# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_compnd_3 _database_code_depnum_ccdc_archive 'CCDC 908505' #TrackingRef '15071_web_deposit_cif_file_0_FernandoJ.Lahoz_1351623726.compnd_3_6_7_9_11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C82 H75 O12 P4 Rh3 S2' _chemical_formula_sum 'C82 H75 O12 P4 Rh3 S2' _chemical_formula_weight 1749.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 18.570(2) _cell_length_b 19.659(2) _cell_length_c 21.045(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.824(2) _cell_angle_gamma 90.00 _cell_volume 7354.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5274 _cell_measurement_theta_min 2.266 _cell_measurement_theta_max 25.77 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3560 _exptl_absorpt_coefficient_mu 0.873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8883 _exptl_absorpt_correction_T_max 0.9398 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within SAINT+ package, v. 6.45. ; _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 SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 78993 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.34 _reflns_number_total 17819 _reflns_number_gt 14589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.45 (Bruker AXS, 2003)' _computing_data_reduction 'SAINT+ v. 6.45 (Bruker AXS, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, SHELXTLv6.12, BrukerAXS' _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. All non-hydrogen atoms were refined with anisotropic displacement parameters. In the last cycles of the refinement, anomalous high displacement parameters were observed for three carbon atoms (C60, C61 and C62) of one of the phenyl rings. A model of static disorder was tried to be established with no sensible results. Eventually dynamic disorder was considered. Hydrogen atoms were included in calculated positions and refined riding (positional and displacement parameters) on their bonded atoms. The three highest residual peaks were under 1 e/A^3 and were observed around the positions of the three carbon atoms C60, C61 and C62. ; _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^)+(0.0290P)^2^+6.0491P] 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 17819 _refine_ls_number_parameters 933 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl134as in P 21/n CELL 0.71073 18.5698 19.6592 21.0452 90.000 106.824 90.000 ZERR 4.00 0.0020 0.0021 0.0023 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H O P S Rh UNIT 328 300 48 16 8 12 OMIT -1 0 1 OMIT 0 1 1 L.S. 4 ACTA BOND $H FMAP 2 PLAN 10 WPDB -2 SIZE 0.072 0.075 0.139 WGHT 0.028900 6.074900 FVAR 0.140330 TEMP -173 MOLE 1 Rh1 6 0.155546 0.719880 0.797219 11.000000 0.011660 0.009760 = 0.010330 0.000490 0.002030 0.000770 Rh2 6 0.098924 0.769326 0.659815 11.000000 0.010860 0.009240 = 0.009730 0.000340 0.003270 0.000190 Rh3 6 -0.002749 0.765050 0.756380 11.000000 0.010740 0.009840 = 0.010380 -0.000610 0.003390 -0.000280 S1 5 0.056687 0.679721 0.712610 11.000000 0.012990 0.010630 = 0.011080 -0.000220 0.003640 -0.000260 S2 5 0.108328 0.825095 0.760203 11.000000 0.013070 0.010450 = 0.011130 -0.000360 0.003720 -0.000470 C1 1 0.269982 0.736240 0.860803 11.000000 0.010580 0.017450 = 0.011490 0.002230 -0.002030 0.002590 C2 1 0.220747 0.727776 0.900480 11.000000 0.014150 0.015760 = 0.012290 0.001480 -0.001160 0.000560 C3 1 0.186308 0.660692 0.886263 11.000000 0.016260 0.013380 = 0.010880 0.001840 0.000970 0.001170 C4 1 0.216640 0.627966 0.839228 11.000000 0.014060 0.012630 = 0.010860 0.002160 -0.000620 0.003130 C5 1 0.265963 0.675380 0.821437 11.000000 0.013090 0.013950 = 0.012080 0.001520 0.000320 0.002000 C6 1 0.318677 0.796546 0.860440 11.000000 0.018960 0.015980 = 0.023620 -0.000400 0.002910 -0.002110 AFIX 137 H6A 2 0.309750 0.831271 0.890708 11.000000 -1.500000 H6B 2 0.306615 0.815221 0.815404 11.000000 -1.500000 H6C 2 0.371642 0.782744 0.874972 11.000000 -1.500000 AFIX 0 C7 1 0.208959 0.776830 0.950670 11.000000 0.023130 0.022910 = 0.016270 -0.003490 0.004660 0.000940 AFIX 137 H7A 2 0.253272 0.776817 0.989693 11.000000 -1.500000 H7B 2 0.164567 0.763304 0.963889 11.000000 -1.500000 H7C 2 0.201296 0.822577 0.931385 11.000000 -1.500000 AFIX 0 C8 1 0.131433 0.632558 0.918487 11.000000 0.022520 0.021310 = 0.011670 0.002200 0.005210 -0.000600 AFIX 137 H8A 2 0.108845 0.591100 0.895264 11.000000 -1.500000 H8B 2 0.091923 0.666224 0.916504 11.000000 -1.500000 H8C 2 0.157310 0.621778 0.964962 11.000000 -1.500000 AFIX 0 C9 1 0.199933 0.557775 0.811042 11.000000 0.022000 0.014760 = 0.018110 0.001810 0.004560 0.001750 AFIX 137 H9A 2 0.161406 0.536726 0.828090 11.000000 -1.500000 H9B 2 0.245893 0.530275 0.824089 11.000000 -1.500000 H9C 2 0.181575 0.560422 0.762514 11.000000 -1.500000 AFIX 0 C10 1 0.310946 0.663323 0.774299 11.000000 0.019110 0.019490 = 0.016290 0.000500 0.005250 0.001850 AFIX 137 H10A 2 0.359017 0.642165 0.797949 11.000000 -1.500000 H10B 2 0.320357 0.706780 0.755320 11.000000 -1.500000 H10C 2 0.283065 0.633088 0.738609 11.000000 -1.500000 AFIX 0 P1 4 0.069764 0.709886 0.568066 11.000000 0.013150 0.010140 = 0.011420 0.000080 0.004250 0.000490 P2 4 0.154966 0.854554 0.627902 11.000000 0.011230 0.010850 = 0.012220 0.000100 0.003770 0.000240 P3 4 -0.101028 0.699229 0.735085 11.000000 0.012880 0.012930 = 0.011360 -0.000280 0.003820 -0.000890 P4 4 -0.045203 0.847394 0.805335 11.000000 0.012160 0.012840 = 0.013100 -0.001300 0.003600 -0.000070 O1 3 -0.014456 0.719159 0.517688 11.000000 0.016260 0.009590 = 0.013220 -0.000070 -0.000170 0.000460 O2 3 0.123434 0.715031 0.519245 11.000000 0.018120 0.015020 = 0.012400 -0.003580 0.006560 -0.002730 O3 3 0.056147 0.628126 0.568800 11.000000 0.013760 0.011370 = 0.013980 0.000900 0.003440 0.001280 O4 3 0.146092 0.856397 0.549445 11.000000 0.019560 0.017950 = 0.011530 0.000640 0.006560 -0.005180 O5 3 0.245699 0.865794 0.661040 11.000000 0.012360 0.014590 = 0.019300 -0.002570 0.004440 0.000190 O6 3 0.141053 0.932921 0.644350 11.000000 0.015350 0.010650 = 0.020800 -0.000770 0.006690 0.000320 O7 3 -0.153569 0.700437 0.658971 11.000000 0.018170 0.013430 = 0.013600 -0.000780 0.001450 0.000640 O8 3 -0.092373 0.616694 0.739211 11.000000 0.016290 0.012380 = 0.012090 0.001450 0.002530 -0.001540 O9 3 -0.162431 0.713946 0.774234 11.000000 0.011800 0.019720 = 0.019150 -0.002030 0.007810 -0.002410 O10 3 -0.101817 0.906733 0.766525 11.000000 0.015700 0.012200 = 0.017140 -0.001590 0.003340 0.000350 O11 3 0.021947 0.895983 0.845846 11.000000 0.014270 0.015970 = 0.019580 -0.005920 0.004050 -0.001310 O12 3 -0.092617 0.832659 0.858529 11.000000 0.016020 0.018520 = 0.015670 -0.000060 0.008490 0.002280 C11 1 -0.044975 0.783415 0.497814 11.000000 0.011600 0.012250 = 0.011750 0.000280 -0.002400 -0.000180 C12 1 -0.021511 0.819295 0.451251 11.000000 0.014620 0.018860 = 0.015970 0.001200 0.003380 0.000120 AFIX 43 H12 2 0.017676 0.802195 0.435046 11.000000 -1.200000 AFIX 0 C13 1 -0.056056 0.881012 0.428256 11.000000 0.024350 0.018930 = 0.016270 0.005160 0.002130 -0.003030 AFIX 43 H13 2 -0.040034 0.906675 0.396573 11.000000 -1.200000 AFIX 0 C14 1 -0.113637 0.904901 0.451542 11.000000 0.019080 0.016040 = 0.021180 0.002400 -0.004750 0.003010 AFIX 43 H14 2 -0.137217 0.947007 0.435828 11.000000 -1.200000 AFIX 0 C15 1 -0.137100 0.867555 0.497810 11.000000 0.013500 0.020270 = 0.020790 -0.004800 0.001920 0.002260 AFIX 43 H15 2 -0.177265 0.883935 0.513101 11.000000 -1.200000 AFIX 0 C16 1 -0.102353 0.806306 0.522042 11.000000 0.014010 0.017030 = 0.016180 0.000290 0.001350 -0.002650 AFIX 43 H16 2 -0.117617 0.780923 0.554328 11.000000 -1.200000 AFIX 0 C17 1 0.122862 0.675178 0.464211 11.000000 0.023690 0.010680 = 0.014620 -0.001750 0.009730 -0.000900 C18 1 0.059182 0.644046 0.423682 11.000000 0.022000 0.022930 = 0.017380 -0.004030 0.006430 -0.004080 AFIX 43 H18 2 0.012272 0.647636 0.433072 11.000000 -1.200000 AFIX 0 C19 1 0.065283 0.607374 0.368892 11.000000 0.032600 0.024880 = 0.021500 -0.008310 0.009990 -0.010510 AFIX 43 H19 2 0.021961 0.585770 0.340752 11.000000 -1.200000 AFIX 0 C20 1 0.132835 0.601835 0.354741 11.000000 0.044930 0.035520 = 0.031010 -0.018400 0.023770 -0.010800 AFIX 43 H20 2 0.136058 0.576649 0.317136 11.000000 -1.200000 AFIX 0 C21 1 0.196172 0.633213 0.395668 11.000000 0.035820 0.042860 = 0.042430 -0.019250 0.026690 -0.008980 AFIX 43 H21 2 0.243082 0.629234 0.386340 11.000000 -1.200000 AFIX 0 C22 1 0.191237 0.670258 0.449989 11.000000 0.024520 0.026950 = 0.028030 -0.009540 0.011500 -0.007930 AFIX 43 H22 2 0.234533 0.692356 0.477609 11.000000 -1.200000 AFIX 0 C23 1 0.110101 0.580545 0.599626 11.000000 0.018630 0.013290 = 0.011250 -0.000840 0.005310 0.004650 C24 1 0.083033 0.517595 0.610818 11.000000 0.017400 0.016600 = 0.019320 -0.000430 0.005460 -0.000440 AFIX 43 H24 2 0.030380 0.509578 0.599347 11.000000 -1.200000 AFIX 0 C25 1 0.133013 0.466500 0.638760 11.000000 0.027430 0.012190 = 0.028160 0.001420 0.009370 0.001380 AFIX 43 H25 2 0.114386 0.423292 0.646692 11.000000 -1.200000 AFIX 0 C26 1 0.209829 0.477141 0.655424 11.000000 0.023660 0.016710 = 0.021610 -0.001390 0.004450 0.005660 AFIX 43 H26 2 0.243951 0.441650 0.674528 11.000000 -1.200000 AFIX 0 C27 1 0.236064 0.540310 0.643795 11.000000 0.017100 0.023810 = 0.016620 -0.001930 0.005740 0.001500 AFIX 43 H27 2 0.288750 0.548082 0.655065 11.000000 -1.200000 AFIX 0 C28 1 0.186779 0.592706 0.615905 11.000000 0.017120 0.015840 = 0.014910 -0.000270 0.006300 0.000740 AFIX 43 H28 2 0.205314 0.636017 0.608157 11.000000 -1.200000 AFIX 0 C29 1 0.188900 0.886763 0.513120 11.000000 0.016680 0.014370 = 0.016350 0.004150 0.006190 0.001000 C30 1 0.181736 0.857673 0.451823 11.000000 0.024650 0.016480 = 0.019560 -0.000670 0.009920 0.000320 AFIX 43 H30 2 0.150566 0.818880 0.438260 11.000000 -1.200000 AFIX 0 C31 1 0.219717 0.884798 0.410246 11.000000 0.030720 0.031390 = 0.020340 0.003800 0.014350 0.005140 AFIX 43 H31 2 0.214490 0.864863 0.368028 11.000000 -1.200000 AFIX 0 C32 1 0.265504 0.941178 0.430202 11.000000 0.028260 0.029990 = 0.030940 0.009150 0.019830 0.002240 AFIX 43 H32 2 0.291659 0.960156 0.401733 11.000000 -1.200000 AFIX 0 C33 1 0.272773 0.969388 0.491403 11.000000 0.026140 0.021690 = 0.033990 0.005170 0.011380 -0.006540 AFIX 43 H33 2 0.304580 1.007761 0.505102 11.000000 -1.200000 AFIX 0 C34 1 0.234619 0.943032 0.533739 11.000000 0.025510 0.019450 = 0.021250 -0.000030 0.010120 -0.003760 AFIX 43 H34 2 0.239758 0.963134 0.575872 11.000000 -1.200000 AFIX 0 C35 1 0.301343 0.819300 0.661950 11.000000 0.012520 0.015280 = 0.018540 0.003230 0.006980 -0.000530 C36 1 0.291508 0.764336 0.618751 11.000000 0.013210 0.019540 = 0.020080 0.001950 0.007190 -0.002240 AFIX 43 H36 2 0.244374 0.756601 0.586696 11.000000 -1.200000 AFIX 0 C37 1 0.351782 0.720902 0.623251 11.000000 0.022390 0.018010 = 0.032280 0.001180 0.014850 0.002250 AFIX 43 H37 2 0.345728 0.683070 0.594089 11.000000 -1.200000 AFIX 0 C38 1 0.420540 0.732171 0.669765 11.000000 0.020510 0.027770 = 0.039180 0.005210 0.013380 0.007970 AFIX 43 H38 2 0.461282 0.701927 0.672727 11.000000 -1.200000 AFIX 0 C39 1 0.429889 0.787492 0.711927 11.000000 0.014020 0.035630 = 0.033530 0.004960 0.003150 -0.000980 AFIX 43 H39 2 0.477236 0.795546 0.743561 11.000000 -1.200000 AFIX 0 C40 1 0.370218 0.831212 0.708069 11.000000 0.016160 0.022080 = 0.021140 0.001850 0.005000 -0.003410 AFIX 43 H40 2 0.376594 0.869251 0.737012 11.000000 -1.200000 AFIX 0 C41 1 0.075333 0.958794 0.654210 11.000000 0.015770 0.009650 = 0.017600 0.003910 0.005950 0.000370 C42 1 0.082990 0.994512 0.712083 11.000000 0.027540 0.014920 = 0.016130 0.002700 0.002980 0.003920 AFIX 43 H42 2 0.130507 0.997532 0.744690 11.000000 -1.200000 AFIX 0 C43 1 0.020282 1.026030 0.722081 11.000000 0.039810 0.021550 = 0.017550 0.001970 0.010930 0.012330 AFIX 43 H43 2 0.024850 1.050932 0.761740 11.000000 -1.200000 AFIX 0 C44 1 -0.048376 1.021375 0.674872 11.000000 0.025780 0.019490 = 0.031950 0.005470 0.016860 0.005050 AFIX 43 H44 2 -0.091020 1.043381 0.681811 11.000000 -1.200000 AFIX 0 C45 1 -0.055516 0.984895 0.617539 11.000000 0.013080 0.019830 = 0.036210 -0.000170 0.003470 0.000370 AFIX 43 H45 2 -0.103160 0.981626 0.585146 11.000000 -1.200000 AFIX 0 C46 1 0.006779 0.952758 0.606797 11.000000 0.021110 0.016630 = 0.022150 -0.004950 0.005990 -0.001750 AFIX 43 H46 2 0.002052 0.927166 0.567508 11.000000 -1.200000 AFIX 0 C47 1 -0.172668 0.645496 0.614463 11.000000 0.018080 0.014860 = 0.008220 0.001170 -0.001140 -0.001930 C48 1 -0.246302 0.623275 0.594860 11.000000 0.019720 0.027030 = 0.012700 -0.001740 0.005400 -0.003800 AFIX 43 H48 2 -0.282954 0.643293 0.612512 11.000000 -1.200000 AFIX 0 C49 1 -0.265525 0.570974 0.548732 11.000000 0.022530 0.031820 = 0.022290 -0.003140 0.002750 -0.011640 AFIX 43 H49 2 -0.315655 0.554234 0.535255 11.000000 -1.200000 AFIX 0 C50 1 -0.212642 0.543330 0.522505 11.000000 0.034440 0.025150 = 0.019930 -0.008000 0.003430 -0.003630 AFIX 43 H50 2 -0.226281 0.507385 0.491137 11.000000 -1.200000 AFIX 0 C51 1 -0.139859 0.567326 0.541331 11.000000 0.025970 0.034990 = 0.019480 -0.006210 0.007920 0.003730 AFIX 43 H51 2 -0.103712 0.548480 0.522354 11.000000 -1.200000 AFIX 0 C52 1 -0.119328 0.618842 0.587846 11.000000 0.013700 0.030680 = 0.018730 -0.001920 0.003610 -0.002140 AFIX 43 H52 2 -0.069179 0.635541 0.601189 11.000000 -1.200000 AFIX 0 C53 1 -0.057237 0.577621 0.794026 11.000000 0.014230 0.014050 = 0.015350 0.002360 0.003410 -0.003800 C54 1 -0.066769 0.588364 0.856109 11.000000 0.018960 0.017030 = 0.021070 0.000280 0.006440 0.001290 AFIX 43 H54 2 -0.093977 0.626775 0.864067 11.000000 -1.200000 AFIX 0 C55 1 -0.036061 0.542296 0.906427 11.000000 0.026860 0.028440 = 0.016470 0.004570 0.004060 -0.000400 AFIX 43 H55 2 -0.042385 0.549156 0.949176 11.000000 -1.200000 AFIX 0 C56 1 0.003777 0.486321 0.895064 11.000000 0.022760 0.021320 = 0.025510 0.007670 0.001640 -0.002180 AFIX 43 H56 2 0.024034 0.454590 0.929671 11.000000 -1.200000 AFIX 0 C57 1 0.013899 0.476858 0.833402 11.000000 0.023510 0.015130 = 0.031350 0.000890 0.007930 0.001470 AFIX 43 H57 2 0.041678 0.438704 0.825769 11.000000 -1.200000 AFIX 0 C58 1 -0.016165 0.522638 0.782128 11.000000 0.021060 0.017010 = 0.018200 -0.002130 0.007520 -0.001860 AFIX 43 H58 2 -0.008683 0.516332 0.739733 11.000000 -1.200000 AFIX 0 C59 1 -0.236940 0.690289 0.754788 11.000000 0.010320 0.022860 = 0.019400 0.003010 0.004730 -0.004310 C60 1 -0.292029 0.737932 0.740002 11.000000 0.026290 0.022840 = 0.089410 0.014890 0.026340 0.002730 AFIX 43 H60 2 -0.279685 0.784949 0.743025 11.000000 -1.200000 AFIX 0 C61 1 -0.366584 0.717297 0.720421 11.000000 0.022440 0.030150 = 0.131980 0.022100 0.019150 0.009340 AFIX 43 H61 2 -0.405436 0.750471 0.709721 11.000000 -1.200000 AFIX 0 C62 1 -0.385016 0.649149 0.716292 11.000000 0.019000 0.035210 = 0.081380 0.018780 0.011130 -0.003020 AFIX 43 H62 2 -0.436205 0.635265 0.702719 11.000000 -1.200000 AFIX 0 C63 1 -0.329112 0.602218 0.731861 11.000000 0.023210 0.026840 = 0.025620 0.006880 0.007100 -0.007590 AFIX 43 H63 2 -0.341398 0.555209 0.729991 11.000000 -1.200000 AFIX 0 C64 1 -0.254737 0.621889 0.750351 11.000000 0.020440 0.023650 = 0.017660 -0.001670 0.009470 -0.001560 AFIX 43 H64 2 -0.215949 0.588646 0.759985 11.000000 -1.200000 AFIX 0 C65 1 -0.172260 0.895647 0.721432 11.000000 0.014190 0.009650 = 0.017180 0.003340 0.002170 -0.001770 C66 1 -0.234425 0.923847 0.735607 11.000000 0.018270 0.014690 = 0.019980 0.000340 0.008450 0.002050 AFIX 43 H66 2 -0.228896 0.946363 0.776687 11.000000 -1.200000 AFIX 0 C67 1 -0.304785 0.918875 0.689235 11.000000 0.018250 0.016910 = 0.029950 0.004470 0.009050 0.003010 AFIX 43 H67 2 -0.347238 0.939565 0.697845 11.000000 -1.200000 AFIX 0 C68 1 -0.313091 0.883796 0.630487 11.000000 0.017390 0.022510 = 0.026360 0.003400 -0.002420 -0.001850 AFIX 43 H68 2 -0.361265 0.879686 0.599015 11.000000 -1.200000 AFIX 0 C69 1 -0.250739 0.854805 0.617994 11.000000 0.027120 0.026290 = 0.014780 -0.003180 0.001320 -0.002300 AFIX 43 H69 2 -0.256783 0.829760 0.578184 11.000000 -1.200000 AFIX 0 C70 1 -0.179424 0.861545 0.662460 11.000000 0.018770 0.017350 = 0.020950 0.001510 0.006070 0.002350 AFIX 43 H70 2 -0.136583 0.843156 0.652585 11.000000 -1.200000 AFIX 0 C71 1 0.024569 0.957051 0.879636 11.000000 0.019750 0.012260 = 0.010990 -0.001520 0.003720 -0.000930 C72 1 0.096039 0.985574 0.901045 11.000000 0.015980 0.015130 = 0.020420 0.001550 0.005690 0.003170 AFIX 43 H72 2 0.137653 0.963307 0.892445 11.000000 -1.200000 AFIX 0 C73 1 0.105891 1.046557 0.934911 11.000000 0.021880 0.016530 = 0.023130 0.000610 0.000050 -0.003170 AFIX 43 H73 2 0.154676 1.066079 0.950079 11.000000 -1.200000 AFIX 0 C74 1 0.045540 1.079423 0.946939 11.000000 0.032650 0.014230 = 0.024620 -0.005950 0.006450 -0.000390 AFIX 43 H74 2 0.052448 1.121916 0.969392 11.000000 -1.200000 AFIX 0 C75 1 -0.025172 1.050079 0.926075 11.000000 0.026380 0.024550 = 0.029740 -0.008800 0.013760 0.001640 AFIX 43 H75 2 -0.066565 1.072451 0.934962 11.000000 -1.200000 AFIX 0 C76 1 -0.036587 0.988439 0.892348 11.000000 0.016700 0.020270 = 0.023260 -0.004780 0.007500 -0.001650 AFIX 43 H76 2 -0.085143 0.968319 0.878352 11.000000 -1.200000 AFIX 0 C77 1 0.005243 0.786121 0.951070 11.000000 0.021910 0.025840 = 0.021760 0.002620 0.009880 0.007000 AFIX 43 H77 2 0.042852 0.811550 0.939125 11.000000 -1.200000 AFIX 0 C78 1 0.024067 0.745554 1.007557 11.000000 0.033630 0.034140 = 0.020240 0.004760 0.007090 0.013760 AFIX 43 H78 2 0.074819 0.743521 1.034542 11.000000 -1.200000 AFIX 0 C79 1 -0.030529 0.708086 1.024823 11.000000 0.054590 0.026310 = 0.023030 0.005760 0.020600 0.012570 AFIX 43 H79 2 -0.017402 0.680525 1.063558 11.000000 -1.200000 AFIX 0 C80 1 -0.104417 0.711036 0.985263 11.000000 0.047450 0.022460 = 0.027790 -0.001040 0.021100 -0.003390 AFIX 43 H80 2 -0.142012 0.685288 0.996896 11.000000 -1.200000 AFIX 0 C81 1 -0.123790 0.751182 0.929000 11.000000 0.028840 0.021140 = 0.023580 -0.004560 0.012630 -0.000910 AFIX 43 H81 2 -0.174465 0.752841 0.901796 11.000000 -1.200000 AFIX 0 C82 1 -0.068877 0.789014 0.912482 11.000000 0.025520 0.014490 = 0.016090 -0.000180 0.010800 0.004890 HKLF 4 END ; 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 0.155546(12) 0.719880(11) 0.797219(11) 0.01082(5) Uani 1 1 d . . . Rh2 Rh 0.098924(12) 0.769326(10) 0.659815(11) 0.00988(5) Uani 1 1 d . . . Rh3 Rh -0.002749(12) 0.765050(11) 0.756380(11) 0.01025(5) Uani 1 1 d . . . S1 S 0.05669(4) 0.67972(3) 0.71261(3) 0.01153(14) Uani 1 1 d . . . S2 S 0.10833(4) 0.82509(3) 0.76020(3) 0.01150(14) Uani 1 1 d . . . C1 C 0.26998(16) 0.73624(14) 0.86080(14) 0.0143(6) Uani 1 1 d . . . C2 C 0.22075(16) 0.72778(14) 0.90048(14) 0.0151(6) Uani 1 1 d . . . C3 C 0.18631(16) 0.66069(14) 0.88626(14) 0.0141(6) Uani 1 1 d . . . C4 C 0.21664(16) 0.62797(14) 0.83923(14) 0.0134(6) Uani 1 1 d . . . C5 C 0.26596(16) 0.67538(14) 0.82144(14) 0.0137(6) Uani 1 1 d . . . C6 C 0.31868(17) 0.79655(15) 0.86044(16) 0.0202(7) Uani 1 1 d . . . H6A H 0.3097 0.8313 0.8907 0.030 Uiso 1 1 calc R . . H6B H 0.3066 0.8152 0.8154 0.030 Uiso 1 1 calc R . . H6C H 0.3716 0.7827 0.8750 0.030 Uiso 1 1 calc R . . C7 C 0.20896(18) 0.77683(15) 0.95067(15) 0.0210(7) Uani 1 1 d . . . H7A H 0.2533 0.7768 0.9897 0.031 Uiso 1 1 calc R . . H7B H 0.1646 0.7633 0.9639 0.031 Uiso 1 1 calc R . . H7C H 0.2013 0.8226 0.9314 0.031 Uiso 1 1 calc R . . C8 C 0.13143(17) 0.63256(15) 0.91849(14) 0.0184(6) Uani 1 1 d . . . H8A H 0.1088 0.5911 0.8953 0.028 Uiso 1 1 calc R . . H8B H 0.0919 0.6662 0.9165 0.028 Uiso 1 1 calc R . . H8C H 0.1573 0.6218 0.9650 0.028 Uiso 1 1 calc R . . C9 C 0.19993(17) 0.55778(14) 0.81104(15) 0.0186(6) Uani 1 1 d . . . H9A H 0.1614 0.5367 0.8281 0.028 Uiso 1 1 calc R . . H9B H 0.2459 0.5303 0.8241 0.028 Uiso 1 1 calc R . . H9C H 0.1816 0.5604 0.7625 0.028 Uiso 1 1 calc R . . C10 C 0.31095(17) 0.66332(15) 0.77430(15) 0.0183(6) Uani 1 1 d . . . H10A H 0.3590 0.6422 0.7979 0.027 Uiso 1 1 calc R . . H10B H 0.3204 0.7068 0.7553 0.027 Uiso 1 1 calc R . . H10C H 0.2831 0.6331 0.7386 0.027 Uiso 1 1 calc R . . P1 P 0.06976(4) 0.70989(4) 0.56807(4) 0.01143(15) Uani 1 1 d . . . P2 P 0.15497(4) 0.85455(4) 0.62790(4) 0.01135(15) Uani 1 1 d . . . P3 P -0.10103(4) 0.69923(4) 0.73509(4) 0.01232(15) Uani 1 1 d . . . P4 P -0.04520(4) 0.84739(4) 0.80534(4) 0.01271(15) Uani 1 1 d . . . O1 O -0.01446(11) 0.71916(9) 0.51769(9) 0.0140(4) Uani 1 1 d . . . O2 O 0.12343(11) 0.71503(10) 0.51925(9) 0.0147(4) Uani 1 1 d . . . O3 O 0.05615(11) 0.62813(9) 0.56880(9) 0.0132(4) Uani 1 1 d . . . O4 O 0.14609(11) 0.85640(10) 0.54944(10) 0.0159(4) Uani 1 1 d . . . O5 O 0.24570(11) 0.86579(10) 0.66104(10) 0.0154(4) Uani 1 1 d . . . O6 O 0.14105(11) 0.93292(9) 0.64435(10) 0.0153(4) Uani 1 1 d . . . O7 O -0.15357(11) 0.70044(10) 0.65897(10) 0.0157(4) Uani 1 1 d . . . O8 O -0.09237(11) 0.61669(9) 0.73921(9) 0.0139(4) Uani 1 1 d . . . O9 O -0.16243(11) 0.71395(10) 0.77423(10) 0.0162(4) Uani 1 1 d . . . O10 O -0.10182(11) 0.90673(10) 0.76652(10) 0.0153(4) Uani 1 1 d . . . O11 O 0.02195(11) 0.89598(10) 0.84585(10) 0.0168(4) Uani 1 1 d . . . O12 O -0.09262(11) 0.83266(10) 0.85853(10) 0.0159(4) Uani 1 1 d . . . C11 C -0.04497(15) 0.78342(14) 0.49781(14) 0.0131(6) Uani 1 1 d . . . C12 C -0.02151(16) 0.81930(15) 0.45125(14) 0.0167(6) Uani 1 1 d . . . H12 H 0.0177 0.8022 0.4350 0.020 Uiso 1 1 calc R . . C13 C -0.05606(18) 0.88101(15) 0.42826(15) 0.0206(7) Uani 1 1 d . . . H13 H -0.0400 0.9067 0.3966 0.025 Uiso 1 1 calc R . . C14 C -0.11364(17) 0.90490(15) 0.45154(15) 0.0210(7) Uani 1 1 d . . . H14 H -0.1372 0.9470 0.4358 0.025 Uiso 1 1 calc R . . C15 C -0.13710(17) 0.86755(15) 0.49781(15) 0.0188(7) Uani 1 1 d . . . H15 H -0.1773 0.8839 0.5131 0.023 Uiso 1 1 calc R . . C16 C -0.10235(16) 0.80631(15) 0.52204(15) 0.0164(6) Uani 1 1 d . . . H16 H -0.1176 0.7809 0.5543 0.020 Uiso 1 1 calc R . . C17 C 0.12286(17) 0.67518(14) 0.46421(14) 0.0154(6) Uani 1 1 d . . . C18 C 0.05918(18) 0.64405(15) 0.42368(15) 0.0206(7) Uani 1 1 d . . . H18 H 0.0123 0.6476 0.4331 0.025 Uiso 1 1 calc R . . C19 C 0.0653(2) 0.60737(16) 0.36889(16) 0.0259(8) Uani 1 1 d . . . H19 H 0.0220 0.5858 0.3408 0.031 Uiso 1 1 calc R . . C20 C 0.1328(2) 0.60183(18) 0.35474(18) 0.0345(9) Uani 1 1 d . . . H20 H 0.1361 0.5766 0.3171 0.041 Uiso 1 1 calc R . . C21 C 0.1962(2) 0.63321(19) 0.39567(19) 0.0371(9) Uani 1 1 d . . . H21 H 0.2431 0.6292 0.3863 0.045 Uiso 1 1 calc R . . C22 C 0.19124(19) 0.67026(17) 0.44999(17) 0.0257(7) Uani 1 1 d . . . H22 H 0.2345 0.6924 0.4776 0.031 Uiso 1 1 calc R . . C23 C 0.11010(16) 0.58054(14) 0.59963(14) 0.0142(6) Uani 1 1 d . . . C24 C 0.08303(17) 0.51760(14) 0.61082(15) 0.0177(6) Uani 1 1 d . . . H24 H 0.0304 0.5096 0.5993 0.021 Uiso 1 1 calc R . . C25 C 0.13301(18) 0.46650(15) 0.63876(16) 0.0223(7) Uani 1 1 d . . . H25 H 0.1144 0.4233 0.6467 0.027 Uiso 1 1 calc R . . C26 C 0.20983(18) 0.47714(15) 0.65542(15) 0.0211(7) Uani 1 1 d . . . H26 H 0.2440 0.4417 0.6745 0.025 Uiso 1 1 calc R . . C27 C 0.23606(17) 0.54031(15) 0.64380(15) 0.0190(6) Uani 1 1 d . . . H27 H 0.2888 0.5481 0.6551 0.023 Uiso 1 1 calc R . . C28 C 0.18678(16) 0.59271(15) 0.61591(14) 0.0156(6) Uani 1 1 d . . . H28 H 0.2053 0.6360 0.6082 0.019 Uiso 1 1 calc R . . C29 C 0.18890(16) 0.88676(14) 0.51312(15) 0.0155(6) Uani 1 1 d . . . C30 C 0.18174(18) 0.85767(15) 0.45182(15) 0.0195(7) Uani 1 1 d . . . H30 H 0.1506 0.8189 0.4383 0.023 Uiso 1 1 calc R . . C31 C 0.21972(19) 0.88480(17) 0.41025(17) 0.0260(7) Uani 1 1 d . . . H31 H 0.2145 0.8649 0.3680 0.031 Uiso 1 1 calc R . . C32 C 0.26550(19) 0.94118(17) 0.43020(17) 0.0274(8) Uani 1 1 d . . . H32 H 0.2917 0.9602 0.4017 0.033 Uiso 1 1 calc R . . C33 C 0.27277(19) 0.96939(17) 0.49140(17) 0.0267(8) Uani 1 1 d . . . H33 H 0.3046 1.0078 0.5051 0.032 Uiso 1 1 calc R . . C34 C 0.23462(18) 0.94303(15) 0.53374(16) 0.0214(7) Uani 1 1 d . . . H34 H 0.2398 0.9631 0.5759 0.026 Uiso 1 1 calc R . . C35 C 0.30134(16) 0.81930(14) 0.66195(15) 0.0149(6) Uani 1 1 d . . . C36 C 0.29151(16) 0.76434(15) 0.61875(15) 0.0171(6) Uani 1 1 d . . . H36 H 0.2444 0.7566 0.5867 0.021 Uiso 1 1 calc R . . C37 C 0.35178(18) 0.72090(16) 0.62325(17) 0.0228(7) Uani 1 1 d . . . H37 H 0.3457 0.6831 0.5941 0.027 Uiso 1 1 calc R . . C38 C 0.42054(19) 0.73217(17) 0.66976(18) 0.0282(8) Uani 1 1 d . . . H38 H 0.4613 0.7019 0.6727 0.034 Uiso 1 1 calc R . . C39 C 0.42989(18) 0.78749(18) 0.71193(18) 0.0285(8) Uani 1 1 d . . . H39 H 0.4772 0.7955 0.7436 0.034 Uiso 1 1 calc R . . C40 C 0.37022(17) 0.83121(16) 0.70807(16) 0.0199(7) Uani 1 1 d . . . H40 H 0.3766 0.8693 0.7370 0.024 Uiso 1 1 calc R . . C41 C 0.07533(16) 0.95879(14) 0.65421(14) 0.0141(6) Uani 1 1 d . . . C42 C 0.08299(18) 0.99451(15) 0.71208(15) 0.0202(7) Uani 1 1 d . . . H42 H 0.1305 0.9975 0.7447 0.024 Uiso 1 1 calc R . . C43 C 0.0203(2) 1.02603(16) 0.72208(16) 0.0257(8) Uani 1 1 d . . . H43 H 0.0248 1.0509 0.7617 0.031 Uiso 1 1 calc R . . C44 C -0.04838(19) 1.02137(16) 0.67487(17) 0.0239(7) Uani 1 1 d . . . H44 H -0.0910 1.0434 0.6818 0.029 Uiso 1 1 calc R . . C45 C -0.05552(17) 0.98490(15) 0.61754(17) 0.0238(7) Uani 1 1 d . . . H45 H -0.1032 0.9816 0.5851 0.029 Uiso 1 1 calc R . . C46 C 0.00678(17) 0.95276(15) 0.60680(16) 0.0200(7) Uani 1 1 d . . . H46 H 0.0021 0.9272 0.5675 0.024 Uiso 1 1 calc R . . C47 C -0.17267(16) 0.64550(14) 0.61446(14) 0.0148(6) Uani 1 1 d . . . C48 C -0.24630(17) 0.62327(16) 0.59486(15) 0.0197(7) Uani 1 1 d . . . H48 H -0.2830 0.6433 0.6125 0.024 Uiso 1 1 calc R . . C49 C -0.26552(19) 0.57097(17) 0.54873(16) 0.0263(8) Uani 1 1 d . . . H49 H -0.3157 0.5542 0.5353 0.032 Uiso 1 1 calc R . . C50 C -0.2126(2) 0.54333(17) 0.52250(16) 0.0274(8) Uani 1 1 d . . . H50 H -0.2263 0.5074 0.4911 0.033 Uiso 1 1 calc R . . C51 C -0.13986(19) 0.56733(17) 0.54133(16) 0.0265(8) Uani 1 1 d . . . H51 H -0.1037 0.5485 0.5224 0.032 Uiso 1 1 calc R . . C52 C -0.11933(17) 0.61884(16) 0.58785(15) 0.0213(7) Uani 1 1 d . . . H52 H -0.0692 0.6355 0.6012 0.026 Uiso 1 1 calc R . . C53 C -0.05724(16) 0.57762(14) 0.79403(14) 0.0147(6) Uani 1 1 d . . . C54 C -0.06677(17) 0.58836(15) 0.85611(15) 0.0189(7) Uani 1 1 d . . . H54 H -0.0940 0.6268 0.8641 0.023 Uiso 1 1 calc R . . C55 C -0.03606(18) 0.54230(17) 0.90643(16) 0.0244(7) Uani 1 1 d . . . H55 H -0.0424 0.5492 0.9492 0.029 Uiso 1 1 calc R . . C56 C 0.00378(18) 0.48632(16) 0.89506(17) 0.0243(7) Uani 1 1 d . . . H56 H 0.0240 0.4546 0.9297 0.029 Uiso 1 1 calc R . . C57 C 0.01390(18) 0.47686(16) 0.83340(17) 0.0233(7) Uani 1 1 d . . . H57 H 0.0417 0.4387 0.8258 0.028 Uiso 1 1 calc R . . C58 C -0.01617(17) 0.52264(15) 0.78213(15) 0.0184(6) Uani 1 1 d . . . H58 H -0.0087 0.5163 0.7397 0.022 Uiso 1 1 calc R . . C59 C -0.23694(16) 0.69029(15) 0.75479(15) 0.0174(6) Uani 1 1 d . . . C60 C -0.2920(2) 0.73793(19) 0.7400(2) 0.0442(11) Uani 1 1 d . . . H60 H -0.2797 0.7849 0.7430 0.053 Uiso 1 1 calc R . . C61 C -0.3666(2) 0.7173(2) 0.7204(3) 0.0622(16) Uani 1 1 d . . . H61 H -0.4054 0.7505 0.7097 0.075 Uiso 1 1 calc R . . C62 C -0.3850(2) 0.64915(19) 0.7163(2) 0.0459(11) Uani 1 1 d . . . H62 H -0.4362 0.6353 0.7027 0.055 Uiso 1 1 calc R . . C63 C -0.32911(18) 0.60222(17) 0.73186(16) 0.0252(7) Uani 1 1 d . . . H63 H -0.3414 0.5552 0.7300 0.030 Uiso 1 1 calc R . . C64 C -0.25474(18) 0.62189(16) 0.75035(15) 0.0197(7) Uani 1 1 d . . . H64 H -0.2159 0.5886 0.7600 0.024 Uiso 1 1 calc R . . C65 C -0.17226(16) 0.89565(14) 0.72143(14) 0.0142(6) Uani 1 1 d . . . C66 C -0.23443(16) 0.92385(14) 0.73561(15) 0.0170(6) Uani 1 1 d . . . H66 H -0.2289 0.9464 0.7767 0.020 Uiso 1 1 calc R . . C67 C -0.30478(17) 0.91887(15) 0.68923(16) 0.0213(7) Uani 1 1 d . . . H67 H -0.3472 0.9396 0.6978 0.026 Uiso 1 1 calc R . . C68 C -0.31309(18) 0.88380(16) 0.63049(16) 0.0239(7) Uani 1 1 d . . . H68 H -0.3613 0.8797 0.5990 0.029 Uiso 1 1 calc R . . C69 C -0.25074(18) 0.85480(16) 0.61799(16) 0.0237(7) Uani 1 1 d . . . H69 H -0.2568 0.8298 0.5782 0.028 Uiso 1 1 calc R . . C70 C -0.17942(17) 0.86154(15) 0.66246(15) 0.0190(6) Uani 1 1 d . . . H70 H -0.1366 0.8432 0.6526 0.023 Uiso 1 1 calc R . . C71 C 0.02457(16) 0.95705(14) 0.87964(14) 0.0145(6) Uani 1 1 d . . . C72 C 0.09604(17) 0.98557(15) 0.90104(15) 0.0171(6) Uani 1 1 d . . . H72 H 0.1377 0.9633 0.8924 0.021 Uiso 1 1 calc R . . C73 C 0.10589(18) 1.04656(15) 0.93491(16) 0.0219(7) Uani 1 1 d . . . H73 H 0.1547 1.0661 0.9501 0.026 Uiso 1 1 calc R . . C74 C 0.04554(19) 1.07942(16) 0.94694(16) 0.0242(7) Uani 1 1 d . . . H74 H 0.0524 1.1219 0.9694 0.029 Uiso 1 1 calc R . . C75 C -0.02517(19) 1.05008(17) 0.92607(17) 0.0257(7) Uani 1 1 d . . . H75 H -0.0666 1.0725 0.9350 0.031 Uiso 1 1 calc R . . C76 C -0.03659(17) 0.98844(15) 0.89235(15) 0.0197(7) Uani 1 1 d . . . H76 H -0.0851 0.9683 0.8784 0.024 Uiso 1 1 calc R . . C77 C 0.00524(18) 0.78612(16) 0.95107(16) 0.0224(7) Uani 1 1 d . . . H77 H 0.0429 0.8115 0.9391 0.027 Uiso 1 1 calc R . . C78 C 0.0241(2) 0.74555(18) 1.00756(17) 0.0295(8) Uani 1 1 d . . . H78 H 0.0748 0.7435 1.0345 0.035 Uiso 1 1 calc R . . C79 C -0.0305(2) 0.70809(18) 1.02482(18) 0.0327(9) Uani 1 1 d . . . H79 H -0.0174 0.6805 1.0636 0.039 Uiso 1 1 calc R . . C80 C -0.1044(2) 0.71104(17) 0.98526(17) 0.0304(8) Uani 1 1 d . . . H80 H -0.1420 0.6853 0.9969 0.036 Uiso 1 1 calc R . . C81 C -0.12379(19) 0.75118(16) 0.92900(16) 0.0235(7) Uani 1 1 d . . . H81 H -0.1745 0.7528 0.9018 0.028 Uiso 1 1 calc R . . C82 C -0.06888(18) 0.78901(15) 0.91248(15) 0.0177(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 0.01166(11) 0.00976(10) 0.01033(11) 0.00049(8) 0.00203(8) 0.00077(8) Rh2 0.01086(11) 0.00924(10) 0.00973(11) 0.00034(8) 0.00327(8) 0.00019(8) Rh3 0.01074(11) 0.00984(10) 0.01038(11) -0.00061(8) 0.00339(8) -0.00028(8) S1 0.0130(3) 0.0106(3) 0.0111(3) -0.0002(3) 0.0036(3) -0.0003(3) S2 0.0131(3) 0.0104(3) 0.0111(3) -0.0004(3) 0.0037(3) -0.0005(3) C1 0.0106(13) 0.0174(14) 0.0115(14) 0.0022(11) -0.0020(11) 0.0026(11) C2 0.0141(14) 0.0158(14) 0.0123(14) 0.0015(11) -0.0012(11) 0.0006(11) C3 0.0163(15) 0.0134(14) 0.0109(14) 0.0018(11) 0.0010(11) 0.0012(11) C4 0.0141(14) 0.0126(14) 0.0109(14) 0.0022(11) -0.0006(11) 0.0031(11) C5 0.0131(14) 0.0140(14) 0.0121(14) 0.0015(11) 0.0003(11) 0.0020(11) C6 0.0190(16) 0.0160(15) 0.0236(17) -0.0004(12) 0.0029(13) -0.0021(12) C7 0.0231(17) 0.0229(16) 0.0163(15) -0.0035(13) 0.0047(13) 0.0009(13) C8 0.0225(16) 0.0213(16) 0.0117(15) 0.0022(12) 0.0052(12) -0.0006(12) C9 0.0220(16) 0.0148(15) 0.0181(16) 0.0018(12) 0.0046(13) 0.0017(12) C10 0.0191(16) 0.0195(15) 0.0163(15) 0.0005(12) 0.0052(12) 0.0019(12) P1 0.0132(4) 0.0101(3) 0.0114(4) 0.0001(3) 0.0042(3) 0.0005(3) P2 0.0112(3) 0.0108(3) 0.0122(4) 0.0001(3) 0.0038(3) 0.0002(3) P3 0.0129(4) 0.0129(4) 0.0114(4) -0.0003(3) 0.0038(3) -0.0009(3) P4 0.0122(4) 0.0128(4) 0.0131(4) -0.0013(3) 0.0036(3) -0.0001(3) O1 0.0163(10) 0.0096(9) 0.0132(10) -0.0001(8) -0.0002(8) 0.0005(8) O2 0.0181(11) 0.0150(10) 0.0124(10) -0.0036(8) 0.0066(8) -0.0027(8) O3 0.0138(10) 0.0114(10) 0.0140(10) 0.0009(8) 0.0034(8) 0.0013(8) O4 0.0196(11) 0.0179(11) 0.0115(10) 0.0006(8) 0.0066(8) -0.0052(8) O5 0.0124(10) 0.0146(10) 0.0193(11) -0.0026(8) 0.0044(8) 0.0002(8) O6 0.0154(10) 0.0107(10) 0.0208(11) -0.0008(8) 0.0067(9) 0.0003(8) O7 0.0182(11) 0.0134(10) 0.0136(10) -0.0008(8) 0.0015(8) 0.0006(8) O8 0.0163(10) 0.0124(10) 0.0121(10) 0.0014(8) 0.0025(8) -0.0015(8) O9 0.0118(10) 0.0197(11) 0.0191(11) -0.0020(8) 0.0078(8) -0.0024(8) O10 0.0157(10) 0.0122(10) 0.0171(11) -0.0016(8) 0.0033(9) 0.0003(8) O11 0.0143(10) 0.0160(10) 0.0196(11) -0.0059(8) 0.0040(9) -0.0013(8) O12 0.0160(10) 0.0185(11) 0.0157(11) -0.0001(8) 0.0085(9) 0.0023(8) C11 0.0116(14) 0.0122(13) 0.0118(14) 0.0003(11) -0.0024(11) -0.0002(10) C12 0.0146(15) 0.0189(15) 0.0160(15) 0.0012(12) 0.0034(12) 0.0001(11) C13 0.0243(17) 0.0189(16) 0.0163(16) 0.0052(12) 0.0021(13) -0.0030(13) C14 0.0191(16) 0.0160(15) 0.0212(17) 0.0024(12) -0.0048(13) 0.0030(12) C15 0.0135(15) 0.0203(16) 0.0208(16) -0.0048(13) 0.0019(12) 0.0023(12) C16 0.0140(15) 0.0170(15) 0.0162(15) 0.0003(12) 0.0014(12) -0.0026(11) C17 0.0237(16) 0.0107(14) 0.0146(15) -0.0018(11) 0.0097(12) -0.0009(11) C18 0.0220(16) 0.0229(16) 0.0174(16) -0.0040(13) 0.0064(13) -0.0041(13) C19 0.0326(19) 0.0249(17) 0.0215(17) -0.0083(14) 0.0100(15) -0.0105(14) C20 0.045(2) 0.036(2) 0.031(2) -0.0184(16) 0.0238(18) -0.0108(17) C21 0.036(2) 0.043(2) 0.042(2) -0.0192(18) 0.0267(19) -0.0090(17) C22 0.0245(18) 0.0269(18) 0.0280(19) -0.0095(14) 0.0115(15) -0.0079(14) C23 0.0186(15) 0.0133(14) 0.0112(14) -0.0008(11) 0.0053(12) 0.0047(11) C24 0.0174(15) 0.0166(15) 0.0193(16) -0.0004(12) 0.0055(13) -0.0004(12) C25 0.0274(18) 0.0122(15) 0.0282(18) 0.0014(13) 0.0094(14) 0.0014(12) C26 0.0237(17) 0.0167(15) 0.0216(17) -0.0014(13) 0.0045(14) 0.0057(12) C27 0.0171(15) 0.0238(16) 