Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global #============================================================================== _journal_coden_Cambridge 222 # SUBMISSION DETAILS # ================== _publ_contact_author_name 'Dr Gillian Reid' _publ_contact_author_address ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email gr@soton.ac.uk _publ_contact_author_fax '023 8059 3781' _publ_contact_author_phone '023 8059 3609' _publ_contact_letter ; Dear Sirs, This file contains structural information in CIF format for two structures offered as supplementary material to a paper submitted to Dalton Transactions. Yours faithfully Gillian Reid ; _publ_requested_journal 'Dalton Trans.' _publ_requested_category ? #============================================================================ # TITLE AND AUTHOR LIST # ===================== _publ_section_title ; Synthesis and properties of Rh(I) and Ir(I) distibine complexes with organometallic co-ligands ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. # Note order: Family_name, first name(s) or initials (or mixture). loop_ _publ_author_name _publ_author_address 'Brown, Michael D.' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Levason, William' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Reid, Gillian' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Webster, Michael' ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; #============================================================================ # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique (to this file) identifier. #============================================================================ # 05mdb008 data_05mdb008 _database_code_depnum_ccdc_archive 'CCDC 604224' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2005-11-24 _chemical_name_systematic ; carbonylbis(1,3-bis(diphenylstibino)propane)rhodium(I) hexafluorophosphate(V) dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H52 O Rh Sb4 1+, F6 P 1-, 0.75(C H2 Cl2)' _chemical_formula_sum 'C55.75 H53.50 Cl1.50 F6 O P Rh Sb4' _chemical_formula_structural '(Rh (C O) (C27 H26 Sb2)2) (P F6) (C H2 Cl2)0.75' _chemical_formula_weight 1527.54 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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_Int_Tables_number 2 # Superceded ** _symmetry_space_group_name_Hall '-P 1' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5141(10) _cell_length_b 20.129(3) _cell_length_c 21.133(3) _cell_angle_alpha 74.016(5) _cell_angle_beta 80.152(7) _cell_angle_gamma 82.929(7) _cell_volume 5427.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 23207 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2958 _exptl_absorpt_coefficient_mu 2.426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8558 # shelxl 0.7935 _exptl_absorpt_correction_T_max 1.0000 # 0.9092 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 94727 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.62 _reflns_number_total 24949 _reflns_number_gt 18216 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+34.7075P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24949 _refine_ls_number_parameters 1265 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.74385(3) 0.81520(2) 0.46239(2) 0.01871(10) Uani 1 1 d . . . Rh2 Rh 0.67462(4) 0.67727(3) 1.00385(2) 0.02263(11) Uani 1 1 d . . . Sb1 Sb 0.88667(3) 0.78980(2) 0.53184(2) 0.02286(10) Uani 1 1 d . . . Sb2 Sb 0.83338(3) 0.92305(2) 0.38868(2) 0.02145(9) Uani 1 1 d . . . Sb3 Sb 0.81349(3) 0.71345(2) 0.40894(2) 0.02243(10) Uani 1 1 d . . . Sb4 Sb 0.60011(3) 0.83622(2) 0.39286(2) 0.02045(9) Uani 1 1 d . . . Sb5 Sb 0.79775(3) 0.63658(2) 0.91321(2) 0.02473(10) Uani 1 1 d . . . Sb6 Sb 0.59411(3) 0.76769(2) 0.90780(2) 0.02500(10) Uani 1 1 d . . . Sb7 Sb 0.54780(3) 0.71691(2) 1.09347(2) 0.02506(10) Uani 1 1 d . . . Sb8 Sb 0.80410(3) 0.75232(2) 1.02435(2) 0.02532(10) Uani 1 1 d . . . O1 O 0.5974(4) 0.8032(3) 0.5891(3) 0.0433(13) Uani 1 1 d . . . O2 O 0.6434(4) 0.5284(3) 1.0754(3) 0.0483(14) Uani 1 1 d . . . C1 C 0.9014(5) 0.6842(3) 0.5856(3) 0.0301(15) Uani 1 1 d . . . C2 C 0.9790(6) 0.6386(4) 0.5696(4) 0.0447(19) Uani 1 1 d . . . H2 H 1.0324 0.6544 0.5351 0.054 Uiso 1 1 calc R . . C3 C 0.9795(8) 0.5694(4) 0.6039(5) 0.059(2) Uani 1 1 d . . . H3 H 1.0323 0.5374 0.5921 0.071 Uiso 1 1 calc R . . C4 C 0.9045(8) 0.5471(5) 0.6545(5) 0.060(3) Uani 1 1 d . . . H4 H 0.9067 0.4997 0.6788 0.072 Uiso 1 1 calc R . . C5 C 0.8271(7) 0.5911(4) 0.6709(4) 0.051(2) Uani 1 1 d . . . H5 H 0.7748 0.5748 0.7061 0.061 Uiso 1 1 calc R . . C6 C 0.8245(6) 0.6602(4) 0.6359(4) 0.0413(19) Uani 1 1 d . . . H6 H 0.7694 0.6914 0.6466 0.050 Uiso 1 1 calc R . . C7 C 0.8793(5) 0.8385(3) 0.6102(3) 0.0245(14) Uani 1 1 d . . . C8 C 0.9475(5) 0.8144(4) 0.6548(3) 0.0328(16) Uani 1 1 d . . . H8 H 0.9930 0.7751 0.6518 0.039 Uiso 1 1 calc R . . C9 C 0.9495(5) 0.8476(4) 0.7040(4) 0.0358(17) Uani 1 1 d . . . H9 H 0.9964 0.8312 0.7347 0.043 Uiso 1 1 calc R . . C10 C 0.8832(5) 0.9046(4) 0.7081(3) 0.0348(17) Uani 1 1 d . . . H10 H 0.8844 0.9272 0.7419 0.042 Uiso 1 1 calc R . . C11 C 0.8165(6) 0.9285(4) 0.6645(4) 0.0369(17) Uani 1 1 d . . . H11 H 0.7720 0.9683 0.6676 0.044 Uiso 1 1 calc R . . C12 C 0.8121(5) 0.8956(4) 0.6152(3) 0.0325(16) Uani 1 1 d . . . H12 H 0.7639 0.9119 0.5854 0.039 Uiso 1 1 calc R . . C13 C 1.0333(5) 0.8159(4) 0.4811(3) 0.0316(16) Uani 1 1 d . . . H13A H 1.0824 0.8008 0.5131 0.038 Uiso 1 1 calc R . . H13B H 1.0533 0.7906 0.4463 0.038 Uiso 1 1 calc R . . C14 C 1.0371(5) 0.8942(4) 0.4489(4) 0.0342(17) Uani 1 1 d . . . H14A H 0.9994 0.9194 0.4808 0.041 Uiso 1 1 calc R . . H14B H 1.1081 0.9056 0.4411 0.041 Uiso 1 1 calc R . . C15 C 0.9945(5) 0.9209(4) 0.3835(3) 0.0310(16) Uani 1 1 d . . . H15A H 1.0266 0.8917 0.3536 0.037 Uiso 1 1 calc R . . H15B H 1.0147 0.9685 0.3625 0.037 Uiso 1 1 calc R . . C16 C 0.7887(5) 1.0220(3) 0.4078(3) 0.0241(14) Uani 1 1 d . . . C17 C 0.8190(5) 1.0821(3) 0.3617(4) 0.0327(16) Uani 1 1 d . . . H17 H 0.8605 1.0792 0.3213 0.039 Uiso 1 1 calc R . . C18 C 0.7892(5) 1.1463(4) 0.3739(4) 0.0398(18) Uani 1 1 d . . . H18 H 0.8089 1.1874 0.3414 0.048 Uiso 1 1 calc R . . C19 C 0.7307(6) 1.1507(4) 0.4333(4) 0.0412(19) Uani 1 1 d . . . H19 H 0.7109 1.1947 0.4420 0.049 Uiso 1 1 calc R . . C20 C 0.7012(5) 1.0910(4) 0.4801(4) 0.0395(18) Uani 1 1 d . . . H20 H 0.6616 1.0940 0.5211 0.047 Uiso 1 1 calc R . . C21 C 0.7293(5) 1.0262(4) 0.4673(4) 0.0327(16) Uani 1 1 d . . . H21 H 0.7079 0.9853 0.4992 0.039 Uiso 1 1 calc R . . C22 C 0.8230(5) 0.9493(3) 0.2850(3) 0.0254(14) Uani 1 1 d . . . C23 C 0.7448(5) 0.9943(3) 0.2587(3) 0.0271(14) Uani 1 1 d . . . H23 H 0.6994 1.0181 0.2862 0.033 Uiso 1 1 calc R . . C24 C 0.7325(5) 1.0047(4) 0.1927(3) 0.0310(15) Uani 1 1 d . . . H24 H 0.6780 1.0347 0.1754 0.037 Uiso 1 1 calc R . . C25 C 0.7996(6) 0.9715(4) 0.1525(4) 0.0363(17) Uani 1 1 d . . . H25 H 0.7916 0.9790 0.1072 0.044 Uiso 1 1 calc R . . C26 C 0.8778(6) 0.9276(4) 0.1775(4) 0.0402(18) Uani 1 1 d . . . H26 H 0.9237 0.9045 0.1496 0.048 Uiso 1 1 calc R . . C27 C 0.8897(5) 0.9169(4) 0.2438(4) 0.0353(17) Uani 1 1 d . . . H27 H 0.9445 0.8869 0.2608 0.042 Uiso 1 1 calc R . . C28 C 0.9697(4) 0.6770(3) 0.3915(3) 0.0267(14) Uani 1 1 d . . . C29 C 1.0030(5) 0.6111(3) 0.4221(4) 0.0340(17) Uani 1 1 d . . . H29 H 0.9573 0.5808 0.4521 0.041 Uiso 1 1 calc R . . C30 C 1.1043(6) 0.5883(4) 0.4092(4) 0.045(2) Uani 1 1 d . . . H30 H 1.1277 0.5428 0.4315 0.054 Uiso 1 1 calc R . . C31 C 1.1713(5) 0.6314(4) 0.3640(4) 0.0390(18) Uani 1 1 d . . . H31 H 1.2400 0.6153 0.3547 0.047 Uiso 1 1 calc R . . C32 C 1.1375(5) 0.6978(4) 0.3326(4) 0.0363(17) Uani 1 1 d . . . H32 H 1.1830 0.7277 0.3018 0.044 Uiso 1 1 calc R . . C33 C 1.0363(5) 0.7214(4) 0.3462(3) 0.0294(15) Uani 1 1 d . . . H33 H 1.0130 0.7673 0.3248 0.035 Uiso 1 1 calc R . . C34 C 0.7522(5) 0.6163(3) 0.4580(3) 0.0257(14) Uani 1 1 d . . . C35 C 0.7561(5) 0.5647(3) 0.4252(4) 