0.001(3) -0.005(3) -0.005(4) C20A 0.051(5) 0.062(6) 0.036(4) -0.022(4) 0.013(4) -0.036(5) C19A 0.034(4) 0.024(3) 0.019(3) 0.000(3) -0.003(3) -0.005(3) C20B 0.049(6) 0.055(7) 0.026(5) -0.012(5) 0.006(4) -0.024(5) C21A 0.057(6) 0.074(7) 0.038(5) -0.024(5) 0.019(4) -0.043(5) C21B 0.054(7) 0.063(8) 0.037(6) -0.020(5) 0.001(5) -0.031(6) C22A 0.036(4) 0.031(4) 0.022(3) 0.000(3) -0.002(3) -0.009(3) C22B 0.036(5) 0.039(6) 0.028(4) -0.008(4) -0.005(4) -0.002(4) C23B 0.033(6) 0.060(10) 0.026(5) -0.007(6) 0.000(3) -0.016(3) C23A 0.033(6) 0.060(10) 0.026(5) -0.007(6) 0.000(3) -0.016(3) C24A 0.029(6) 0.070(5) 0.026(3) -0.012(3) 0.000(4) -0.011(5) C24B 0.029(6) 0.070(5) 0.026(3) -0.012(3) 0.000(4) -0.011(5) C29A 0.027(5) 0.060(8) 0.020(6) -0.006(5) -0.007(4) -0.002(4) C29B 0.058(5) 0.051(5) 0.031(4) -0.013(3) 0.001(3) -0.011(4) C30A 0.022(5) 0.024(4) 0.030(6) -0.001(4) -0.011(4) -0.005(4) C30B 0.022(5) 0.024(4) 0.030(6) -0.001(4) -0.011(4) -0.005(4) N1 0.0252(17) 0.0260(18) 0.0346(19) 0.0085(15) -0.0082(15) -0.0037(14) N2 0.0243(17) 0.0243(17) 0.036(2) 0.0056(14) -0.0084(15) -0.0028(14) N3A 0.028(3) 0.026(3) 0.022(3) -0.004(3) -0.002(2) -0.007(2) N3B 0.021(4) 0.027(4) 0.035(6) 0.004(4) -0.010(4) -0.007(3) O1 0.0309(16) 0.0359(17) 0.0272(15) 0.0051(13) -0.0079(12) -0.0114(13) O2 0.0343(16) 0.0237(14) 0.0306(15) 0.0021(12) -0.0070(13) -0.0097(12) O3 0.0237(14) 0.0361(16) 0.0248(14) 0.0053(12) -0.0076(11) -0.0104(12) O4 0.0247(15) 0.0331(16) 0.0281(15) 0.0017(12) 0.0004(12) 0.0022(12) O5 0.0298(9) 0.0397(11) 0.1016(18) -0.0016(12) 0.0018(10) -0.0078(9) O6 0.055(2) 0.0302(18) 0.065(3) -0.0013(17) -0.044(2) -0.0022(16) O7 0.0292(15) 0.0220(14) 0.0373(17) -0.0017(12) -0.0063(13) -0.0038(12) O8 0.0315(16) 0.0294(16) 0.0330(16) 0.0064(13) 0.0005(13) -0.0047(13) O9A 0.038(3) 0.051(4) 0.027(3) -0.013(3) 0.003(2) -0.016(3) O9B 0.058(5) 0.051(5) 0.031(4) -0.013(3) 0.001(3) -0.011(4) F1 0.062(4) 0.040(4) 0.077(6) 0.005(3) -0.026(4) -0.027(4) F2 0.063(2) 0.022(2) 0.105(5) 0.007(2) -0.028(3) -0.0013(17) F3 0.094(4) 0.062(3) 0.055(3) 0.012(2) -0.012(2) -0.046(3) F2A 0.063(2) 0.022(2) 0.105(5) 0.007(2) -0.028(3) -0.0013(17) F1A 0.062(4) 0.040(4) 0.077(6) 0.005(3) -0.026(4) -0.027(4) F3A 0.094(4) 0.062(3) 0.055(3) 0.012(2) -0.012(2) -0.046(3) C18 0.028(3) 0.072(5) 0.033(3) 0.005(3) -0.002(2) 