0.0166(15) -0.0019(12) 0.0057(13) 0.0015(12) C28 0.0171(15) 0.0158(14) 0.0149(15) -0.0003(11) 0.0063(12) 0.0007(11) C29 0.0167(15) 0.0144(14) 0.0164(15) 0.0041(11) 0.0062(12) 0.0010(11) C30 0.0246(17) 0.0165(15) 0.0196(16) -0.0007(12) 0.0099(13) 0.0003(12) C31 0.0307(19) 0.0314(19) 0.0203(17) 0.0038(14) 0.0144(15) 0.0051(15) C32 0.0283(19) 0.0300(19) 0.031(2) 0.0092(15) 0.0198(16) 0.0022(15) C33 0.0261(18) 0.0217(17) 0.034(2) 0.0052(14) 0.0114(16) -0.0065(14) C34 0.0255(17) 0.0194(16) 0.0212(17) 0.0000(13) 0.0101(14) -0.0038(13) C35 0.0125(14) 0.0153(14) 0.0185(15) 0.0032(12) 0.0070(12) -0.0005(11) C36 0.0132(14) 0.0195(15) 0.0201(16) 0.0020(12) 0.0072(12) -0.0022(12) C37 0.0224(17) 0.0180(16) 0.0323(19) 0.0012(14) 0.0149(14) 0.0022(13) C38 0.0205(17) 0.0278(18) 0.039(2) 0.0052(16) 0.0134(15) 0.0080(14) C39 0.0140(16) 0.036(2) 0.034(2) 0.0050(16) 0.0031(14) -0.0010(14) C40 0.0162(15) 0.0221(16) 0.0211(16) 0.0019(13) 0.0050(13) -0.0034(12) C41 0.0158(15) 0.0096(13) 0.0176(15) 0.0039(11) 0.0059(12) 0.0004(11) C42 0.0275(17) 0.0149(15) 0.0161(16) 0.0027(12) 0.0030(13) 0.0039(12) C43 0.040(2) 0.0216(17) 0.0175(16) 0.0020(13) 0.0109(15) 0.0123(15) C44 0.0258(18) 0.0195(16) 0.0319(19) 0.0055(14) 0.0169(15) 0.0050(13) C45 0.0131(15) 0.0198(16) 0.036(2) -0.0002(14) 0.0035(14) 0.0004(12) C46 0.0211(16) 0.0166(15) 0.0221(17) -0.0049(12) 0.0060(13) -0.0018(12) C47 0.0181(15) 0.0149(14) 0.0082(14) 0.0012(11) -0.0011(11) -0.0019(11) C48 0.0197(16) 0.0270(17) 0.0127(15) -0.0017(13) 0.0054(12) -0.0038(13) C49 0.0225(17) 0.0318(19) 0.0223(18) -0.0031(14) 0.0028(14) -0.0116(14) C50 0.034(2) 0.0251(18) 0.0199(17) -0.0080(14) 0.0034(15) -0.0036(15) C51 0.0260(18) 0.0350(19) 0.0195(17) -0.0062(14) 0.0079(14) 0.0037(15) C52 0.0137(15) 0.0307(18) 0.0187(16) -0.0019(13) 0.0036(13) -0.0021(13) C53 0.0142(15) 0.0140(14) 0.0153(15) 0.0024(11) 0.0034(12) -0.0038(11) C54 0.0190(16) 0.0170(15) 0.0211(16) 0.0003(12) 0.0064(13) 0.0013(12) C55 0.0269(18) 0.0284(18) 0.0165(16) 0.0046(13) 0.0041(14) -0.0004(14) C56 0.0228(17) 0.0213(17) 0.0255(18) 0.0077(14) 0.0016(14) -0.0022(13) C57 0.0235(17) 0.0151(15) 0.0314(19) 0.0009(13) 0.0079(15) 0.0015(12) C58 0.0211(16) 0.0170(15) 0.0182(16) -0.0021(12) 0.0075(13) -0.0019(12) C59 0.0103(14) 0.0229(16) 0.0194(16) 0.0030(12) 0.0047(12) -0.0043(12) C60 0.026(2) 0.0228(19) 0.089(4) 0.015(2) 0.026(2) 0.0027(15) C61 0.022(2) 0.030(2) 0.132(5) 0.022(3) 0.019(3) 0.0093(17) C62 0.0190(19) 0.035(2) 0.081(3) 0.019(2) 0.011(2) -0.0030(16) C63 0.0232(17) 0.0268(18) 0.0256(18) 0.0069(14) 0.0071(14) -0.0076(14) C64 0.0204(16) 0.0237(16) 0.0177(16) -0.0017(13) 0.0095(13) -0.0016(13) C65 0.0142(14) 0.0097(13) 0.0172(15) 0.0033(11) 0.0022(12) -0.0018(10) C66 0.0183(16) 0.0147(14) 0.0200(16) 0.0003(12) 0.0085(13) 0.0021(11) C67 0.0182(16) 0.0169(15) 0.0300(18) 0.0045(13) 0.0090(14) 0.0030(12) C68 0.0174(16) 0.0225(17) 0.0264(18) 0.0034(14) -0.0024(14) -0.0018(13) C69 0.0271(18) 0.0263(17) 0.0148(16) -0.0032(13) 0.0013(13) -0.0023(14) C70 0.0188(16) 0.0173(15) 0.0210(16) 0.0015(12) 0.0061(13) 0.0024(12) C71 0.0197(15) 0.0123(14) 0.0110(14) -0.0015(11) 0.0037(12) -0.0009(11) C72 0.0160(15) 0.0151(15) 0.0204(16) 0.0016(12) 0.0057(12) 0.0032(11) C73 0.0219(17) 0.0165(15) 0.0231(17) 0.0006(13) 0.0000(14) -0.0032(12) C74 0.0327(19) 0.0142(15) 0.0246(18) -0.0059(13) 0.0064(15) -0.0004(13) C75 0.0264(18) 0.0246(17) 0.0297(19) -0.0088(14) 0.0138(15) 0.0016(14) C76 0.0167(16) 0.0203(16) 0.0233(17) -0.0048(13) 0.0075(13) -0.0017(12) C77 0.0219(17) 0.0258(17) 0.0218(17) 0.0026(13) 0.0099(14) 0.0070(13) C78 0.034(2) 0.034(2) 0.0202(17) 0.0048(15) 0.0071(15) 0.0138(16) C79 0.055(3) 0.0263(19) 0.0230(18) 0.0058(15) 0.0206(18) 0.0126(17) C80 0.047(2) 0.0225(18) 0.0278(19) -0.0010(14) 0.0211(17) -0.0034(16) C81 0.0288(18) 0.0211(16) 0.0236(17) -0.0046(13) 0.0126(14) -0.0009(13) C82 0.0255(17) 0.0145(14) 0.0161(15) -0.0002(12) 0.0108(13) 0.0049(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 C3 2.138(3) . ? Rh1 C5 2.150(3) . ? Rh1 C2 2.166(3) . ? Rh1 C4 2.180(3) . ? Rh1 C1 2.183(3) . ? Rh1 S2 2.2932(7) . ? Rh1 S1 2.2960(7) . ? Rh1 Rh2 2.9415(4) . ? Rh1 Rh3 2.9505(4) . ? Rh2 P2 2.1785(8) . ? Rh2 P1 2.1867(8) . ? Rh2 S1 2.3361(7) . ? Rh2 S2 2.3415(8) . ? Rh2 Rh3 3.1500(4) . ? Rh3 P3 2.1754(8) . ? Rh3 P4 2.1849(8) . ? Rh3 S1 2.3386(7) . ? Rh3 S2 2.3576(8) . ? C1 C2 1.415(4) . ? C1 C5 1.445(4) . ? C1 C6 1.492(4) . ? C2 C3 1.458(4) . ? C2 C7 1.492(4) . ? C3 C4 1.426(4) . ? C3 C8 1.485(4) . ? C4 C5 1.431(4) . ? C4 C9 1.499(4) . ? C5 C10 1.489(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? P1 O1 1.626(2) . ? P1 O3 1.628(2) . ? P1 O2 1.628(2) . ? P2 O4 1.612(2) . ? P2 O6 1.616(2) . ? P2 O5 1.641(2) . ? P3 O9 1.614(2) . ? P3 O7 1.617(2) . ? P3 O8 1.630(2) . ? P4 O11 1.606(2) . ? P4 O10 1.624(2) . ? P4 O12 1.638(2) . ? O1 C11 1.398(3) . ? O2 C17 1.396(3) . ? O3 C23 1.387(3) . ? O4 C29 1.387(3) . ? O5 C35 1.376(3) . ? O6 C41 1.392(3) . ? O7 C47 1.406(3) . ? O8 C53 1.382(3) . ? O9 C59 1.404(3) . ? O10 C65 1.393(3) . ? O11 C71 1.389(3) . ? O12 C82 1.389(3) . ? C11 C12 1.377(4) . ? C11 C16 1.383(4) . ? C12 C13 1.392(4) . ? C12 H12 0.9500 . ? C13 C14 1.381(4) . ? C13 H13 0.9500 . ? C14 C15 1.387(4) . ? C14 H14 0.9500 . ? C15 C16 1.391(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.384(4) . ? C17 C22 1.390(4) . ? C18 C19 1.392(4) . ? C18 H18 0.9500 . ? C19 C20 1.375(5) . ? C19 H19 0.9500 . ? C20 C21 1.385(5) . ? C20 H20 0.9500 . ? C21 C22 1.381(5) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.381(4) . ? C23 C28 1.386(4) . ? C24 C25 1.379(4) . ? C24 H24 0.9500 . ? C25 C26 1.383(4) . ? C25 H25 0.9500 . ? C26 C27 1.381(4) . ? C26 H26 0.9500 . ? C27 C28 1.390(4) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.382(4) . ? C29 C34 1.385(4) . ? C30 C31 1.380(4) . ? C30 H30 0.9500 . ? C31 C32 1.386(5) . ? C31 H31 0.9500 . ? C32 C33 1.373(5) . ? C32 H32 0.9500 . ? C33 C34 1.389(4) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C40 1.384(4) . ? C35 C36 1.390(4) . ? C36 C37 1.389(4) . ? C36 H36 0.9500 . ? C37 C38 1.384(5) . ? C37 H37 0.9500 . ? C38 C39 1.382(5) . ? C38 H38 0.9500 . ? C39 C40 1.386(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C46 1.377(4) . ? C41 C42 1.377(4) . ? C42 C43 1.388(4) . ? C42 H42 0.9500 . ? C43 C44 1.374(5) . ? C43 H43 0.9500 . ? C44 C45 1.377(5) . ? C44 H44 0.9500 . ? C45 C46 1.393(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C52 1.375(4) . ? C47 C48 1.380(4) . ? C48 C49 1.388(4) . ? C48 H48 0.9500 . ? C49 C50 1.370(5) . ? C49 H49 0.9500 . ? C50 C51 1.377(5) . ? C50 H50 0.9500 . ? C51 C52 1.383(4) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.385(4) . ? C53 C58 1.387(4) . ? C54 C55 1.385(4) . ? C54 H54 0.9500 . ? C55 C56 1.385(5) . ? C55 H55 0.9500 . ? C56 C57 1.377(5) . ? C56 H56 0.9500 . ? C57 C58 1.392(4) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C60 1.355(4) . ? C59 C64 1.381(4) . ? C60 C61 1.386(5) . ? C60 H60 0.9500 . ? C61 C62 1.379(5) . ? C61 H61 0.9500 . ? C62 C63 1.356(5) . ? C62 H62 0.9500 . ? C63 C64 1.377(4) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 C70 1.383(4) . ? C65 C66 1.389(4) . ? C66 C67 1.390(4) . ? C66 H66 0.9500 . ? C67 C68 1.385(5) . ? C67 H67 0.9500 . ? C68 C69 1.382(5) . ? C68 H68 0.9500 . ? C69 C70 1.389(4) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? C71 C76 1.385(4) . ? C71 C72 1.390(4) . ? C72 C73 1.380(4) . ? C72 H72 0.9500 . ? C73 C74 1.379(4) . ? C73 H73 0.9500 . ? C74 C75 1.384(4) . ? C74 H74 0.9500 . ? C75 C76 1.389(4) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77 C82 1.382(4) . ? C77 C78 1.390(4) . ? C77 H77 0.9500 . ? C78 C79 1.384(5) . ? C78 H78 0.9500 . ? C79 C80 1.385(5) . ? C79 H79 0.9500 . ? C80 C81 1.381(5) . ? C80 H80 0.9500 . ? C81 C82 1.385(4) . ? C81 H81 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 C3 Rh1 C5 64.94(11) . . ? C3 Rh1 C2 39.61(10) . . ? C5 Rh1 C2 64.75(11) . . ? C3 Rh1 C4 38.55(11) . . ? C5 Rh1 C4 38.57(10) . . ? C2 Rh1 C4 65.06(10) . . ? C3 Rh1 C1 64.99(11) . . ? C5 Rh1 C1 38.95(10) . . ? C2 Rh1 C1 37.99(11) . . ? C4 Rh1 C1 64.75(10) . . ? C3 Rh1 S2 140.12(8) . . ? C5 Rh1 S2 133.79(8) . . ? C2 Rh1 S2 108.90(8) . . ? C4 Rh1 S2 171.21(8) . . ? C1 Rh1 S2 106.50(8) . . ? C3 Rh1 S1 116.32(8) . . ? C5 Rh1 S1 122.51(8) . . ? C2 Rh1 S1 153.15(8) . . ? C4 Rh1 S1 103.59(7) . . ? C1 Rh1 S1 160.76(8) . . ? S2 Rh1 S1 84.57(3) . . ? C3 Rh1 Rh2 165.97(8) . . ? C5 Rh1 Rh2 114.36(8) . . ? C2 Rh1 Rh2 154.13(8) . . ? C4 Rh1 Rh2 131.95(8) . . ? C1 Rh1 Rh2 124.17(8) . . ? S2 Rh1 Rh2 51.335(18) . . ? S1 Rh1 Rh2 51.183(19) . . ? C3 Rh1 Rh3 114.20(8) . . ? C5 Rh1 Rh3 173.06(8) . . ? C2 Rh1 Rh3 119.42(8) . . ? C4 Rh1 Rh3 136.49(8) . . ? C1 Rh1 Rh3 147.71(8) . . ? S2 Rh1 Rh3 51.598(18) . . ? S1 Rh1 Rh3 51.101(19) . . ? Rh2 Rh1 Rh3 64.638(8) . . ? P2 Rh2 P1 99.04(3) . . ? P2 Rh2 S1 169.32(3) . . ? P1 Rh2 S1 89.17(3) . . ? P2 Rh2 S2 90.03(3) . . ? P1 Rh2 S2 169.02(3) . . ? S1 Rh2 S2 82.62(3) . . ? P2 Rh2 Rh1 119.37(2) . . ? P1 Rh2 Rh1 128.18(2) . . ? S1 Rh2 Rh1 49.979(18) . . ? S2 Rh2 Rh1 49.881(18) . . ? P2 Rh2 Rh3 130.42(2) . . ? P1 Rh2 Rh3 120.93(2) . . ? S1 Rh2 Rh3 47.670(18) . . ? S2 Rh2 Rh3 48.125(19) . . ? Rh1 Rh2 Rh3 57.820(9) . . ? P3 Rh3 P4 98.17(3) . . ? P3 Rh3 S1 87.46(3) . . ? P4 Rh3 S1 173.23(3) . . ? P3 Rh3 S2 168.06(3) . . ? P4 Rh3 S2 92.55(3) . . ? S1 Rh3 S2 82.22(3) . . ? P3 Rh3 Rh1 125.92(2) . . ? P4 Rh3 Rh1 123.41(2) . . ? S1 Rh3 Rh1 49.825(18) . . ? S2 Rh3 Rh1 49.663(18) . . ? P3 Rh3 Rh2 120.44(2) . . ? P4 Rh3 Rh2 130.53(2) . . ? S1 Rh3 Rh2 47.601(18) . . ? S2 Rh3 Rh2 47.688(18) . . ? Rh1 Rh3 Rh2 57.542(9) . . ? Rh1 S1 Rh2 78.84(2) . . ? Rh1 S1 Rh3 79.07(2) . . ? Rh2 S1 Rh3 84.73(2) . . ? Rh1 S2 Rh2 78.78(2) . . ? Rh1 S2 Rh3 78.74(2) . . ? Rh2 S2 Rh3 84.19(2) . . ? C2 C1 C5 107.8(3) . . ? C2 C1 C6 126.3(3) . . ? C5 C1 C6 125.9(3) . . ? C2 C1 Rh1 70.35(16) . . ? C5 C1 Rh1 69.32(15) . . ? C6 C1 Rh1 126.71(19) . . ? C1 C2 C3 107.8(3) . . ? C1 C2 C7 126.4(3) . . ? C3 C2 C7 125.7(3) . . ? C1 C2 Rh1 71.66(16) . . ? C3 C2 Rh1 69.19(15) . . ? C7 C2 Rh1 127.1(2) . . ? C4 C3 C2 108.2(3) . . ? C4 C3 C8 127.6(3) . . ? C2 C3 C8 124.2(3) . . ? C4 C3 Rh1 72.31(16) . . ? C2 C3 Rh1 71.20(16) . . ? C8 C3 Rh1 123.9(2) . . ? C3 C4 C5 107.4(2) . . ? C3 C4 C9 127.7(3) . . ? C5 C4 C9 124.8(3) . . ? C3 C4 Rh1 69.14(15) . . ? C5 C4 Rh1 69.59(15) . . ? C9 C4 Rh1 125.37(19) . . ? C4 C5 C1 108.7(3) . . ? C4 C5 C10 126.6(3) . . ? C1 C5 C10 124.6(3) . . ? C4 C5 Rh1 71.84(16) . . ? C1 C5 Rh1 71.73(16) . . ? C10 C5 Rh1 125.95(19) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 P1 O3 89.66(10) . . ? O1 P1 O2 103.32(11) . . ? O3 P1 O2 101.09(10) . . ? O1 P1 Rh2 117.49(8) . . ? O3 P1 Rh2 121.25(8) . . ? O2 P1 Rh2 118.92(8) . . ? O4 P2 O6 102.87(11) . . ? O4 P2 O5 102.73(11) . . ? O6 P2 O5 89.35(10) . . ? O4 P2 Rh2 114.64(8) . . ? O6 P2 Rh2 123.15(8) . . ? O5 P2 Rh2 119.72(8) . . ? O9 P3 O7 100.96(11) . . ? O9 P3 O8 102.97(11) . . ? O7 P3 O8 95.12(10) . . ? O9 P3 Rh3 117.55(8) . . ? O7 P3 Rh3 115.16(8) . . ? O8 P3 Rh3 121.14(8) . . ? O11 P4 O10 97.47(11) . . ? O11 P4 O12 103.34(11) . . ? O10 P4 O12 94.19(11) . . ? O11 P4 Rh3 111.12(8) . . ? O10 P4 Rh3 124.37(8) . . ? O12 P4 Rh3 122.00(8) . . ? C11 O1 P1 121.77(17) . . ? C17 O2 P1 129.02(18) . . ? C23 O3 P1 125.26(18) . . ? C29 O4 P2 132.01(18) . . ? C35 O5 P2 126.23(18) . . ? C41 O6 P2 125.57(18) . . ? C47 O7 P3 127.75(17) . . ? C53 O8 P3 127.80(18) . . ? C59 O9 P3 125.03(19) . . ? C65 O10 P4 125.02(17) . . ? C71 O11 P4 133.84(19) . . ? C82 O12 P4 124.17(18) . . ? C12 C11 C16 122.2(3) . . ? C12 C11 O1 119.4(3) . . ? C16 C11 O1 118.2(3) . . ? C11 C12 C13 119.0(3) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C14 C13 C12 119.9(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.1(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 120.6(3) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C11 C16 C15 118.1(3) . . ? C11 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? C18 C17 C22 120.5(3) . . ? C18 C17 O2 124.0(3) . . ? C22 C17 O2 115.5(3) . . ? C17 C18 C19 118.7(3) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? C20 C19 C18 121.2(3) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 119.6(3) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 120.1(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C17 119.9(3) . . ? C21 C22 H22 120.0 . . ? C17 C22 H22 120.0 . . ? C24 C23 C28 120.7(3) . . ? C24 C23 O3 115.8(3) . . ? C28 C23 O3 123.4(3) . . ? C25 C24 C23 119.5(3) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C26 121.0(3) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C27 C26 C25 118.8(3) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C26 C27 C28 121.2(3) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C23 C28 C27 118.7(3) . . ? C23 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C30 C29 C34 120.5(3) . . ? C30 C29 O4 114.9(3) . . ? C34 C29 O4 124.6(3) . . ? C31 C30 C29 120.2(3) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 119.9(3) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C33 C32 C31 119.5(3) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C34 121.4(3) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C29 C34 C33 118.5(3) . . ? C29 C34 H34 120.8 . . ? C33 C34 H34 120.8 . . ? O5 C35 C40 115.8(3) . . ? O5 C35 C36 123.5(3) . . ? C40 C35 C36 120.7(3) . . ? C37 C36 C35 118.9(3) . . ? C37 C36 H36 120.6 . . ? C35 C36 H36 120.6 . . ? C38 C37 C36 120.7(3) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C39 C38 C37 119.9(3) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 120.0(3) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C35 C40 C39 119.8(3) . . ? C35 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C46 C41 C42 121.5(3) . . ? C46 C41 O6 121.8(3) . . ? C42 C41 O6 116.6(3) . . ? C41 C42 C43 119.0(3) . . ? C41 C42 H42 120.5 . . ? C43 C42 H42 120.5 . . ? C44 C43 C42 120.3(3) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 120.2(3) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C46 120.3(3) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C41 C46 C45 118.7(3) . . ? C41 C46 H46 120.6 . . ? C45 C46 H46 120.6 . . ? C52 C47 C48 121.7(3) . . ? C52 C47 O7 119.4(3) . . ? C48 C47 O7 118.6(3) . . ? C47 C48 C49 118.4(3) . . ? C47 C48 H48 120.8 . . ? C49 C48 H48 120.8 . . ? C50 C49 C48 120.4(3) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C49 C50 C51 120.4(3) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C50 C51 C52 120.1(3) . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C47 C52 C51 118.9(3) . . ? C47 C52 H52 120.5 . . ? C51 C52 H52 120.5 . . ? O8 C53 C54 123.0(3) . . ? O8 C53 C58 115.7(3) . . ? C54 C53 C58 121.1(3) . . ? C53 C54 C55 119.0(3) . . ? C53 C54 H54 120.5 . . ? C55 C54 H54 120.5 . . ? C54 C55 C56 120.7(3) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C57 C56 C55 119.7(3) . . ? C57 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C56 C57 C58 120.7(3) . . ? C56 C57 H57 119.7 . . ? C58 C57 H57 119.7 . . ? C53 C58 C57 118.8(3) . . ? C53 C58 H58 120.6 . . ? C57 C58 H58 120.6 . . ? C60 C59 C64 120.5(3) . . ? C60 C59 O9 116.9(3) . . ? C64 C59 O9 122.6(3) . . ? C59 C60 C61 119.3(3) . . ? C59 C60 H60 120.4 . . ? C61 C60 H60 120.4 . . ? C62 C61 C60 120.8(4) . . ? C62 C61 H61 119.6 . . ? C60 C61 H61 119.6 . . ? C63 C62 C61 119.1(3) . . ? C63 C62 H62 120.4 . . ? C61 C62 H62 120.4 . . ? C62 C63 C64 120.8(3) . . ? C62 C63 H63 119.6 . . ? C64 C63 H63 119.6 . . ? C63 C64 C59 119.5(3) . . ? C63 C64 H64 120.2 . . ? C59 C64 H64 120.2 . . ? C70 C65 C66 121.1(3) . . ? C70 C65 O10 121.0(3) . . ? C66 C65 O10 117.8(3) . . ? C65 C66 C67 119.5(3) . . ? C65 C66 H66 120.3 . . ? C67 C66 H66 120.3 . . ? C68 C67 C66 120.1(3) . . ? C68 C67 H67 120.0 . . ? C66 C67 H67 120.0 . . ? C69 C68 C67 119.5(3) . . ? C69 C68 H68 120.3 . . ? C67 C68 H68 120.3 . . ? C68 C69 C70 121.3(3) . . ? C68 C69 H69 119.3 . . ? C70 C69 H69 119.3 . . ? C65 C70 C69 118.4(3) . . ? C65 C70 H70 120.8 . . ? C69 C70 H70 120.8 . . ? C76 C71 O11 125.1(3) . . ? C76 C71 C72 121.1(3) . . ? O11 C71 C72 113.8(3) . . ? C73 C72 C71 119.3(3) . . ? C73 C72 H72 120.4 . . ? C71 C72 H72 120.4 . . ? C74 C73 C72 120.6(3) . . ? C74 C73 H73 119.7 . . ? C72 C73 H73 119.7 . . ? C73 C74 C75 119.6(3) . . ? C73 C74 H74 120.2 . . ? C75 C74 H74 120.2 . . ? C74 C75 C76 121.1(3) . . ? C74 C75 H75 119.5 . . ? C76 C75 H75 119.5 . . ? C71 C76 C75 118.4(3) . . ? C71 C76 H76 120.8 . . ? C75 C76 H76 120.8 . . ? C82 C77 C78 119.2(3) . . ? C82 C77 H77 120.4 . . ? C78 C77 H77 120.4 . . ? C79 C78 C77 120.5(3) . . ? C79 C78 H78 119.7 . . ? C77 C78 H78 119.7 . . ? C78 C79 C80 119.6(3) . . ? C78 C79 H79 120.2 . . ? C80 C79 H79 120.2 . . ? C81 C80 C79 120.4(3) . . ? C81 C80 H80 119.8 . . ? C79 C80 H80 119.8 . . ? C80 C81 C82 119.6(3) . . ? C80 C81 H81 120.2 . . ? C82 C81 H81 120.2 . . ? C77 C82 C81 120.7(3) . . ? C77 C82 O12 122.1(3) . . ? C81 C82 O12 117.0(3) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.912 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.101 data_compnd_6 _database_code_depnum_ccdc_archive 'CCDC 908506' #TrackingRef '15071_web_deposit_cif_file_0_FernandoJ.Lahoz_1351623726.compnd_3_6_7_9_11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C80 H72 O12 P4 Pd Rh2 S2' _chemical_formula_sum 'C80 H72 O12 P4 Pd Rh2 S2' _chemical_formula_weight 1725.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 28.003(8) _cell_length_b 11.553(3) _cell_length_c 22.405(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7248(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5308 _cell_measurement_theta_min 2.273 _cell_measurement_theta_max 22.142 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8257 _exptl_absorpt_correction_T_max 0.9561 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within SAINT+ package, v. 6.45. ; _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 SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 80905 _diffrn_reflns_av_R_equivalents 0.1186 _diffrn_reflns_av_sigmaI/netI 0.0894 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.73 _reflns_number_total 15385 _reflns_number_gt 12725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.45 (Bruker AXS, 2003)' _computing_data_reduction 'SAINT+ v. 6.45 (Bruker AXS, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, SHELXTLv6.12, BrukerAXS' _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. All non-hydrogen atoms were refined with anisotropic displacement parameters. Hydrogen atoms were included in calculated positions and refined riding (positional and displacement parameters) on their bonded atoms. Highest residuals were under 1 e/A^3 and were observed close to the metal atoms, with no chemical sense. ; _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^)+(0.0305P)^2^+9.1172P] 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 SHELXL _refine_ls_extinction_coef 0.00007(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 15385 _refine_ls_number_parameters 911 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.1002 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl150bs in Pna2(1) CELL 0.71073 28.0031 11.5529 22.4052 90.000 90.000 90.000 ZERR 4.00 0.0084 0.0034 0.0067 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H O P S Rh Pd UNIT 320 288 48 16 8 8 4 SHEL 100 0.790 MERG 2 L.S. 4 OMIT 28 0 18 OMIT 10 3 -19 OMIT 2 0 0 ACTA 54 BOND $H FMAP 2 PLAN 20 WPDB -2 CONF SIZE 0.05 0.07 0.22 TEMP -173.00 WGHT 0.030500 9.117201 EXTI 0.000073 FVAR 0.13365 PD 7 0.201754 0.116911 0.146883 11.00000 0.01437 0.01960 = 0.01894 0.00045 -0.00026 -0.00007 RH2 6 0.239580 0.306307 0.063600 11.00000 0.01214 0.01992 = 0.01656 -0.00150 0.00036 -0.00019 RH3 6 0.133553 0.313297 0.110490 11.00000 0.01208 0.01932 = 0.01607 -0.00164 -0.00015 -0.00076 S1 5 0.175272 0.174274 0.053503 11.00000 0.01583 0.02116 = 0.01898 -0.00293 0.00079 0.00022 S2 5 0.207714 0.314441 0.161170 11.00000 0.01526 0.01939 = 0.01955 -0.00403 0.00004 -0.00228 C1 1 0.248846 0.068399 0.223478 11.00000 0.02874 0.02157 = 0.02725 0.00912 -0.00302 -0.00362 AFIX 43 H1 2 0.265225 0.139090 0.216396 11.00000 -1.20000 AFIX 0 C2 1 0.203282 0.075761 0.244110 11.00000 0.02320 0.01852 = 0.02018 0.00485 -0.00622 0.00156 AFIX 43 H2 2 0.191274 0.150857 0.252665 11.00000 -1.20000 AFIX 0 C3 1 0.170809 -0.023388 0.254366 11.00000 0.03121 0.02311 = 0.02005 0.00191 -0.00127 0.00026 AFIX 23 H3A 2 0.137743 0.006390 0.257324 11.00000 -1.20000 H3B 2 0.178941 -0.058898 0.293275 11.00000 -1.20000 AFIX 0 C4 1 0.172068 -0.119302 0.205800 11.00000 0.01927 0.03171 = 0.02648 0.00764 0.00434 0.00224 AFIX 23 H4A 2 0.197682 -0.175177 0.215673 11.00000 -1.20000 H4B 2 0.141335 -0.161647 0.206286 11.00000 -1.20000 AFIX 0 C5 1 0.180512 -0.072835 0.144420 11.00000 0.03044 0.01930 = 0.02752 0.00383 -0.00483 0.01587 AFIX 43 H5 2 0.153001 -0.050594 0.122420 11.00000 -1.20000 AFIX 0 C6 1 0.222878 -0.059123 0.116983 11.00000 0.03022 0.01981 = 0.03225 -0.00070 0.00203 -0.00289 AFIX 43 H6 2 0.222374 -0.035830 0.076324 11.00000 -1.20000 AFIX 0 C7 1 0.271586 -0.077839 0.145691 11.00000 0.02346 0.03122 = 0.04522 0.00202 0.00640 0.00352 AFIX 23 H7A 2 0.279823 -0.160914 0.142304 11.00000 -1.20000 H7B 2 0.295600 -0.033862 0.122511 11.00000 -1.20000 AFIX 0 C8 1 0.275834 -0.042810 0.210768 11.00000 0.01561 0.03440 = 0.04991 -0.00783 -0.00211 0.00184 AFIX 23 H8A 2 0.263021 -0.105525 0.236267 11.00000 -1.20000 H8B 2 0.309945 -0.032042 0.220965 11.00000 -1.20000 AFIX 0 P1 4 0.265823 0.287657 -0.026867 11.00000 0.01400 0.01944 = 0.01955 -0.00039 0.00080 0.00000 O1 3 0.259738 0.388746 -0.077119 11.00000 0.01215 0.02896 = 0.02038 0.00185 0.00211 -0.00005 C11 1 0.217559 0.443598 -0.090858 11.00000 0.01901 0.02799 = 0.01758 -0.00162 -0.00501 0.00381 C12 1 0.221655 0.540528 -0.124728 11.00000 0.02416 0.03516 = 0.01832 0.00412 0.00614 -0.00303 AFIX 43 H12 2 0.252221 0.568020 -0.136448 11.00000 -1.20000 AFIX 0 C13 1 0.179849 0.600033 -0.142334 11.00000 0.03966 0.03064 = 0.02114 0.00073 -0.00200 0.00957 AFIX 43 H13 2 0.182286 0.668176 -0.165870 11.00000 -1.20000 AFIX 0 C14 1 0.135507 0.559452 -0.125439 11.00000 0.02719 0.03994 = 0.02535 0.01320 0.00125 0.00154 AFIX 43 H14 2 0.107465 0.599264 -0.137608 11.00000 -1.20000 AFIX 0 C15 1 0.131986 0.462188 -0.091273 11.00000 0.01535 0.03720 = 0.03008 -0.00329 -0.00018 -0.00031 AFIX 43 H15 2 0.101495 0.434534 -0.079351 11.00000 -1.20000 AFIX 0 C16 1 0.172873 0.403694 -0.073947 11.00000 0.02080 0.03062 = 0.02742 0.00615 0.00196 0.00042 AFIX 43 H16 2 0.170277 0.335729 -0.050300 11.00000 -1.20000 AFIX 0 O2 3 0.322894 0.271452 -0.034449 11.00000 0.02363 0.03166 = 0.01730 -0.00225 0.00116 0.00269 C17 1 0.350990 0.274092 -0.086494 11.00000 0.00646 0.03218 = 0.01882 -0.00025 -0.00246 0.00732 C18 1 0.344650 0.195498 -0.130706 11.00000 0.01674 0.02628 = 0.02510 0.00137 0.00399 0.00008 AFIX 43 H18 2 0.319232 0.141156 -0.128858 11.00000 -1.20000 AFIX 0 C19 1 0.376484 0.195844 -0.179528 11.00000 0.02238 0.03101 = 0.02100 -0.00721 0.00184 0.01061 AFIX 43 H19 2 0.371927 0.143039 -0.211529 11.00000 -1.20000 AFIX 0 C20 1 0.413546 0.271280 -0.180914 11.00000 0.01959 0.03418 = 0.02670 0.00505 0.01532 0.00384 AFIX 43 H20 2 0.435122 0.271162 -0.213635 11.00000 -1.20000 AFIX 0 C21 1 0.419710 0.348349 -0.134383 11.00000 0.02462 0.03234 = 0.02802 -0.00009 0.00384 -0.00411 AFIX 43 H21 2 0.445975 0.400374 -0.135139 11.00000 -1.20000 AFIX 0 C22 1 0.388233 0.351128 -0.086575 11.00000 0.02778 0.02319 = 0.03341 -0.00879 0.01156 0.00000 AFIX 43 H22 2 0.392363 0.404782 -0.054860 11.00000 -1.20000 AFIX 0 O3 3 0.244524 0.183440 -0.069152 11.00000 0.01890 0.02251 = 0.02260 0.00160 0.00011 -0.00186 C23 1 0.248127 0.067936 -0.054927 11.00000 0.01659 0.03271 = 0.02293 -0.01050 0.00858 -0.00239 C24 1 0.216867 -0.006198 -0.080937 11.00000 0.02668 0.04490 = 0.03745 -0.00414 0.00232 -0.00156 AFIX 43 H24 2 0.192679 0.024005 -0.106262 11.00000 -1.20000 AFIX 0 C25 1 0.219119 -0.123406 -0.071787 11.00000 0.04258 0.02554 = 0.07807 -0.01373 0.00916 -0.00677 AFIX 43 H25 2 0.197064 -0.173451 -0.091076 11.00000 -1.20000 AFIX 0 C26 1 0.253374 -0.167899 -0.034655 11.00000 0.03479 0.02143 = 0.06926 0.00152 0.02552 0.00840 AFIX 43 H26 2 0.254587 -0.248764 -0.027109 11.00000 -1.20000 AFIX 0 C27 1 0.285848 -0.095357 -0.008470 11.00000 0.03587 0.02498 = 0.05345 0.00134 0.01510 0.01054 AFIX 43 H27 2 0.309963 -0.125945 0.016841 11.00000 -1.20000 AFIX 0 C28 1 0.283500 0.023786 -0.019000 11.00000 0.03896 0.02593 = 0.03129 -0.00665 0.01115 0.00112 AFIX 43 H28 2 0.306310 0.074133 -0.001359 11.00000 -1.20000 AFIX 0 P2 4 0.294465 0.426644 0.090484 11.00000 0.01374 0.02173 = 0.01751 -0.00143 0.00121 0.00190 O4 3 0.331276 0.469105 0.038607 11.00000 0.01378 0.02306 = 0.01840 0.00366 0.00198 -0.00501 C29 1 0.368573 0.546378 0.047401 11.00000 0.00672 0.02650 = 0.01775 -0.00018 0.00660 -0.00226 C30 1 0.411248 0.509974 0.072238 11.00000 0.01694 0.02544 = 0.02581 0.00025 0.00729 0.00014 AFIX 43 H30 2 0.415241 0.432164 0.085010 11.00000 -1.20000 AFIX 0 C31 1 0.448110 0.589537 0.078102 11.00000 0.01608 0.03368 = 0.03843 -0.00492 0.00323 -0.00004 AFIX 43 H31 2 0.477344 0.565987 0.095859 11.00000 -1.20000 AFIX 0 C32 1 0.443067 0.702267 0.058604 11.00000 0.02469 0.03147 = 0.02961 -0.00524 0.00464 -0.01006 AFIX 43 H32 2 0.468319 0.756368 0.063448 11.00000 -1.20000 AFIX 0 C33 1 0.401378 0.734543 0.032369 11.00000 0.03961 0.01940 = 0.03759 0.00952 0.00170 -0.00344 AFIX 43 H33 2 0.398269 0.811256 0.017601 11.00000 -1.20000 AFIX 0 C34 1 0.362763 0.657828 0.026448 11.00000 0.02003 0.02746 = 0.03103 0.00671 -0.00165 -0.00228 AFIX 43 H34 2 0.333622 0.681845 0.008619 11.00000 -1.20000 AFIX 0 O5 3 0.330773 0.389854 0.144268 11.00000 0.01589 0.03607 = 0.02599 0.00326 -0.00653 0.00262 C35 1 0.350598 0.281078 0.150647 11.00000 0.01206 0.02900 = 0.03361 0.02537 0.00150 0.00114 C36 1 0.363543 0.213759 0.101579 11.00000 0.01828 0.02838 = 0.03960 0.00806 -0.00799 0.00387 AFIX 43 H36 2 0.358236 0.242814 0.062472 11.00000 -1.20000 AFIX 0 C37 1 0.383856 0.106053 0.108613 11.00000 0.03147 0.03913 = 0.06774 -0.00620 0.00094 0.00417 AFIX 43 H37 2 0.391244 0.058806 0.075161 11.00000 -1.20000 AFIX 0 C38 1 0.393524 0.067556 0.168873 11.00000 0.01312 0.04199 = 0.08418 0.03690 0.00154 -0.00116 AFIX 43 H38 2 0.407815 -0.005831 0.175715 11.00000 -1.20000 AFIX 0 C39 1 0.382182 0.136105 0.214899 11.00000 0.02580 0.06896 = 0.05369 0.04502 0.00072 0.01459 AFIX 43 H39 2 0.389625 0.111294 0.254239 11.00000 -1.20000 AFIX 0 C40 1 0.359846 0.242507 0.206945 11.00000 0.01738 0.06149 = 0.02648 0.00153 0.00769 -0.00915 AFIX 43 H40 2 0.351094 0.287989 0.240533 11.00000 -1.20000 AFIX 0 O6 3 0.279678 0.550214 0.118514 11.00000 0.02176 0.02134 = 0.02391 -0.00172 -0.00325 0.00229 C41 1 0.289540 0.592162 0.176675 11.00000 0.02119 0.03038 = 0.02376 -0.01383 0.00466 0.00574 C42 1 0.332413 0.641596 0.187720 11.00000 0.02308 0.05767 = 0.03488 -0.02177 0.00359 -0.00741 AFIX 43 H42 2 0.356604 0.642767 0.157999 11.00000 -1.20000 AFIX 0 C43 1 0.340377 0.691003 0.243890 11.00000 0.02548 0.06247 = 0.03768 -0.02458 0.00068 -0.00600 AFIX 43 H43 2 0.370501 0.724616 0.252828 11.00000 -1.20000 AFIX 0 C44 1 0.305060 0.691107 0.285882 11.00000 0.04764 0.04042 = 0.02464 -0.01211 -0.00080 -0.00159 AFIX 43 H44 2 0.310285 0.724456 0.324085 11.00000 -1.20000 AFIX 0 C45 1 0.261447 0.641631 0.271702 11.00000 0.04043 0.05043 = 0.03981 -0.00375 0.02004 0.00090 AFIX 43 H45 2 0.236801 0.640669 0.300835 11.00000 -1.20000 AFIX 0 C46 1 0.253004 0.594148 0.216805 11.00000 0.02707 0.04292 = 0.03849 -0.01721 0.01853 -0.02082 AFIX 43 H46 2 0.222541 0.563434 0.206936 11.00000 -1.20000 AFIX 0 P3 4 0.069143 0.309405 0.057534 11.00000 0.01475 0.02420 = 0.01690 -0.00047 -0.00225 -0.00028 O7 3 0.047855 0.434837 0.044136 11.00000 0.01922 0.02122 = 0.01903 -0.00117 -0.00836 -0.00635 C47 1 0.013384 0.469665 0.002583 11.00000 0.01122 0.02919 = 0.01514 -0.00103 0.00276 0.00084 C48 1 -0.027191 0.405511 -0.009415 11.00000 0.01621 0.03424 = 0.03102 0.01117 -0.00917 -0.00511 AFIX 43 H48 2 -0.032505 0.332689 0.009125 11.00000 -1.20000 AFIX 0 C49 1 -0.059693 0.451179 -0.049329 11.00000 0.02801 0.04945 = 0.03694 0.00584 -0.01666 -0.00934 AFIX 43 H49 2 -0.087720 0.408265 -0.058335 11.00000 -1.20000 AFIX 0 C50 1 -0.052906 0.556461 -0.076451 11.00000 0.03253 0.02728 = 0.03020 -0.00465 -0.00899 0.01406 AFIX 43 H50 2 -0.076007 0.585304 -0.103709 11.00000 -1.20000 AFIX 0 C51 1 -0.012714 0.619899 -0.064114 11.00000 0.03108 0.03211 = 0.02822 0.00611 -0.00158 0.00763 AFIX 43 H51 2 -0.007728 0.693340 -0.082141 11.00000 -1.20000 AFIX 0 C52 1 0.020583 0.574069 -0.024550 11.00000 0.02724 0.02802 = 0.01638 -0.00550 -0.00060 -0.00270 AFIX 43 H52 2 0.048924 0.616289 -0.016233 11.00000 -1.20000 AFIX 0 O8 3 0.069082 0.265113 -0.011424 11.00000 0.02784 0.01531 = 0.01284 -0.00404 0.00298 -0.00245 C53 1 0.061603 0.156171 -0.038134 11.00000 0.01528 0.02582 = 0.01969 -0.00918 -0.00302 -0.00330 C54 1 0.091893 0.131689 -0.085029 11.00000 0.01631 0.05247 = 0.04709 -0.01410 0.00402 -0.00690 AFIX 43 H54 2 0.117631 0.181824 -0.094760 11.00000 -1.20000 AFIX 0 C55 1 0.083452 0.030354 -0.117878 11.00000 0.03389 0.05045 = 0.04763 -0.03343 0.01556 -0.00615 AFIX 43 H55 2 0.102975 0.012736 -0.151343 11.00000 -1.20000 AFIX 0 C56 1 0.047410 -0.043152 -0.102148 11.00000 0.04767 0.02421 = 0.03519 -0.01524 -0.00940 -0.00257 AFIX 43 H56 2 0.042990 -0.113442 -0.123448 11.00000 -1.20000 AFIX 0 C57 1 0.018216 -0.016452 -0.056712 11.00000 0.04195 0.03080 = 0.02994 0.00029 -0.00415 -0.00978 AFIX 43 H57 2 -0.007223 -0.067126 -0.046503 11.00000 -1.20000 AFIX 0 C58 1 0.025003 0.084567 -0.024665 11.00000 0.03309 0.03099 = 0.03210 -0.00403 0.01134 -0.00530 AFIX 43 H58 2 0.003831 0.103689 0.006963 11.00000 -1.20000 AFIX 0 O9 3 0.021213 0.243071 0.082037 11.00000 0.01443 0.02499 = 0.01954 0.00591 0.00041 -0.00365 C59 1 0.019693 0.167800 0.130092 11.00000 0.01232 0.02505 = 0.01550 -0.00545 -0.00859 -0.00658 C60 1 0.052699 0.079279 0.136942 11.00000 0.01756 0.02198 = 0.02750 -0.00279 -0.00227 -0.00540 AFIX 43 H60 2 0.078628 0.070781 0.109952 11.00000 -1.20000 AFIX 0 C61 1 0.046655 0.002848 0.184817 11.00000 0.02510 0.02153 = 0.04465 0.00487 -0.00554 -0.00036 AFIX 43 H61 2 0.069342 -0.057175 0.190805 11.00000 -1.20000 AFIX 0 C62 1 0.008324 0.012614 0.223753 11.00000 0.03492 0.02919 = 0.03196 0.01423 -0.00285 -0.01280 AFIX 43 H62 2 0.004302 -0.040617 0.255677 11.00000 -1.20000 AFIX 0 C63 1 -0.023639 0.101108 0.214993 11.00000 0.02045 0.04418 = 0.02999 0.00234 -0.00152 -0.00562 AFIX 43 H63 2 -0.050089 0.108072 0.241301 11.00000 -1.20000 AFIX 0 C64 1 -0.018663 0.180529 0.169161 11.00000 0.01069 0.04457 = 0.02946 0.01141 0.00286 -0.00005 AFIX 43 H64 2 -0.040823 0.242121 0.164463 11.00000 -1.20000 AFIX 0 P4 4 0.103966 0.438038 0.172254 11.00000 0.01247 0.02004 = 0.01824 -0.00203 0.00058 -0.00056 O10 3 0.114501 0.576372 0.168146 11.00000 0.02085 0.02145 = 0.01855 0.00188 0.00147 -0.00036 C65 1 0.117631 0.638250 0.113303 11.00000 0.02655 0.02206 = 0.02401 0.00058 0.00058 -0.00355 C66 1 0.086372 0.731113 0.107077 11.00000 0.01746 0.03004 = 0.04564 -0.01185 0.00579 -0.00091 AFIX 43 H66 2 0.063553 0.747983 0.137223 11.00000 -1.20000 AFIX 0 C67 1 0.089150 0.797404 0.056847 11.00000 0.02552 0.03158 = 0.03375 0.00421 -0.01228 -0.00337 AFIX 43 H67 2 0.068717 0.862485 0.052432 11.00000 -1.20000 AFIX 0 C68 1 0.121644 0.770502 0.012052 11.00000 0.03152 0.02621 = 0.03279 0.00669 -0.01026 -0.00355 AFIX 43 H68 2 0.122738 0.815053 -0.023560 11.00000 -1.20000 AFIX 0 C69 1 0.152898 0.676427 0.020134 11.00000 0.03226 0.03437 = 0.03187 -0.00245 -0.00014 -0.00561 AFIX 43 H69 2 0.175805 0.658503 -0.009746 11.00000 -1.20000 AFIX 0 C70 1 0.150440 0.610316 0.071079 11.00000 0.01987 0.02607 = 0.03434 -0.00160 0.00198 -0.00463 AFIX 43 H70 2 0.171292 0.546349 0.076621 11.00000 -1.20000 AFIX 0 O11 3 0.122129 0.438803 0.241503 11.00000 0.01391 0.02239 = 0.01351 -0.00121 -0.00049 -0.00282 C71 1 0.122243 0.343354 0.279345 11.00000 0.02389 0.02176 = 0.01982 -0.01085 -0.00264 -0.00258 C72 1 0.087842 0.258159 0.276313 11.00000 0.02915 0.02647 = 0.01299 0.00483 -0.00379 0.00761 AFIX 43 H72 2 0.064749 0.258629 0.245254 11.00000 -1.20000 AFIX 0 C73 1 0.087466 0.171696 0.319334 11.00000 0.03928 0.02790 = 0.02942 -0.00230 0.00736 -0.00314 AFIX 43 H73 2 0.063766 0.112927 0.317867 11.00000 -1.20000 AFIX 0 C74 1 0.121094 0.170360 0.364055 11.00000 0.04209 0.02684 = 0.02794 -0.00329 -0.00443 0.00821 AFIX 43 H74 2 0.120661 0.110916 0.393347 11.00000 -1.20000 AFIX 0 C75 1 0.155301 0.255412 0.366139 11.00000 0.04123 0.03455 = 0.02094 -0.00626 -0.01293 0.00782 AFIX 43 H75 2 0.178803 0.253841 0.396706 11.00000 -1.20000 AFIX 0 C76 1 0.155946 0.343809 0.324036 11.00000 