Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'David H. Farrar' 'Elena V. Grachova' 'Alan Lough' 'Charles Patirana' 'Anthony J. Poe' 'Sergey P. Tunik' _publ_contact_author_name 'David H. Farrar' _publ_contact_author_address ; ? ; _publ_contact_author_email 'dfarrar@chem.utoronto.ca' data_s9582 _database_code_CSD 163529 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '1 Rh6(CO)15(P(OPh)3)' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H15 O18 P Rh6' _chemical_formula_weight 1347.88 _chemical_melting_point ? _chemical_compound_source ? 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' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.336(2) _cell_length_b 10.3350(12) _cell_length_c 20.122(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.178(9) _cell_angle_gamma 90.00 _cell_volume 3764.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 4.84 _cell_measurement_theta_max 15.04 _exptl_crystal_description 'flat needle' _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.378 _exptl_crystal_density_method ? _exptl_crystal_F_000 2568 _exptl_absorpt_coefficient_mu 2.691 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.4840 _exptl_absorpt_correction_T_max 0.8198 _exptl_absorpt_process_details 'SHELXTL' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'Less than 4' _diffrn_reflns_number 11285 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 30.00 _reflns_number_total 10976 _reflns_number_gt 8886 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w==1/[\s^2^(Fo^2^)+(0.0271P)^2^] 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 10976 _refine_ls_number_parameters 524 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_all 0.0660 _refine_ls_wR_factor_ref 0.0634 _refine_ls_goodness_of_fit_all 0.973 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 0.973 _refine_ls_restrained_S_obs 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh10 Rh 0.229406(12) 0.17308(2) 0.011624(10) 0.01580(5) Uani 1 d . . Rh20 Rh 0.356054(13) 0.32383(2) 0.013957(11) 0.01824(5) Uani 1 d . . Rh21 Rh 0.369091(12) 0.06806(2) 0.043607(11) 0.01759(5) Uani 1 d . . Rh31 Rh 0.282722(13) 0.10000(2) 0.142820(11) 0.01789(5) Uani 1 d . . Rh30 Rh 0.268684(13) 0.35571(2) 0.111288(11) 0.01939(5) Uani 1 d . . Rh40 Rh 0.406265(13) 0.24807(2) 0.144337(11) 0.01955(5) Uani 1 d . . C10 C 0.2403(2) 0.3755(3) -0.00265(15) 0.0217(6) Uani 1 d . . O10 O 0.20792(13) 0.4578(2) -0.03325(11) 0.0268(5) Uani 1 d . . C11 C 0.2629(2) -0.0177(3) 0.04972(15) 0.0206(6) Uani 1 d . . O11 O 0.24044(13) -0.1220(2) 0.04180(11) 0.0262(5) Uani 1 d . . C20 C 0.4550(2) 0.2157(3) 0.05488(15) 0.0241(6) Uani 1 d . . O20 O 0.51545(13) 0.2168(2) 0.04456(11) 0.0289(5) Uani 1 d . . C30 C 0.3173(2) 0.2683(3) 0.20585(15) 0.0249(6) Uani 1 d . . O30 O 0.31592(14) 0.2916(3) 0.26139(11) 0.0314(5) Uani 1 d . . C40 C 0.1315(2) 0.1546(3) 0.02658(14) 0.0239(6) Uani 1 d . . O40 O 0.07538(14) 0.1370(3) 0.04092(12) 0.0368(6) Uani 1 d . . C50 C 0.3726(2) 0.3197(3) -0.07737(15) 0.0246(6) Uani 1 d . . O50 O 0.3870(2) 0.3256(3) -0.12918(12) 0.0389(6) Uani 1 d . . C51 C 0.3804(2) 0.0225(3) -0.0452(2) 0.0235(6) Uani 1 d . . O51 O 0.38929(15) 0.0010(3) -0.09799(12) 0.0343(6) Uani 1 d . . C60 C 0.3970(2) 0.4920(4) 0.0261(2) 0.0355(8) Uani 1 d . . O60 O 0.4222(2) 0.5894(3) 0.0340(2) 0.0734(13) Uani 1 d . . C61 C 0.4268(2) -0.0736(3) 0.0849(2) 0.0250(6) Uani 1 d . . O61 O 0.4605(2) -0.1555(3) 0.10970(13) 0.0392(6) Uani 1 d . . C70 C 0.1698(2) 0.3769(3) 0.1236(2) 0.0277(7) Uani 1 d . . O70 O 0.1101(2) 0.3904(3) 0.12846(15) 0.0454(7) Uani 1 d . . C71 C 0.1917(2) 0.0848(3) 0.17628(15) 0.0244(6) Uani 1 d . . O71 O 0.13908(15) 0.0811(3) 0.19848(13) 0.0372(6) Uani 1 d . . C80 C 0.2928(2) 0.5324(4) 0.1307(2) 0.0337(8) Uani 1 d . . O80 O 0.3060(2) 0.6371(3) 0.1424(2) 0.0585(9) Uani 1 d . . C81 C 0.3274(2) -0.0390(3) 0.19609(15) 0.0250(6) Uani 1 d . . O81 O 0.3548(2) -0.1222(3) 0.22613(13) 0.0406(6) Uani 1 d . . C90 C 0.4575(2) 0.4023(4) 0.1744(2) 0.0358(8) Uani 1 d . . O90 O 0.4875(2) 0.4927(3) 0.1918(2) 0.0671(10) Uani 1 d . . C91 C 0.4716(2) 0.1402(3) 0.2028(2) 0.0295(7) Uani 1 d . . O91 O 0.5115(2) 0.0768(3) 0.23559(15) 0.0512(8) Uani 1 d . . P P 0.19756(4) 0.11594(8) -0.09709(4) 0.01805(14) Uani 1 d . . O1 O 0.11506(13) 0.1341(3) -0.13464(11) 0.0301(5) Uani 1 d . . C111 C 0.0544(2) 0.1939(3) -0.11484(14) 0.0214(6) Uani 1 d . . C112 C 0.0563(2) 0.3225(3) -0.0981(2) 0.0292(7) Uani 1 d . . H11A H 0.0994(2) 0.3727(3) -0.0995(2) 0.035 Uiso 1 calc R . C113 C -0.0056(2) 0.3770(4) -0.0793(2) 0.0380(8) Uani 1 d . . H11B H -0.0053(2) 0.4658(4) -0.0670(2) 0.046 Uiso 1 calc R . C114 C -0.0685(2) 0.3031(4) -0.0782(2) 0.0402(9) Uani 1 d . . H11C H -0.1110(2) 0.3410(4) -0.0646(2) 0.048 Uiso 1 calc R . C115 C -0.0694(2) 0.1761(4) -0.0967(2) 0.0367(8) Uani 1 d . . H11D H -0.1130(2) 0.1264(4) -0.0968(2) 0.044 Uiso 1 calc R . C116 C -0.0077(2) 0.1195(3) -0.1151(2) 0.0298(7) Uani 1 d . . H11E H -0.0081(2) 0.0309(3) -0.1277(2) 0.036 Uiso 1 calc R . O2 O 0.20987(12) -0.0313(2) -0.11477(11) 0.0227(4) Uani 1 d . . C121 C 0.1529(2) -0.1206(3) -0.1351(2) 0.0240(6) Uani 1 d . . C122 C 0.1293(2) -0.1405(4) -0.2022(2) 0.0317(7) Uani 1 d . . H12A H 0.1505(2) -0.0939(4) -0.2351(2) 0.038 Uiso 1 calc R . C123 C 0.0740(2) -0.2299(4) -0.2211(2) 0.0377(9) Uani 1 d . . H12B H 0.0567(2) -0.2446(4) -0.2676(2) 0.045 Uiso 1 calc R . C124 C 0.0437(2) -0.2973(4) -0.1742(2) 0.0352(8) Uani 1 d . . H12C H 0.0067(2) -0.3603(4) -0.1880(2) 0.042 Uiso 1 calc R . C125 C 0.0669(3) -0.2741(5) -0.1067(2) 0.0466(11) Uani 1 d . . H12D H 0.0449(3) -0.3193(5) -0.0739(2) 0.056 Uiso 1 calc R . C126 C 0.1221(2) -0.1849(4) -0.0871(2) 0.0397(9) Uani 1 d . . H12E H 0.1386(2) -0.1684(4) -0.0407(2) 0.048 Uiso 1 calc R . O3 O 0.24400(12) 0.1891(2) -0.14559(10) 0.0235(4) Uani 1 d . . C131 C 0.2311(2) 0.1681(3) -0.21592(14) 0.0226(6) Uani 1 d . . C132 C 0.1769(2) 0.2355(4) -0.2551(2) 0.0337(8) Uani 1 d . . H13A H 0.1470(2) 0.2949(4) -0.2353(2) 0.040 Uiso 1 calc R . C133 C 0.1654(2) 0.2166(4) -0.3245(2) 0.0413(9) Uani 1 d . . H13B H 0.1268(2) 0.2613(4) -0.3524(2) 0.050 Uiso 1 calc R . C134 C 0.2103(2) 0.1328(4) -0.3522(2) 0.0400(9) Uani 1 d . . H13C H 0.2035(2) 0.1210(4) -0.3996(2) 0.048 Uiso 1 calc R . C135 C 0.2647(2) 0.0664(4) -0.3120(2) 0.0421(9) Uani 1 d . . H13D H 0.2953(2) 0.0079(4) -0.3315(2) 0.051 Uiso 1 calc R . C136 C 0.2755(2) 0.0839(4) -0.2429(2) 0.0330(8) Uani 1 d . . H13E H 0.3132(2) 0.0379(4) -0.2147(2) 0.040 Uiso 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 Rh10 0.01486(10) 0.01691(10) 0.01565(9) 0.00041(8) 0.00250(7) -0.00099(8) Rh20 0.01926(11) 0.01783(10) 0.01799(10) 0.00176(8) 0.00405(8) -0.00414(9) Rh21 0.01598(10) 0.01765(10) 0.01906(10) -0.00028(8) 0.00258(8) 0.00016(8) Rh31 0.01803(11) 0.01871(10) 0.01700(9) 0.00271(8) 0.00300(8) -0.00239(9) Rh30 0.02231(11) 0.01697(10) 0.01930(10) -0.00155(8) 0.00453(8) -0.00005(9) Rh40 0.01841(11) 0.02082(11) 0.01856(10) -0.00026(8) 0.00036(8) -0.00463(9) C10 0.0222(15) 0.0202(14) 0.0232(13) 0.0019(11) 0.0045(11) -0.0028(12) O10 0.0284(12) 0.0204(11) 0.0302(11) 0.0073(9) 0.0007(9) 0.0011(9) C11 0.0188(14) 0.0193(14) 0.0236(13) 0.0020(11) 0.0029(11) -0.0016(11) O11 0.0270(12) 0.0189(10) 0.0307(11) 0.0005(9) -0.0013(9) -0.0054(9) C20 0.0211(14) 0.027(2) 0.0236(13) 0.0007(12) 0.0016(11) -0.0061(12) O20 0.0189(11) 0.0365(13) 0.0319(11) 0.0025(10) 0.0058(9) -0.0024(10) C30 0.026(2) 0.027(2) 0.0213(13) -0.0023(12) 0.0031(11) -0.0025(13) O30 0.0369(14) 0.0376(14) 0.0199(10) -0.0033(10) 0.0054(9) -0.0024(11) C40 0.0228(15) 0.030(2) 0.0188(12) 0.0027(12) 0.0035(11) -0.0009(13) O40 0.0220(12) 0.058(2) 0.0310(12) 0.0076(12) 0.0054(10) -0.0053(12) C50 0.0237(15) 0.027(2) 0.0229(14) 0.0012(12) 0.0039(11) -0.0033(13) O50 0.0396(15) 0.054(2) 0.0261(11) 0.0010(12) 0.0135(11) -0.0057(13) C51 0.0206(14) 0.0242(15) 0.0253(14) -0.0004(12) 0.0026(11) 0.0010(12) O51 0.0385(14) 0.0404(15) 0.0243(11) -0.0043(10) 0.0059(10) 0.0081(12) C60 0.047(2) 0.031(2) 0.030(2) 0.0008(14) 0.011(2) -0.015(2) O60 0.126(4) 0.044(2) 0.055(2) -0.004(2) 0.027(2) -0.052(2) C61 0.0226(15) 0.026(2) 0.0271(14) -0.0010(12) 0.0057(12) 0.0003(13) O61 0.044(2) 0.0328(14) 0.0401(14) 0.0047(11) 0.0033(12) 0.0144(12) C70 0.032(2) 0.027(2) 0.0248(14) 0.0011(12) 0.0084(13) 0.0056(14) O70 0.0308(15) 0.055(2) 0.054(2) 0.0080(14) 0.0162(13) 0.0173(14) C71 0.025(2) 0.0248(15) 0.0230(13) 0.0029(12) 0.0025(11) -0.0040(13) O71 0.0325(14) 0.044(2) 0.0385(13) 0.0022(12) 0.0166(11) -0.0026(12) C80 0.045(2) 0.027(2) 0.028(2) -0.0024(13) 0.0041(15) -0.005(2) O80 0.083(3) 0.0260(14) 0.065(2) -0.0083(14) 0.007(2) -0.007(2) C81 0.025(2) 0.027(2) 0.0221(13) 0.0033(12) 0.0013(12) -0.0029(13) O81 0.048(2) 0.0350(14) 0.0373(14) 0.0151(11) 0.0012(12) 0.0071(13) C90 0.034(2) 0.036(2) 0.036(2) -0.002(2) 0.0004(15) -0.010(2) O90 0.070(2) 0.043(2) 0.082(2) -0.015(2) -0.007(2) -0.030(2) C91 0.023(2) 0.032(2) 0.033(2) 0.0034(14) -0.0011(13) -0.0080(14) O91 0.044(2) 0.051(2) 0.050(2) 0.0190(14) -0.0170(14) -0.0005(15) P 0.0161(3) 0.0196(3) 0.0182(3) -0.0008(3) 0.0020(3) -0.0009(3) O1 0.0193(11) 0.0439(14) 0.0254(11) -0.0090(10) -0.0017(9) 0.0076(10) C111 0.0163(13) 0.0263(15) 0.0209(13) -0.0001(11) 0.0012(10) 0.0003(12) C112 0.026(2) 0.025(2) 0.035(2) 0.0049(13) 0.0004(13) -0.0037(13) C113 0.039(2) 0.029(2) 0.044(2) -0.002(2) 0.000(2) 0.011(2) C114 0.025(2) 0.054(2) 0.041(2) 0.001(2) 0.0054(15) 0.012(2) C115 0.024(2) 0.046(2) 0.041(2) 0.000(2) 0.0075(14) -0.008(2) C116 0.026(2) 0.026(2) 0.035(2) -0.0003(14) 0.0017(13) -0.0020(14) O2 0.0202(10) 0.0206(10) 0.0276(10) -0.0042(8) 0.0044(8) -0.0024(9) C121 0.024(2) 0.0218(14) 0.0257(14) -0.0046(12) 0.0036(12) -0.0041(12) C122 0.038(2) 0.032(2) 0.0256(15) -0.0008(13) 0.0057(14) -0.012(2) C123 0.045(2) 0.042(2) 0.026(2) -0.0084(15) 0.0042(15) -0.014(2) C124 0.035(2) 0.036(2) 0.035(2) -0.012(2) 0.0075(15) -0.017(2) C125 0.053(3) 0.057(3) 0.032(2) -0.001(2) 0.013(2) -0.031(2) C126 