0.000(3) F4 0.045(3) 0.116(4) 0.029(2) -0.005(2) -0.0010(17) -0.004(3) F5 0.061(4) 0.084(4) 0.053(4) 0.036(3) -0.009(3) -0.001(4) F6 0.038(2) 0.094(4) 0.040(2) -0.006(2) -0.0040(17) -0.012(2) C18A 0.028(3) 0.072(5) 0.033(3) 0.005(3) -0.002(2) 0.000(3) F5A 0.061(4) 0.084(4) 0.053(4) 0.036(3) -0.009(3) -0.001(4) F4A 0.045(3) 0.116(4) 0.029(2) -0.005(2) -0.0010(17) -0.004(3) F6A 0.038(2) 0.094(4) 0.040(2) -0.006(2) -0.0040(17) -0.012(2) F7 0.0574(16) 0.068(2) 0.0439(17) 0.0045(14) -0.0165(13) -0.0091(16) F8 0.0574(16) 0.068(2) 0.0439(17) 0.0045(14) -0.0165(13) -0.0091(16) F9 0.0574(16) 0.068(2) 0.0439(17) 0.0045(14) -0.0165(13) -0.0091(16) F7A 0.0574(16) 0.068(2) 0.0439(17) 0.0045(14) -0.0165(13) -0.0091(16) F9A 0.0574(16) 0.068(2) 0.0439(17) 0.0045(14) -0.0165(13) -0.0091(16) F8A 0.0574(16) 0.068(2) 0.0439(17) 0.0045(14) -0.0165(13) -0.0091(16) C13 0.0298(9) 0.0397(11) 0.1016(18) -0.0016(12) 0.0018(10) -0.0078(9) C14 0.0298(9) 0.0397(11) 0.1016(18) -0.0016(12) 0.0018(10) -0.0078(9) F10 0.0298(9) 0.0397(11) 0.1016(18) -0.0016(12) 0.0018(10) -0.0078(9) F11 0.0298(9) 0.0397(11) 0.1016(18) -0.0016(12) 0.0018(10) -0.0078(9) F12 0.0298(9) 0.0397(11) 0.1016(18) -0.0016(12) 0.0018(10) -0.0078(9) C14A 0.0298(9) 0.0397(11) 0.1016(18) -0.0016(12) 0.0018(10) -0.0078(9) F12A 0.0298(9) 0.0397(11) 0.1016(18) -0.0016(12) 0.0018(10) -0.0078(9) F10A 0.0298(9) 0.0397(11) 0.1016(18) -0.0016(12) 0.0018(10) -0.0078(9) F11A 0.0298(9) 0.0397(11) 0.1016(18) -0.0016(12) 0.0018(10) -0.0078(9) F13 0.074(2) 0.071(2) 0.0420(18) 0.0251(17) -0.0254(17) -0.028(2) F14 0.065(2) 0.077(3) 0.049(2) 0.0221(18) -0.0046(17) -0.041(2) F15 0.079(3) 0.0389(18) 0.057(2) 0.0081(15) 0.0001(19) -0.0171(17) F16 0.113(4) 0.0239(16) 0.074(3) 0.0038(16) 0.003(2) 0.0023(19) F17 0.079(3) 0.049(2) 0.049(2) -0.0213(16) 0.0034(18) -0.0185(18) F18 0.0414(19) 0.065(2) 0.083(3) -0.027(2) 0.0108(18) -0.0119(17) F19 0.059(2) 0.0290(15) 0.065(2) -0.0005(14) -0.0033(17) 0.0022(14) F20 0.0510(19) 0.0532(19) 0.0345(15) -0.0177(14) 0.0053(13) -0.0055(15) F21 0.0289(15) 0.091(3) 0.067(2) -0.040(2) 0.0025(15) -0.0187(17) F22 0.061(5) 0.041(2) 0.072(5) 0.018(3) -0.044(4) -0.012(3) F23 0.054(2) 0.052(5) 0.049(4) 0.011(3) -0.026(2) -0.032(3) F24 0.083(3) 0.101(5) 0.023(3) -0.001(3) 0.001(2) -0.060(3) F24A 0.083(3) 0.101(5) 