0.02325 0.02346 = 0.02741 -0.01105 -0.00625 -0.00052 AFIX 43 H76 2 0.179240 0.403459 0.326087 11.00000 -1.20000 AFIX 0 O12 3 0.046365 0.436293 0.180254 11.00000 0.01685 0.02304 = 0.01986 -0.00496 -0.00151 -0.00279 C77 1 0.019715 0.517223 0.213107 11.00000 0.01412 0.02201 = 0.02074 -0.00688 -0.00253 -0.00564 C78 1 0.014767 0.505990 0.273527 11.00000 0.01999 0.02581 = 0.02776 0.00269 -0.00259 0.00712 AFIX 43 H78 2 0.030664 0.445049 0.293914 11.00000 -1.20000 AFIX 0 C79 1 -0.013668 0.584072 0.305407 11.00000 0.01667 0.04788 = 0.03267 -0.00270 0.00475 0.00433 AFIX 43 H79 2 -0.017598 0.575952 0.347314 11.00000 -1.20000 AFIX 0 C80 1 -0.035693 0.672101 0.275465 11.00000 0.01387 0.04088 = 0.03683 -0.01245 0.00743 0.00544 AFIX 43 H80 2 -0.054273 0.726708 0.297045 11.00000 -1.20000 AFIX 0 C81 1 -0.031346 0.683144 0.213668 11.00000 0.02234 0.03041 = 0.04590 -0.00032 -0.00268 0.00605 AFIX 43 H81 2 -0.047244 0.743931 0.193159 11.00000 -1.20000 AFIX 0 C82 1 -0.003220 0.603377 0.182262 11.00000 0.01180 0.02804 = 0.02672 -0.00108 0.00027 0.00345 AFIX 43 H82 2 -0.000083 0.608925 0.140140 11.00000 -1.20000 REM fjl150bs in Pna2(1) REM R1 = 0.0600 for 12725 Fo > 4sig(Fo) and 0.0787 for all 15385 data REM 911 parameters refined using 1 restraints HKLF 4 REM fjl150bs in Pna2(1) REM R1 = 0.0600 for 12725 Fo > 4sig(Fo) and 0.0787 for all 15385 data REM 911 parameters refined using 1 restraints END WGHT 0.0302 9.3579 REM Highest difference peak 0.768, deepest hole -1.092, 1-sigma level 0.117 Q1 1 0.1344 0.1944 0.1096 11.00000 0.05 0.77 Q2 1 0.2091 0.2539 0.1910 11.00000 0.05 0.73 Q3 1 0.1331 0.3799 0.1356 11.00000 0.05 0.67 Q4 1 0.1998 0.1719 0.1730 11.00000 0.05 0.63 Q5 1 0.1365 0.3660 0.0818 11.00000 0.05 0.62 Q6 1 0.1619 0.2255 0.1783 11.00000 0.05 0.58 Q7 1 0.1409 0.3145 0.0477 11.00000 0.05 0.57 Q8 1 0.2094 0.1789 0.1198 11.00000 0.05 0.56 Q9 1 0.2010 -0.0041 0.1521 11.00000 0.05 0.56 Q10 1 0.1422 0.4496 0.0639 11.00000 0.05 0.56 Q11 1 0.2386 0.2347 0.0401 11.00000 0.05 0.55 Q12 1 0.2010 0.0581 0.1186 11.00000 0.05 0.55 Q13 1 0.1279 0.4534 0.1510 11.00000 0.05 0.54 Q14 1 0.2470 0.3101 0.1219 11.00000 0.05 0.53 Q15 1 0.2831 0.1053 0.0283 11.00000 0.05 0.53 Q16 1 0.1698 0.3784 0.0515 11.00000 0.05 0.52 Q17 1 0.1310 0.2604 0.0798 11.00000 0.05 0.50 Q18 1 0.2402 0.4169 0.1220 11.00000 0.05 0.50 Q19 1 0.2695 0.3598 -0.0001 11.00000 0.05 0.50 Q20 1 0.1403 0.3998 0.0434 11.00000 0.05 0.49 ; 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 Pd Pd 0.201754(17) 0.11691(4) 0.14688(3) 0.01764(11) Uani 1 1 d . . . Rh2 Rh 0.239580(17) 0.30631(5) 0.06360(2) 0.01621(12) Uani 1 1 d . . . Rh3 Rh 0.133553(17) 0.31330(5) 0.11049(2) 0.01582(11) Uani 1 1 d . . . S1 S 0.17527(6) 0.17427(15) 0.05350(8) 0.0187(4) Uani 1 1 d . . . S2 S 0.20771(6) 0.31444(15) 0.16117(7) 0.0181(4) Uani 1 1 d . . . C1 C 0.2488(3) 0.0684(6) 0.2235(3) 0.0259(17) Uani 1 1 d . . . H1 H 0.2652 0.1391 0.2164 0.031 Uiso 1 1 calc R . . C2 C 0.2033(2) 0.0758(6) 0.2441(3) 0.0206(15) Uani 1 1 d . . . H2 H 0.1913 0.1509 0.2527 0.025 Uiso 1 1 calc R . . C3 C 0.1708(3) -0.0234(6) 0.2544(3) 0.0248(17) Uani 1 1 d . . . H3A H 0.1377 0.0064 0.2573 0.030 Uiso 1 1 calc R . . H3B H 0.1789 -0.0589 0.2933 0.030 Uiso 1 1 calc R . . C4 C 0.1721(2) -0.1193(7) 0.2058(3) 0.0258(17) Uani 1 1 d . . . H4A H 0.1977 -0.1752 0.2157 0.031 Uiso 1 1 calc R . . H4B H 0.1413 -0.1616 0.2063 0.031 Uiso 1 1 calc R . . C5 C 0.1805(2) -0.0728(6) 0.1444(4) 0.0258(16) Uani 1 1 d . . . H5 H 0.1530 -0.0506 0.1224 0.031 Uiso 1 1 calc R . . C6 C 0.2229(2) -0.0591(6) 0.1170(4) 0.0274(17) Uani 1 1 d . . . H6 H 0.2224 -0.0358 0.0763 0.033 Uiso 1 1 calc R . . C7 C 0.2716(2) -0.0778(7) 0.1457(4) 0.0333(19) Uani 1 1 d . . . H7A H 0.2798 -0.1609 0.1423 0.040 Uiso 1 1 calc R . . H7B H 0.2956 -0.0339 0.1225 0.040 Uiso 1 1 calc R . . C8 C 0.2758(3) -0.0428(7) 0.2108(4) 0.033(2) Uani 1 1 d . . . H8A H 0.2630 -0.1055 0.2363 0.040 Uiso 1 1 calc R . . H8B H 0.3099 -0.0320 0.2210 0.040 Uiso 1 1 calc R . . P1 P 0.26582(6) 0.28766(16) -0.02687(8) 0.0177(4) Uani 1 1 d . . . O1 O 0.25974(15) 0.3887(4) -0.0771(2) 0.0205(11) Uani 1 1 d . . . C11 C 0.2176(2) 0.4436(6) -0.0909(3) 0.0215(16) Uani 1 1 d . . . C12 C 0.2217(3) 0.5405(7) -0.1247(3) 0.0259(17) Uani 1 1 d . . . H12 H 0.2522 0.5680 -0.1364 0.031 Uiso 1 1 calc R . . C13 C 0.1798(3) 0.6000(7) -0.1423(3) 0.0305(19) Uani 1 1 d . . . H13 H 0.1823 0.6682 -0.1659 0.037 Uiso 1 1 calc R . . C14 C 0.1355(3) 0.5595(7) -0.1254(3) 0.0308(19) Uani 1 1 d . . . H14 H 0.1075 0.5993 -0.1376 0.037 Uiso 1 1 calc R . . C15 C 0.1320(3) 0.4622(7) -0.0913(3) 0.0275(18) Uani 1 1 d . . . H15 H 0.1015 0.4345 -0.0794 0.033 Uiso 1 1 calc R . . C16 C 0.1729(2) 0.4037(7) -0.0739(3) 0.0263(18) Uani 1 1 d . . . H16 H 0.1703 0.3357 -0.0503 0.032 Uiso 1 1 calc R . . O2 O 0.32289(17) 0.2715(4) -0.0344(2) 0.0242(12) Uani 1 1 d . . . C17 C 0.3510(2) 0.2741(6) -0.0865(3) 0.0192(16) Uani 1 1 d . . . C18 C 0.3447(2) 0.1955(7) -0.1307(3) 0.0227(16) Uani 1 1 d . . . H18 H 0.3192 0.1412 -0.1289 0.027 Uiso 1 1 calc R . . C19 C 0.3765(2) 0.1958(7) -0.1795(3) 0.0248(17) Uani 1 1 d . . . H19 H 0.3719 0.1430 -0.2115 0.030 Uiso 1 1 calc R . . C20 C 0.4135(2) 0.2713(7) -0.1809(3) 0.0268(18) Uani 1 1 d . . . H20 H 0.4351 0.2712 -0.2136 0.032 Uiso 1 1 calc R . . C21 C 0.4197(3) 0.3483(7) -0.1344(3) 0.0283(18) Uani 1 1 d . . . H21 H 0.4460 0.4004 -0.1351 0.034 Uiso 1 1 calc R . . C22 C 0.3882(3) 0.3511(6) -0.0866(4) 0.0281(18) Uani 1 1 d . . . H22 H 0.3924 0.4048 -0.0549 0.034 Uiso 1 1 calc R . . O3 O 0.24452(16) 0.1834(4) -0.0692(2) 0.0213(11) Uani 1 1 d . . . C23 C 0.2481(2) 0.0679(7) -0.0549(3) 0.0241(17) Uani 1 1 d . . . C24 C 0.2169(3) -0.0062(8) -0.0809(4) 0.036(2) Uani 1 1 d . . . H24 H 0.1927 0.0240 -0.1063 0.044 Uiso 1 1 calc R . . C25 C 0.2191(3) -0.1234(8) -0.0718(5) 0.049(3) Uani 1 1 d . . . H25 H 0.1971 -0.1735 -0.0911 0.058 Uiso 1 1 calc R . . C26 C 0.2534(3) -0.1679(7) -0.0347(4) 0.042(2) Uani 1 1 d . . . H26 H 0.2546 -0.2488 -0.0271 0.050 Uiso 1 1 calc R . . C27 C 0.2858(3) -0.0954(7) -0.0085(4) 0.038(2) Uani 1 1 d . . . H27 H 0.3100 -0.1259 0.0168 0.046 Uiso 1 1 calc R . . C28 C 0.2835(3) 0.0238(7) -0.0190(4) 0.0321(19) Uani 1 1 d . . . H28 H 0.3063 0.0741 -0.0014 0.038 Uiso 1 1 calc R . . P2 P 0.29447(6) 0.42664(16) 0.09048(8) 0.0177(4) Uani 1 1 d . . . O4 O 0.33128(15) 0.4691(4) 0.0386(2) 0.0184(11) Uani 1 1 d . . . C29 C 0.3686(2) 0.5464(6) 0.0474(3) 0.0170(15) Uani 1 1 d . . . C30 C 0.4112(2) 0.5100(6) 0.0722(3) 0.0227(16) Uani 1 1 d . . . H30 H 0.4152 0.4322 0.0850 0.027 Uiso 1 1 calc R . . C31 C 0.4481(2) 0.5895(6) 0.0781(4) 0.0294(19) Uani 1 1 d . . . H31 H 0.4773 0.5660 0.0959 0.035 Uiso 1 1 calc R . . C32 C 0.4431(2) 0.7023(7) 0.0586(4) 0.0286(17) Uani 1 1 d . . . H32 H 0.4683 0.7564 0.0634 0.034 Uiso 1 1 calc R . . C33 C 0.4014(3) 0.7345(7) 0.0324(4) 0.0322(19) Uani 1 1 d . . . H33 H 0.3983 0.8113 0.0176 0.039 Uiso 1 1 calc R . . C34 C 0.3628(3) 0.6578(6) 0.0264(3) 0.0262(17) Uani 1 1 d . . . H34 H 0.3336 0.6818 0.0086 0.031 Uiso 1 1 calc R . . O5 O 0.33077(15) 0.3899(4) 0.1443(3) 0.0260(11) Uani 1 1 d . . . C35 C 0.3506(2) 0.2811(6) 0.1506(4) 0.0249(17) Uani 1 1 d . . . C36 C 0.3635(2) 0.2138(6) 0.1016(4) 0.0288(18) Uani 1 1 d . . . H36 H 0.3582 0.2428 0.0625 0.035 Uiso 1 1 calc R . . C37 C 0.3839(3) 0.1061(7) 0.1086(5) 0.046(2) Uani 1 1 d . . . H37 H 0.3912 0.0588 0.0752 0.055 Uiso 1 1 calc R . . C38 C 0.3935(3) 0.0676(8) 0.1689(5) 0.046(3) Uani 1 1 d . . . H38 H 0.4078 -0.0058 0.1757 0.056 Uiso 1 1 calc R . . C39 C 0.3822(3) 0.1361(9) 0.2149(5) 0.049(3) Uani 1 1 d . . . H39 H 0.3896 0.1113 0.2542 0.059 Uiso 1 1 calc R . . C40 C 0.3598(3) 0.2425(8) 0.2069(4) 0.035(2) Uani 1 1 d . . . H40 H 0.3511 0.2880 0.2405 0.042 Uiso 1 1 calc R . . O6 O 0.27968(16) 0.5502(4) 0.1185(2) 0.0223(11) Uani 1 1 d . . . C41 C 0.2895(2) 0.5922(6) 0.1767(3) 0.0251(17) Uani 1 1 d . . . C42 C 0.3324(3) 0.6416(8) 0.1877(4) 0.039(2) Uani 1 1 d . . . H42 H 0.3566 0.6428 0.1580 0.046 Uiso 1 1 calc R . . C43 C 0.3404(3) 0.6910(8) 0.2439(4) 0.042(2) Uani 1 1 d . . . H43 H 0.3705 0.7246 0.2528 0.050 Uiso 1 1 calc R . . C44 C 0.3051(3) 0.6911(8) 0.2859(4) 0.038(2) Uani 1 1 d . . . H44 H 0.3103 0.7245 0.3241 0.045 Uiso 1 1 calc R . . C45 C 0.2614(3) 0.6416(8) 0.2717(4) 0.044(2) Uani 1 1 d . . . H45 H 0.2368 0.6407 0.3008 0.052 Uiso 1 1 calc R . . C46 C 0.2530(3) 0.5941(7) 0.2168(4) 0.036(2) Uani 1 1 d . . . H46 H 0.2225 0.5634 0.2069 0.043 Uiso 1 1 calc R . . P3 P 0.06914(6) 0.30940(16) 0.05753(8) 0.0186(4) Uani 1 1 d . . . O7 O 0.04785(16) 0.4348(4) 0.0441(2) 0.0198(11) Uani 1 1 d . . . C47 C 0.0134(2) 0.4697(7) 0.0026(3) 0.0185(16) Uani 1 1 d . . . C48 C -0.0272(2) 0.4055(7) -0.0094(3) 0.0272(18) Uani 1 1 d . . . H48 H -0.0325 0.3327 0.0091 0.033 Uiso 1 1 calc R . . C49 C -0.0597(3) 0.4512(8) -0.0493(4) 0.038(2) Uani 1 1 d . . . H49 H -0.0877 0.4083 -0.0583 0.046 Uiso 1 1 calc R . . C50 C -0.0529(3) 0.5565(7) -0.0765(4) 0.0300(19) Uani 1 1 d . . . H50 H -0.0760 0.5853 -0.1037 0.036 Uiso 1 1 calc R . . C51 C -0.0127(3) 0.6199(7) -0.0641(3) 0.0305(19) Uani 1 1 d . . . H51 H -0.0077 0.6933 -0.0821 0.037 Uiso 1 1 calc R . . C52 C 0.0206(3) 0.5741(7) -0.0246(3) 0.0239(17) Uani 1 1 d . . . H52 H 0.0489 0.6163 -0.0162 0.029 Uiso 1 1 calc R . . O8 O 0.06908(17) 0.2651(4) -0.0114(2) 0.0187(10) Uani 1 1 d . . . C53 C 0.0616(2) 0.1562(6) -0.0381(3) 0.0203(16) Uani 1 1 d . . . C54 C 0.0919(3) 0.1317(8) -0.0850(4) 0.039(2) Uani 1 1 d . . . H54 H 0.1176 0.1818 -0.0948 0.046 Uiso 1 1 calc R . . C55 C 0.0835(3) 0.0304(8) -0.1179(4) 0.044(2) Uani 1 1 d . . . H55 H 0.1030 0.0127 -0.1513 0.053 Uiso 1 1 calc R . . C56 C 0.0474(3) -0.0432(7) -0.1021(4) 0.036(2) Uani 1 1 d . . . H56 H 0.0430 -0.1134 -0.1234 0.043 Uiso 1 1 calc R . . C57 C 0.0182(3) -0.0165(7) -0.0567(4) 0.034(2) Uani 1 1 d . . . H57 H -0.0072 -0.0671 -0.0465 0.041 Uiso 1 1 calc R . . C58 C 0.0250(3) 0.0846(7) -0.0247(4) 0.0321(19) Uani 1 1 d . . . H58 H 0.0038 0.1037 0.0070 0.038 Uiso 1 1 calc R . . O9 O 0.02121(15) 0.2431(4) 0.0820(2) 0.0197(11) Uani 1 1 d . . . C59 C 0.0197(2) 0.1678(6) 0.1301(3) 0.0176(16) Uani 1 1 d . . . C60 C 0.0527(2) 0.0793(6) 0.1369(3) 0.0223(17) Uani 1 1 d . . . H60 H 0.0786 0.0708 0.1100 0.027 Uiso 1 1 calc R . . C61 C 0.0467(3) 0.0028(7) 0.1848(4) 0.0304(19) Uani 1 1 d . . . H61 H 0.0693 -0.0572 0.1908 0.037 Uiso 1 1 calc R . . C62 C 0.0083(3) 0.0126(7) 0.2238(4) 0.032(2) Uani 1 1 d . . . H62 H 0.0043 -0.0406 0.2557 0.038 Uiso 1 1 calc R . . C63 C -0.0236(3) 0.1011(7) 0.2150(4) 0.032(2) Uani 1 1 d . . . H63 H -0.0501 0.1081 0.2413 0.038 Uiso 1 1 calc R . . C64 C -0.0187(2) 0.1805(7) 0.1692(3) 0.0282(18) Uani 1 1 d . . . H64 H -0.0408 0.2421 0.1645 0.034 Uiso 1 1 calc R . . P4 P 0.10397(6) 0.43804(16) 0.17225(8) 0.0169(4) Uani 1 1 d . . . O10 O 0.11450(16) 0.5764(4) 0.1681(2) 0.0203(11) Uani 1 1 d . . . C65 C 0.1176(2) 0.6383(6) 0.1133(4) 0.0242(16) Uani 1 1 d . . . C66 C 0.0864(2) 0.7311(6) 0.1071(4) 0.0310(18) Uani 1 1 d . . . H66 H 0.0636 0.7480 0.1372 0.037 Uiso 1 1 calc R . . C67 C 0.0891(2) 0.7974(7) 0.0568(4) 0.0303(18) Uani 1 1 d . . . H67 H 0.0687 0.8625 0.0524 0.036 Uiso 1 1 calc R . . C68 C 0.1216(3) 0.7705(7) 0.0121(4) 0.0302(19) Uani 1 1 d . . . H68 H 0.1227 0.8151 -0.0236 0.036 Uiso 1 1 calc R . . C69 C 0.1529(3) 0.6764(7) 0.0201(4) 0.0328(19) Uani 1 1 d . . . H69 H 0.1758 0.6585 -0.0097 0.039 Uiso 1 1 calc R . . C70 C 0.1504(2) 0.6103(6) 0.0711(3) 0.0268(17) Uani 1 1 d . . . H70 H 0.1713 0.5463 0.0766 0.032 Uiso 1 1 calc R . . O11 O 0.12213(15) 0.4388(4) 0.2415(2) 0.0166(10) Uani 1 1 d . . . C71 C 0.1222(2) 0.3434(6) 0.2793(3) 0.0218(16) Uani 1 1 d . . . C72 C 0.0878(3) 0.2582(6) 0.2763(3) 0.0229(16) Uani 1 1 d . . . H72 H 0.0647 0.2586 0.2453 0.027 Uiso 1 1 calc R . . C73 C 0.0875(3) 0.1717(7) 0.3193(4) 0.032(2) Uani 1 1 d . . . H73 H 0.0638 0.1129 0.3179 0.039 Uiso 1 1 calc R . . C74 C 0.1211(3) 0.1704(7) 0.3641(4) 0.0323(19) Uani 1 1 d . . . H74 H 0.1207 0.1109 0.3933 0.039 Uiso 1 1 calc R . . C75 C 0.1553(3) 0.2554(7) 0.3661(3) 0.0322(19) Uani 1 1 d . . . H75 H 0.1788 0.2538 0.3967 0.039 Uiso 1 1 calc R . . C76 C 0.1559(3) 0.3438(6) 0.3240(3) 0.0247(17) Uani 1 1 d . . . H76 H 0.1792 0.4035 0.3261 0.030 Uiso 1 1 calc R . . O12 O 0.04636(15) 0.4363(4) 0.1803(2) 0.0199(11) Uani 1 1 d . . . C77 C 0.0197(2) 0.5172(6) 0.2131(3) 0.0190(16) Uani 1 1 d . . . C78 C 0.0148(2) 0.5060(7) 0.2735(3) 0.0245(17) Uani 1 1 d . . . H78 H 0.0307 0.4450 0.2939 0.029 Uiso 1 1 calc R . . C79 C -0.0137(3) 0.5841(7) 0.3054(4) 0.032(2) Uani 1 1 d . . . H79 H -0.0176 0.5760 0.3473 0.039 Uiso 1 1 calc R . . C80 C -0.0357(2) 0.6721(7) 0.2755(4) 0.0305(19) Uani 1 1 d . . . H80 H -0.0543 0.7267 0.2970 0.037 Uiso 1 1 calc R . . C81 C -0.0313(3) 0.6831(7) 0.2137(4) 0.0329(19) Uani 1 1 d . . . H81 H -0.0472 0.7439 0.1932 0.039 Uiso 1 1 calc R . . C82 C -0.0032(2) 0.6034(6) 0.1823(3) 0.0222(17) Uani 1 1 d . . . H82 H -0.0001 0.6089 0.1401 0.027 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 Pd 0.0144(2) 0.0196(3) 0.0189(3) 0.0004(3) -0.0003(2) -0.0001(2) Rh2 0.0121(2) 0.0199(3) 0.0166(3) -0.0015(3) 0.0004(2) -0.0002(2) Rh3 0.0121(2) 0.0193(3) 0.0161(3) -0.0016(3) -0.0001(2) -0.0008(2) S1 0.0158(8) 0.0212(9) 0.0190(10) -0.0029(8) 0.0008(7) 0.0002(7) S2 0.0153(8) 0.0194(9) 0.0196(10) -0.0040(7) 0.0000(6) -0.0023(7) C1 0.029(4) 0.022(4) 0.027(4) 0.009(3) -0.003(3) -0.004(3) C2 0.023(4) 0.019(4) 0.020(4) 0.005(3) -0.006(3) 0.002(3) C3 0.031(4) 0.023(4) 0.020(4) 0.002(3) -0.001(3) 0.000(3) C4 0.019(4) 0.032(5) 0.026(4) 0.008(4) 0.004(3) 0.002(3) C5 0.030(4) 0.019(4) 0.028(4) 0.004(4) -0.005(4) 0.016(3) C6 0.030(4) 0.020(4) 0.032(5) -0.001(4) 0.002(3) -0.003(3) C7 0.023(4) 0.031(5) 0.045(5) 0.002(5) 0.006(4) 0.004(3) C8 0.016(4) 0.034(5) 0.050(6) -0.008(4) -0.002(3) 0.002(3) P1 0.0140(9) 0.0194(10) 0.0195(10) -0.0004(8) 0.0008(7) 0.0000(7) O1 0.012(2) 0.029(3) 0.020(3) 0.002(2) 0.0021(19) 0.000(2) C11 0.019(4) 0.028(4) 0.018(4) -0.002(3) -0.005(3) 0.004(3) C12 0.024(4) 0.035(5) 0.018(4) 0.004(3) 0.006(3) -0.003(3) C13 0.040(5) 0.031(5) 0.021(4) 0.001(4) -0.002(3) 0.010(4) C14 0.027(4) 0.040(5) 0.025(4) 0.013(4) 0.001(3) 0.002(4) C15 0.015(4) 0.037(5) 0.030(5) -0.003(4) 0.000(3) 0.000(3) C16 0.021(4) 0.031(5) 0.027(4) 0.006(4) 0.002(3) 0.000(3) O2 0.024(3) 0.032(3) 0.017(3) -0.002(2) 0.001(2) 0.003(2) C17 0.006(3) 0.032(4) 0.019(4) 0.000(3) -0.002(3) 0.007(3) C18 0.017(3) 0.026(4) 0.025(4) 0.001(4) 0.004(3) 0.000(3) C19 0.022(4) 0.031(4) 0.021(4) -0.007(4) 0.002(3) 0.011(3) C20 0.020(4) 0.034(5) 0.027(4) 0.005(4) 0.015(3) 0.004(3) C21 0.025(4) 0.032(5) 0.028(4) 0.000(4) 0.004(3) -0.004(3) C22 0.028(4) 0.023(4) 0.033(5) -0.009(4) 0.012(3) 0.000(3) O3 0.019(2) 0.023(3) 0.023(3) 0.002(2) 0.000(2) -0.002(2) C23 0.017(4) 0.033(5) 0.023(4) -0.011(3) 0.009(3) -0.002(3) C24 0.027(4) 0.045(6) 0.037(5) -0.004(4) 0.002(4) -0.002(4) C25 0.043(5) 0.026(5) 0.078(8) -0.014(5) 0.009(5) -0.007(4) C26 0.035(5) 0.021(5) 0.069(7) 0.002(4) 0.026(5) 0.008(4) C27 0.036(5) 0.025(5) 0.053(6) 0.001(4) 0.015(4) 0.011(4) C28 0.039(5) 0.026(5) 0.031(5) -0.007(4) 0.011(4) 0.001(4) P2 0.0137(8) 0.0217(10) 0.0175(9) -0.0014(8) 0.0012(7) 0.0019(7) O4 0.014(2) 0.023(3) 0.018(3) 0.004(2) 0.0020(19) -0.005(2) C29 0.007(3) 0.026(4) 0.018(4) 0.000(3) 0.007(2) -0.002(3) C30 0.017(3) 0.025(4) 0.026(5) 0.000(3) 0.007(3) 0.000(3) C31 0.016(4) 0.034(5) 0.038(5) -0.005(4) 0.003(3) 0.000(3) C32 0.025(4) 0.031(4) 0.030(4) -0.005(4) 0.005(4) -0.010(3) C33 0.040(5) 0.019(4) 0.038(5) 0.010(4) 0.002(4) -0.003(3) C34 0.020(4) 0.027(4) 0.031(4) 0.007(3) -0.002(3) -0.002(3) O5 0.016(2) 0.036(3) 0.026(3) 0.003(3) -0.007(2) 0.003(2) C35 0.012(3) 0.029(4) 0.034(4) 0.025(4) 0.001(3) 0.001(3) C36 0.018(3) 0.028(4) 0.040(5) 0.008(4) -0.008(3) 0.004(3) C37 0.031(5) 0.039(5) 0.068(7) -0.006(6) 0.001(5) 0.004(4) C38 0.013(4) 0.042(6) 0.084(8) 0.037(6) 0.002(4) -0.001(4) C39 0.026(5) 0.069(7) 0.054(7) 0.045(6) 0.001(4) 0.015(5) C40 0.017(4) 0.061(6) 0.026(5) 0.002(4) 0.008(3) -0.009(4) O6 0.022(2) 0.021(3) 0.024(3) -0.002(2) -0.003(2) 0.002(2) C41 0.021(4) 0.030(5) 0.024(4) -0.014(3) 0.005(3) 0.006(3) C42 0.023(4) 0.058(6) 0.035(5) -0.022(4) 0.004(3) -0.007(4) C43 0.025(4) 0.062(6) 0.038(5) -0.025(5) 0.001(4) -0.006(4) C44 0.048(5) 0.040(5) 0.025(4) -0.012(4) -0.001(4) -0.002(4) C45 0.040(5) 0.050(6) 0.040(6) -0.004(5) 0.020(4) 0.001(4) C46 0.027(4) 0.043(5) 0.038(5) -0.017(4) 0.019(4) -0.021(4) P3 0.0148(8) 0.0242(10) 0.0169(9) -0.0005(9) -0.0023(7) -0.0003(7) O7 0.019(2) 0.021(3) 0.019(3) -0.001(2) -0.0084(19) -0.006(2) C47 0.011(3) 0.029(4) 0.015(4) -0.001(3) 0.003(3) 0.001(3) C48 0.016(4) 0.034(5) 0.031(5) 0.011(4) -0.009(3) -0.005(3) C49 0.028(4) 0.049(6) 0.037(5) 0.006(4) -0.017(4) -0.009(4) C50 0.033(4) 0.027(5) 0.030(5) -0.005(4) -0.009(3) 0.014(4) C51 0.031(4) 0.032(5) 0.028(5) 0.006(4) -0.002(3) 0.008(4) C52 0.027(4) 0.028(4) 0.016(4) -0.006(3) -0.001(3) -0.003(3) O8 0.028(3) 0.015(3) 0.013(3) -0.004(2) 0.003(2) -0.002(2) C53 0.015(3) 0.026(4) 0.020(4) -0.009(3) -0.003(3) -0.003(3) C54 0.016(4) 0.052(6) 0.047(6) -0.014(5) 0.004(4) -0.007(4) C55 0.034(5) 0.050(6) 0.048(6) -0.033(5) 0.016(4) -0.006(4) C56 0.048(5) 0.024(5) 0.035(5) -0.015(4) -0.009(4) -0.003(4) C57 0.042(5) 0.031(5) 0.030(5) 0.000(4) -0.004(4) -0.010(4) C58 0.033(4) 0.031(5) 0.032(5) -0.004(4) 0.011(4) -0.005(4) O9 0.014(2) 0.025(3) 0.020(3) 0.006(2) 0.0004(19) -0.004(2) C59 0.012(3) 0.025(4) 0.016(4) -0.005(3) -0.009(2) -0.007(3) C60 0.018(3) 0.022(4) 0.028(4) -0.003(3) -0.002(3) -0.005(3) C61 0.025(4) 0.022(4) 0.045(5) 0.005(4) -0.006(4) 0.000(3) C62 0.035(5) 0.029(5) 0.032(5) 0.014(4) -0.003(4) -0.013(4) C63 0.020(4) 0.044(5) 0.030(5) 0.002(4) -0.002(3) -0.006(4) C64 0.011(3) 0.045(5) 0.029(4) 0.011(4) 0.003(3) 0.000(3) P4 0.0125(8) 0.0200(10) 0.0182(10) -0.0020(8) 0.0006(7) -0.0006(7) O10 0.021(2) 0.021(3) 0.019(3) 0.002(2) 0.0015(19) 0.000(2) C65 0.027(4) 0.022(4) 0.024(4) 0.001(4) 0.001(3) -0.004(3) C66 0.017(3) 0.030(4) 0.046(5) -0.012(4) 0.006(4) -0.001(3) C67 0.026(4) 0.032(4) 0.034(5) 0.004(4) -0.012(4) -0.003(3) C68 0.032(4) 0.026(5) 0.033(5) 0.007(4) -0.010(3) -0.004(3) C69 0.032(4) 0.034(5) 0.032(5) -0.002(4) 0.000(4) -0.006(4) C70 0.020(4) 0.026(4) 0.034(5) -0.002(4) 0.002(3) -0.005(3) O11 0.014(2) 0.022(3) 0.014(3) -0.001(2) -0.0005(18) -0.0028(19) C71 0.024(4) 0.022(4) 0.020(4) -0.011(3) -0.003(3) -0.003(3) C72 0.029(4) 0.026(4) 0.013(4) 0.005(3) -0.004(3) 0.008(3) C73 0.039(5) 0.028(5) 0.029(5) -0.002(4) 0.007(4) -0.003(4) C74 0.042(5) 0.027(5) 0.028(5) -0.003(4) -0.004(4) 0.008(4) C75 0.041(5) 0.035(5) 0.021(4) -0.006(4) -0.013(4) 0.008(4) C76 0.023(4) 0.023(4) 0.027(4) -0.011(3) -0.006(3) -0.001(3) O12 0.017(2) 0.023(3) 0.020(3) -0.005(2) -0.002(2) -0.003(2) C77 0.014(3) 0.022(4) 0.021(4) -0.007(3) -0.003(3) -0.006(3) C78 0.020(4) 0.026(4) 0.028(4) 0.003(3) -0.003(3) 0.007(3) C79 0.017(4) 0.048(6) 0.033(5) -0.003(4) 0.005(3) 0.004(4) C80 0.014(3) 0.041(5) 0.037(5) -0.012(4) 0.007(3) 0.005(3) C81 0.022(4) 0.030(5) 0.046(5) 0.000(4) -0.003(3) 0.006(3) C82 0.012(3) 0.028(4) 0.027(4) -0.001(3) 0.000(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C6 2.221(7) . ? Pd C2 2.230(7) . ? Pd C1 2.236(7) . ? Pd C5 2.272(7) . ? Pd S2 2.3104(19) . ? Pd S1 2.317(2) . ? Pd Rh2 3.0645(10) . ? Pd Rh3 3.0757(9) . ? Rh2 P2 2.1582(19) . ? Rh2 P1 2.167(2) . ? Rh2 S2 2.3631(18) . ? Rh2 S1 2.3708(18) . ? Rh2 Rh3 3.1505(11) . ? Rh3 P3 2.1594(18) . ? Rh3 P4 2.1629(19) . ? Rh3 S1 2.3611(18) . ? Rh3 S2 2.3669(17) . ? C1 C2 1.360(10) . ? C1 C8 1.518(10) . ? C1 H1 0.9500 . ? C2 C3 1.480(10) . ? C2 H2 0.9500 . ? C3 C4 1.553(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.495(10) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.346(10) . ? C5 H5 0.9500 . ? C6 C7 1.523(10) . ? C6 H6 0.9500 . ? C7 C8 1.518(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? P1 O2 1.618(5) . ? P1 O1 1.631(5) . ? P1 O3 1.644(5) . ? O1 C11 1.375(8) . ? C11 C12 1.358(10) . ? C11 C16 1.386(10) . ? C12 C13 1.414(10) . ? C12 H12 0.9500 . ? C13 C14 1.380(11) . ? C13 H13 0.9500 . ? C14 C15 1.363(10) . ? C14 H14 0.9500 . ? C15 C16 1.385(10) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? O2 C17 1.407(8) . ? C17 C18 1.355(10) . ? C17 C22 1.371(10) . ? C18 C19 1.411(9) . ? C18 H18 0.9500 . ? C19 C20 1.356(10) . ? C19 H19 0.9500 . ? C20 C21 1.382(10) . ? C20 H20 0.9500 . ? C21 C22 1.388(10) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? O3 C23 1.376(9) . ? C23 C24 1.356(10) . ? C23 C28 1.375(11) . ? C24 C25 1.371(12) . ? C24 H24 0.9500 . ? C25 C26 1.370(13) . ? C25 H25 0.9500 . ? C26 C27 1.369(12) . ? C26 H26 0.9500 . ? C27 C28 1.398(11) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? P2 O6 1.614(5) . ? P2 O4 1.629(5) . ? P2 O5 1.633(5) . ? O4 C29 1.388(7) . ? C29 C34 1.380(10) . ? C29 C30 1.384(9) . ? C30 C31 1.388(9) . ? C30 H30 0.9500 . ? C31 C32 1.381(10) . ? C31 H31 0.9500 . ? C32 C33 1.359(10) . ? C32 H32 0.9500 . ? C33 C34 1.404(10) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? O5 C35 1.381(8) . ? C35 C40 1.363(11) . ? C35 C36 1.395(11) . ? C36 C37 1.377(10) . ? C36 H36 0.9500 . ? C37 C38 1.447(13) . ? C37 H37 0.9500 . ? C38 C39 1.338(13) . ? C38 H38 0.9500 . ? C39 C40 1.391(12) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? O6 C41 1.417(8) . ? C41 C42 1.352(10) . ? C41 C46 1.362(9) . ? C42 C43 1.400(11) . ? C42 H42 0.9500 . ? C43 C44 1.365(11) . ? C43 H43 0.9500 . ? C44 C45 1.385(12) . ? C44 H44 0.9500 . ? C45 C46 1.367(12) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? P3 O7 1.595(5) . ? P3 O8 1.628(5) . ? P3 O9 1.640(5) . ? O7 C47 1.400(8) . ? C47 C52 1.366(10) . ? C47 C48 1.383(9) . ? C48 C49 1.381(10) . ? C48 H48 0.9500 . ? C49 C50 1.373(11) . ? C49 H49 0.9500 . ? C50 C51 1.371(11) . ? C50 H50 0.9500 . ? C51 C52 1.391(10) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? O8 C53 1.409(8) . ? C53 C58 1.351(10) . ? C53 C54 1.380(10) . ? C54 C55 1.403(11) . ? C54 H54 0.9500 . ? C55 C56 1.365(11) . ? C55 H55 0.9500 . ? C56 C57 1.342(11) . ? C56 H56 0.9500 . ? C57 C58 1.383(11) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? O9 C59 1.385(7) . ? C59 C60 1.387(9) . ? C59 C64 1.393(9) . ? C60 C61 1.400(10) . ? C60 H60 0.9500 . ? C61 C62 1.388(11) . ? C61 H61 0.9500 . ? C62 C63 1.373(11) . ? C62 H62 0.9500 . ? C63 C64 1.384(10) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? P4 O12 1.623(5) . ? P4 O10 1.628(5) . ? P4 O11 1.633(5) . ? O10 C65 1.424(8) . ? C65 C70 1.358(10) . ? C65 C66 1.392(9) . ? C66 C67 1.364(11) . ? C66 H66 0.9500 . ? C67 C68 1.390(11) . ? C67 H67 0.9500 . ? C68 C69 1.407(11) . ? C68 H68 0.9500 . ? C69 C70 1.375(11) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? O11 C71 1.391(8) . ? C71 C76 1.376(9) . ? C71 C72 1.379(10) . ? C72 C73 1.388(10) . ? C72 H72 0.9500 . ? C73 C74 1.375(11) . ? C73 H73 0.9500 . ? C74 C75 1.373(11) . ? C74 H74 0.9500 . ? C75 C76 1.390(11) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? O12 C77 1.405(8) . ? C77 C78 1.367(10) . ? C77 C82 1.371(9) . ? C78 C79 1.399(10) . ? C78 H78 0.9500 . ? C79 C80 1.366(11) . ? C79 H79 0.9500 . ? C80 C81 1.396(11) . ? C80 H80 0.9500 . ? C81 C82 1.402(10) . ? C81 H81 0.9500 . ? C82 H82 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 C6 Pd C2 95.4(3) . . ? C6 Pd C1 81.1(3) . . ? C2 Pd C1 35.5(2) . . ? C6 Pd C5 34.8(2) . . ? C2 Pd C5 79.8(3) . . ? C1 Pd C5 86.1(3) . . ? C6 Pd S2 157.94(19) . . ? C2 Pd S2 94.23(19) . . ? C1 Pd S2 95.7(2) . . ? C5 Pd S2 167.22(19) . . ? C6 Pd S1 94.3(2) . . ? C2 Pd S1 161.69(18) . . ? C1 Pd S1 162.52(19) . . ? C5 Pd S1 99.8(2) . . ? S2 Pd S1 82.28(6) . . ? C6 Pd Rh2 112.2(2) . . ? C2 Pd Rh2 137.76(18) . . ? C1 Pd Rh2 116.26(19) . . ? C5 Pd Rh2 139.9(2) . . ? S2 Pd Rh2 49.77(5) . . ? S1 Pd Rh2 49.95(4) . . ? C6 Pd Rh3 139.5(2) . . ? C2 Pd Rh3 115.35(18) . . ? C1 Pd Rh3 139.0(2) . . ? C5 Pd Rh3 122.87(17) . . ? S2 Pd Rh3 49.68(4) . . ? S1 Pd Rh3 49.52(4) . . ? Rh2 Pd Rh3 61.74(2) . . ? P2 Rh2 P1 94.80(7) . . ? P2 Rh2 S2 89.15(7) . . ? P1 Rh2 S2 175.89(7) . . ? P2 Rh2 S1 169.11(7) . . ? P1 Rh2 S1 95.99(7) . . ? S2 Rh2 S1 80.04(6) . . ? P2 Rh2 Pd 122.42(6) . . ? P1 Rh2 Pd 128.01(6) . . ? S2 Rh2 Pd 48.29(5) . . ? S1 Rh2 Pd 48.41(5) . . ? P2 Rh2 Rh3 124.16(5) . . ? P1 Rh2 Rh3 129.35(5) . . ? S2 Rh2 Rh3 48.29(4) . . ? S1 Rh2 Rh3 48.12(4) . . ? Pd Rh2 Rh3 59.304(18) . . ? P3 Rh3 P4 92.61(7) . . ? P3 Rh3 S1 95.85(7) . . ? P4 Rh3 S1 171.40(7) . . ? P3 Rh3 S2 175.25(7) . . ? P4 Rh3 S2 91.46(7) . . ? S1 Rh3 S2 80.16(6) . . ? P3 Rh3 Pd 130.46(6) . . ? P4 Rh3 Pd 124.04(6) . . ? S1 Rh3 Pd 48.27(5) . . ? S2 Rh3 Pd 48.10(5) . . ? P3 Rh3 Rh2 127.11(6) . . ? P4 Rh3 Rh2 126.26(5) . . ? S1 Rh3 Rh2 48.39(4) . . ? S2 Rh3 Rh2 48.18(5) . . ? Pd Rh3 Rh2 58.96(2) . . ? Pd S1 Rh3 82.22(6) . . ? Pd S1 Rh2 81.65(6) . . ? Rh3 S1 Rh2 83.49(6) . . ? Pd S2 Rh2 81.94(6) . . ? Pd S2 Rh3 82.22(6) . . ? Rh2 S2 Rh3 83.53(6) . . ? C2 C1 C8 125.7(7) . . ? C2 C1 Pd 72.0(4) . . ? C8 C1 Pd 111.2(5) . . ? C2 C1 H1 117.1 . . ? C8 C1 H1 117.1 . . ? Pd C1 H1 86.6 . . ? C1 C2 C3 125.5(7) . . ? C1 C2 Pd 72.5(4) . . ? C3 C2 Pd 107.7(5) . . ? C1 C2 H2 117.2 . . ? C3 C2 H2 117.2 . . ? Pd C2 H2 89.7 . . ? C2 C3 C4 115.4(6) . . ? C2 C3 H3A 108.4 . . ? C4 C3 H3A 108.4 . . ? C2 C3 H3B 108.4 . . ? C4 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? C5 C4 C3 113.1(6) . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C4 127.0(7) . . ? C6 C5 Pd 70.5(4) . . ? C4 C5 Pd 111.4(5) . . ? C6 C5 H5 116.5 . . ? C4 C5 H5 116.5 . . ? Pd C5 H5 87.9 . . ? C5 C6 C7 125.4(8) . . ? C5 C6 Pd 74.6(4) . . ? C7 C6 Pd 103.9(5) . . ? C5 C6 H6 117.3 . . ? C7 C6 H6 117.3 . . ? Pd C6 H6 91.5 . . ? C8 C7 C6 116.0(6) . . ? C8 C7 H7A 108.3 . . ? C6 C7 H7A 108.3 . . ? C8 C7 H7B 108.3 . . ? C6 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C1 C8 C7 111.5(7) . . ? C1 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? C1 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? O2 P1 O1 96.5(2) . . ? O2 P1 O3 102.3(3) . . ? O1 P1 O3 95.1(3) . . ? O2 P1 Rh2 116.4(2) . . ? O1 P1 Rh2 122.62(19) . . ? O3 P1 Rh2 119.26(18) . . ? C11 O1 P1 125.0(4) . . ? C12 C11 O1 115.6(6) . . ? C12 C11 C16 120.2(7) . . ? O1 C11 C16 124.1(7) . . ? C11 C12 C13 119.2(7) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C14 C13 C12 120.2(7) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 119.9(7) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.0(7) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C11 120.5(7) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? C17 O2 P1 129.6(4) . . ? C18 C17 C22 122.2(7) . . ? C18 C17 O2 121.2(6) . . ? C22 C17 O2 116.1(6) . . ? C17 C18 C19 118.8(7) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C20 C19 C18 120.2(7) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 119.5(7) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C20 C21 C22 121.2(7) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C17 C22 C21 118.0(7) . . ? C17 C22 H22 121.0 . . ? C21 C22 H22 121.0 . . ? C23 O3 P1 123.4(4) . . ? C24 C23 C28 118.8(8) . . ? C24 C23 O3 117.8(7) . . ? C28 C23 O3 123.3(7) . . ? C23 C24 C25 122.0(9) . . ? C23 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C26 C25 C24 119.6(9) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C27 C26 C25 119.7(8) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 120.0(9) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C23 C28 C27 119.9(8) . . ? C23 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? O6 P2 O4 100.0(3) . . ? O6 P2 O5 95.9(3) . . ? O4 P2 O5 102.2(2) . . ? O6 P2 Rh2 119.72(18) . . ? O4 P2 Rh2 116.45(19) . . ? O5 P2 Rh2 118.8(2) . . ? C29 O4 P2 124.6(4) . . ? C34 C29 C30 121.5(6) . . ? C34 C29 O4 117.6(6) . . ? C30 C29 O4 120.8(6) . . ? C29 C30 C31 118.6(7) . . ? C29 C30 H30 120.7 . . ? C31 C30 H30 120.7 . . ? C32 C31 C30 121.2(7) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C33 C32 C31 118.9(7) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C32 C33 C34 121.9(7) . . ? C32 C33 H33 119.0 . . ? C34 C33 H33 119.0 . . ? C29 C34 C33 117.8(7) . . ? C29 C34 H34 121.1 . . ? C33 C34 H34 121.1 . . ? C35 O5 P2 124.3(5) . . ? C40 C35 O5 118.0(8) . . ? C40 C35 C36 119.9(7) . . ? O5 C35 C36 122.0(7) . . ? C37 C36 C35 121.4(8) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C36 C37 C38 117.5(9) . . ? C36 C37 H37 121.3 . . ? C38 C37 H37 121.3 . . ? C39 C38 C37 119.5(9) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C40 122.1(9) . . ? C38 C39 H39 119.0 . . ? C40 C39 H39 119.0 . . ? C35 C40 C39 119.5(8) . . ? C35 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C41 O6 P2 127.6(5) . . ? C42 C41 C46 122.6(7) . . ? C42 C41 O6 119.0(6) . . ? C46 C41 O6 117.8(6) . . ? C41 C42 C43 118.6(8) . . ? C41 C42 H42 120.7 . . ? C43 C42 H42 120.7 . . ? C44 C43 C42 120.3(8) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 118.7(8) . . ? C43 C44 H44 120.6 . . ? C45 C44 H44 120.6 . . ? C46 C45 C44 121.6(8) . . ? C46 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? C41 C46 C45 118.1(7) . . ? C41 C46 H46 121.0 . . ? C45 C46 H46 121.0 . . ? O7 P3 O8 96.1(2) . . ? O7 P3 O9 100.5(2) . . ? O8 P3 O9 99.8(2) . . ? O7 P3 Rh3 113.36(18) . . ? O8 P3 Rh3 121.94(19) . . ? O9 P3 Rh3 120.62(19) . . ? C47 O7 P3 130.1(4) . . ? C52 C47 C48 120.5(7) . . ? C52 C47 O7 116.6(6) . . ? C48 C47 O7 122.8(7) . . ? C49 C48 C47 117.6(7) . . ? C49 C48 H48 121.2 . . ? C47 C48 H48 121.2 . . ? C50 C49 C48 122.3(7) . . ? C50 C49 H49 118.9 . . ? C48 C49 H49 118.9 . . ? C51 C50 C49 119.9(7) . . ? C51 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? C50 C51 C52 118.4(8) . . ? C50 C51 H51 120.8 . . ? C52 C51 H51 120.8 . . ? C47 C52 C51 121.4(7) . . ? C47 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? C53 O8 P3 133.2(4) . . ? C58 C53 C54 120.7(7) . . ? C58 C53 O8 124.4(7) . . ? C54 C53 O8 114.5(6) . . ? C53 C54 C55 117.8(8) . . ? C53 C54 H54 121.1 . . ? C55 C54 H54 121.1 . . ? C56 C55 C54 120.5(8) . . ? C56 C55 H55 119.7 . . ? C54 C55 H55 119.7 . . ? C57 C56 C55 120.2(8) . . ? C57 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C56 C57 C58 120.3(8) . . ? C56 C57 H57 119.9 . . ? C58 C57 H57 119.9 . . ? C53 C58 C57 120.3(8) . . ? C53 C58 H58 119.8 . . ? C57 C58 H58 119.8 . . ? C59 O9 P3 125.4(4) . . ? O9 C59 C60 121.9(6) . . ? O9 C59 C64 116.5(6) . . ? C60 C59 C64 121.5(7) . . ? C59 C60 C61 118.0(7) . . ? C59 C60 H60 121.0 . . ? C61 C60 H60 121.0 . . ? C62 C61 C60 121.6(7) . . ? C62 C61 H61 119.2 . . ? C60 C61 H61 119.2 . . ? C63 C62 C61 118.4(7) . . ? C63 C62 H62 120.8 . . ? C61 C62 H62 120.8 . . ? C62 C63 C64 122.3(7) . . ? C62 C63 H63 118.9 . . ? C64 C63 H63 118.9 . . ? C63 C64 C59 118.3(7) . . ? C63 C64 H64 120.9 . . ? C59 C64 H64 120.9 . . ? O12 P4 O10 101.5(3) . . ? O12 P4 O11 101.8(2) . . ? O10 P4 O11 89.5(2) . . ? O12 P4 Rh3 116.30(19) . . ? O10 P4 Rh3 123.27(19) . . ? O11 P4 Rh3 119.49(19) . . ? C65 O10 P4 123.6(4) . . ? C70 C65 C66 122.6(7) . . ? C70 C65 O10 121.6(6) . . ? C66 C65 O10 115.8(7) . . ? C67 C66 C65 118.7(7) . . ? C67 C66 H66 120.7 . . ? C65 C66 H66 120.7 . . ? C66 C67 C68 120.5(7) . . ? C66 C67 H67 119.7 . . ? C68 C67 H67 119.7 . . ? C67 C68 C69 119.1(7) . . ? C67 C68 H68 120.4 . . ? C69 C68 H68 120.4 . . ? C70 C69 C68 120.3(8) . . ? C70 C69 H69 119.8 . . ? C68 C69 H69 119.8 . . ? C65 C70 C69 118.7(7) . . ? C65 C70 H70 120.6 . . ? C69 C70 H70 120.6 . . ? C71 O11 P4 125.1(4) . . ? C76 C71 C72 121.2(7) . . ? C76 C71 O11 116.2(6) . . ? C72 C71 O11 122.3(6) . . ? C71 C72 C73 119.0(7) . . ? C71 C72 H72 120.5 . . ? C73 C72 H72 120.5 . . ? C74 C73 C72 120.6(8) . . ? C74 C73 H73 119.7 . . ? C72 C73 H73 119.7 . . ? C75 C74 C73 119.6(8) . . ? C75 C74 H74 120.2 . . ? C73 C74 H74 120.2 . . ? C74 C75 C76 120.8(7) . . ? C74 C75 H75 119.6 . . ? C76 C75 H75 119.6 . . ? C71 C76 C75 118.8(7) . . ? C71 C76 H76 120.6 . . ? C75 C76 H76 120.6 . . ? C77 O12 P4 125.3(4) . . ? C78 C77 C82 121.4(7) . . ? C78 C77 O12 120.6(6) . . ? C82 C77 O12 117.9(6) . . ? C77 C78 C79 120.1(7) . . ? C77 C78 H78 119.9 . . ? C79 C78 H78 119.9 . . ? C80 C79 C78 119.1(8) . . ? C80 C79 H79 120.4 . . ? C78 C79 H79 120.4 . . ? C79 C80 C81 121.1(7) . . ? C79 C80 H80 119.5 . . ? C81 C80 H80 119.5 . . ? C80 C81 C82 119.1(7) . . ? C80 C81 H81 120.4 . . ? C82 C81 H81 120.4 . . ? C77 C82 C81 119.2(7) . . ? C77 C82 H82 120.4 . . ? C81 C82 H82 120.