0.045(2) 0.051(2) 0.0221(15) -0.004(2) 0.0045(15) -0.022(2) O3 0.0257(11) 0.0274(11) 0.0163(9) -0.0006(8) 0.0001(8) -0.0092(9) C131 0.026(2) 0.0245(15) 0.0169(12) 0.0004(11) 0.0029(11) -0.0043(12) C132 0.042(2) 0.031(2) 0.027(2) 0.0029(13) 0.0042(14) 0.007(2) C133 0.052(2) 0.040(2) 0.029(2) 0.006(2) -0.005(2) 0.005(2) C134 0.056(3) 0.045(2) 0.0173(14) -0.0016(14) 0.0003(15) -0.011(2) C135 0.050(2) 0.050(2) 0.028(2) -0.007(2) 0.011(2) 0.004(2) C136 0.034(2) 0.043(2) 0.0225(14) 0.0038(14) 0.0076(13) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh10 C40 1.876(3) . ? Rh10 C10 2.125(3) . ? Rh10 C11 2.169(3) . ? Rh10 P 2.2511(8) . ? Rh10 Rh21 2.7616(4) . ? Rh10 Rh30 2.7644(4) . ? Rh10 Rh31 2.7699(4) . ? Rh10 Rh20 2.7905(4) . ? Rh20 C60 1.893(4) . ? Rh20 C50 1.910(3) . ? Rh20 C10 2.163(3) . ? Rh20 C20 2.178(3) . ? Rh20 Rh21 2.7120(4) . ? Rh20 Rh30 2.7407(4) . ? Rh20 Rh40 2.7519(4) . ? Rh21 C51 1.892(3) . ? Rh21 C61 1.916(3) . ? Rh21 C11 2.160(3) . ? Rh21 C20 2.179(3) . ? Rh21 Rh40 2.7556(4) . ? Rh21 Rh31 2.7588(4) . ? Rh31 C81 1.898(3) . ? Rh31 C71 1.904(3) . ? Rh31 C30 2.186(3) . ? Rh31 C11 2.215(3) . ? Rh31 Rh30 2.7204(4) . ? Rh31 Rh40 2.7299(4) . ? Rh30 C70 1.881(4) . ? Rh30 C80 1.904(4) . ? Rh30 C30 2.166(3) . ? Rh30 C10 2.278(3) . ? Rh30 Rh40 2.7401(4) . ? Rh40 C90 1.900(4) . ? Rh40 C91 1.900(3) . ? Rh40 C20 2.160(3) . ? Rh40 C30 2.209(3) . ? C10 O10 1.157(4) . ? C11 O11 1.156(4) . ? C20 O20 1.160(4) . ? C30 O30 1.148(4) . ? C40 O40 1.128(4) . ? C50 O50 1.117(4) . ? C51 O51 1.122(4) . ? C60 O60 1.108(4) . ? C61 O61 1.118(4) . ? C70 O70 1.124(4) . ? C71 O71 1.126(4) . ? C80 O80 1.126(5) . ? C81 O81 1.122(4) . ? C90 O90 1.112(5) . ? C91 O91 1.117(4) . ? P O3 1.586(2) . ? P O2 1.587(2) . ? P O1 1.590(2) . ? O1 C111 1.385(4) . ? C111 C112 1.370(5) . ? C111 C116 1.375(4) . ? C112 C113 1.373(5) . ? C113 C114 1.387(6) . ? C114 C115 1.363(6) . ? C115 C116 1.376(5) . ? O2 C121 1.405(4) . ? C121 C126 1.366(5) . ? C121 C122 1.367(4) . ? C122 C123 1.380(5) . ? C123 C124 1.360(5) . ? C124 C125 1.378(5) . ? C125 C126 1.380(5) . ? O3 C131 1.414(3) . ? C131 C132 1.359(5) . ? C131 C136 1.361(5) . ? C132 C133 1.393(5) . ? C133 C134 1.373(6) . ? C134 C135 1.366(6) . ? C135 C136 1.386(5) . ? 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 C40 Rh10 C10 103.54(13) . . ? C40 Rh10 C11 94.32(13) . . ? C10 Rh10 C11 156.26(12) . . ? C40 Rh10 P 91.30(9) . . ? C10 Rh10 P 98.18(8) . . ? C11 Rh10 P 96.89(8) . . ? C40 Rh10 Rh21 142.94(10) . . ? C10 Rh10 Rh21 108.37(8) . . ? C11 Rh10 Rh21 50.22(8) . . ? P Rh10 Rh21 102.16(2) . . ? C40 Rh10 Rh30 95.63(10) . . ? C10 Rh10 Rh30 53.62(8) . . ? C11 Rh10 Rh30 109.75(8) . . ? P Rh10 Rh30 151.80(2) . . ? Rh21 Rh10 Rh30 88.549(12) . . ? C40 Rh10 Rh31 91.18(9) . . ? C10 Rh10 Rh31 111.77(8) . . ? C11 Rh10 Rh31 51.55(8) . . ? P Rh10 Rh31 148.43(2) . . ? Rh21 Rh10 Rh31 59.834(11) . . ? Rh30 Rh10 Rh31 58.886(10) . . ? C40 Rh10 Rh20 150.31(10) . . ? C10 Rh10 Rh20 49.99(8) . . ? C11 Rh10 Rh20 108.27(8) . . ? P Rh10 Rh20 104.42(2) . . ? Rh21 Rh10 Rh20 58.477(11) . . ? Rh30 Rh10 Rh20 59.124(10) . . ? Rh31 Rh10 Rh20 88.279(12) . . ? C60 Rh20 C50 91.41(14) . . ? C60 Rh20 C10 98.8(2) . . ? C50 Rh20 C10 99.18(13) . . ? C60 Rh20 C20 97.6(2) . . ? C50 Rh20 C20 95.83(13) . . ? C10 Rh20 C20 157.40(11) . . ? C60 Rh20 Rh21 147.90(13) . . ? C50 Rh20 Rh21 99.65(10) . . ? C10 Rh20 Rh21 108.93(8) . . ? C20 Rh20 Rh21 51.52(8) . . ? C60 Rh20 Rh30 93.55(12) . . ? C50 Rh20 Rh30 152.98(10) . . ? C10 Rh20 Rh30 53.80(8) . . ? C20 Rh20 Rh30 109.77(8) . . ? Rh21 Rh20 Rh30 90.057(10) . . ? C60 Rh20 Rh40 94.16(11) . . ? C50 Rh20 Rh40 146.14(10) . . ? C10 Rh20 Rh40 112.85(8) . . ? C20 Rh20 Rh40 50.33(8) . . ? Rh21 Rh20 Rh40 60.568(8) . . ? Rh30 Rh20 Rh40 59.850(10) . . ? C60 Rh20 Rh10 145.70(13) . . ? C50 Rh20 Rh10 103.34(10) . . ? C10 Rh20 Rh10 48.81(8) . . ? C20 Rh20 Rh10 111.15(8) . . ? Rh21 Rh20 Rh10 60.228(10) . . ? Rh30 Rh20 Rh10 59.963(10) . . ? Rh40 Rh20 Rh10 90.467(12) . . ? C51 Rh21 C61 94.81(13) . . ? C51 Rh21 C11 100.80(12) . . ? C61 Rh21 C11 95.84(13) . . ? C51 Rh21 C20 94.94(12) . . ? C61 Rh21 C20 98.63(13) . . ? C11 Rh21 C20 157.60(12) . . ? C51 Rh21 Rh20 93.08(10) . . ? C61 Rh21 Rh20 149.68(10) . . ? C11 Rh21 Rh20 111.33(8) . . ? C20 Rh21 Rh20 51.48(9) . . ? C51 Rh21 Rh40 144.25(10) . . ? C61 Rh21 Rh40 98.16(10) . . ? C11 Rh21 Rh40 110.77(8) . . ? C20 Rh21 Rh40 50.26(8) . . ? Rh20 Rh21 Rh40 60.433(10) . . ? C51 Rh21 Rh31 151.13(10) . . ? C61 Rh21 Rh31 96.79(9) . . ? C11 Rh21 Rh31 51.79(8) . . ? C20 Rh21 Rh31 109.26(8) . . ? Rh20 Rh21 Rh31 90.112(10) . . ? Rh40 Rh21 Rh31 59.345(9) . . ? C51 Rh21 Rh10 96.60(9) . . ? C61 Rh21 Rh10 145.94(10) . . ? C11 Rh21 Rh10 50.49(8) . . ? C20 Rh21 Rh10 112.17(9) . . ? Rh20 Rh21 Rh10 61.295(9) . . ? Rh40 Rh21 Rh10 91.001(12) . . ? Rh31 Rh21 Rh10 60.233(10) . . ? C81 Rh31 C71 93.51(14) . . ? C81 Rh31 C30 102.43(13) . . ? C71 Rh31 C30 92.89(13) . . ? C81 Rh31 C11 93.43(12) . . ? C71 Rh31 C11 102.66(12) . . ? C30 Rh31 C11 157.07(11) . . ? C81 Rh31 Rh30 152.03(10) . . ? C71 Rh31 Rh30 96.15(10) . . ? C30 Rh31 Rh30 50.98(8) . . ? C11 Rh31 Rh30 109.85(8) . . ? C81 Rh31 Rh40 97.80(10) . . ? C71 Rh31 Rh40 144.62(10) . . ? C30 Rh31 Rh40 51.97(9) . . ? C11 Rh31 Rh40 109.94(8) . . ? Rh30 Rh31 Rh40 60.364(10) . . ? C81 Rh31 Rh21 94.16(10) . . ? C71 Rh31 Rh21 152.02(9) . . ? C30 Rh31 Rh21 111.59(8) . . ? C11 Rh31 Rh21 50.03(8) . . ? Rh30 Rh31 Rh21 89.504(10) . . ? Rh40 Rh31 Rh21 60.270(10) . . ? C81 Rh31 Rh10 143.08(10) . . ? C71 Rh31 Rh10 99.41(9) . . ? C30 Rh31 Rh10 111.20(8) . . ? C11 Rh31 Rh10 50.07(8) . . ? Rh30 Rh31 Rh10 60.457(8) . . ? Rh40 Rh31 Rh10 91.368(12) . . ? Rh21 Rh31 Rh10 59.933(10) . . ? C70 Rh30 C80 93.3(2) . . ? C70 Rh30 C30 101.74(13) . . ? C80 Rh30 C30 99.83(14) . . ? C70 Rh30 C10 92.94(12) . . ? C80 Rh30 C10 97.37(13) . . ? C30 Rh30 C10 156.59(12) . . ? C70 Rh30 Rh31 98.02(11) . . ? C80 Rh30 Rh31 150.88(11) . . ? C30 Rh30 Rh31 51.64(9) . . ? C10 Rh30 Rh31 108.65(8) . . ? C70 Rh30 Rh40 152.19(10) . . ? C80 Rh30 Rh40 99.51(12) . . ? C30 Rh30 Rh40 51.91(9) . . ? C10 Rh30 Rh40 109.56(8) . . ? Rh31 Rh30 Rh40 59.989(9) . . ? C70 Rh30 Rh20 142.51(10) . . ? C80 Rh30 Rh20 96.82(12) . . ? C30 Rh30 Rh20 111.82(9) . . ? C10 Rh30 Rh20 50.03(8) . . ? Rh31 Rh30 Rh20 90.319(10) . . ? Rh40 Rh30 Rh20 60.278(11) . . ? C70 Rh30 Rh10 91.71(10) . . ? C80 Rh30 Rh10 145.92(10) . . ? C30 Rh30 Rh10 112.06(9) . . ? C10 Rh30 Rh10 48.68(8) . . ? Rh31 Rh30 Rh10 60.658(10) . . ? Rh40 Rh30 Rh10 91.268(12) . . ? Rh20 Rh30 Rh10 60.912(9) . . ? C90 Rh40 C91 93.7(2) . . ? C90 Rh40 C20 98.40(15) . . ? C91 Rh40 C20 96.97(14) . . ? C90 Rh40 C30 96.54(15) . . ? C91 Rh40 C30 99.04(14) . . ? C20 Rh40 C30 157.28(11) . . ? C90 Rh40 Rh31 147.28(12) . . ? C91 Rh40 Rh31 96.77(10) . . ? C20 Rh40 Rh31 110.91(8) . . ? C30 Rh40 Rh31 51.23(8) . . ? C90 Rh40 Rh30 97.25(12) . . ? C91 Rh40 Rh30 148.56(11) . . ? C20 Rh40 Rh30 110.37(8) . . ? C30 Rh40 Rh30 50.53(8) . . ? Rh31 Rh40 Rh30 59.648(11) . . ? C90 Rh40 Rh20 97.96(11) . . ? C91 Rh40 Rh20 147.04(11) . . ? C20 Rh40 Rh20 50.91(9) . . ? C30 Rh40 Rh20 110.05(8) . . ? Rh31 Rh40 Rh20 89.885(12) . . ? Rh30 Rh40 Rh20 59.872(11) . . ? C90 Rh40 Rh21 148.50(12) . . ? C91 Rh40 Rh21 96.70(11) . . ? C20 Rh40 Rh21 50.88(8) . . ? C30 Rh40 Rh21 110.97(8) . . ? Rh31 Rh40 Rh21 60.385(10) . . ? Rh30 Rh40 Rh21 89.165(12) . . ? Rh20 Rh40 Rh21 58.999(10) . . ? O10 C10 Rh10 138.2(2) . . ? O10 C10 Rh20 132.1(2) . . ? Rh10 C10 Rh20 81.19(11) . . ? O10 C10 Rh30 128.1(2) . . ? Rh10 C10 Rh30 77.70(10) . . ? Rh20 C10 Rh30 76.17(10) . . ? O11 C11 Rh21 132.8(3) . . ? O11 C11 Rh10 136.4(2) . . ? Rh21 C11 Rh10 79.28(10) . . ? O11 C11 Rh31 129.5(2) . . ? Rh21 C11 Rh31 78.18(10) . . ? Rh10 C11 Rh31 78.38(10) . . ? O20 C20 Rh40 133.0(2) . . ? O20 C20 Rh20 133.6(3) . . ? Rh40 C20 Rh20 78.76(11) . . ? O20 C20 Rh21 133.2(3) . . ? Rh40 C20 Rh21 78.86(10) . . ? Rh20 C20 Rh21 76.99(10) . . ? O30 C30 Rh30 134.2(3) . . ? O30 C30 Rh31 133.0(3) . . ? Rh30 C30 Rh31 77.38(10) . . ? O30 C30 Rh40 134.4(3) . . ? Rh30 C30 Rh40 77.56(10) . . ? Rh31 C30 Rh40 76.81(10) . . ? O40 C40 Rh10 173.4(3) . . ? O50 C50 Rh20 173.7(3) . . ? O51 C51 Rh21 176.4(3) . . ? O60 C60 Rh20 178.6(4) . . ? O61 C61 Rh21 179.2(3) . . ? O70 C70 Rh30 177.4(3) . . ? O71 C71 Rh31 176.2(3) . . ? O80 C80 Rh30 179.0(4) . . ? O81 C81 Rh31 178.0(3) . . ? O90 C90 Rh40 179.7(4) . . ? O91 C91 Rh40 177.7(3) . . ? O3 P O2 102.11(12) . . ? O3 P O1 102.40(13) . . ? O2 P O1 99.50(13) . . ? O3 P Rh10 113.04(8) . . ? O2 P Rh10 116.44(9) . . ? O1 P Rh10 120.69(9) . . ? C111 O1 P 131.5(2) . . ? C112 C111 C116 122.1(3) . . ? C112 C111 O1 121.0(3) . . ? C116 C111 O1 116.9(3) . . ? C111 C112 C113 118.5(3) . . ? C112 C113 C114 120.3(4) . . ? C115 C114 C113 120.0(4) . . ? C114 C115 C116 120.6(4) . . ? C111 C116 C115 118.5(3) . . ? C121 O2 P 124.7(2) . . ? C126 C121 C122 121.6(3) . . ? C126 C121 O2 119.1(3) . . ? C122 C121 O2 119.3(3) . . ? C121 C122 C123 118.4(3) . . ? C124 C123 C122 121.0(3) . . ? C123 C124 C125 120.0(3) . . ? C124 C125 C126 119.6(3) . . ? C121 C126 C125 119.4(3) . . ? C131 O3 P 121.5(2) . . ? C132 C131 C136 121.7(3) . . ? C132 C131 O3 119.5(3) . . ? C136 C131 O3 118.8(3) . . ? C131 C132 C133 119.3(3) . . ? C134 C133 C132 119.4(4) . . ? C135 C134 C133 120.4(3) . . ? C134 C135 C136 120.2(4) . . ? C131 C136 C135 119.1(3) . . ? _refine_diff_density_max 0.604 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.123 #======END data_k9863 _database_code_CSD 163530 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '2 Rh6(CO)15(P(4-F3CC6H4)3)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H13 Cl3 F9 O15 P Rh6' _chemical_formula_weight 1623.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 34.1310(10) _cell_length_b 9.8589(2) _cell_length_c 27.8430(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.2680(10) _cell_angle_gamma 90.00 _cell_volume 9368.