0.0334(16) Uani 1 1 d . . . H35 H 0.7885 0.5720 0.3805 0.040 Uiso 1 1 calc R . . C36 C 0.7128(6) 0.5026(4) 0.4570(4) 0.0393(18) Uani 1 1 d . . . H36 H 0.7161 0.4674 0.4345 0.047 Uiso 1 1 calc R . . C37 C 0.6654(5) 0.4928(4) 0.5215(4) 0.0342(17) Uani 1 1 d . . . H37 H 0.6351 0.4507 0.5435 0.041 Uiso 1 1 calc R . . C38 C 0.6615(5) 0.5438(4) 0.5547(4) 0.0371(17) Uani 1 1 d . . . H38 H 0.6291 0.5367 0.5994 0.044 Uiso 1 1 calc R . . C39 C 0.7048(5) 0.6050(4) 0.5226(3) 0.0309(15) Uani 1 1 d . . . H39 H 0.7018 0.6400 0.5454 0.037 Uiso 1 1 calc R . . C40 C 0.7812(5) 0.7232(3) 0.3107(3) 0.0259(14) Uani 1 1 d . . . H40A H 0.8191 0.7609 0.2792 0.031 Uiso 1 1 calc R . . H40B H 0.8064 0.6796 0.2980 0.031 Uiso 1 1 calc R . . C41 C 0.6712(5) 0.7382(3) 0.3026(3) 0.0275(15) Uani 1 1 d . . . H41A H 0.6313 0.7078 0.3410 0.033 Uiso 1 1 calc R . . H41B H 0.6610 0.7261 0.2620 0.033 Uiso 1 1 calc R . . C42 C 0.6302(5) 0.8141(3) 0.2977(3) 0.0271(14) Uani 1 1 d . . . H42A H 0.5673 0.8235 0.2775 0.033 Uiso 1 1 calc R . . H42B H 0.6800 0.8453 0.2682 0.033 Uiso 1 1 calc R . . C43 C 0.4728(4) 0.7774(3) 0.4322(3) 0.0232(13) Uani 1 1 d . . . C44 C 0.3869(5) 0.7951(3) 0.4008(3) 0.0271(14) Uani 1 1 d . . . H44 H 0.3848 0.8338 0.3630 0.032 Uiso 1 1 calc R . . C45 C 0.3048(5) 0.7560(4) 0.4251(4) 0.0325(16) Uani 1 1 d . . . H45 H 0.2461 0.7681 0.4039 0.039 Uiso 1 1 calc R . . C46 C 0.3070(5) 0.6999(4) 0.4796(4) 0.0346(17) Uani 1 1 d . . . H46 H 0.2504 0.6732 0.4956 0.042 Uiso 1 1 calc R . . C47 C 0.3915(6) 0.6825(4) 0.5110(4) 0.0390(18) Uani 1 1 d . . . H47 H 0.3929 0.6441 0.5490 0.047 Uiso 1 1 calc R . . C48 C 0.4750(5) 0.7212(3) 0.4869(3) 0.0306(15) Uani 1 1 d . . . H48 H 0.5336 0.7089 0.5082 0.037 Uiso 1 1 calc R . . C49 C 0.5322(4) 0.9388(3) 0.3665(3) 0.0224(13) Uani 1 1 d . . . C50 C 0.4883(5) 0.9647(3) 0.3093(3) 0.0284(15) Uani 1 1 d . . . H50 H 0.4824 0.9348 0.2826 0.034 Uiso 1 1 calc R . . C51 C 0.4531(5) 1.0332(4) 0.2908(4) 0.0344(16) Uani 1 1 d . . . H51 H 0.4230 1.0505 0.2514 0.041 Uiso 1 1 calc R . . C52 C 0.4615(5) 1.0773(4) 0.3297(4) 0.0356(17) Uani 1 1 d . . . H52 H 0.4377 1.1248 0.3165 0.043 Uiso 1 1 calc R . . C53 C 0.5046(5) 1.0519(4) 0.3877(4) 0.0332(16) Uani 1 1 d . . . H53 H 0.5108 1.0816 0.4145 0.040 Uiso 1 1 calc R . . C54 C 0.5383(5) 0.9826(3) 0.4057(3) 0.0270(14) Uani 1 1 d . . . H54 H 0.5662 0.9647 0.4459 0.032 Uiso 1 1 calc R . . C55 C 0.6523(5) 0.8077(3) 0.5410(4) 0.0276(15) Uani 1 1 d . . . C56 C 0.9442(5) 0.6048(3) 0.9385(3) 0.0285(15) Uani 1 1 d . . . C57 C 1.0291(5) 0.6063(4) 0.8901(4) 0.0362(17) Uani 1 1 d . . . H57 H 1.0220 0.6179 0.8443 0.043 Uiso 1 1 calc R . . C58 C 1.1233(5) 0.5907(4) 0.9099(4) 0.0393(18) Uani 1 1 d . . . H58 H 1.1814 0.5909 0.8773 0.047 Uiso 1 1 calc R . . C59 C 1.1341(5) 0.5750(4) 0.9756(4) 0.0369(18) Uani 1 1 d . . . H59 H 1.1997 0.5651 0.9881 0.044 Uiso 1 1 calc R . . C60 C 1.0507(5) 0.5732(4) 1.0242(4) 0.0366(17) Uani 1 1 d . . . H60 H 1.0588 0.5628 1.0698 0.044 Uiso 1 1 calc R . . C61 C 0.9558(5) 0.5867(3) 1.0055(4) 0.0336(16) Uani 1 1 d . . . H61 H 0.8980 0.5836 1.0385 0.040 Uiso 1 1 calc R . . C62 C 0.7567(5) 0.5514(3) 0.8848(3) 0.0270(14) Uani 1 1 d . . . C63 C 0.8241(5) 0.5209(4) 0.8421(3) 0.0302(15) Uani 1 1 d . . . H63 H 0.8878 0.5388 0.8246 0.036 Uiso 1 1 calc R . . C64 C 0.7989(6) 0.4638(4) 0.8247(4) 0.0383(18) Uani 1 1 d . . . H64 H 0.8455 0.4424 0.7958 0.046 Uiso 1 1 calc R . . C65 C 0.7073(6) 0.4392(4) 0.8492(4) 0.045(2) Uani 1 1 d . . . H65 H 0.6893 0.4013 0.8362 0.054 Uiso 1 1 calc R . . C66 C 0.6392(6) 0.4684(4) 0.8930(4) 0.049(2) Uani 1 1 d . . . H66 H 0.5762 0.4496 0.9111 0.059 Uiso 1 1 calc R . . C67 C 0.6645(6) 0.5259(4) 0.9104(4) 0.0384(18) Uani 1 1 d . . . H67 H 0.6181 0.5470 0.9396 0.046 Uiso 1 1 calc R . . C68 C 0.8345(5) 0.7067(3) 0.8176(3) 0.0313(15) Uani 1 1 d . . . H68A H 0.8790 0.7403 0.8220 0.038 Uiso 1 1 calc R . . H68B H 0.8732 0.6801 0.7872 0.038 Uiso 1 1 calc R . . C69 C 0.7442(5) 0.7471(3) 0.7859(3) 0.0298(15) Uani 1 1 d . . . H69A H 0.7667 0.7680 0.7381 0.036 Uiso 1 1 calc R . . H69B H 0.6936 0.7143 0.7889 0.036 Uiso 1 1 calc R . . C70 C 0.6944(5) 0.8040(3) 0.8178(3) 0.0291(15) Uani 1 1 d . . . H70A H 0.6564 0.8384 0.7856 0.035 Uiso 1 1 calc R . . H70B H 0.7476 0.8280 0.8275 0.035 Uiso 1 1 calc R . . C71 C 0.4801(5) 0.7420(4) 0.8625(3) 0.0313(15) Uani 1 1 d . . . C72 C 0.4584(5) 0.6736(4) 0.8740(4) 0.0365(17) Uani 1 1 d . . . H72 H 0.4942 0.6375 0.9027 0.044 Uiso 1 1 calc R . . C73 C 0.3854(6) 0.6586(4) 0.8441(4) 0.048(2) Uani 1 1 d . . . H73 H 0.3698 0.6119 0.8526 0.057 Uiso 1 1 calc R . . C74 C 0.3343(6) 0.7104(5) 0.8018(5) 0.054(2) Uani 1 1 d . . . H74 H 0.2844 0.6991 0.7806 0.064 Uiso 1 1 calc R . . C75 C 0.3548(6) 0.7788(5) 0.7898(4) 0.050(2) Uani 1 1 d . . . H75 H 0.3184 0.8147 0.7611 0.060 Uiso 1 1 calc R . . C76 C 0.4283(5) 0.7944(4) 0.8199(3) 0.0348(17) Uani 1 1 d . . . H76 H 0.4436 0.8411 0.8115 0.042 Uiso 1 1 calc R . . C77 C 0.5257(5) 0.8656(3) 0.9199(3) 0.0293(15) Uani 1 1 d . . . C78 C 0.5803(6) 0.9240(4) 0.9000(4) 0.0364(17) Uani 1 1 d . . . H78 H 0.6485 0.9208 0.8798 0.044 Uiso 1 1 calc R . . C79 C 0.5347(6) 0.9873(4) 0.9098(4) 0.0405(18) Uani 1 1 d . . . H79 H 0.5711 1.0275 0.8955 0.049 Uiso 1 1 calc R . . C80 C 0.4367(6) 0.9907(4) 0.9402(4) 0.0399(18) Uani 1 1 d . . . H80 H 0.4063 1.0336 0.9476 0.048 Uiso 1 1 calc R . . C81 C 0.3820(6) 0.9341(4) 0.9601(4) 0.0383(18) Uani 1 1 d . . . H81 H 0.3146 0.9375 0.9816 0.046 Uiso 1 1 calc R . . C82 C 0.4252(5) 0.8711(4) 0.9486(3) 0.0319(16) Uani 1 1 d . . . H82 H 0.3864 0.8322 0.9604 0.038 Uiso 1 1 calc R . . C83 C 0.3961(5) 0.7297(3) 1.0762(3) 0.0277(15) Uani 1 1 d . . . C84 C 0.3700(5) 0.6991(4) 1.0308(3) 0.0324(16) Uani 1 1 d . . . H84 H 0.4179 0.6684 1.0122 0.039 Uiso 1 1 calc R . . C85 C 0.2746(5) 0.7130(4) 1.0124(4) 0.0409(18) Uani 1 1 d . . . H85 H 0.2571 0.6923 0.9810 0.049 Uiso 1 1 calc R . . C86 C 0.2048(6) 0.7571(5) 1.0399(4) 0.048(2) Uani 1 1 d . . . H86 H 0.1394 0.7668 1.0272 0.057 Uiso 1 1 calc R . . C87 C 0.2300(5) 0.7872(4) 1.0860(4) 0.044(2) Uani 1 1 d . . . H87 H 0.1814 0.8170 1.1053 0.053 Uiso 1 1 calc R . . C88 C 0.3253(5) 0.7742(4) 1.1039(3) 0.0348(17) Uani 1 1 d . . . H88 H 0.3428 0.7955 1.1349 0.042 Uiso 1 1 calc R . . C89 C 0.5402(5) 0.6575(3) 1.1949(3) 0.0272(14) Uani 1 1 d . . . C90 C 0.4673(5) 0.6781(4) 1.2428(3) 0.0307(15) Uani 1 1 d . . . H90 H 0.4190 0.7159 1.2300 0.037 Uiso 1 1 calc R . . C91 C 0.4663(5) 0.6426(4) 1.3092(3) 0.0348(17) Uani 1 1 d . . . H91 H 0.4163 0.6561 1.3417 0.042 Uiso 1 1 calc R . . C92 C 0.5351(6) 0.5889(4) 1.3288(4) 0.0436(19) Uani 1 1 d . . . H92 H 0.5334 0.5657 1.3746 0.052 Uiso 1 1 calc R . . C93 C 0.6090(6) 0.5678(4) 1.2811(4) 0.045(2) Uani 1 1 d . . . H93 H 0.6575 0.5303 1.2943 0.054 Uiso 1 1 calc R . . C94 C 0.6101(5) 0.6026(4) 1.2144(4) 0.0361(17) Uani 1 1 d . . . H94 H 0.6594 0.5885 1.1818 0.043 Uiso 1 1 calc R . . C95 C 0.5609(5) 0.8170(3) 1.1075(4) 0.0312(16) Uani 1 1 d . . . H95A H 0.5417 0.8529 1.0681 0.037 Uiso 1 1 calc R . . H95B H 0.5117 0.8231 1.1464 0.037 Uiso 1 1 calc R . . C96 C 0.6644(5) 0.8300(4) 1.1183(3) 0.0296(15) Uani 1 1 d . . . H96A H 0.6904 0.7890 1.1510 0.036 Uiso 1 1 calc R . . H96B H 0.6572 0.8700 1.1379 0.036 Uiso 1 1 calc R . . C97 C 0.7420(5) 0.8444(3) 1.0557(3) 0.0311(15) Uani 1 1 d . . . H97A H 0.7976 0.8672 1.0639 0.037 Uiso 1 1 calc R . . H97B H 0.7100 0.8771 1.0192 0.037 Uiso 1 1 calc R . . C98 C 0.8848(4) 0.7080(3) 1.1069(3) 0.0255(14) Uani 1 1 d . . . C99 C 0.8684(5) 0.6414(4) 1.1459(3) 0.0334(16) Uani 1 1 d . . . H99 H 0.8228 0.6155 1.1349 0.040 Uiso 1 1 calc R . . C100 C 0.9178(6) 0.6121(4) 1.2010(4) 0.0378(18) Uani 1 1 d . . . H100 H 0.9071 0.5661 1.2270 0.045 Uiso 1 1 calc R . . C101 C 0.9827(5) 0.6508(4) 1.2176(4) 0.0384(18) Uani 1 1 d . . . H101 H 1.0153 0.6316 1.2558 0.046 Uiso 1 1 calc R . . C102 C 1.0004(5) 0.7165(4) 1.1792(4) 0.0379(18) Uani 1 1 d . . . H102 H 1.0457 0.7423 1.1906 0.045 Uiso 1 1 calc