0.023(3) -0.001(3) 0.001(2) -0.060(3) F22A 0.061(5) 0.041(2) 0.072(5) 0.018(3) -0.044(4) -0.012(3) F23A 0.054(2) 0.052(5) 0.049(4) 0.011(3) -0.026(2) -0.032(3) P1 0.0191(4) 0.0233(5) 0.0220(5) 0.0008(4) -0.0036(4) -0.0026(4) P2 0.0229(5) 0.0225(5) 0.0244(5) 0.0023(4) -0.0049(4) -0.0052(4) P3 0.0228(5) 0.0219(5) 0.0257(5) 0.0031(4) -0.0042(4) -0.0043(4) P4 0.0232(5) 0.0229(5) 0.0366(6) 0.0018(4) -0.0131(4) -0.0041(4) Cl1A 0.0234(12) 0.0284(11) 0.0235(15) -0.0038(9) -0.0017(9) -0.0081(8) Cl1B 0.023(2) 0.0336(16) 0.035(2) -0.0064(15) -0.0039(16) -0.0072(17) Cl2 0.0236(4) 0.0305(5) 0.0317(5) 0.0022(4) -0.0009(4) -0.0088(4) Cl3 0.0260(4) 0.0240(4) 0.0245(4) -0.0010(3) -0.0066(3) -0.0055(4) Cl4 0.0258(5) 0.0294(5) 0.0422(6) -0.0007(4) -0.0107(4) -0.0104(4) Rh1 0.01880(15) 0.02026(15) 0.01989(15) 0.00050(11) -0.00377(11) -0.00364(11) Rh2 0.01915(15) 0.02157(16) 0.02481(16) 0.00116(11) -0.00618(11) -0.00443(11) C1S 0.0656(16) 0.0476(13) 0.0683(16) 0.0074(12) -0.0256(13) -0.0065(11) C2S 0.0656(16) 0.0476(13) 0.0683(16) 0.0074(12) -0.0256(13) -0.0065(11) C3S 0.0656(16) 0.0476(13) 0.0683(16) 0.0074(12) -0.0256(13) -0.0065(11) C4S 0.0656(16) 0.0476(13) 0.0683(16) 0.0074(12) -0.0256(13) -0.0065(11) C5S 0.0656(16) 0.0476(13) 0.0683(16) 0.0074(12) -0.0256(13) -0.0065(11) C6S 0.0656(16) 0.0476(13) 0.0683(16) 0.0074(12) -0.0256(13) -0.0065(11) C7S 0.0656(16) 0.0476(13) 0.0683(16) 0.0074(12) -0.0256(13) -0.0065(11) _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 N2 1.493(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.486(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 O1 1.422(6) . ? C3 C4 1.495(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 F15 1.323(7) . ? C4 F13 1.334(6) . ? C4 F14 1.334(6) . ? C5 O2 1.433(5) . ? C5 C6 1.497(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 F16 1.309(6) . ? C6 F17 1.324(6) . ? C6 F18 1.339(7) . ? C7 O4 1.424(5) . ? C7 C8 1.497(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 F21 1.315(6) . ? C8 F19 1.320(6) . ? C8 F20 1.346(6) . ? C9 O3 1.429(5) . ? C9 C10 1.487(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 F22 1.21(2) . ? C10 F23 1.21(3) . ? C10 F24 1.25(3) . ? C10 F24A 1.333(8) . ? C10 F23A 1.363(9) . ? C10 F22A 1.367(9) . ? C11 O6 1.439(7) . ? C11 C12 1.450(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 