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 8287 _cell_measurement_theta_min 4.13 _cell_measurement_theta_max 25.02 _exptl_crystal_description block _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6176 _exptl_absorpt_coefficient_mu 2.371 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Denzo-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _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 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 19849 _diffrn_reflns_av_R_equivalents 0.074 _diffrn_reflns_av_sigmaI/netI 0.0687 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8287 _reflns_number_gt 5885 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'Bruker SHELXTL V5.1' _computing_structure_refinement 'Bruker SHELXTL V5.1' _computing_molecular_graphics 'Bruker SHELXTL V5.1' _computing_publication_material 'Bruker SHELXTL V5.1' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0129P)^2^+104.2786P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000028(13) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8030 _refine_ls_number_parameters 641 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.004 _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 Rh10 Rh 0.381215(15) 0.61479(5) 0.186850(18) 0.02074(14) Uani 1 1 d . . . Rh20 Rh 0.397852(16) 0.33737(5) 0.186404(19) 0.02370(15) Uani 1 1 d . . . Rh21 Rh 0.321483(16) 0.41871(6) 0.190590(19) 0.02483(15) Uani 1 1 d . . . Rh30 Rh 0.415504(15) 0.49386(5) 0.265900(18) 0.02221(15) Uani 1 1 d . . . Rh31 Rh 0.338485(16) 0.57385(6) 0.270538(19) 0.02463(15) Uani 1 1 d . . . Rh40 Rh 0.356973(16) 0.30214(5) 0.270860(19) 0.02465(15) Uani 1 1 d . . . C10 C 0.4365(2) 0.5129(6) 0.1897(2) 0.0242(16) Uani 1 1 d . . . O10 O 0.46812(14) 0.5350(5) 0.17574(17) 0.0298(11) Uani 1 1 d . . . C11 C 0.3196(2) 0.6421(8) 0.1963(2) 0.0296(17) Uani 1 1 d . . . O11 O 0.29662(14) 0.7241(5) 0.18609(17) 0.0318(12) Uani 1 1 d . . . C20 C 0.3446(2) 0.2126(8) 0.2026(3) 0.0342(18) Uani 1 1 d . . . O20 O 0.33449(15) 0.1074(5) 0.18981(18) 0.0356(13) Uani 1 1 d . . . C30 C 0.3728(2) 0.4579(7) 0.3228(3) 0.0291(17) Uani 1 1 d . . . O30 O 0.37473(15) 0.4604(5) 0.36439(18) 0.0392(13) Uani 1 1 d . . . C40 C 0.39229(19) 0.7915(7) 0.2069(2) 0.0228(15) Uani 1 1 d . . . O40 O 0.39672(16) 0.8987(5) 0.22141(19) 0.0418(14) Uani 1 1 d . . . C50 C 0.3958(2) 0.2902(7) 0.1196(3) 0.0316(17) Uani 1 1 d . . . O50 O 0.39245(17) 0.2498(6) 0.08207(19) 0.0462(15) Uani 1 1 d . . . C51 C 0.3114(2) 0.3886(7) 0.1251(3) 0.0330(18) Uani 1 1 d . . . O51 O 0.30468(19) 0.3629(6) 0.0859(2) 0.0520(16) Uani 1 1 d . . . C60 C 0.4362(2) 0.2006(7) 0.2007(3) 0.0297(17) Uani 1 1 d . . . O60 O 0.45755(15) 0.1171(5) 0.21039(19) 0.0395(13) Uani 1 1 d . . . C61 C 0.2680(2) 0.3927(8) 0.2076(3) 0.0356(19) Uani 1 1 d . . . O61 O 0.23595(18) 0.3778(7) 0.2171(2) 0.0598(17) Uani 1 1 d . . . C70 C 0.4407(2) 0.6538(8) 0.2896(3) 0.0337(18) Uani 1 1 d . . . O70 O 0.45595(19) 0.7470(6) 0.3025(2) 0.0563(17) Uani 1 1 d . . . C71 C 0.3469(2) 0.7459(8) 0.2999(3) 0.0334(18) Uani 1 1 d . . . O71 O 0.35204(18) 0.8441(6) 0.3197(2) 0.0560(17) Uani 1 1 d . . . C80 C 0.4558(2) 0.3766(7) 0.2903(2) 0.0272(16) Uani 1 1 d . . . O80 O 0.47804(16) 0.3052(5) 0.3049(2) 0.0443(14) Uani 1 1 d . . . C81 C 0.2878(2) 0.5591(8) 0.2976(3) 0.0346(18) Uani 1 1 d . . . O81 O 0.25751(18) 0.5518(6) 0.3139(2) 0.0562(16) Uani 1 1 d . . . C90 C 0.3886(2) 0.1614(7) 0.2976(3) 0.0283(17) Uani 1 1 d . . . O90 O 0.40773(16) 0.0799(6) 0.3136(2) 0.0456(15) Uani 1 1 d . . . C91 C 0.3116(3) 0.2372(8) 0.3035(3) 0.042(2) Uani 1 1 d . . . O91 O 0.28581(19) 0.1950(7) 0.3241(3) 0.074(2) Uani 1 1 d . . . P P 0.38610(5) 0.69531(18) 0.10789(6) 0.0242(4) Uani 1 1 d . . . C111 C 0.4242(2) 0.8254(7) 0.0994(2) 0.0277(16) Uani 1 1 d . . . C112 C 0.4232(2) 0.9087(7) 0.0586(3) 0.0341(18) Uani 1 1 d . . . H11A H 0.4025 0.8982 0.0359 0.041 Uiso 1 1 calc R . . C113 C 0.4514(2) 1.0049(8) 0.0509(3) 0.0373(19) Uani 1 1 d . . . H11B H 0.4501 1.0616 0.0233 0.045 Uiso 1 1 calc R . . C114 C 0.4818(2) 1.0188(7) 0.0835(3) 0.0291(17) Uani 1 1 d . . . C115 C 0.4845(2) 0.9358(7) 0.1229(3) 0.0325(18) Uani 1 1 d . . . H11C H 0.5059 0.9439 0.1446 0.039 Uiso 1 1 calc R . . C116 C 0.4555(2) 0.8399(7) 0.1308(2) 0.0265(16) Uani 1 1 d . . . H11D H 0.4571 0.7831 0.1583 0.032 Uiso 1 1 calc R . . C117 C 0.5114(3) 1.1296(9) 0.0775(3) 0.049(2) Uani 1 1 d . . . F11 F 0.54496(18) 1.1044(8) 0.0964(3) 0.125(3) Uani 1 1 d . . . F12 F 0.4990(2) 1.2458(6) 0.09864(19) 0.084(2) Uani 1 1 d . . . F13 F 0.51616(16) 1.1665(5) 0.03227(17) 0.0619(15) Uani 1 1 d . . . C121 C 0.3412(2) 0.7831(7) 0.0908(2) 0.0264(16) Uani 1 1 d . . . C122 C 0.3081(2) 0.7123(7) 0.0749(3) 0.0315(17) Uani 1 1 d . . . H12A H 0.3095 0.6166 0.0711 0.038 Uiso 1 1 calc R . . C123 C 0.2736(2) 0.7779(7) 0.0648(3) 0.0340(18) Uani 1 1 d . . . H12B H 0.2518 0.7280 0.0529 0.041 Uiso 1 1 calc R . . C124 C 0.2703(2) 0.9167(7) 0.0720(3) 0.0310(17) Uani 1 1 d . . . C125 C 0.3021(2) 0.9872(7) 0.0898(3) 0.0354(18) Uani 1 1 d . . . H12C H 0.3000 1.0819 0.0957 0.042 Uiso 1 1 calc R . . C126 C 0.3369(2) 0.9207(8) 0.0992(3) 0.0324(18) Uani 1 1 d . . . H12D H 0.3584 0.9707 0.1117 0.039 Uiso 1 1 calc R . . C127 C 0.2328(3) 0.9877(9) 0.0607(3) 0.045(2) Uani 1 1 d . . . F21 F 0.20298(18) 0.9351(8) 0.0831(3) 0.118(3) Uani 1 1 d . . . F22 F 0.22366(19) 0.9829(8) 0.0156(2) 0.103(3) Uani 1 1 d . . . F23 F 0.23220(19) 1.1150(6) 0.0733(3) 0.106(3) Uani 1 1 d . . . C131 C 0.3997(2) 0.5860(7) 0.0568(2) 0.0270(16) Uani 1 1 d . . . C132 C 0.4371(2) 0.5258(7) 0.0595(2) 0.0316(17) Uani 1 1 d . . . H13A H 0.4529 0.5364 0.0874 0.038 Uiso 1 1 calc R . . C133 C 0.4505(2) 0.4505(8) 0.0206(3) 0.0370(19) Uani 1 1 d . . . H13B H 0.4760 0.4118 0.0218 0.044 Uiso 1 1 calc R . . C134 C 0.4277(2) 0.4316(8) -0.0191(3) 0.0351(18) Uani 1 1 d . . . C135 C 0.3907(3) 0.4906(8) -0.0221(3) 0.045(2) Uani 1 1 d . . . H13C H 0.3749 0.4781 -0.0499 0.054 Uiso 1 1 calc R . . C136 C 0.3772(2) 0.5674(8) 0.0159(2) 0.0360(19) Uani 1 1 d . . . H13D H 0.3521 0.6083 0.0138 0.043 Uiso 1 1 calc R . . C137 C 0.4433(3) 0.3564(10) -0.0613(3) 0.052(3) Uani 1 1 d . . . F31 F 0.4678(2) 0.2582(7) -0.04842(19) 0.112(3) Uani 1 1 d . . . F32 F 0.46295(18) 0.4339(6) -0.09130(18) 0.0778(18) Uani 1 1 d . . . F33 F 0.41565(18) 0.2975(6) -0.08822(18) 0.0704(16) Uani 1 1 d . . . C1 C 0.3412(3) 1.0334(11) -0.0676(4) 0.080(3) Uani 1 1 d . . . H1A H 0.3575 1.0715 -0.0942 0.096 Uiso 1 1 calc R . . Cl1 Cl 0.35175(12) 0.8622(4) -0.06365(15) 0.1155(13) Uani 1 1 d . . . Cl2 Cl 0.35308(13) 1.1218(4) -0.01595(11) 0.1118(13) Uani 1 1 d . . . Cl3 Cl 0.29180(10) 1.0556(3) -0.08374(13) 0.0983(10) 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 Rh10 0.0188(3) 0.0238(3) 0.0196(3) -0.0020(2) -0.0008(2) 0.0011(2) Rh20 0.0226(3) 0.0257(3) 0.0227(3) -0.0033(2) -0.0006(2) 0.0015(2) Rh21 0.0194(3) 0.0287(3) 0.0264(3) -0.0017(2) -0.0042(2) -0.0018(2) Rh30 0.0182(3) 0.0269(3) 0.0215(3) -0.0012(2) -0.0028(2) -0.0018(2) Rh31 0.0196(3) 0.0300(3) 0.0244(3) -0.0037(2) 0.0026(2) -0.0004(2) Rh40 0.0206(3) 0.0283(3) 0.0250(3) 0.0014(2) -0.0017(2) -0.0032(2) C10 0.033(5) 0.020(4) 0.020(3) -0.001(3) -0.005(3) 0.002(3) O10 0.017(3) 0.040(3) 0.033(3) 0.001(2) 0.000(2) -0.001(2) C11 0.017(4) 0.046(5) 0.026(4) -0.004(4) 0.005(3) -0.009(4) O11 0.022(3) 0.036(3) 0.038(3) 0.000(2) 0.002(2) 0.006(2) C20 0.032(5) 0.037(5) 0.034(4) -0.001(4) -0.005(4) 0.004(4) O20 0.038(3) 0.029(3) 0.040(3) -0.008(2) -0.009(3) -0.004(2) C30 0.025(4) 0.031(4) 0.031(4) -0.005(3) 0.005(3) 0.001(3) O30 0.039(3) 0.056(4) 0.023(3) -0.001(3) 0.005(2) -0.008(3) C40 0.018(4) 0.031(4) 0.019(4) 0.006(3) 0.005(3) -0.002(3) O40 0.049(4) 0.030(3) 0.046(3) -0.009(3) 0.006(3) -0.006(3) C50 0.032(4) 0.031(4) 0.032(4) 0.002(4) -0.005(4) 0.001(3) O50 0.059(4) 0.050(4) 0.030(3) -0.013(3) 0.002(3) -0.009(3) C51 0.040(5) 0.026(4) 0.032(4) -0.007(3) -0.013(4) 0.004(3) O51 0.075(5) 0.042(3) 0.039(3) -0.007(3) -0.018(3) -0.001(3) C60 0.035(5) 0.021(4) 0.033(4) -0.006(3) 0.006(4) -0.006(3) O60 0.032(3) 0.031(3) 0.056(4) -0.001(3) -0.007(3) 0.007(3) C61 0.031(5) 0.038(5) 0.038(5) 0.003(4) -0.012(4) 0.001(4) O61 0.026(4) 0.076(5) 0.076(4) 0.010(4) 0.002(3) -0.011(3) C70 0.028(4) 0.032(4) 0.041(5) 0.008(4) -0.006(4) -0.004(4) O70 0.059(4) 0.041(4) 0.069(4) -0.010(3) -0.016(3) -0.020(3) C71 0.027(4) 0.043(5) 0.030(4) -0.004(4) 0.004(3) -0.002(4) O71 0.056(4) 0.053(4) 0.059(4) -0.032(3) 0.016(3) -0.012(3) C80 0.023(4) 0.029(4) 0.030(4) 0.000(3) 0.004(3) 0.003(3) O80 0.034(3) 0.039(3) 0.059(4) 0.007(3) -0.015(3) 0.006(3) C81 0.029(5) 0.041(5) 0.034(4) -0.001(4) 0.002(4) -0.009(4) O81 0.031(4) 0.079(5) 0.059(4) 0.004(3) 0.019(3) -0.002(3) C90 0.031(4) 0.023(4) 0.031(4) 0.006(3) -0.007(3) -0.004(3) O90 0.043(4) 0.039(3) 0.055(4) 0.009(3) -0.013(3) -0.004(3) C91 0.030(5) 0.049(5) 0.046(5) 0.015(4) 0.002(4) -0.001(4) O91 0.033(4) 0.093(5) 0.094(5) 0.035(4) 0.015(4) -0.005(4) P 0.0215(10) 0.0290(10) 0.0222(9) -0.0007(8) 0.0002(8) 0.0048(8) C111 0.025(4) 0.033(4) 0.026(4) 0.000(3) 0.005(3) 0.002(3) C112 0.038(5) 0.039(4) 0.026(4) 0.007(3) 0.003(4) 0.003(4) C113 0.044(5) 0.041(5) 0.027(4) 0.008(4) 0.006(4) 0.001(4) C114 0.029(4) 0.027(4) 0.031(4) -0.001(3) 0.004(3) 0.002(3) C115 0.024(4) 0.040(4) 0.034(4) -0.001(4) 0.000(3) 0.004(3) C116 0.026(4) 0.025(4) 0.029(4) 0.006(3) 0.000(3) 0.003(3) C117 0.049(6) 0.059(6) 0.038(5) 0.005(5) -0.002(4) -0.013(5) F11 0.053(4) 0.136(6) 0.185(7) 0.107(6) -0.051(5) -0.054(4) F12 0.131(6) 0.059(4) 0.063(4) -0.014(3) 0.019(4) -0.039(4) F13 0.071(4) 0.070(4) 0.045(3) 0.006(3) 0.020(3) -0.024(3) C121 0.025(4) 0.033(4) 0.021(4) -0.002(3) 0.002(3) 0.003(3) C122 0.031(4) 0.028(4) 0.036(4) -0.004(3) -0.008(4) 0.003(3) C123 0.031(4) 0.034(4) 0.036(4) -0.002(4) -0.007(4) -0.005(3) C124 0.031(4) 0.034(4) 0.028(4) 0.000(3) -0.006(3) 0.007(3) C125 0.036(5) 0.028(4) 0.042(5) -0.011(4) 0.003(4) 0.005(3) C126 0.022(4) 0.040(5) 0.035(4) -0.006(4) -0.010(3) 0.001(3) C127 0.036(5) 0.046(5) 0.053(6) -0.003(4) -0.006(4) 0.010(4) F21 0.035(4) 0.144(7) 