R . . C103 C 0.9522(5) 0.7452(4) 1.1236(3) 0.0311(16) Uani 1 1 d . . . H103 H 0.9652 0.7905 1.0970 0.037 Uiso 1 1 calc R . . C104 C 0.9189(5) 0.8000(3) 0.9492(3) 0.0268(14) Uani 1 1 d . . . C105 C 0.9000(5) 0.8668(4) 0.9107(3) 0.0362(17) Uani 1 1 d . . . H105 H 0.8360 0.8911 0.9179 0.043 Uiso 1 1 calc R . . C106 C 0.9756(6) 0.8987(4) 0.8607(4) 0.0396(18) Uani 1 1 d . . . H106 H 0.9631 0.9447 0.8347 0.047 Uiso 1 1 calc R . . C107 C 1.0671(6) 0.8631(5) 0.8500(4) 0.044(2) Uani 1 1 d . . . H107 H 1.1181 0.8846 0.8164 0.053 Uiso 1 1 calc R . . C108 C 1.0860(5) 0.7970(4) 0.8868(4) 0.0397(18) Uani 1 1 d . . . H108 H 1.1497 0.7727 0.8783 0.048 Uiso 1 1 calc R . . C109 C 1.0126(5) 0.7647(4) 0.9367(4) 0.0329(16) Uani 1 1 d . . . H109 H 1.0265 0.7187 0.9623 0.039 Uiso 1 1 calc R . . C110 C 0.6549(5) 0.5854(4) 1.0480(4) 0.0340(16) Uani 1 1 d . . . P1 P 0.82822(18) 0.37197(14) 0.30254(12) 0.0567(6) Uani 1 1 d . . . P2 P 0.23302(15) 0.90788(11) 0.22399(11) 0.0403(5) Uani 1 1 d . . . F1 F 0.7820(5) 0.4208(3) 0.2398(3) 0.0863(19) Uani 1 1 d . . . F2 F 0.7227(4) 0.3385(5) 0.3297(3) 0.108(3) Uani 1 1 d . . . F3 F 0.8613(4) 0.3139(3) 0.2627(3) 0.0698(15) Uani 1 1 d . . . F4 F 0.8709(4) 0.3230(3) 0.3663(3) 0.0740(16) Uani 1 1 d . . . F5 F 0.9352(5) 0.4011(3) 0.2738(3) 0.0871(19) Uani 1 1 d . . . F6 F 0.7957(7) 0.4302(4) 0.3409(3) 0.137(4) Uani 1 1 d . . . F7 F 0.2489(4) 0.9291(3) 0.1455(2) 0.0693(15) Uani 1 1 d . . . F8 F 0.1281(4) 0.9529(3) 0.2270(2) 0.0608(13) Uani 1 1 d . . . F9 F 0.2878(5) 0.9721(3) 0.2248(3) 0.086(2) Uani 1 1 d . . . F10 F 0.2179(4) 0.8846(3) 0.3030(2) 0.0666(15) Uani 1 1 d . . . F11 F 0.3369(5) 0.8629(4) 0.2210(3) 0.113(3) Uani 1 1 d . . . F12 F 0.1748(5) 0.8445(3) 0.2225(3) 0.0843(19) Uani 1 1 d . . . Cl1 Cl 0.5579(2) 0.53520(14) 0.75411(15) 0.0780(8) Uani 1 1 d . . . Cl2 Cl 0.5262(2) 0.67105(14) 0.66480(13) 0.0712(7) Uani 1 1 d . . . C111 C 0.4772(7) 0.5914(5) 0.7021(5) 0.061(3) Uani 1 1 d . . . H11A H 0.4668 0.5698 0.6672 0.074 Uiso 1 1 calc R . . H11B H 0.4108 0.5986 0.7286 0.074 Uiso 1 1 calc R . . Cl3 Cl 0.0476(2) 0.93082(16) 0.00929(15) 0.0859(8) Uani 1 1 d D . . C112 C 0.0423(14) 1.0050(8) 0.0338(10) 0.074(6) Uiso 0.50 1 d PD . . H11C H 0.1098 1.0230 0.0233 0.089 Uiso 0.50 1 calc PR . . H11D H 0.0212 0.9953 0.0825 0.089 Uiso 0.50 1 calc PR . . 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 0.0168(2) 0.0186(2) 0.0201(2) -0.00469(19) -0.00324(19) 0.00066(18) Rh2 0.0225(2) 0.0220(3) 0.0206(3) -0.0035(2) -0.0014(2) 0.00151(19) Sb1 0.0203(2) 0.0265(2) 0.0219(2) -0.00646(18) -0.00594(17) 0.00210(17) Sb2 0.0211(2) 0.0209(2) 0.0219(2) -0.00479(17) -0.00229(17) -0.00281(16) Sb3 0.0218(2) 0.0203(2) 0.0253(2) -0.00755(17) -0.00402(17) 0.00234(16) Sb4 0.0183(2) 0.0203(2) 0.0225(2) -0.00449(17) -0.00556(17) 0.00052(16) Sb5 0.0245(2) 0.0248(2) 0.0219(2) -0.00415(18) -0.00109(18) 0.00215(17) Sb6 0.0248(2) 0.0247(2) 0.0222(2) -0.00275(18) -0.00290(18) 0.00224(17) Sb7 0.0242(2) 0.0261(2) 0.0225(2) -0.00543(18) -0.00032(18) 0.00079(17) Sb8 0.0246(2) 0.0256(2) 0.0245(2) -0.00600(18) -0.00301(18) 0.00064(17) O1 0.039(3) 0.052(3) 0.034(3) -0.013(3) 0.009(2) 0.002(2) O2 0.061(4) 0.029(3) 0.046(3) -0.005(3) 0.009(3) -0.003(3) C1 0.037(4) 0.023(3) 0.032(4) -0.006(3) -0.015(3) 0.005(3) C2 0.049(5) 0.037(4) 0.051(5) -0.014(4) -0.015(4) 0.005(4) C3 0.075(7) 0.034(5) 0.070(7) -0.018(5) -0.019(5) 0.016(4) C4 0.098(8) 0.039(5) 0.042(5) -0.001(4) -0.028(5) 0.001(5) C5 0.069(6) 0.044(5) 0.037(5) -0.001(4) -0.018(4) -0.002(4) C6 0.052(5) 0.033(4) 0.040(5) -0.002(3) -0.020(4) -0.004(4) C7 0.027(3) 0.030(4) 0.018(3) -0.008(3) -0.002(3) -0.005(3) C8 0.032(4) 0.039(4) 0.028(4) -0.009(3) -0.007(3) -0.004(3) C9 0.033(4) 0.048(5) 0.031(4) -0.011(3) -0.006(3) -0.015(3) C10 0.041(4) 0.043(4) 0.026(4) -0.015(3) 0.004(3) -0.019(3) C11 0.046(4) 0.025(4) 0.036(4) -0.011(3) 0.002(4) 0.003(3) C12 0.037(4) 0.033(4) 0.025(4) -0.009(3) -0.004(3) 0.006(3) C13 0.019(3) 0.046(4) 0.031(4) -0.014(3) -0.006(3) 0.002(3) C14 0.022(3) 0.049(5) 0.035(4) -0.016(4) -0.003(3) -0.007(3) C15 0.021(3) 0.036(4) 0.035(4) -0.007(3) -0.001(3) -0.009(3) C16 0.025(3) 0.019(3) 0.031(4) -0.009(3) -0.007(3) -0.001(2) C17 0.038(4) 0.027(4) 0.033(4) -0.010(3) 0.000(3) -0.009(3) C18 0.042(4) 0.021(4) 0.058(5) -0.010(3) -0.008(4) -0.004(3) C19 0.045(4) 0.033(4) 0.053(5) -0.022(4) -0.011(4) 0.001(3) C20 0.036(4) 0.049(5) 0.040(5) -0.025(4) -0.004(3) 0.002(3) C21 0.028(4) 0.034(4) 0.038(4) -0.011(3) -0.009(3) -0.001(3) C22 0.029(3) 0.025(3) 0.023(3) -0.008(3) 0.003(3) -0.009(3) C23 0.028(3) 0.024(3) 0.028(4) -0.002(3) -0.004(3) -0.007(3) C24 0.033(4) 0.031(4) 0.028(4) -0.005(3) -0.005(3) -0.002(3) C25 0.046(4) 0.041(4) 0.024(4) -0.008(3) -0.009(3) -0.006(3) C26 0.048(5) 0.042(4) 0.031(4) -0.016(4) -0.002(4) 0.003(4) C27 0.039(4) 0.037(4) 0.028(4) -0.007(3) -0.005(3) 0.002(3) C28 0.018(3) 0.032(4) 0.030(4) -0.010(3) 0.000(3) -0.001(3) C29 0.019(3) 0.026(4) 0.052(5) -0.004(3) -0.006(3) 0.004(3) C30 0.035(4) 0.031(4) 0.066(6) -0.009(4) -0.014(4) 0.004(3) C31 0.020(3) 0.035(4) 0.064(5) -0.017(4) -0.010(3) 0.004(3) C32 0.026(4) 0.045(5) 0.039(4) -0.012(4) -0.002(3) -0.010(3) C33 0.029(4) 0.029(4) 0.033(4) -0.009(3) -0.010(3) 0.000(3) C34 0.024(3) 0.020(3) 0.035(4) -0.009(3) -0.006(3) 0.000(3) C35 0.038(4) 0.029(4) 0.034(4) -0.014(3) -0.001(3) 0.000(3) C36 0.046(4) 0.021(4) 0.054(5) -0.017(3) -0.003(4) -0.002(3) C37 0.029(4) 0.024(4) 0.045(5) -0.003(3) 0.001(3) -0.004(3) C38 0.039(4) 0.033(4) 0.030(4) 0.000(3) 0.000(3) 0.004(3) C39 0.032(4) 0.029(4) 0.032(4) -0.009(3) -0.005(3) 0.002(3) C40 0.027(3) 0.027(3) 0.026(4) -0.012(3) -0.007(3) 0.005(3) C41 0.033(4) 0.029(4) 0.023(4) -0.010(3) -0.006(3) -0.005(3) C42 0.033(4) 0.027(4) 0.025(4) -0.011(3) -0.012(3) 0.004(3) C43 0.021(3) 0.020(3) 0.027(4) -0.006(3) -0.003(3) -0.002(2) C44 0.024(3) 0.028(4) 0.029(4) -0.008(3) -0.003(3) -0.002(3) C45 0.021(3) 0.041(4) 0.041(4) -0.019(4) -0.006(3) 0.003(3) C46 0.030(4) 0.032(4) 0.047(5) -0.020(4) 0.002(3) -0.010(3) C47 0.042(4) 0.033(4) 0.042(5) -0.005(3) -0.006(4) -0.009(3) C48 0.029(4) 0.029(4) 0.034(4) -0.005(3) -0.008(3) -0.003(3) C49 0.020(3) 0.019(3) 0.024(3) 0.004(3) -0.009(3) 0.002(2) C50 0.032(4) 0.021(3) 0.032(4) -0.005(3) -0.010(3) 0.000(3) C51 0.034(4) 0.032(4) 0.037(4) -0.010(3) -0.011(3) 0.005(3) C52 0.039(4) 0.025(4) 0.039(4) -0.001(3) -0.010(3) 0.003(3) C53 0.032(4) 0.031(4) 0.036(4) -0.008(3) -0.011(3) 0.005(3) C54 0.030(4) 0.025(3) 0.025(4) -0.002(3) -0.009(3) 0.000(3) C55 0.022(3) 0.027(4) 0.038(4) -0.013(3) -0.011(3) 0.005(3) C56 0.025(3) 0.027(4) 0.033(4) -0.011(3) -0.002(3) 0.005(3) C57 0.026(4) 0.034(4) 0.043(5) -0.001(3) -0.006(3) 0.002(3) C58 0.030(4) 0.040(4) 0.041(5) -0.002(4) -0.001(3) -0.004(3) C59 0.025(4) 0.029(4) 0.056(5) -0.004(4) -0.016(4) 0.002(3) C60 0.037(4) 0.035(4) 0.037(4) -0.008(3) -0.011(3) 0.007(3) C61 0.037(4) 0.023(3) 0.037(4) -0.006(3) -0.004(3) 0.004(3) C62 0.026(3) 0.024(3) 0.027(4) -0.001(3) -0.002(3) -0.002(3) C63 0.032(4) 0.032(4) 0.024(4) -0.006(3) -0.005(3) 0.006(3) C64 0.048(5) 0.035(4) 0.030(4) -0.011(3) -0.009(3) 0.014(3) C65 0.057(5) 0.028(4) 0.055(5) -0.018(4) -0.006(4) -0.011(4) C66 0.047(5) 0.035(4) 0.066(6) -0.015(4) 0.003(4) -0.010(4) C67 0.043(4) 0.030(4) 0.041(5) -0.012(3) -0.008(4) 0.008(3) C68 0.031(4) 0.029(4) 0.029(4) -0.004(3) 0.001(3) 0.000(3) C69 0.031(4) 0.030(4) 0.025(4) -0.006(3) 0.003(3) -0.004(3) C70 0.031(4) 0.026(4) 0.025(4) 0.000(3) -0.004(3) 0.005(3) C71 0.029(4) 0.032(4) 0.031(4) -0.008(3) -0.003(3) -0.001(3) C72 0.037(4) 0.037(4) 0.036(4) -0.013(3) 0.002(3) -0.004(3) C73 0.045(5) 0.041(5) 0.064(6) -0.024(4) -0.007(4) -0.008(4) C74 0.047(5) 0.067(6) 0.061(6) -0.034(5) -0.020(4) -0.003(4) C75 0.045(5) 0.058(6) 0.050(5) -0.012(4) -0.025(4) 0.009(4) C76 0.032(4) 0.039(4) 0.031(4) -0.005(3) -0.005(3) -0.004(3) C77 0.039(4) 0.028(4) 0.021(3) -0.009(3) -0.006(3) 0.007(3) C78 0.041(4) 0.029(4) 0.036(4) -0.005(3) -0.005(3) -0.002(3) C79 