F7 1.273(8) . ? C12 F8 1.302(12) . ? C12 F7A 1.320(14) . ? C12 F9 1.377(8) . ? C12 F8A 1.43(2) . ? C12 F9A 1.469(16) . ? C15 O7 1.428(6) . ? C15 C16 1.460(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 F2 1.297(8) . ? C16 F3A 1.331(15) . ? C16 F1 1.348(8) . ? C16 F1A 1.352(17) . ? C16 F3 1.382(8) . ? C16 F2A 1.418(16) . ? C17 O8 1.422(6) . ? C17 C18 1.471(8) . ? C17 C18A 1.487(17) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 H17C 0.9900 . ? C17 H17D 0.9900 . ? C19B C24B 1.364(17) . ? C19B C20B 1.401(16) . ? C19B N3B 1.426(15) . ? C20A C21A 1.371(12) . ? C20A C19A 1.399(12) . ? C20A H20A 0.9500 . ? C19A C24A 1.366(14) . ? C19A N3A 1.397(10) . ? C20B C21B 1.380(15) . ? C20B H20B 0.9500 . ? C21A C22A 1.405(13) . ? C21A H21A 0.9500 . ? C21B C22B 1.390(17) . ? C21B H21B 0.9500 . ? C22A C23B 1.32(3) . ? C22A O9A 1.355(9) . ? C22B O9B 1.355(13) . ? C22B C23A 1.42(2) . ? C23B C24A 1.40(4) . ? C23B H23B 0.9500 . ? C23A C24B 1.40(3) . ? C23A H23A 0.9500 . ? C24A H24A 0.9500 . ? C24B H24B 0.9500 . ? C29A O9A 1.49(2) . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C29B O9B 1.43(4) . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30A N3A 1.14(2) . ? C30A Rh2 1.99(2) . ? C30B N3B 1.139(18) . ? C30B Rh1 1.901(17) . ? N1 P3 1.654(4) . ? N1 P4 1.663(4) . ? N2 P1 1.655(4) . ? N2 P2 1.657(4) . ? O1 P2 1.591(3) . ? O2 P2 1.600(3) . ? O3 P1 1.592(3) . ? O4 P1 1.599(3) . ? O5 C13 1.430(7) . ? O5 P4 1.587(4) . ? O6 P4 1.590(4) . ? O7 P3 1.588(3) . ? O8 P3 1.600(3) . ? C18 F4 1.330(9) . ? C18 F5 1.332(12) . ? C18 F6 1.369(9) . ? C18A F4A 1.33(4) . ? C18A F5A 1.33(3) . ? C18A F6A 1.35(3) . ? C13 C14A 1.445(12) . ? C13 C14 1.46(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 H13C 0.9900 . ? C13 H13D 0.9900 . ? C14 F11 1.29(2) . ? C14 F10 1.32(2) . ? C14 F12 1.39(2) . ? C14A F11A 1.308(15) . ? C14A F12A 1.313(14) . ? C14A F10A 1.378(15) . ? P1 Rh1 2.2868(10) . ? P2 Rh2 2.2870(11) . ? P3 Rh1 2.2913(11) . ? P4 Rh2 2.2838(11) . ? Cl1A Rh1 2.316(3) . ? Cl1B Rh2 2.256(6) . ? Cl2 Rh1 2.4352(10) . ? Cl3 Rh1 2.4203(10) . ? Cl3 Rh2 2.4329(10) . ? Cl4 Rh2 2.4436(11) . ? Rh1 Rh2 2.6233(4) . ? C1S C2S 1.537(11) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C2S C7S 1.376(10) . ? C2S C3S 1.390(10) . ? C3S C4S 1.375(11) . ? C3S H3S 0.9500 . ? C4S C5S 1.367(10) . ? C4S H4S 0.9500 . ? C5S C6S 1.365(10) . ? C5S H5S 0.9500 . ? C6S C7S 1.337(11) . ? C6S H6S 0.9500 . ? C7S H7S 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 H1A 109.5 . . ? N2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O1 C3 C4 108.0(4) . . ? O1 C3 H3A 110.1 . . ? C4 C3 H3A 110.1 . . ? O1 C3 H3B 110.1 . . ? C4 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? F15 C4 F13 106.5(5) . . ? F15 C4 F14 108.1(5) . . ? F13 C4 F14 107.3(4) . . ? F15 C4 C3 112.5(4) . . ? F13 C4 C3 112.2(5) . . ? F14 C4 C3 110.0(5) . . ? O2 C5 C6 107.8(4) . . ? O2 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? O2 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.5 . . ? F16 C6 F17 107.7(4) . . ? F16 C6 F18 108.1(5) . . ? F17 C6 F18 106.7(5) . . ? F16 C6 C5 112.2(5) . . ? F17 C6 C5 110.6(5) . . ? F18 C6 C5 111.3(4) . . ? O4 C7 C8 106.0(4) . . ? O4 C7 H7A 110.5 . . ? C8 C7 H7A 110.5 . . ? O4 C7 H7B 110.5 . . ? C8 C7 H7B 110.5 . . ? H7A C7 H7B 108.7 . . ? F21 C8 F19 107.8(5) . . ? F21 C8 F20 107.0(4) . . ? F19 C8 F20 106.7(4) . . ? F21 C8 C7 113.2(4) . . ? F19 C8 C7 112.6(4) . . ? F20 C8 C7 109.3(4) . . ? O3 C9 C10 106.4(4) . . ? O3 C9 H9A 110.5 . . ? C10 C9 H9A 110.5 . . ? O3 C9 H9B 110.5 . . ? C10 C9 H9B 110.5 . . ? H9A C9 H9B 108.6 . . ? F22 C10 F23 104(2) . . ? F22 C10 F24 100.1(17) . . ? F23 C10 F24 101(4) . . ? F22 C10 F24A 79(2) . . ? F23 C10 F24A 106(3) . . ? F24 C10 F24A 21.1(18) . . ? F22 C10 F23A 117.5(14) . . ? F23 C10 F23A 13(2) . . ? F24 C10 F23A 100(2) . . ? F24A C10 F23A 109.2(7) . . ? F22 C10 F22A 29(2) . . ? F23 C10 F22A 95(3) . . ? F24 C10 F22A 128.9(17) . . ? F24A C10 F22A 107.8(5) . . ? F23A C10 F22A 105.7(6) . . ? F22 C10 C9 124.3(17) . . ? F23 C10 C9 120(2) . . ? F24 C10 C9 102(2) . . ? F24A C10 C9 114.7(5) . . ? F23A C10 C9 108.3(5) . . ? F22A C10 C9 110.8(5) . . ? O6 C11 C12 108.1(5) . . ? O6 C11 H11A 110.1 . . ? C12 C11 H11A 110.1 . . ? O6 C11 H11B 110.1 . . ? C12 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? F7 C12 F8 100.7(6) . . ? F7 C12 F7A 46.0(6) . . ? F8 C12 F7A 122.9(8) . . ? F7 C12 F9 101.9(5) . . ? F8 C12 F9 108.2(7) . . ? F7A C12 F9 57.4(7) . . ? F7 C12 F8A 113.6(9) . . ? F8 C12 F8A 13.4(9) . . ? F7A C12 F8A 128.9(11) . . ? F9 C12 F8A 100.8(10) . . ? F7 C12 C11 119.5(7) . . ? F8 C12 C11 