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Pd Rh2 P2 -111.1(2) . . . . ? C2 Pd Rh2 P2 15.8(3) . . . . ? C1 Pd Rh2 P2 -20.3(2) . . . . ? C5 Pd Rh2 P2 -138.1(3) . . . . ? S2 Pd Rh2 P2 53.86(8) . . . . ? S1 Pd Rh2 P2 172.63(8) . . . . ? Rh3 Pd Rh2 P2 113.36(6) . . . . ? C6 Pd Rh2 P1 17.4(2) . . . . ? C2 Pd Rh2 P1 144.3(3) . . . . ? C1 Pd Rh2 P1 108.2(2) . . . . ? C5 Pd Rh2 P1 -9.6(3) . . . . ? S2 Pd Rh2 P1 -177.67(9) . . . . ? S1 Pd Rh2 P1 -58.90(8) . . . . ? Rh3 Pd Rh2 P1 -118.16(6) . . . . ? C6 Pd Rh2 S2 -165.0(2) . . . . ? C2 Pd Rh2 S2 -38.0(3) . . . . ? C1 Pd Rh2 S2 -74.1(2) . . . . ? C5 Pd Rh2 S2 168.1(3) . . . . ? S1 Pd Rh2 S2 118.77(8) . . . . ? Rh3 Pd Rh2 S2 59.51(5) . . . . ? C6 Pd Rh2 S1 76.2(2) . . . . ? C2 Pd Rh2 S1 -156.8(3) . . . . ? C1 Pd Rh2 S1 167.1(2) . . . . ? C5 Pd Rh2 S1 49.3(3) . . . . ? S2 Pd Rh2 S1 -118.77(8) . . . . ? Rh3 Pd Rh2 S1 -59.27(6) . . . . ? C6 Pd Rh2 Rh3 135.5(2) . . . . ? C2 Pd Rh2 Rh3 -97.5(3) . . . . ? C1 Pd Rh2 Rh3 -133.6(2) . . . . ? C5 Pd Rh2 Rh3 108.6(3) . . . . ? S2 Pd Rh2 Rh3 -59.51(5) . . . . ? S1 Pd Rh2 Rh3 59.27(6) . . . . ? C6 Pd Rh3 P3 22.6(3) . . . . ? C2 Pd Rh3 P3 -113.2(2) . . . . ? C1 Pd Rh3 P3 -147.2(3) . . . . ? C5 Pd Rh3 P3 -19.0(3) . . . . ? S2 Pd Rh3 P3 173.98(9) . . . . ? S1 Pd Rh3 P3 54.46(9) . . . . ? Rh2 Pd Rh3 P3 114.35(7) . . . . ? C6 Pd Rh3 P4 153.0(3) . . . . ? C2 Pd Rh3 P4 17.2(2) . . . . ? C1 Pd Rh3 P4 -16.8(3) . . . . ? C5 Pd Rh3 P4 111.4(3) . . . . ? S2 Pd Rh3 P4 -55.61(8) . . . . ? S1 Pd Rh3 P4 -175.13(8) . . . . ? Rh2 Pd Rh3 P4 -115.24(6) . . . . ? C6 Pd Rh3 S1 -31.9(3) . . . . ? C2 Pd Rh3 S1 -167.6(2) . . . . ? C1 Pd Rh3 S1 158.4(3) . . . . ? C5 Pd Rh3 S1 -73.4(3) . . . . ? S2 Pd Rh3 S1 119.52(8) . . . . ? Rh2 Pd Rh3 S1 59.89(6) . . . . ? C6 Pd Rh3 S2 -151.4(3) . . . . ? C2 Pd Rh3 S2 72.9(2) . . . . ? C1 Pd Rh3 S2 38.8(3) . . . . ? C5 Pd Rh3 S2 167.0(3) . . . . ? S1 Pd Rh3 S2 -119.52(8) . . . . ? Rh2 Pd Rh3 S2 -59.64(6) . . . . ? C6 Pd Rh3 Rh2 -91.8(3) . . . . ? C2 Pd Rh3 Rh2 132.5(2) . . . . ? C1 Pd Rh3 Rh2 98.5(3) . . . . ? C5 Pd Rh3 Rh2 -133.3(2) . . . . ? S2 Pd Rh3 Rh2 59.64(6) . . . . ? S1 Pd Rh3 Rh2 -59.89(6) . . . . ? P2 Rh2 Rh3 P3 129.84(9) . . . . ? P1 Rh2 Rh3 P3 -3.57(10) . . . . ? S2 Rh2 Rh3 P3 -179.13(9) . . . . ? S1 Rh2 Rh3 P3 -59.93(9) . . . . ? Pd Rh2 Rh3 P3 -119.63(7) . . . . ? P2 Rh2 Rh3 P4 1.11(10) . . . . ? P1 Rh2 Rh3 P4 -132.30(9) . . . . ? S2 Rh2 Rh3 P4 52.13(9) . . . . ? S1 Rh2 Rh3 P4 171.33(9) . . . . ? Pd Rh2 Rh3 P4 111.64(7) . . . . ? P2 Rh2 Rh3 S1 -170.22(9) . . . . ? P1 Rh2 Rh3 S1 56.36(9) . . . . ? S2 Rh2 Rh3 S1 -119.20(8) . . . . ? Pd Rh2 Rh3 S1 -59.70(6) . . . . ? P2 Rh2 Rh3 S2 -51.02(9) . . . . ? P1 Rh2 Rh3 S2 175.57(9) . . . . ? S1 Rh2 Rh3 S2 119.20(8) . . . . ? Pd Rh2 Rh3 S2 59.50(6) . . . . ? P2 Rh2 Rh3 Pd -110.53(7) . . . . ? P1 Rh2 Rh3 Pd 116.06(7) . . . . ? S2 Rh2 Rh3 Pd -59.50(6) . . . . ? S1 Rh2 Rh3 Pd 59.70(6) . . . . ? C6 Pd S1 Rh3 159.88(18) . . . . ? C2 Pd S1 Rh3 38.0(6) . . . . ? C1 Pd S1 Rh3 -126.4(7) . . . . ? C5 Pd S1 Rh3 125.21(18) . . . . ? S2 Pd S1 Rh3 -42.03(5) . . . . ? Rh2 Pd S1 Rh3 -84.51(6) . . . . ? C6 Pd S1 Rh2 -115.61(19) . . . . ? C2 Pd S1 Rh2 122.6(6) . . . . ? C1 Pd S1 Rh2 -41.8(7) . . . . ? C5 Pd S1 Rh2 -150.28(18) . . . . ? S2 Pd S1 Rh2 42.48(5) . . . . ? Rh3 Pd S1 Rh2 84.51(6) . . . . ? P3 Rh3 S1 Pd -141.51(6) . . . . ? S2 Rh3 S1 Pd 41.10(6) . . . . ? Rh2 Rh3 S1 Pd 82.42(5) . . . . ? P3 Rh3 S1 Rh2 136.07(7) . . . . ? S2 Rh3 S1 Rh2 -41.32(6) . . . . ? Pd Rh3 S1 Rh2 -82.42(5) . . . . ? P2 Rh2 S1 Pd -35.0(4) . . . . ? P1 Rh2 S1 Pd 137.29(6) . . . . ? S2 Rh2 S1 Pd -41.63(6) . . . . ? Rh3 Rh2 S1 Pd -83.05(6) . . . . ? P2 Rh2 S1 Rh3 48.1(4) . . . . ? P1 Rh2 S1 Rh3 -139.66(6) . . . . ? S2 Rh2 S1 Rh3 41.42(6) . . . . ? Pd Rh2 S1 Rh3 83.05(6) . . . . ? C6 Pd S2 Rh2 39.7(6) . . . . ? C2 Pd S2 Rh2 155.47(18) . . . . ? C1 Pd S2 Rh2 119.91(19) . . . . ? C5 Pd S2 Rh2 -142.9(9) . . . . ? S1 Pd S2 Rh2 -42.61(5) . . . . ? Rh3 Pd S2 Rh2 -84.52(5) . . . . ? C6 Pd S2 Rh3 124.2(6) . . . . ? C2 Pd S2 Rh3 -120.01(18) . . . . ? C1 Pd S2 Rh3 -155.58(19) . . . . ? C5 Pd S2 Rh3 -58.4(9) . . . . ? S1 Pd S2 Rh3 41.90(5) . . . . ? Rh2 Pd S2 Rh3 84.52(5) . . . . ? P2 Rh2 S2 Pd -137.02(6) . . . . ? S1 Rh2 S2 Pd 41.73(5) . . . . ? Rh3 Rh2 S2 Pd 83.02(5) . . . . ? P2 Rh2 S2 Rh3 139.96(7) . . . . ? S1 Rh2 S2 Rh3 -41.29(6) . . . . ? Pd Rh2 S2 Rh3 -83.02(5) . . . . ? P4 Rh3 S2 Pd 136.84(6) . . . . ? S1 Rh3 S2 Pd -41.23(6) . . . . ? Rh2 Rh3 S2 Pd -82.71(5) . . . . ? P4 Rh3 S2 Rh2 -140.45(7) . . . . ? S1 Rh3 S2 Rh2 41.48(6) . . . . ? Pd Rh3 S2 Rh2 82.71(5) . . . . ? C6 Pd C1 C2 -112.6(5) . . . . ? C5 Pd C1 C2 -77.9(5) . . . . ? S2 Pd C1 C2 89.4(4) . . . . ? S1 Pd C1 C2 171.6(5) . . . . ? Rh2 Pd C1 C2 136.9(4) . . . . ? Rh3 Pd C1 C2 60.6(5) . . . . ? C6 Pd C1 C8 9.6(5) . . . . ? C2 Pd C1 C8 122.2(7) . . . . ? C5 Pd C1 C8 44.3(5) . . . . ? S2 Pd C1 C8 -148.5(5) . . . . ? S1 Pd C1 C8 -66.2(9) . . . . ? Rh2 Pd C1 C8 -100.9(5) . . . . ? Rh3 Pd C1 C8 -177.2(4) . . . . ? C8 C1 C2 C3 -4.0(12) . . . . ? Pd C1 C2 C3 99.6(7) . . . . ? C8 C1 C2 Pd -103.6(7) . . . . ? C6 Pd C2 C1 66.3(5) . . . . ? C5 Pd C2 C1 97.6(5) . . . . ? S2 Pd C2 C1 -93.8(4) . . . . ? S1 Pd C2 C1 -172.0(5) . . . . ? Rh2 Pd C2 C1 -65.7(5) . . . . ? Rh3 Pd C2 C1 -140.8(4) . . . . ? C6 Pd C2 C3 -56.3(5) . . . . ? C1 Pd C2 C3 -122.6(7) . . . . ? C5 Pd C2 C3 -25.0(5) . . . . ? S2 Pd C2 C3 143.6(5) . . . . ? S1 Pd C2 C3 65.4(9) . . . . ? Rh2 Pd C2 C3 171.7(3) . . . . ? Rh3 Pd C2 C3 96.7(5) . . . . ? C1 C2 C3 C4 -41.2(10) . . . . ? Pd C2 C3 C4 39.6(7) . . . . ? C2 C3 C4 C5 -34.4(9) . . . . ? C3 C4 C5 C6 91.6(9) . . . . ? C3 C4 C5 Pd 10.3(7) . . . . ? C2 Pd C5 C6 -115.2(5) . . . . ? C1 Pd C5 C6 -80.0(5) . . . . ? S2 Pd C5 C6 -178.3(7) . . . . ? S1 Pd C5 C6 83.4(5) . . . . ? Rh2 Pd C5 C6 47.3(6) . . . . ? Rh3 Pd C5 C6 131.1(4) . . . . ? C6 Pd C5 C4 123.2(7) . . . . ? C2 Pd C5 C4 7.9(5) . . . . ? C1 Pd C5 C4 43.1(5) . . . . ? S2 Pd C5 C4 -55.1(11) . . . . ? S1 Pd C5 C4 -153.5(4) . . . . ? Rh2 Pd C5 C4 170.5(3) . . . . ? Rh3 Pd C5 C4 -105.7(4) . . . . ? C4 C5 C6 C7 -6.3(12) . . . . ? Pd C5 C6 C7 96.4(7) . . . . ? C4 C5 C6 Pd -102.6(8) . . . . ? C2 Pd C6 C5 63.4(5) . . . . ? C1 Pd C6 C5 96.0(5) . . . . ? S2 Pd C6 C5 179.0(4) . . . . ? S1 Pd C6 C5 -101.0(5) . . . . ? Rh2 Pd C6 C5 -149.2(4) . . . . ? Rh3 Pd C6 C5 -77.3(6) . . . . ? C2 Pd C6 C7 -60.0(5) . . . . ? C1 Pd C6 C7 -27.5(5) . . . . ? C5 Pd C6 C7 -123.5(8) . . . . ? S2 Pd C6 C7 55.5(9) . . . . ? S1 Pd C6 C7 135.5(5) . . . . ? Rh2 Pd C6 C7 87.3(5) . . . . ? Rh3 Pd C6 C7 159.3(4) . . . . ? C5 C6 C7 C8 -36.0(11) . . . . ? Pd C6 C7 C8 44.9(8) . . . . ? C2 C1 C8 C7 94.2(9) . . . . ? Pd C1 C8 C7 11.6(8) . . . . ? C6 C7 C8 C1 -39.3(9) . . . . ? P2 Rh2 P1 O2 44.5(2) . . . . ? S1 Rh2 P1 O2 -134.1(2) . . . . ? Pd Rh2 P1 O2 -94.0(2) . . . . ? Rh3 Rh2 P1 O2 -172.6(2) . . . . ? P2 Rh2 P1 O1 -73.4(2) . . . . ? S1 Rh2 P1 O1 108.0(2) . . . . ? Pd Rh2 P1 O1 148.1(2) . . . . ? Rh3 Rh2 P1 O1 69.5(2) . . . . ? P2 Rh2 P1 O3 167.9(2) . . . . ? S1 Rh2 P1 O3 -10.6(2) . . . . ? Pd Rh2 P1 O3 29.5(2) . . . . ? Rh3 Rh2 P1 O3 -49.2(2) . . . . ? O2 P1 O1 C11 -177.9(5) . . . . ? O3 P1 O1 C11 79.1(6) . . . . ? Rh2 P1 O1 C11 -50.7(6) . . . . ? P1 O1 C11 C12 167.0(5) . . . . ? P1 O1 C11 C16 -15.1(10) . . . . ? O1 C11 C12 C13 178.1(6) . . . . ? C16 C11 C12 C13 0.1(12) . . . . ? C11 C12 C13 C14 -0.3(12) . . . . ? C12 C13 C14 C15 0.5(12) . . . . ? C13 C14 C15 C16 -0.5(12) . . . . ? C14 C15 C16 C11 0.3(12) . . . . ? C12 C11 C16 C15 -0.1(12) . . . . ? O1 C11 C16 C15 -177.9(7) . . . . ? O1 P1 O2 C17 -38.3(6) . . . . ? O3 P1 O2 C17 58.4(6) . . . . ? Rh2 P1 O2 C17 -169.8(5) . . . . ? P1 O2 C17 C18 -62.5(9) . . . . ? P1 O2 C17 C22 124.9(6) . . . . ? C22 C17 C18 C19 -2.4(11) . . . . ? O2 C17 C18 C19 -174.6(6) . . . . ? C17 C18 C19 C20 2.1(11) . . . . ? C18 C19 C20 C21 -0.5(11) . . . . ? C19 C20 C21 C22 -0.9(12) . . . . ? C18 C17 C22 C21 1.0(11) . . . . ? O2 C17 C22 C21 173.6(6) . . . . ? C20 C21 C22 C17 0.7(12) . . . . ? O2 P1 O3 C23 70.1(5) . . . . ? O1 P1 O3 C23 167.9(5) . . . . ? Rh2 P1 O3 C23 -60.0(5) . . . . ? P1 O3 C23 C24 158.6(5) . . . . ? P1 O3 C23 C28 -25.7(9) . . . . ? C28 C23 C24 C25 0.9(12) . . . . ? O3 C23 C24 C25 176.8(7) . . . . ? C23 C24 C25 C26 1.0(14) . . . . ? C24 C25 C26 C27 -1.9(14) . . . . ? C25 C26 C27 C28 0.9(13) . . . . ? C24 C23 C28 C27 -1.9(11) . . . . ? O3 C23 C28 C27 -177.5(7) . . . . ? C26 C27 C28 C23 1.0(12) . . . . ? P1 Rh2 P2 O6 125.1(2) . . . . ? S2 Rh2 P2 O6 -56.1(2) . . . . ? S1 Rh2 P2 O6 -62.6(5) . . . . ? Pd Rh2 P2 O6 -93.1(2) . . . . ? Rh3 Rh2 P2 O6 -20.6(2) . . . . ? P1 Rh2 P2 O4 4.6(2) . . . . ? S2 Rh2 P2 O4 -176.6(2) . . . . ? S1 Rh2 P2 O4 176.9(4) . . . . ? Pd Rh2 P2 O4 146.37(19) . . . . ? Rh3 Rh2 P2 O4 -141.08(19) . . . . ? P1 Rh2 P2 O5 -118.2(2) . . . . ? S2 Rh2 P2 O5 60.6(2) . . . . ? S1 Rh2 P2 O5 54.1(5) . . . . ? Pd Rh2 P2 O5 23.5(2) . . . . ? Rh3 Rh2 P2 O5 96.1(2) . . . . ? O6 P2 O4 C29 49.2(5) . . . . ? O5 P2 O4 C29 -49.2(5) . . . . ? Rh2 P2 O4 C29 179.7(4) . . . . ? P2 O4 C29 C34 -104.8(7) . . . . ? P2 O4 C29 C30 80.0(7) . . . . ? C34 C29 C30 C31 2.6(11) . . . . ? O4 C29 C30 C31 177.6(6) . . . . ? C29 C30 C31 C32 -1.3(11) . . . . ? C30 C31 C32 C33 -1.1(12) . . . . ? C31 C32 C33 C34 2.3(12) . . . . ? C30 C29 C34 C33 -1.4(11) . . . . ? O4 C29 C34 C33 -176.6(6) . . . . ? C32 C33 C34 C29 -1.1(12) . . . . ? O6 P2 O5 C35 170.2(5) . . . . ? O4 P2 O5 C35 -88.2(5) . . . . ? Rh2 P2 O5 C35 41.5(6) . . . . ? P2 O5 C35 C40 -148.5(5) . . . . ? P2 O5 C35 C36 35.0(8) . . . . ? C40 C35 C36 C37 2.7(10) . . . . ? O5 C35 C36 C37 179.1(6) . . . . ? C35 C36 C37 C38 -3.0(11) . . . . ? C36 C37 C38 C39 0.7(12) . . . . ? C37 C38 C39 C40 2.1(13) . . . . ? O5 C35 C40 C39 -176.5(7) . . . . ? C36 C35 C40 C39 0.0(11) . . . . ? C38 C39 C40 C35 -2.5(13) . . . . ? O4 P2 O6 C41 -114.5(5) . . . . ? O5 P2 O6 C41 -11.0(6) . . . . ? Rh2 P2 O6 C41 117.1(5) . . . . ? P2 O6 C41 C42 83.4(9) . . . . ? P2 O6 C41 C46 -104.9(8) . . . . ? C46 C41 C42 C43 3.7(14) . . . . ? O6 C41 C42 C43 175.0(7) . . . . ? C41 C42 C43 C44 -1.4(14) . . . . ? C42 C43 C44 C45 -0.1(14) . . . . ? C43 C44 C45 C46 -0.6(14) . . . . ? C42 C41 C46 C45 -4.3(14) . . . . ? O6 C41 C46 C45 -175.7(8) . . . . ? C44 C45 C46 C41 2.7(14) . . . . ? P4 Rh3 P3 O7 45.2(2) . . . . ? S1 Rh3 P3 O7 -136.3(2) . . . . ? Pd Rh3 P3 O7 -173.95(19) . . . . ? Rh2 Rh3 P3 O7 -95.8(2) . . . . ? P4 Rh3 P3 O8 159.2(2) . . . . ? S1 Rh3 P3 O8 -22.4(2) . . . . ? Pd Rh3 P3 O8 -60.0(2) . . . . ? Rh2 Rh3 P3 O8 18.2(2) . . . . ? P4 Rh3 P3 O9 -73.8(2) . . . . ? S1 Rh3 P3 O9 104.6(2) . . . . ? Pd Rh3 P3 O9 67.0(2) . . . . ? Rh2 Rh3 P3 O9 145.2(2) . . . . ? O8 P3 O7 C47 36.7(6) . . . . ? O9 P3 O7 C47 -64.5(6) . . . . ? Rh3 P3 O7 C47 165.4(5) . . . . ? P3 O7 C47 C52 -142.4(6) . . . . ? P3 O7 C47 C48 40.1(9) . . . . ? C52 C47 C48 C49 -0.2(11) . . . . ? O7 C47 C48 C49 177.2(7) . . . . ? C47 C48 C49 C50 -0.3(13) . . . . ? C48 C49 C50 C51 0.0(13) . . . . ? C49 C50 C51 C52 0.8(12) . . . . ? C48 C47 C52 C51 1.0(11) . . . . ? O7 C47 C52 C51 -176.5(6) . . . . ? C50 C51 C52 C47 -1.3(11) . . . . ? O7 P3 O8 C53 -146.2(6) . . . . ? O9 P3 O8 C53 -44.5(6) . . . . ? Rh3 P3 O8 C53 91.3(6) . . . . ? P3 O8 C53 C58 47.7(10) . . . . ? P3 O8 C53 C54 -139.3(6) . . . . ? C58 C53 C54 C55 -0.2(13) . . . . ? O8 C53 C54 C55 -173.5(7) . . . . ? C53 C54 C55 C56 -2.4(14) . . . . ? C54 C55 C56 C57 3.1(14) . . . . ? C55 C56 C57 C58 -1.3(13) . . . . ? C54 C53 C58 C57 1.9(12) . . . . ? O8 C53 C58 C57 174.5(7) . . . . ? C56 C57 C58 C53 -1.2(13) . . . . ? O7 P3 O9 C59 -138.5(5) . . . . ? O8 P3 O9 C59 123.4(5) . . . . ? Rh3 P3 O9 C59 -13.2(6) . . . . ? P3 O9 C59 C60 -47.3(8) . . . . ? P3 O9 C59 C64 137.0(5) . . . . ? O9 C59 C60 C61 -176.0(6) . . . . ? C64 C59 C60 C61 -0.5(10) . . . . ? C59 C60 C61 C62 1.5(11) . . . . ? C60 C61 C62 C63 -1.1(12) . . . . ? C61 C62 C63 C64 -0.4(12) . . . . ? C62 C63 C64 C59 1.4(12) . . . . ? O9 C59 C64 C63 174.8(6) . . . . ? C60 C59 C64 C63 -0.9(11) . . . . ? P3 Rh3 P4 O12 28.1(2) . . . . ? S2 Rh3 P4 O12 -154.3(2) . . . . ? Pd Rh3 P4 O12 -116.4(2) . . . . ? Rh2 Rh3 P4 O12 169.6(2) . . . . ? P3 Rh3 P4 O10 -98.0(2) . . . . ? S2 Rh3 P4 O10 79.6(2) . . . . ? Pd Rh3 P4 O10 117.5(2) . . . . ? Rh2 Rh3 P4 O10 43.5(2) . . . . ? P3 Rh3 P4 O11 150.9(2) . . . . ? S2 Rh3 P4 O11 -31.5(2) . . . . ? Pd Rh3 P4 O11 6.4(2) . . . . ? Rh2 Rh3 P4 O11 -67.6(2) . . . . ? O12 P4 O10 C65 -93.7(5) . . . . ? O11 P4 O10 C65 164.3(5) . . . . ? Rh3 P4 O10 C65 38.6(6) . . . . ? P4 O10 C65 C70 -59.5(8) . . . . ? P4 O10 C65 C66 123.0(6) . . . . ? C70 C65 C66 C67 -0.7(11) . . . . ? O10 C65 C66 C67 176.8(6) . . . . ? C65 C66 C67 C68 1.9(11) . . . . ? C66 C67 C68 C69 -2.3(11) . . . . ? C67 C68 C69 C70 1.6(11) . . . . ? C66 C65 C70 C69 0.0(11) . . . . ? O10 C65 C70 C69 -177.4(6) . . . . ? C68 C69 C70 C65 -0.5(11) . . . . ? O12 P4 O11 C71 76.1(5) . . . . ? O10 P4 O11 C71 177.7(5) . . . . ? Rh3 P4 O11 C71 -53.6(5) . . . . ? P4 O11 C71 C76 152.5(5) . . . . ? P4 O11 C71 C72 -33.6(9) . . . . ? C76 C71 C72 C73 0.0(11) . . . . ? O11 C71 C72 C73 -173.6(6) . . . . ? C71 C72 C73 C74 -0.5(11) . . . . ? C72 C73 C74 C75 0.1(12) . . . . ? C73 C74 C75 C76 0.9(12) . . . . ? C72 C71 C76 C75 0.9(11) . . . . ? O11 C71 C76 C75 174.8(6) . . . . ? C74 C75 C76 C71 -1.4(12) . . . . ? O10 P4 O12 C77 -36.6(6) . . . . ? O11 P4 O12 C77 55.3(6) . . . . ? Rh3 P4 O12 C77 -173.0(5) . . . . ? P4 O12 C77 C78 -83.2(8) . . . . ? P4 O12 C77 C82 100.4(6) . . . . ? C82 C77 C78 C79 -0.8(11) . . . . ? O12 C77 C78 C79 -177.1(6) . . . . ? C77 C78 C79 C80 -0.9(11) . . . . ? C78 C79 C80 C81 1.9(12) . . . . ? C79 C80 C81 C82 -1.1(12) . . . . ? C78 C77 C82 C81 1.6(10) . . . . ? O12 C77 C82 C81 177.9(6) . . . . ? C80 C81 C82 C77 -0.7(11) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.768 _refine_diff_density_min -1.092 _refine_diff_density_rms 0.117 data_compnd_7 _database_code_depnum_ccdc_archive 'CCDC 908507' #TrackingRef '15071_web_deposit_cif_file_0_FernandoJ.Lahoz_1351623726.compnd_3_6_7_9_11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C80 H72 O12 P4 Pt Rh2 S2, C H2 Cl2' _chemical_formula_sum 'C81 H74 Cl2 O12 P4 Pt Rh2 S2' _chemical_formula_weight 1899.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.019(3) _cell_length_b 14.506(4) _cell_length_c 23.261(6) _cell_angle_alpha 88.088(4) _cell_angle_beta 79.405(4) _cell_angle_gamma 63.931(4) _cell_volume 3873.1(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4205 _cell_measurement_theta_min 2.254 _cell_measurement_theta_max 21.985 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.182 _exptl_crystal_size_mid 0.137 _exptl_crystal_size_min 0.078 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1900 _exptl_absorpt_coefficient_mu 2.489 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6601 _exptl_absorpt_correction_T_max 0.8295 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within SAINT+ package, v. 6.45. ; _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 SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 48268 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.0753 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.48 _reflns_number_total 18337 _reflns_number_gt 13706 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.45 (Bruker AXS, 2003)' _computing_data_reduction 'SAINT+ v. 6.45 (Bruker AXS, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, SHELXTLv6.12, BrukerAXS' _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. All non-hydrogen non-disordered atoms were refined with anisotropic displace- ment parameters. Static disorder was observed for 6 phenyl rings of the phos- phite ligands. They were modelled on the base of two moieties of complementary occupancy; eventually all occupancy parameters refined to similar values close to 0.5, and a common fixed occupancy factor was assumed. An additional disordered dichloromethane solvent molecule was observed in the crystal structure. Two molecules, with complementary occupancies were included in the last cycles of refinement. All hydrogens were included in calculated positions and were refined with riding positional and thermal parameters. Only two electro density residual were observed above 1 e/A^3, but all of them were in close proximity of the metal atoms with no chemical sense. ; _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^)+(0.0418P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18337 _refine_ls_number_parameters 974 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.0992 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl145as in P-1 CELL 0.71073 13.0191 14.5059 23.2608 88.088 79.405 63.931 ZERR 2.00 0.0031 0.0035 0.0056 0.004 0.004 0.004 LATT 1 SFAC C H O P S CL RH PT UNIT 162 148 24 8 4 4 4 2 MERG 2 SIZE 0.182 0.137 0.078 OMIT 1 1 4 OMIT 3 3 1 FMAP 2 PLAN 20 ACTA 54 BOND $H WPDB -2 L.S. 4 TEMP -173.00 DFIX 31.0 0.05 C83A CL1A C83a CL2a DFIX 31.0 0.05 C83b Cl1b C83b Cl2b DFIX 31.66 0.05 Cl1a Cl2a Cl1b Cl2b WGHT 0.041800 FVAR 1.88185 0.34026 1.67962 PT 8 0.324394 0.390211 0.323473 11.00000 0.02916 0.02970 = 0.01612 0.00159 -0.00195 -0.01937 RH2 7 0.257400 0.343658 0.211245 11.00000 0.01394 0.02765 = 0.01850 -0.00428 -0.00057 -0.00896 RH3 7 0.414992 0.165415 0.277606 11.00000 0.01350 0.03000 = 0.02173 -0.00685 -0.00010 -0.00888 S1 5 0.439523 0.306712 0.235356 11.00000 0.01994 0.04560 = 0.01595 0.00151 -0.00218 -0.01819 S2 5 0.224403 0.296862 0.308739 11.00000 0.01691 0.02417 = 0.02295 -0.00336 0.00176 -0.01009 C1 1 0.190213 0.494689 0.393940 11.00000 0.04681 0.03090 = 0.02243 -0.00384 -0.00091 -0.02206 AFIX 43 H1 2 0.135212 0.487491 0.375001 11.00000 -1.20000 AFIX 0 C2 1 0.265179 0.408749 0.418932 11.00000 0.05487 0.03123 = 0.01664 -0.00027 -0.00083 -0.02664 AFIX 43 H2 2 0.252145 0.349244 0.418978 11.00000 -1.20000 AFIX 0 C3 1 0.364608 0.401271 0.445798 11.00000 0.06504 0.03753 = 0.02344 0.00742 -0.00975 -0.02981 AFIX 23 H3A 2 0.418695 0.327808 0.447365 11.00000 -1.20000 H3B 2 0.333923 0.430851 0.486565 11.00000 -1.20000 AFIX 0 C4 1 0.432847 0.456380 0.412737 11.00000 0.05858 0.03125 = 0.03352 0.01094 -0.02337 -0.02707 AFIX 23 H4A 2 0.392360 0.530217 0.425450 11.00000 -1.20000 H4B 2 0.511192 0.427635 0.422990 11.00000 -1.20000 AFIX 0 C5 1 0.445640 0.445685 0.346728 11.00000 0.04612 0.03275 = 0.02756 0.01013 -0.01459 -0.02759 AFIX 43 H5 2 0.507950 0.385873 0.326379 11.00000 -1.20000 AFIX 0 C6 1 0.371637 0.518165 0.314580 11.00000 0.04479 0.04382 = 0.02689 0.00684 -0.01293 -0.03372 AFIX 43 H6 2 0.389874 0.506284 0.273226 11.00000 -1.20000 AFIX 0 C7 1 0.264834 0.614123 0.339438 11.00000 0.05796 0.03360 = 0.03209 0.01533 -0.01766 -0.02801 AFIX 23 H7A 2 0.215999 0.640457 0.309142 11.00000 -1.20000 H7B 2 0.289386 0.666933 0.348195 11.00000 -1.20000 AFIX 0 C8 1 0.190422 0.600513 0.394920 11.00000 0.06851 0.02668 = 0.03175 0.00038 -0.01223 -0.02293 AFIX 23 H8A 2 0.109539 0.654953 0.398653 11.00000 -1.20000 H8B 2 0.220944 0.608222 0.429503 11.00000 -1.20000 AFIX 0 P1 4 0.310085 0.385082 0.123744 11.00000 0.01854 0.04432 = 0.01803 -0.00336 -0.00064 -0.01355 REM Phenyl O1 C11-C16 - Two complete moieties O1 3 0.395750 0.295668 0.074756 11.00000 0.02341 0.06596 = 0.02436 -0.01991 0.00310 -0.01538 PART 1 C11A 1 0.513899 0.284968 0.048337 10.50000 0.02615 C12A 1 0.594763 0.255621 0.084027 10.50000 0.03047 AFIX 43 H12A 2 0.572782 0.253070 0.125101 10.50000 -1.20000 AFIX 0 C13A 1 0.710210 0.229636 0.058238 10.50000 0.03209 AFIX 43 H13A 2 0.767416 0.208584 0.082279 10.50000 -1.20000 AFIX 0 C14A 1 0.742601 0.233612 0.000261 10.50000 0.03169 AFIX 43 H14A 2 0.821350 0.206881 -0.019542 10.50000 -1.20000 AFIX 0 C15A 1 0.653309 0.278475 -0.025727 10.50000 0.02814 AFIX 43 H15A 2 0.668860 0.306356 -0.061991 10.50000 -1.20000 AFIX 0 C16A 1 0.542263 0.291638 -0.009332 10.50000 0.02632 AFIX 43 H16A 2 0.490482 0.304168 -0.035755 10.50000 -1.20000 AFIX 0 PART 2 C11B 1 0.510335 0.262940 0.052044 10.50000 0.01797 C12B 1 0.600090 0.199067 0.079875 10.50000 0.02753 AFIX 43 H12B 2 0.583755 0.171092 0.115976 10.50000 -1.20000 AFIX 0 C13B 1 0.712888 0.176947 0.054400 10.50000 0.02945 AFIX 43 H13B 2 0.774935 0.133289 0.073043 10.50000 -1.20000 AFIX 0 C14B 1 0.736856 0.217592 0.001961 10.50000 0.02457 AFIX 43 H14B 2 0.812272 0.214096 -0.010364 10.50000 -1.20000 AFIX 0 C15B 1 0.653722 0.263837 -0.033710 10.50000 0.02817 AFIX 43 H15B 2 0.672758 0.269256 -0.074714 10.50000 -1.20000 AFIX 0 C16B 1 0.535737 0.302382 -0.001132 10.50000 0.02572 AFIX 43 H16B 2 0.474429 0.355637 -0.016333 10.50000 -1.20000 AFIX 0 PART 0 REM Phenyl O2 C17-C22 - OK O2 3 0.384464 0.450936 0.113710 11.00000 0.02473 0.05326 = 0.02285 0.00091 -0.00166 -0.02147 C17 1 0.364890 0.539413 0.143676 11.00000 0.04234 0.05747 = 0.02116 0.01884 -0.01227 -0.03780 C18 1 0.255088 0.611842 0.170285 11.00000 0.05166 0.05071 = 0.02200 0.00881 -0.00329 -0.03468 AFIX 43 H18 2 0.188926 0.599352 0.171652 11.00000 -1.20000 AFIX 0 C19 1 0.243261 0.702245 0.194734 11.00000 0.08235 0.05035 = 0.02495 0.01250 -0.01086 -0.04064 AFIX 43 H19 2 0.168602 0.752011 0.213328 11.00000 -1.20000 AFIX 0 C20 1 0.338833 0.720642 0.192326 11.00000 0.13737 0.07876 = 0.05400 0.03906 -0.05508 -0.08272 AFIX 43 H20 2 0.329215 0.784775 0.207108 11.00000 -1.20000 AFIX 0 C21 1 0.449383 0.646098 0.168424 11.00000 0.09692 0.10080 = 0.07031 0.05674 -0.05557 -0.08372 AFIX 43 H21 2 0.515946 0.656905 0.169348 11.00000 -1.20000 AFIX 0 C22 1 0.461619 0.555529 0.143141 11.00000 0.04981 0.08201 = 0.04019 0.03294 -0.02593 -0.04785 AFIX 43 H22 2 0.536552 0.504874 0.125535 11.00000 -1.20000 AFIX 0 REM Phenyl O3 C23-C28 - two moieties sharing two atoms C23 and C26 O3 3 0.202558 0.448350 0.091298 11.00000 0.02160 0.05200 = 0.01734 0.00460 -0.00165 -0.01663 C23 1 0.203297 0.472411 0.032571 11.00000 0.02789 0.03717 = 0.02296 0.00633 -0.00277 -0.01650 PART 1 10.5 C24A 1 0.262351 0.521411 -0.000811 10.50000 0.03470 0.03742 = 0.01576 0.00750 -0.00705 -0.02333 AFIX 43 H24A 2 0.313456 0.538731 0.015777 10.50000 -1.20000 AFIX 0 C25A 1 0.248202 0.545828 -0.058368 10.50000 0.03161 0.02540 = 0.03394 0.00760 0.00810 0.00379 AFIX 43 H25A 2 0.292816 0.576323 -0.080704 10.50000 -1.20000 AFIX 0 C27A 1 0.097279 0.492082 -0.047205 10.50000 0.03212 0.03979 = 0.02219 0.00189 -0.00657 -0.01223 AFIX 43 H27A 2 0.038519 0.487022 -0.063923 10.50000 -1.20000 AFIX 0 C28A 1 0.111202 0.465905 0.009072 10.50000 0.02752 0.04036 = 0.02752 0.01642 -0.00649 -0.01702 AFIX 43 H28A 2 0.059881 0.443325 0.032772 10.50000 -1.20000 AFIX 0 PART 2 10.5 C24B 1 0.192245 0.562796 0.021919 10.50000 0.06620 0.07101 = 0.01933 0.01124 -0.01595 -0.04110 AFIX 43 H24B 2 0.187961 0.608451 0.051607 10.50000 -1.20000 AFIX 0 C25B 1 0.186624 0.591724 -0.037692 10.50000 0.08605 0.04682 = 0.04513 0.02168 -0.04137 -0.04149 AFIX 43 H25B 2 0.187214 0.655253 -0.048496 10.50000 -1.20000 AFIX 0 C27B 1 0.215515 0.425416 -0.066392 10.50000 0.03266 0.03780 = 0.03456 -0.00591 -0.01904 -0.00551 AFIX 43 H27B 2 0.235254 0.374960 -0.096740 10.50000 -1.20000 AFIX 0 C28B 1 0.222184 0.394848 -0.008459 10.50000 0.03680 0.03826 = 0.03370 0.01098 -0.01432 -0.01244 AFIX 43 H28B 2 0.238294 0.326687 0.002111 10.50000 -1.20000 AFIX 0 PART 0 C26 1 0.180289 0.528985 -0.080451 11.00000 0.06166 0.05828 = 0.01844 0.00632 -0.00391 -0.02752 AFIX 43 H26 2 0.179923 0.539826 -0.120932 11.00000 -1.20000 AFIX 0 P2 4 0.089402 0.370652 0.193681 11.00000 0.01437 0.01821 = 0.03239 0.00211 -0.00493 -0.00558 REM Phenyl O4 C29-C34 - two phenyl rings with one common pivot atom O4 3 -0.002457 0.485443 0.181456 11.00000 0.01771 0.02252 = 0.05204 0.01010 -0.00119 -0.00412 C29 1 -0.024743 0.572393 0.215698 11.00000 0.01842 0.01253 = 0.10097 -0.00627 0.01635 -0.00489 PART 1 C30A 1 -0.009381 0.561390 0.283732 10.50000 0.02416 AFIX 43 H30A 2 0.020241 0.496005 0.300142 10.50000 -1.20000 AFIX 0 C31A 1 -0.041062 0.650976 0.317269 10.50000 0.02918 AFIX 43 H31A 2 -0.038798 0.646610 0.357895 10.50000 -1.20000 AFIX 0 C32A 1 -0.075898 0.746589 0.292973 10.50000 0.02372 AFIX 43 H32A 2 -0.092166 0.805784 0.316175 10.50000 -1.20000 AFIX 0 C33A 1 -0.086609 0.754587 0.234660 10.50000 0.02397 AFIX 43 H33A 2 -0.114066 0.819854 0.218041 10.50000 -1.20000 AFIX 0 C34A 1 -0.056853 0.666297 0.200565 10.50000 0.02633 AFIX 43 H34A 2 -0.060668 0.676443 0.160308 10.50000 -1.20000 AFIX 0 PART 2 C30B 1 -0.022699 0.577762 0.264102 10.50000 0.02848 AFIX 43 H30B 2 -0.000440 0.517893 0.286052 10.50000 -1.20000 AFIX 0 C31B 1 -0.053583 0.674317 0.291224 10.50000 0.03761 AFIX 43 H31B 2 -0.049745 0.679009 0.331346 10.50000 -1.20000 AFIX 0 C32B 1 -0.088333 0.759579 0.260817 10.50000 0.03106 AFIX 43 H32B 2 -0.108848 0.824006 0.279697 10.50000 -1.20000 AFIX 0 C33B 1 -0.094587 0.754889 0.202987 10.50000 0.04315 AFIX 43 H33B 2 -0.118323 0.815857 0.181996 10.50000 -1.20000 AFIX 0 C34B 1 -0.066187 0.660624 0.174383 10.50000 0.03327 AFIX 43 H34B 2 -0.071868 0.652627 0.134889 10.50000 -1.20000 AFIX 0 PART 0 REM Phenyl O5 C35-C40 - two phenyl rings with one common pivot atom O5 3 0.076685 0.323811 0.135044 11.00000 0.03509 0.03011 = 0.03593 0.00940 -0.01962 -0.01756 C35 1 0.133931 0.219482 0.117380 11.00000 0.02816 0.04223 = 0.02060 -0.00741 0.00281 -0.02182 PART 1 10.5 C36A 1 0.203818 0.139878 0.152987 10.50000 0.02541 AFIX 43 H36A 2 0.217407 0.161060 0.187901 10.50000 -1.20000 AFIX 0 C37A 1 0.250952 0.036521 0.139080 10.50000 0.02956 AFIX 43 H37A 2 0.293934 -0.012492 0.164187 10.50000 -1.20000 AFIX 0 C38A 1 0.233712 0.005228 0.086449 10.50000 0.02616 AFIX 43 H38A 2 0.265210 -0.065957 0.075887 10.50000 -1.20000 AFIX 0 C39A 1 0.170844 0.077637 0.049601 10.50000 0.03873 AFIX 43 H39A 2 0.160943 0.056425 0.013645 10.50000 -1.20000 AFIX 0 C40A 1 0.122032 0.183511 0.066896 10.50000 0.03282 AFIX 43 H40A 2 0.078513 0.232128 0.041788 10.50000 -1.20000 AFIX 0 PART 2 10.5 C36B 1 0.186771 0.147193 0.148946 10.50000 0.03946 AFIX 43 H36B 2 0.187656 0.159911 0.188610 10.50000 -1.20000 AFIX 0 C37B 1 0.244645 0.046103 0.121960 10.50000 0.03030 AFIX 43 H37B 2 0.286614 -0.011006 0.143180 10.50000 -1.20000 AFIX 0 C38B 1 0.238565 0.032421 0.063598 10.50000 0.04588 AFIX 43 H38B 2 0.275064 -0.034219 0.044634 10.50000 -1.20000 AFIX 0 C39B 1 0.178609 0.117556 0.034343 10.50000 0.05372 AFIX 43 H39B 2 0.176717 0.107585 -0.005536 10.50000 -1.20000 AFIX 0 C40B 1 0.123275 0.212608 0.058055 10.50000 0.03609 AFIX 43 H40B 2 0.080691 0.270460 0.037481 10.50000 -1.20000 AFIX 0 PART 0 REM Phenyl O6 C41-C46 - OK O6 3 0.008106 0.337246 0.243892 11.00000 0.01739 0.02549 = 0.04002 0.01225 -0.01270 -0.01099 C41 1 -0.103173 0.353759 0.236071 11.00000 0.01882 0.03724 = 0.03117 0.01859 -0.01317 -0.01630 C42 1 -0.196256 0.446835 0.254406 11.00000 0.02451 0.04287 = 0.03693 0.00941 -0.00545 -0.01742 AFIX 43 H42 2 -0.185492 0.499648 0.271628 11.00000 -1.20000 AFIX 0 C43 1 -0.308375 0.462995 0.247300 11.00000 0.01406 0.05678 = 0.04931 0.01902 -0.00362 -0.01292 AFIX 43 H43 2 -0.373822 0.527086 0.259385 11.00000 -1.20000 AFIX 0 C44 1 -0.321560 0.385796 0.222971 11.00000 0.02507 0.06655 = 0.04643 0.03262 -0.01966 -0.03027 AFIX 43 H44 2 -0.396948 0.396580 0.218317 11.00000 -1.20000 AFIX 0 C45 1 -0.228015 0.292408 0.204957 11.00000 0.03658 0.04485 = 0.05263 0.02478 -0.02342 -0.03024 AFIX 43 H45 2 -0.238833 0.239880 0.187444 11.00000 -1.20000 AFIX 0 C46 1 -0.118307 0.275329 0.212437 11.00000 0.03171 0.03353 = 0.05004 0.02143 -0.01835 -0.01981 AFIX 43 H46 2 -0.053782 0.210246 0.201438 11.00000 -1.20000 AFIX 0 P3 4 0.592022 0.051210 0.245586 11.00000 0.01383 0.04461 = 0.02807 -0.01414 -0.00176 -0.00711 O7 3 0.679043 -0.003112 0.291499 11.00000 0.01789 0.02994 = 0.02812 -0.00455 -0.00266 -0.00978 C47 1 0.676927 0.051580 0.339445 11.00000 0.01632 0.03395 = 0.01978 -0.00294 -0.00058 -0.01141 C48 1 0.691805 -0.000316 0.390656 11.00000 0.03370 0.04891 = 0.03213 0.01245 -0.00580 -0.02435 AFIX 43 H48 2 0.697976 -0.068050 0.392222 11.00000 -1.20000 AFIX 0 C49 1 0.697541 0.047832 0.439421 11.00000 0.06148 0.07678 = 0.02050 0.01443 -0.01031 -0.03749 AFIX 43 H49 2 0.706910 0.013390 0.474925 11.00000 -1.20000 AFIX 0 C50 1 0.689697 0.145695 0.436648 11.00000 0.06353 0.06519 = 0.02622 -0.00970 -0.01278 -0.02838 AFIX 43 H50 2 0.695279 0.177937 0.470049 11.00000 -1.20000 AFIX 0 C51 1 0.673936 0.196593 0.386123 11.00000 0.03855 0.03468 = 0.03910 -0.01001 -0.01340 -0.01160 AFIX 43 H51 2 0.668076 0.264234 0.384920 11.00000 -1.20000 AFIX 0 C52 1 0.666369 0.151286 0.336693 11.00000 0.02155 0.03317 = 0.03120 0.00349 -0.00711 -0.01290 AFIX 43 H52 2 0.654287 0.187255 0.301795 11.00000 -1.20000 AFIX 0 REM Phenyl O8 C53-C58 - Two complete moieties O8 3 0.671028 0.088322 0.197051 11.00000 0.01242 0.08100 = 0.01732 0.00328 -0.00143 -0.00233 PART 1 C53A 1 0.788237 0.008155 0.174658 10.50000 0.02010 C54A 1 0.871134 0.018488 0.199516 10.50000 0.02632 AFIX 43 H54A 2 0.847236 0.065232 0.232375 10.50000 -1.20000 AFIX 0 C55A 1 0.990633 -0.039124 0.176983 10.50000 0.02814 AFIX 43 H55A 2 1.047669 -0.034595 0.195458 10.50000 -1.20000 AFIX 0 C56A 1 1.022817 -0.102312 0.127405 10.50000 0.02823 AFIX 43 H56A 2 1.103034 -0.140893 0.111104 10.50000 -1.20000 AFIX 0 C57A 1 0.940394 -0.110183 0.101293 10.50000 0.03122 AFIX 43 H57A 2 0.963778 -0.154000 0.067139 10.50000 -1.20000 AFIX 0 C58A 1 0.823123 -0.054270 0.124710 10.50000 0.02726 AFIX 43 H58A 2 0.766403 -0.059111 0.106110 10.50000 -1.20000 AFIX 0 PART 2 C53B 1 0.791016 0.042999 0.175126 10.50000 0.01877 C54B 1 0.872818 0.032044 0.207076 10.50000 0.02087 AFIX 43 H54B 2 0.849952 0.057960 0.246680 10.50000 -1.20000 AFIX 0 C55B 1 0.988865 -0.016746 0.181791 10.50000 0.02476 AFIX 43 H55B 2 1.045772 -0.020570 0.203364 10.50000 -1.20000 AFIX 0 C56B 1 1.023409 -0.059824 0.126005 10.50000 0.02759 AFIX 43 H56B 2 1.103930 -0.094880 0.109391 10.50000 -1.20000 AFIX 0 C57B 1 0.941632 -0.052357 0.094053 10.50000 0.03432 AFIX 43 H57B 2 0.965328 -0.083051 0.055482 10.50000 -1.20000 AFIX 0 C58B 1 0.821672 0.001331 0.118824 10.50000 0.02953 AFIX 43 H58B 2 0.763874 0.008346 0.097050 10.50000 -1.20000 AFIX 0 PART 0 REM Phenyl O9 C59-C64 - Two complete moieties O9 3 0.619652 -0.059908 0.218257 11.00000 0.01920 0.06670 = 0.07185 -0.05245 -0.00892 -0.00105 PART 1 C59A 1 0.583009 -0.055442 0.158461 10.50000 0.01974 C60A 1 0.536007 0.027209 0.123084 10.50000 0.02843 AFIX 43 H60A 2 0.523481 0.094436 0.133910 10.50000 -1.20000 AFIX 0 C61A 1 0.509000 0.007140 0.072479 10.50000 0.03311 AFIX 43 H61A 2 0.477399 0.061494 0.047440 10.50000 -1.20000 AFIX 0 C62A 1 0.526819 -0.091970 0.056541 10.50000 0.03960 AFIX 43 H62A 2 0.511544 -0.105165 0.020063 10.50000 -1.20000 AFIX 0 C63A 1 0.566154 -0.169189 0.093676 10.50000 0.04243 AFIX 43 H63A 2 0.574466 -0.235638 0.084261 10.50000 -1.20000 AFIX 0 C64A 1 0.594373 -0.149665 0.146115 10.50000 0.03507 AFIX 43 H64A 2 0.621223 -0.202664 0.172545 10.50000 -1.20000 AFIX 0 PART 2 C59B 1 0.601068 -0.098911 0.173327 10.50000 0.02356 C60B 1 0.536671 -0.026325 0.139104 10.50000 0.02607 AFIX 43 H60B 2 0.493831 0.043678 0.152827 10.50000 -1.20000 AFIX 0 C61B 1 0.535578 -0.058278 0.082758 10.50000 0.03749 AFIX 43 H61B 2 0.491518 -0.009267 0.057979 10.50000 -1.20000 AFIX 0 C62B 1 0.597689 -0.159685 0.063383 10.50000 0.04031 AFIX 43 H62B 2 0.598688 -0.180345 0.024876 10.50000 -1.20000 AFIX 0 C63B 1 0.657944 -0.230653 0.099603 10.50000 0.04251 AFIX 43 H63B 2 0.700184 -0.300729 0.085957 10.50000 -1.20000 AFIX 0 C64B 1 0.658965 -0.202930 0.155765 10.50000 0.03067 AFIX 43 H64B 2 0.697838 -0.253141 0.181474 10.50000 -1.20000 AFIX 0 PART 0 P4 4 0.370071 0.050627 0.321935 11.00000 0.01556 0.02496 = 0.03829 -0.00796 -0.00169 -0.00778 O10 3 0.480267 -0.046419 0.338436 11.00000 0.01790 0.02749 = 0.05007 -0.00074 -0.00549 -0.00839 C65 1 0.495700 -0.143851 0.355579 11.00000 0.02844 0.02495 = 0.05029 -0.00715 -0.00914 -0.01088 C66 1 0.411254 -0.162631 0.391832 11.00000 0.03048 0.02915 = 0.03215 -0.00458 -0.00829 -0.00739 AFIX 43 H66 2 0.336414 -0.108099 0.405612 11.00000 -1.20000 AFIX 0 C67 1 0.437021 -0.262016 0.407869 11.00000 0.04250 0.03538 = 0.04438 0.00141 -0.01533 -0.01915 AFIX 43 H67 2 0.378247 -0.275540 0.431834 11.00000 -1.20000 AFIX 0 C68 1 0.545264 -0.341255 0.389980 11.00000 0.05422 0.02688 = 0.09651 0.00058 -0.02561 -0.01749 AFIX 43 H68 2 0.562401 -0.409096 0.401584 11.00000 -1.20000 AFIX 0 C69 1 0.628581 -0.320069 0.354759 11.00000 0.04302 0.02452 = 0.15951 -0.03023 0.00894 -0.00802 AFIX 43 H69 2 0.704522 -0.374070 0.342578 11.00000 -1.20000 AFIX 0 C70 1 0.604511 -0.221918 0.336597 11.00000 0.02818 0.02519 = 0.12434 -0.01934 0.01142 -0.01073 AFIX 43 H70 2 0.662470 -0.208973 0.311412 11.00000 -1.20000 AFIX 0 O11 3 0.312592 -0.005831 0.288857 11.00000 0.01977 0.03316 = 0.05482 -0.01886 -0.00418 -0.00905 C71 1 0.201142 -0.000318 0.305360 11.00000 0.02526 0.02745 = 0.04776 0.00331 -0.01519 -0.01414 C72 1 0.103984 0.092277 0.308554 11.00000 0.02835 0.02605 = 0.05038 0.01046 -0.01231 -0.01454 AFIX 43 H72 2 0.111343 0.153999 0.300656 11.00000 -1.20000 AFIX 0 C73 1 -0.004929 0.093978 0.323505 11.00000 0.02627 0.04734 = 0.05589 0.02000 -0.01788 -0.01502 AFIX 43 H73 2 -0.072950 0.157607 0.327170 11.00000 -1.20000 AFIX 0 C74 1 -0.015080 0.003125 0.333149 11.00000 