0.051(5) 0.025(4) 0.046(5) -0.013(3) -0.004(4) -0.001(3) C80 0.046(5) 0.033(4) 0.038(5) -0.009(3) -0.006(4) 0.009(3) C81 0.036(4) 0.041(4) 0.030(4) -0.001(3) -0.009(3) 0.013(3) C82 0.027(4) 0.035(4) 0.029(4) -0.002(3) -0.005(3) 0.001(3) C83 0.023(3) 0.034(4) 0.022(3) -0.002(3) -0.002(3) 0.002(3) C84 0.026(4) 0.045(4) 0.026(4) -0.013(3) 0.000(3) 0.000(3) C85 0.033(4) 0.048(5) 0.042(5) -0.012(4) -0.004(3) -0.008(3) C86 0.033(4) 0.068(6) 0.046(5) -0.018(4) -0.009(4) -0.003(4) C87 0.021(4) 0.063(5) 0.045(5) -0.018(4) 0.006(3) 0.006(3) C88 0.031(4) 0.043(4) 0.027(4) -0.009(3) -0.004(3) 0.008(3) C89 0.026(3) 0.031(4) 0.024(4) -0.006(3) -0.003(3) -0.002(3) C90 0.027(3) 0.041(4) 0.024(4) -0.010(3) 0.001(3) -0.002(3) C91 0.029(4) 0.049(5) 0.024(4) -0.010(3) 0.009(3) -0.013(3) C92 0.045(5) 0.052(5) 0.030(4) 0.001(4) -0.006(4) -0.012(4) C93 0.053(5) 0.045(5) 0.034(5) -0.006(4) -0.013(4) 0.007(4) C94 0.038(4) 0.037(4) 0.029(4) -0.007(3) -0.003(3) 0.006(3) C95 0.033(4) 0.025(4) 0.036(4) -0.014(3) 0.002(3) 0.000(3) C96 0.035(4) 0.029(4) 0.024(4) -0.008(3) -0.004(3) 0.003(3) C97 0.034(4) 0.026(4) 0.034(4) -0.009(3) -0.007(3) -0.001(3) C98 0.019(3) 0.028(3) 0.025(4) -0.004(3) -0.002(3) 0.006(3) C99 0.032(4) 0.041(4) 0.029(4) -0.014(3) -0.009(3) 0.008(3) C100 0.048(5) 0.031(4) 0.026(4) -0.005(3) 0.003(3) 0.011(3) C101 0.035(4) 0.049(5) 0.029(4) -0.013(4) -0.007(3) 0.017(3) C102 0.029(4) 0.054(5) 0.032(4) -0.016(4) -0.007(3) 0.006(3) C103 0.027(3) 0.039(4) 0.023(4) -0.005(3) 0.001(3) 0.002(3) C104 0.026(3) 0.031(4) 0.024(4) -0.003(3) -0.009(3) -0.008(3) C105 0.035(4) 0.041(4) 0.029(4) 0.002(3) -0.013(3) -0.004(3) C106 0.045(5) 0.041(4) 0.029(4) 0.004(3) -0.008(3) -0.014(4) C107 0.041(5) 0.068(6) 0.026(4) -0.010(4) -0.005(3) -0.023(4) C108 0.028(4) 0.053(5) 0.038(4) -0.013(4) 0.004(3) -0.014(3) C109 0.031(4) 0.027(4) 0.041(4) -0.010(3) -0.006(3) 0.000(3) C110 0.034(4) 0.034(4) 0.029(4) -0.008(3) 0.004(3) 0.003(3) P1 0.0483(14) 0.0774(18) 0.0462(14) -0.0237(13) -0.0082(11) 0.0069(12) P2 0.0396(11) 0.0435(12) 0.0383(12) -0.0175(10) 0.0021(9) -0.0004(9) F1 0.098(4) 0.100(5) 0.056(4) -0.024(3) -0.026(3) 0.037(4) F2 0.048(3) 0.220(8) 0.051(4) -0.023(4) -0.002(3) -0.019(4) F3 0.075(4) 0.072(4) 0.072(4) -0.034(3) -0.007(3) -0.015(3) F4 0.070(4) 0.091(4) 0.059(4) -0.010(3) -0.019(3) -0.005(3) F5 0.093(4) 0.109(5) 0.072(4) -0.028(4) -0.009(3) -0.047(4) F6 0.211(9) 0.133(6) 0.083(5) -0.076(5) -0.063(5) 0.100(6) F7 0.081(4) 0.092(4) 0.041(3) -0.024(3) 0.008(3) -0.036(3) F8 0.062(3) 0.055(3) 0.057(3) -0.010(3) -0.010(3) 0.017(2) F9 0.092(4) 0.112(5) 0.074(4) -0.052(4) 0.019(3) -0.058(4) F10 0.056(3) 0.091(4) 0.040(3) -0.008(3) -0.006(2) 0.023(3) F11 0.076(4) 0.174(7) 0.095(5) -0.079(5) -0.011(4) 0.069(4) F12 0.125(5) 0.052(3) 0.078(4) -0.020(3) 0.006(4) -0.036(3) Cl1 0.0719(17) 0.0742(18) 0.082(2) 0.0004(15) -0.0295(15) -0.0054(14) Cl2 0.0748(17) 0.0672(16) 0.0639(16) -0.0081(13) -0.0011(13) -0.0094(13) C111 0.058(6) 0.069(7) 0.056(6) -0.013(5) -0.020(5) 0.006(5) Cl3 0.101(2) 0.080(2) 0.0685(19) -0.0171(15) 0.0040(16) -0.0037(16) _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 C55 1.875(7) . ? Rh1 Sb1 2.5404(6) . ? Rh1 Sb4 2.5579(6) . ? Rh1 Sb2 2.5967(7) . ? Rh1 Sb3 2.6062(7) . ? Rh2 C110 1.856(7) . ? Rh2 Sb7 2.5585(7) . ? Rh2 Sb5 2.5588(7) . ? Rh2 Sb8 2.6080(7) . ? Rh2 Sb6 2.6173(7) . ? Sb1 C1 2.119(7) . ? Sb1 C7 2.129(6) . ? Sb1 C13 2.138(6) . ? Sb2 C22 2.133(6) . ? Sb2 C16 2.136(6) . ? Sb2 C15 2.156(6) . ? Sb3 C34 2.139(6) . ? Sb3 C40 2.146(6) . ? Sb3 C28 2.152(6) . ? Sb4 C49 2.120(6) . ? Sb4 C43 2.127(6) . ? Sb4 C42 2.139(6) . ? Sb5 C56 2.116(6) . ? Sb5 C62 2.126(7) . ? Sb5 C68 2.139(7) . ? Sb6 C71 2.129(7) . ? Sb6 C77 2.134(6) . ? Sb6 C70 2.142(7) . ? Sb7 C83 2.116(6) . ? Sb7 C89 2.140(7) . ? Sb7 C95 2.148(6) . ? Sb8 C104 2.129(6) . ? Sb8 C98 2.140(6) . ? Sb8 C97 2.164(7) . ? O1 C55 1.141(8) . ? O2 C110 1.151(8) . ? C1 C2 1.367(10) . ? C1 C6 1.382(10) . ? C2 C3 1.381(11) . ? C2 H2 0.9500 . ? C3 C4 1.361(13) . ? C3 H3 0.9500 . ? C4 C5 1.347(12) . ? C4 H4 0.9500 . ? C5 C6 1.384(10) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.381(9) . ? C7 C12 1.391(9) . ? C8 C9 1.389(9) . ? C8 H8 0.9500 . ? C9 C10 1.379(10) . ? C9 H9 0.9500 . ? C10 C11 1.352(10) . ? C10 H10 0.9500 . ? C11 C12 1.394(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.539(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.523(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.384(9) . ? C16 C21 1.389(9) . ? C17 C18 1.386(9) . ? C17 H17 0.9500 . ? C18 C19 1.384(11) . ? C18 H18 0.9500 . ? C19 C20 1.382(11) . ? C19 H19 0.9500 . ? C20 C21 1.398(10) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.377(9) . ? C22 C23 1.391(9) . ? C23 C24 1.387(9) . ? C23 H23 0.9500 . ? C24 C25 1.375(10) . ? C24 H24 0.9500 . ? C25 C26 1.371(10) . ? C25 H25 0.9500 . ? C26 C27 1.392(10) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.364(9) . ? C28 C33 1.400(9) . ? C29 C30 1.395(10) . ? C29 H29 0.9500 . ? C30 C31 1.388(11) . ? C30 H30 0.9500 . ? C31 C32 1.379(10) . ? C31 H31 0.9500 . ? C32 C33 1.399(9) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.375(9) . ? C34 C35 1.389(9) . ? C35 C36 1.393(10) . ? C35 H35 0.9500 . ? C36 C37 1.376(10) . ? C36 H36 0.9500 . ? C37 C38 1.386(10) . ? C37 H37 0.9500 . ? C38 C39 1.380(10) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.510(9) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.541(9) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C48 1.377(9) . ? C43 C44 1.396(9) . ? C44 C45 1.383(9) . ? C44 H44 0.9500 . ? C45 C46 1.375(10) . ? C45 H45 0.9500 . ? C46 C47 1.378(10) . ? C46 H46 0.9500 . ? C47 C48 1.393(9) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.380(9) . ? C49 C54 1.383(9) . ? C50 C51 1.374(9) . ? C50 H50 0.9500 . ? C51 C52 1.389(10) . ? C51 H51 0.9500 . ? C52 C53 1.390(10) . ? C52 H52 0.9500 . ? C53 C54 1.380(9) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C56 C61 1.392(10) . ? C56 C57 1.397(9) . ? C57 C58 1.381(10) . ? C57 H57 0.9500 . ? C58 C59 1.365(10) . ? C58 H58 0.9500 . ? C59 C60 1.387(10) . ? C59 H59 0.9500 . ? C60 C61 1.381(10) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 C67 1.373(10) . ? C62 C63 1.381(9) . ? C63 C64 1.394(10) . ? C63 H63 0.9500 . ? C64 C65 1.356(11) . ? C64 H64 0.9500 . ? C65 C66 1.386(11) . ? C65 H65 0.9500 . ? C66 C67 1.402(10) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C68 C69 1.529(9) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.516(9) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C76 1.387(10) . ? C71 C72 1.389(10) . ? C72 C73 1.362(10) . ? C72 H72 0.9500 . ? C73 C74 1.372(12) . ? C73 H73 0.9500 . ? C74 C75 1.385(12) . ? C74 H74 0.9500 . ? C75 C76 1.375(10) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77 C78 1.391(10) . ? C77 C82 1.394(9) . ? C78 C79 1.398(10) . ? C78 H78 0.9500 . ? C79 C80 1.371(10) . ? C79 H79 0.9500 . ? C80 C81 1.364(10) . ? C80 H80 0.9500 . ? C81 C82 1.394(10) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C84 1.386(9) . ? C83 C88 1.395(9) . ? C84 C85 1.384(10) . ? C84 H84 0.9500 . ? C85 C86 1.379(11) . ? C85 H85 0.9500 . ? C86 C87 1.387(11) . ? C86 H86 0.9500 . ? C87 C88 1.379(10) . ? C87 H87 0.9500 . ? C88 H88 0.9500 . ? C89 C94 1.381(9) . ? C89 C90 1.399(9) . ? C90 C91 1.387(9) . ? C90 H90 0.9500 . ? C91 C92 1.356(10) . ? C91 H91 0.9500 . ? C92 C93 1.409(11) . ? C92 H92 0.9500 . ? C93 C94 1.389(10) . ? C93 H93 0.9500 . ? C94 H94 0.9500 . ? C95 C96 1.520(9) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 C97 1.523(9) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 C99 1.388(9) . ? C98 C103 1.393(9) . ? C99 C100 1.393(10) . ? C99 H99 0.9500 . ? C100 C101 1.386(11) . ? C100 H100 0.9500 . ? C101 C102 1.373(11) . ? C101 H101 0.9500 . ? C102 C103 1.389(9) . ? C102 H102 0.9500 . ? C103 H103 0.9500 . ? C104 C105 1.385(9) . ? C104 C109 1.394(9) . ? C105 C106 1.411(10) . ? C105 