113.1(6) . . ? F7A C12 C11 123.6(7) . . ? F9 C12 C11 112.1(6) . . ? F8A C12 C11 107.2(9) . . ? F7 C12 F9A 129.1(7) . . ? F8 C12 F9A 99.8(8) . . ? F7A C12 F9A 84.0(9) . . ? F9 C12 F9A 27.2(5) . . ? F8A C12 F9A 88.3(11) . . ? C11 C12 F9A 93.5(7) . . ? O7 C15 C16 109.4(4) . . ? O7 C15 H15A 109.8 . . ? C16 C15 H15A 109.8 . . ? O7 C15 H15B 109.8 . . ? C16 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? F2 C16 F3A 58.0(10) . . ? F2 C16 F1 104.7(6) . . ? F3A C16 F1 112.1(10) . . ? F2 C16 F1A 120.4(17) . . ? F3A C16 F1A 112(3) . . ? F1 C16 F1A 17.4(18) . . ? F2 C16 F3 104.4(6) . . ? F3A C16 F3 47.1(10) . . ? F1 C16 F3 110.0(7) . . ? F1A C16 F3 97(2) . . ? F2 C16 F2A 32.2(8) . . ? F3A C16 F2A 90.1(13) . . ? F1 C16 F2A 90.9(11) . . ? F1A C16 F2A 108.3(19) . . ? F3 C16 F2A 136.5(10) . . ? F2 C16 C15 117.3(6) . . ? F3A C16 C15 135.3(10) . . ? F1 C16 C15 111.7(7) . . ? F1A C16 C15 107(2) . . ? F3 C16 C15 108.3(5) . . ? F2A C16 C15 97.6(9) . . ? O8 C17 C18 110.2(5) . . ? O8 C17 C18A 100.8(11) . . ? C18 C17 C18A 36.6(12) . . ? O8 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? C18A C17 H17A 142.4 . . ? O8 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? C18A C17 H17B 80.7 . . ? H17A C17 H17B 108.1 . . ? O8 C17 H17C 111.6 . . ? C18 C17 H17C 75.4 . . ? C18A C17 H17C 111.6 . . ? H17A C17 H17C 36.4 . . ? H17B C17 H17C 133.3 . . ? O8 C17 H17D 111.6 . . ? C18 C17 H17D 131.8 . . ? C18A C17 H17D 111.6 . . ? H17A C17 H17D 77.4 . . ? H17B C17 H17D 32.5 . . ? H17C C17 H17D 109.4 . . ? C24B C19B C20B 121.6(11) . . ? C24B C19B N3B 119.1(11) . . ? C20B C19B N3B 119.2(9) . . ? C21A C20A C19A 118.8(9) . . ? C21A C20A H20A 120.6 . . ? C19A C20A H20A 120.6 . . ? C24A C19A N3A 120.0(8) . . ? C24A C19A C20A 120.0(8) . . ? N3A C19A C20A 119.9(7) . . ? C21B C20B C19B 117.8(11) . . ? C21B C20B H20B 121.1 . . ? C19B C20B H20B 121.1 . . ? C20A C21A C22A 120.6(8) . . ? C20A C21A H21A 119.7 . . ? C22A C21A H21A 119.7 . . ? C20B C21B C22B 121.0(11) . . ? C20B C21B H21B 119.5 . . ? C22B C21B H21B 119.5 . . ? C23B C22A O9A 124.5(16) . . ? C23B C22A C21A 119.7(16) . . ? O9A C22A C21A 115.7(7) . . ? O9B C22B C21B 115.5(11) . . ? O9B C22B C23A 123.6(13) . . ? C21B C22B C23A 120.9(12) . . ? C22A C23B C24A 121(2) . . ? C22A C23B H23B 119.5 . . ? C24A C23B H23B 119.5 . . ? C24B C23A