0.03842 0.07903 = 0.07058 0.04113 -0.03074 -0.04374 AFIX 43 H74 2 -0.089907 0.004476 0.342611 11.00000 -1.20000 AFIX 0 C75 1 0.082663 -0.088217 0.329016 11.00000 0.06855 0.04988 = 0.08872 0.03909 -0.05442 -0.04582 AFIX 43 H75 2 0.075294 -0.150127 0.336026 11.00000 -1.20000 AFIX 0 C76 1 0.192120 -0.091609 0.314757 11.00000 0.05041 0.02374 = 0.06617 0.01326 -0.03801 -0.02024 AFIX 43 H76 2 0.259967 -0.155318 0.311451 11.00000 -1.20000 AFIX 0 O12 3 0.274786 0.080252 0.382209 11.00000 0.02011 0.02715 = 0.03919 -0.00555 0.00239 -0.01255 C77 1 0.273634 0.132834 0.431273 11.00000 0.03917 0.02353 = 0.03306 0.00205 0.00763 -0.02006 C78 1 0.163742 0.191083 0.465035 11.00000 0.03858 0.03304 = 0.04535 -0.00032 0.01443 -0.00694 AFIX 43 H78 2 0.096126 0.195256 0.452860 11.00000 -1.20000 AFIX 0 C79 1 0.153608 0.242035 0.515573 11.00000 0.05899 0.05296 = 0.04380 -0.00763 0.02402 -0.01296 AFIX 43 H79 2 0.078790 0.282531 0.538341 11.00000 -1.20000 AFIX 0 C80 1 0.251885 0.234801 0.533634 11.00000 0.11602 0.03301 = 0.02334 -0.00478 0.01698 -0.02894 AFIX 43 H80 2 0.244627 0.269788 0.569055 11.00000 -1.20000 AFIX 0 C81 1 0.362236 0.176138 0.499997 11.00000 0.07802 0.05063 = 0.02614 0.01278 -0.01177 -0.04587 AFIX 43 H81 2 0.430000 0.170175 0.512809 11.00000 -1.20000 AFIX 0 C82 1 0.372009 0.126896 0.447979 11.00000 0.04032 0.03057 = 0.03049 -0.00048 0.00474 -0.01715 AFIX 43 H82 2 0.446278 0.089233 0.423986 11.00000 -1.20000 AFIX 0 PART 1 C83A 1 0.088781 0.625223 0.600557 21.00000 0.05612 0.05590 = 0.28919 -0.01623 -0.07503 0.01046 AFIX 23 H83A 2 0.032124 0.674658 0.578198 21.00000 -1.20000 H83B 2 0.058646 0.641898 0.643067 21.00000 -1.20000 AFIX 0 CL1A 6 0.124420 0.496708 0.581189 21.00000 0.05338 0.05770 = 0.09262 -0.00944 0.02815 -0.02649 CL2A 6 0.224158 0.620353 0.579876 21.00000 0.05613 0.07135 = 0.09166 -0.01906 -0.00629 -0.04041 PART 2 C83B 1 0.081681 0.618305 0.604899 -21.00000 0.02879 0.04982 = 0.02349 -0.01063 0.00622 -0.01165 AFIX 23 H83C 2 0.001826 0.667725 0.623326 -21.00000 -1.20000 H83D 2 0.122759 0.579904 0.636184 -21.00000 -1.20000 AFIX 0 CL1B 6 0.075804 0.532806 0.555487 -21.00000 0.08023 0.10041 = 0.05407 -0.01915 0.01225 -0.06672 CL2B 6 0.153716 0.682577 0.567916 -21.00000 0.05530 0.07255 = 0.09171 -0.02047 0.00563 -0.04239 PART 0 HKLF 4 REM fjl145as in P-1 REM R1 = 0.0456 for 13706 Fo > 4sig(Fo) and 0.0681 for all 18337 data REM 974 parameters refined using 6 restraints END WGHT 0.0418 0.0000 REM Highest difference peak 1.348, deepest hole -0.937, 1-sigma level 0.129 Q1 1 0.2997 0.3311 0.3227 11.00000 0.05 1.35 Q2 1 0.3593 0.4462 0.3233 11.00000 0.05 1.23 Q3 1 0.2825 0.3907 0.2107 11.00000 0.05 0.91 Q4 1 0.3876 0.1223 0.2731 11.00000 0.05 0.86 Q5 1 0.4440 0.2249 0.2809 11.00000 0.05 0.84 Q6 1 0.2344 0.2847 0.2066 11.00000 0.05 0.83 Q7 1 0.4322 0.1823 0.3051 11.00000 0.05 0.80 Q8 1 0.2388 0.4097 0.3281 11.00000 0.05 0.79 Q9 1 0.2396 0.3257 0.1812 11.00000 0.05 0.74 Q10 1 0.4053 0.3997 0.3093 11.00000 0.05 0.73 Q11 1 0.2607 0.3450 0.2402 11.00000 0.05 0.72 Q12 1 0.3174 0.3028 0.2108 11.00000 0.05 0.70 Q13 1 0.2993 0.3697 0.2900 11.00000 0.05 0.68 Q14 1 0.3432 0.4224 0.3588 11.00000 0.05 0.66 Q15 1 0.1944 0.3922 0.2132 11.00000 0.05 0.66 Q16 1 0.2225 0.0699 0.0419 11.00000 0.05 0.63 Q17 1 0.3799 0.1486 0.2954 11.00000 0.05 0.62 Q18 1 0.4665 0.1261 0.2767 11.00000 0.05 0.61 Q19 1 0.3552 0.4207 0.2878 11.00000 0.05 0.61 Q20 1 -0.1018 0.3176 0.2195 11.00000 0.05 0.59 ; 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 Pt Pt 0.324394(16) 0.390211(14) 0.323473(8) 0.02297(6) Uani 1 1 d . . . Rh2 Rh 0.25740(3) 0.34366(3) 0.211245(15) 0.02032(8) Uani 1 1 d . . . Rh3 Rh 0.41499(3) 0.16542(3) 0.277606(16) 0.02225(9) Uani 1 1 d . . . S1 S 0.43952(10) 0.30671(10) 0.23536(5) 0.0259(3) Uani 1 1 d . . . S2 S 0.22440(9) 0.29686(9) 0.30874(5) 0.0216(2) Uani 1 1 d . . . C1 C 0.1902(5) 0.4947(4) 0.3939(2) 0.0322(12) Uani 1 1 d . . . H1 H 0.1352 0.4875 0.3750 0.039 Uiso 1 1 calc R . . C2 C 0.2652(5) 0.4087(4) 0.4189(2) 0.0322(12) Uani 1 1 d . . . H2 H 0.2521 0.3492 0.4190 0.039 Uiso 1 1 calc R . . C3 C 0.3646(5) 0.4013(4) 0.4458(2) 0.0393(13) Uani 1 1 d . . . H3A H 0.4187 0.3278 0.4474 0.047 Uiso 1 1 calc R . . H3B H 0.3339 0.4309 0.4866 0.047 Uiso 1 1 calc R . . C4 C 0.4328(5) 0.4564(4) 0.4127(2) 0.0366(13) Uani 1 1 d . . . H4A H 0.3924 0.5302 0.4254 0.044 Uiso 1 1 calc R . . H4B H 0.5112 0.4276 0.4230 0.044 Uiso 1 1 calc R . . C5 C 0.4456(5) 0.4457(4) 0.3467(2) 0.0308(12) Uani 1 1 d . . . H5 H 0.5079 0.3859 0.3264 0.037 Uiso 1 1 calc R . . C6 C 0.3716(5) 0.5182(4) 0.3146(2) 0.0325(12) Uani 1 1 d . . . H6 H 0.3899 0.5063 0.2732 0.039 Uiso 1 1 calc R . . C7 C 0.2648(5) 0.6141(4) 0.3394(2) 0.0374(13) Uani 1 1 d . . . H7A H 0.2160 0.6405 0.3091 0.045 Uiso 1 1 calc R . . H7B H 0.2894 0.6669 0.3482 0.045 Uiso 1 1 calc R . . C8 C 0.1904(5) 0.6005(4) 0.3949(2) 0.0412(14) Uani 1 1 d . . . H8A H 0.1095 0.6550 0.3987 0.049 Uiso 1 1 calc R . . H8B H 0.2209 0.6082 0.4295 0.049 Uiso 1 1 calc R . . P1 P 0.31008(11) 0.38508(11) 0.12374(5) 0.0273(3) Uani 1 1 d . A . O1 O 0.3957(3) 0.2957(3) 0.07476(15) 0.0400(9) Uani 1 1 d . . . C11A C 0.5139(11) 0.2850(10) 0.0483(6) 0.026(3) Uiso 0.50 1 d P A 1 C12A C 0.5948(9) 0.2556(8) 0.0840(5) 0.030(2) Uiso 0.50 1 d P A 1 H12A H 0.5728 0.2531 0.1251 0.037 Uiso 0.50 1 calc PR A 1 C13A C 0.7102(9) 0.2296(8) 0.0582(5) 0.032(2) Uiso 0.50 1 d P A 1 H13A H 0.7674 0.2086 0.0823 0.039 Uiso 0.50 1 calc PR A 1 C14A C 0.7426(15) 0.2336(12) 0.0003(8) 0.032(5) Uiso 0.50 1 d P A 1 H14A H 0.8213 0.2069 -0.0195 0.038 Uiso 0.50 1 calc PR A 1 C15A C 0.6533(14) 0.2785(12) -0.0257(7) 0.028(4) Uiso 0.50 1 d P A 1 H15A H 0.6689 0.3064 -0.0620 0.034 Uiso 0.50 1 calc PR A 1 C16A C 0.5423(16) 0.2916(13) -0.0093(8) 0.026(5) Uiso 0.50 1 d P A 1 H16A H 0.4905 0.3042 -0.0358 0.032 Uiso 0.50 1 calc PR A 1 C11B C 0.5103(10) 0.2629(9) 0.0520(5) 0.018(3) Uiso 0.50 1 d P A 2 C12B C 0.6001(8) 0.1991(8) 0.0799(4) 0.028(2) Uiso 0.50 1 d P A 2 H12B H 0.5838 0.1711 0.1160 0.033 Uiso 0.50 1 calc PR A 2 C13B C 0.7129(9) 0.1769(8) 0.0544(4) 0.029(2) Uiso 0.50 1 d P A 2 H13B H 0.7749 0.1333 0.0730 0.035 Uiso 0.50 1 calc PR A 2 C14B C 0.7369(13) 0.2176(12) 0.0020(7) 0.025(4) Uiso 0.50 1 d P A 2 H14B H 0.8123 0.2141 -0.0104 0.029 Uiso 0.50 1 calc PR A 2 C15B C 0.6537(14) 0.2638(12) -0.0337(7) 0.028(4) Uiso 0.50 1 d P A 2 H15B H 0.6728 0.2693 -0.0747 0.034 Uiso 0.50 1 calc PR A 2 C16B C 0.5357(17) 0.3024(14) -0.0011(8) 0.026(5) Uiso 0.50 1 d P A 2 H16B H 0.4744 0.3556 -0.0163 0.031 Uiso 0.50 1 calc PR A 2 O2 O 0.3845(3) 0.4509(3) 0.11371(14) 0.0324(8) Uani 1 1 d . . . C17 C 0.3649(5) 0.5394(4) 0.1437(2) 0.0340(13) Uani 1 1 d . A . C18 C 0.2551(5) 0.6118(4) 0.1703(2) 0.0377(13) Uani 1 1 d . . . H18 H 0.1889 0.5994 0.1717 0.045 Uiso 1 1 calc R A . C19 C 0.2433(6) 0.7022(5) 0.1947(2) 0.0485(16) Uani 1 1 d . A . H19 H 0.1686 0.7520 0.2133 0.058 Uiso 1 1 calc R . . C20 C 0.3388(8) 0.7206(6) 0.1923(3) 0.073(2) Uani 1 1 d . . . H20 H 0.3292 0.7848 0.2071 0.087 Uiso 1 1 calc R A . C21 C 0.4494(8) 0.6461(7) 0.1684(3) 0.070(2) Uani 1 1 d . A . H21 H 0.5159 0.6569 0.1693 0.084 Uiso 1 1 calc R . . C22 C 0.4616(5) 0.5555(5) 0.1431(2) 0.0487(16) Uani 1 1 d . . . H22 H 0.5366 0.5049 0.1255 0.058 Uiso 1 1 calc R A . O3 O 0.2026(3) 0.4483(3) 0.09130(13) 0.0305(8) Uani 1 1 d . . . C23 C 0.2033(4) 0.4724(4) 0.0326(2) 0.0289(11) Uani 1 1 d . A . C24A C 0.2624(10) 0.5214(8) -0.0008(4) 0.026(2) Uani 0.50 1 d P A 1 H24A H 0.3135 0.5387 0.0158 0.032 Uiso 0.50 1 calc PR A 1 C25A C 0.2482(11) 0.5458(9) -0.0584(6) 0.039(3) Uani 0.50 1 d P A 1 H25A H 0.2928 0.5763 -0.0807 0.046 Uiso 0.50 1 calc PR A 1 C27A C 0.0973(9) 0.4921(8) -0.0472(4) 0.033(2) Uani 0.50 1 d P A 1 H27A H 0.0385 0.4870 -0.0639 0.039 Uiso 0.50 1 calc PR A 1 C28A C 0.1112(8) 0.4659(8) 0.0091(4) 0.031(2) Uani 0.50 1 d P A 1 H28A H 0.0599 0.4433 0.0328 0.037 Uiso 0.50 1 calc PR A 1 C24B C 0.1922(12) 0.5628(11) 0.0219(5) 0.047(3) Uani 0.50 1 d P A 2 H24B H 0.1880 0.6085 0.0516 0.057 Uiso 0.50 1 calc PR A 2 C25B C 0.1866(14) 0.5917(11) -0.0377(6) 0.051(4) Uani 0.50 1 d P A 2 H25B H 0.1872 0.6553 -0.0485 0.061 Uiso 0.50 1 calc PR A 2 C27B C 0.2155(9) 0.4254(8) -0.0664(5) 0.037(3) Uani 0.50 1 d P A 2 H27B H 0.2353 0.3750 -0.0967 0.044 Uiso 0.50 1 calc PR A 2 C28B C 0.2222(9) 0.3948(9) -0.0085(5) 0.037(3) Uani 0.50 1 d P A 2 H28B H 0.2383 0.3267 0.0021 0.044 Uiso 0.50 1 calc PR A 2 C26 C 0.1803(6) 0.5290(5) -0.0805(2) 0.0463(15) Uani 1 1 d . . . H26 H 0.1799 0.5398 -0.1209 0.056 Uiso 1 1 calc R A 1 P2 P 0.08940(10) 0.37065(9) 0.19368(6) 0.0222(3) Uani 1 1 d . . . O4 O -0.0025(3) 0.4854(2) 0.18146(16) 0.0335(8) Uani 1 1 d . B . C29 C -0.0247(4) 0.5724(4) 0.2157(3) 0.0484(18) Uani 1 1 d . . . C30A C -0.0094(9) 0.5614(8) 0.2837(5) 0.024(2) Uiso 0.50 1 d P B 1 H30A H 0.0202 0.4960 0.3001 0.029 Uiso 0.50 1 calc PR B 1 C31A C -0.0411(9) 0.6510(8) 0.3173(5) 0.029(2) Uiso 0.50 1 d P B 1 H31A H -0.0388 0.6466 0.3579 0.035 Uiso 0.50 1 calc PR B 1 C32A C -0.0759(8) 0.7466(8) 0.2930(5) 0.024(2) Uiso 0.50 1 d P B 1 H32A H -0.0922 0.8058 0.3162 0.028 Uiso 0.50 1 calc PR B 1 C33A C -0.0866(9) 0.7546(8) 0.2347(6) 0.024(2) Uiso 0.50 1 d P B 1 H33A H -0.1141 0.8199 0.2180 0.029 Uiso 0.50 1 calc PR B 1 C34A C -0.0569(9) 0.6663(8) 0.2006(5) 0.026(2) Uiso 0.50 1 d P B 1 H34A H -0.0607 0.6764 0.1603 0.032 Uiso 0.50 1 calc PR B 1 C30B C -0.0227(10) 0.5778(9) 0.2641(6) 0.028(3) Uiso 0.50 1 d P B 2 H30B H -0.0004 0.5179 0.2861 0.034 Uiso 0.50 1 calc PR B 2 C31B C -0.0536(10) 0.6743(9) 0.2912(5) 0.038(3) Uiso 0.50 1 d P B 2 H31B H -0.0497 0.6790 0.3313 0.045 Uiso 0.50 1 calc PR B 2 C32B C -0.0883(9) 0.7596(9) 0.2608(7) 0.031(3) Uiso 0.50 1 d P B 2 H32B H -0.1088 0.8240 0.2797 0.037 Uiso 0.50 1 calc PR B 2 C33B C -0.0946(10) 0.7549(9) 0.2030(6) 0.043(3) Uiso 0.50 1 d P B 2 H33B H -0.1183 0.8159 0.1820 0.052 Uiso 0.50 1 calc PR B 2 C34B C -0.0662(10) 0.6606(8) 0.1744(5) 0.033(2) Uiso 0.50 1 d P B 2 H34B H -0.0719 0.6526 0.1349 0.040 Uiso 0.50 1 calc PR B 2 O5 O 0.0767(3) 0.3238(2) 0.13504(15) 0.0309(8) Uani 1 1 d . C . C35 C 0.1339(4) 0.2195(4) 0.1174(2) 0.0288(11) Uani 1 1 d . . . C36A C 0.2038(16) 0.1399(14) 0.1530(8) 0.025(5) Uiso 0.50 1 d P C 1 H36A H 0.2174 0.1611 0.1879 0.030 Uiso 0.50 1 calc PR C 1 C37A C 0.2510(11) 0.0365(10) 0.1391(6) 0.030(3) Uiso 0.50 1 d P C 1 H37A H 0.2939 -0.0125 0.1642 0.035 Uiso 0.50 1 calc PR C 1 C38A C 0.2337(9) 0.0052(8) 0.0864(5) 0.026(2) Uiso 0.50 1 d P C 1 H38A H 0.2652 -0.0660 0.0759 0.031 Uiso 0.50 1 calc PR C 1 C39A C 0.1708(10) 0.0776(10) 0.0496(5) 0.039(3) Uiso 0.50 1 d P C 1 H39A H 0.1609 0.0564 0.0136 0.046 Uiso 0.50 1 calc PR C 1 C40A C 0.1220(11) 0.1835(10) 0.0669(6) 0.033(3) Uiso 0.50 1 d P C 1 H40A H 0.0785 0.2321 0.0418 0.039 Uiso 0.50 1 calc PR C 1 C36B C 0.1868(17) 0.1472(17) 0.1489(10) 0.039(7) Uiso 0.50 1 d P C 2 H36B H 0.1877 0.1599 0.1886 0.047 Uiso 0.50 1 calc PR C 2 C37B C 0.2446(11) 0.0461(10) 0.1220(6) 0.030(3) Uiso 0.50 1 d P C 2 H37B H 0.2866 -0.0110 0.1432 0.036 Uiso 0.50 1 calc PR C 2 C38B C 0.2386(12) 0.0324(11) 0.0636(6) 0.046(3) Uiso 0.50 1 d P C 2 H38B H 0.2751 -0.0342 0.0446 0.055 Uiso 0.50 1 calc PR C 2 C39B C 0.1786(12) 0.1176(11) 0.0343(6) 0.054(3) Uiso 0.50 1 d P C 2 H39B H 0.1767 0.1076 -0.0055 0.064 Uiso 0.50 1 calc PR C 2 C40B C 0.1233(11) 0.2126(10) 0.0581(6) 0.036(3) Uiso 0.50 1 d P C 2 H40B H 0.0807 0.2705 0.0375 0.043 Uiso 0.50 1 calc PR C 2 O6 O 0.0081(3) 0.3372(2) 0.24389(14) 0.0263(7) Uani 1 1 d . . . C41 C -0.1032(4) 0.3538(4) 0.2361(2) 0.0268(11) Uani 1 1 d . . . C42 C -0.1963(4) 0.4468(4) 0.2544(2) 0.0341(12) Uani 1 1 d . . . H42 H -0.1855 0.4996 0.2716 0.041 Uiso 1 1 calc R . . C43 C -0.3084(4) 0.4630(5) 0.2473(2) 0.0418(14) Uani 1 1 d . . . H43 H -0.3738 0.5271 0.2594 0.050 Uiso 1 1 calc R . . C44 C -0.3216(5) 0.3858(5) 0.2230(2) 0.0412(15) Uani 1 1 d . . . H44 H -0.3969 0.3966 0.2183 0.049 Uiso 1 1 calc R . . C45 C -0.2280(5) 0.2924(4) 0.2050(2) 0.0386(14) Uani 1 1 d . . . H45 H -0.2388 0.2399 0.1874 0.046 Uiso 1 1 calc R . . C46 C -0.1183(4) 0.2753(4) 0.2124(2) 0.0354(13) Uani 1 1 d . . . H46 H -0.0538 0.2102 0.2014 0.042 Uiso 1 1 calc R . . P3 P 0.59202(11) 0.05121(11) 0.24559(6) 0.0309(3) Uani 1 1 d . D . O7 O 0.6790(3) -0.0031(2) 0.29150(14) 0.0257(7) Uani 1 1 d . . . C47 C 0.6769(4) 0.0516(4) 0.3394(2) 0.0235(10) Uani 1 1 d . . . C48 C 0.6918(4) -0.0003(4) 0.3907(2) 0.0363(13) Uani 1 1 d . . . H48 H 0.6980 -0.0681 0.3922 0.044 Uiso 1 1 calc R . . C49 C 0.6975(5) 0.0478(5) 0.4394(2) 0.0503(16) Uani 1 1 d . . . H49 H 0.7069 0.0134 0.4749 0.060 Uiso 1 1 calc R . . C50 C 0.6897(5) 0.1457(5) 0.4366(2) 0.0507(16) Uani 1 1 d . . . H50 H 0.6953 0.1779 0.4700 0.061 Uiso 1 1 calc R . . C51 C 0.6739(5) 0.1966(4) 0.3861(2) 0.0380(13) Uani 1 1 d . . . H51 H 0.6681 0.2642 0.3849 0.046 Uiso 1 1 calc R . . C52 C 0.6664(4) 0.1513(4) 0.3367(2) 0.0281(11) Uani 1 1 d . . . H52 H 0.6543 0.1873 0.3018 0.034 Uiso 1 1 calc R . . O8 O 0.6710(3) 0.0883(3) 0.19705(14) 0.0439(10) Uani 1 1 d . . . C53A C 0.7882(8) 0.0082(8) 0.1747(4) 0.020(2) Uiso 0.50 1 d P D 1 C54A C 0.8711(14) 0.0185(12) 0.1995(7) 0.026(4) Uiso 0.50 1 d P D 1 H54A H 0.8472 0.0652 0.2324 0.032 Uiso 0.50 1 calc PR D 1 C55A C 0.9906(12) -0.0391(10) 0.1770(6) 0.028(4) Uiso 0.50 1 d P D 1 H55A H 1.0477 -0.0346 0.1955 0.034 Uiso 0.50 1 calc PR D 1 C56A C 1.0228(9) -0.1023(8) 0.1274(4) 0.028(2) Uiso 0.50 1 d P D 1 H56A H 1.1030 -0.1409 0.1111 0.034 Uiso 0.50 1 calc PR D 1 C57A C 0.9404(9) -0.1102(8) 0.1013(5) 0.031(2) Uiso 0.50 1 d P D 1 H57A H 0.9638 -0.1540 0.0671 0.037 Uiso 0.50 1 calc PR D 1 C58A C 0.8231(8) -0.0543(8) 0.1247(4) 0.027(2) Uiso 0.50 1 d P D 1 H58A H 0.7664 -0.0591 0.1061 0.033 Uiso 0.50 1 calc PR D 1 C53B C 0.7910(8) 0.0430(8) 0.1751(4) 0.019(2) Uiso 0.50 1 d P D 2 C54B C 0.8728(13) 0.0320(11) 0.2071(7) 0.021(4) Uiso 0.50 1 d P D 2 H54B H 0.8500 0.0580 0.2467 0.025 Uiso 0.50 1 calc PR D 2 C55B C 0.9889(12) -0.0167(10) 0.1818(6) 0.025(3) Uiso 0.50 1 d P D 2 H55B H 1.0458 -0.0206 0.2034 0.030 Uiso 0.50 1 calc PR D 2 C56B C 1.0234(9) -0.0598(8) 0.1260(4) 0.028(2) Uiso 0.50 1 d P D 2 H56B H 1.1039 -0.0949 0.1094 0.033 Uiso 0.50 1 calc PR D 2 C57B C 0.9416(9) -0.0524(8) 0.0941(5) 0.034(2) Uiso 0.50 1 d P D 2 H57B H 0.9653 -0.0831 0.0555 0.041 Uiso 0.50 1 calc PR D 2 C58B C 0.8217(9) 0.0013(8) 0.1188(4) 0.030(2) Uiso 0.50 1 d P D 2 H58B H 0.7639 0.0083 0.0971 0.035 Uiso 0.50 1 calc PR D 2 O9 O 0.6197(3) -0.0599(3) 0.21826(19) 0.0577(13) Uani 1 1 d . . . C59A C 0.5830(9) -0.0554(8) 0.1585(4) 0.0197(19) Uiso 0.50 1 d P D 1 C60A C 0.5360(8) 0.0272(8) 0.1231(4) 0.028(2) Uiso 0.50 1 d P D 1 H60A H 0.5235 0.0944 0.1339 0.034 Uiso 0.50 1 calc PR D 1 C61A C 0.5090(9) 0.0071(8) 0.0725(5) 0.033(2) Uiso 0.50 1 d P D 1 H61A H 0.4774 0.0615 0.0474 0.040 Uiso 0.50 1 calc PR D 1 C62A C 0.5268(10) -0.0920(9) 0.0565(5) 0.040(3) Uiso 0.50 1 d P D 1 H62A H 0.5115 -0.1052 0.0201 0.048 Uiso 0.50 1 calc PR D 1 C63A C 0.5662(10) -0.1692(9) 0.0937(5) 0.042(3) Uiso 0.50 1 d P D 1 H63A H 0.5745 -0.2356 0.0843 0.051 Uiso 0.50 1 calc PR D 1 C64A C 0.5944(9) -0.1497(9) 0.1461(5) 0.035(2) Uiso 0.50 1 d P D 1 H64A H 0.6212 -0.2027 0.1725 0.042 Uiso 0.50 1 calc PR D 1 C59B C 0.6011(8) -0.0989(8) 0.1733(4) 0.024(2) Uiso 0.50 1 d P D 2 C60B C 0.5367(9) -0.0263(8) 0.1391(4) 0.026(2) Uiso 0.50 1 d P D 2 H60B H 0.4938 0.0437 0.1528 0.031 Uiso 0.50 1 calc PR D 2 C61B C 0.5356(10) -0.0583(9) 0.0828(5) 0.037(3) Uiso 0.50 1 d P D 2 H61B H 0.4915 -0.0093 0.0580 0.045 Uiso 0.50 1 calc PR D 2 C62B C 0.5977(10) -0.1597(9) 0.0634(6) 0.040(3) Uiso 0.50 1 d P D 2 H62B H 0.5987 -0.1803 0.0249 0.048 Uiso 0.50 1 calc PR D 2 C63B C 0.6579(10) -0.2307(9) 0.0996(5) 0.043(3) Uiso 0.50 1 d P D 2 H63B H 0.7002 -0.3007 0.0860 0.051 Uiso 0.50 1 calc PR D 2 C64B C 0.6590(9) -0.2029(8) 0.1558(4) 0.031(2) Uiso 0.50 1 d P D 2 H64B H 0.6978 -0.2531 0.1815 0.037 Uiso 0.50 1 calc PR D 2 P4 P 0.37007(10) 0.05063(10) 0.32194(6) 0.0269(3) Uani 1 1 d . . . O10 O 0.4803(3) -0.0464(2) 0.33844(16) 0.0325(8) Uani 1 1 d . . . C65 C 0.4957(4) -0.1439(4) 0.3556(2) 0.0344(12) Uani 1 1 d . . . C66 C 0.4113(4) -0.1626(4) 0.3918(2) 0.0322(12) Uani 1 1 d . . . H66 H 0.3364 -0.1081 0.4056 0.039 Uiso 1 1 calc R . . C67 C 0.4370(5) -0.2620(4) 0.4079(2) 0.0390(13) Uani 1 1 d . . . H67 H 0.3782 -0.2755 0.4318 0.047 Uiso 1 1 calc R . . C68 C 0.5453(6) -0.3413(4) 0.3900(3) 0.0577(18) Uani 1 1 d . . . H68 H 0.5624 -0.4091 0.4016 0.069 Uiso 1 1 calc R . . C69 C 0.6286(6) -0.3201(5) 0.3548(4) 0.081(3) Uani 1 1 d . . . H69 H 0.7045 -0.3741 0.3426 0.098 Uiso 1 1 calc R . . C70 C 0.6045(5) -0.2219(4) 0.3366(3) 0.063(2) Uani 1 1 d . . . H70 H 0.6625 -0.2090 0.3114 0.075 Uiso 1 1 calc R . . O11 O 0.3126(3) -0.0058(3) 0.28886(16) 0.0368(9) Uani 1 1 d . . . C71 C 0.2011(4) -0.0003(4) 0.3054(2) 0.0314(12) Uani 1 1 d . . . C72 C 0.1040(4) 0.0923(4) 0.3086(2) 0.0335(12) Uani 1 1 d . . . H72 H 0.1113 0.1540 0.3007 0.040 Uiso 1 1 calc R . . C73 C -0.0049(5) 0.0940(4) 0.3235(3) 0.0426(14) Uani 1 1 d . . . H73 H -0.0729 0.1576 0.3272 0.051 Uiso 1 1 calc R . . C74 C -0.0151(5) 0.0031(5) 0.3331(3) 0.0541(18) Uani 1 1 d . . . H74 H -0.0899 0.0045 0.3426 0.065 Uiso 1 1 calc R . . C75 C 0.0827(6) -0.0882(5) 0.3290(3) 0.0570(19) Uani 1 1 d . . . H75 H 0.0753 -0.1501 0.3360 0.068 Uiso 1 1 calc R . . C76 C 0.1921(5) -0.0916(4) 0.3148(3) 0.0418(14) Uani 1 1 d . . . H76 H 0.2600 -0.1553 0.3115 0.050 Uiso 1 1 calc R . . O12 O 0.2748(3) 0.0803(2) 0.38221(15) 0.0290(8) Uani 1 1 d . . . C77 C 0.2736(4) 0.1328(4) 0.4313(2) 0.0317(12) Uani 1 1 d . . . C78 C 0.1637(5) 0.1911(4) 0.4650(3) 0.0454(15) Uani 1 1 d . . . H78 H 0.0961 0.1953 0.4529 0.054 Uiso 1 1 calc R . . C79 C 0.1536(6) 0.2420(5) 0.5156(3) 0.0608(19) Uani 1 1 d . . . H79 H 0.0788 0.2825 0.5383 0.073 Uiso 1 1 calc R . . C80 C 0.2519(7) 0.2348(5) 0.5336(3) 0.063(2) Uani 1 1 d . . . H80 H 0.2446 0.2698 0.5691 0.076 Uiso 1 1 calc R . . C81 C 0.3622(6) 0.1761(4) 0.5000(2) 0.0451(15) Uani 1 1 d . . . H81 H 0.4300 0.1702 0.5128 0.054 Uiso 1 1 calc R . . C82 C 0.3720(5) 0.1269(4) 0.4480(2) 0.0348(12) Uani 1 1 d . . . H82 H 0.4463 0.0892 0.4240 0.042 Uiso 1 1 calc R . . C83A C 0.089(3) 0.625(3) 0.601(2) 0.14(2) Uani 0.340(10) 1 d PD E 1 H83A H 0.0321 0.6747 0.5782 0.168 Uiso 0.340(10) 1 calc PR E 1 H83B H 0.0586 0.6419 0.6431 0.168 Uiso 0.340(10) 1 calc PR E 1 Cl1A Cl 0.1244(8) 0.4967(5) 0.5812(5) 0.073(3) Uani 0.340(10) 1 d PD E 1 Cl2A Cl 0.2242(9) 0.6204(8) 0.5799(3) 0.069(3) Uani 0.340(10) 1 d PD E 1 C83B C 0.0817(12) 0.6183(11) 0.6049(5) 0.037(4) Uani 0.660(10) 1 d PD E 2 H83C H 0.0018 0.6677 0.6233 0.045 Uiso 0.660(10) 1 calc PR E 2 H83D H 0.1228 0.5799 0.6362 0.045 Uiso 0.660(10) 1 calc PR E 2 Cl1B Cl 0.0758(5) 0.5328(5) 0.55549(18) 0.0712(15) Uani 0.660(10) 1 d PD E 2 Cl2B Cl 0.1537(4) 0.6826(4) 0.56792(17) 0.0701(16) Uani 0.660(10) 1 d PD E 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 Pt 0.02916(11) 0.02970(11) 0.01612(9) 0.00159(7) -0.00195(7) -0.01937(9) Rh2 0.01394(18) 0.0277(2) 0.01850(18) -0.00428(15) -0.00057(14) -0.00896(15) Rh3 0.01350(18) 0.0300(2) 0.02173(19) -0.00685(15) -0.00010(14) -0.00888(16) S1 0.0199(6) 0.0456(7) 0.0160(6) 0.0015(5) -0.0022(5) -0.0182(6) S2 0.0169(6) 0.0242(6) 0.0229(6) -0.0034(5) 0.0018(4) -0.0101(5) C1 0.047(3) 0.031(3) 0.022(3) -0.004(2) -0.001(2) -0.022(3) C2 0.055(3) 0.031(3) 0.017(2) 0.000(2) -0.001(2) -0.027(3) C3 0.065(4) 0.038(3) 0.023(3) 0.007(2) -0.010(3) -0.030(3) C4 0.059(4) 0.031(3) 0.034(3) 0.011(2) -0.023(3) -0.027(3) C5 0.046(3) 0.033(3) 0.028(3) 0.010(2) -0.015(2) -0.028(3) C6 0.045(3) 0.044(3) 0.027(3) 0.007(2) -0.013(2) -0.034(3) C7 0.058(4) 0.034(3) 0.032(3) 0.015(2) -0.018(3) -0.028(3) C8 0.069(4) 0.027(3) 0.032(3) 0.000(2) -0.012(3) -0.023(3) P1 0.0185(6) 0.0443(8) 0.0180(6) -0.0034(6) -0.0006(5) -0.0136(6) O1 0.0234(19) 0.066(3) 0.0244(19) -0.0199(18) 0.0031(15) -0.0154(19) O2 0.0247(18) 0.053(2) 0.0228(18) 0.0009(16) -0.0017(14) -0.0215(18) C17 0.042(3) 0.057(4) 0.021(3) 0.019(2) -0.012(2) -0.038(3) C18 0.052(4) 0.051(3) 0.022(3) 0.009(2) -0.003(2) -0.035(3) C19 0.082(5) 0.050(4) 0.025(3) 0.012(3) -0.011(3) -0.041(4) C20 0.137(8) 0.079(6) 0.054(5) 0.039(4) -0.055(5) -0.083(6) C21 0.097(6) 0.101(6) 0.070(5) 0.057(5) -0.056(5) -0.084(6) C22 0.050(4) 0.082(5) 0.040(3) 0.033(3) -0.026(3) -0.048(4) O3 0.0216(18) 0.052(2) 0.0173(17) 0.0046(16) -0.0017(14) -0.0166(17) C23 0.028(3) 0.037(3) 0.023(3) 0.006(2) -0.003(2) -0.017(2) C24A 0.035(6) 0.037(6) 0.016(5) 0.008(4) -0.007(4) -0.023(5) C25A 0.032(7) 0.025(6) 0.034(7) 0.008(5) 0.008(6) 0.004(5) C27A 0.032(6) 0.040(6) 0.022(5) 0.002(4) -0.007(4) -0.012(5) C28A 0.028(5) 0.040(6) 0.028(5) 0.016(5) -0.006(4) -0.017(5) C24B 0.066(10) 0.071(10) 0.019(6) 0.011(6) -0.016(6) -0.041(8) C25B 0.086(12) 0.047(9) 0.045(9) 0.022(7) -0.041(8) -0.041(9) C27B 0.033(6) 0.038(6) 0.035(6) -0.006(5) -0.019(5) -0.006(5) C28B 0.037(6) 0.038(6) 0.034(6) 0.011(5) -0.014(5) -0.012(5) C26 0.062(4) 0.058(4) 0.018(3) 0.006(3) -0.004(3) -0.028(4) P2 0.0144(6) 0.0182(6) 0.0324(7) 0.0021(5) -0.0049(5) -0.0056(5) O4 0.0177(17) 0.0225(18) 0.052(2) 0.0101(16) -0.0012(16) -0.0041(15) C29 0.018(3) 0.013(2) 0.101(6) -0.006(3) 0.016(3) -0.005(2) O5 0.035(2) 0.0301(19) 0.036(2) 0.0094(16) -0.0196(16) -0.0176(17) C35 0.028(3) 0.042(3) 0.021(3) -0.007(2) 0.003(2) -0.022(2) O6 0.0174(16) 0.0255(17) 0.040(2) 0.0122(15) -0.0127(14) -0.0110(14) C41 0.019(2) 0.037(3) 0.031(3) 0.019(2) -0.013(2) -0.016(2) C42 0.025(3) 0.043(3) 0.037(3) 0.009(2) -0.005(2) -0.017(3) C43 0.014(3) 0.057(4) 0.049(4) 0.019(3) -0.004(2) -0.013(3) C44 0.025(3) 0.067(4) 0.046(3) 0.033(3) -0.020(2) -0.030(3) C45 0.037(3) 0.045(3) 0.053(4) 0.025(3) -0.023(3) -0.030(3) C46 0.032(3) 0.034(3) 0.050(3) 0.021(3) -0.018(2) -0.020(3) P3 0.0138(6) 0.0446(8) 0.0281(7) -0.0141(6) -0.0018(5) -0.0071(6) O7 0.0179(17) 0.0299(18) 0.0281(18) -0.0046(14) -0.0027(14) -0.0098(15) C47 0.016(2) 0.034(3) 0.020(2) -0.003(2) -0.0006(18) -0.011(2) C48 0.034(3) 0.049(3) 0.032(3) 0.012(3) -0.006(2) -0.024(3) C49 0.061(4) 0.077(5) 0.021(3) 0.014(3) -0.010(3) -0.037(4) C50 0.064(4) 0.065(4) 0.026(3) -0.010(3) -0.013(3) -0.028(4) C51 0.039(3) 0.035(3) 0.039(3) -0.010(2) -0.013(3) -0.012(3) C52 0.022(2) 0.033(3) 0.031(3) 0.003(2) -0.007(2) -0.013(2) O8 0.0124(17) 0.081(3) 0.0173(18) 0.0033(18) -0.0014(14) -0.0023(18) O9 0.019(2) 0.067(3) 0.072(3) -0.052(2) -0.009(2) -0.0010(19) P4 0.0156(6) 0.0250(6) 0.0383(8) -0.0080(6) -0.0017(5) -0.0078(5) O10 0.0179(17) 0.0275(18) 0.050(2) -0.0007(16) -0.0055(16) -0.0084(15) C65 0.028(3) 0.025(3) 0.050(3) -0.007(2) -0.009(2) -0.011(2) C66 0.030(3) 0.029(3) 0.032(3) -0.005(2) -0.008(2) -0.007(2) C67 0.043(3) 0.035(3) 0.044(3) 0.001(3) -0.015(3) -0.019(3) C68 0.054(4) 0.027(3) 0.097(6) 0.001(3) -0.026(4) -0.017(3) C69 0.043(4) 0.025(3) 0.160(8) -0.030(4) 0.009(5) -0.008(3) C70 0.028(3) 0.025(3) 0.124(6) -0.019(4) 0.011(4) -0.011(3) O11 0.0198(18) 0.033(2) 0.055(2) -0.0189(18) -0.0042(17) -0.0091(16) C71 0.025(3) 0.027(3) 0.048(3) 0.003(2) -0.015(2) -0.014(2) C72 0.028(3) 0.026(3) 0.050(3) 0.010(2) -0.012(2) -0.015(2) C73 0.026(3) 0.047(3) 0.056(4) 0.020(3) -0.018(3) -0.015(3) C74 0.038(3) 0.079(5) 0.071(4) 0.041(4) -0.031(3) -0.044(4) C75 0.069(5) 0.050(4) 0.089(5) 0.039(4) -0.054(4) -0.046(4) C76 0.050(4) 0.024(3) 0.066(4) 0.013(3) -0.038(3) -0.020(3) O12 0.0201(17) 0.0271(18) 0.039(2) -0.0055(15) 0.0024(15) -0.0126(15) C77 0.039(3) 0.024(3) 0.033(3) 0.002(2) 0.008(2) -0.020(2) C78 0.039(3) 0.033(3) 0.045(4) 0.000(3) 0.014(3) -0.007(3) C79 0.059(5) 0.053(4) 0.044(4) -0.008(3) 0.024(3) -0.013(4) C80 0.116(6) 0.033(3) 0.023(3) -0.005(3) 0.017(4) -0.029(4) C81 0.078(5) 0.051(4) 0.026(3) 0.013(3) -0.012(3) -0.046(4) C82 0.040(3) 0.031(3) 0.030(3) 0.000(2) 0.005(2) -0.017(3) C83A 0.06(3) 0.06(3) 0.29(6) -0.02(3) -0.08(3) 0.01(2) Cl1A 0.053(4) 0.058(4) 0.093(7) -0.009(4) 0.028(4) -0.026(3) Cl2A 0.056(5) 0.071(6) 0.092(5) -0.019(4) -0.006(3) -0.040(5) C83B 0.029(8) 0.050(9) 0.023(5) -0.011(5) 0.006(5) -0.012(7) Cl1B 0.080(3) 0.100(3) 0.054(2) -0.019(2) 0.0123(18) -0.067(3) Cl2B 0.055(3) 0.073(3) 0.092(2) -0.020(2) 0.0056(18) -0.042(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C6 2.190(4) . ? Pt C1 2.196(5) . ? Pt C2 2.197(5) . ? Pt C5 2.212(5) . ? Pt S1 2.3141(12) . ? Pt S2 2.3217(11) . ? Pt Rh2 3.0829(7) . ? Pt Rh3 3.0906(8) . ? Rh2 P2 2.1608(13) . ? Rh2 P1 2.1775(13) . ? Rh2 S1 2.3613(13) . ? Rh2 S2 2.3630(13) . ? Rh2 Rh3 3.0844(7) . ? Rh3 P4 2.1674(14) . ? Rh3 P3 2.1694(14) . ? Rh3 S2 2.3643(12) . ? Rh3 S1 2.3652(13) . ? C1 C2 1.391(7) . ? C1 C8 1.537(6) . ? C1 H1 0.9500 . ? C2 C3 1.499(7) . ? C2 H2 0.9500 . ? C3 C4 1.534(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.519(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.384(7) . ? C5 H5 0.9500 . ? C6 C7 1.504(7) . ? C6 H6 0.9500 . ? C7 C8 1.528(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? P1 O1 1.608(4) . ? P1 O3 1.608(3) . ? P1 O2 1.619(3) . ? O1 C11B 1.354(12) . ? O1 C11A 1.489(13) . ? C11A C16A 1.34(2) . ? C11A C12A 1.372(16) . ? C12A C13A 1.395(13) . ? C12A H12A 0.9500 . ? C13A C14A 1.344(19) . ? C13A H13A 0.9500 . ? C14A C15A 1.31(2) . ? C14A H14A 0.9500 . ? C15A C16A 1.35(2) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C11B C12B 1.389(15) . ? C11B C16B 1.39(2) . ? C12B C13B 1.374(13) . ? C12B H12B 0.9500 . ? C13B C14B 1.381(18) . ? C13B H13B 0.9500 . ? C14B C15B 1.40(2) . ? C14B H14B 0.9500 . ? C15B C16B 1.45(2) . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? O2 C17 1.380(6) . ? C17 C22 1.376(7) . ? C17 C18 1.389(8) . ? C18 C19 1.381(7) . ? C18 H18 0.9500 . ? C19 C20 1.374(9) . ? C19 H19 0.9500 . ? C20 C21 1.388(10) . ? C20 H20 0.9500 . ? C21 C22 1.389(10) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? O3 C23 1.398(5) . ? C23 C24B 1.275(14) . ? C23 C24A 1.387(10) . ? C23 C28B 1.407(12) . ? C23 C28A 1.445(11) . ? C24A C25A 1.398(16) . ? C24A H24A 0.9500 . ? C25A C26 1.213(15) . ? C25A H25A 0.9500 . ? C27A C28A 1.373(13) . ? C27A C26 1.492(11) . ? C27A H27A 0.9500 . ? C28A H28A 0.9500 . ? C24B C25B 1.441(16) . ? C24B H24B 0.9500 . ? C25B C26 1.407(14) . ? C25B H25B 0.9500 . ? C27B C28B 1.410(14) . ? C27B C26 1.411(12) . ? C27B H27B 0.9500 . ? C28B H28B 0.9500 . ? C26 H26 0.9500 . ? P2 O5 1.610(3) . ? P2 O4 1.621(3) . ? P2 O6 1.636(3) . ? O4 C29 1.404(7) . ? C29 C30B 1.137(13) . ? C29 C34A 1.295(11) . ? C29 C34B 1.534(13) . ? C29 C30A 1.625(13) . ? C30A C31A 1.395(14) . ? C30A H30A 0.9500 . ? C31A C32A 1.392(14) . ? C31A H31A 0.9500 . ? C32A C33A 1.385(15) . ? C32A H32A 0.9500 . ? C33A C34A 1.392(15) . ? C33A H33A 0.9500 . ? C34A H34A 0.9500 . ? C30B C31B 1.411(16) . ? C30B H30B 0.9500 . ? C31B C32B 1.342(16) . ? C31B H31B 0.9500 . ? C32B C33B 1.368(17) . ? C32B H32B 0.9500 . ? C33B C34B 1.405(16) . ? C33B H33B 0.9500 . ? C34B H34B 0.9500 . ? O5 C35 1.397(6) . ? C35 C36B 1.27(2) . ? C35 C40A 1.362(13) . ? C35 C40B 1.423(14) . ? C35 C36A 1.462(19) . ? C36A C37A 1.37(2) . ? C36A H36A 0.9500 . ? C37A C38A 1.408(16) . ? C37A H37A 0.9500 . ? C38A C39A 1.396(16) . ? C38A H38A 0.9500 . ? C39A C40A 1.419(17) . ? C39A H39A 0.9500 . ? C40A H40A 0.9500 . ? C36B C37B 1.42(3) . ? C36B H36B 0.9500 . ? C37B C38B 1.400(18) . ? C37B H37B 0.9500 . ? C38B C39B 1.375(19) . ? C38B H38B 0.9500 . ? C39B C40B 1.325(18) . ? C39B H39B 0.9500 . ? C40B H40B 0.9500 . ? O6 C41 1.407(5) . ? C41 C42 1.372(7) . ? C41 C46 1.383(7) . ? C42 C43 1.414(7) . ? C42 H42 0.9500 . ? C43 C44 1.360(8) . ? C43 H43 0.9500 . ? C44 C45 1.376(8) . ? C44 H44 0.9500 . ? C45 C46 1.382(7) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? P3 O9 1.614(4) . ? P3 O8 1.625(4) . ? P3 O7 1.628(3) . ? O7 C47 1.379(5) . ? C47 C48 1.386(6) . ? C47 C52 1.392(6) . ? C48 C49 1.382(8) . ? C48 H48 0.9500 . ? C49 C50 1.378(8) . ? C49 H49 0.9500 . ? C50 C51 1.366(8) . ? C50 H50 0.9500 . ? C51 C52 1.383(7) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? O8 C53B 1.400(10) . ? O8 C53A 1.463(10) . ? C53A C58A 1.375(13) . ? C53A C54A 1.378(18) . ? C54A C55A 1.41(2) . ? C54A H54A 0.9500 . ? C55A C56A 1.379(17) . ? C55A H55A 0.9500 . ? C56A C57A 1.373(14) . ? C56A H56A 0.9500 . ? C57A C58A 1.386(13) . ? C57A H57A 0.9500 . ? C58A H58A 0.9500 . ? C53B C54B 1.359(18) . ? C53B C58B 1.374(14) . ? C54B C55B 1.38(2) . ? C54B H54B 0.9500 . ? C55B C56B 1.367(17) . ? C55B H55B 0.9500 . ? C56B C57B 1.372(14) . ? C56B H56B 0.9500 . ? C57B C58B 1.417(14) . ? C57B H57B 0.9500 . ? C58B H58B 0.9500 . ? O9 C59B 1.313(10) . ? O9 C59A 1.542(11) . ? C59A C64A 1.344(14) . ? C59A C60A 1.401(14) . ? C60A C61A 1.363(14) . ? C60A H60A 0.9500 . ? C61A C62A 1.403(15) . ? C61A H61A 0.9500 . ? C62A C63A 1.363(16) . ? C62A H62A 0.9500 . ? C63A C64A 1.408(15) . ? C63A H63A 0.9500 . ? C64A H64A 0.9500 . ? C59B C60B 1.363(14) . ? C59B C64B 1.393(14) . ? C60B C61B 1.409(15) . ? C60B H60B 0.9500 . ? C61B C62B 1.373(16) . ? C61B H61B 0.9500 . ? C62B C63B 1.364(16) . ? C62B H62B 0.9500 . ? C63B C64B 1.384(15) . ? C63B H63B 0.9500 . ? C64B H64B 0.9500 . ? P4 O10 1.606(3) . ? P4 O11 1.617(3) . ? P4 O12 1.619(3) . ? O10 C65 1.393(6) . ? C65 C70 1.370(7) . ? C65 C66 1.379(7) . ? C66 C67 1.384(7) . ? C66 H66 0.9500 . ? C67 C68 1.369(8) . ? C67 H67 0.9500 . ? C68 C69 1.375(9) . ? C68 H68 0.9500 . ? C69 C70 1.386(9) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? O11 C71 1.398(5) . ? C71 C72 1.374(7) . ? C71 C76 1.387(6) . ? C72 C73 1.386(7) . ? C72 H72 0.9500 . ? C73 C74 1.388(8) . ? C73 H73 0.9500 . ? C74 C75 1.366(8) . ? C74 H74 0.9500 . ? C75 C76 1.382(8) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? O12 C77 1.388(6) . ? C77 C82 1.372(7) . ? C77 C78 1.395(7) . ? C78 C79 1.364(9) . ? C78 H78 0.9500 . ? C79 C80 1.379(10) . ? C79 H79 0.9500 . ? C80 C81 1.399(9) . ? C80 H80 0.9500 . ? C81 C82 1.383(7) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83A Cl2A 1.71(3) . ? C83A Cl1A 1.76(4) . ? C83A H83A 0.9900 . ? C83A H83B 0.9900 . ? C83B Cl2B 1.705(13) . ? C83B Cl1B 1.754(13) . ? C83B H83C 0.9900 . ? C83B H83D 0.9900 . ? 