H105 0.9500 . ? C106 C107 1.367(11) . ? C106 H106 0.9500 . ? C107 C108 1.362(11) . ? C107 H107 0.9500 . ? C108 C109 1.394(10) . ? C108 H108 0.9500 . ? C109 H109 0.9500 . ? P1 F6 1.581(6) . ? P1 F5 1.585(6) . ? P1 F4 1.586(6) . ? P1 F1 1.590(6) . ? P1 F2 1.600(7) . ? P1 F3 1.601(6) . ? P2 F9 1.572(6) . ? P2 F11 1.575(6) . ? P2 F7 1.578(5) . ? P2 F8 1.588(5) . ? P2 F10 1.589(5) . ? P2 F12 1.590(6) . ? Cl1 C111 1.761(9) . ? Cl2 C111 1.737(10) . ? C111 H11A 0.9900 . ? C111 H11B 0.9900 . ? Cl3 C112 1.700(14) . ? Cl3 C112 1.822(14) 2_575 ? C112 Cl3 1.822(14) 2_575 ? C112 H11C 0.9900 . ? C112 H11D 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 C55 Rh1 Sb1 88.67(19) . . ? C55 Rh1 Sb4 91.36(19) . . ? Sb1 Rh1 Sb4 177.99(2) . . ? C55 Rh1 Sb2 128.5(2) . . ? Sb1 Rh1 Sb2 87.70(2) . . ? Sb4 Rh1 Sb2 93.85(2) . . ? C55 Rh1 Sb3 125.2(2) . . ? Sb1 Rh1 Sb3 91.26(2) . . ? Sb4 Rh1 Sb3 87.08(2) . . ? Sb2 Rh1 Sb3 106.16(2) . . ? C110 Rh2 Sb7 90.1(2) . . ? C110 Rh2 Sb5 89.4(2) . . ? Sb7 Rh2 Sb5 178.53(3) . . ? C110 Rh2 Sb8 126.4(2) . . ? Sb7 Rh2 Sb8 88.26(2) . . ? Sb5 Rh2 Sb8 93.15(2) . . ? C110 Rh2 Sb6 133.8(2) . . ? Sb7 Rh2 Sb6 92.33(2) . . ? Sb5 Rh2 Sb6 87.04(2) . . ? Sb8 Rh2 Sb6 99.78(2) . . ? C1 Sb1 C7 100.2(3) . . ? C1 Sb1 C13 106.7(3) . . ? C7 Sb1 C13 98.8(3) . . ? C1 Sb1 Rh1 112.14(18) . . ? C7 Sb1 Rh1 119.50(17) . . ? C13 Sb1 Rh1 117.29(18) . . ? C22 Sb2 C16 99.5(2) . . ? C22 Sb2 C15 99.4(3) . . ? C16 Sb2 C15 100.2(2) . . ? C22 Sb2 Rh1 116.59(16) . . ? C16 Sb2 Rh1 119.50(18) . . ? C15 Sb2 Rh1 118.07(19) . . ? C34 Sb3 C40 98.7(3) . . ? C34 Sb3 C28 98.9(2) . . ? C40 Sb3 C28 96.6(2) . . ? C34 Sb3 Rh1 115.38(18) . . ? C40 Sb3 Rh1 116.86(17) . . ? C28 Sb3 Rh1 125.49(17) . . ? C49 Sb4 C43 102.1(2) . . ? C49 Sb4 C42 100.4(2) . . ? C43 Sb4 C42 97.6(3) . . ? C49 Sb4 Rh1 116.84(17) . . ? C43 Sb4 Rh1 117.89(17) . . ? C42 Sb4 Rh1 118.55(17) . . ? C56 Sb5 C62 104.1(2) . . ? C56 Sb5 C68 99.8(3) . . ? C62 Sb5 C68 100.4(3) . . ? C56 Sb5 Rh2 113.79(18) . . ? C62 Sb5 Rh2 116.02(18) . . ? C68 Sb5 Rh2 120.18(18) . . ? C71 Sb6 C77 98.0(3) . . ? C71 Sb6 C70 96.4(3) . . ? C77 Sb6 C70 98.5(3) . . ? C71 Sb6 Rh2 121.66(19) . . ? C77 Sb6 Rh2 121.31(17) . . ? C70 Sb6 Rh2 115.84(17) . . ? C83 Sb7 C89 103.5(2) . . ? C83 Sb7 C95 99.5(3) . . ? C89 Sb7 C95 98.6(3) . . ? C83 Sb7 Rh2 114.78(18) . . ? C89 Sb7 Rh2 119.67(18) . . ? C95 Sb7 Rh2 117.59(19) . . ? C104 Sb8 C98 102.2(2) . . ? C104 Sb8 C97 96.9(3) . . ? C98 Sb8 C97 95.8(3) . . ? C104 Sb8 Rh2 123.46(17) . . ? C98 Sb8 Rh2 117.15(18) . . ? C97 Sb8 Rh2 116.22(18) . . ? C2 C1 C6 119.3(7) . . ? C2 C1 Sb1 123.1(6) . . ? C6 C1 Sb1 117.4(5) . . ? C1 C2 C3 119.7(8) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 120.1(8) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 121.1(9) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 119.3(9) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C1 C6 C5 120.4(8) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C8 C7 C12 120.0(6) . . ? C8 C7 Sb1 118.1(5) . . ? C12 C7 Sb1 121.8(5) . . ? C7 C8 C9 119.9(7) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 119.7(7) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.6(7) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 120.8(7) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C7 C12 C11 119.0(7) . . ? C7 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 Sb1 112.2(4) . . ? C14 C13 H13A 109.2 . . ? Sb1 C13 H13A 109.2 . . ? C14 C13 H13B 109.2 . . ? Sb1 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C15 C14 C13 115.4(6) . . ? C15 C14 H14A 108.4 . . ? C13 C14 H14A 108.4 . . ? C15 C14 H14B 108.4 . . ? C13 C14 H14B 108.4 . . ? H14A C14 H14B 107.5 . . ? C14 C15 Sb2 116.8(4) . . ? C14 C15 H15A 108.1 . . ? Sb2 C15 H15A 108.1 . . ? C14 C15 H15B 108.1 . . ? Sb2 C15 H15B 108.1 . . ? H15A C15 H15B 107.3 . . ? C17 C16 C21 119.6(6) . . ? C17 C16 Sb2 120.6(5) . . ? C21 C16 Sb2 119.7(5) . . ? C16 C17 C18 120.6(7) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C19 C18 C17 119.9(7) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C20 C19 C18 119.9(7) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.3(7) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C16 C21 C20 119.6(7) . . ? C16 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C27 C22 C23 118.7(6) . . ? C27 C22 Sb2 119.7(5) . . ? C23 C22 Sb2 121.3(5) . . ? C24 C23 C22 120.6(6) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 119.7(7) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 120.4(7) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 119.8(7) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C22 C27 C26 120.7(7) . . ? C22 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C29 C28 C33 120.2(6) . . ? C29 C28 Sb3 121.0(5) . . ? C33 C28 Sb3 118.8(5) . . ? C28 C29 C30 119.9(7) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.6(7) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C32 C31 C30 119.4(7) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? C31 C32 C33 120.2(7) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C28 119.5(6) . . ? C32 C33 H33 120.2 . . ? C28 C33 H33 120.2 . . ? C39 C34 C35 118.9(6) . . ? C39 C34 Sb3 119.7(5) . . ? C35 C34 Sb3 121.3(5) . . ? C34 C35 C36 120.7(7) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C37 C36 C35 119.3(7) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? C36 C37 C38 120.4(6) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C39 C38 C37 119.7(7) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C34 C39 C38 121.0(7) . . ? C34 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C41 C40 Sb3 114.9(4) . . ? C41 C40 H40A 108.5 . . ? Sb3 C40 H40A 108.5 . . ? C41 C40 H40B 108.5 . . ? Sb3 C40 H40B 108.5 . . ? H40A C40 H40B 107.5 . . ? C40 C41 C42 114.5(5) . . ? C40 C41 H41A 108.6 . . ? C42 C41 H41A 108.6 . . ? C40 C41 H41B 108.6 . . ? C42 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? C41 C42 Sb4 112.1(4) . . ? C41 C42 H42A 109.2 . . ? Sb4 C42 H42A 109.2 . . ? C41 C42 H42B 109.2 . . ? Sb4 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? C48 C43 C44 119.9(6) . . ? C48 C43 Sb4 121.0(5) . . ? C44 C43 Sb4 119.1(5) . . ? C45 C44 C43 119.4(6) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C46 C45 C44 120.8(6) . . ? C46 C45 H45 119.6 . . ? C44 C45 H45 119.6 . . ? C45 C46 C47 119.9(6) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C48 119.9(7) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C43 C48 C47 120.1(6) . . ? C43 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C50 C49 C54 119.0(6) . . ? C50 C49 Sb4 122.3(5) . . ? C54 C49 Sb4 118.6(4) . . ? C51 C50 C49 120.6(6) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C50 C51 C52 120.1(7) . . ? C50 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C51 C52 C53 120.0(7) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C54 C53 C52 118.8(7) . . ? C54 C53 H53 120.6 . . ? C52 C53 H53 120.6 . . ? C53 C54 C49 121.5(6) . . ? C53 C54 H54 119.2 . . ? C49 C54 H54 119.2 . . ? O1 C55 Rh1 179.3(6) . . ? C61 C56 C57 119.8(6) . . ? C61 C56 Sb5 118.1(5) . . ? C57 C56 Sb5 121.9(5) . . ? C58 C57 C56 119.0(7) . . ? C58 C57 H57 120.5 . . ? C56 C57 H57 120.5 . . ? C59 C58 C57 120.8(7) . . ? C59 C58 H58 119.6 . . ? C57 C58 H58 119.6 . . ? C58 C59 C60 120.9(7) . . ? C58 C59 H59 119.5 . . ? C60 C59 H59 119.5 . . ? C61 C60 C59 119.0(7) . . ? C61 C60 H60 120.5 . . ? C59 C60 H60 120.5 . . ? C60 C61 C56 120.4(7) . . ? C60 C61 H61 119.8 . . ? C56 C61 H61 119.8 . . ? C67 C62 C63 120.3(6) . . ? C67 C62 Sb5 119.8(5) . . ? C63 C62 Sb5 119.8(5) . . ? C62 C63 C64 120.2(7) . . ? C62 C63 H63 119.9 . . ? C64 C63 H63 119.9 . . ? C65 C64 C63 119.4(7) . . ? C65 C64 H64 120.3 . . ? C63 C64 H64 120.3 . . ? C64 C65 C66 121.3(7) . . ? C64 C65 H65 119.4 . . ? C66 C65 H65 119.4 . . ? C65 C66 C67 119.3(7) . . ? C65 C66 H66 120.4 . . ? C67 C66 H66 120.4 . . ? C62 C67 C66 119.5(7) . . ? C62 C67 H67 120.3 . . ? C66 C67 H67 120.3 . . ? C69 C68 Sb5 115.1(4) . . ? C69 C68 H68A 108.5 . . ? Sb5 C68 H68A 108.5 . . ? C69 C68 H68B 108.5 . . ? Sb5 C68 H68B 108.5 . . ? H68A C68 H68B 107.5 . . ? C70 C69 C68 113.8(6) . . ? C70 C69 H69A 108.8 . . ? C68 C69 H69A 108.8 . . ? C70 C69 H69B 108.8 . . ? C68 C69 H69B 108.8 . . ? H69A C69 H69B 107.7 . . ? C69 C70 Sb6 113.9(4) . . ? C69 C70 H70A 108.8 . . ? Sb6 C70 H70A 108.8 . . ? C69 C70 H70B 108.8 . . ? Sb6 C70 H70B 108.8 . . ? H70A C70 H70B 107.7 . . ? C76 C71 C72 119.7(7) . . ? C76 C71 Sb6 119.3(5) . . ? C72 C71 Sb6 121.0(5) . . ? C73 C72 C71 119.8(7) . . ? C73 C72 H72 120.1 . . ? C71 C72 H72 120.1 . . ? C72 C73 C74 120.5(8) . . ? C72 C73 H73 119.7 . . ? C74 C73 H73 119.7 . . ? C73 C74 C75 120.5(8) . . ? C73 C74 H74 119.7 . . ? C75 C74 H74 119.7 . . ? C76 C75 C74 119.2(8) . . ? C76 C75 H75 120.4 . . ? C74 C75 H75 120.4 . . ? C75 C76 C71 120.2(7) . . ? C75 C76 H76 119.9 . . ? C71 C76 H76 119.9 . . ? C78 C77 C82 119.5(6) . . ? C78 C77 Sb6 120.9(5) . . ? C82 C77 Sb6 119.6(5) . . ? C77 C78 C79 120.0(7) . . ? C77 C78 H78 120.0 . . ? C79 C78 H78 120.0 . . ? C80 C79 C78 119.4(7) . . ? C80 C79 H79 120.3 . . ? C78 C79 H79 120.3 . . ? C81 C80 C79 121.5(7) . . ? C81 C80 H80 119.2 . . ? C79 C80 H80 119.2 . . ? C80 C81 C82 119.8(7) . . ? C80 C81 H81 120.1 . . ? C82 C81 H81 120.1 . . ? C77 C82 C81 119.7(7) . . ? C77 C82 H82 120.1 . . ? C81 C82 H82 120.1 . . ? C84 C83 C88 119.8(6) . . ? C84 C83 Sb7 118.7(5) . . ? C88 C83 Sb7 121.1(5) . . ? C85 C84 C83 120.2(7) . . ? C85 C84 H84 119.9 . . ? C83 C84 H84 119.9 . . ? C86 C85 C84 119.9(7) . . ? C86 C85 H85 120.1 . . ? C84 C85 H85 120.1 . . ? C85 C86 C87 120.2(7) . . ? C85 C86 H86 119.9 . . ? C87 C86 H86 119.9 . . ? C88 C87 C86 120.2(7) . . ? C88 C87 H87 119.9 . . ? C86 C87 H87 119.9 . . ? C87 C88 C83 119.7(7) . . ? C87 C88 H88 120.1 . . ? C83 C88 H88 120.1 . . ? C94 C89 C90 119.7(6) . . ? C94 C89 Sb7 121.2(5) . . ? C90 C89 Sb7 118.9(5) . . ? C91 C90 C89 119.1(7) . . ? C91 C90 H90 120.4 . . ? C89 C90 H90 120.4 . . ? C92 C91 C90 121.6(7) . . ? C92 C91 H91 119.2 . . ? C90 C91 H91 119.2 . . ? C91 C92 C93 119.8(7) . . ? C91 C92 H92 120.1 . . ? C93 C92 H92 120.1 . . ? C94 C93 C92 119.1(7) . . ? C94 C93 H93 120.5 . . ? C92 C93 H93 120.5 . . ? C89 C94 C93 120.7(7) . . ? C89 C94 H94 119.7 . . ? C93 C94 H94 119.7 . . ? C96 C95 Sb7 115.8(4) . . ? C96 C95 H95A 108.3 . . ? Sb7 C95 H95A 108.3 . . ? C96 C95 H95B 108.3 . . ? Sb7 C95 H95B 108.3 . . ? H95A C95 H95B 107.4 . . ? C95 C96 C97 114.9(6) . . ? C95 C96 H96A 108.6 . . ? C97 C96 H96A 108.6 . . ? C95 C96 H96B 108.6 . . ? C97 C96 H96B 108.6 . . ? H96A C96 H96B 107.5 . . ? C96 C97 Sb8 113.7(4) . . ? C96 C97 H97A 108.8 . . ? Sb8 C97 H97A 108.8 . . ? C96 C97 H97B 108.8 . . ? Sb8 C97 H97B 108.8 . . ? H97A C97 H97B 107.7 . . ? C99 C98 C103 118.7(6) . . ? C99 C98 Sb8 119.9(5) . . ? C103 C98 Sb8 121.4(5) . . ? C98 C99 C100 121.0(7) . . ? C98 C99 H99 119.5 . . ? C100 C99 H99 119.5 . . ? C101 C100 C99 119.1(7) . . ? C101 C100 H100 120.4 . . ? C99 C100 H100 120.4 . . ? C102 C101 C100 120.5(7) . . ? C102 C101 H101 119.7 . . ? C100 C101 H101 119.7 . . ? C101 C102 C103 120.2(7) . . ? C101 C102 H102 119.9 . . ? C103 C102 H102 119.9 . . ? C102 C103 C98 120.4(7) . . ? C102 C103 H103 119.8 . . ? C98 C103 H103 119.8 . . ? C105 C104 C109 118.9(6) . . ? C105 C104 Sb8 119.7(5) . . ? C109 C104 Sb8 121.3(5) . . ? C104 C105 C106 120.1(7) . . ? C104 C105 H105 120.0 . . ? C106 C105 H105 120.0 . . ? C107 C106 C105 119.7(7) . . ? C107 C106 H106 120.2 . . ? C105 C106 H106 120.2 . . ? C108 C107 C106 120.8(7) . . ? C108 C107 H107 119.6 . . ? C106 C107 H107 119.6 . . ? C107 C108 C109 120.4(7) . . ? C107 C108 H108 119.8 . . ? C109 C108 H108 119.8 . . ? C108 C109 C104 120.1(7) . . ? C108 C109 H109 120.0 . . ? C104 C109 H109 120.0 . . ? O2 C110 Rh2 179.5(7) . . ? F6 P1 F5 91.9(5) . . ? F6 P1 F4 89.7(3) . . ? F5 P1 F4 90.9(3) . . ? F6 P1 F1 89.7(4) . . ? F5 P1 F1 90.7(4) . . ? F4 P1 F1 178.3(4) . . ? F6 P1 F2 91.7(5) . . ? F5 P1 F2 176.4(4) . . ? F4 P1 F2 88.6(3) . . ? F1 P1 F2 89.8(4) . . ? F6 P1 F3 179.1(4) . . ? F5 P1 F3 87.7(3) . . ? F4 P1 F3 91.1(3) . . ? F1 P1 F3 89.5(3) . . ? F2 P1 F3 88.7(4) . . ? F9 P2 F11 90.5(4) . . ? F9 P2 F7 90.9(3) . . ? F11 P2 F7 88.3(3) . . ? F9 P2 F8 89.8(3) . . ? F11 P2 F8 179.7(4) . . ? F7 P2 F8 91.7(3) . . ? F9 P2 F10 90.1(3) . . ? F11 P2 F10 90.7(3) . . ? F7 P2 F10 178.6(3) . . ? F8 P2 F10 89.3(3) . . ? F9 P2 F12 178.2(4) . . ? F11 P2 F12 91.1(4) . . ? F7 P2 F12 88.5(3) . . ? F8 P2 F12 88.6(3) . . ? F10 P2 F12 90.5(3) . . ? Cl2 C111 Cl1 111.6(5) . . ? Cl2 C111 H11A 109.3 . . ? Cl1 C111 H11A 109.3 . . ? Cl2 C111 H11B 109.3 . . ? Cl1 C111 H11B 109.3 . . ? H11A C111 H11B 108.0 . . ? C112 Cl3 C112 70.7(9) . 2_575 ? Cl3 C112 Cl3 109.3(9) . 2_575 ? Cl3 C112 H11C 109.8 . . ? Cl3 C112 H11C 109.8 2_575 . ? Cl3 C112 H11D 109.8 . . ? Cl3 C112 H11D 109.8 2_575 . ? H11C C112 H11D 108.3 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.535 _refine_diff_density_min -1.573 _refine_diff_density_rms 0.169 #===END OF CIF ============================================================== # 05mdb024 data_05mdb024 _database_code_depnum_ccdc_archive 'CCDC 604225' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-02-16 _chemical_name_systematic ; Dichloro(1,3-bis(diphenylstibino)propane)(1,3-bis(chlorophenylstibino)- propane)rhodium(III) chloride chloroform solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H42 Cl4 Rh Sb4 1+, Cl 1-, C H Cl3' _chemical_formula_sum 'C43 H43 Cl8 Rh Sb4' _chemical_formula_structural '((Rh Cl2) (C27 H26 Sb2) (C15 H16 Cl2 Sb2)) (Cl) (C H Cl3)' _chemical_formula_weight 1433.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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/c' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2ybc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 28.147(6) _cell_length_b 10.9609(16) _cell_length_c 15.724(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.095(8) _cell_angle_gamma 90.00 _cell_volume 4705.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6754 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 3.096 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7141 # shelxl 0.7077 _exptl_absorpt_correction_T_max 1.0000 # 0.8862 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31249 _diffrn_reflns_av_R_equivalents 0.0895 _diffrn_reflns_av_sigmaI/netI 0.1200 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9970 _reflns_number_gt 6847 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+131.0000P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9970 _refine_ls_number_parameters 505 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1508 _refine_ls_R_factor_gt 0.1057 _refine_ls_wR_factor_ref 0.1730 _refine_ls_wR_factor_gt 0.1492 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.164 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.71944(4) 0.51400(8) 0.34107(6) 0.0162(2) Uani 1 1 d . . . Sb1 Sb 0.65561(3) 0.48318(7) 0.19333(5) 0.01750(19) Uani 1 1 d U . . Sb2 Sb 0.78512(3) 0.40925(7) 0.27568(5) 0.0194(2) Uani 1 1 d . . . Sb3 Sb 0.78206(3) 0.53528(7) 0.49427(5) 0.0197(2) Uani 1 1 d . . . Sb4 Sb 0.66477(3) 0.64180(7) 0.41965(5) 0.0191(2) Uani 1 1 d . . . Cl1 Cl 0.74583(11) 0.6915(2) 0.27462(17) 0.0141(6) Uani 1 1 d . . . Cl2 Cl 0.68787(12) 0.3373(2) 0.39475(18) 0.0178(6) Uani 1 1 d . . . Cl3 Cl 0.81431(13) 0.3280(3) 0.5164(2) 0.0272(7) Uani 1 1 d . . . Cl4 Cl 0.58414(13) 0.5480(3) 0.3735(2) 0.0249(7) Uani 1 1 d . . . C1 C 0.6002(5) 0.6208(11) 0.1561(7) 0.018(3) Uani 1 1 d . . . C2 C 0.5543(5) 0.5928(12) 0.1046(9) 0.027(3) Uani 1 1 d . . . H2 H 0.5473 0.5119 0.0837 0.032 Uiso 1 1 calc R . . C3 C 0.5185(5) 0.6819(12) 0.0834(9) 0.028(3) Uani 1 1 d . . . H3 H 0.4874 0.6625 0.0463 0.033 Uiso 1 1 calc R . . C4 C 0.5278(6) 0.7993(12) 0.1161(9) 0.029(3) Uani 1 1 d . . . H4 H 0.5029 0.8598 0.1033 0.034 Uiso 1 1 calc R . . C5 C 0.5742(5) 0.8274(11) 0.1682(7) 