0.175(8) 0.054(6) 0.020(4) 0.029(4) F22 0.086(5) 0.159(7) 0.064(4) -0.028(4) -0.041(3) 0.079(5) F23 0.077(4) 0.064(4) 0.175(7) -0.045(4) -0.066(5) 0.041(3) C131 0.028(4) 0.026(4) 0.028(4) -0.001(3) 0.000(3) -0.001(3) C132 0.034(4) 0.038(4) 0.023(4) 0.004(3) -0.003(3) 0.006(4) C133 0.037(5) 0.037(4) 0.037(4) 0.000(4) 0.006(4) 0.008(4) C134 0.044(5) 0.037(4) 0.024(4) -0.001(3) -0.004(4) 0.009(4) C135 0.055(6) 0.059(6) 0.022(4) -0.008(4) -0.009(4) 0.007(4) C136 0.038(5) 0.045(5) 0.024(4) -0.007(4) -0.008(3) 0.013(4) C137 0.068(7) 0.065(6) 0.024(4) 0.002(4) 0.008(5) 0.035(5) F31 0.157(7) 0.136(6) 0.044(3) -0.027(4) -0.012(4) 0.112(6) F32 0.087(5) 0.105(5) 0.042(3) -0.020(3) 0.032(3) -0.011(4) F33 0.089(4) 0.072(4) 0.050(3) -0.033(3) 0.010(3) 0.002(3) C1 0.084(9) 0.083(8) 0.071(7) 0.017(6) -0.013(6) -0.022(7) Cl1 0.111(3) 0.091(2) 0.144(3) 0.011(2) -0.030(2) 0.015(2) Cl2 0.156(4) 0.116(3) 0.0627(19) 0.0046(18) -0.024(2) -0.043(3) Cl3 0.074(2) 0.098(2) 0.123(3) -0.001(2) -0.025(2) 0.0119(18) _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 Rh10 C40 1.868(7) . ? Rh10 C11 2.137(7) . ? Rh10 C10 2.138(7) . ? Rh10 P 2.3440(18) . ? Rh10 Rh30 2.7588(7) . ? Rh10 Rh31 2.7841(8) . ? Rh10 Rh20 2.7934(7) . ? Rh10 Rh21 2.8118(8) . ? Rh20 C50 1.917(8) . ? Rh20 C60 1.920(8) . ? Rh20 C10 2.177(7) . ? Rh20 C20 2.241(8) . ? Rh20 Rh21 2.7301(8) . ? Rh20 Rh40 2.7618(8) . ? Rh20 Rh30 2.7623(7) . ? Rh21 C51 1.879(7) . ? Rh21 C61 1.907(9) . ? Rh21 C20 2.205(8) . ? Rh21 C11 2.209(8) . ? Rh21 Rh31 2.7603(7) . ? Rh21 Rh40 2.7853(7) . ? Rh30 C70 1.912(8) . ? Rh30 C80 1.919(7) . ? Rh30 C30 2.186(7) . ? Rh30 C10 2.249(7) . ? Rh30 Rh31 2.7481(8) . ? Rh30 Rh40 2.7542(7) . ? Rh31 C81 1.897(9) . ? Rh31 C71 1.905(8) . ? Rh31 C30 2.187(7) . ? Rh31 C11 2.264(7) . ? Rh31 Rh40 2.7521(8) . ? Rh40 C90 1.908(7) . ? Rh40 C91 1.910(9) . ? Rh40 C20 2.135(8) . ? Rh40 C30 2.176(7) . ? C10 O10 1.171(8) . ? C11 O11 1.161(8) . ? C20 O20 1.150(8) . ? C30 O30 1.160(8) . ? C40 O40 1.141(8) . ? C50 O50 1.125(8) . ? C51 O51 1.141(8) . ? C60 O60 1.130(8) . ? C61 O61 1.135(9) . ? C70 O70 1.114(8) . ? C71 O71 1.127(9) . ? C80 O80 1.110(8) . ? C81 O81 1.132(9) . ? C90 O90 1.125(8) . ? C91 O91 1.132(9) . ? P C121 1.821(7) . ? P C111 1.843(7) . ? P C131 1.845(7) . ? C111 C116 1.383(9) . ? C111 C112 1.402(9) . ? C112 C113 1.370(10) . ? C113 C114 1.382(10) . ? C114 C115 1.373(10) . ? C114 C117 1.497(11) . ? C115 C116 1.387(10) . ? C117 F11 1.284(10) . ? C117 F13 1.322(9) . ? C117 F12 1.357(10) . ? C121 C126 1.385(10) . ? C121 C122 1.399(10) . ? C122 C123 1.372(10) . ? C123 C124 1.387(10) . ? C124 C125 1.381(10) . ? C124 C127 1.491(10) . ? C125 C126 1.379(10) . ? C127 F22 1.293(9) . ? C127 F21 1.303(11) . ? C127 F23 1.303(10) . ? C131 C136 1.383(9) . ? C131 C132 1.410(10) . ? C132 C133 1.391(10) . ? C133 C134 1.363(10) . ? C134 C135 1.391(11) . ? C134 C137 1.489(11) . ? C135 C136 1.381(10) . ? C137 F32 1.319(11) . ? C137 F31 1.327(9) . ? C137 F33 1.335(11) . ? C1 Cl2 1.728(11) . ? C1 Cl1 1.729(12) . ? C1 Cl3 1.757(12) . ? 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 C40 Rh10 C11 92.5(3) . . ? C40 Rh10 C10 104.5(3) . . ? C11 Rh10 C10 157.3(3) . . ? C40 Rh10 P 87.1(2) . . ? C11 Rh10 P 98.5(2) . . ? C10 Rh10 P 97.34(19) . . ? C40 Rh10 Rh30 94.56(19) . . ? C11 Rh10 Rh30 111.72(19) . . ? C10 Rh10 Rh30 52.86(18) . . ? P Rh10 Rh30 149.63(5) . . ? C40 Rh10 Rh31 89.5(2) . . ? C11 Rh10 Rh31 52.82(19) . . ? C10 Rh10 Rh31 111.47(18) . . ? P Rh10 Rh31 150.91(5) . . ? Rh30 Rh10 Rh31 59.441(19) . . ? C40 Rh10 Rh20 150.9(2) . . ? C11 Rh10 Rh20 108.9(2) . . ? C10 Rh10 Rh20 50.26(18) . . ? P Rh10 Rh20 108.19(5) . . ? Rh30 Rh10 Rh20 59.666(18) . . ? Rh31 Rh10 Rh20 88.23(2) . . ? C40 Rh10 Rh21 140.9(2) . . ? C11 Rh10 Rh21 50.8(2) . . ? C10 Rh10 Rh21 108.36(18) . . ? P Rh10 Rh21 108.81(5) . . ? Rh30 Rh10 Rh21 88.76(2) . . ? Rh31 Rh10 Rh21 59.109(19) . . ? Rh20 Rh10 Rh21 58.296(19) . . ? C50 Rh20 C60 93.0(3) . . ? C50 Rh20 C10 104.7(3) . . ? C60 Rh20 C10 97.9(3) . . ? C50 Rh20 C20 92.1(3) . . ? C60 Rh20 C20 97.2(3) . . ? C10 Rh20 C20 156.7(3) . . ? C50 Rh20 Rh21 94.7(2) . . ? C60 Rh20 Rh21 148.0(2) . . ? C10 Rh20 Rh21 110.04(19) . . ? C20 Rh20 Rh21 51.52(19) . . ? C50 Rh20 Rh40 141.1(2) . . ? C60 Rh20 Rh40 94.7(2) . . ? C10 Rh20 Rh40 111.84(18) . . ? C20 Rh20 Rh40 49.18(19) . . ? Rh21 Rh20 Rh40 60.95(2) . . ? C50 Rh20 Rh30 156.8(2) . . ? C60 Rh20 Rh30 94.6(2) . . ? C10 Rh20 Rh30 52.57(18) . . ? C20 Rh20 Rh30 108.60(19) . . ? Rh21 Rh20 Rh30 90.37(2) . . ? Rh40 Rh20 Rh30 59.812(19) . . ? C50 Rh20 Rh10 103.6(2) . . ? C60 Rh20 Rh10 145.6(2) . . ? C10 Rh20 Rh10 49.05(19) . . ? C20 Rh20 Rh10 111.8(2) . . ? Rh21 Rh20 Rh10 61.190(19) . . ? Rh40 Rh20 Rh10 90.91(2) . . ? Rh30 Rh20 Rh10 59.546(18) . . ? C51 Rh21 C61 92.7(3) . . ? C51 Rh21 C20 93.8(3) . . ? C61 Rh21 C20 100.5(3) . . ? C51 Rh21 C11 102.8(3) . . ? C61 Rh21 C11 95.0(3) . . ? C20 Rh21 C11 156.7(3) . . ? C51 Rh21 Rh20 94.8(2) . . ? C61 Rh21 Rh20 152.5(2) . . ? C20 Rh21 Rh20 52.7(2) . . ? C11 Rh21 Rh20 108.90(18) . . ? C51 Rh21 Rh31 155.2(2) . . ? C61 Rh21 Rh31 94.2(2) . . ? C20 Rh21 Rh31 108.32(19) . . ? C11 Rh21 Rh31 52.81(18) . . ? Rh20 Rh21 Rh31 90.00(2) . . ? C51 Rh21 Rh40 142.3(2) . . ? C61 Rh21 Rh40 99.2(2) . . ? C20 Rh21 Rh40 48.98(19) . . ? C11 Rh21 Rh40 111.48(18) . . ? Rh20 Rh21 Rh40 60.089(19) . . ? Rh31 Rh21 Rh40 59.505(19) . . ? C51 Rh21 Rh10 101.7(2) . . ? C61 Rh21 Rh10 142.9(2) . . ? C20 Rh21 Rh10 112.3(2) . . ? C11 Rh21 Rh10 48.59(18) . . ? Rh20 Rh21 Rh10 60.514(19) . . ? Rh31 Rh21 Rh10 59.945(19) . . ? Rh40 Rh21 Rh10 90.04(2) . . ? C70 Rh30 C80 93.1(3) . . ? C70 Rh30 C30 100.6(3) . . ? C80 Rh30 C30 97.2(3) . . ? C70 Rh30 C10 96.4(3) . . ? C80 Rh30 C10 98.8(3) . . ? C30 Rh30 C10 155.9(3) . . ? C70 Rh30 Rh31 100.1(2) . . ? C80 Rh30 Rh31 147.2(2) . . ? C30 Rh30 Rh31 51.08(19) . . ? C10 Rh30 Rh31 109.20(18) . . ? C70 Rh30 Rh40 150.9(2) . . ? C80 Rh30 Rh40 95.0(2) . . ? C30 Rh30 Rh40 50.68(18) . . ? C10 Rh30 Rh40 109.78(18) . . ? Rh31 Rh30 Rh40 60.02(2) . . ? C70 Rh30 Rh10 96.2(2) . . ? C80 Rh30 Rh10 147.5(2) . . ? C30 Rh30 Rh10 111.51(19) . . ? C10 Rh30 Rh10 49.26(18) . . ? Rh31 Rh30 Rh10 60.737(19) . . ? Rh40 Rh30 Rh10 91.80(2) . . ? C70 Rh30 Rh20 146.4(2) . . ? C80 Rh30 Rh20 95.7(2) . . ? C30 Rh30 Rh20 110.27(19) . . ? C10 Rh30 Rh20 50.21(17) . . ? Rh31 Rh30 Rh20 89.59(2) . . ? Rh40 Rh30 Rh20 60.086(19) . . ? Rh10 Rh30 Rh20 60.788(18) . . ? C81 Rh31 C71 92.0(3) . . ? C81 Rh31 C30 100.6(3) . . ? C71 Rh31 C30 95.8(3) . . ? C81 Rh31 C11 97.4(3) . . ? C71 Rh31 C11 99.8(3) . . ? C30 Rh31 C11 155.8(3) . . ? C81 Rh31 Rh30 150.7(2) . . ? C71 Rh31 Rh30 97.6(2) . . ? C30 Rh31 Rh30 51.04(19) . . ? C11 Rh31 Rh30 108.09(18) . . ? C81 Rh31 Rh40 97.7(2) . . ? C71 Rh31 Rh40 146.2(2) . . ? C30 Rh31 Rh40 50.71(18) . . ? C11 Rh31 Rh40 110.9(2) . . ? Rh30 Rh31 Rh40 60.098(19) . . ? C81 Rh31 Rh21 95.1(2) . . ? C71 Rh31 Rh21 150.5(2) . . ? C30 Rh31 Rh21 110.90(19) . . ? C11 Rh31 Rh21 51.00(19) . . ? Rh30 Rh31 Rh21 90.04(2) . . ? Rh40 Rh31 Rh21 60.699(19) . . ? C81 Rh31 Rh10 145.7(2) . . ? C71 Rh31 Rh10 98.7(2) . . ? C30 Rh31 Rh10 110.56(19) . . ? C11 Rh31 Rh10 48.77(18) . . ? Rh30 Rh31 Rh10 59.823(19) . . ? Rh40 Rh31 Rh10 91.31(2) . . ? Rh21 Rh31 Rh10 60.946(19) . . ? C90 Rh40 C91 91.6(3) . . ? C90 Rh40 C20 99.0(3) . . ? C91 Rh40 C20 97.4(3) . . ? C90 Rh40 C30 96.6(3) . . ? C91 Rh40 C30 96.9(3) . . ? C20 Rh40 C30 158.5(3) . . ? C90 Rh40 Rh31 147.0(2) . . ? C91 Rh40 Rh31 98.1(3) . . ? C20 Rh40 Rh31 110.8(2) . . ? C30 Rh40 Rh31 51.07(19) . . ? C90 Rh40 Rh30 96.3(2) . . ? C91 Rh40 Rh30 147.5(3) . . ? C20 Rh40 Rh30 112.3(2) . . ? C30 Rh40 Rh30 51.0(2) . . ? Rh31 Rh40 Rh30 59.88(2) . . ? C90 Rh40 Rh20 97.8(2) . . ? C91 Rh40 Rh20 149.5(2) . . ? C20 Rh40 Rh20 52.6(2) . . ? C30 Rh40 Rh20 110.6(2) . . ? Rh31 Rh40 Rh20 89.52(2) . . ? Rh30 Rh40 Rh20 60.102(19) . . ? C90 Rh40 Rh21 148.9(2) . . ? C91 Rh40 Rh21 99.8(2) . . ? C20 Rh40 Rh21 51.2(2) . . ? C30 Rh40 Rh21 110.37(19) . . ? Rh31 Rh40 Rh21 59.796(19) . . ? Rh30 Rh40 Rh21 89.39(2) . . ? Rh20 Rh40 Rh21 58.965(19) . . ? O10 C10 Rh10 135.7(5) . . ? O10 C10 Rh20 133.9(5) . . ? Rh10 C10 Rh20 80.7(3) . . ? O10 C10 Rh30 128.8(5) . . ? Rh10 C10 Rh30 77.9(3) . . ? Rh20 C10 Rh30 77.2(2) . . ? O11 C11 Rh10 136.2(6) . . ? O11 C11 Rh21 134.1(5) . . ? Rh10 C11 Rh21 80.6(3) . . ? O11 C11 Rh31 128.3(6) . . ? Rh10 C11 Rh31 78.4(2) . . ? Rh21 C11 Rh31 76.2(2) . . ? O20 C20 Rh40 135.0(6) . . ? O20 C20 Rh21 132.6(6) . . ? Rh40 C20 Rh21 79.8(3) . . ? O20 C20 Rh20 132.5(6) . . ? Rh40 C20 Rh20 78.2(3) . . ? Rh21 C20 Rh20 75.8(3) . . ? O30 C30 Rh40 133.7(6) . . ? O30 C30 Rh30 133.3(6) . . ? Rh40 C30 Rh30 78.3(2) . . ? O30 C30 Rh31 132.9(6) . . ? Rh40 C30 Rh31 78.2(2) . . ? Rh30 C30 Rh31 77.9(2) . . ? O40 C40 Rh10 174.9(6) . . ? O50 C50 Rh20 172.3(7) . . ? O51 C51 Rh21 176.1(7) . . ? O60 C60 Rh20 176.8(7) . . ? O61 C61 Rh21 179.1(7) . . ? O70 C70 Rh30 178.3(8) . . ? O71 C71 Rh31 176.2(7) . . ? O80 C80 Rh30 177.3(7) . . ? O81 C81 Rh31 179.2(8) . . ? O90 C90 Rh40 178.9(7) . . ? O91 C91 Rh40 177.0(7) . . ? C121 P C111 103.2(3) . . ? C121 P C131 106.9(3) . . ? C111 P C131 97.3(3) . . ? C121 P Rh10 110.1(2) . . ? C111 P Rh10 114.2(2) . . ? C131 P Rh10 123.0(2) . . ? C116 C111 C112 118.0(7) . . ? C116 C111 P 122.2(5) . . ? C112 C111 P 119.7(5) . . ? C113 C112 C111 121.1(7) . . ? C112 C113 C114 119.5(7) . . ? C115 C114 C113 120.9(7) . . ? C115 C114 C117 118.8(7) . . ? C113 C114 C117 120.3(7) . . ? C114 C115 C116 119.3(7) . . ? C111 C116 C115 121.2(6) . . ? F11 C117 F13 109.3(8) . . ? F11 C117 F12 105.3(8) . . ? F13 C117 F12 102.8(7) . . ? F11 C117 C114 114.5(7) . . ? F13 C117 C114 113.1(7) . . ? F12 C117 C114 110.9(7) . . ? C126 C121 C122 117.1(6) . . ? C126 C121 P 120.8(5) . . ? C122 C121 P 121.5(5) . . ? C123 C122 C121 121.4(7) . . ? C122 C123 C124 120.4(7) . . ? C125 C124 C123 118.9(7) . . ? C125 C124 C127 120.8(7) . . ? C123 C124 C127 120.2(7) . . ? C126 C125 C124 120.2(7) . . ? C125 C126 C121 121.8(7) . . ? F22 C127 F21 105.4(8) . . ? F22 C127 F23 107.1(8) . . ? F21 C127 F23 103.9(8) . . ? F22 C127 C124 113.0(7) . . ? F21 C127 C124 112.5(7) . . ? F23 C127 C124 114.1(7) . . ? C136 C131 C132 119.0(7) . . ? C136 C131 P 124.9(6) . . ? C132 C131 P 115.9(5) . . ? C133 C132 C131 119.0(6) . . ? C134 C133 C132 121.0(7) . . ? C133 C134 C135 120.4(7) . . ? C133 C134 C137 120.2(7) . . ? C135 C134 C137 119.3(7) . . ? C136 C135 C134 119.3(7) . . ? C135 C136 C131 121.2(7) . . ? F32 C137 F31 105.8(8) . . ? F32 C137 F33 104.8(7) . . ? F31 C137 F33 106.0(8) . . ? F32 C137 C134 113.4(8) . . ? F31 C137 C134 112.2(7) . . ? F33 C137 C134 113.9(8) . . ? Cl2 C1 Cl1 113.1(6) . . ? Cl2 C1 Cl3 111.8(7) . . ? Cl1 C1 Cl3 109.7(6) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.043 _refine_diff_density_min -1.092 _refine_diff_density_rms 0.188 #======END data_k9884a _database_code_CSD 163531 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '3 Rh6(CO)15(P(4-ClC6H4)3)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H28 Cl3 O15 P Rh6' _chemical_formula_weight 1503.