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 C6 Pt C1 81.30(19) . . ? C6 Pt C2 96.86(18) . . ? C1 Pt C2 36.93(18) . . ? C6 Pt C5 36.64(17) . . ? C1 Pt C5 88.2(2) . . ? C2 Pt C5 81.16(18) . . ? C6 Pt S1 94.69(14) . . ? C1 Pt S1 166.73(14) . . ? C2 Pt S1 156.19(14) . . ? C5 Pt S1 96.17(14) . . ? C6 Pt S2 156.75(14) . . ? C1 Pt S2 96.09(13) . . ? C2 Pt S2 94.53(13) . . ? C5 Pt S2 166.47(13) . . ? S1 Pt S2 82.57(4) . . ? C6 Pt Rh2 112.31(13) . . ? C1 Pt Rh2 120.49(14) . . ? C2 Pt Rh2 140.69(13) . . ? C5 Pt Rh2 137.61(12) . . ? S1 Pt Rh2 49.41(3) . . ? S2 Pt Rh2 49.43(3) . . ? C6 Pt Rh3 140.65(14) . . ? C1 Pt Rh3 137.42(12) . . ? C2 Pt Rh3 111.88(13) . . ? C5 Pt Rh3 120.45(14) . . ? S1 Pt Rh3 49.38(3) . . ? S2 Pt Rh3 49.33(3) . . ? Rh2 Pt Rh3 59.949(12) . . ? P2 Rh2 P1 91.96(5) . . ? P2 Rh2 S1 176.14(5) . . ? P1 Rh2 S1 91.58(4) . . ? P2 Rh2 S2 95.79(4) . . ? P1 Rh2 S2 172.23(4) . . ? S1 Rh2 S2 80.70(4) . . ? P2 Rh2 Pt 130.19(4) . . ? P1 Rh2 Pt 125.16(4) . . ? S1 Rh2 Pt 48.09(3) . . ? S2 Rh2 Pt 48.27(3) . . ? P2 Rh2 Rh3 127.01(4) . . ? P1 Rh2 Rh3 125.42(4) . . ? S1 Rh2 Rh3 49.32(3) . . ? S2 Rh2 Rh3 49.29(3) . . ? Pt Rh2 Rh3 60.149(17) . . ? P4 Rh3 P3 91.42(5) . . ? P4 Rh3 S2 91.95(5) . . ? P3 Rh3 S2 176.57(5) . . ? P4 Rh3 S1 172.47(5) . . ? P3 Rh3 S1 96.05(5) . . ? S2 Rh3 S1 80.59(4) . . ? P4 Rh3 Rh2 125.78(4) . . ? P3 Rh3 Rh2 127.81(4) . . ? S2 Rh3 Rh2 49.25(3) . . ? S1 Rh3 Rh2 49.21(3) . . ? P4 Rh3 Pt 125.61(4) . . ? P3 Rh3 Pt 129.67(4) . . ? S2 Rh3 Pt 48.14(3) . . ? S1 Rh3 Pt 47.96(3) . . ? Rh2 Rh3 Pt 59.902(17) . . ? Pt S1 Rh2 82.50(4) . . ? Pt S1 Rh3 82.66(4) . . ? Rh2 S1 Rh3 81.47(4) . . ? Pt S2 Rh2 82.30(4) . . ? Pt S2 Rh3 82.52(4) . . ? Rh2 S2 Rh3 81.45(4) . . ? C2 C1 C8 124.4(5) . . ? C2 C1 Pt 71.6(3) . . ? C8 C1 Pt 111.9(3) . . ? C2 C1 H1 117.8 . . ? C8 C1 H1 117.8 . . ? Pt C1 H1 86.5 . . ? C1 C2 C3 126.1(4) . . ? C1 C2 Pt 71.5(3) . . ? C3 C2 Pt 107.5(3) . . ? C1 C2 H2 117.0 . . ? C3 C2 H2 117.0 . . ? Pt C2 H2 91.1 . . ? C2 C3 C4 114.0(4) . . ? C2 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? C2 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 112.5(4) . . ? C5 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? C5 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C4 123.7(5) . . ? C6 C5 Pt 70.8(3) . . ? C4 C5 Pt 111.2(3) . . ? C6 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? Pt C5 H5 88.0 . . ? C5 C6 C7 125.7(5) . . ? C5 C6 Pt 72.5(3) . . ? C7 C6 Pt 107.6(3) . . ? C5 C6 H6 117.2 . . ? C7 C6 H6 117.2 . . ? Pt C6 H6 89.9 . . ? C6 C7 C8 115.0(4) . . ? C6 C7 H7A 108.5 . . ? C8 C7 H7A 108.5 . . ? C6 C7 H7B 108.5 . . ? C8 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C7 C8 C1 111.7(4) . . ? C7 C8 H8A 109.3 . . ? C1 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C1 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? O1 P1 O3 101.33(19) . . ? O1 P1 O2 95.60(19) . . ? O3 P1 O2 103.45(18) . . ? O1 P1 Rh2 119.29(16) . . ? O3 P1 Rh2 113.32(12) . . ? O2 P1 Rh2 120.63(13) . . ? C11B O1 P1 130.7(6) . . ? C11A O1 P1 121.4(5) . . ? C16A C11A C12A 122.0(13) . . ? C16A C11A O1 120.2(12) . . ? C12A C11A O1 117.3(10) . . ? C11A C12A C13A 118.1(10) . . ? C11A C12A H12A 121.0 . . ? C13A C12A H12A 121.0 . . ? C14A C13A C12A 121.7(12) . . ? C14A C13A H13A 119.1 . . ? C12A C13A H13A 119.1 . . ? C15A C14A C13A 112.2(15) . . ? C15A C14A H14A 123.9 . . ? C13A C14A H14A 123.9 . . ? C14A C15A C16A 130.4(17) . . ? C14A C15A H15A 114.8 . . ? C16A C15A H15A 114.8 . . ? C11A C16A C15A 112.2(17) . . ? C11A C16A H16A 123.9 . . ? C15A C16A H16A 123.9 . . ? O1 C11B C12B 124.3(10) . . ? O1 C11B C16B 115.8(12) . . ? C12B C11B C16B 119.8(12) . . ? C13B C12B C11B 119.0(10) . . ? C13B C12B H12B 120.5 . . ? C11B C12B H12B 120.5 . . ? C12B C13B C14B 120.6(11) . . ? C12B C13B H13B 119.7 . . ? C14B C13B H13B 119.7 . . ? C13B C14B C15B 122.3(14) . . ? C13B C14B H14B 118.9 . . ? C15B C14B H14B 118.9 . . ? C14B C15B C16B 112.5(15) . . ? C14B C15B H15B 123.8 . . ? C16B C15B H15B 123.8 . . ? C11B C16B C15B 121.2(16) . . ? C11B C16B H16B 119.4 . . ? C15B C16B H16B 119.4 . . ? C17 O2 P1 128.9(3) . . ? C22 C17 O2 115.6(5) . . ? C22 C17 C18 120.7(6) . . ? O2 C17 C18 123.5(4) . . ? C19 C18 C17 119.2(5) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C20 C19 C18 120.4(7) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 120.4(7) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C22 119.3(6) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C17 C22 C21 119.8(7) . . ? C17 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C23 O3 P1 129.4(3) . . ? C24B C23 O3 114.9(7) . . ? C24A C23 O3 128.3(6) . . ? C24B C23 C28B 127.0(8) . . ? C24A C23 C28B 99.9(7) . . ? O3 C23 C28B 118.0(6) . . ? C24B C23 C28A 104.3(8) . . ? C24A C23 C28A 116.3(7) . . ? O3 C23 C28A 113.8(5) . . ? C28B C23 C28A 56.4(6) . . ? C23 C24A C25A 121.3(10) . . ? C23 C24A H24A 119.3 . . ? C25A C24A H24A 119.3 . . ? C26 C25A C24A 121.5(11) . . ? C26 C25A H25A 119.2 . . ? C24A C25A H25A 119.2 . . ? C28A C27A C26 115.8(9) . . ? C28A C27A H27A 122.1 . . ? C26 C27A H27A 122.1 . . ? C27A C28A C23 120.5(8) . . ? C27A C28A H28A 119.7 . . ? C23 C28A H28A 119.7 . . ? C23 C24B C25B 116.2(11) . . ? C23 C24B H24B 121.9 . . ? C25B C24B H24B 121.9 . . ? C26 C25B C24B 122.2(11) . . ? C26 C25B H25B 118.9 . . ? C24B C25B H25B 118.9 . . ? C28B C27B C26 121.7(9) . . ? C28B C27B H27B 119.1 . . ? C26 C27B H27B 119.1 . . ? C23 C28B C27B 115.3(9) . . ? C23 C28B H28B 122.4 . . ? C27B C28B H28B 122.4 . . ? C25A C26 C27B 98.6(8) . . ? C25B C26 C27B 114.6(8) . . ? C25A C26 C27A 123.3(8) . . ? C25B C26 C27A 102.1(8) . . ? C27B C26 C27A 57.8(6) . . ? C25A C26 H26 118.4 . . ? C25B C26 H26 128.3 . . ? C27B C26 H26 113.9 . . ? C27A C26 H26 118.4 . . ? O5 P2 O4 91.55(19) . . ? O5 P2 O6 101.20(17) . . ? O4 P2 O6 101.42(16) . . ? O5 P2 Rh2 121.74(14) . . ? O4 P2 Rh2 120.08(13) . . ? O6 P2 Rh2 116.24(13) . . ? C29 O4 P2 122.4(4) . . ? C30B C29 C34A 103.3(9) . . ? C30B C29 O4 128.1(8) . . ? C34A C29 O4 128.6(8) . . ? C30B C29 C34B 127.9(9) . . ? O4 C29 C34B 103.7(7) . . ? C34A C29 C30A 111.5(8) . . ? O4 C29 C30A 120.0(5) . . ? C34B C29 C30A 136.3(7) . . ? C31A C30A C29 117.9(9) . . ? C31A C30A H30A 121.0 . . ? C29 C30A H30A 121.0 . . ? C32A C31A C30A 122.0(11) . . ? C32A C31A H31A 119.0 . . ? C30A C31A H31A 119.0 . . ? C33A C32A C31A 119.4(10) . . ? C33A C32A H32A 120.3 . . ? C31A C32A H32A 120.3 . . ? C32A C33A C34A 119.5(10) . . ? C32A C33A H33A 120.2 . . ? C34A C33A H33A 120.2 . . ? C29 C34A C33A 129.5(11) . . ? C29 C34A H34A 115.3 . . ? C33A C34A H34A 115.3 . . ? C29 C30B C31B 119.3(12) . . ? C29 C30B H30B 120.4 . . ? C31B C30B H30B 120.4 . . ? C32B C31B C30B 120.6(13) . . ? C32B C31B H31B 119.7 . . ? C30B C31B H31B 119.7 . . ? C31B C32B C33B 120.9(12) . . ? C31B C32B H32B 119.6 . . ? C33B C32B H32B 119.6 . . ? C32B C33B C34B 120.5(12) . . ? C32B C33B H33B 119.7 . . ? C34B C33B H33B 119.7 . . ? C33B C34B C29 110.7(10) . . ? C33B C34B H34B 124.7 . . ? C29 C34B H34B 124.7 . . ? C35 O5 P2 124.0(3) . . ? C36B C35 C40A 112.1(12) . . ? C36B C35 O5 125.2(11) . . ? C40A C35 O5 121.9(7) . . ? C36B C35 C40B 128.2(12) . . ? O5 C35 C40B 106.6(7) . . ? C40A C35 C36A 114.7(10) . . ? O5 C35 C36A 123.3(8) . . ? C40B C35 C36A 129.6(10) . . ? C37A C36A C35 124.0(15) . . ? C37A C36A H36A 118.0 . . ? C35 C36A H36A 118.0 . . ? C36A C37A C38A 118.0(13) . . ? C36A C37A H37A 121.0 . . ? C38A C37A H37A 121.0 . . ? C39A C38A C37A 120.8(10) . . ? C39A C38A H38A 119.6 . . ? C37A C38A H38A 119.6 . . ? C38A C39A C40A 118.7(11) . . ? C38A C39A H39A 120.6 . . ? C40A C39A H39A 120.6 . . ? C35 C40A C39A 123.8(11) . . ? C35 C40A H40A 118.1 . . ? C39A C40A H40A 118.1 . . ? C35 C36B C37B 116.7(17) . . ? C35 C36B H36B 121.6 . . ? C37B C36B H36B 121.6 . . ? C38B C37B C36B 118.8(14) . . ? C38B C37B H37B 120.6 . . ? C36B C37B H37B 120.6 . . ? C39B C38B C37B 118.5(13) . . ? C39B C38B H38B 120.7 . . ? C37B C38B H38B 120.7 . . ? C40B C39B C38B 124.4(14) . . ? C40B C39B H39B 117.8 . . ? C38B C39B H39B 117.8 . . ? C39B C40B C35 113.4(12) . . ? C39B C40B H40B 123.3 . . ? C35 C40B H40B 123.3 . . ? C41 O6 P2 119.6(3) . . ? C42 C41 C46 121.0(5) . . ? C42 C41 O6 119.0(4) . . ? C46 C41 O6 120.0(4) . . ? C41 C42 C43 119.1(5) . . ? C41 C42 H42 120.5 . . ? C43 C42 H42 120.5 . . ? C44 C43 C42 119.3(5) . . ? C44 C43 H43 120.4 . . ? C42 C43 H43 120.4 . . ? C43 C44 C45 121.4(5) . . ? C43 C44 H44 119.3 . . ? C45 C44 H44 119.3 . . ? C44 C45 C46 119.8(5) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C45 C46 C41 119.5(5) . . ? C45 C46 H46 120.3 . . ? C41 C46 H46 120.3 . . ? O9 P3 O8 102.5(2) . . ? O9 P3 O7 90.7(2) . . ? O8 P3 O7 101.71(17) . . ? O9 P3 Rh3 121.60(14) . . ? O8 P3 Rh3 116.00(15) . . ? O7 P3 Rh3 119.83(13) . . ? C47 O7 P3 121.3(3) . . ? O7 C47 C48 116.1(4) . . ? O7 C47 C52 122.8(4) . . ? C48 C47 C52 121.1(5) . . ? C49 C48 C47 119.1(5) . . ? C49 C48 H48 120.5 . . ? C47 C48 H48 120.5 . . ? C50 C49 C48 120.1(5) . . ? C50 C49 H49 119.9 . . ? C48 C49 H49 119.9 . . ? C51 C50 C49 120.3(5) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C50 C51 C52 121.1(5) . . ? C50 C51 H51 119.5 . . ? C52 C51 H51 119.5 . . ? C51 C52 C47 118.2(5) . . ? C51 C52 H52 120.9 . . ? C47 C52 H52 120.9 . . ? C53B O8 P3 131.1(5) . . ? C53A O8 P3 114.5(5) . . ? C58A C53A C54A 119.1(10) . . ? C58A C53A O8 126.7(8) . . ? C54A C53A O8 112.0(10) . . ? C53A C54A C55A 121.0(13) . . ? C53A C54A H54A 119.5 . . ? C55A C54A H54A 119.5 . . ? C56A C55A C54A 118.3(13) . . ? C56A C55A H55A 120.9 . . ? C54A C55A H55A 120.9 . . ? C57A C56A C55A 120.8(11) . . ? C57A C56A H56A 119.6 . . ? C55A C56A H56A 119.6 . . ? C56A C57A C58A 120.1(10) . . ? C56A C57A H57A 120.0 . . ? C58A C57A H57A 120.0 . . ? C53A C58A C57A 120.5(9) . . ? C53A C58A H58A 119.7 . . ? C57A C58A H58A 119.7 . . ? C54B C53B C58B 121.4(11) . . ? C54B C53B O8 124.3(9) . . ? C58B C53B O8 114.1(8) . . ? C53B C54B C55B 119.7(13) . . ? C53B C54B H54B 120.2 . . ? C55B C54B H54B 120.2 . . ? C56B C55B C54B 120.8(13) . . ? C56B C55B H55B 119.6 . . ? C54B C55B H55B 119.6 . . ? C55B C56B C57B 119.9(11) . . ? C55B C56B H56B 120.0 . . ? C57B C56B H56B 120.0 . . ? C56B C57B C58B 119.7(10) . . ? C56B C57B H57B 120.1 . . ? C58B C57B H57B 120.1 . . ? C53B C58B C57B 118.3(10) . . ? C53B C58B H58B 120.8 . . ? C57B C58B H58B 120.8 . . ? C59B O9 P3 139.0(6) . . ? C59A O9 P3 113.5(5) . . ? C64A C59A C60A 122.5(10) . . ? C64A C59A O9 106.3(9) . . ? C60A C59A O9 131.0(8) . . ? C61A C60A C59A 117.2(10) . . ? C61A C60A H60A 121.4 . . ? C59A C60A H60A 121.4 . . ? C60A C61A C62A 121.5(11) . . ? C60A C61A H61A 119.2 . . ? C62A C61A H61A 119.2 . . ? C63A C62A C61A 119.6(12) . . ? C63A C62A H62A 120.2 . . ? C61A C62A H62A 120.2 . . ? C62A C63A C64A 119.4(11) . . ? C62A C63A H63A 120.3 . . ? C64A C63A H63A 120.3 . . ? C59A C64A C63A 119.4(11) . . ? C59A C64A H64A 120.3 . . ? C63A C64A H64A 120.3 . . ? O9 C59B C60B 113.4(9) . . ? O9 C59B C64B 123.3(9) . . ? C60B C59B C64B 122.2(9) . . ? C59B C60B C61B 118.0(10) . . ? C59B C60B H60B 121.0 . . ? C61B C60B H60B 121.0 . . ? C62B C61B C60B 120.5(11) . . ? C62B C61B H61B 119.7 . . ? C60B C61B H61B 119.7 . . ? C63B C62B C61B 119.8(12) . . ? C63B C62B H62B 120.1 . . ? C61B C62B H62B 120.1 . . ? C62B C63B C64B 121.5(11) . . ? C62B C63B H63B 119.2 . . ? C64B C63B H63B 119.2 . . ? C63B C64B C59B 117.7(10) . . ? C63B C64B H64B 121.1 . . ? C59B C64B H64B 121.1 . . ? O10 P4 O11 101.09(18) . . ? O10 P4 O12 103.03(19) . . ? O11 P4 O12 95.79(17) . . ? O10 P4 Rh3 113.25(13) . . ? O11 P4 Rh3 119.42(16) . . ? O12 P4 Rh3 120.93(13) . . ? C65 O10 P4 132.1(3) . . ? C70 C65 C66 120.6(5) . . ? C70 C65 O10 115.5(5) . . ? C66 C65 O10 123.7(4) . . ? C65 C66 C67 119.1(5) . . ? C65 C66 H66 120.5 . . ? C67 C66 H66 120.5 . . ? C68 C67 C66 121.5(5) . . ? C68 C67 H67 119.3 . . ? C66 C67 H67 119.3 . . ? C67 C68 C69 118.2(6) . . ? C67 C68 H68 120.9 . . ? C69 C68 H68 120.9 . . ? C68 C69 C70 121.6(6) . . ? C68 C69 H69 119.2 . . ? C70 C69 H69 119.2 . . ? C65 C70 C69 118.9(6) . . ? C65 C70 H70 120.6 . . ? C69 C70 H70 120.6 . . ? C71 O11 P4 127.0(3) . . ? C72 C71 C76 121.4(5) . . ? C72 C71 O11 120.6(4) . . ? C76 C71 O11 117.9(5) . . ? C71 C72 C73 118.8(5) . . ? C71 C72 H72 120.6 . . ? C73 C72 H72 120.6 . . ? C72 C73 C74 120.3(5) . . ? C72 C73 H73 119.9 . . ? C74 C73 H73 119.9 . . ? C75 C74 C73 119.9(5) . . ? C75 C74 H74 120.0 . . ? C73 C74 H74 120.0 . . ? C74 C75 C76 120.8(5) . . ? C74 C75 H75 119.6 . . ? C76 C75 H75 119.6 . . ? C75 C76 C71 118.8(5) . . ? C75 C76 H76 120.6 . . ? C71 C76 H76 120.6 . . ? C77 O12 P4 125.8(3) . . ? C82 C77 O12 123.9(4) . . ? C82 C77 C78 120.8(5) . . ? O12 C77 C78 115.3(5) . . ? C79 C78 C77 119.8(6) . . ? C79 C78 H78 120.1 . . ? C77 C78 H78 120.1 . . ? C78 C79 C80 120.0(6) . . ? C78 C79 H79 120.0 . . ? C80 C79 H79 120.0 . . ? C79 C80 C81 120.3(6) . . ? C79 C80 H80 119.9 . . ? C81 C80 H80 119.9 . . ? C82 C81 C80 119.5(6) . . ? C82 C81 H81 120.2 . . ? C80 C81 H81 120.2 . . ? C77 C82 C81 119.5(5) . . ? C77 C82 H82 120.2 . . ? C81 C82 H82 120.2 . . ? Cl2A C83A Cl1A 98.5(18) . . ? Cl2A C83A H83A 112.1 . . ? Cl1A C83A H83A 112.1 . . ? Cl2A C83A H83B 112.1 . . ? Cl1A C83A H83B 112.1 . . ? H83A C83A H83B 109.7 . . ? Cl2B C83B Cl1B 108.9(6) . . ? Cl2B C83B H83C 109.9 . . ? Cl1B C83B H83C 109.9 . . ? Cl2B C83B H83D 109.9 . . ? Cl1B C83B H83D 109.9 . . ? H83C C83B H83D 108.3 . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.348 _refine_diff_density_min -0.937 _refine_diff_density_rms 0.129 data_compnd_9 _database_code_depnum_ccdc_archive 'CCDC 908508' #TrackingRef '15071_web_deposit_cif_file_0_FernandoJ.Lahoz_1351623726.compnd_3_6_7_9_11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H42 O2 P2 Pt Rh2 S2, C H2 Cl2' _chemical_formula_sum 'C47 H44 Cl2 O2 P2 Pt Rh2 S2' _chemical_formula_weight 1238.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.1580 0.1710 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0120 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1090 0.1020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.9660 8.9300 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -0.9980 0.9850 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1330 0.1340 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.5720(10) _cell_length_b 9.4620(5) _cell_length_c 21.3660(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.623(5) _cell_angle_gamma 90.00 _cell_volume 4434.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 23463 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 27.92 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.078 _exptl_crystal_size_mid 0.0325 _exptl_crystal_size_min 0.0195 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 4.430 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.892 _exptl_absorpt_correction_T_max 1.391 _exptl_absorpt_process_details ; R. H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38. ; _exptl_special_details ; Data was collected in BM16 line in ESRF synchrotron, Grenoble (France) ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.73820 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator 'A Si111 double-crystal' _diffrn_measurement_device_type 'Single-axis HUBER diffractometer' _diffrn_measurement_method 'fi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23463 _diffrn_reflns_av_R_equivalents 0.0773 _diffrn_reflns_av_sigmaI/netI 0.0797 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 28.16 _reflns_number_total 4729 _reflns_number_gt 4649 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Z. Otwinowski)' _computing_cell_refinement 'HKL2000(Z. Otwinowski and W. Minor,1997)' _computing_data_reduction 'HKL2000(Z. Otwinowski and W. Minor,1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (L. Farrugia, 1997) ' _computing_publication_material 'WingX (L. Farrugia, 1999)' _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. Hydrogens have been introduced in the model in calculated positions and refined with a riding model. ; _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^)+(0.0185P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4729 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl07e in C 2/c CELL 0.73820 22.5720 9.4620 21.3660 90.000 103.623 90.000 ZERR 4.00 0.0010 0.0005 0.0010 0.000 0.005 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C 2.31000 20.84392 1.02000 10.20751 1.58860 0.56870 = 0.86500 51.65125 0.21560 0.003 0.002 7.305 0.770 12.011 SFAC H 0.49300 10.51091 0.32291 26.12573 0.14019 3.14236 = 0.04081 57.79977 0.00304 0.000 0.000 0.000 0.320 1.008 SFAC CL 11.46041 0.01040 7.19641 1.16620 6.25561 18.51942 = 1.64550 47.77846 -9.55741 0.158 0.171 713.191 0.990 35.453 SFAC O 3.04850 13.27711 2.28680 5.70111 1.54630 0.32390 = 0.86700 32.90894 0.25080 0.012 0.007 27.408 0.660 15.999 SFAC P 6.43451 1.90670 4.17910 27.15704 1.78000 0.52600 = 1.49080 68.16457 1.11490 0.109 0.102 424.796 1.100 30.974 SFAC PT 27.00594 1.51293 17.76392 8.81175 15.71312 0.42459 = 5.78371 38.61034 11.68831 -1.966 8.930 37139.754 1.380 195.080 SFAC RH 19.29572 0.75154 14.35011 8.21759 4.73425 25.87494 = 1.28918 98.60629 5.32800 -0.998 0.985 4096.329 1.390 102.906 SFAC S 6.90531 1.46790 5.20341 22.21512 1.43790 0.25360 = 1.58630 56.17207 0.86690 0.133 0.134 555.873 1.040 32.066 UNIT 188 176 8 8 8 4 8 8 MERG 2 FMAP 2 PLAN 15 SIZE 0.078 0.0325 0.0195 TEMP -173 BOND $H ACTA 53 CONF LIST 1 WPDB -2 L.S. 6 WGHT 0.018500 FVAR 0.34976 PT 6 0.500000 -0.050380 0.250000 10.50000 0.00816 0.00692 = 0.00681 0.00000 0.00076 0.00000 RH2 7 0.429529 0.227701 0.241040 11.00000 0.00732 0.00718 = 0.00522 -0.00133 0.00028 -0.00035 S1 8 0.507859 0.132364 0.323332 11.00000 0.01016 0.00974 = 0.00509 -0.00025 -0.00012 -0.00133 P2 5 0.356457 0.265606 0.150617 11.00000 0.00701 0.00781 = 0.00747 -0.00116 0.00038 -0.00001 C1 1 0.464797 -0.216325 0.178994 11.00000 0.02265 0.01163 = 0.01070 -0.00635 0.00400 -0.00262 AFIX 13 H1 2 0.439482 -0.180178 0.137216 11.00000 -1.20000 AFIX 0 C2 1 0.527447 -0.202771 0.185414 11.00000 0.02143 0.01301 = 0.01207 -0.00389 0.00764 0.00113 AFIX 13 H2 2 0.538989 -0.159352 0.147294 11.00000 -1.20000 AFIX 0 C3 1 0.576396 -0.295467 0.226082 11.00000 0.03177 0.01614 = 0.02399 0.00180 0.01582 0.01133 AFIX 23 H3A 2 0.615987 -0.245671 0.233049 11.00000 -1.20000 H3B 2 0.579645 -0.383354 0.201970 11.00000 -1.20000 AFIX 0 C4 1 0.564818 -0.334699 0.291404 11.00000 0.02544 0.01644 = 0.02031 0.00317 0.00632 0.00737 AFIX 23 H4A 2 0.538170 -0.419071 0.286278 11.00000 -1.20000 H4B 2 0.604065 -0.359872 0.321144 11.00000 -1.20000 AFIX 0 C5 1 0.387028 0.303361 0.296623 11.00000 0.01250 0.01386 = 0.01537 -0.00004 0.00328 -0.00057 O1 4 0.361594 0.350154 0.332065 11.00000 0.02989 0.03169 = 0.01821 -0.00749 0.01261 0.00302 C6 1 0.282926 0.341793 0.156022 11.00000 0.01407 0.01064 = 0.01006 0.00053 0.00611 0.00132 C7 1 0.282584 0.467455 0.189826 11.00000 0.01750 0.01175 = 0.01898 -0.00031 0.00822 -0.00212 AFIX 43 H7 2 0.320120 0.508584 0.211813 11.00000 -1.20000 AFIX 0 C8 1 0.228446 0.533123 0.191834 11.00000 0.02301 0.01122 = 0.02497 -0.00051 0.01363 0.00276 AFIX 43 H8 2 0.228907 0.619114 0.214895 11.00000 -1.20000 AFIX 0 C9 1 0.173001 0.473157 0.159968 11.00000 0.01503 0.02322 = 0.02246 0.00427 0.01042 0.00584 AFIX 43 H9 2 0.135654 0.518009 0.161261 11.00000 -1.20000 AFIX 0 C10 1 0.172874 0.347842 0.126476 11.00000 0.01221 0.02947 = 0.02459 -0.00492 0.00580 0.00234 AFIX 43 H10 2 0.135304 0.306369 0.104811 11.00000 -1.20000 AFIX 0 C11 1 0.227510 0.282593 0.124461 11.00000 0.01352 0.02273 = 0.01470 -0.00487 0.00252 0.00091 AFIX 43 H11 2 0.227039 0.196720 0.101311 11.00000 -1.20000 AFIX 0 C12 1 0.374689 0.375477 0.087141 11.00000 0.01143 0.00734 = 0.01022 -0.00221 0.00210 0.00037 C13 1 0.330010 0.413203 0.032300 11.00000 0.01049 0.01526 = 0.01310 -0.00003 -0.00259 0.00103 AFIX 43 H13 2 0.289546 0.379043 0.026936 11.00000 -1.20000 AFIX 0 C14 1 0.344453 0.500194 -0.014284 11.00000 0.02374 0.01755 = 0.00970 0.00250 -0.00210 0.00056 AFIX 43 H14 2 0.313941 0.524520 -0.051533 11.00000 -1.20000 AFIX 0 C15 1 0.403377 0.551850 -0.006651 11.00000 0.02370 0.01974 = 0.01173 0.00410 0.00691 0.00253 AFIX 43 H15 2 0.413321 0.610974 -0.038632 11.00000 -1.20000 AFIX 0 C16 1 0.447558 0.516306 0.048097 11.00000 0.01435 0.01562 = 0.01620 0.00134 0.00575 -0.00061 AFIX 43 H16 2 0.487628 0.553196 0.053886 11.00000 -1.20000 AFIX 0 C17 1 0.433969 0.427791 0.094364 11.00000 0.01260 0.01376 = 0.01128 -0.00110 0.00236 0.00079 AFIX 43 H17 2 0.464903 0.402471 0.131087 11.00000 -1.20000 AFIX 0 C18 1 0.334866 0.093039 0.112804 11.00000 0.00678 0.01044 = 0.01199 -0.00249 -0.00152 0.00161 C19 1 0.340284 0.057286 0.051602 11.00000 0.02025 0.01745 = 0.01648 -0.00563 0.00553 -0.00196 AFIX 43 H19 2 0.353392 0.125866 0.025309 11.00000 -1.20000 AFIX 0 C20 1 0.326361 -0.080658 0.028421 11.00000 0.02594 0.02194 = 0.02012 -0.01183 0.00243 -0.00140 AFIX 43 H20 2 0.330131 -0.105144 -0.013588 11.00000 -1.20000 AFIX 0 C21 1 0.307315 -0.180378 0.066187 11.00000 0.02134 0.01429 = 0.03168 -0.00934 -0.00153 -0.00490 AFIX 43 H21 2 0.298254 -0.273663 0.050376 11.00000 -1.20000 AFIX 0 C22 1 0.301297 -0.144657 0.127649 11.00000 0.02634 0.01375 = 0.02748 0.00375 -0.00079 -0.00603 AFIX 43 H22 2 0.287302 -0.212868 0.153459 11.00000 -1.20000 AFIX 0 C23 1 0.315792 -0.009356 0.150974 11.00000 0.02396 0.01497 = 0.01522 -0.00158 0.00377 -0.00343 AFIX 43 H23 2 0.312745 0.014120 0.193333 11.00000 -1.20000 AFIX 0 C24 1 0.473001 -0.022793 1.004875 10.50000 0.02555 0.03686 = 0.05718 0.01541 0.00161 -0.00241 AFIX 23 H24A 2 0.463768 0.012642 1.045131 10.50000 -1.20000 H24B 2 0.438064 -0.008248 0.967568 10.50000 -1.20000 AFIX 0 CL1A 3 0.506972 0.138120 0.991124 10.50000 0.10192 0.02418 = 0.04049 -0.00035 0.02718 -0.00978 CL1B 3 0.520584 -0.165885 1.006303 10.50000 0.03440 0.02933 = 0.02779 0.00451 0.01332 0.00249 HKLF 4 REM fjl07e in C 2/c REM R1 = 0.0332 for 4649 Fo > 4sig(Fo) and 0.0335 for all 4729 data REM 276 parameters refined using 0 restraints END WGHT 0.0177 0.0000 REM Highest difference peak 1.400, deepest hole -2.055, 1-sigma level 0.202 Q1 1 0.5280 -0.1591 0.2404 11.00000 0.05 1.40 Q2 1 0.5302 0.0629 0.2365 11.00000 0.05 1.12 Q3 1 0.5185 -0.0550 0.2013 11.00000 0.05 0.92 Q4 1 0.4516 0.1126 0.2261 11.00000 0.05 0.83 Q5 1 0.3903 0.1363 0.2441 11.00000 0.05 0.82 Q6 1 0.4660 0.4467 0.1488 11.00000 0.05 0.82 Q7 1 0.4786 0.1739 0.2732 11.00000 0.05 0.81 Q8 1 0.3197 -0.2397 0.0623 11.00000 0.05 0.80 Q9 1 0.4560 0.3392 0.2332 11.00000 0.05 0.73 Q10 1 0.3827 0.3285 0.2407 11.00000 0.05 0.73 Q11 1 0.4564 0.0191 0.2038 11.00000 0.05 0.71 Q12 1 0.4719 -0.0451 0.9667 11.00000 0.05 0.69 Q13 1 0.5393 -0.3606 0.2406 11.00000 0.05 0.68 Q14 1 0.1020 0.4994 0.1770 11.00000 0.05 0.64 Q15 1 0.4415 -0.0574 0.9748 11.00000 0.05 0.64 ; 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 Pt Pt 0.5000 -0.050380(14) 0.2500 0.00746(8) Uani 1 2 d S . . Rh2 Rh 0.429529(9) 0.22770(2) 0.241040(9) 0.00677(8) Uani 1 1 d . . . S1 S 0.50786(3) 0.13236(7) 0.32333(3) 0.00865(14) Uani 1 1 d . . . P2 P 0.35646(3) 0.26561(7) 0.15062(3) 0.00765(15) Uani 1 1 d . . . C1 C 0.46480(15) -0.2163(3) 0.17899(14) 0.0150(6) Uani 1 1 d . . . H1 H 0.4395 -0.1802 0.1372 0.018 Uiso 1 1 calc R . . C2 C 0.52745(15) -0.2028(3) 0.18541(15) 0.0149(6) Uani 1 1 d . . . H2 H 0.5390 -0.1594 0.1473 0.018 Uiso 1 1 calc R . . C3 C 0.57640(17) -0.2955(4) 0.22608(16) 0.0224(7) Uani 1 1 d . . . H3A H 0.6160 -0.2457 0.2330 0.027 Uiso 1 1 calc R . . H3B H 0.5796 -0.3834 0.2020 0.027 Uiso 1 1 calc R . . C4 C 0.56482(17) -0.3347(3) 0.29140(16) 0.0206(7) Uani 1 1 d . . . H4A H 0.5382 -0.4191 0.2863 0.025 Uiso 1 1 calc R . . H4B H 0.6041 -0.3599 0.3211 0.025 Uiso 1 1 calc R . . C5 C 0.38703(14) 0.3034(3) 0.29662(14) 0.0139(6) Uani 1 1 d . . . O1 O 0.36159(12) 0.3502(3) 0.33206(12) 0.0254(5) Uani 1 1 d . . . C6 C 0.28293(14) 0.3418(3) 0.15602(14) 0.0110(5) Uani 1 1 d . . . C7 C 0.28258(16) 0.4675(3) 0.18983(17) 0.0154(6) Uani 1 1 d . . . H7 H 0.3201 0.5086 0.2118 0.019 Uiso 1 1 calc R . . C8 C 0.22845(17) 0.5331(3) 0.19183(18) 0.0184(7) Uani 1 1 d . . . H8 H 0.2289 0.6191 0.2149 0.022 Uiso 1 1 calc R . . C9 C 0.17300(16) 0.4732(4) 0.15997(18) 0.0192(7) Uani 1 1 d . . . H9 H 0.1357 0.5180 0.1613 0.023 Uiso 1 1 calc R . . C10 C 0.17287(15) 0.3478(4) 0.12648(17) 0.0218(7) Uani 1 1 d . . . H10 H 0.1353 0.3064 0.1048 0.026 Uiso 1 1 calc R . . C11 C 0.22751(15) 0.2826(4) 0.12446(15) 0.0171(6) Uani 1 1 d . . . H11 H 0.2270 0.1967 0.1013 0.021 Uiso 1 1 calc R . . C12 C 0.37469(13) 0.3755(3) 0.08714(14) 0.0097(5) Uani 1 1 d . . . C13 C 0.33001(14) 0.4132(3) 0.03230(15) 0.0138(6) Uani 1 1 d . . . H13 H 0.2895 0.3790 0.0269 0.017 Uiso 1 1 calc R . . C14 C 0.34445(15) 0.5002(3) -0.01428(15) 0.0180(6) Uani 1 1 d . . . H14 H 0.3139 0.5245 -0.0515 0.022 Uiso 1 1 calc R . . C15 C 0.40338(18) 0.5519(3) -0.00665(17) 0.0179(7) Uani 1 1 d . . . H15 H 0.4133 0.6110 -0.0386 0.022 Uiso 1 1 calc R . . C16 C 0.44756(15) 0.5163(3) 0.04810(15) 0.0150(6) Uani 1 1 d . . . H16 H 0.4876 0.5532 0.0539 0.018 Uiso 1 1 calc R . . C17 C 0.43397(15) 0.4278(3) 0.09436(15) 0.0126(6) Uani 1 1 d . . . H17 H 0.4649 0.4025 0.1311 0.015 Uiso 1 1 calc R . . C18 C 0.33487(13) 0.0930(3) 0.11280(14) 0.0104(5) Uani 1 1 d . . . C19 C 0.34028(17) 0.0573(3) 0.05160(18) 0.0179(7) Uani 1 1 d . . . H19 H 0.3534 0.1259 0.0253 0.021 Uiso 1 1 calc R . . C20 C 0.32636(17) -0.0807(4) 0.02842(18) 0.0232(7) Uani 1 1 d . . . H20 H 0.3301 -0.1051 -0.0136 0.028 Uiso 1 1 calc R . . C21 C 0.30731(16) -0.1804(4) 0.06619(18) 0.0237(7) Uani 1 1 d . . . H21 H 0.2983 -0.2737 0.0504 0.028 Uiso 1 1 calc R . . C22 C 0.30130(17) -0.1447(4) 0.12765(18) 0.0237(7) Uani 1 1 d . . . H22 H 0.2873 -0.2129 0.1535 0.028 Uiso 1 1 calc R . . C23 C 0.31579(16) -0.0094(4) 0.15097(16) 0.0182(6) Uani 1 1 d . . . H23 H 0.3127 0.0141 0.1933 0.022 Uiso 1 1 calc R . . C24 C 0.4730(4) -0.0228(10) 1.0049(6) 0.041(2) Uani 0.50 1 d P . . H24A H 0.4638 0.0126 1.0451 0.049 Uiso 0.50 1 calc PR . . H24B H 0.4381 -0.0082 0.9676 0.049 Uiso 0.50 1 calc PR . . Cl1A Cl 0.5070(2) 0.1381(3) 0.99112(16) 0.0538(9) Uani 0.50 1 d P . . Cl1B Cl 0.52058(12) -0.1659(3) 1.00630(13) 0.0295(5) Uani 0.50 1 d P . . 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 Pt 0.00816(11) 0.00692(11) 0.00681(10) 0.000 0.00076(7) 0.000 Rh2 0.00732(13) 0.00718(13) 0.00522(13) -0.00133(7) 0.00028(9) -0.00035(7) S1 0.0102(3) 0.0097(3) 0.0051(3) -0.0002(2) -0.0001(3) -0.0013(2) P2 0.0070(3) 0.0078(3) 0.0075(3) -0.0012(2) 0.0004(3) 0.0000(2) C1 0.0226(16) 0.0116(14) 0.0107(13) -0.0064(11) 0.0040(12) -0.0026(11) C2 0.0214(15) 0.0130(13) 0.0121(13) -0.0039(11) 0.0076(12) 0.0011(12) C3 0.0318(19) 0.0161(15) 0.0240(17) 0.0018(13) 0.0158(15) 0.0113(13) C4 0.0254(17) 0.0164(16) 0.0203(16) 0.0032(12) 0.0063(14) 0.0074(13) C5 0.0125(14) 0.0139(14) 0.0154(14) 0.0000(12) 0.0033(12) -0.0006(11) O1 0.0299(13) 0.0317(14) 0.0182(11) -0.0075(10) 0.0126(11) 0.0030(10) C6 0.0141(14) 0.0106(13) 0.0101(12) 0.0005(10) 0.0061(11) 0.0013(10) C7 0.0175(16) 0.0117(13) 0.0190(16) -0.0003(11) 0.0082(13) -0.0021(11) C8 0.0230(18) 0.0112(13) 0.0250(17) -0.0005(12) 0.0136(15) 0.0028(12) C9 0.0150(16) 0.0232(15) 0.0225(17) 0.0043(14) 0.0104(14) 0.0058(12) C10 0.0122(15) 0.0295(18) 0.0246(17) -0.0049(14) 0.0058(13) 0.0023(12) C11 0.0135(14) 0.0227(16) 0.0147(14) -0.0049(12) 0.0025(12) 0.0009(12) C12 0.0114(13) 0.0073(12) 0.0102(13) -0.0022(10) 0.0021(11) 0.0004(10) C13 0.0105(14) 0.0153(13) 0.0131(14) 0.0000(12) -0.0026(12) 0.0010(11) C14 0.0237(17) 0.0176(16) 0.0097(14) 0.0025(12) -0.0021(12) 0.0006(13) C15 0.0237(18) 0.0197(18) 0.0117(15) 0.0041(11) 0.0069(14) 0.0025(11) C16 0.0144(14) 0.0156(14) 0.0162(14) 0.0013(12) 0.0058(12) -0.0006(12) C17 0.0126(15) 0.0138(13) 0.0113(14) -0.0011(11) 0.0024(12) 0.0008(11) C18 0.0068(12) 0.0104(13) 0.0120(13) -0.0025(11) -0.0015(11) 0.0016(10) C19 0.0203(18) 0.0174(17) 0.0165(16) -0.0056(11) 0.0055(14) -0.0020(11) C20 0.0259(19) 0.0219(15) 0.0201(16) -0.0118(14) 0.0024(14) -0.0014(14) C21 0.0213(17) 0.0143(15) 0.0317(18) -0.0093(14) -0.0015(15) -0.0049(12) C22 0.0263(18) 0.0138(15) 0.0275(18) 0.0038(13) -0.0008(15) -0.0060(13) C23 0.0240(17) 0.0150(15) 0.0152(15) -0.0016(13) 0.0038(13) -0.0034(13) C24 0.026(4) 0.037(5) 0.057(6) 0.015(4) 0.002(4) -0.002(4) Cl1A 0.102(3) 0.0242(15) 0.0405(13) -0.0004(10) 0.027(2) -0.0098(17) Cl1B 0.0344(12) 0.0293(13) 0.0278(11) 0.0045(9) 0.0133(10) 0.0025(10) _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 Pt C2 2.184(3) 2_655 ? Pt C2 2.184(3) . ? Pt C1 2.198(3) . ? Pt C1 2.198(3) 2_655 ? Pt S1 2.3120(7) . ? Pt S1 2.3120(7) 2_655 ? Pt Rh2 3.0572(3) . ? Pt Rh2 3.0572(3) 2_655 ? Rh2 C5 1.838(3) . ? Rh2 P2 2.2540(7) . ? Rh2 S1 2.3594(7) . ? Rh2 S1 2.3704(7) 2_655 ? Rh2 Rh2 3.1135(4) 2_655 ? S1 Rh2 2.3704(7) 2_655 ? P2 C12 1.831(3) . ? P2 C18 1.836(3) . ? P2 C6 1.838(3) . ? C1 C2 1.394(5) . ? C1 C4 1.517(4) 2_655 ? C1 H1 1.0000 . ? C2 C3 1.514(4) . ? C2 H2 1.0000 . ? C3 C4 1.525(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C1 1.517(4) 2_655 ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 O1 1.142(4) . ? C6 C11 1.391(4) . ? C6 C7 1.392(4) . ? C7 C8 1.381(5) . ? C7 H7 0.9500 . ? C8 C9 1.397(5) . ? C8 H8 0.9500 . ? C9 C10 1.385(5) . ? C9 H9 0.9500 . ? C10 C11 1.389(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.400(4) . ? C12 C17 1.401(4) . ? C13 C14 1.388(5) . ? C13 H13 0.9500 . ? C14 C15 1.390(5) . ? C14 H14 0.9500 . ? C15 C16 1.388(5) . ? C15 H15 0.9500 . ? C16 C17 1.384(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.384(5) . ? C18 C23 1.398(5) . ? C19 C20 1.405(4) . ? C19 H19 0.9500 . ? C20 C21 1.375(6) . ? C20 H20 0.9500 . ? C21 C22 1.393(5) . ? C21 H21 0.9500 . ? C22 C23 1.385(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 Cl1A 1.176(10) 5_657 ? C24 C24 1.354(19) 5_657 ? C24 Cl1B 1.724(10) . ? C24 Cl1A 1.760(10) . ? C24 Cl1B 1.811(10) 5_657 ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? Cl1A Cl1B 0.689(4) 5_657 ? Cl1A C24 1.176(10) 5_657 ? Cl1B Cl1A 0.689(4) 5_657 ? Cl1B C24 1.811(10) 5_657 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pt C2 97.37(17) 2_655 . ? C2 Pt C1 81.62(12) 2_655 . ? C2 Pt C1 37.10(12) . . ? C2 Pt C1 37.10(12) 2_655 2_655 ? C2 Pt C1 81.62(12) . 2_655 ? C1 Pt C1 88.81(16) . 2_655 ? C2 Pt S1 93.07(8) 2_655 . ? C2 Pt S1 159.08(9) . . ? C1 Pt S1 163.67(9) . . ? C1 Pt S1 96.25(8) 2_655 . ? C2 Pt S1 159.08(9) 2_655 2_655 ? C2 Pt S1 93.06(8) . 2_655 ? C1 Pt S1 96.25(8) . 2_655 ? C1 Pt S1 163.67(9) 2_655 2_655 ? S1 Pt S1 83.18(3) . 2_655 ? C2 Pt Rh2 112.77(8) 2_655 . ? C2 Pt Rh2 138.55(8) . . ? C1 Pt Rh2 118.26(8) . . ? C1 Pt Rh2 139.13(8) 2_655 . ? S1 Pt Rh2 49.797(17) . . ? S1 Pt Rh2 50.072(18) 2_655 . ? C2 Pt Rh2 138.55(8) 2_655 2_655 ? C2 Pt Rh2 112.76(9) . 2_655 ? C1 Pt Rh2 139.13(8) . 2_655 ? C1 Pt Rh2 118.26(8) 2_655 2_655 ? S1 Pt Rh2 50.071(18) . 2_655 ? S1 Pt Rh2 49.797(17) 2_655 2_655 ? Rh2 Pt Rh2 61.222(9) . 2_655 ? C5 Rh2 P2 95.96(9) . . ? C5 Rh2 S1 94.64(9) . . ? P2 Rh2 S1 165.51(3) . . ? C5 Rh2 S1 174.99(9) . 2_655 ? P2 Rh2 S1 88.81(3) . 2_655 ? S1 Rh2 S1 80.93(3) . 2_655 ? C5 Rh2 Pt 129.62(10) . . ? P2 Rh2 Pt 117.10(2) . . ? S1 Rh2 Pt 48.453(17) . . ? S1 Rh2 Pt 48.414(17) 2_655 . ? C5 Rh2 Rh2 126.45(9) . 2_655 ? P2 Rh2 Rh2 128.73(2) . 2_655 ? S1 Rh2 Rh2 48.983(18) . 2_655 ? S1 Rh2 Rh2 48.680(17) 2_655 2_655 ? Pt Rh2 Rh2 59.389(4) . 2_655 ? Pt S1 Rh2 81.75(2) . . ? Pt S1 Rh2 81.52(2) . 2_655 ? Rh2 S1 Rh2 82.34(2) . 2_655 ? C12 P2 C18 105.17(13) . . ? C12 P2 C6 100.82(13) . . ? C18 P2 C6 103.09(13) . . ? C12 P2 Rh2 118.59(10) . . ? C18 P2 Rh2 107.49(9) . . ? C6 P2 Rh2 119.86(10) . . ? C2 C1 C4 124.3(3) . 2_655 ? C2 C1 Pt 70.91(17) . . ? C4 C1 Pt 111.3(2) 2_655 . ? C2 C1 H1 114.2 . . ? C4 C1 H1 114.2 2_655 . ? Pt C1 H1 114.2 . . ? C1 C2 C3 126.1(3) . . ? C1 C2 Pt 71.99(17) . . ? C3 C2 Pt 107.3(2) . . ? C1 C2 H2 114.2 . . ? C3 C2 H2 114.2 . . ? Pt C2 H2 114.2 . . ? C2 C3 C4 114.0(3) . . ? C2 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? C2 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C1 C4 C3 112.9(3) 2_655 . ? C1 C4 H4A 109.0 2_655 . ? C3 C4 H4A 109.0 . . ? C1 C4 H4B 109.0 2_655 . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? O1 C5 Rh2 178.7(3) . . ? C11 C6 C7 118.8(3) . . ? C11 C6 P2 122.3(2) . . ? C7 C6 P2 118.9(2) . . ? C8 C7 C6 120.9(3) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 120.0(3) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 119.5(3) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 120.2(3) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C6 120.6(3) . . ? C10 C11 H11 119.7 . . ? C6 C11 H11 119.7 . . ? C13 C12 C17 118.9(3) . . ? C13 C12 P2 121.4(2) . . ? C17 C12 P2 119.6(2) . . ? C14 C13 C12 120.4(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.3(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 119.4(3) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 C16 C15 120.8(3) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C12 120.1(3) . . ? C16 C17 H17 119.9 . . ? C12 C17 H17 119.9 . . ? C19 C18 C23 119.3(3) . . ? C19 C18 P2 124.0(2) . . ? C23 C18 P2 116.5(2) . . ? C18 C19 C20 119.9(3) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 120.4(3) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.0(3) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 119.8(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C18 120.7(3) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? Cl1A C24 C24 87.8(10) 5_657 5_657 ? Cl1B C24 Cl1A 112.8(6) . . ? Cl1A C24 H24A 114.0 5_657 . ? Cl1B C24 H24A 120.6 . . ? Cl1A C24 H24A 92.4 . . ? Cl1B C24 H24A 79.7 5_657 . ? Cl1A C24 H24B 114.0 5_657 . ? Cl1B C24 H24B 119.9 . . ? Cl1A C24 H24B 92.4 . . ? Cl1B C24 H24B 80.2 5_657 . ? H24A C24 H24B 111.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Pt Rh2 C5 20.20(15) 2_655 . . . ? C2 Pt Rh2 C5 153.44(18) . . . . ? C1 Pt Rh2 C5 112.84(15) . . . . ? C1 Pt Rh2 C5 -12.98(18) 2_655 . . . ? S1 Pt Rh2 C5 -53.62(12) . . . . ? S1 Pt Rh2 C5 -173.93(12) 2_655 . . . ? Rh2 Pt Rh2 C5 -113.98(12) 2_655 . . . ? C2 Pt Rh2 P2 -104.90(9) 2_655 . . . ? C2 Pt Rh2 P2 28.34(13) . . . . ? C1 Pt Rh2 P2 -12.26(10) . . . . ? C1 Pt Rh2 P2 -138.09(13) 2_655 . . . ? S1 Pt Rh2 P2 -178.72(3) . . . . ? S1 Pt Rh2 P2 60.96(3) 2_655 . . . ? Rh2 Pt Rh2 P2 120.92(2) 2_655 . . . ? C2 Pt Rh2 S1 73.82(9) 2_655 . . . ? C2 Pt Rh2 S1 -152.94(13) . . . . ? C1 Pt Rh2 S1 166.46(10) . . . . ? C1 Pt Rh2 S1 40.64(13) 2_655 . . . ? S1 Pt Rh2 S1 -120.32(3) 2_655 . . . ? Rh2 Pt Rh2 S1 -60.36(2) 2_655 . . . ? C2 Pt Rh2 S1 -165.87(9) 2_655 . . 2_655 ? C2 Pt Rh2 S1 -32.62(13) . . . 2_655 ? C1 Pt Rh2 S1 -73.23(10) . . . 2_655 ? C1 Pt Rh2 S1 160.95(13) 2_655 . . 2_655 ? S1 Pt Rh2 S1 120.32(3) . . . 2_655 ? Rh2 Pt Rh2 S1 59.96(2) 2_655 . . 2_655 ? C2 Pt Rh2 Rh2 134.18(9) 2_655 . . 2_655 ? C2 Pt Rh2 Rh2 -92.58(13) . . . 2_655 ? C1 Pt Rh2 Rh2 -133.18(10) . . . 2_655 ? C1 Pt Rh2 Rh2 101.00(13) 2_655 . . 2_655 ? S1 Pt Rh2 Rh2 60.36(2) . . . 2_655 ? S1 Pt Rh2 Rh2 -59.96(2) 2_655 . . 2_655 ? C2 Pt S1 Rh2 -117.52(9) 2_655 . . . ? C2 Pt S1 Rh2 122.5(2) . . . . ? C1 Pt S1 Rh2 -47.2(3) . . . . ? C1 Pt S1 Rh2 -154.62(9) 2_655 . . . ? S1 Pt S1 Rh2 41.813(13) 2_655 . . . ? Rh2 Pt S1 Rh2 83.42(2) 2_655 . . . ? C2 Pt S1 Rh2 159.06(9) 2_655 . . 2_655 ? C2 Pt S1 Rh2 39.1(2) . . . 2_655 ? C1 Pt S1 Rh2 -130.6(3) . . . 2_655 ? C1 Pt S1 Rh2 121.96(9) 2_655 . . 2_655 ? S1 Pt S1 Rh2 -41.607(14) 2_655 . . 2_655 ? Rh2 Pt S1 Rh2 -83.42(2) . . . 