0.018(3) Uani 1 1 d . . . H5 H 0.5810 0.9080 0.1901 0.022 Uiso 1 1 calc R . . C6 C 0.6106(5) 0.7395(10) 0.1884(7) 0.017(3) Uani 1 1 d . . . H6 H 0.6421 0.7593 0.2236 0.021 Uiso 1 1 calc R . . C7 C 0.6086(5) 0.3271(10) 0.1655(8) 0.019(3) Uani 1 1 d . . . C8 C 0.6121(5) 0.2518(11) 0.0954(9) 0.029(3) Uani 1 1 d U . . H8 H 0.6373 0.2633 0.0656 0.035 Uiso 1 1 calc R . . C9 C 0.5772(6) 0.1591(12) 0.0705(10) 0.034(3) Uani 1 1 d U . . H9 H 0.5795 0.1056 0.0241 0.041 Uiso 1 1 calc R . . C10 C 0.5402(6) 0.1440(12) 0.1114(9) 0.031(3) Uani 1 1 d U . . H10 H 0.5166 0.0814 0.0929 0.037 Uiso 1 1 calc R . . C11 C 0.5371(6) 0.2209(12) 0.1804(9) 0.033(4) Uani 1 1 d . . . H11 H 0.5113 0.2111 0.2091 0.040 Uiso 1 1 calc R . . C12 C 0.5716(5) 0.3112(12) 0.2068(8) 0.022(3) Uani 1 1 d . . . H12 H 0.5696 0.3630 0.2542 0.026 Uiso 1 1 calc R . . C13 C 0.6854(5) 0.4836(12) 0.0800(8) 0.021(3) Uani 1 1 d U . . H13A H 0.6583 0.4677 0.0278 0.025 Uiso 1 1 calc R . . H13B H 0.6979 0.5667 0.0734 0.025 Uiso 1 1 calc R . . C14 C 0.7269(6) 0.3918(12) 0.0791(8) 0.028(3) Uani 1 1 d U . . H14A H 0.7175 0.3113 0.0984 0.034 Uiso 1 1 calc R . . H14B H 0.7301 0.3830 0.0182 0.034 Uiso 1 1 calc R . . C15 C 0.7762(5) 0.4280(11) 0.1372(8) 0.024(3) Uani 1 1 d U . . H15A H 0.7825 0.5142 0.1248 0.029 Uiso 1 1 calc R . . H15B H 0.8017 0.3782 0.1201 0.029 Uiso 1 1 calc R . . C16 C 0.8559(5) 0.4903(12) 0.3134(9) 0.025(3) Uani 1 1 d . . . C17 C 0.8675(6) 0.5941(13) 0.2710(9) 0.030(3) Uani 1 1 d . . . H17 H 0.8434 0.6304 0.2249 0.036 Uiso 1 1 calc R . . C18 C 0.9129(6) 0.6429(14) 0.2956(10) 0.035(4) Uani 1 1 d . . . H18 H 0.9200 0.7155 0.2682 0.042 Uiso 1 1 calc R . . C19 C 0.9490(6) 0.5888(15) 0.3600(11) 0.044(4) Uani 1 1 d . . . H19 H 0.9810 0.6228 0.3747 0.053 Uiso 1 1 calc R . . C20 C 0.9391(6) 0.4864(15) 0.4028(10) 0.040(4) Uani 1 1 d . . . H20 H 0.9639 0.4506 0.4479 0.048 Uiso 1 1 calc R . . C21 C 0.8923(6) 0.4354(14) 0.3795(9) 0.033(3) Uani 1 1 d . . . H21 H 0.8850 0.3640 0.4082 0.040 Uiso 1 1 calc R . . C22 C 0.8030(5) 0.2208(10) 0.2957(8) 0.021(3) Uani 1 1 d . . . C23 C 0.8464(6) 0.1799(11) 0.2725(9) 0.028(3) Uani 1 1 d . . . H23 H 0.8643 0.2349 0.2453 0.034 Uiso 1 1 calc R . . C24 C 0.8624(6) 0.0635(12) 0.2889(8) 0.026(3) Uani 1 1 d . . . H24 H 0.8916 0.0384 0.2738 0.032 Uiso 1 1 calc R . . C25 C 0.8371(6) -0.0186(12) 0.3270(9) 0.032(4) Uani 1 1 d . . . H25 H 0.8483 -0.1003 0.3374 0.038 Uiso 1 1 calc R . . C26 C 0.7951(6) 0.0191(12) 0.3498(9) 0.034(4) Uani 1 1 d . . . H26 H 0.7772 -0.0377 0.3754 0.040 Uiso 1 1 calc R . . C27 C 0.7781(6) 0.1412(11) 0.3359(9) 0.031(4) Uani 1 1 d . . . H27 H 0.7499 0.1670 0.3542 0.037 Uiso 1 1 calc R . . C28 C 0.8547(5) 0.6134(11) 0.5301(9) 0.022(3) Uani 1 1 d . . . C29 C 0.8899(5) 0.5528(12) 0.5939(8) 0.025(3) Uani 1 1 d . . . H29 H 0.8825 0.4788 0.6194 0.030 Uiso 1 1 calc R . . C30 C 0.9367(5) 0.6054(13) 0.6189(9) 0.032(3) Uani 1 1 d . . . H30 H 0.9616 0.5671 0.6624 0.039 Uiso 1 1 calc R . . C31 C 0.9462(6) 0.7098(14) 0.5815(10) 0.035(4) Uani 1 1 d . . . H31 H 0.9778 0.7452 0.6005 0.042 Uiso 1 1 calc R . . C32 C 0.9120(6) 0.7669(14) 0.5171(10) 0.035(4) Uani 1 1 d . . . H32 H 0.9202 0.8385 0.4898 0.042 Uiso 1 1 calc R . . C33 C 0.8641(5) 0.7177(12) 0.4915(9) 0.023(3) Uani 1 1 d . . . H33 H 0.8392 0.7570 0.4485 0.028 Uiso 1 1 calc R . . C34 C 0.7573(6) 0.5251(13) 0.6115(9) 0.030(3) Uani 1 1 d . . . H34A H 0.7744 0.4567 0.6473 0.036 Uiso 1 1 calc R . . H34B H 0.7670 0.6011 0.6453 0.036 Uiso 1 1 calc R . . C35 C 0.7020(6) 0.5074(13) 0.5986(9) 0.033(4) Uani 1 1 d . . . H35A H 0.6927 0.4320 0.5638 0.040 Uiso 1 1 calc R . . H35B H 0.6957 0.4928 0.6570 0.040 Uiso 1 1 calc R . . C36 C 0.6681(5) 0.6078(13) 0.5548(8) 0.027(3) Uani 1 1 d . . . H36A H 0.6781 0.6843 0.5878 0.033 Uiso 1 1 calc R . . H36B H 0.6346 0.5879 0.5601 0.033 Uiso 1 1 calc R . . C37 C 0.6350(5) 0.8224(11) 0.3954(8) 0.022(3) Uani 1 1 d . . . C38 C 0.6608(6) 0.9130(12) 0.3629(8) 0.025(3) Uani 1 1 d . . . H38 H 0.6918 0.8954 0.3519 0.030 Uiso 1 1 calc R . . C39 C 0.6408(7) 1.0286(12) 0.3470(8) 0.032(4) Uani 1 1 d . . . H39 H 0.6585 1.0911 0.3262 0.038 Uiso 1 1 calc R . . C40 C 0.5952(6) 1.0533(13) 0.3612(9) 0.033(4) Uani 1 1 d . . . H40 H 0.5812 1.1322 0.3491 0.039 Uiso 1 1 calc R . . C41 C 0.5699(6) 0.9615(12) 0.3936(10) 0.033(3) Uani 1 1 d . . . H41 H 0.5390 0.9794 0.4050 0.040 Uiso 1 1 calc R . . C42 C 0.5890(5) 0.8442(11) 0.4094(9) 0.022(3) Uani 1 1 d . . . H42 H 0.5712 0.7812 0.4292 0.026 Uiso 1 1 calc R . . Cl6 Cl 0.9942(2) 0.9726(4) 0.3723(3) 0.0636(14) Uani 1 1 d . . . Cl7 Cl 1.0878(3) 0.8865(6) 0.4695(5) 0.139(4) Uani 1 1 d . . . Cl8 Cl 1.0451(2) 0.7880(5) 0.2992(3) 0.0691(15) Uani 1 1 d . . . C43 C 1.0530(8) 0.9171(17) 0.3661(14) 0.073(7) Uani 1 1 d . . . H43 H 1.0698 0.9816 0.3391 0.088 Uiso 1 1 calc R . . Cl5 Cl 0.75116(13) 0.7717(3) 0.4964(2) 0.0237(7) 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 0.0152(5) 0.0161(5) 0.0174(4) -0.0002(4) 0.0044(4) 0.0003(4) Sb1 0.0162(5) 0.0169(4) 0.0187(4) 0.0007(3) 0.0029(3) 0.0003(3) Sb2 0.0171(5) 0.0194(4) 0.0220(4) -0.0015(3) 0.0053(3) -0.0004(3) Sb3 0.0183(5) 0.0216(4) 0.0184(4) 0.0005(3) 0.0028(3) -0.0004(4) Sb4 0.0188(5) 0.0189(4) 0.0201(4) 0.0006(3) 0.0058(3) 0.0023(3) Cl1 0.0138(15) 0.0112(12) 0.0178(13) 0.0004(10) 0.0048(11) -0.0018(11) Cl2 0.0185(16) 0.0139(13) 0.0216(14) 0.0006(11) 0.0062(12) -0.0008(12) Cl3 0.027(2) 0.0234(16) 0.0304(16) 0.0044(13) 0.0046(14) 0.0024(14) Cl4 0.0212(18) 0.0230(15) 0.0306(16) -0.0005(13) 0.0064(14) -0.0027(13) C1 0.010(7) 0.026(6) 0.017(6) -0.002(5) 0.003(5) 0.006(5) C2 0.023(8) 0.020(6) 0.036(7) -0.002(6) 0.005(6) -0.002(6) C3 0.017(8) 0.028(7) 0.039(8) 0.013(6) 0.009(6) -0.002(6) C4 0.032(9) 0.026(7) 0.029(7) 0.006(6) 0.008(6) 0.012(6) C5 0.013(7) 0.028(7) 0.017(6) 0.004(5) 0.009(5) 0.000(5) C6 0.019(7) 0.018(6) 0.013(5) 0.002(5) -0.001(5) -0.002(5) C7 0.018(7) 0.014(6) 0.020(6) 0.001(5) -0.004(5) -0.003(5) C8 0.013(7) 0.024(7) 0.044(8) -0.007(6) -0.007(6) 0.002(5) C9 0.032(9) 0.025(7) 0.042(8) -0.015(6) 0.003(6) -0.002(6) C10 0.028(8) 0.022(7) 0.038(8) 0.007(6) 0.000(6) 0.003(6) C11 0.035(10) 0.034(8) 0.028(7) 0.014(6) 0.003(7) 0.001(7) C12 0.024(8) 0.031(7) 0.012(5) -0.002(5) 0.006(5) -0.009(6) C13 0.021(6) 0.031(7) 0.015(5) 0.010(5) 0.011(5) 0.000(5) C14 0.038(8) 0.030(7) 0.014(6) -0.009(5) 0.000(5) 0.012(6) C15 0.026(7) 0.018(6) 0.032(7) -0.005(5) 0.012(6) 0.009(5) C16 0.018(8) 0.028(7) 0.031(7) -0.008(6) 0.010(6) -0.005(6) C17 0.028(9) 0.036(8) 0.027(7) -0.009(6) 0.011(6) -0.010(7) C18 0.027(9) 0.040(8) 0.044(9) -0.011(7) 0.021(7) -0.009(7) C19 0.029(10) 0.058(10) 0.048(9) -0.018(8) 0.017(8) -0.027(8) C20 0.028(10) 0.056(10) 0.036(8) -0.014(8) 0.009(7) 0.006(8) C21 0.024(9) 0.038(8) 0.035(8) -0.002(6) 0.005(7) 0.008(7) C22 0.030(8) 0.010(5) 0.022(6) -0.001(5) 0.007(6) -0.005(5) C23 0.031(9) 0.020(6) 0.032(7) 0.000(6) 0.005(6) -0.001(6) C24 0.034(9) 0.028(7) 0.022(6) 0.002(5) 0.017(6) 0.016(6) C25 0.038(10) 0.022(7) 0.030(7) -0.003(6) -0.003(7) 0.008(7) C26 0.037(10) 0.024(7) 0.036(8) 0.007(6) 0.001(7) -0.005(7) C27 0.030(9) 0.018(6) 0.035(8) 0.001(6) -0.009(6) 0.011(6) C28 0.010(7) 0.023(6) 0.034(7) -0.005(5) 0.007(6) -0.002(5) C29 0.025(8) 0.031(7) 0.018(6) -0.006(5) 0.003(6) -0.002(6) C30 0.014(8) 0.037(8) 0.040(8) 0.009(7) -0.007(6) 0.003(6) C31 0.017(8) 0.049(9) 0.040(8) -0.017(7) 0.008(7) 0.003(7) C32 0.022(9) 0.042(8) 0.046(9) -0.001(7) 0.019(7) -0.005(7) C33 0.008(7) 0.031(7) 0.032(7) 0.003(6) 0.008(5) 0.002(5) C34 0.022(8) 0.035(8) 0.033(7) 0.004(6) 0.006(6) 0.005(6) C35 0.037(10) 0.044(8) 0.019(6) 0.005(6) 0.008(6) 0.000(7) C36 0.015(7) 0.044(8) 0.023(6) 0.006(6) 0.003(5) -0.001(6) C37 0.026(8) 0.019(6) 0.020(6) -0.003(5) 0.003(6) 0.007(6) C38 0.028(8) 0.029(7) 0.021(6) -0.004(5) 0.010(6) -0.001(6) C39 0.064(12) 0.022(7) 0.011(6) -0.003(5) 0.010(6) -0.007(7) C40 0.035(10) 0.034(8) 0.030(7) -0.010(6) 0.010(7) 0.004(7) C41 0.025(9) 0.028(7) 0.044(8) 0.002(6) 0.003(7) 