C22B 116.6(14) . . ? C24B C23A H23A 121.7 . . ? C22B C23A H23A 121.7 . . ? C19A C24A C23B 119.5(13) . . ? C19A C24A H24A 120.3 . . ? C23B C24A H24A 120.3 . . ? C19B C24B C23A 121.5(15) . . ? C19B C24B H24B 119.3 . . ? C23A C24B H24B 119.3 . . ? O9B C29B H29D 109.5 . . ? O9B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? O9B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? N3A C30A Rh2 178.8(15) . . ? N3B C30B Rh1 179.2(14) . . ? C2 N1 P3 120.5(3) . . ? C2 N1 P4 119.7(3) . . ? P3 N1 P4 119.4(2) . . ? C1 N2 P1 120.1(3) . . ? C1 N2 P2 119.9(3) . . ? P1 N2 P2 119.5(2) . . ? C30A N3A C19A 169.4(12) . . ? C30B N3B C19B 171.4(11) . . ? C3 O1 P2 123.7(3) . . ? C5 O2 P2 124.9(3) . . ? C9 O3 P1 121.5(3) . . ? C7 O4 P1 123.9(3) . . ? C13 O5 P4 120.6(4) . . ? C11 O6 P4 125.4(3) . . ? C15 O7 P3 122.9(3) . . ? C17 O8 P3 124.5(3) . . ? C22A O9A C29A 117.9(10) . . ? C22B O9B C29B 114.2(16) . . ? F4 C18 F5 107.8(6) . . ? F4 C18 F6 106.6(7) . . ? F5 C18 F6 106.8(6) . . ? F4 C18 C17 111.9(5) . . ? F5 C18 C17 113.6(8) . . ? F6 C18 C17 109.8(6) . . ? F4A C18A F5A 105(2) . . ? F4A C18A F6A 103.9(19) . . ? F5A C18A F6A 110(2) . . ? F4A C18A C17 103.8(19) . . ? F5A C18A C17 124(2) . . ? F6A C18A C17 107.6(19) . . ? O5 C13 C14A 106.4(6) . . ? O5 C13 C14 110.7(8) . . ? C14A C13 C14 23.9(9) . . ? O5 C13 H13A 109.5 . . ? C14A C13 H13A 130.7 . . ? C14 C13 H13A 109.5 . . ? O5 C13 H13B 109.5 . . ? C14A C13 H13B 90.0 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? O5 C13 H13C 110.4 . . ? C14A C13 H13C 110.4 . . ? C14 C13 H13C 87.3 . . ? H13A C13 H13C 24.2 . . ? H13B C13 H13C 126.8 . . ? O5 C13 H13D 110.4 . . ? C14A C13 H13D 110.4 . . ? C14 C13 H13D 126.3 . . ? H13A C13 H13D 87.2 . . ? H13B C13 H13D 22.5 . . ? H13C C13 H13D 108.6 . . ? F11 C14 F10 120.6(18) . . ? F11 C14 F12 108.8(15) . . ? F10 C14 F12 105.2(13) . . ? F11 C14 C13 97.5(12) . . ? F10 C14 C13 118.1(16) . . ? F12 C14 C13 105.8(14) . . ? F11A C14A F12A 105.7(11) . . ? F11A C14A F10A 103.8(9) . . ? F12A C14A F10A 106.5(9) . . ? F11A C14A C13 116.3(10) . . ? F12A C14A C13 113.7(9) . . ? F10A C14A C13 110.0(10) . . ? O3 P1 O4 98.09(17) . . ? O3 P1 N2 99.14(18) . . ? O4 P1 N2 104.17(19) . . ? O3 P1 Rh1 118.07(13) . . ? O4 P1 Rh1 117.30(12) . . ? N2 P1 Rh1 116.89(13) . . ? O1 P2 O2 97.80(17) . . ? O1 P2 N2 