2_655 ? C5 Rh2 S1 Pt 141.52(10) . . . . ? P2 Rh2 S1 Pt 4.55(11) . . . . ? S1 Rh2 S1 Pt -40.83(2) 2_655 . . . ? Rh2 Rh2 S1 Pt -82.48(2) 2_655 . . . ? C5 Rh2 S1 Rh2 -136.00(10) . . . 2_655 ? P2 Rh2 S1 Rh2 87.03(11) . . . 2_655 ? S1 Rh2 S1 Rh2 41.64(3) 2_655 . . 2_655 ? Pt Rh2 S1 Rh2 82.48(2) . . . 2_655 ? C5 Rh2 P2 C12 121.03(14) . . . . ? S1 Rh2 P2 C12 -102.11(15) . . . . ? S1 Rh2 P2 C12 -57.44(11) 2_655 . . . ? Pt Rh2 P2 C12 -98.29(11) . . . . ? Rh2 Rh2 P2 C12 -27.12(11) 2_655 . . . ? C5 Rh2 P2 C18 -120.02(14) . . . . ? S1 Rh2 P2 C18 16.84(16) . . . . ? S1 Rh2 P2 C18 61.51(11) 2_655 . . . ? Pt Rh2 P2 C18 20.66(11) . . . . ? Rh2 Rh2 P2 C18 91.83(11) 2_655 . . . ? C5 Rh2 P2 C6 -2.98(15) . . . . ? S1 Rh2 P2 C6 133.88(14) . . . . ? S1 Rh2 P2 C6 178.56(11) 2_655 . . . ? Pt Rh2 P2 C6 137.70(11) . . . . ? Rh2 Rh2 P2 C6 -151.13(11) 2_655 . . . ? C2 Pt C1 C2 -114.2(2) 2_655 . . . ? C1 Pt C1 C2 -77.63(19) 2_655 . . . ? S1 Pt C1 C2 173.9(2) . . . . ? S1 Pt C1 C2 86.80(18) 2_655 . . . ? Rh2 Pt C1 C2 134.42(16) . . . . ? Rh2 Pt C1 C2 56.8(2) 2_655 . . . ? C2 Pt C1 C4 6.1(2) 2_655 . . 2_655 ? C2 Pt C1 C4 120.3(3) . . . 2_655 ? C1 Pt C1 C4 42.70(19) 2_655 . . 2_655 ? S1 Pt C1 C4 -65.8(4) . . . 2_655 ? S1 Pt C1 C4 -152.9(2) 2_655 . . 2_655 ? Rh2 Pt C1 C4 -105.3(2) . . . 2_655 ? Rh2 Pt C1 C4 177.11(17) 2_655 . . 2_655 ? C4 C1 C2 C3 -4.6(5) 2_655 . . . ? Pt C1 C2 C3 98.6(3) . . . . ? C4 C1 C2 Pt -103.2(3) 2_655 . . . ? C2 Pt C2 C1 65.51(17) 2_655 . . . ? C1 Pt C2 C1 99.2(2) 2_655 . . . ? S1 Pt C2 C1 -175.21(18) . . . . ? S1 Pt C2 C1 -96.32(17) 2_655 . . . ? Rh2 Pt C2 C1 -71.9(2) . . . . ? Rh2 Pt C2 C1 -143.59(16) 2_655 . . . ? C2 Pt C2 C3 -57.7(2) 2_655 . . . ? C1 Pt C2 C3 -123.2(3) . . . . ? C1 Pt C2 C3 -24.0(2) 2_655 . . . ? S1 Pt C2 C3 61.6(4) . . . . ? S1 Pt C2 C3 140.5(2) 2_655 . . . ? Rh2 Pt C2 C3 164.92(16) . . . . ? Rh2 Pt C2 C3 93.2(2) 2_655 . . . ? C1 C2 C3 C4 -40.6(5) . . . . ? Pt C2 C3 C4 39.4(3) . . . . ? C2 C3 C4 C1 -36.0(4) . . . 2_655 ? C12 P2 C6 C11 97.1(3) . . . . ? C18 P2 C6 C11 -11.4(3) . . . . ? Rh2 P2 C6 C11 -130.7(2) . . . . ? C12 P2 C6 C7 -79.2(3) . . . . ? C18 P2 C6 C7 172.3(2) . . . . ? Rh2 P2 C6 C7 53.0(3) . . . . ? C11 C6 C7 C8 -0.4(5) . . . . ? P2 C6 C7 C8 176.0(3) . . . . ? C6 C7 C8 C9 0.3(5) . . . . ? C7 C8 C9 C10 0.0(5) . . . . ? C8 C9 C10 C11 -0.2(5) . . . . ? C9 C10 C11 C6 0.1(5) . . . . ? C7 C6 C11 C10 0.2(5) . . . . ? P2 C6 C11 C10 -176.1(3) . . . . ? C18 P2 C12 C13 65.5(3) . . . . ? C6 P2 C12 C13 -41.4(3) . . . . ? Rh2 P2 C12 C13 -174.4(2) . . . . ? C18 P2 C12 C17 -117.0(2) . . . . ? C6 P2 C12 C17 136.1(2) . . . . ? Rh2 P2 C12 C17 3.1(3) . . . . ? C17 C12 C13 C14 0.5(5) . . . . ? P2 C12 C13 C14 178.0(2) . . . . ? C12 C13 C14 C15 -0.6(5) . . . . ? C13 C14 C15 C16 -0.3(5) . . . . ? C14 C15 C16 C17 1.4(5) . . . . ? C15 C16 C17 C12 -1.5(5) . . . . ? C13 C12 C17 C16 0.6(5) . . . . ? P2 C12 C17 C16 -177.0(2) . . . . ? C12 P2 C18 C19 7.4(3) . . . . ? C6 P2 C18 C19 112.6(3) . . . . ? Rh2 P2 C18 C19 -119.8(3) . . . . ? C12 P2 C18 C23 -177.0(2) . . . . ? C6 P2 C18 C23 -71.8(3) . . . . ? Rh2 P2 C18 C23 55.7(3) . . . . ? C23 C18 C19 C20 0.3(5) . . . . ? P2 C18 C19 C20 175.8(3) . . . . ? C18 C19 C20 C21 0.1(5) . . . . ? C19 C20 C21 C22 0.5(6) . . . . ? C20 C21 C22 C23 -1.4(6) . . . . ? C21 C22 C23 C18 1.7(5) . . . . ? C19 C18 C23 C22 -1.2(5) . . . . ? P2 C18 C23 C22 -177.0(3) . . . . ? Cl1A C24 Cl1A Cl1B -179.1(13) 5_657 . . 5_657 ? C24 C24 Cl1A Cl1B -179.1(13) 5_657 . . 5_657 ? Cl1B C24 Cl1A Cl1B -179.5(7) . . . 5_657 ? Cl1A C24 Cl1A C24 -0.008(3) 5_657 . . 5_657 ? Cl1B C24 Cl1A C24 -0.4(5) . . . 5_657 ? Cl1B C24 Cl1A C24 179.1(13) 5_657 . . 5_657 ? C24 C24 Cl1B Cl1A 178.7(18) 5_657 . . 5_657 ? Cl1A C24 Cl1B Cl1A 179.0(14) . . . 5_657 ? Cl1B C24 Cl1B Cl1A 178.7(18) 5_657 . . 5_657 ? Cl1A C24 Cl1B C24 -178.7(18) 5_657 . . 5_657 ? Cl1A C24 Cl1B C24 0.3(4) . . . 5_657 ? Cl1B C24 Cl1B C24 0.003(2) 5_657 . . 5_657 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.400 _refine_diff_density_min -2.055 _refine_diff_density_rms 0.202 data_compnd_11 _database_code_depnum_ccdc_archive 'CCDC 908509' #TrackingRef '15071_web_deposit_cif_file_0_FernandoJ.Lahoz_1351623726.compnd_3_6_7_9_11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H66 O12 P4 Rh2 Ru S2, 0.5(C H2 Cl2)' _chemical_formula_sum 'C78.50 H67 Cl O12 P4 Rh2 Ru S2' _chemical_formula_weight 1732.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.1988(9) _cell_length_b 16.1145(11) _cell_length_c 17.0522(11) _cell_angle_alpha 89.6900(10) _cell_angle_beta 68.6920(10) _cell_angle_gamma 83.6650(10) _cell_volume 3610.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 23318 _cell_measurement_theta_min 2.545 _cell_measurement_theta_max 29.3545 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.390 _exptl_crystal_size_mid 0.263 _exptl_crystal_size_min 0.168 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1754 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7192 _exptl_absorpt_correction_T_max 0.8628 _exptl_absorpt_process_details ; Multi-scan correction included in APEX2 package (Bruker AXS, 2008) ; _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 SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 39759 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 29.58 _reflns_number_total 18257 _reflns_number_gt 15945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v. 2009.7 (Bruker AXS, 2008)' _computing_cell_refinement 'APEX2 v. 2009.7 (Bruker AXS, 2008)' _computing_data_reduction 'APEX2 v. 2009.7 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. All non-hydrogen non-disordered atoms were refined with anisotropic displacement parameters. In the last cycles of the refinement, one of the phenyl groups of the phosphite ligands was observed disordered; it was modeled with two isotropic moieties with complementary occupancy factors. The fragment with lower occupancy was refined with geometrical constrains. Hydrogen atoms were included in calculated positions and refined riding (positional and displacement parameters) on their bonded atoms. The three highest residual peaks were slightly over 1 e/A^3 and were observed around the positions of the metal atoms. ; _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^)+(0.0544P)^2^+3.5978P] 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 18257 _refine_ls_number_parameters 896 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.001 _iucr_refine_instructions_details ; TITL fjl105dm in P-1 CELL 0.71073 14.1988 16.1145 17.0522 89.690 68.692 83.665 ZERR 2.00 0.0009 0.0011 0.0011 0.001 0.001 0.001 LATT 1 SFAC C H O P S Ru Rh Cl UNIT 157 134 24 8 4 2 4 2 MERG 2 OMIT 0 0 1 OMIT 0 1 0 L.S. 4 ACTA 55 BOND $H FMAP 2 PLAN 15 CONF WPDB -2 SIZE 0.390 0.263 0.168 FREE Ru Rh3 FREE Rh2 Rh3 FREE Ru Rh2 TEMP -173.00 WGHT 0.054400 3.597800 FVAR 0.21191 0.56904 RU 6 -0.017004 0.249910 0.360703 11.00000 0.02676 0.01931 = 0.02000 -0.00131 -0.00908 0.00031 RH2 7 0.114217 0.272882 0.188343 11.00000 0.02477 0.01549 = 0.01708 0.00015 -0.00836 0.00103 RH3 7 0.206604 0.205871 0.322011 11.00000 0.02661 0.01648 = 0.01757 -0.00017 -0.00801 0.00055 S1 5 0.115497 0.332701 0.312024 11.00000 0.03050 0.01627 = 0.02096 -0.00138 -0.01064 0.00063 S2 5 0.098055 0.150886 0.265341 11.00000 0.02804 0.01665 = 0.02044 0.00071 -0.00958 0.00041 P1 4 0.143101 0.386097 0.116898 11.00000 0.02798 0.01797 = 0.02403 0.00286 -0.01181 -0.00127 P2 4 0.094802 0.207611 0.085120 11.00000 0.03089 0.01765 = 0.01900 0.00108 -0.01047 -0.00167 P3 4 0.290653 0.265230 0.385562 11.00000 0.03001 0.02024 = 0.02417 -0.00071 -0.00985 -0.00296 P4 4 0.298557 0.086752 0.315883 11.00000 0.02490 0.01850 = 0.01857 -0.00040 -0.00739 0.00075 O2 3 0.060082 0.438235 0.085933 11.00000 0.02975 0.02158 = 0.02226 0.00293 -0.01148 0.00084 O1 3 0.225722 0.381096 0.021179 11.00000 0.02890 0.03256 = 0.03290 0.01268 -0.00403 0.00238 O3 3 0.180425 0.459170 0.159279 11.00000 0.06198 0.02281 = 0.04921 0.01004 -0.04010 -0.01254 O4 3 0.069010 0.267356 0.017771 11.00000 0.05188 0.02000 = 0.02481 0.00162 -0.01954 -0.00392 O6 3 0.187952 0.147959 0.016850 11.00000 0.03985 0.02515 = 0.02561 -0.00082 -0.00850 0.00000 O5 3 0.012331 0.140571 0.105165 11.00000 0.03538 0.02173 = 0.02982 0.00047 -0.01199 -0.00281 O9 3 0.331276 0.205085 0.445702 11.00000 0.03581 0.02150 = 0.03507 -0.00113 -0.02065 -0.00204 O8 3 0.239186 0.347925 0.446243 11.00000 0.03694 0.01832 = 0.03203 -0.00299 -0.01576 -0.00230 O7 3 0.396191 0.302176 0.333314 11.00000 0.03694 0.03643 = 0.04215 -0.00155 -0.00618 -0.01270 O10 3 0.419454 0.094462 0.285807 11.00000 0.02549 0.02199 = 0.03035 0.00110 -0.00876 -0.00158 O11 3 0.299808 0.015371 0.249578 11.00000 0.03586 0.02028 = 0.02336 -0.00112 -0.01215 -0.00168 O12 3 0.285455 0.030443 0.397310 11.00000 0.03087 0.02303 = 0.01927 0.00090 -0.00663 0.00483 C1 1 -0.147865 0.346135 0.415191 11.00000 0.03213 0.02549 = 0.03076 -0.00174 -0.01079 0.00555 AFIX 43 H1 2 -0.156170 0.404399 0.406762 11.00000 -1.20000 AFIX 0 C2 1 -0.115248 0.316783 0.479783 11.00000 0.03329 0.02799 = 0.02357 -0.00450 -0.00873 0.00100 AFIX 43 H2 2 -0.101017 0.354980 0.515109 11.00000 -1.20000 AFIX 0 C3 1 -0.103651 0.229485 0.491988 11.00000 0.03430 0.03220 = 0.02306 0.00257 -0.00873 0.00046 AFIX 43 H3 2 -0.077593 0.209387 0.533438 11.00000 -1.20000 AFIX 0 C4 1 -0.130139 0.172458 0.443686 11.00000 0.03468 0.02217 = 0.03744 0.00031 -0.01032 -0.00453 AFIX 43 H4 2 -0.126896 0.114680 0.455176 11.00000 -1.20000 AFIX 0 C5 1 -0.161652 0.201838 0.377846 11.00000 0.03026 0.03764 = 0.03216 -0.00746 -0.00862 -0.00678 AFIX 43 H5 2 -0.178266 0.163698 0.343946 11.00000 -1.20000 AFIX 0 C6 1 -0.168382 0.288638 0.362566 11.00000 0.03018 0.04205 = 0.02986 -0.00319 -0.01392 0.00340 AFIX 43 H6 2 -0.186732 0.308226 0.316834 11.00000 -1.20000 AFIX 0 C11 1 0.317107 0.330201 -0.007850 11.00000 0.02536 0.02433 = 0.03639 0.00774 -0.00655 -0.00459 C12 1 0.366245 0.297742 0.044147 11.00000 0.02781 0.03483 = 0.04137 0.00657 -0.00986 -0.00358 AFIX 43 H12 2 0.337673 0.309185 0.103244 11.00000 -1.20000 AFIX 0 C13 1 0.459446 0.247448 0.007278 11.00000 0.03132 0.04134 = 0.05108 0.00879 -0.01687 -0.00067 AFIX 43 H13 2 0.494152 0.223917 0.041882 11.00000 -1.20000 AFIX 0 C14 1 0.501240 0.231786 -0.078619 11.00000 0.03250 0.03811 = 0.05346 -0.00080 -0.00961 0.00275 AFIX 43 H14 2 0.564585 0.197859 -0.102874 11.00000 -1.20000 AFIX 0 C15 1 0.451055 0.265417 -0.129601 11.00000 0.03935 0.04236 = 0.03855 0.00013 -0.00706 0.00129 AFIX 43 H15 2 0.480202 0.254711 -0.188797 11.00000 -1.20000 AFIX 0 C16 1 0.358309 0.314714 -0.094460 11.00000 0.03436 0.03778 = 0.03811 0.00843 -0.00992 -0.00274 AFIX 43 H16 2 0.323425 0.337587 -0.129193 11.00000 -1.20000 AFIX 0 C17 1 -0.043012 0.454958 0.134065 11.00000 0.02951 0.01594 = 0.02686 0.00393 -0.01149 0.00103 C18 1 -0.078767 0.474605 0.219442 11.00000 0.03743 0.02765 = 0.02773 0.00212 -0.01300 0.00498 AFIX 43 H18 2 -0.033441 0.473742 0.249015 11.00000 -1.20000 AFIX 0 C19 1 -0.182841 0.495659 0.260842 11.00000 0.04272 0.03899 = 0.03381 0.00642 -0.00429 0.00943 AFIX 43 H19 2 -0.209042 0.509633 0.319480 11.00000 -1.20000 AFIX 0 C20 1 -0.248507 0.496523 0.217926 11.00000 0.03089 0.04338 = 0.06194 0.01490 -0.01066 0.00428 AFIX 43 H20 2 -0.319531 0.510836 0.246989 11.00000 -1.20000 AFIX 0 C21 1 -0.210881 0.476501 0.132347 11.00000 0.03977 0.03661 = 0.06113 0.01504 -0.02926 -0.00510 AFIX 43 H21 2 -0.256308 0.477084 0.102890 11.00000 -1.20000 AFIX 0 C22 1 -0.107558 0.455667 0.089544 11.00000 0.04110 0.02323 = 0.03726 0.00653 -0.02243 -0.00436 AFIX 43 H22 2 -0.081389 0.442123 0.030821 11.00000 -1.20000 AFIX 0 C23 1 0.214865 0.530296 0.113671 11.00000 0.05282 0.02214 = 0.06584 0.01125 -0.03935 -0.01406 C24 1 0.317167 0.530592 0.068329 11.00000 0.04867 0.03357 = 0.19150 0.03336 -0.05652 -0.01533 AFIX 43 H24 2 0.364025 0.483301 0.067167 11.00000 -1.20000 AFIX 0 C25 1 0.351381 0.601668 0.023822 11.00000 0.05068 0.04363 = 0.21600 0.03593 -0.03848 -0.02369 AFIX 43 H25 2 0.421891 0.603056 -0.007189 11.00000 -1.20000 AFIX 0 C26 1 0.282561 0.669331 0.025210 11.00000 0.07455 0.02973 = 0.11132 0.02211 -0.03993 -0.02392 AFIX 43 H26 2 0.305283 0.716938 -0.006088 11.00000 -1.20000 AFIX 0 C27 1 0.181767 0.668019 0.071516 11.00000 0.06779 0.01992 = 0.06029 0.00342 -0.03883 -0.00535 AFIX 43 H27 2 0.135137 0.715758 0.073560 11.00000 -1.20000 AFIX 0 C28 1 0.145810 0.598311 0.115787 11.00000 0.04827 0.02354 = 0.03920 -0.00197 -0.02149 -0.00349 AFIX 43 H28 2 0.075206 0.597514 0.146835 11.00000 -1.20000 AFIX 0 C29 1 0.076349 0.245411 -0.063367 11.00000 0.04296 0.02329 = 0.02265 -0.00007 -0.01567 -0.00040 C30 1 0.112340 0.303378 -0.123994 11.00000 0.03797 0.02372 = 0.02744 0.00160 -0.01317 -0.00094 AFIX 43 H30 2 0.132403 0.353813 -0.109893 11.00000 -1.20000 AFIX 0 C31 1 0.118743 0.286921 -0.205544 11.00000 0.04489 0.03115 = 0.02438 0.00323 -0.01200 0.00597 AFIX 43 H31 2 0.141908 0.326910 -0.247323 11.00000 -1.20000 AFIX 0 C32 1 0.091595 0.212511 -0.226662 11.00000 0.05640 0.03385 = 0.02570 -0.00517 -0.02217 0.01127 AFIX 43 H32 2 0.097889 0.200861 -0.283016 11.00000 -1.20000 AFIX 0 C33 1 0.055529 0.155707 -0.165604 11.00000 0.06296 0.02528 = 0.03688 -0.00276 -0.03099 0.00033 AFIX 43 H33 2 0.036798 0.104805 -0.180075 11.00000 -1.20000 AFIX 0 C34 1 0.046167 0.171821 -0.083159 11.00000 0.05779 0.02555 = 0.03201 0.00400 -0.02556 -0.00587 AFIX 43 H34 2 0.019493 0.133069 -0.040857 11.00000 -1.20000 AFIX 0 C35 1 -0.092744 0.158751 0.144917 11.00000 0.03495 0.03183 = 0.02378 -0.00016 -0.01439 -0.00521 C36 1 -0.143988 0.237580 0.149941 11.00000 0.04347 0.03014 = 0.03894 0.00121 -0.01727 -0.00861 AFIX 43 H36 2 -0.107512 0.283969 0.129034 11.00000 -1.20000 AFIX 0 C37 1 -0.249901 0.248355 0.186052 11.00000 0.04559 0.03771 = 0.04830 -0.00602 -0.02044 0.00181 AFIX 43 H37 2 -0.285661 0.302530 0.189987 11.00000 -1.20000 AFIX 0 C38 1 -0.303786 0.180739 0.216366 11.00000 0.03636 0.05753 = 0.03969 -0.00263 -0.01492 -0.00844 AFIX 43 H38 2 -0.376018 0.188073 0.240692 11.00000 -1.20000 AFIX 0 C39 1 -0.249590 0.101795 0.210342 11.00000 0.04641 0.04242 = 0.03980 0.00761 -0.01957 -0.01921 AFIX 43 H39 2 -0.285303 0.054895 0.230678 11.00000 -1.20000 AFIX 0 C40 1 -0.145202 0.091265 0.175321 11.00000 0.04557 0.03105 = 0.03394 0.00256 -0.02086 -0.00878 AFIX 43 H40 2 -0.109070 0.037349 0.172046 11.00000 -1.20000 AFIX 0 C41 1 0.225289 0.066425 0.026695 11.00000 0.03472 0.02470 = 0.02584 -0.00307 -0.01142 0.00320 C42 1 0.183289 0.000550 0.005803 11.00000 0.03869 0.03100 = 0.03980 -0.00884 -0.01933 0.00114 AFIX 43 H42 2 0.122913 0.010462 -0.006384 11.00000 -1.20000 AFIX 0 C43 1 0.229959 -0.079925 0.002801 11.00000 0.04745 0.02650 = 0.04145 -0.00712 -0.02090 0.00053 AFIX 43 H43 2 0.202121 -0.125738 -0.011898 11.00000 -1.20000 AFIX 0 C44 1 0.316786 -0.093325 0.021178 11.00000 0.04020 0.03324 = 0.03847 -0.00652 -0.01263 0.00799 AFIX 43 H44 2 0.349059 -0.148620 0.018830 11.00000 -1.20000 AFIX 0 C45 1 0.357566 -0.027443 0.042975 11.00000 0.03335 0.04165 = 0.04409 0.00603 -0.01730 -0.00212 AFIX 43 H45 2 0.417487 -0.037807 0.055769 11.00000 -1.20000 AFIX 0 C46 1 0.312296 0.053507 0.046433 11.00000 0.04270 0.03630 = 0.03194 0.00372 -0.01583 -0.01175 AFIX 43 H46 2 0.339898 0.099063 0.061878 11.00000 -1.20000 PART 1 C47A 1 0.402375 0.375784 0.285098 21.00000 0.05767 C48A 1 0.327968 0.443880 0.301258 21.00000 0.07158 AFIX 43 H48A 2 0.262322 0.441254 0.342926 21.00000 -1.20000 AFIX 0 C49A 1 0.350889 0.518102 0.254665 21.00000 0.08842 AFIX 43 H49A 2 0.301438 0.563922 0.257404 21.00000 -1.20000 AFIX 0 C50A 1 0.461056 0.515381 0.201389 21.00000 0.12213 AFIX 43 H50A 2 0.487532 0.566262 0.181277 21.00000 -1.20000 AFIX 0 C51A 1 0.509600 0.460486 0.185526 21.00000 0.08150 AFIX 43 H51A 2 0.572719 0.461731 0.140127 21.00000 -1.20000 AFIX 0 C52A 1 0.490180 0.381027 0.226470 21.00000 0.08281 AFIX 43 H52A 2 0.540875 0.334159 0.210448 21.00000 -1.20000 AFIX 0 C83 1 0.464769 0.457036 0.443900 10.50000 0.07760 0.09641 = 0.10912 -0.04019 -0.04194 0.00436 AFIX 23 H83A 2 0.458682 0.467315 0.388552 10.50000 -1.20000 H83B 2 0.446680 0.400050 0.459557 10.50000 -1.20000 AFIX 0 CL1 8 0.379191 0.525763 0.515538 10.50000 0.06219 0.08650 = 0.10968 -0.01911 0.00371 0.00252 CL2 8 0.589973 0.459551 0.432501 10.50000 0.05386 0.10273 = 0.09241 0.01234 0.00619 -0.01164 PART 2 AFIX 66 C47B 1 0.412137 0.383256 0.309754 -21.00000 0.03500 C48B 1 0.447758 0.429699 0.359341 -21.00000 0.06138 AFIX 43 H48B 2 0.463883 0.404265 0.403983 -21.00000 -1.20000 AFIX 65 C49B 1 0.459784 0.513357 0.343609 -21.00000 0.06397 AFIX 43 H49B 2 0.484129 0.545099 0.377500 -21.00000 -1.20000 AFIX 65 C50B 1 0.436191 0.550571 0.278290 -21.00000 0.07978 AFIX 43 H50B 2 0.444410 0.607748 0.267539 -21.00000 -1.20000 AFIX 65 C51B 1 0.400570 0.504129 0.228703 -21.00000 0.12782 AFIX 43 H51B 2 0.384445 0.529564 0.184061 -21.00000 -1.20000 AFIX 65 C52B 1 0.388543 0.420471 0.244434 -21.00000 0.09786 AFIX 43 H52B 2 0.364198 0.388730 0.210543 -21.00000 -1.20000 AFIX 0 PART 0 C53 1 0.145273 0.358305 0.510421 11.00000 0.03572 0.02245 = 0.02482 -0.00401 -0.01815 0.00244 C54 1 0.097849 0.293044 0.555440 11.00000 0.03193 0.02580 = 0.03098 -0.00174 -0.01622 0.00241 AFIX 43 H54 2 0.127015 0.236815 0.539971 11.00000 -1.20000 AFIX 0 C55 1 0.006870 0.311169 0.623634 11.00000 0.03420 0.04458 = 0.02983 0.00036 -0.01537 0.00170 AFIX 43 H55 2 -0.026281 0.267003 0.655121 11.00000 -1.20000 AFIX 0 C56 1 -0.035801 0.393340 0.645987 11.00000 0.03926 0.05403 = 0.03119 -0.01512 -0.01585 0.01124 AFIX 43 H56 2 -0.097270 0.405364 0.693280 11.00000 -1.20000 AFIX 0 C57 1 0.010849 0.457120 0.599746 11.00000 0.05910 0.03282 = 0.04539 -0.02002 -0.02983 0.01540 AFIX 43 H57 2 -0.019520 0.513200 0.614190 11.00000 -1.20000 AFIX 0 C58 1 0.101967 0.440382 0.532100 11.00000 0.05120 0.02229 = 0.03942 -0.00767 -0.02537 0.00450 AFIX 43 H58 2 0.134597 0.484828 0.500750 11.00000 -1.20000 AFIX 0 C59 1 0.390606 0.229984 0.489747 11.00000 0.03432 0.02672 = 0.04272 0.00201 -0.02242 -0.00345 C60 1 0.494085 0.210623 0.455024 11.00000 0.03407 0.06116 = 0.05409 -0.00113 -0.01832 -0.00031 AFIX 43 H60 2 0.525573 0.183149 0.401134 11.00000 -1.20000 AFIX 0 C61 1 0.551962 0.232320 0.500897 11.00000 0.03814 0.08409 = 0.09044 0.01178 -0.03527 -0.01144 AFIX 43 H61 2 0.623802 0.218869 0.478139 11.00000 -1.20000 AFIX 0 C62 1 0.507090 0.272625 0.578073 11.00000 0.07812 0.06312 = 0.09133 0.00657 -0.06750 -0.02003 AFIX 43 H62 2 0.547714 0.287743 0.608151 11.00000 -1.20000 AFIX 0 C63 1 0.403386 0.291182 0.611973 11.00000 0.07740 0.04557 = 0.06445 -0.01091 -0.05084 -0.00014 AFIX 43 H63 2 0.372174 0.319075 0.665673 11.00000 -1.20000 AFIX 0 C64 1 0.343911 0.269427 0.568242 11.00000 0.04661 0.03554 = 0.04676 -0.00549 -0.03029 0.00272 AFIX 43 H64 2 0.271930 0.281483 0.591941 11.00000 -1.20000 AFIX 0 C65 1 0.491865 0.025123 0.275751 11.00000 0.02154 0.02237 = 0.02966 -0.00008 -0.00816 -0.00204 C66 1 0.542222 -0.012417 0.196400 11.00000 0.02869 0.03258 = 0.02657 0.00149 -0.00621 -0.00583 AFIX 43 H66 2 0.527170 0.008170 0.149450 11.00000 -1.20000 AFIX 0 C67 1 0.614731 -0.080303 0.186512 11.00000 0.02785 0.03580 = 0.03479 -0.00613 0.00063 -0.00039 AFIX 43 H67 2 0.649427 -0.106809 0.132459 11.00000 -1.20000 AFIX 0 C68 1 0.636918 -0.109670 0.254386 11.00000 0.02590 0.03261 = 0.05306 0.00152 -0.00953 0.00152 AFIX 43 H68 2 0.686741 -0.156414 0.247025 11.00000 -1.20000 AFIX 0 C69 1 0.587066 -0.071503 0.333342 11.00000 0.03099 0.03613 = 0.04397 0.00623 -0.01816 -0.00245 AFIX 43 H69 2 0.602722 -0.092146 0.380002 11.00000 -1.20000 AFIX 0 C70 1 0.514295 -0.003197 0.344632 11.00000 0.02781 0.03160 = 0.03002 -0.00223 -0.01034 -0.00310 AFIX 43 H70 2 0.480415 0.023715 0.398583 11.00000 -1.20000 AFIX 0 C71 1 0.274257 -0.065839 0.261219 11.00000 0.02339 0.02131 = 0.02261 -0.00502 -0.00389 0.00025 C72 1 0.203477 -0.086233 0.228575 11.00000 0.02707 0.03256 = 0.03060 -0.00323 -0.00994 -0.00035 AFIX 43 H72 2 0.169369 -0.044536 0.205612 11.00000 -1.20000 AFIX 0 C73 1 0.183006 -0.168498 0.229853 11.00000 0.03426 0.04149 = 0.04467 -0.00664 -0.01421 -0.01085 AFIX 43 H73 2 0.135426 -0.183451 0.206639 11.00000 -1.20000 AFIX 0 C74 1 0.231208 -0.228899 0.264596 11.00000 0.03657 0.02656 = 0.05383 -0.00383 -0.00803 -0.00808 AFIX 43 H74 2 0.217449 -0.285274 0.264642 11.00000 -1.20000 AFIX 0 C75 1 0.299086 -0.207154 0.299066 11.00000 0.03220 0.02413 = 0.05100 0.00334 -0.01046 -0.00011 AFIX 43 H75 2 0.330224 -0.248512 0.324676 11.00000 -1.20000 AFIX 0 C76 1 0.323068 -0.125328 0.297093 11.00000 0.02898 0.02499 = 0.03953 0.00012 -0.01392 -0.00154 AFIX 43 H76 2 0.371397 -0.110719 0.319640 11.00000 -1.20000 AFIX 0 C77 1 0.211119 0.041482 0.477115 11.00000 0.02886 0.01682 = 0.01976 0.00027 -0.00737 -0.00293 C78 1 0.109242 0.060361 0.490465 11.00000 0.03117 0.02065 = 0.02393 0.00265 -0.01143 -0.00219 AFIX 43 H78 2 0.087502 0.071033 0.444480 11.00000 -1.20000 AFIX 0 C79 1 0.038683 0.063479 0.572914 11.00000 0.02792 0.02269 = 0.03157 0.00012 -0.00775 -0.00237 AFIX 43 H79 2 -0.031766 0.076567 0.583148 11.00000 -1.20000 AFIX 0 C80 1 0.070386 0.047662 0.640054 11.00000 0.03724 0.03116 = 0.02311 -0.00311 -0.00503 -0.00684 AFIX 43 H80 2 0.021761 0.048589 0.695845 11.00000 -1.20000 AFIX 0 C81 1 0.173140 0.030531 0.625396 11.00000 0.04064 0.04242 = 0.02215 -0.00025 -0.01399 -0.00866 AFIX 43 H81 2 0.195099 0.021015 0.671416 11.00000 -1.20000 AFIX 0 C82 1 0.244292 0.027174 0.543840 11.00000 0.02902 0.03488 = 0.02507 0.00088 -0.01213 -0.00432 AFIX 43 H82 2 0.314844 0.015238 0.533722 11.00000 -1.20000 HKLF 4 REM fjl105dm in P-1 REM R1 = 0.0344 for 15945 Fo > 4sig(Fo) and 0.0401 for all 18257 data REM 896 parameters refined using 0 restraints END WGHT 0.0543 3.6159 REM Highest difference peak 1.269, deepest hole -1.056, 1-sigma level 0.092 Q1 1 0.2576 0.2117 0.3259 11.00000 0.05 1.27 Q2 1 0.1189 0.2887 0.2239 11.00000 0.05 1.20 Q3 1 0.4957 0.3388 0.2064 11.00000 0.05 1.15 Q4 1 0.5251 0.4149 0.1575 11.00000 0.05 1.11 Q5 1 0.1403 0.2426 -0.0021 11.00000 0.05 1.00 Q6 1 0.5029 0.4862 0.2091 11.00000 0.05 0.93 Q7 1 0.4373 0.3537 0.2863 11.00000 0.05 0.91 Q8 1 0.0956 0.1096 0.0791 11.00000 0.05 0.87 Q9 1 0.3596 0.4281 0.2639 11.00000 0.05 0.82 Q10 1 0.4954 0.4039 0.2411 11.00000 0.05 0.79 Q11 1 0.2842 0.6805 0.0738 11.00000 0.05 0.76 Q12 1 -0.2209 0.3482 0.4878 11.00000 0.05 0.76 Q13 1 -0.0321 0.2278 0.0909 11.00000 0.05 0.76 Q14 1 0.0811 0.2410 0.1873 11.00000 0.05 0.75 Q15 1 0.4355 0.5352 0.2037 11.00000 0.05 0.71 ; 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 Ru Ru -0.017004(15) 0.249910(11) 0.360703(12) 0.02210(5) Uani 1 1 d . . . Rh2 Rh 0.114217(14) 0.272882(10) 0.188343(11) 0.01918(5) Uani 1 1 d . . . Rh3 Rh 0.206604(14) 0.205871(11) 0.322011(11) 0.02048(5) Uani 1 1 d . . . S1 S 0.11550(5) 0.33270(3) 0.31202(4) 0.02249(11) Uani 1 1 d . . . S2 S 0.09806(5) 0.15089(3) 0.26534(4) 0.02175(11) Uani 1 1 d . . . P1 P 0.14310(5) 0.38610(4) 0.11690(4) 0.02280(12) Uani 1 1 d . . . P2 P 0.09480(5) 0.20761(4) 0.08512(4) 0.02223(12) Uani 1 1 d . . . P3 P 0.29065(5) 0.26523(4) 0.38556(4) 0.02481(13) Uani 1 1 d . A . P4 P 0.29856(5) 0.08675(4) 0.31588(4) 0.02107(12) Uani 1 1 d . . . O2 O 0.06008(14) 0.43823(10) 0.08593(11) 0.0243(3) Uani 1 1 d . . . O1 O 0.22572(15) 0.38110(12) 0.02118(13) 0.0340(4) Uani 1 1 d . . . O3 O 0.18043(18) 0.45917(12) 0.15928(14) 0.0385(5) Uani 1 1 d . . . O4 O 0.06901(16) 0.26736(11) 0.01777(12) 0.0307(4) Uani 1 1 d . . . O6 O 0.18795(15) 0.14796(11) 0.01685(12) 0.0315(4) Uani 1 1 d . . . O5 O 0.01233(15) 0.14057(11) 0.10516(12) 0.0290(4) Uani 1 1 d . . . O9 O 0.33128(15) 0.20509(11) 0.44570(12) 0.0287(4) Uani 1 1 d . . . O8 O 0.23919(15) 0.34793(11) 0.44624(12) 0.0283(4) Uani 1 1 d . . . O7 O 0.39619(16) 0.30218(13) 0.33331(14) 0.0401(5) Uani 1 1 d . . . O10 O 0.41945(13) 0.09446(11) 0.28581(12) 0.0264(4) Uani 1 1 d . . . O11 O 0.29981(14) 0.01537(11) 0.24958(11) 0.0262(4) Uani 1 1 d . . . O12 O 0.28546(14) 0.03044(11) 0.39731(11) 0.0257(4) Uani 1 1 d . . . C1 C -0.1479(2) 0.34614(17) 0.41519(17) 0.0304(5) Uani 1 1 d . . . H1 H -0.1562 0.4044 0.4068 0.036 Uiso 1 1 calc R . . C2 C -0.1152(2) 0.31678(16) 0.47978(16) 0.0291(5) Uani 1 1 d . . . H2 H -0.1010 0.3550 0.5151 0.035 Uiso 1 1 calc R . . C3 C -0.1037(2) 0.22948(17) 0.49199(17) 0.0307(5) Uani 1 1 d . . . H3 H -0.0776 0.2094 0.5334 0.037 Uiso 1 1 calc R . . C4 C -0.1301(2) 0.17246(17) 0.44369(18) 0.0321(6) Uani 1 1 d . . . H4 H -0.1269 0.1147 0.4552 0.039 Uiso 1 1 calc R . . C5 C -0.1617(2) 0.20184(18) 0.37785(18) 0.0339(6) Uani 1 1 d . . . H5 H -0.1783 0.1637 0.3439 0.041 Uiso 1 1 calc R . . C6 C -0.1684(2) 0.28864(19) 0.36257(18) 0.0338(6) Uani 1 1 d . . . H6 H -0.1867 0.3082 0.3168 0.041 Uiso 1 1 calc R . . C11 C 0.3171(2) 0.33020(16) -0.00785(18) 0.0299(5) Uani 1 1 d . . . C12 C 0.3662(2) 0.29774(18) 0.0441(2) 0.0355(6) Uani 1 1 d . . . H12 H 0.3377 0.3092 0.1032 0.043 Uiso 1 1 calc R . . C13 C 0.4594(2) 0.2474(2) 0.0073(2) 0.0410(7) Uani 1 1 d . . . H13 H 0.4942 0.2239 0.0419 0.049 Uiso 1 1 calc R . . C14 C 0.5012(2) 0.2318(2) -0.0786(2) 0.0436(7) Uani 1 1 d . . . H14 H 0.5646 0.1979 -0.1029 0.052 Uiso 1 1 calc R . . C15 C 0.4511(2) 0.2654(2) -0.1296(2) 0.0426(7) Uani 1 1 d . . . H15 H 0.4802 0.2547 -0.1888 0.051 Uiso 1 1 calc R . . C16 C 0.3583(2) 0.31471(19) -0.0945(2) 0.0378(6) Uani 1 1 d . . . H16 H 0.3234 0.3376 -0.1292 0.045 Uiso 1 1 calc R . . C17 C -0.04301(19) 0.45496(14) 0.13407(16) 0.0241(5) Uani 1 1 d . . . C18 C -0.0788(2) 0.47461(17) 0.21944(17) 0.0313(6) Uani 1 1 d . . . H18 H -0.0334 0.4737 0.2490 0.038 Uiso 1 1 calc R . . C19 C -0.1828(2) 0.4957(2) 0.2608(2) 0.0424(7) Uani 1 1 d . . . H19 H -0.2090 0.5096 0.3195 0.051 Uiso 1 1 calc R . . C20 C -0.2485(2) 0.4965(2) 0.2179(2) 0.0479(8) Uani 1 1 d . . . H20 H -0.3195 0.5108 0.2470 0.057 Uiso 1 1 calc R . . C21 C -0.2109(2) 0.47650(19) 0.1323(2) 0.0428(7) Uani 1 1 d . . . H21 H -0.2563 0.4771 0.1029 0.051 Uiso 1 1 calc R . . C22 C -0.1076(2) 0.45567(16) 0.08954(19) 0.0315(6) Uani 1 1 d . . . H22 H -0.0814 0.4421 0.0308 0.038 Uiso 1 1 calc R . . C23 C 0.2149(3) 0.53030(17) 0.1137(2) 0.0412(7) Uani 1 1 d . . . C24 C 0.3172(3) 0.5306(2) 0.0683(4) 0.0869(19) Uani 1 1 d . . . H24 H 0.3640 0.4833 0.0672 0.104 Uiso 1 1 calc R . . C25 C 0.3514(4) 0.6017(3) 0.0238(5) 0.105(2) Uani 1 1 d . . . H25 H 0.4219 0.6031 -0.0072 0.126 Uiso 1 1 calc R . . C26 C 0.2826(4) 0.6693(2) 0.0252(3) 0.0688(12) Uani 1 1 d . . . H26 H 0.3053 0.7169 -0.0061 0.083 Uiso 1 1 calc R . . C27 C 0.1818(3) 0.66802(18) 0.0715(2) 0.0450(8) Uani 1 1 d . . . H27 H 0.1351 0.7158 0.0736 0.054 Uiso 1 1 calc R . . C28 C 0.1458(3) 0.59831(17) 0.11579(19) 0.0355(6) Uani 1 1 d . . . H28 H 0.0752 0.5975 0.1468 0.043 Uiso 1 1 calc R . . C29 C 0.0763(2) 0.24541(16) -0.06337(16) 0.0289(5) Uani 1 1 d . . . C30 C 0.1123(2) 0.30338(16) -0.12399(17) 0.0296(5) Uani 1 1 d . . . H30 H 0.1324 0.3538 -0.1099 0.035 Uiso 1 1 calc R . . C31 C 0.1187(2) 0.28692(18) -0.20554(17) 0.0345(6) Uani 1 1 d . . . H31 H 0.1419 0.3269 -0.2473 0.041 Uiso 1 1 calc R . . C32 C 0.0916(3) 0.21251(18) -0.22666(18) 0.0379(7) Uani 1 1 d . . . H32 H 0.0979 0.2009 -0.2830 0.046 Uiso 1 1 calc R . . C33 C 0.0555(3) 0.15571(18) -0.16560(19) 0.0385(7) Uani 1 1 d . . . H33 H 0.0368 0.1048 -0.1801 0.046 Uiso 1 1 calc R . . C34 C 0.0462(3) 0.17182(17) -0.08316(18) 0.0358(6) Uani 1 1 d . . . H34 H 0.0195 0.1331 -0.0409 0.043 Uiso 1 1 calc R . . C35 C -0.0927(2) 0.15875(17) 0.14492(16) 0.0290(5) Uani 1 1 d . . . C36 C -0.1440(2) 0.23758(18) 0.1499(2) 0.0365(6) Uani 1 1 d . . . H36 H -0.1075 0.2840 0.1290 0.044 Uiso 1 1 calc R . . C37 C -0.2499(3) 0.2484(2) 0.1861(2) 0.0434(7) Uani 1 1 d . . . H37 H -0.2857 0.3025 0.1900 0.052 Uiso 1 1 calc R . . C38 C -0.3038(3) 0.1807(2) 0.2164(2) 0.0440(7) Uani 1 1 d . . . H38 H -0.3760 0.1881 0.2407 0.053 Uiso 1 1 calc R . . C39 C -0.2496(3) 0.1018(2) 0.2103(2) 0.0407(7) Uani 1 1 d . . . H39 H -0.2853 0.0549 0.2307 0.049 Uiso 1 1 calc R . . C40 C -0.1452(2) 0.09126(18) 0.17532(18) 0.0347(6) Uani 1 1 d . . . H40 H -0.1091 0.0373 0.1720 0.042 Uiso 1 1 calc R . . C41 C 0.2253(2) 0.06643(16) 0.02670(17) 0.0288(5) Uani 1 1 d . . . C42 C 0.1833(2) 0.00055(18) 0.00580(19) 0.0355(6) Uani 1 1 d . . . H42 H 0.1229 0.0105 -0.0064 0.043 Uiso 1 1 calc R . . C43 C 0.2300(2) -0.07992(18) 0.0028(2) 0.0375(6) Uani 1 1 d . . . H43 H 0.2021 -0.1257 -0.0119 0.045 Uiso 1 1 calc R . . C44 C 0.3168(2) -0.09332(19) 0.0212(2) 0.0387(6) Uani 1 1 d . . . H44 H 0.3491 -0.1486 0.0188 0.046 Uiso 1 1 calc R . . C45 C 0.3576(2) -0.0274(2) 0.0430(2) 0.0390(6) Uani 1 1 d . . . H45 H 0.4175 -0.0378 0.0558 0.047 Uiso 1 1 calc R . . C46 C 0.3123(2) 0.05351(17) 0.04643(17) 0.0358(6) Uani 1 1 d . . . H46 H 0.3399 0.0991 0.0619 0.043 Uiso 1 1 calc R . . C47A C 0.4024(2) 0.37578(17) 0.28510(17) 0.0577(19) Uiso 0.569(5) 1 d PR A 1 C48A C 0.3280(2) 0.44388(17) 0.30126(17) 0.072(2) Uiso 0.569(5) 1 d PR A 1 H48A H 0.2623 0.4413 0.3429 0.086 Uiso 0.569(5) 1 calc PR A 1 C49A C 0.3509(9) 0.5181(7) 0.2547(7) 0.088(3) Uiso 0.569(5) 1 d P A 1 H49A H 0.3014 0.5639 0.2574 0.106 Uiso 0.569(5) 1 calc PR A 1 C50A C 0.4611(12) 0.5154(10) 0.2014(9) 0.122(4) Uiso 0.569(5) 1 d P A 1 H50A H 0.4875 0.5663 0.1813 0.147 Uiso 0.569(5) 1 calc PR A 1 C51A C 0.5096(8) 0.4605(6) 0.1855(6) 0.082(3) Uiso 0.569(5) 1 d P A 1 H51A H 0.5727 0.4617 0.1401 0.098 Uiso 0.569(5) 1 calc PR A 1 C52A C 0.4902(8) 0.3810(6) 0.2265(6) 0.083(3) Uiso 0.569(5) 1 d P A 1 H52A H 0.5409 0.3342 0.2104 0.099 Uiso 0.569(5) 1 calc PR A 1 C83 C 0.4648(8) 0.4570(8) 0.4439(8) 0.093(4) Uani 0.50 1 d P B 1 H83A H 0.4587 0.4673 0.3886 0.112 Uiso 0.50 1 calc PR B 1 H83B H 0.4467 0.4000 0.4596 0.112 Uiso 0.50 1 calc PR B 1 Cl1 Cl 0.3792(2) 0.52576(19) 0.5155(2) 0.0968(10) Uani 0.50 1 d P . 1 Cl2 Cl 0.5900(2) 0.4596(2) 0.4325(2) 0.0921(9) Uani 0.50 1 d P . 