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 27.5907(8) _cell_length_b 9.8040(3) _cell_length_c 36.9074(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.5350(10) _cell_angle_gamma 90.00 _cell_volume 9781.8(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 9641 _cell_measurement_theta_min 4.06 _cell_measurement_theta_max 26.16 _exptl_crystal_description block _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.042 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5792 _exptl_absorpt_coefficient_mu 2.237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Denzo-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scan with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 35663 _diffrn_reflns_av_R_equivalents 0.093 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 4.06 _diffrn_reflns_theta_max 26.16 _reflns_number_total 9641 _reflns_number_gt 6536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'Bruker SHELXTL V5.1' _computing_structure_refinement 'Bruker SHELXTL V5.1' _computing_molecular_graphics 'Bruker SHELXTL V5.1' _computing_publication_material 'Bruker SHELXTL V5.1' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0366P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000072(16) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9641 _refine_ls_number_parameters 594 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1012 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh10 Rh 0.343124(17) 0.13239(5) 0.111073(13) 0.02573(13) Uani 1 1 d . . . Rh20 Rh 0.359130(18) -0.07059(5) 0.166482(13) 0.02771(13) Uani 1 1 d . . . Rh21 Rh 0.333430(18) -0.14792(5) 0.093596(13) 0.02713(13) Uani 1 1 d . . . Rh30 Rh 0.275664(18) 0.09566(5) 0.158774(14) 0.03083(13) Uani 1 1 d . . . Rh31 Rh 0.249857(18) 0.01878(5) 0.084856(13) 0.02956(13) Uani 1 1 d . . . Rh40 Rh 0.264519(18) -0.17795(5) 0.139622(13) 0.02910(13) Uani 1 1 d . . . C10 C 0.3585(2) 0.1535(7) 0.17058(17) 0.0328(15) Uani 1 1 d . . . O10 O 0.37986(16) 0.2294(4) 0.19250(12) 0.0377(11) Uani 1 1 d . . . C11 C 0.3175(2) 0.0366(6) 0.05857(18) 0.0274(14) Uani 1 1 d . . . O11 O 0.31969(16) 0.0597(4) 0.02742(12) 0.0346(10) Uani 1 1 d . . . C20 C 0.3356(2) -0.2739(7) 0.14551(17) 0.0336(15) Uani 1 1 d . . . O20 O 0.35151(16) -0.3843(4) 0.15385(12) 0.0369(11) Uani 1 1 d . . . C30 C 0.2090(3) -0.0124(7) 0.13025(18) 0.0412(17) Uani 1 1 d . . . O30 O 0.16703(17) -0.0049(5) 0.13195(13) 0.0464(12) Uani 1 1 d . . . C40 C 0.3207(2) 0.3113(7) 0.10161(17) 0.0311(14) Uani 1 1 d . . . O40 O 0.30531(17) 0.4207(5) 0.09586(13) 0.0427(12) Uani 1 1 d . . . C50 C 0.4284(2) -0.0997(6) 0.16995(17) 0.0326(15) Uani 1 1 d . . . O50 O 0.46997(17) -0.1223(5) 0.17138(14) 0.0460(12) Uani 1 1 d . . . C51 C 0.3990(3) -0.2099(6) 0.09140(18) 0.0360(16) Uani 1 1 d . . . O51 O 0.43627(18) -0.2613(5) 0.09250(13) 0.0469(12) Uani 1 1 d . . . C60 C 0.3608(3) -0.1048(7) 0.21859(18) 0.0398(17) Uani 1 1 d . . . O60 O 0.3606(2) -0.1286(5) 0.24853(13) 0.0573(15) Uani 1 1 d . . . C61 C 0.3045(2) -0.2757(6) 0.05626(18) 0.0338(15) Uani 1 1 d . . . O61 O 0.28700(18) -0.3563(5) 0.03473(13) 0.0473(13) Uani 1 1 d . . . C70 C 0.2510(3) 0.2784(8) 0.1559(2) 0.0485(19) Uani 1 1 d . . . O70 O 0.2369(2) 0.3884(6) 0.15657(17) 0.0716(18) Uani 1 1 d . . . C71 C 0.2191(3) 0.1846(7) 0.0651(2) 0.0464(19) Uani 1 1 d . . . O71 O 0.2012(2) 0.2831(6) 0.05303(18) 0.077(2) Uani 1 1 d . . . C80 C 0.2675(2) 0.0803(7) 0.2088(2) 0.0392(16) Uani 1 1 d . . . O80 O 0.2627(2) 0.0726(6) 0.23917(15) 0.0650(16) Uani 1 1 d . . . C81 C 0.2083(2) -0.0910(7) 0.04829(18) 0.0348(15) Uani 1 1 d . . . O81 O 0.18275(19) -0.1588(5) 0.02738(13) 0.0553(14) Uani 1 1 d . . . C90 C 0.2484(3) -0.2452(7) 0.18507(19) 0.0426(17) Uani 1 1 d . . . O90 O 0.2372(2) -0.2895(6) 0.21087(15) 0.0736(18) Uani 1 1 d . . . C91 C 0.2264(2) -0.3169(7) 0.10949(17) 0.0319(15) Uani 1 1 d . . . O91 O 0.20526(18) -0.3985(5) 0.09153(13) 0.0490(13) Uani 1 1 d . . . P P 0.42120(6) 0.20566(16) 0.10012(4) 0.0270(4) Uani 1 1 d . . . C111 C 0.4548(2) 0.2980(6) 0.14118(16) 0.0256(13) Uani 1 1 d . . . C112 C 0.4448(2) 0.4374(6) 0.14396(17) 0.0336(15) Uani 1 1 d . . . H11A H 0.4239 0.4810 0.1245 0.040 Uiso 1 1 calc R . . C113 C 0.4657(2) 0.5117(7) 0.17541(17) 0.0359(16) Uani 1 1 d . . . H11B H 0.4588 0.6041 0.1770 0.043 Uiso 1 1 calc R . . C114 C 0.4969(2) 0.4456(6) 0.20438(16) 0.0320(15) Uani 1 1 d . . . C115 C 0.5062(2) 0.3078(7) 0.20267(18) 0.0370(16) Uani 1 1 d . . . H11C H 0.5269 0.2652 0.2224 0.044 Uiso 1 1 calc R . . C116 C 0.4850(2) 0.2320(6) 0.17164(16) 0.0321(15) Uani 1 1 d . . . H11D H 0.4906 0.1385 0.1710 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.52378(7) 0.53987(18) 0.24360(5) 0.0478(5) Uani 1 1 d . . . C121 C 0.4189(2) 0.3354(6) 0.06339(15) 0.0246(13) Uani 1 1 d . . . C122 C 0.4618(2) 0.4099(6) 0.06074(16) 0.0307(14) Uani 1 1 d . . . H12A H 0.4907 0.3938 0.0780 0.037 Uiso 1 1 calc R . . C123 C 0.4623(2) 0.5063(6) 0.03339(17) 0.0323(15) Uani 1 1 d . . . H12B H 0.4909 0.5550 0.0324 0.039 Uiso 1 1 calc R . . C124 C 0.4187(2) 0.5287(6) 0.00737(16) 0.0322(15) Uani 1 1 d . . . C125 C 0.3763(2) 0.4547(6) 0.00819(17) 0.0311(14) Uani 1 1 d . . . H12C H 0.3480 0.4691 -0.0098 0.037 Uiso 1 1 calc R . . C126 C 0.3758(2) 0.3593(6) 0.03570(16) 0.0297(14) Uani 1 1 d . . . H12D H 0.3471 0.3103 0.0361 0.036 Uiso 1 1 calc R . . Cl2 Cl 0.41927(6) 0.64868(18) -0.02803(5) 0.0421(4) Uani 1 1 d . . . C131 C 0.4650(2) 0.0868(6) 0.08478(17) 0.0315(14) Uani 1 1 d . . . C132 C 0.5147(3) 0.0684(7) 0.10205(19) 0.0463(19) Uani 1 1 d . . . H13A H 0.5269 0.1151 0.1239 0.056 Uiso 1 1 calc R . . C133 C 0.5463(3) -0.0175(8) 0.0876(2) 0.051(2) Uani 1 1 d . . . H13B H 0.5790 -0.0287 0.0997 0.061 Uiso 1 1 calc R . . C134 C 0.5280(3) -0.0863(7) 0.05476(19) 0.0426(17) Uani 1 1 d . . . C135 C 0.4796(2) -0.0689(6) 0.03658(17) 0.0338(15) Uani 1 1 d . . . H13C H 0.4679 -0.1132 0.0143 0.041 Uiso 1 1 calc R . . C136 C 0.4486(2) 0.0152(6) 0.05183(17) 0.0347(15) Uani 1 1 d . . . H13D H 0.4158 0.0244 0.0398 0.042 Uiso 1 1 calc R . . Cl3 Cl 0.56723(7) -0.1979(2) 0.03663(6) 0.0567(5) Uani 1 1 d . . . C41 C 0.3935(4) -0.1415(12) 0.3624(3) 0.096(4) Uani 1 1 d . . . H41A H 0.3982 -0.1825 0.3865 0.143 Uiso 1 1 calc R . . H41B H 0.4158 -0.1823 0.3486 0.143 Uiso 1 1 calc R . . H41C H 0.3600 -0.1560 0.3495 0.143 Uiso 1 1 calc R . . C42 C 0.4034(4) 0.0072(11) 0.3663(3) 0.087(3) Uani 1 1 d . . . H42A H 0.4385 0.0222 0.3751 0.104 Uiso 1 1 calc R . . H42B H 0.3859 0.0451 0.3843 0.104 Uiso 1 1 calc R . . C43 C 0.3867(3) 0.0792(10) 0.3291(2) 0.070(3) Uani 1 1 d . . . H43A H 0.4022 0.0351 0.3108 0.084 Uiso 1 1 calc R . . H43B H 0.3512 0.0681 0.3213 0.084 Uiso 1 1 calc R . . C44 C 0.3988(4) 0.2295(10) 0.3299(3) 0.078(3) Uani 1 1 d . . . H44A H 0.4344 0.2404 0.3366 0.094 Uiso 1 1 calc R . . H44B H 0.3844 0.2730 0.3488 0.094 Uiso 1 1 calc R . . C45 C 0.3794(4) 0.3046(10) 0.2919(3) 0.090(3) Uani 1 1 d . . . H45A H 0.3906 0.2532 0.2726 0.108 Uiso 1 1 calc R . . H45B H 0.3436 0.3008 0.2866 0.108 Uiso 1 1 calc R . . C46 C 0.3940(5) 0.4462(12) 0.2889(3) 0.119(4) Uani 1 1 d . . . H46A H 0.4298 0.4504 0.2937 0.142 Uiso 1 1 calc R . . H46B H 0.3831 0.4980 0.3082 0.142 Uiso 1 1 calc R . . C47 C 0.3742(4) 0.5148(10) 0.2522(3) 0.095(3) Uani 1 1 d . . . H47A H 0.3806 0.6110 0.2544 0.142 Uiso 1 1 calc R . . H47B H 0.3392 0.4997 0.2453 0.142 Uiso 1 1 calc R . . H47C H 0.3902 0.4772 0.2336 0.142 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 Rh10 0.0279(3) 0.0208(2) 0.0277(3) -0.00122(19) 0.0039(2) 0.0013(2) Rh20 0.0294(3) 0.0258(3) 0.0267(3) -0.0003(2) 0.0025(2) 0.0023(2) Rh21 0.0308(3) 0.0227(3) 0.0274(3) -0.0020(2) 0.0047(2) 0.0005(2) Rh30 0.0332(3) 0.0279(3) 0.0322(3) -0.0007(2) 0.0085(2) 0.0053(2) Rh31 0.0277(3) 0.0271(3) 0.0316(3) 0.0029(2) 0.0004(2) 0.0015(2) Rh40 0.0297(3) 0.0271(3) 0.0302(3) 0.0019(2) 0.0052(2) -0.0004(2) C10 0.032(3) 0.032(4) 0.035(4) -0.005(3) 0.007(3) -0.004(3) O10 0.040(3) 0.037(3) 0.036(2) -0.011(2) 0.009(2) -0.002(2) C11 0.024(3) 0.018(3) 0.040(4) -0.005(3) 0.005(3) 0.003(2) O11 0.039(3) 0.034(3) 0.030(2) 0.000(2) 0.006(2) -0.004(2) C20 0.034(4) 0.036(4) 0.028(3) -0.007(3) 0.001(3) -0.006(3) O20 0.040(3) 0.027(3) 0.044(3) 0.004(2) 0.008(2) 0.004(2) C30 0.049(5) 0.039(4) 0.037(4) 0.000(3) 0.012(3) 0.008(3) O30 0.034(3) 0.051(3) 0.056(3) 0.005(2) 0.014(2) 0.006(2) C40 0.030(3) 0.031(4) 0.031(3) -0.005(3) 0.002(3) -0.002(3) O40 0.047(3) 0.026(3) 0.055(3) 0.003(2) 0.010(2) 0.008(2) C50 0.042(4) 0.022(3) 0.033(3) -0.002(3) 0.005(3) -0.002(3) O50 0.031(3) 0.036(3) 0.070(3) -0.004(2) 0.006(2) 0.005(2) C51 0.047(4) 0.023(3) 0.037(4) 0.000(3) 0.006(3) 0.003(3) O51 0.049(3) 0.036(3) 0.057(3) 0.008(2) 0.014(3) 0.014(2) C60 0.045(4) 0.039(4) 0.031(4) -0.001(3) -0.001(3) 0.004(3) O60 0.076(4) 0.062(4) 0.031(3) 0.005(2) 0.004(3) 0.001(3) C61 0.038(4) 0.027(3) 0.035(4) 0.002(3) 0.004(3) -0.002(3) O61 0.059(3) 