99.44(18) . . ? O2 P2 N2 104.93(18) . . ? O1 P2 Rh2 118.00(13) . . ? O2 P2 Rh2 116.46(12) . . ? N2 P2 Rh2 117.14(14) . . ? O7 P3 O8 97.60(18) . . ? O7 P3 N1 98.57(18) . . ? O8 P3 N1 104.49(19) . . ? O7 P3 Rh1 118.96(13) . . ? O8 P3 Rh1 116.88(13) . . ? N1 P3 Rh1 117.04(14) . . ? O5 P4 O6 97.8(2) . . ? O5 P4 N1 99.1(2) . . ? O6 P4 N1 104.2(2) . . ? O5 P4 Rh2 117.72(19) . . ? O6 P4 Rh2 117.69(14) . . ? N1 P4 Rh2 117.00(13) . . ? Rh1 Cl3 Rh2 65.44(3) . . ? C30B Rh1 P1 89.2(4) . . ? C30B Rh1 P3 89.4(4) . . ? P1 Rh1 P3 173.90(4) . . ? C30B Rh1 Cl1A 7.2(6) . . ? P1 Rh1 Cl1A 89.18(7) . . ? P3 Rh1 Cl1A 88.68(7) . . ? C30B Rh1 Cl3 152.0(5) . . ? P1 Rh1 Cl3 91.51(4) . . ? P3 Rh1 Cl3 92.52(4) . . ? Cl1A Rh1 Cl3 159.21(8) . . ? C30B Rh1 Cl2 98.4(5) . . ? P1 Rh1 Cl2 86.97(4) . . ? P3 Rh1 Cl2 87.36(4) . . ? Cl1A Rh1 Cl2 91.15(8) . . ? Cl3 Rh1 Cl2 109.63(4) . . ? C30B Rh1 Rh2 94.5(5) . . ? P1 Rh1 Rh2 93.20(3) . . ? P3 Rh1 Rh2 92.83(3) . . ? Cl1A Rh1 Rh2 101.71(8) . . ? Cl3 Rh1 Rh2 57.51(3) . . ? Cl2 Rh1 Rh2 167.14(3) . . ? C30A Rh2 Cl1B 7.4(7) . . ? C30A Rh2 P4 90.4(5) . . ? Cl1B Rh2 P4 89.31(15) . . ? C30A Rh2 P2 88.5(5) . . ? Cl1B Rh2 P2 88.83(15) . . ? P4 Rh2 P2 174.08(4) . . ? C30A Rh2 Cl3 152.4(5) . . ? Cl1B Rh2 Cl3 159.72(17) . . ? P4 Rh2 Cl3 90.61(4) . . ? P2 Rh2 Cl3 93.08(4) . . ? C30A Rh2 Cl4 96.5(5) . . ? Cl1B Rh2 Cl4 89.13(17) . . ? P4 Rh2 Cl4 87.68(4) . . ? P2 Rh2 Cl4 86.68(4) . . ? Cl3 Rh2 Cl4 111.13(4) . . ? C30A Rh2 Rh1 95.4(5) . . ? Cl1B Rh2 Rh1 102.71(17) . . ? P4 Rh2 Rh1 93.16(3) . . ? P2 Rh2 Rh1 92.73(3) . . ? Cl3 Rh2 Rh1 57.05(2) . . ? Cl4 Rh2 Rh1 168.14(3) . . ? C2S C1S H1SA 109.5 . . ? C2S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? C2S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? C7S C2S C3S 118.7(7) . . ? C7S C2S C1S 120.3(7) . . ? C3S C2S C1S 120.9(7) . . ? C4S C3S C2S 119.1(7) . . ? C4S C3S H3S 120.4 . . ? C2S C3S H3S 120.4 . . ? C5S C4S C3S 120.0(7) . . ? C5S C4S H4S 120.0 . . ? C3S C4S H4S 120.0 . . ? C6S C5S C4S 120.8(8) . . ? C6S C5S H5S 119.6 . . ? C4S C5S H5S 119.6 . . ? C7S C6S C5S 119.3(8) . . ? C7S C6S H6S 120.3 . . ? C5S C6S H6S 120.3 . . ? C6S C7S C2S 122.1(7) . . ? C6S C7S H7S 119.0 . . ? C2S C7S H7S 119.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.758 _refine_diff_density_min -1.556 _refine_diff_density_rms 0.176