1 C47B C 0.4121(5) 0.3833(3) 0.3098(4) 0.0350(15) Uiso 0.431(5) 1 d PG A 2 C48B C 0.4478(5) 0.4297(4) 0.3593(4) 0.061(2) Uiso 0.431(5) 1 d PG A 2 H48B H 0.4639 0.4043 0.4040 0.074 Uiso 0.431(5) 1 calc PR A 2 C49B C 0.4598(6) 0.5134(4) 0.3436(4) 0.064(3) Uiso 0.431(5) 1 d PG A 2 H49B H 0.4841 0.5451 0.3775 0.077 Uiso 0.431(5) 1 calc PR A 2 C50B C 0.4362(7) 0.5506(3) 0.2783(5) 0.080(3) Uiso 0.431(5) 1 d PG A 2 H50B H 0.4444 0.6077 0.2675 0.096 Uiso 0.431(5) 1 calc PR A 2 C51B C 0.4006(8) 0.5041(5) 0.2287(5) 0.128(7) Uiso 0.431(5) 1 d PG A 2 H51B H 0.3844 0.5296 0.1841 0.153 Uiso 0.431(5) 1 calc PR A 2 C52B C 0.3885(7) 0.4205(5) 0.2444(5) 0.098(4) Uiso 0.431(5) 1 d PG A 2 H52B H 0.3642 0.3887 0.2105 0.117 Uiso 0.431(5) 1 calc PR A 2 C53 C 0.1453(2) 0.35830(15) 0.51042(16) 0.0261(5) Uani 1 1 d . . . C54 C 0.0978(2) 0.29304(16) 0.55544(17) 0.0287(5) Uani 1 1 d . . . H54 H 0.1270 0.2368 0.5400 0.034 Uiso 1 1 calc R . . C55 C 0.0069(2) 0.3112(2) 0.62363(18) 0.0357(6) Uani 1 1 d . . . H55 H -0.0263 0.2670 0.6551 0.043 Uiso 1 1 calc R . . C56 C -0.0358(2) 0.3933(2) 0.6460(2) 0.0419(7) Uani 1 1 d . . . H56 H -0.0973 0.4054 0.6933 0.050 Uiso 1 1 calc R . . C57 C 0.0108(3) 0.4571(2) 0.5997(2) 0.0443(8) Uani 1 1 d . . . H57 H -0.0195 0.5132 0.6142 0.053 Uiso 1 1 calc R . . C58 C 0.1020(2) 0.44038(17) 0.53210(19) 0.0358(6) Uani 1 1 d . . . H58 H 0.1346 0.4848 0.5008 0.043 Uiso 1 1 calc R . . C59 C 0.3906(2) 0.22998(17) 0.48975(19) 0.0322(6) Uani 1 1 d . . . C60 C 0.4941(3) 0.2106(2) 0.4550(2) 0.0496(8) Uani 1 1 d . . . H60 H 0.5256 0.1831 0.4011 0.059 Uiso 1 1 calc R . . C61 C 0.5520(3) 0.2323(3) 0.5009(3) 0.0673(12) Uani 1 1 d . . . H61 H 0.6238 0.2189 0.4781 0.081 Uiso 1 1 calc R . . C62 C 0.5071(4) 0.2726(3) 0.5781(3) 0.0663(12) Uani 1 1 d . . . H62 H 0.5477 0.2877 0.6082 0.080 Uiso 1 1 calc R . . C63 C 0.4034(3) 0.2912(2) 0.6120(3) 0.0560(10) Uani 1 1 d . . . H63 H 0.3722 0.3191 0.6657 0.067 Uiso 1 1 calc R . . C64 C 0.3439(3) 0.26943(19) 0.5682(2) 0.0398(7) Uani 1 1 d . . . H64 H 0.2719 0.2815 0.5919 0.048 Uiso 1 1 calc R . . C65 C 0.49186(18) 0.02512(15) 0.27575(16) 0.0249(5) Uani 1 1 d . . . C66 C 0.5422(2) -0.01242(17) 0.19640(17) 0.0302(5) Uani 1 1 d . . . H66 H 0.5272 0.0082 0.1495 0.036 Uiso 1 1 calc R . . C67 C 0.6147(2) -0.08030(18) 0.18651(19) 0.0364(6) Uani 1 1 d . . . H67 H 0.6494 -0.1068 0.1325 0.044 Uiso 1 1 calc R . . C68 C 0.6369(2) -0.10967(19) 0.2544(2) 0.0390(7) Uani 1 1 d . . . H68 H 0.6867 -0.1564 0.2470 0.047 Uiso 1 1 calc R . . C69 C 0.5871(2) -0.07150(19) 0.3333(2) 0.0359(6) Uani 1 1 d . . . H69 H 0.6027 -0.0921 0.3800 0.043 Uiso 1 1 calc R . . C70 C 0.5143(2) -0.00320(17) 0.34463(17) 0.0299(5) Uani 1 1 d . . . H70 H 0.4804 0.0237 0.3986 0.036 Uiso 1 1 calc R . . C71 C 0.27426(18) -0.06584(15) 0.26122(15) 0.0239(5) Uani 1 1 d . . . C72 C 0.2035(2) -0.08623(17) 0.22858(17) 0.0305(5) Uani 1 1 d . . . H72 H 0.1694 -0.0445 0.2056 0.037 Uiso 1 1 calc R . . C73 C 0.1830(2) -0.1685(2) 0.2299(2) 0.0396(7) Uani 1 1 d . . . H73 H 0.1354 -0.1835 0.2066 0.048 Uiso 1 1 calc R . . C74 C 0.2312(2) -0.22890(18) 0.2646(2) 0.0410(7) Uani 1 1 d . . . H74 H 0.2174 -0.2853 0.2646 0.049 Uiso 1 1 calc R . . C75 C 0.2991(2) -0.20715(17) 0.2991(2) 0.0374(6) Uani 1 1 d . . . H75 H 0.3302 -0.2485 0.3247 0.045 Uiso 1 1 calc R . . C76 C 0.3231(2) -0.12533(16) 0.29709(18) 0.0309(5) Uani 1 1 d . . . H76 H 0.3714 -0.1107 0.3196 0.037 Uiso 1 1 calc R . . C77 C 0.21112(19) 0.04148(14) 0.47712(15) 0.0222(4) Uani 1 1 d . . . C78 C 0.1092(2) 0.06036(15) 0.49047(16) 0.0249(5) Uani 1 1 d . . . H78 H 0.0875 0.0710 0.4445 0.030 Uiso 1 1 calc R . . C79 C 0.0387(2) 0.06348(16) 0.57291(17) 0.0283(5) Uani 1 1 d . . . H79 H -0.0318 0.0766 0.5831 0.034 Uiso 1 1 calc R . . C80 C 0.0704(2) 0.04766(17) 0.64005(17) 0.0319(6) Uani 1 1 d . . . H80 H 0.0218 0.0486 0.6958 0.038 Uiso 1 1 calc R . . C81 C 0.1731(2) 0.03053(19) 0.62540(17) 0.0340(6) Uani 1 1 d . . . H81 H 0.1951 0.0210 0.6714 0.041 Uiso 1 1 calc R . . C82 C 0.2443(2) 0.02717(17) 0.54384(16) 0.0290(5) Uani 1 1 d . . . H82 H 0.3148 0.0152 0.5337 0.035 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 Ru 0.02676(10) 0.01931(9) 0.02000(9) -0.00131(7) -0.00908(8) 0.00031(7) Rh2 0.02477(9) 0.01549(8) 0.01708(9) 0.00015(6) -0.00836(7) 0.00103(6) Rh3 0.02661(10) 0.01648(9) 0.01757(9) -0.00017(6) -0.00801(7) 0.00055(6) S1 0.0305(3) 0.0163(2) 0.0210(3) -0.0014(2) -0.0106(2) 0.0006(2) S2 0.0280(3) 0.0167(2) 0.0204(3) 0.0007(2) -0.0096(2) 0.0004(2) P1 0.0280(3) 0.0180(3) 0.0240(3) 0.0029(2) -0.0118(2) -0.0013(2) P2 0.0309(3) 0.0177(3) 0.0190(3) 0.0011(2) -0.0105(2) -0.0017(2) P3 0.0300(3) 0.0202(3) 0.0242(3) -0.0007(2) -0.0098(3) -0.0030(2) P4 0.0249(3) 0.0185(3) 0.0186(3) -0.0004(2) -0.0074(2) 0.0008(2) O2 0.0297(9) 0.0216(8) 0.0223(8) 0.0029(6) -0.0115(7) 0.0008(7) O1 0.0289(10) 0.0326(10) 0.0329(10) 0.0127(8) -0.0040(8) 0.0024(8) O3 0.0620(14) 0.0228(9) 0.0492(12) 0.0100(8) -0.0401(11) -0.0125(9) O4 0.0519(12) 0.0200(8) 0.0248(9) 0.0016(7) -0.0195(9) -0.0039(8) O6 0.0399(11) 0.0251(9) 0.0256(9) -0.0008(7) -0.0085(8) 0.0000(8) O5 0.0354(10) 0.0217(8) 0.0298(9) 0.0005(7) -0.0120(8) -0.0028(7) O9 0.0358(10) 0.0215(8) 0.0351(10) -0.0011(7) -0.0207(8) -0.0020(7) O8 0.0369(10) 0.0183(8) 0.0320(10) -0.0030(7) -0.0158(8) -0.0023(7) O7 0.0369(11) 0.0364(11) 0.0421(12) -0.0015(9) -0.0062(9) -0.0127(9) O10 0.0255(9) 0.0220(8) 0.0303(9) 0.0011(7) -0.0088(7) -0.0016(7) O11 0.0359(10) 0.0203(8) 0.0234(9) -0.0011(6) -0.0121(7) -0.0017(7) O12 0.0309(9) 0.0230(8) 0.0193(8) 0.0009(6) -0.0066(7) 0.0048(7) C1 0.0321(13) 0.0255(12) 0.0308(13) -0.0017(10) -0.0108(11) 0.0056(10) C2 0.0333(14) 0.0280(13) 0.0236(12) -0.0045(10) -0.0087(10) 0.0010(10) C3 0.0343(14) 0.0322(13) 0.0231(12) 0.0026(10) -0.0087(11) 0.0005(11) C4 0.0347(14) 0.0222(12) 0.0374(15) 0.0003(10) -0.0103(12) -0.0045(10) C5 0.0303(14) 0.0376(15) 0.0322(14) -0.0075(11) -0.0086(11) -0.0068(11) C6 0.0302(14) 0.0421(15) 0.0299(14) -0.0032(11) -0.0139(11) 0.0034(11) C11 0.0254(12) 0.0243(12) 0.0364(14) 0.0077(10) -0.0066(11) -0.0046(9) C12 0.0278(13) 0.0348(14) 0.0414(16) 0.0066(12) -0.0099(12) -0.0036(11) C13 0.0313(15) 0.0413(16) 0.0511(19) 0.0088(14) -0.0169(13) -0.0007(12) C14 0.0325(15) 0.0381(16) 0.053(2) -0.0008(14) -0.0096(14) 0.0027(12) C15 0.0394(16) 0.0424(17) 0.0386(16) 0.0001(13) -0.0071(13) 0.0013(13) C16 0.0344(15) 0.0378(15) 0.0381(16) 0.0084(12) -0.0099(12) -0.0027(12) C17 0.0295(12) 0.0159(10) 0.0269(12) 0.0039(9) -0.0115(10) 0.0010(8) C18 0.0374(14) 0.0277(13) 0.0277(13) 0.0021(10) -0.0130(11) 0.0050(10) C19 0.0427(17) 0.0390(16) 0.0338(15) 0.0064(12) -0.0043(13) 0.0094(13) C20 0.0309(15) 0.0434(18) 0.062(2) 0.0149(16) -0.0107(15) 0.0043(13) C21 0.0398(16) 0.0366(16) 0.061(2) 0.0150(14) -0.0293(16) -0.0051(12) C22 0.0411(15) 0.0232(12) 0.0373(15) 0.0065(10) -0.0224(12) -0.0044(10) C23 0.0528(19) 0.0221(13) 0.066(2) 0.0112(13) -0.0394(17) -0.0141(12) C24 0.049(2) 0.0336(19) 0.191(6) 0.033(3) -0.057(3) -0.0153(16) C25 0.051(3) 0.044(2) 0.216(7) 0.036(3) -0.038(3) -0.0237(19) C26 0.075(3) 0.0297(17) 0.111(4) 0.022(2) -0.040(3) -0.0239(17) C27 0.068(2) 0.0199(13) 0.060(2) 0.0034(13) -0.0388(18) -0.0054(13) C28 0.0483(17) 0.0235(13) 0.0392(15) -0.0020(11) -0.0215(13) -0.0035(11) C29 0.0430(15) 0.0233(12) 0.0227(12) -0.0001(9) -0.0157(11) -0.0004(10) C30 0.0380(14) 0.0237(12) 0.0274(13) 0.0016(10) -0.0132(11) -0.0009(10) C31 0.0449(16) 0.0312(14) 0.0244(13) 0.0032(10) -0.0120(12) 0.0060(11) C32 0.0564(19) 0.0339(14) 0.0257(13) -0.0052(11) -0.0222(13) 0.0113(13) C33 0.063(2) 0.0253(13) 0.0369(15) -0.0028(11) -0.0310(15) 0.0003(12) C34 0.0578(19) 0.0256(13) 0.0320(14) 0.0040(11) -0.0256(14) -0.0059(12) C35 0.0349(14) 0.0318(13) 0.0238(12) -0.0002(10) -0.0144(11) -0.0052(10) C36 0.0435(16) 0.0301(14) 0.0389(16) 0.0012(11) -0.0173(13) -0.0086(12) C37 0.0456(18) 0.0377(16) 0.0483(19) -0.0060(13) -0.0204(15) 0.0018(13) C38 0.0364(16) 0.058(2) 0.0397(17) -0.0026(14) -0.0149(13) -0.0084(14) C39 0.0464(17) 0.0424(17) 0.0398(16) 0.0076(13) -0.0196(14) -0.0192(14) C40 0.0456(16) 0.0310(14) 0.0339(14) 0.0026(11) -0.0209(13) -0.0088(12) C41 0.0347(14) 0.0247(12) 0.0258(12) -0.0031(9) -0.0114(11) 0.0032(10) C42 0.0387(15) 0.0310(14) 0.0398(16) -0.0088(11) -0.0193(13) 0.0011(11) C43 0.0474(17) 0.0265(13) 0.0415(16) -0.0071(11) -0.0209(14) 0.0005(12) C44 0.0402(16) 0.0332(15) 0.0385(16) -0.0065(12) -0.0126(13) 0.0080(12) C45 0.0334(15) 0.0417(16) 0.0441(17) 0.0060(13) -0.0173(13) -0.0021(12) C46 0.0427(16) 0.0363(15) 0.0319(14) 0.0037(11) -0.0158(12) -0.0118(12) C83 0.078(7) 0.096(8) 0.109(9) -0.040(7) -0.042(7) 0.004(6) Cl1 0.0622(16) 0.0865(19) 0.110(2) -0.0191(17) 0.0037(16) 0.0025(13) Cl2 0.0539(14) 0.103(2) 0.092(2) 0.0123(17) 0.0062(13) -0.0116(13) C53 0.0357(13) 0.0224(11) 0.0248(12) -0.0040(9) -0.0182(10) 0.0024(9) C54 0.0319(13) 0.0258(12) 0.0310(13) -0.0017(10) -0.0162(11) 0.0024(10) C55 0.0342(14) 0.0446(16) 0.0298(14) 0.0004(12) -0.0154(12) 0.0017(12) C56 0.0393(16) 0.0540(19) 0.0312(15) -0.0151(13) -0.0159(13) 0.0112(14) C57 0.059(2) 0.0328(15) 0.0454(18) -0.0200(13) -0.0298(16) 0.0154(14) C58 0.0512(17) 0.0223(12) 0.0394(16) -0.0077(11) -0.0254(14) 0.0045(11) C59 0.0343(14) 0.0267(13) 0.0427(16) 0.0020(11) -0.0224(12) -0.0035(10) C60 0.0341(16) 0.061(2) 0.054(2) -0.0011(17) -0.0183(15) -0.0003(15) C61 0.0381(19) 0.084(3) 0.090(3) 0.012(3) -0.035(2) -0.0114(19) C62 0.078(3) 0.063(2) 0.091(3) 0.007(2) -0.068(3) -0.020(2) C63 0.077(3) 0.0456(19) 0.064(2) -0.0109(17) -0.051(2) -0.0001(18) C64 0.0466(17) 0.0355(15) 0.0468(18) -0.0055(13) -0.0303(15) 0.0027(12) C65 0.0215(11) 0.0224(11) 0.0297(12) -0.0001(9) -0.0082(10) -0.0020(9) C66 0.0287(13) 0.0326(13) 0.0266(13) 0.0015(10) -0.0062(10) -0.0058(10) C67 0.0278(13) 0.0358(15) 0.0348(15) -0.0061(12) 0.0006(11) -0.0004(11) C68 0.0259(13) 0.0326(14) 0.0531(19) 0.0015(13) -0.0095(13) 0.0015(11) C69 0.0310(14) 0.0361(15) 0.0440(16) 0.0062(12) -0.0182(12) -0.0025(11) C70 0.0278(13) 0.0316(13) 0.0300(13) -0.0022(10) -0.0103(10) -0.0031(10) C71 0.0234(11) 0.0213(11) 0.0226(11) -0.0050(9) -0.0039(9) 0.0002(9) C72 0.0271(13) 0.0326(13) 0.0306(13) -0.0032(10) -0.0099(11) -0.0003(10) C73 0.0343(15) 0.0415(16) 0.0447(17) -0.0066(13) -0.0142(13) -0.0108(12) C74 0.0366(15) 0.0266(14) 0.0538(19) -0.0038(12) -0.0080(14) -0.0081(11) C75 0.0322(14) 0.0241(13) 0.0510(18) 0.0033(12) -0.0105(13) -0.0001(10) C76 0.0290(13) 0.0250(12) 0.0395(15) 0.0001(10) -0.0139(11) -0.0015(10) C77 0.0289(12) 0.0168(10) 0.0198(11) 0.0003(8) -0.0074(9) -0.0029(8) C78 0.0312(13) 0.0206(11) 0.0239(12) 0.0026(9) -0.0114(10) -0.0022(9) C79 0.0279(13) 0.0227(12) 0.0316(13) 0.0001(10) -0.0077(10) -0.0024(9) C80 0.0372(14) 0.0312(13) 0.0231(12) -0.0031(10) -0.0050(11) -0.0068(11) C81 0.0406(15) 0.0424(16) 0.0222(12) -0.0003(11) -0.0140(11) -0.0087(12) C82 0.0290(13) 0.0349(14) 0.0251(12) 0.0009(10) -0.0121(10) -0.0043(10) _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 Ru C6 2.160(3) . ? Ru C3 2.171(3) . ? Ru C5 2.195(3) . ? Ru C1 2.201(3) . ? Ru C2 2.205(3) . ? Ru C4 2.216(3) . ? Ru S2 2.3198(6) . ? Ru S1 2.3271(6) . ? Rh2 P2 2.1719(6) . ? Rh2 P1 2.1815(6) . ? Rh2 S1 2.3305(6) . ? Rh2 S2 2.3439(6) . ? Rh3 P3 2.1718(7) . ? Rh3 P4 2.1795(6) . ? Rh3 S1 2.3350(6) . ? Rh3 S2 2.3425(6) . ? P1 O2 1.6135(18) . ? P1 O3 1.617(2) . ? P1 O1 1.624(2) . ? P2 O4 1.6112(19) . ? P2 O5 1.6246(19) . ? P2 O6 1.625(2) . ? P3 O7 1.617(2) . ? P3 O9 1.6185(19) . ? P3 O8 1.6220(18) . ? P4 O11 1.6115(18) . ? P4 O12 1.6192(18) . ? P4 O10 1.6223(19) . ? O2 C17 1.390(3) . ? O1 C11 1.380(3) . ? O3 C23 1.413(3) . ? O4 C29 1.394(3) . ? O6 C41 1.394(3) . ? O5 C35 1.394(3) . ? O9 C59 1.404(3) . ? O8 C53 1.377(3) . ? O7 C47B 1.383(5) . ? O7 C47A 1.432(3) . ? O10 C65 1.398(3) . ? O11 C71 1.390(3) . ? O12 C77 1.384(3) . ? C1 C2 1.403(4) . ? C1 C6 1.417(4) . ? C1 H1 0.9500 . ? C2 C3 1.421(4) . ? C2 H2 0.9500 . ? C3 C4 1.405(4) . ? C3 H3 0.9500 . ? C4 C5 1.413(4) . ? C4 H4 0.9500 . ? C5 C6 1.421(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C11 C12 1.382(4) . ? C11 C16 1.389(4) . ? C12 C13 1.403(4) . ? C12 H12 0.9500 . ? C13 C14 1.379(5) . ? C13 H13 0.9500 . ? C14 C15 1.385(5) . ? C14 H14 0.9500 . ? C15 C16 1.387(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.382(4) . ? C17 C22 1.386(4) . ? C18 C19 1.390(4) . ? C18 H18 0.9500 . ? C19 C20 1.378(5) . ? C19 H19 0.9500 . ? C20 C21 1.385(5) . ? C20 H20 0.9500 . ? C21 C22 1.383(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.376(6) . ? C23 C28 1.379(4) . ? C24 C25 1.403(6) . ? C24 H24 0.9500 . ? C25 C26 1.376(6) . ? C25 H25 0.9500 . ? C26 C27 1.363(6) . ? C26 H26 0.9500 . ? C27 C28 1.389(4) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.383(4) . ? C29 C34 1.388(4) . ? C30 C31 1.385(4) . ? C30 H30 0.9500 . ? C31 C32 1.387(4) . ? C31 H31 0.9500 . ? C32 C33 1.375(4) . ? C32 H32 0.9500 . ? C33 C34 1.386(4) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C40 1.378(4) . ? C35 C36 1.379(4) . ? C36 C37 1.393(5) . ? C36 H36 0.9500 . ? C37 C38 1.389(5) . ? C37 H37 0.9500 . ? C38 C39 1.396(5) . ? C38 H38 0.9500 . ? C39 C40 1.373(5) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.381(4) . ? C41 C46 1.388(4) . ? C42 C43 1.382(4) . ? C42 H42 0.9500 . ? C43 C44 1.373(4) . ? C43 H43 0.9500 . ? C44 C45 1.377(4) . ? C44 H44 0.9500 . ? C45 C46 1.381(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47A C52A 1.295(10) . ? C47A C48A 1.3900 . ? C48A C49A 1.434(11) . ? C48A H48A 0.9500 . ? C49A C50A 1.49(2) . ? C49A H49A 0.9500 . ? C50A C51A 1.031(15) . ? C50A H50A 0.9500 . ? C51A C52A 1.460(13) . ? C51A H51A 0.9500 . ? C52A H52A 0.9500 . ? C83 Cl1 1.683(11) . ? C83 Cl2 1.722(11) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? Cl1 Cl2 1.157(4) 2_666 ? Cl2 Cl1 1.158(4) 2_666 ? C47B C48B 1.3900 . ? C47B C52B 1.3900 . ? C48B C49B 1.3900 . ? C48B H48B 0.9500 . ? C49B C50B 1.3900 . ? C49B H49B 0.9500 . ? C50B C51B 1.3900 . ? C50B H50B 0.9500 . ? C51B C52B 1.3900 . ? C51B H51B 0.9500 . ? C52B H52B 0.9500 . ? C53 C54 1.386(4) . ? C53 C58 1.387(3) . ? C54 C55 1.391(4) . ? C54 H54 0.9500 . ? C55 C56 1.388(4) . ? C55 H55 0.9500 . ? C56 C57 1.371(5) . ? C56 H56 0.9500 . ? C57 C58 1.385(5) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C60 1.369(4) . ? C59 C64 1.381(4) . ? C60 C61 1.394(5) . ? C60 H60 0.9500 . ? C61 C62 1.367(7) . ? C61 H61 0.9500 . ? C62 C63 1.370(6) . ? C62 H62 0.9500 . ? C63 C64 1.385(4) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 C66 1.385(4) . ? C65 C70 1.387(4) . ? C66 C67 1.383(4) . ? C66 H66 0.9500 . ? C67 C68 1.374(5) . ? C67 H67 0.9500 . ? C68 C69 1.383(4) . ? C68 H68 0.9500 . ? C69 C70 1.387(4) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? C71 C72 1.382(4) . ? C71 C76 1.389(4) . ? C72 C73 1.387(4) . ? C72 H72 0.9500 . ? C73 C74 1.381(5) . ? C73 H73 0.9500 . ? C74 C75 1.373(5) . ? C74 H74 0.9500 . ? C75 C76 1.395(4) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77 C78 1.379(4) . ? C77 C82 1.390(3) . ? C78 C79 1.396(4) . ? C78 H78 0.9500 . ? C79 C80 1.387(4) . ? C79 H79 0.9500 . ? C80 C81 1.384(4) . ? C80 H80 0.9500 . ? C81 C82 1.388(4) . ? C81 H81 0.9500 . ? C82 H82 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 C6 Ru C3 80.82(11) . . ? C6 Ru C5 38.07(11) . . ? C3 Ru C5 67.74(11) . . ? C6 Ru C1 37.90(10) . . ? C3 Ru C1 67.84(10) . . ? C5 Ru C1 68.10(11) . . ? C6 Ru C2 67.94(10) . . ? C3 Ru C2 37.89(10) . . ? C5 Ru C2 80.15(10) . . ? C1 Ru C2 37.13(10) . . ? C6 Ru C4 68.11(11) . . ? C3 Ru C4 37.34(10) . . ? C5 Ru C4 37.37(11) . . ? C1 Ru C4 79.93(10) . . ? C2 Ru C4 67.60(10) . . ? C6 Ru S2 123.77(8) . . ? C3 Ru S2 125.55(7) . . ? C5 Ru S2 101.11(8) . . ? C1 Ru S2 159.60(7) . . ? C2 Ru S2 161.72(7) . . ? C4 Ru S2 102.22(7) . . ? C6 Ru S1 123.26(8) . . ? C3 Ru S1 125.62(8) . . ? C5 Ru S1 159.33(8) . . ? C1 Ru S1 100.74(8) . . ? C2 Ru S1 101.64(7) . . ? C4 Ru S1 161.46(8) . . ? S2 Ru S1 83.68(2) . . ? P2 Rh2 P1 91.71(2) . . ? P2 Rh2 S1 171.55(2) . . ? P1 Rh2 S1 94.91(2) . . ? P2 Rh2 S2 90.76(2) . . ? P1 Rh2 S2 174.81(2) . . ? S1 Rh2 S2 83.07(2) . . ? P3 Rh3 P4 90.60(2) . . ? P3 Rh3 S1 92.41(2) . . ? P4 Rh3 S1 173.55(2) . . ? P3 Rh3 S2 173.01(2) . . ? P4 Rh3 S2 94.51(2) . . ? S1 Rh3 S2 83.01(2) . . ? Ru S1 Rh2 77.004(19) . . ? Ru S1 Rh3 80.13(2) . . ? Rh2 S1 Rh3 84.90(2) . . ? Ru S2 Rh3 80.123(19) . . ? Ru S2 Rh2 76.882(18) . . ? Rh3 S2 Rh2 84.43(2) . . ? O2 P1 O3 101.77(10) . . ? O2 P1 O1 90.06(10) . . ? O3 P1 O1 101.47(12) . . ? O2 P1 Rh2 123.17(7) . . ? O3 P1 Rh2 115.48(8) . . ? O1 P1 Rh2 120.11(8) . . ? O4 P2 O5 103.99(10) . . ? O4 P2 O6 96.37(10) . . ? O5 P2 O6 96.02(10) . . ? O4 P2 Rh2 114.83(7) . . ? O5 P2 Rh2 119.72(7) . . ? O6 P2 Rh2 121.76(8) . . ? O7 P3 O9 98.11(12) . . ? O7 P3 O8 95.56(11) . . ? O9 P3 O8 101.92(10) . . ? O7 P3 Rh3 121.44(9) . . ? O9 P3 Rh3 114.85(7) . . ? O8 P3 Rh3 120.66(8) . . ? O11 P4 O12 99.38(9) . . ? O11 P4 O10 100.05(10) . . ? O12 P4 O10 99.08(10) . . ? O11 P4 Rh3 118.12(7) . . ? O12 P4 Rh3 122.85(7) . . ? O10 P4 Rh3 113.46(7) . . ? C17 O2 P1 124.81(15) . . ? C11 O1 P1 125.64(17) . . ? C23 O3 P1 120.39(19) . . ? C29 O4 P2 127.64(16) . . ? C41 O6 P2 127.66(17) . . ? C35 O5 P2 125.82(17) . . ? C59 O9 P3 124.04(17) . . ? C53 O8 P3 126.77(16) . . ? C47B O7 P3 129.0(3) . . ? C47A O7 P3 123.79(19) . . ? C65 O10 P4 122.56(15) . . ? C71 O11 P4 131.17(16) . . ? C77 O12 P4 128.56(15) . . ? C2 C1 C6 119.8(2) . . ? C2 C1 Ru 71.60(15) . . ? C6 C1 Ru 69.47(15) . . ? C2 C1 H1 120.1 . . ? C6 C1 H1 120.1 . . ? Ru C1 H1 131.6 . . ? C1 C2 C3 119.5(2) . . ? C1 C2 Ru 71.27(15) . . ? C3 C2 Ru 69.74(15) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? Ru C2 H2 131.5 . . ? C4 C3 C2 121.0(3) . . ? C4 C3 Ru 73.08(16) . . ? C2 C3 Ru 72.36(15) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? Ru C3 H3 127.1 . . ? C3 C4 C5 119.4(2) . . ? C3 C4 Ru 69.58(15) . . ? C5 C4 Ru 70.48(16) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? Ru C4 H4 132.6 . . ? C4 C5 C6 119.7(2) . . ? C4 C5 Ru 72.15(16) . . ? C6 C5 Ru 69.64(16) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? Ru C5 H5 130.7 . . ? C1 C6 C5 120.3(3) . . ? C1 C6 Ru 72.63(16) . . ? C5 C6 Ru 72.29(16) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? Ru C6 H6 127.3 . . ? O1 C11 C12 123.3(3) . . ? O1 C11 C16 115.1(2) . . ? C12 C11 C16 121.6(3) . . ? C11 C12 C13 118.2(3) . . ? C11 C12 H12 120.9 . . ? C13 C12 H12 120.9 . . ? C14 C13 C12 120.7(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.1(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 120.2(3) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 119.2(3) . . ? C15 C16 H16 120.4 . . ? C11 C16 H16 120.4 . . ? C18 C17 C22 122.0(3) . . ? C18 C17 O2 122.6(2) . . ? C22 C17 O2 115.3(2) . . ? C17 C18 C19 118.2(3) . . ? C17 C18 H18 120.9 . . ? C19 C18 H18 120.9 . . ? C20 C19 C18 120.8(3) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 119.9(3) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 120.4(3) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C17 118.6(3) . . ? C21 C22 H22 120.7 . . ? C17 C22 H22 120.7 . . ? C24 C23 C28 121.2(3) . . ? C24 C23 O3 119.2(3) . . ? C28 C23 O3 119.6(3) . . ? C23 C24 C25 119.1(4) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C26 C25 C24 119.8(4) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C27 C26 C25 120.0(4) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 121.4(3) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C23 C28 C27 118.5(3) . . ? C23 C28 H28 120.7 . . ? C27 C28 H28 120.7 . . ? C30 C29 C34 120.9(2) . . ? C30 C29 O4 115.9(2) . . ? C34 C29 O4 123.1(2) . . ? C29 C30 C31 119.1(3) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C30 C31 C32 120.5(3) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C33 C32 C31 119.6(3) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C34 120.8(3) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C33 C34 C29 119.0(3) . . ? C33 C34 H34 120.5 . . ? C29 C34 H34 120.5 . . ? C40 C35 C36 120.7(3) . . ? C40 C35 O5 115.7(2) . . ? C36 C35 O5 123.6(2) . . ? C35 C36 C37 119.2(3) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C38 C37 C36 120.7(3) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 118.6(3) . . ? C37 C38 H38 120.7 . . ? C39 C38 H38 120.7 . . ? C40 C39 C38 120.7(3) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C35 120.1(3) . . ? C39 C40 H40 119.9 . . ? C35 C40 H40 119.9 . . ? C42 C41 C46 121.5(2) . . ? C42 C41 O6 119.2(2) . . ? C46 C41 O6 118.8(2) . . ? C41 C42 C43 119.3(3) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C44 C43 C42 119.7(3) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C43 C44 C45 120.7(3) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C44 C45 C46 120.7(3) . . ? C44 C45 H45 119.6 . . ? C46 C45 H45 119.6 . . ? C45 C46 C41 118.1(2) . . ? C45 C46 H46 120.9 . . ? C41 C46 H46 120.9 . . ? C52A C47A C48A 118.4(5) . . ? C52A C47A O7 115.0(5) . . ? C48A C47A O7 126.21(14) . . ? C47A C48A C49A 119.6(5) . . ? C47A C48A H48A 120.2 . . ? C49A C48A H48A 120.2 . . ? C48A C49A C50A 112.5(10) . . ? C48A C49A H49A 123.8 . . ? C50A C49A H49A 123.7 . . ? C51A C50A C49A 122.6(16) . . ? C51A C50A H50A 118.7 . . ? C49A C50A H50A 118.7 . . ? C50A C51A C52A 126.0(14) . . ? C50A C51A H51A 117.0 . . ? C52A C51A H51A 117.0 . . ? C47A C52A C51A 118.6(9) . . ? C47A C52A H52A 120.7 . . ? C51A C52A H52A 120.7 . . ? Cl1 C83 Cl2 115.9(6) . . ? Cl1 C83 H83A 108.3 . . ? Cl2 C83 H83A 108.3 . . ? Cl1 C83 H83B 108.3 . . ? Cl2 C83 H83B 108.3 . . ? H83A C83 H83B 107.4 . . ? Cl2 Cl1 C83 109.3(5) 2_666 . ? Cl1 Cl2 C83 127.2(5) 2_666 . ? O7 C47B C48B 116.1(4) . . ? O7 C47B C52B 123.8(4) . . ? C48B C47B C52B 120.0 . . ? C49B C48B C47B 120.0 . . ? C49B C48B H48B 120.0 . . ? C47B C48B H48B 120.0 . . ? C48B C49B C50B 120.0 . . ? C48B C49B H49B 120.0 . . ? C50B C49B H49B 120.0 . . ? C51B C50B C49B 120.0 . . ? C51B C50B H50B 120.0 . . ? C49B C50B H50B 120.0 . . ? C50B C51B C52B 120.0 . . ? C50B C51B H51B 120.0 . . ? C52B C51B H51B 120.0 . . ? C51B C52B C47B 120.0 . . ? C51B C52B H52B 120.0 . . ? C47B C52B H52B 120.0 . . ? O8 C53 C54 123.7(2) . . ? O8 C53 C58 115.6(2) . . ? C54 C53 C58 120.6(3) . . ? C53 C54 C55 119.0(3) . . ? C53 C54 H54 120.5 . . ? C55 C54 H54 120.5 . . ? C56 C55 C54 120.4(3) . . ? C56 C55 H55 119.8 . . ? C54 C55 H55 119.8 . . ? C57 C56 C55 119.9(3) . . ? C57 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C56 C57 C58 120.5(3) . . ? C56 C57 H57 119.8 . . ? C58 C57 H57 119.8 . . ? C57 C58 C53 119.6(3) . . ? C57 C58 H58 120.2 . . ? C53 C58 H58 120.2 . . ? C60 C59 C64 121.4(3) . . ? C60 C59 O9 118.6(3) . . ? C64 C59 O9 119.9(3) . . ? C59 C60 C61 118.2(4) . . ? C59 C60 H60 120.9 . . ? C61 C60 H60 120.9 . . ? C62 C61 C60 121.1(4) . . ? C62 C61 H61 119.4 . . ? C60 C61 H61 119.4 . . ? C61 C62 C63 119.9(3) . . ? C61 C62 H62 120.1 . . ? C63 C62 H62 120.1 . . ? C62 C63 C64 120.2(4) . . ? C62 C63 H63 119.9 . . ? C64 C63 H63 119.9 . . ? C59 C64 C63 119.1(3) . . ? C59 C64 H64 120.4 . . ? C63 C64 H64 120.4 . . ? C66 C65 C70 121.2(2) . . ? C66 C65 O10 119.2(2) . . ? C70 C65 O10 119.6(2) . . ? C67 C66 C65 119.0(3) . . ? C67 C66 H66 120.5 . . ? C65 C66 H66 120.5 . . ? C68 C67 C66 120.4(3) . . ? C68 C67 H67 119.8 . . ? C66 C67 H67 119.8 . . ? C67 C68 C69 120.3(3) . . ? C67 C68 H68 119.8 . . ? C69 C68 H68 119.8 . . ? C68 C69 C70 120.2(3) . . ? C68 C69 H69 119.9 . . ? C70 C69 H69 119.9 . . ? C69 C70 C65 118.8(3) . . ? C69 C70 H70 120.6 . . ? C65 C70 H70 120.6 . . ? C72 C71 C76 121.5(2) . . ? C72 C71 O11 116.2(2) . . ? C76 C71 O11 122.1(2) . . ? C71 C72 C73 119.0(3) . . ? C71 C72 H72 120.5 . . ? C73 C72 H72 120.5 . . ? C74 C73 C72 120.6(3) . . ? C74 C73 H73 119.7 . . ? C72 C73 H73 119.7 . . ? C75 C74 C73 119.8(3) . . ? C75 C74 H74 120.1 . . ? C73 C74 H74 120.1 . . ? C74 C75 C76 121.1(3) . . ? C74 C75 H75 119.5 . . ? C76 C75 H75 119.5 . . ? C71 C76 C75 118.1(3) . . ? C71 C76 H76 121.0 . . ? C75 C76 H76 121.0 . . ? C78 C77 O12 122.6(2) . . ? C78 C77 C82 121.4(2) . . ? O12 C77 C82 116.0(2) . . ? C77 C78 C79 118.7(2) . . ? C77 C78 H78 120.7 . . ? C79 C78 H78 120.7 . . ? C80 C79 C78 120.7(3) . . ? C80 C79 H79 119.7 . . ? C78 C79 H79 119.7 . . ? C81 C80 C79 119.7(3) . . ? C81 C80 H80 120.1 . . ? C79 C80 H80 120.1 . . ? C80 C81 C82 120.4(3) . . ? C80 C81 H81 119.8 . . ? C82 C81 H81 119.8 . . ? C81 C82 C77 119.2(3) . . ? C81 C82 H82 120.4 . . ? C77 C82 H82 120.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Ru S1 Rh2 -81.35(9) . . . . ? C3 Ru S1 Rh2 175.05(9) . . . . ? C5 Ru S1 Rh2 -59.6(2) . . . . ? C1 Ru S1 Rh2 -114.62(7) . . . . ? C2 Ru S1 Rh2 -152.48(7) . . . . ? C4 Ru S1 Rh2 155.1(2) . . . . ? S2 Ru S1 Rh2 45.240(18) . . . . ? C6 Ru S1 Rh3 -168.34(9) . . . . ? C3 Ru S1 Rh3 88.05(9) . . . . ? C5 Ru S1 Rh3 -146.6(2) . . . . ? C1 Ru S1 Rh3 158.39(7) . . . . ? C2 Ru S1 Rh3 120.53(7) . . . . ? C4 Ru S1 Rh3 68.1(2) . . . . ? S2 Ru S1 Rh3 -41.753(19) . . . . ? P1 Rh2 S1 Ru 140.09(2) . . . . ? S2 Rh2 S1 Ru -44.718(19) . . . . ? P1 Rh2 S1 Rh3 -138.89(2) . . . . ? S2 Rh2 S1 Rh3 36.31(2) . . . . ? P3 Rh3 S1 Ru -133.38(2) . . . . ? S2 Rh3 S1 Ru 41.328(19) . . . . ? P3 Rh3 S1 Rh2 148.95(2) . . . . ? S2 Rh3 S1 Rh2 -36.34(2) . . . . ? C6 Ru S2 Rh3 167.73(10) . . . . ? C3 Ru S2 Rh3 -88.27(10) . . . . ? C5 Ru S2 Rh3 -158.76(8) . . . . ? C1 Ru S2 Rh3 145.5(2) . . . . ? C2 Ru S2 Rh3 -66.6(2) . . . . ? C4 Ru S2 Rh3 -120.58(8) . . . . ? S1 Ru S2 Rh3 41.591(19) . . . . ? C6 Ru S2 Rh2 81.20(10) . . . . ? C3 Ru S2 Rh2 -174.80(9) . . . . ? C5 Ru S2 Rh2 114.71(8) . . . . ? C1 Ru S2 Rh2 58.9(2) . . . . ? C2 Ru S2 Rh2 -153.1(2) . . . . ? C4 Ru S2 Rh2 152.89(8) . . . . ? S1 Ru S2 Rh2 -44.938(19) . . . . ? P4 Rh3 S2 Ru 144.50(2) . . . . ? S1 Rh3 S2 Ru -41.487(19) . . . . ? P4 Rh3 S2 Rh2 -137.89(2) . . . . ? S1 Rh3 S2 Rh2 36.13(2) . . . . ? P2 Rh2 S2 Ru -129.28(2) . . . . ? S1 Rh2 S2 Ru 44.92(2) . . . . ? P2 Rh2 S2 Rh3 149.59(2) . . . . ? S1 Rh2 S2 Rh3 -36.20(2) . . . . ? P2 Rh2 P1 O2 62.78(8) . . . . ? S1 Rh2 P1 O2 -111.96(8) . . . . ? P2 Rh2 P1 O3 -171.66(10) . . . . ? S1 Rh2 P1 O3 13.60(10) . . . . ? P2 Rh2 P1 O1 -49.58(10) . . . . ? S1 Rh2 P1 O1 135.67(9) . . . . ? P1 Rh2 P2 O4 -20.18(9) . . . . ? S2 Rh2 P2 O4 164.39(9) . . . . ? P1 Rh2 P2 O5 -144.99(8) . . . . ? S2 Rh2 P2 O5 39.57(8) . . . . ? P1 Rh2 P2 O6 95.31(9) . . . . ? S2 Rh2 P2 O6 -80.13(9) . . . . ? P4 Rh3 P3 O7 85.74(10) . . . . ? S1 Rh3 P3 O7 -88.55(10) . . . . ? P4 Rh3 P3 O9 -31.99(9) . . . . ? S1 Rh3 P3 O9 153.72(9) . . . . ? P4 Rh3 P3 O8 -154.63(9) . . . . ? S1 Rh3 P3 O8 31.08(9) . . . . ? P3 Rh3 P4 O11 -161.84(8) . . . . ? S2 Rh3 P4 O11 22.95(8) . . . . ? P3 Rh3 P4 O12 73.76(9) . . . . ? S2 Rh3 P4 O12 -101.46(9) . . . . ? P3 Rh3 P4 O10 -45.25(8) . . . . ? S2 Rh3 P4 O10 139.53(8) . . . . ? O3 P1 O2 C17 -89.9(2) . . . . ? O1 P1 O2 C17 168.3(2) . . . . ? Rh2 P1 O2 C17 41.5(2) . . . . ? O2 P1 O1 C11 -167.4(2) . . . . ? O3 P1 O1 C11 90.6(2) . . . . ? Rh2 P1 O1 C11 -38.1(3) . . . . ? O2 P1 O3 C23 -52.9(3) . . . . ? O1 P1 O3 C23 39.6(2) . . . . ? Rh2 P1 O3 C23 171.2(2) . . . . ? O5 P2 O4 C29 -64.0(2) . . . . ? O6 P2 O4 C29 33.9(2) . . . . ? Rh2 P2 O4 C29 163.3(2) . . . . ? O4 P2 O6 C41 -156.8(2) . . . . ? O5 P2 O6 C41 -52.0(2) . . . . ? Rh2 P2 O6 C41 78.7(2) . . . . ? O4 P2 O5 C35 -65.5(2) . . . . ? O6 P2 O5 C35 -163.7(2) . . . . ? Rh2 P2 O5 C35 64.3(2) . . . . ? O7 P3 O9 C59 47.0(2) . . . . ? O8 P3 O9 C59 -50.4(2) . . . . ? Rh3 P3 O9 C59 177.32(19) . . . . ? O7 P3 O8 C53 -178.0(2) . . . . ? O9 P3 O8 C53 -78.5(2) . . . . ? Rh3 P3 O8 C53 50.1(2) . . . . ? O9 P3 O7 C47B -138.0(4) . . . . ? O8 P3 O7 C47B -35.1(4) . . . . ? Rh3 P3 O7 C47B 96.2(4) . . . . ? O9 P3 O7 C47A -162.9(2) . . . . ? O8 P3 O7 C47A -60.0(2) . . . . ? Rh3 P3 O7 C47A 71.3(2) . . . . ? O11 P4 O10 C65 -51.6(2) . . . . ? O12 P4 O10 C65 49.7(2) . . . . ? Rh3 P4 O10 C65 -178.40(16) . . . . ? O12 P4 O11 C71 13.2(2) . . . . ? O10 P4 O11 C71 114.2(2) . . . . ? Rh3 P4 O11 C71 -122.2(2) . . . . ? O11 P4 O12 C77 -124.2(2) . . . . ? O10 P4 O12 C77 133.9(2) . . . . ? Rh3 P4 O12 C77 8.2(2) . . . . ? C6 Ru C1 C2 133.2(3) . . . . ? C3 Ru C1 C2 29.11(16) . . . . ? C5 Ru C1 C2 103.03(18) . . . . ? C4 Ru C1 C2 66.01(17) . . . . ? S2 Ru C1 C2 164.00(17) . . . . ? S1 Ru C1 C2 -95.14(16) . . . . ? C3 Ru C1 C6 -104.05(19) . . . . ? C5 Ru C1 C6 -30.13(17) . . . . ? C2 Ru C1 C6 -133.2(3) . . . . ? C4 Ru C1 C6 -67.15(18) . . . . ? S2 Ru C1 C6 30.8(3) . . . . ? S1 Ru C1 C6 131.70(16) . . . . ? C6 C1 C2 C3 -0.3(4) . . . . ? Ru C1 C2 C3 -52.3(2) . . . . ? C6 C1 C2 Ru 51.9(2) . . . . ? C6 Ru C2 C1 -28.91(17) . . . . ? C3 Ru C2 C1 -132.8(2) . . . . ? C5 Ru C2 C1 -66.56(17) . . . . ? C4 Ru C2 C1 -103.36(18) . . . . ? S2 Ru C2 C1 -162.17(19) . . . . ? S1 Ru C2 C1 92.47(16) . . . . ? C6 Ru C2 C3 103.90(18) . . . . ? C5 Ru C2 C3 66.25(17) . . . . ? C1 Ru C2 C3 132.8(2) . . . . ? C4 Ru C2 C3 29.46(16) . . . . ? S2 Ru C2 C3 -29.4(3) . . . . ? S1 Ru C2 C3 -134.71(15) . . . . ? C1 C2 C3 C4 -3.8(4) . . . . ? Ru C2 C3 C4 -56.8(2) . . . . ? C1 C2 C3 Ru 53.0(2) . . . . ? C6 Ru C3 C4 65.74(17) . . . . ? C5 Ru C3 C4 28.44(16) . . . . ? C1 Ru C3 C4 102.87(18) . . . . ? C2 Ru C3 C4 131.4(2) . . . . ? S2 Ru C3 C4 -59.47(18) . . . . ? S1 Ru C3 C4 -169.67(13) . . . . ? C6 Ru C3 C2 -65.69(17) . . . . ? C5 Ru C3 C2 -102.99(18) . . . . ? C1 Ru C3 C2 -28.56(16) . . . . ? C4 Ru C3 C2 -131.4(2) . . . . ? S2 Ru C3 C2 169.10(13) . . . . ? S1 Ru C3 C2 58.90(18) . . . . ? C2 C3 C4 C5 4.7(4) . . . . ? Ru C3 C4 C5 -51.8(2) . . . . ? C2 C3 C4 Ru 56.5(2) . . . . ? C6 Ru C4 C3 -104.08(18) . . . . ? C5 Ru C4 C3 -133.4(2) . . . . ? C1 Ru C4 C3 -66.49(17) . . . . ? C2 Ru C4 C3 -29.87(16) . . . . ? S2 Ru C4 C3 134.19(15) . . . . ? S1 Ru C4 C3 27.3(3) . . . . ? C6 Ru C4 C5 29.35(16) . . . . ? C3 Ru C4 C5 133.4(2) . . . . ? C1 Ru C4 C5 66.95(17) . . . . ? C2 Ru C4 C5 103.56(18) . . . . ? S2 Ru C4 C5 -92.37(15) . . . . ? S1 Ru C4 C5 160.71(19) . . . . ? C3 C4 C5 C6 -1.4(4) . . . . ? Ru C4 C5 C6 -52.8(2) . . . . ? C3 C4 C5 Ru 51.4(2) . . . . ? C6 Ru C5 C4 -132.5(2) . . . . ? C3 Ru C5 C4 -28.41(16) . . . . ? C1 Ru C5 C4 -102.46(17) . . . . ? C2 Ru C5 C4 -65.82(16) . . . . ? S2 Ru C5 C4 95.63(15) . . . . ? S1 Ru C5 C4 -162.68(16) . . . . ? C3 Ru C5 C6 104.06(18) . . . . ? C1 Ru C5 C6 30.01(16) . . . . ? C2 Ru C5 C6 66.65(17) . . . . ? C4 Ru C5 C6 132.5(2) . . . . ? S2 Ru C5 C6 -131.90(15) . . . . ? S1 Ru C5 C6 -30.2(3) . . . . ? C2 C1 C6 C5 3.6(4) . . . . ? Ru C1 C6 C5 56.5(2) . . . . ? C2 C1 C6 Ru -52.9(2) . . . . ? C4 C5 C6 C1 -2.7(4) . . . . ? Ru C5 C6 C1 -56.6(2) . . . . ? C4 C5 C6 Ru 54.0(2) . . . . ? C3 Ru C6 C1 65.51(17) . . . . ? C5 Ru C6 C1 130.9(3) . . . . ? C2 Ru C6 C1 28.36(16) . . . . ? C4 Ru C6 C1 102.09(18) . . . . ? S2 Ru C6 C1 -167.59(13) . . . . ? S1 Ru C6 C1 -61.32(18) . . . . ? C3 Ru C6 C5 -65.43(17) . . . . ? C1 Ru C6 C5 -130.9(3) . . . . ? C2 Ru C6 C5 -102.58(18) . . . . ? C4 Ru C6 C5 -28.85(16) . . . . ? S2 Ru C6 C5 61.47(18) . . . . ? S1 Ru C6 C5 167.74(13) . . . . ? P1 O1 C11 C12 -22.3(4) . . . . ? P1 O1 C11 C16 158.9(2) . . . . ? O1 C11 C12 C13 -179.3(3) . . . . ? C16 C11 C12 C13 -0.6(4) . . . . ? C11 C12 C13 C14 0.8(5) . . . . ? C12 C13 C14 C15 -0.3(5) . . . . ? C13 C14 C15 C16 -0.3(5) . . . . ? C14 C15 C16 C11 0.4(5) . . . . ? O1 C11 C16 C15 178.8(3) . . . . ? C12 C11 C16 C15 0.0(4) . . . . ? P1 O2 C17 C18 39.0(3) . . . . ? P1 O2 C17 C22 -144.85(18) . . . . ? C22 C17 C18 C19 -0.1(4) . . . . ? O2 C17 C18 C19 175.8(2) . . . . ? C17 C18 C19 C20 0.3(4) . . . . ? C18 C19 C20 C21 -0.2(5) . . . . ? C19 C20 C21 C22 -0.1(5) . . . . ? C20 C21 C22 C17 0.3(4) . . . . ? C18 C17 C22 C21 -0.2(4) . . . . ? O2 C17 C22 C21 -176.4(2) . . . . ? P1 O3 C23 C24 -92.9(4) . . . . ? P1 O3 C23 C28 87.6(3) . . . . ? C28 C23 C24 C25 0.2(8) . . . . ? O3 C23 C24 C25 -179.3(5) . . . . ? C23 C24 C25 C26 -0.8(10) . . . . ? C24 C25 C26 C27 1.7(9) . . . . ? C25 C26 C27 C28 -2.1(7) . . . . ? C24 C23 C28 C27 -0.5(5) . . . . ? O3 C23 C28 C27 179.0(3) . . . . ? C26 C27 C28 C23 1.5(5) . . . . ? P2 O4 C29 C30 -141.0(2) . . . . ? P2 O4 C29 C34 41.4(4) . . . . ? C34 C29 C30 C31 -0.5(4) . . . . ? O4 C29 C30 C31 -178.1(2) . . . . ? C29 C30 C31 C32 -1.4(4) . . . . ? C30 C31 C32 C33 1.7(5) . . . . ? C31 C32 C33 C34 -0.1(5) . . . . ? C32 C33 C34 C29 -1.7(5) . . . . ? C30 C29 C34 C33 2.0(5) . . . . ? O4 C29 C34 C33 179.4(3) . . . . ? P2 O5 C35 C40 -163.44(19) . . . . ? P2 O5 C35 C36 20.5(4) . . . . ? C40 C35 C36 C37 -0.2(4) . . . . ? O5 C35 C36 C37 175.7(3) . . . . ? C35 C36 C37 C38 -0.3(5) . . . . ? C36 C37 C38 C39 0.4(5) . . . . ? C37 C38 C39 C40 0.1(5) . . . . ? C38 C39 C40 C35 -0.6(5) . . . . ? C36 C35 C40 C39 0.6(4) . . . . ? O5 C35 C40 C39 -175.5(3) . . . . ? P2 O6 C41 C42 89.1(3) . . . . ? P2 O6 C41 C46 -99.4(3) . . . . ? C46 C41 C42 C43 -1.3(5) . . . . ? O6 C41 C42 C43 169.9(3) . . . . ? C41 C42 C43 C44 0.5(5) . . . . ? C42 C43 C44 C45 0.3(5) . . . . ? C43 C44 C45 C46 -0.3(5) . . . . ? C44 C45 C46 C41 -0.5(4) . . . . ? C42 C41 C46 C45 1.3(4) . . . . ? O6 C41 C46 C45 -170.0(3) . . . . ? C47B O7 C47A C52A 90.4(10) . . . . ? P3 O7 C47A C52A -157.9(5) . . . . ? C47B O7 C47A C48A -82.4(8) . . . . ? P3 O7 C47A C48A 29.3(3) . . . . ? C52A C47A C48A C49A -1.6(7) . . . . ? O7 C47A C48A C49A 171.0(5) . . . . ? C47A C48A C49A C50A -8.3(10) . . . . ? C48A C49A C50A C51A 18.1(19) . . . . ? C49A C50A C51A C52A -16(2) . . . . ? C48A C47A C52A C51A 5.3(10) . . . . ? O7 C47A C52A C51A -168.1(7) . . . . ? C50A C51A C52A C47A 4.2(19) . . . . ? Cl2 C83 Cl1 Cl2 -28.0(10) . . . 2_666 ? Cl1 C83 Cl2 Cl1 33.8(12) . . . 2_666 ? C47A O7 C47B C48B -176.4(10) . . . . ? P3 O7 C47B C48B 100.4(5) . . . . ? C47A O7 C47B C52B 7.9(7) . . . . ? P3 O7 C47B C52B -75.4(6) . . . . ? O7 C47B C48B C49B -175.9(5) . . . . ? C52B C47B C48B C49B 0.0 . . . . ? C47B C48B C49B C50B 0.0 . . . . ? C48B C49B C50B C51B 0.0 . . . . ? C49B C50B C51B C52B 0.0 . . . . ? C50B C51B C52B C47B 0.0 . . . . ? O7 C47B C52B C51B 175.6(6) . . . . ? C48B C47B C52B C51B 0.0 . . . . ? P3 O8 C53 C54 27.1(3) . . . . ? P3 O8 C53 C58 -156.99(19) . . . . ? O8 C53 C54 C55 174.7(2) . . . . ? C58 C53 C54 C55 -1.0(4) . . . . ? C53 C54 C55 C56 0.2(4) . . . . ? C54 C55 C56 C57 1.2(4) . . . . ? C55 C56 C57 C58 -1.8(5) . . . . ? C56 C57 C58 C53 1.0(4) . . . . ? O8 C53 C58 C57 -175.6(2) . . . . ? C54 C53 C58 C57 0.4(4) . . . . ? P3 O9 C59 C60 -97.0(3) . . . . ? P3 O9 C59 C64 86.2(3) . . . . ? C64 C59 C60 C61 -0.4(5) . . . . ? O9 C59 C60 C61 -177.2(3) . . . . ? C59 C60 C61 C62 -0.7(6) . . . . ? C60 C61 C62 C63 1.0(7) . . . . ? C61 C62 C63 C64 -0.2(6) . . . . ? C60 C59 C64 C63 1.2(5) . . . . ? O9 C59 C64 C63 178.0(3) . . . . ? C62 C63 C64 C59 -0.9(6) . . . . ? P4 O10 C65 C66 96.1(3) . . . . ? P4 O10 C65 C70 -85.9(3) . . . . ? C70 C65 C66 C67 1.2(4) . . . . ? O10 C65 C66 C67 179.2(2) . . . . ? C65 C66 C67 C68 -0.4(4) . . . . ? C66 C67 C68 C69 -0.1(4) . . . . ? C67 C68 C69 C70 -0.1(4) . . . . ? C68 C69 C70 C65 0.8(4) . . . . ? C66 C65 C70 C69 -1.4(4) . . . . ? O10 C65 C70 C69 -179.3(2) . . . . ? P4 O11 C71 C72 126.0(2) . . . . ? P4 O11 C71 C76 -59.3(3) . . . . ? C76 C71 C72 C73 -1.7(4) . . . . ? O11 C71 C72 C73 173.0(2) . . . . ? C71 C72 C73 C74 1.2(4) . . . . ? C72 C73 C74 C75 0.8(5) . . . . ? C73 C74 C75 C76 -2.2(5) . . . . ? C72 C71 C76 C75 0.3(4) . . . . ? O11 C71 C76 C75 -174.1(2) . . . . ? C74 C75 C76 C71 1.7(4) . . . . ? P4 O12 C77 C78 44.7(3) . . . . ? P4 O12 C77 C82 -139.2(2) . . . . ? O12 C77 C78 C79 174.7(2) . . . . ? C82 C77 C78 C79 -1.2(4) . . . . ? C77 C78 C79 C80 -0.2(4) . . . . ? C78 C79 C80 C81 1.5(4) . . . . ? C79 C80 C81 C82 -1.5(4) . . . . ? C80 C81 C82 C77 0.2(4) . . . . ? C78 C77 C82 C81 1.2(4) . . . . ? O12 C77 C82 C81 -174.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.269 _refine_diff_density_min -1.056 _refine_diff_density_rms 0.092 #===END