0.036(3) 0.041(3) -0.007(2) -0.003(2) -0.005(2) C70 0.063(5) 0.036(4) 0.053(5) 0.006(3) 0.025(4) 0.015(4) O70 0.093(5) 0.046(4) 0.087(4) 0.011(3) 0.044(4) 0.025(3) C71 0.044(4) 0.039(4) 0.049(4) 0.007(3) -0.007(4) 0.000(3) O71 0.066(4) 0.041(3) 0.104(5) 0.018(3) -0.027(4) 0.012(3) C80 0.037(4) 0.038(4) 0.045(4) -0.004(3) 0.014(3) 0.003(3) O80 0.077(4) 0.072(4) 0.052(3) 0.000(3) 0.029(3) 0.008(3) C81 0.036(4) 0.029(4) 0.037(4) 0.010(3) 0.003(3) -0.003(3) O81 0.063(3) 0.052(3) 0.043(3) 0.005(3) -0.008(3) -0.022(3) C90 0.049(4) 0.047(4) 0.031(4) 0.008(3) 0.008(3) -0.006(4) O90 0.087(5) 0.082(5) 0.052(4) 0.007(3) 0.016(3) -0.026(4) C91 0.033(3) 0.029(4) 0.032(3) 0.008(3) 0.004(3) 0.007(3) O91 0.054(3) 0.038(3) 0.050(3) -0.005(2) -0.001(3) -0.011(2) P 0.0297(8) 0.0234(8) 0.0271(8) -0.0019(7) 0.0033(7) 0.0010(7) C111 0.027(3) 0.023(3) 0.029(3) 0.001(2) 0.010(3) 0.001(3) C112 0.042(4) 0.029(4) 0.027(3) 0.005(3) 0.000(3) 0.007(3) C113 0.038(4) 0.027(3) 0.041(4) -0.009(3) 0.006(3) 0.004(3) C114 0.040(4) 0.031(4) 0.024(3) -0.002(3) 0.002(3) -0.002(3) C115 0.038(4) 0.038(4) 0.031(3) 0.007(3) -0.003(3) 0.000(3) C116 0.038(4) 0.023(3) 0.034(3) 0.001(3) 0.002(3) -0.003(3) Cl1 0.0582(11) 0.0445(10) 0.0345(9) -0.0126(8) -0.0052(8) 0.0043(9) C121 0.028(3) 0.020(3) 0.027(3) -0.001(2) 0.009(3) 0.005(2) C122 0.029(3) 0.036(4) 0.027(3) -0.005(3) 0.005(3) 0.008(3) C123 0.031(3) 0.036(4) 0.033(3) -0.002(3) 0.013(3) -0.002(3) C124 0.046(4) 0.028(3) 0.025(3) 0.001(3) 0.011(3) 0.012(3) C125 0.030(3) 0.029(3) 0.032(3) -0.005(3) 0.001(3) 0.001(3) C126 0.032(3) 0.026(3) 0.030(3) -0.005(3) 0.002(3) -0.003(3) Cl2 0.0469(10) 0.0408(10) 0.0389(9) 0.0108(8) 0.0093(8) 0.0026(8) C131 0.036(4) 0.024(3) 0.036(4) 0.005(3) 0.010(3) 0.007(3) C132 0.039(4) 0.055(5) 0.039(4) -0.017(3) -0.005(3) 0.015(3) C133 0.036(4) 0.063(5) 0.049(5) -0.013(4) -0.004(4) 0.016(4) C134 0.054(4) 0.037(4) 0.040(4) -0.003(3) 0.017(4) 0.009(3) C135 0.037(4) 0.033(4) 0.033(3) -0.005(3) 0.010(3) 0.001(3) C136 0.034(4) 0.036(4) 0.034(4) -0.004(3) 0.007(3) 0.006(3) Cl3 0.0600(12) 0.0520(12) 0.0641(13) -0.0063(9) 0.0267(10) 0.0200(10) C41 0.100(8) 0.106(9) 0.096(8) 0.007(7) 0.056(7) 0.025(7) C42 0.068(7) 0.106(9) 0.082(7) 0.035(6) 0.003(5) 0.013(6) C43 0.059(6) 0.081(7) 0.071(6) -0.003(5) 0.015(5) 0.014(5) C44 0.084(7) 0.076(7) 0.086(7) -0.003(6) 0.042(6) 0.003(6) C45 0.127(9) 0.060(7) 0.096(8) 0.003(6) 0.055(7) 0.011(6) C46 0.165(13) 0.087(9) 0.119(10) 0.009(8) 0.066(9) 0.022(9) C47 0.131(10) 0.053(6) 0.104(8) 0.008(6) 0.032(7) 0.016(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh10 C40 1.869(7) . ? Rh10 C11 2.142(6) . ? Rh10 C10 2.162(6) . ? Rh10 P 2.3808(17) . ? Rh10 Rh31 2.7934(7) . ? Rh10 Rh21 2.8233(7) . ? Rh10 Rh20 2.8242(7) . ? Rh10 Rh30 2.8291(7) . ? Rh20 C50 1.912(7) . ? Rh20 C60 1.944(7) . ? Rh20 C20 2.189(6) . ? Rh20 C10 2.203(6) . ? Rh20 Rh21 2.7479(7) . ? Rh20 Rh30 2.7891(7) . ? Rh20 Rh40 2.8053(7) . ? Rh21 C61 1.914(6) . ? Rh21 C51 1.926(7) . ? Rh21 C11 2.216(6) . ? Rh21 C20 2.270(7) . ? Rh21 Rh31 2.7919(7) . ? Rh21 Rh40 2.8069(7) . ? Rh30 C70 1.911(7) . ? Rh30 C80 1.912(7) . ? Rh30 C30 2.199(7) . ? Rh30 C10 2.310(6) . ? Rh30 Rh40 2.7754(7) . ? Rh30 Rh31 2.7822(7) . ? Rh31 C71 1.909(7) . ? Rh31 C81 1.917(7) . ? Rh31 C30 2.219(7) . ? Rh31 C11 2.276(6) . ? Rh31 Rh40 2.7645(7) . ? Rh40 C91 1.932(7) . ? Rh40 C90 1.935(7) . ? Rh40 C20 2.148(7) . ? Rh40 C30 2.210(7) . ? C10 O10 1.168(7) . ? C11 O11 1.185(7) . ? C20 O20 1.184(7) . ? C30 O30 1.176(8) . ? C40 O40 1.157(7) . ? C50 O50 1.159(7) . ? C51 O51 1.138(7) . ? C60 O60 1.130(8) . ? C61 O61 1.156(7) . ? C70 O70 1.149(8) . ? C71 O71 1.135(8) . ? C80 O80 1.156(8) . ? C81 O81 1.147(7) . ? C90 O90 1.144(8) . ? C91 O91 1.124(7) . ? P C131 1.847(6) . ? P C111 1.848(6) . ? P C121 1.851(6) . ? C111 C112 1.403(8) . ? C111 C116 1.414(8) . ? C112 C113 1.393(8) . ? C113 C114 1.392(8) . ? C114 C115 1.378(9) . ? C114 Cl1 1.752(6) . ? C115 C116 1.393(8) . ? C121 C122 1.410(8) . ? C121 C126 1.424(8) . ? C122 C123 1.385(8) . ? C123 C124 1.397(8) . ? C124 C125 1.383(9) . ? C124 Cl2 1.760(6) . ? C125 C126 1.382(8) . ? C131 C136 1.399(9) . ? C131 C132 1.403(9) . ? C132 C133 1.393(10) . ? C133 C134 1.391(9) . ? C134 C135 1.380(9) . ? C134 Cl3 1.762(7) . ? C135 C136 1.386(9) . ? C41 C42 1.485(14) . ? C42 C43 1.530(12) . ? C43 C44 1.509(12) . ? C44 C45 1.579(13) . ? C45 C46 1.455(14) . ? C46 C47 1.514(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C40 Rh10 C11 101.8(2) . . ? C40 Rh10 C10 95.2(3) . . ? C11 Rh10 C10 157.4(2) . . ? C40 Rh10 P 87.8(2) . . ? C11 Rh10 P 97.17(17) . . ? C10 Rh10 P 98.24(17) . . ? C40 Rh10 Rh31 93.55(18) . . ? C11 Rh10 Rh31 52.95(16) . . ? C10 Rh10 Rh31 111.71(17) . . ? P Rh10 Rh31 149.73(4) . . ? C40 Rh10 Rh21 149.08(18) . . ? C11 Rh10 Rh21 50.77(16) . . ? C10 Rh10 Rh21 108.40(17) . . ? P Rh10 Rh21 107.61(4) . . ? Rh31 Rh10 Rh21 59.610(17) . . ? C40 Rh10 Rh20 142.6(2) . . ? C11 Rh10 Rh20 108.76(16) . . ? C10 Rh10 Rh20 50.31(17) . . ? P Rh10 Rh20 108.65(4) . . ? Rh31 Rh10 Rh20 88.263(19) . . ? Rh21 Rh10 Rh20 58.230(16) . . ? C40 Rh10 Rh30 90.1(2) . . ? C11 Rh10 Rh30 111.60(17) . . ? C10 Rh10 Rh30 53.11(17) . . ? P Rh10 Rh30 150.96(4) . . ? Rh31 Rh10 Rh30 59.315(18) . . ? Rh21 Rh10 Rh30 88.52(2) . . ? Rh20 Rh10 Rh30 59.123(17) . . ? C50 Rh20 C60 94.7(3) . . ? C50 Rh20 C20 96.3(2) . . ? C60 Rh20 C20 98.0(3) . . ? C50 Rh20 C10 99.6(2) . . ? C60 Rh20 C10 95.9(3) . . ? C20 Rh20 C10 157.9(2) . . ? C50 Rh20 Rh21 94.78(19) . . ? C60 Rh20 Rh21 150.6(2) . . ? C20 Rh20 Rh21 53.31(17) . . ? C10 Rh20 Rh21 109.78(16) . . ? C50 Rh20 Rh30 152.66(18) . . ? C60 Rh20 Rh30 93.3(2) . . ? C20 Rh20 Rh30 108.43(17) . . ? C10 Rh20 Rh30 53.57(16) . . ? Rh21 Rh20 Rh30 90.873(19) . . ? C50 Rh20 Rh40 144.60(18) . . ? C60 Rh20 Rh40 97.0(2) . . ? C20 Rh20 Rh40 49.05(17) . . ? C10 Rh20 Rh40 112.26(16) . . ? Rh21 Rh20 Rh40 60.714(17) . . ? Rh30 Rh20 Rh40 59.484(18) . . ? C50 Rh20 Rh10 99.39(19) . . ? C60 Rh20 Rh10 143.8(2) . . ? C20 Rh20 Rh10 113.16(17) . . ? C10 Rh20 Rh10 49.05(16) . . ? Rh21 Rh20 Rh10 60.869(17) . . ? Rh30 Rh20 Rh10 60.527(17) . . ? Rh40 Rh20 Rh10 90.503(19) . . ? C61 Rh21 C51 91.3(3) . . ? C61 Rh21 C11 96.2(2) . . ? C51 Rh21 C11 108.1(2) . . ? C61 Rh21 C20 100.9(2) . . ? C51 Rh21 C20 89.8(3) . . ? C11 Rh21 C20 154.9(2) . . ? C61 Rh21 Rh20 150.92(19) . . ? C51 Rh21 Rh20 93.88(19) . . ? C11 Rh21 Rh20 109.15(16) . . ? C20 Rh21 Rh20 50.64(15) . . ? C61 Rh21 Rh31 94.80(19) . . ? C51 Rh21 Rh31 160.25(19) . . ? C11 Rh21 Rh31 52.54(16) . . ? C20 Rh21 Rh31 107.35(17) . . ? Rh20 Rh21 Rh31 89.83(2) . . ? C61 Rh21 Rh40 97.5(2) . . ? C51 Rh21 Rh40 138.44(19) . . ? C11 Rh21 Rh40 111.07(16) . . ? C20 Rh21 Rh40 48.65(16) . . ? Rh20 Rh21 Rh40 60.655(17) . . ? Rh31 Rh21 Rh40 59.174(17) . . ? C61 Rh21 Rh10 143.91(19) . . ? C51 Rh21 Rh10 105.66(19) . . ? C11 Rh21 Rh10 48.49(15) . . ? C20 Rh21 Rh10 110.58(16) . . ? Rh20 Rh21 Rh10 60.900(17) . . ? Rh31 Rh21 Rh10 59.661(17) . . ? Rh40 Rh21 Rh10 90.49(2) . . ? C70 Rh30 C80 91.1(3) . . ? C70 Rh30 C30 99.8(3) . . ? C80 Rh30 C30 100.1(3) . . ? C70 Rh30 C10 96.2(3) . . ? C80 Rh30 C10 98.1(3) . . ? C30 Rh30 C10 155.4(2) . . ? C70 Rh30 Rh40 150.6(2) . . ? C80 Rh30 Rh40 98.1(2) . . ? C30 Rh30 Rh40 51.17(18) . . ? C10 Rh30 Rh40 109.90(16) . . ? C70 Rh30 Rh31 100.4(2) . . ? C80 Rh30 Rh31 150.5(2) . . ? C30 Rh30 Rh31 51.29(19) . . ? C10 Rh30 Rh31 107.52(16) . . ? Rh40 Rh30 Rh31 59.658(17) . . ? C70 Rh30 Rh20 146.2(2) . . ? C80 Rh30 Rh20 96.3(2) . . ? C30 Rh30 Rh20 111.18(18) . . ? C10 Rh30 Rh20 50.11(16) . . ? Rh40 Rh30 Rh20 60.549(17) . . ? Rh31 Rh30 Rh20 89.19(2) . . ? C70 Rh30 Rh10 96.7(2) . . ? C80 Rh30 Rh10 146.2(2) . . ? C30 Rh30 Rh10 110.76(19) . . ? C10 Rh30 Rh10 48.47(16) . . ? Rh40 Rh30 Rh10 91.01(2) . . ? Rh31 Rh30 Rh10 59.703(17) . . ? Rh20 Rh30 Rh10 60.351(17) . . ? C71 Rh31 C81 92.9(3) . . ? C71 Rh31 C30 98.7(3) . . ? C81 Rh31 C30 97.6(3) . . ? C71 Rh31 C11 96.4(3) . . ? C81 Rh31 C11 99.8(3) . . ? C30 Rh31 C11 156.3(2) . . ? C71 Rh31 Rh40 149.5(2) . . ? C81 Rh31 Rh40 95.88(18) . . ? C30 Rh31 Rh40 51.23(18) . . ? C11 Rh31 Rh40 110.65(15) . . ? C71 Rh31 Rh30 98.7(2) . . ? C81 Rh31 Rh30 147.3(2) . . ? C30 Rh31 Rh30 50.65(18) . . ? C11 Rh31 Rh30 109.04(15) . . ? Rh40 Rh31 Rh30 60.048(17) . . ? C71 Rh31 Rh21 146.8(2) . . ? C81 Rh31 Rh21 96.7(2) . . ? C30 Rh31 Rh21 111.36(18) . . ? C11 Rh31 Rh21 50.61(15) . . ? Rh40 Rh31 Rh21 60.683(18) . . ? Rh30 Rh31 Rh21 90.102(19) . . ? C71 Rh31 Rh10 95.8(2) . . ? C81 Rh31 Rh10 148.0(2) . . ? C30 Rh31 Rh10 111.40(18) . . ? C11 Rh31 Rh10 48.68(15) . . ? Rh40 Rh31 Rh10 92.003(19) . . ? Rh30 Rh31 Rh10 60.983(17) . . ? Rh21 Rh31 Rh10 60.729(17) . . ? C91 Rh40 C90 93.8(3) . . ? C91 Rh40 C20 97.5(2) . . ? C90 Rh40 C20 97.3(3) . . ? C91 Rh40 C30 98.5(3) . . ? C90 Rh40 C30 96.5(3) . . ? C20 Rh40 C30 158.1(3) . . ? C91 Rh40 Rh31 95.05(17) . . ? C90 Rh40 Rh31 147.8(2) . . ? C20 Rh40 Rh31 112.14(18) . . ? C30 Rh40 Rh31 51.52(19) . . ? C91 Rh40 Rh30 148.01(17) . . ? C90 Rh40 Rh30 98.1(2) . . ? C20 Rh40 Rh30 110.19(17) . . ? C30 Rh40 Rh30 50.81(19) . . ? Rh31 Rh40 Rh30 60.294(17) . . ? C91 Rh40 Rh20 146.02(19) . . ? C90 Rh40 Rh20 100.4(2) . . ? C20 Rh40 Rh20 50.34(16) . . ? C30 Rh40 Rh20 110.25(19) . . ? Rh31 Rh40 Rh20 89.22(2) . . ? Rh30 Rh40 Rh20 59.967(17) . . ? C91 Rh40 Rh21 94.74(19) . . ? C90 Rh40 Rh21 149.5(2) . . ? C20 Rh40 Rh21 52.51(17) . . ? C30 Rh40 Rh21 111.10(19) . . ? Rh31 Rh40 Rh21 60.142(18) . . ? Rh30 Rh40 Rh21 89.93(2) . . ? Rh20 Rh40 Rh21 58.632(17) . . ? O10 C10 Rh10 137.2(5) . . ? O10 C10 Rh20 132.3(5) . . ? Rh10 C10 Rh20 80.6(2) . . ? O10 C10 Rh30 129.1(5) . . ? Rh10 C10 Rh30 78.4(2) . . ? Rh20 C10 Rh30 76.3(2) . . ? O11 C11 Rh10 136.2(5) . . ? O11 C11 Rh21 132.8(5) . . ? Rh10 C11 Rh21 80.7(2) . . ? O11 C11 Rh31 129.3(4) . . ? Rh10 C11 Rh31 78.4(2) . . ? Rh21 C11 Rh31 76.8(2) . . ? O20 C20 Rh40 135.2(5) . . ? O20 C20 Rh20 132.2(4) . . ? Rh40 C20 Rh20 80.6(2) . . ? O20 C20 Rh21 131.5(5) . . ? Rh40 C20 Rh21 