0.008(6) C42 0.010(7) 0.021(6) 0.040(7) -0.003(6) 0.015(6) 0.000(5) Cl6 0.046(3) 0.063(3) 0.076(3) -0.008(2) 0.005(3) 0.011(2) Cl7 0.134(7) 0.095(5) 0.131(6) -0.035(4) -0.078(5) 0.065(5) Cl8 0.052(4) 0.093(4) 0.067(3) 0.000(3) 0.024(3) 0.019(3) C43 0.063(17) 0.048(11) 0.088(15) 0.014(11) -0.019(13) 0.012(10) Cl5 0.0240(19) 0.0219(15) 0.0258(15) -0.0019(12) 0.0070(13) 0.0010(13) _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 Cl2 2.371(3) . ? Rh1 Cl1 2.410(3) . ? Rh1 Sb1 2.5896(13) . ? Rh1 Sb2 2.5920(14) . ? Rh1 Sb4 2.6045(14) . ? Rh1 Sb3 2.6261(13) . ? Sb1 C7 2.142(12) . ? Sb1 C1 2.146(12) . ? Sb1 C13 2.146(12) . ? Sb2 C16 2.130(14) . ? Sb2 C22 2.131(12) . ? Sb2 C15 2.140(13) . ? Sb3 C34 2.126(15) . ? Sb3 C28 2.162(13) . ? Sb3 Cl3 2.440(3) . ? Sb3 Cl5 2.736(3) . ? Sb4 C36 2.137(13) . ? Sb4 C37 2.147(12) . ? Sb4 Cl4 2.435(4) . ? Sb4 Cl5 2.823(3) . ? C1 C2 1.380(18) . ? C1 C6 1.401(16) . ? C2 C3 1.385(19) . ? C2 H2 0.9500 . ? C3 C4 1.386(19) . ? C3 H3 0.9500 . ? C4 C5 1.398(19) . ? C4 H4 0.9500 . ? C5 C6 1.385(17) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.366(18) . ? C7 C8 1.399(18) . ? C8 C9 1.401(19) . ? C8 H8 0.9500 . ? C9 C10 1.36(2) . ? C9 H9 0.9500 . ? C10 C11 1.39(2) . ? C10 H10 0.9500 . ? C11 C12 1.378(19) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.544(18) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.518(19) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.396(19) . ? C16 C21 1.405(19) . ? C17 C18 1.35(2) . ? C17 H17 0.9500 . ? C18 C19 1.38(2) . ? C18 H18 0.9500 . ? C19 C20 1.37(2) . ? C19 H19 0.9500 . ? C20 C21 1.40(2) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.37(2) . ? C22 C23 1.43(2) . ? C23 C24 1.357(18) . ? C23 H23 0.9500 . ? C24 C25 1.37(2) . ? C24 H24 0.9500 . ? C25 C26 1.38(2) . ? C25 H25 0.9500 . ? C26 C27 1.420(18) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.349(18) . ? C28 C29 1.394(18) . ? C29 C30 1.403(19) . ? C29 H29 0.9500 . ? C30 C31 1.34(2) . ? C30 H30 0.9500 . ? C31 C32 1.37(2) . ? C31 H31 0.9500 . ? C32 C33 1.42(2) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.53(2) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.509(19) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C42 1.384(18) . ? C37 C38 1.399(19) . ? C38 C39 1.384(19) . ? C38 H38 0.9500 . ? C39 C40 1.38(2) . ? C39 H39 0.9500 . ? C40 C41 1.40(2) . ? C40 H40 0.9500 . ? C41 C42 1.393(18) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? Cl6 C43 1.79(2) . ? Cl7 C43 1.71(2) . ? Cl8 C43 1.75(2) . ? C43 H43 1.0000 . ? 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 Cl2 Rh1 Cl1 174.86(11) . . ? Cl2 Rh1 Sb1 88.54(8) . . ? Cl1 Rh1 Sb1 86.34(7) . . ? Cl2 Rh1 Sb2 98.32(8) . . ? Cl1 Rh1 Sb2 81.99(8) . . ? Sb1 Rh1 Sb2 89.56(4) . . ? Cl2 Rh1 Sb4 87.39(8) . . ? Cl1 Rh1 Sb4 92.96(8) . . ? Sb1 Rh1 Sb4 97.75(5) . . ? Sb2 Rh1 Sb4 170.86(5) . . ? Cl2 Rh1 Sb3 88.39(8) . . ? Cl1 Rh1 Sb3 96.73(8) . . ? Sb1 Rh1 Sb3 176.92(5) . . ? Sb2 Rh1 Sb3 91.09(4) . . ? Sb4 Rh1 Sb3 81.90(4) . . ? C7 Sb1 C1 97.7(5) . . ? C7 Sb1 C13 100.3(5) . . ? C1 Sb1 C13 100.2(5) . . ? C7 Sb1 Rh1 123.1(3) . . ? C1 Sb1 Rh1 116.9(3) . . ? C13 Sb1 Rh1 114.8(4) . . ? C16 Sb2 C22 101.1(5) . . ? C16 Sb2 C15 96.5(5) . . ? C22 Sb2 C15 102.0(5) . . ? C16 Sb2 Rh1 114.5(4) . . ? C22 Sb2 Rh1 122.4(4) . . ? C15 Sb2 Rh1 116.3(4) . . ? C34 Sb3 C28 106.5(5) . . ? C34 Sb3 Cl3 91.0(4) . . ? C28 Sb3 Cl3 92.1(3) . . ? C34 Sb3 Rh1 120.1(4) . . ? C28 Sb3 Rh1 130.9(4) . . ? Cl3 Sb3 Rh1 101.03(8) . . ? C34 Sb3 Cl5 82.3(4) . . ? C28 Sb3 Cl5 84.6(3) . . ? Cl3 Sb3 Cl5 171.30(11) . . ? Rh1 Sb3 Cl5 87.19(7) . . ? C36 Sb4 C37 104.9(5) . . ? C36 Sb4 Cl4 92.0(4) . . ? C37 Sb4 Cl4 92.3(4) . . ? C36 Sb4 Rh1 119.4(4) . . ? C37 Sb4 Rh1 131.4(4) . . ? Cl4 Sb4 Rh1 104.29(9) . . ? C36 Sb4 Cl5 80.7(4) . . ? C37 Sb4 Cl5 82.5(4) . . ? Cl4 Sb4 Cl5 169.59(11) . . ? Rh1 Sb4 Cl5 85.82(8) . . ? C2 C1 C6 120.1(11) . . ? C2 C1 Sb1 121.1(9) . . ? C6 C1 Sb1 118.7(9) . . ? C1 C2 C3 120.4(12) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C2 C3 C4 120.3(13) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C5 119.1(13) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 120.9(12) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C1 119.0(11) . . ? C5 C6 H6 120.5 . . ? C1 C6 H6 120.5 . . ? C12 C7 C8 120.5(12) . . ? C12 C7 Sb1 120.6(9) . . ? C8 C7 Sb1 118.2(10) . . ? C7 C8 C9 118.0(15) . . ? C7 C8 H8 121.0 . . ? C9 C8 H8 121.0 . . ? C10 C9 C8 121.4(14) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 119.6(14) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 119.7(15) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C7 C12 C11 120.8(12) . . ? C7 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 Sb1 117.0(8) . . ? C14 C13 H13A 108.0 . . ? Sb1 C13 H13A 108.0 . . ? C14 C13 H13B 108.0 . . ? Sb1 C13 H13B 108.0 . . ? H13A C13 H13B 107.3 . . ? C15 C14 C13 114.1(10) . . ? C15 C14 H14A 108.7 . . ? C13 C14 H14A 108.7 . . ? C15 C14 H14B 108.7 . . ? C13 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C14 C15 Sb2 116.8(10) . . ? C14 C15 H15A 108.1 . . ? Sb2 C15 H15A 108.1 . . ? C14 C15 H15B 108.1 . . ? Sb2 C15 H15B 108.1 . . ? H15A C15 H15B 107.3 . . ? C17 C16 C21 119.4(14) . . ? C17 C16 Sb2 121.2(10) . . ? C21 C16 Sb2 119.4(11) . . ? C18 C17 C16 120.0(14) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 121.0(15) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 120.6(16) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 119.4(15) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C20 C21 C16 119.5(15) . . ? C20 C21 H21 120.2 . . ? C16 C21 H21 120.2 . . ? C27 C22 C23 119.0(12) . . ? C27 C22 Sb2 123.9(11) . . ? C23 C22 Sb2 116.8(9) . . ? C24 C23 C22 120.7(13) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 121.0(14) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C24 C25 C26 119.1(13) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C25 C26 C27 121.4(15) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C22 C27 C26 118.7(15) . . ? C22 C27 H27 120.7 . . ? C26 C27 H27 120.7 . . ? C33 C28 C29 123.1(13) . . ? C33 C28 Sb3 119.6(10) . . ? C29 C28 Sb3 117.4(10) . . ? C28 C29 C30 117.3(13) . . ? C28 C29 H29 121.3 . . ? C30 C29 H29 121.3 . . ? C31 C30 C29 120.1(13) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 122.3(15) . . ? C30 C31 H31 118.9 . . ? C32 C31 H31 118.9 . . ? C31 C32 C33 119.1(14) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C28 C33 C32 118.1(13) . . ? C28 C33 H33 121.0 . . ? C32 C33 H33 121.0 . . ? C35 C34 Sb3 115.4(9) . . ? C35 C34 H34A 108.4 . . ? Sb3 C34 H34A 108.4 . . ? C35 C34 H34B 108.4 . . ? Sb3 C34 H34B 108.4 . . ? H34A C34 H34B 107.5 . . ? C36 C35 C34 118.5(12) . . ? C36 C35 H35A 107.7 . . ? C34 C35 H35A 107.7 . . ? C36 C35 H35B 107.7 . . ? C34 C35 H35B 107.7 . . ? H35A C35 H35B 107.1 . . ? C35 C36 Sb4 116.7(10) . . ? C35 C36 H36A 108.1 . . ? Sb4 C36 H36A 108.1 . . ? C35 C36 H36B 108.1 . . ? Sb4 C36 H36B 108.1 . . ? H36A C36 H36B 107.3 . . ? C42 C37 C38 121.6(12) . . ? C42 C37 Sb4 118.1(10) . . ? C38 C37 Sb4 120.3(11) . . ? C39 C38 C37 119.5(14) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C40 C39 C38 120.2(14) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 119.6(14) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C42 C41 C40 121.3(15) . . ? C42 C41 H41 119.4 . . ? C40 C41 H41 119.4 . . ? C37 C42 C41 117.9(13) . . ? C37 C42 H42 121.1 . . ? C41 C42 H42 121.1 . . ? Cl7 C43 Cl8 111.9(10) . . ? Cl7 C43 Cl6 109.7(14) . . ? Cl8 C43 Cl6 109.0(12) . . ? Cl7 C43 H43 108.7 . . ? Cl8 C43 H43 108.7 . . ? Cl6 C43 H43 108.7 . . ? Sb3 Cl5 Sb4 76.13(8) . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 1.625 _refine_diff_density_min -1.606 _refine_diff_density_rms 0.319 #===END OF CIF ============================================================== # # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # #===END OF FILE =============================================================