78.8(2) . . ? Rh20 C20 Rh21 76.1(2) . . ? O30 C30 Rh30 133.1(5) . . ? O30 C30 Rh40 134.2(6) . . ? Rh30 C30 Rh40 78.0(2) . . ? O30 C30 Rh31 133.3(5) . . ? Rh30 C30 Rh31 78.1(3) . . ? Rh40 C30 Rh31 77.2(2) . . ? O40 C40 Rh10 177.8(6) . . ? O50 C50 Rh20 177.3(6) . . ? O51 C51 Rh21 171.0(6) . . ? O60 C60 Rh20 177.5(7) . . ? O61 C61 Rh21 177.5(6) . . ? O70 C70 Rh30 175.6(7) . . ? O71 C71 Rh31 179.1(8) . . ? O80 C80 Rh30 179.2(7) . . ? O81 C81 Rh31 177.6(6) . . ? O90 C90 Rh40 176.5(7) . . ? O91 C91 Rh40 178.1(6) . . ? C131 P C111 108.0(3) . . ? C131 P C121 97.9(3) . . ? C111 P C121 101.7(3) . . ? C131 P Rh10 122.1(2) . . ? C111 P Rh10 109.4(2) . . ? C121 P Rh10 115.60(19) . . ? C112 C111 C116 118.8(5) . . ? C112 C111 P 117.6(4) . . ? C116 C111 P 123.2(4) . . ? C113 C112 C111 121.0(6) . . ? C114 C113 C112 119.1(6) . . ? C115 C114 C113 120.9(6) . . ? C115 C114 Cl1 120.2(5) . . ? C113 C114 Cl1 118.9(5) . . ? C114 C115 C116 120.6(6) . . ? C115 C116 C111 119.5(6) . . ? C122 C121 C126 117.1(5) . . ? C122 C121 P 120.0(4) . . ? C126 C121 P 122.7(4) . . ? C123 C122 C121 122.4(5) . . ? C122 C123 C124 118.4(6) . . ? C125 C124 C123 121.2(6) . . ? C125 C124 Cl2 120.0(5) . . ? C123 C124 Cl2 118.8(5) . . ? C126 C125 C124 120.2(5) . . ? C125 C126 C121 120.6(6) . . ? C136 C131 C132 116.6(6) . . ? C136 C131 P 117.7(5) . . ? C132 C131 P 125.6(5) . . ? C133 C132 C131 122.3(6) . . ? C134 C133 C132 118.7(6) . . ? C135 C134 C133 120.8(6) . . ? C135 C134 Cl3 120.0(5) . . ? C133 C134 Cl3 119.2(6) . . ? C134 C135 C136 119.5(6) . . ? C135 C136 C131 122.2(6) . . ? C41 C42 C43 110.5(9) . . ? C44 C43 C42 114.1(8) . . ? C43 C44 C45 113.9(8) . . ? C46 C45 C44 117.5(10) . . ? C45 C46 C47 115.8(11) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.16 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.878 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.147 #======END data_s9762 _database_code_CSD 163532 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '4 Rh6(CO)15(P(4-FC6H4)3)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H12 F3 O15 P Rh6' _chemical_formula_weight 1353.86 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 10.4639(16) _cell_length_b 16.376(3) _cell_length_c 11.9344(16) _cell_angle_alpha 90.00 _cell_angle_beta 112.986(10) _cell_angle_gamma 90.00 _cell_volume 1882.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 54 _cell_measurement_theta_min 5.26 _cell_measurement_theta_max 11.00 _exptl_crystal_description 'block' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.388 _exptl_crystal_density_method none _exptl_crystal_F_000 1284 _exptl_absorpt_coefficient_mu 2.696 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.638 _exptl_absorpt_correction_T_max 0.819 _exptl_absorpt_process_details 'SHELXTL' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'less than 1.0' _diffrn_reflns_number 4453 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4231 _reflns_number_gt 3357 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0132P)^2^+7.6126P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4231 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0740 _refine_ls_wR_factor_gt 0.0684 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _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 Rh10 Rh 1.08112(5) -0.2500 -0.28045(5) 0.01389(12) Uani 1 2 d S . . Rh21 Rh 1.33351(4) -0.16681(2) -0.24000(3) 0.01531(9) Uani 1 1 d . . . Rh31 Rh 1.11879(4) -0.16569(3) -0.46887(3) 0.01736(10) Uani 1 1 d . . . Rh40 Rh 1.35952(6) -0.2500 -0.43313(5) 0.01717(13) Uani 1 2 d S . . C11 C 1.1258(5) -0.1228(3) -0.2778(5) 0.0202(10) Uani 1 1 d . . . O11 O 1.0855(4) -0.0607(2) -0.2553(4) 0.0256(8) Uani 1 1 d . . . C20 C 1.4981(7) -0.2500 -0.2466(6) 0.0191(15) Uani 1 2 d S . . O20 O 1.6207(6) -0.2500 -0.1944(5) 0.0281(13) Uani 1 2 d S . . C30 C 1.1610(8) -0.2500 -0.5899(7) 0.0230(16) Uani 1 2 d S . . O30 O 1.1282(6) -0.2500 -0.6968(5) 0.0296(13) Uani 1 2 d S . . C40 C 0.8886(8) -0.2500 -0.3656(7) 0.0232(16) Uani 1 2 d S . . O40 O 0.7714(6) -0.2500 -0.4189(6) 0.0348(14) Uani 1 2 d S . . C51 C 1.4372(6) -0.1547(4) -0.0680(5) 0.0254(12) Uani 1 1 d . . . O51 O 1.5149(5) -0.1465(3) 0.0287(4) 0.0418(12) Uani 1 1 d . . . C61 C 1.3926(6) -0.0611(4) -0.2702(5) 0.0254(12) Uani 1 1 d . . . O61 O 1.4227(5) 0.0017(3) -0.2895(5) 0.0432(12) Uani 1 1 d . . . C71 C 0.9267(6) -0.1482(4) -0.5660(5) 0.0302(13) Uani 1 1 d . . . O71 O 0.8150(5) -0.1360(3) -0.6280(5) 0.0518(14) Uani 1 1 d . . . C81 C 1.1696(6) -0.0678(4) -0.5272(5) 0.0276(12) Uani 1 1 d . . . O81 O 1.1985(5) -0.0110(3) -0.5667(5) 0.0460(12) Uani 1 1 d . . . C91 C 1.4542(6) -0.1626(4) -0.4763(5) 0.0267(12) Uani 1 1 d . . . O91 O 1.5107(5) -0.1096(3) -0.4967(5) 0.0448(12) Uani 1 1 d . . . P P 1.04144(18) -0.2500 -0.09917(16) 0.0139(3) Uani 1 2 d S . . C21 C 0.9386(5) -0.1641(3) -0.0801(5) 0.0193(10) Uani 1 1 d . . . C22 C 0.9327(7) -0.1511(4) 0.0335(5) 0.0318(13) Uani 1 1 d . . . H22A H 0.9919 -0.1825 0.1020 0.038 Uiso 1 1 d R . . C23 C 0.8420(7) -0.0941(4) 0.0489(6) 0.0375(15) Uani 1 1 d . . . H23A H 0.8374 -0.0852 0.1267 0.045 Uiso 1 1 d R . . C24 C 0.7593(6) -0.0507(3) -0.0511(6) 0.0280(13) Uani 1 1 d . . . C25 C 0.7649(6) -0.0580(3) -0.1633(5) 0.0266(12) Uani 1 1 d . . . H25A H 0.7070 -0.0249 -0.2303 0.032 Uiso 1 1 d R . . C26 C 0.8567(5) -0.1160(3) -0.1776(5) 0.0222(11) Uani 1 1 d . . . H26A H 0.8638 -0.1224 -0.2549 0.027 Uiso 1 1 d R . . F2 F 0.6654(4) 0.0027(2) -0.0378(4) 0.0398(9) Uani 1 1 d . . . C31 C 1.1934(7) -0.2500 0.0422(6) 0.0196(15) Uani 1 2 d S . . C32 C 1.2534(6) -0.1770(4) 0.0968(5) 0.0328(14) Uani 1 1 d . . . H32A H 1.2102 -0.1261 0.0626 0.039 Uiso 1 1 d R . . C33 C 1.3729(6) -0.1767(4) 0.2009(6) 0.0370(15) Uani 1 1 d . . . H33A H 1.4146 -0.1266 0.2399 0.044 Uiso 1 1 d R . . C34 C 1.4322(8) -0.2500 0.2487(7) 0.032(2) Uani 1 2 d S . . F3 F 1.5541(5) -0.2500 0.3502(4) 0.0466(16) Uani 1 2 d S . . 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 Rh10 0.0131(2) 0.0153(3) 0.0128(3) 0.000 0.0044(2) 0.000 Rh21 0.01520(18) 0.01361(19) 0.01685(19) -0.00103(15) 0.00595(15) -0.00120(14) Rh31 0.01741(19) 0.0182(2) 0.01567(19) 0.00379(15) 0.00565(15) 0.00208(15) Rh40 0.0182(3) 0.0179(3) 0.0176(3) 0.000 0.0095(2) 0.000 C11 0.023(2) 0.015(2) 0.024(3) 0.002(2) 0.010(2) -0.004(2) O11 0.026(2) 0.0160(19) 0.036(2) -0.0037(16) 0.0144(18) 0.0020(16) C20 0.018(3) 0.029(4) 0.014(3) 0.000 0.010(3) 0.000 O20 0.021(3) 0.031(3) 0.033(3) 0.000 0.011(2) 0.000 C30 0.022(4) 0.025(4) 0.020(4) 0.000 0.006(3) 0.000 O30 0.035(3) 0.038(3) 0.013(3) 0.000 0.006(2) 0.000 C40 0.024(4) 0.033(4) 0.014(3) 0.000 0.010(3) 0.000 O40 0.016(3) 0.056(4) 0.031(3) 0.000 0.007(2) 0.000 C51 0.027(3) 0.026(3) 0.025(3) -0.003(2) 0.012(2) 0.000(2) O51 0.033(2) 0.061(3) 0.025(2) -0.009(2) 0.005(2) -0.001(2) C61 0.022(3) 0.024(3) 0.029(3) 0.005(2) 0.008(2) -0.001(2) O61 0.040(3) 0.023(2) 0.053(3) 0.008(2) 0.004(2) -0.010(2) C71 0.029(3) 0.030(3) 0.031(3) 0.009(3) 0.011(3) 0.005(2) O71 0.030(2) 0.060(3) 0.052(3) 0.017(3) 0.000(2) 0.010(2) C81 0.028(3) 0.030(3) 0.025(3) 0.005(2) 0.010(2) 0.004(2) O81 0.047(3) 0.037(3) 0.050(3) 0.022(2) 0.014(2) -0.002(2) C91 0.030(3) 0.032(3) 0.023(3) 0.001(2) 0.016(2) 0.003(3) O91 0.049(3) 0.036(3) 0.061(3) 0.002(2) 0.033(2) -0.015(2) P 0.0156(8) 0.0139(8) 0.0130(8) 0.000 0.0065(7) 0.000 C21 0.020(2) 0.016(2) 0.022(2) 0.000(2) 0.008(2) 0.000(2) C22 0.046(4) 0.029(3) 0.025(3) 0.002(2) 0.018(3) 0.012(3) C23 0.052(4) 0.033(3) 0.033(3) 0.000(3) 0.023(3) 0.012(3) C24 0.030(3) 0.016(3) 0.045(4) -0.004(2) 0.023(3) -0.002(2) C25 0.026(3) 0.021(3) 0.035(3) 0.003(2) 0.013(2) 0.005(2) C26 0.024(3) 0.021(3) 0.025(3) 0.006(2) 0.012(2) 0.002(2) F2 0.047(2) 0.0246(18) 0.059(3) -0.0001(18) 0.034(2) 0.0110(16) C31 0.012(3) 0.032(4) 0.015(3) 0.000 0.005(3) 0.000 C32 0.036(3) 0.032(3) 0.025(3) 0.007(3) 0.006(3) -0.013(3) C33 0.031(3) 0.045(4) 0.030(3) 0.000(3) 0.007(3) -0.023(3) C34 0.014(3) 0.066(6) 0.015(4) 0.000 0.006(3) 0.000 F3 0.018(2) 0.094(5) 0.018(2) 0.000 -0.004(2) 0.000 _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 Rh10 C40 1.869(8) . ? Rh10 C11 2.133(5) . ? Rh10 C11 2.133(5) 4 ? Rh10 P 2.3568(18) . ? Rh10 Rh31 2.7948(7) 4 ? Rh10 Rh31 2.7948(7) . ? Rh10 Rh21 2.8405(7) . ? Rh10 Rh21 2.8405(7) 4 ? Rh21 C61 1.919(6) . ? Rh21 C51 1.921(6) . ? Rh21 C11 2.164(5) . ? Rh21 C20 2.221(5) . ? Rh21 Rh21 2.7248(9) 4 ? Rh21 Rh31 2.7778(7) . ? Rh21 Rh40 2.7808(7) . ? Rh31 C81 1.904(6) . ? Rh31 C71 1.909(6) . ? Rh31 C30 2.165(6) . ? Rh31 C11 2.360(5) . ? Rh31 Rh40 2.7557(7) . ? Rh31 Rh31 2.7614(9) 4 ? Rh40 C91 1.923(6) . ? Rh40 C91 1.923(6) 4 ? Rh40 C20 2.130(7) . ? Rh40 C30 2.187(8) . ? Rh40 Rh31 2.7557(7) 4 ? Rh40 Rh21 2.7808(7) 4 ? C11 O11 1.172(6) . ? C20 O20 1.188(9) . ? C20 Rh21 2.221(5) 4 ? C30 O30 1.184(9) . ? C30 Rh31 2.165(6) 4 ? C40 O40 1.140(9) . ? C51 O51 1.131(7) . ? C61 O61 1.125(7) . ? C71 O71 1.131(7) . ? C81 O81 1.136(7) . ? C91 O91 1.129(7) . ? P C31 1.811(7) . ? P C21 1.839(5) 4 ? P C21 1.839(5) . ? C21 C26 1.389(7) . ? C21 C22 1.397(7) . ? C22 C23 1.394(8) . ? C23 C24 1.367(9) . ? C24 C25 1.368(8) . ? C24 F2 1.370(6) . ? C25 C26 1.408(7) . ? C31 C32 1.389(7) . ? C31 C32 1.389(7) 4 ? C32 C33 1.376(8) . ? C33 C34 1.370(8) . ? C34 C33 1.370(8) 4 ? C34 F3 1.374(9) . ? 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 C40 Rh10 C11 101.05(14) . . ? C40 Rh10 C11 101.05(14) . 4 ? C11 Rh10 C11 155.3(3) . 4 ? C40 Rh10 P 87.7(2) . . ? C11 Rh10 P 95.89(14) . . ? C11 Rh10 P 95.89(14) 4 . ? C40 Rh10 Rh31 91.34(19) . 4 ? C11 Rh10 Rh31 113.30(14) . 4 ? C11 Rh10 Rh31 55.28(14) 4 4 ? P Rh10 Rh31 150.385(12) . 4 ? C40 Rh10 Rh31 91.34(19) . . ? C11 Rh10 Rh31 55.28(14) . . ? C11 Rh10 Rh31 113.30(14) 4 . ? P Rh10 Rh31 150.385(12) . . ? Rh31 Rh10 Rh31 59.21(2) 4 . ? C40 Rh10 Rh21 145.67(12) . . ? C11 Rh10 Rh21 49.08(14) . . ? C11 Rh10 Rh21 106.39(14) 4 . ? P Rh10 Rh21 109.23(4) . . ? Rh31 Rh10 Rh21 87.70(2) 4 . ? Rh31 Rh10 Rh21 59.060(17) . . ? C40 Rh10 Rh21 145.67(12) . 4 ? C11 Rh10 Rh21 106.39(14) . 4 ? C11 Rh10 Rh21 49.08(14) 4 4 ? P Rh10 Rh21 109.23(4) . 4 ? Rh31 Rh10 Rh21 59.060(17) 4 4 ? Rh31 Rh10 Rh21 87.70(2) . 4 ? Rh21 Rh10 Rh21 57.32(2) . 4 ? C61 Rh21 C51 91.1(2) . . ? C61 Rh21 C11 91.8(2) . . ? C51 Rh21 C11 106.9(2) . . ? C61 Rh21 C20 103.6(2) . . ? C51 Rh21 C20 88.8(2) . . ? C11 Rh21 C20 157.9(2) . . ? C61 Rh21 Rh21 154.42(17) . 4 ? C51 Rh21 Rh21 95.92(18) . 4 ? C11 Rh21 Rh21 109.46(13) . 4 ? C20 Rh21 Rh21 52.16(11) . 4 ? C61 Rh21 Rh31 90.33(17) . . ? C51 Rh21 Rh31 162.25(16) . . ? C11 Rh21 Rh31 55.38(14) . . ? C20 Rh21 Rh31 108.05(18) . . ? Rh21 Rh21 Rh31 90.378(13) 4 . ? C61 Rh21 Rh40 98.23(18) . . ? C51 Rh21 Rh40 137.65(17) . . ? C11 Rh21 Rh40 113.95(14) . . ? C20 Rh21 Rh40 48.85(18) . . ? Rh21 Rh21 Rh40 60.663(11) 4 . ? Rh31 Rh21 Rh40 59.440(18) . . ? C61 Rh21 Rh10 138.35(16) . . ? C51 Rh21 Rh10 109.30(17) . . ? C11 Rh21 Rh10 48.14(13) . . ? C20 Rh21 Rh10 112.46(12) . . ? Rh21 Rh21 Rh10 61.338(11) 4 . ? Rh31 Rh21 Rh10 59.650(18) . . ? Rh40 Rh21 Rh10 90.55(2) . . ? C81 Rh31 C71 91.7(2) . . ? C81 Rh31 C30 97.7(2) . . ? C71 Rh31 C30 97.5(3) . . ? C81 Rh31 C11 101.2(2) . . ? C71 Rh31 C11 99.8(2) . . ? C30 Rh31 C11 153.8(2) . . ? C81 Rh31 Rh40 96.29(17) . . ? C71 Rh31 Rh40 148.32(19) . . ? C30 Rh31 Rh40 51.1(2) . . ? C11 Rh31 Rh40 108.54(13) . . ? C81 Rh31 Rh31 147.33(18) . 4 ? C71 Rh31 Rh31 98.63(19) . 4 ? C30 Rh31 Rh31 50.38(14) . 4 ? C11 Rh31 Rh31 107.32(12) . 4 ? Rh40 Rh31 Rh31 59.931(12) . 4 ? C81 Rh31 Rh21 97.52(17) . . ? C71 Rh31 Rh21 148.58(19) . . ? C30 Rh31 Rh21 110.77(19) . . ? C11 Rh31 Rh21 48.98(13) . . ? Rh40 Rh31 Rh21 60.335(19) . . ? Rh31 Rh31 Rh21 89.622(13) 4 . ? C81 Rh31 Rh10 149.01(18) . . ? C71 Rh31 Rh10 96.71(18) . . ? C30 Rh31 Rh10 110.58(14) . . ? C11 Rh31 Rh10 47.97(12) . . ? Rh40 Rh31 Rh10 92.04(2) . . ? Rh31 Rh31 Rh10 60.394(12) 4 . ? Rh21 Rh31 Rh10 61.290(18) . . ? C91 Rh40 C91 96.2(3) . 4 ? C91 Rh40 C20 93.9(2) . . ? C91 Rh40 C20 93.9(2) 4 . ? C91 Rh40 C30 100.8(2) . . ? C91 Rh40 C30 100.8(2) 4 . ? C20 Rh40 C30 157.8(3) . . ? C91 Rh40 Rh31 150.15(17) . 4 ? C91 Rh40 Rh31 96.96(17) 4 4 ? C20 Rh40 Rh31 111.69(16) . 4 ? C30 Rh40 Rh31 50.36(16) . 4 ? C91 Rh40 Rh31 96.96(17) . . ? C91 Rh40 Rh31 150.15(17) 4 . ? C20 Rh40 Rh31 111.69(16) . . ? C30 Rh40 Rh31 50.36(16) . . ? Rh31 Rh40 Rh31 60.14(2) 4 . ? C91 Rh40 Rh21 94.87(17) . . ? C91 Rh40 Rh21 144.54(17) 4 . ? C20 Rh40 Rh21 51.73(14) . . ? C30 Rh40 Rh21 109.97(18) . . ? Rh31 Rh40 Rh21 89.68(2) 4 . ? Rh31 Rh40 Rh21 60.226(17) . . ? C91 Rh40 Rh21 144.54(17) . 4 ? C91 Rh40 Rh21 94.87(17) 4 4 ? C20 Rh40 Rh21 51.73(14) . 4 ? C30 Rh40 Rh21 109.97(18) . 4 ? Rh31 Rh40 Rh21 60.226(17) 4 4 ? Rh31 Rh40 Rh21 89.68(2) . 4 ? Rh21 Rh40 Rh21 58.67(2) . 4 ? O11 C11 Rh10 139.0(4) . . ? O11 C11 Rh21 131.6(4) . . ? Rh10 C11 Rh21 82.78(19) . . ? O11 C11 Rh31 127.0(4) . . ? Rh10 C11 Rh31 76.76(17) . . ? Rh21 C11 Rh31 75.63(17) . . ? O20 C20 Rh40 134.7(6) . . ? O20 C20 Rh21 132.5(3) . 4 ? Rh40 C20 Rh21 79.4(2) . 4 ? O20 C20 Rh21 132.5(3) . . ? Rh40 C20 Rh21 79.4(2) . . ? Rh21 C20 Rh21 75.7(2) 4 . ? O30 C30 Rh31 132.1(3) . . ? O30 C30 Rh31 132.1(3) . 4 ? Rh31 C30 Rh31 79.2(3) . 4 ? O30 C30 Rh40 134.5(6) . . ? Rh31 C30 Rh40 78.6(2) . . ? Rh31 C30 Rh40 78.6(2) 4 . ? O40 C40 Rh10 179.1(7) . . ? O51 C51 Rh21 169.7(5) . . ? O61 C61 Rh21 177.6(5) . . ? O71 C71 Rh31 176.4(6) . . ? O81 C81 Rh31 177.0(6) . . ? O91 C91 Rh40 176.8(5) . . ? C31 P C21 103.2(2) . 4 ? C31 P C21 103.2(2) . . ? C21 P C21 99.9(3) 4 . ? C31 P Rh10 116.7(2) . . ? C21 P Rh10 115.79(17) 4 . ? C21 P Rh10 115.79(17) . . ? C26 C21 C22 118.7(5) . . ? C26 C21 P 122.0(4) . . ? C22 C21 P 119.1(4) . . ? C23 C22 C21 121.4(6) . . ? C24 C23 C22 117.7(6) . . ? C23 C24 C25 123.7(5) . . ? C23 C24 F2 117.9(5) . . ? C25 C24 F2 118.4(5) . . ? C24 C25 C26 118.0(5) . . ? C21 C26 C25 120.5(5) . . ? C32 C31 C32 118.8(7) . 4 ? C32 C31 P 120.6(4) . . ? C32 C31 P 120.6(4) 4 . ? C33 C32 C31 120.8(6) . . ? C34 C33 C32 118.5(6) . . ? C33 C34 C33 122.5(7) . 4 ? C33 C34 F3 118.7(4) . . ? C33 C34 F3 118.7(4) 4 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.843 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.145 #======END data_k98176 _database_code_CSD 163533 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '5 Rh6(CO)15(P(4-OMeC6H4)3)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H35 O18 P Rh6' _chemical_formula_weight 1476.13 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' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6763(3) _cell_length_b 13.3834(6) _cell_length_c 18.6774(8) _cell_angle_alpha 93.056(2) _cell_angle_beta 97.363(2) _cell_angle_gamma 96.616(3) _cell_volume 2377.14(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 9085 _cell_measurement_theta_min 4.1 _cell_measurement_theta_max 26.42 _exptl_crystal_description needle _exptl_crystal_colour purple _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 2.140 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7124 _exptl_absorpt_correction_T_max 0.8823 _exptl_absorpt_process_details 'Denzo-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _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 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 40694 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 26.42 _reflns_number_total 9085 _reflns_number_gt 5956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'Bruker SHELXTL V5.1' _computing_structure_refinement 'Bruker SHELXTL V5.1' _computing_molecular_graphics 'Bruker SHELXTL V5.1' _computing_publication_material 'Bruker SHELXTL V5.1' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0596P)^2^] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9085 _refine_ls_number_parameters 651 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0780 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.003 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 Rh10 Rh 1.03708(5) -0.28604(4) -0.30389(3) 0.02358(13) Uani 1 1 d . A . Rh20 Rh 1.30656(5) -0.32733(4) -0.32632(3) 0.02510(14) Uani 1 1 d . . . Rh21 Rh 1.27511(5) -0.14310(4) -0.26600(3) 0.02603(14) Uani 1 1 d . . . Rh30 Rh 1.10845(5) -0.30237(4) -0.44298(3) 0.02538(14) Uani 1 1 d . . . Rh31 Rh 1.07876(5) -0.11606(4) -0.38270(3) 0.02642(14) Uani 1 1 d . . . Rh40 Rh 1.34117(5) -0.16106(4) -0.40599(3) 0.02680(14) Uani 1 1 d . . . C10 C 1.1023(7) -0.4162(5) -0.3555(4) 0.0294(15) Uani 1 1 d . . . O10 O 1.0659(5) -0.5019(4) -0.3627(3) 0.0327(11) Uani 1 1 d . . . C11 C 1.0507(7) -0.1323(5) -0.2635(4) 0.0299(15) Uani 1 1 d . . . O11 O 0.9924(5) -0.0845(4) -0.2268(3) 0.0358(11) Uani 1 1 d . . . C20 C 1.4621(7) -0.1879(5) -0.3056(4) 0.0308(16) Uani 1 1 d . . . O20 O 1.5798(5) -0.1744(4) -0.2827(3) 0.0381(12) Uani 1 1 d . . . C30 C 1.1516(7) -0.1548(5) -0.4844(4) 0.0354(17) Uani 1 1 d . . . O30 O 1.1375(5) -0.1242(4) -0.5408(3) 0.0388(12) Uani 1 1 d . . . C40 C 0.8451(7) -0.3009(5) -0.3393(4) 0.0285(15) Uani 1 1 d . . . O40 O 0.7308(5) -0.3073(4) -0.3631(3) 0.0392(12) Uani 1 1 d . . . C50 C 1.3869(7) -0.3735(5) -0.2373(4) 0.0357(17) Uani 1 1 d . . . O50 O 1.4477(5) -0.3944(4) -0.1860(3) 0.0480(14) Uani 1 1 d . . . C51 C 1.3329(7) -0.1690(5) -0.1686(4) 0.0365(17) Uani 1 1 d . . . O51 O 1.3756(5) -0.1809(4) -0.1111(3) 0.0507(15) Uani 1 1 d . . . C60 C 1.4046(7) -0.4139(5) -0.3814(4) 0.0333(16) Uani 1 1 d . . . O60 O 1.4600(5) -0.4655(4) -0.4146(3) 0.0466(14) Uani 1 1 d . . . C61 C 1.3241(7) -0.0014(6) -0.2477(4) 0.0414(19) Uani 1 1 d . . . O61 O 1.3478(7) 0.0841(4) -0.2369(4) 0.0664(18) Uani 1 1 d . . . C70 C 0.9221(7) -0.3313(5) -0.4939(4) 0.0340(16) Uani 1 1 d . . . O70 O 0.8151(5) -0.3452(4) -0.5259(3) 0.0490(14) Uani 1 1 d . . . C71 C 0.8841(7) -0.1087(5) -0.4173(4) 0.0355(17) Uani 1 1 d . . . O71 O 0.7711(5) -0.1020(4) -0.4379(3) 0.0509(15) Uani 1 1 d . . . C80 C 1.1835(7) -0.3868(5) -0.5090(4) 0.0334(16) Uani 1 1 d . . . O80 O 1.2299(5) -0.4371(4) -0.5478(3) 0.0475(14) Uani 1 1 d . . . C81 C 1.1266(7) 0.0244(6) -0.3846(4) 0.0351(17) Uani 1 1 d . . . O81 O 1.1592(5) 0.1080(4) -0.3895(3) 0.0548(16) Uani 1 1 d . . . C90 C 1.4494(7) -0.2198(6) -0.4706(4) 0.0384(18) Uani 1 1 d . . . O90 O 1.5113(6) -0.2574(4) -0.5103(3) 0.0493(14) Uani 1 1 d . . . C91 C 1.4290(7) -0.0276(6) -0.4118(4) 0.0368(17) Uani 1 1 d . . . O91 O 1.4830(6) 0.0510(4) -0.4154(3) 0.0613(17) Uani 1 1 d . . . P P 0.98208(17) -0.36523(13) -0.19884(9) 0.0263(4) Uani 1 1 d . . . C111 C 0.8282(6) -0.4617(5) -0.2152(4) 0.0279(15) Uani 1 1 d . A . C112 C 0.7643(8) -0.4938(6) -0.1565(4) 0.0391(18) Uani 1 1 d . . . H11A H 0.8012 -0.4665 -0.1090 0.047 Uiso 1 1 calc R A . C113 C 0.6480(8) -0.5650(6) -0.1668(4) 0.0431(19) Uani 1 1 d . A . H11B H 0.6065 -0.5877 -0.1263 0.052 Uiso 1 1 calc R . . C114 C 0.5909(7) -0.6036(5) -0.2355(4) 0.0348(17) Uani 1 1 d . . . C115 C 0.6567(7) -0.5773(5) -0.2938(4) 0.0373(17) Uani 1 1 d . A . H11C H 0.6215 -0.6067 -0.3410 0.045 Uiso 1 1 calc R . . C116 C 0.7758(7) -0.5069(5) -0.2824(4) 0.0330(16) Uani 1 1 d . . . H11D H 0.8227 -0.4895 -0.3225 0.040 Uiso 1 1 calc R A . O1 O 0.4707(5) -0.6704(4) -0.2403(3) 0.0489(14) Uani 1 1 d . A . C1 C 0.4018(9) -0.7037(7) -0.3112(6) 0.072(3) Uani 1 1 d . . . H1A H 0.3115 -0.7433 -0.3076 0.108 Uiso 1 1 calc R A . H1B H 0.4608 -0.7455 -0.3356 0.108 Uiso 1 1 calc R . . H1C H 0.3858 -0.6450 -0.3390 0.108 Uiso 1 1 calc R . . C121 C 0.9386(10) -0.2679(7) -0.1350(5) 0.031(5) Uani 0.51 1 d PG A 1 C122 C 1.0342(7) -0.2129(8) -0.0813(5) 0.034(3) Uani 0.51 1 d PG A 1 H12A H 1.1302 -0.2237 -0.0761 0.041 Uiso 0.51 1 calc PR A 1 C123 C 0.9895(9) -0.1419(7) -0.0352(5) 0.037(3) Uani 0.51 1 d PG A 1 H12B H 1.0549 -0.1043 0.0015 0.045 Uiso 0.51 1 calc PR A 1 C124 C 0.8490(10) -0.1261(8) -0.0428(6) 0.043(4) Uani 0.51 1 d PG A 1 C125 C 0.7534(8) -0.1811(9) -0.0965(6) 0.039(4) Uani 0.51 1 d PG A 1 H12C H 0.6574 -0.1703 -0.1017 0.047 Uiso 0.51 1 calc PR A 1 C126 C 0.7981(10) -0.2521(8) -0.1426(5) 0.034(4) Uani 0.51 1 d PG A 1 H12D H 0.7327 -0.2897 -0.1793 0.041 Uiso 0.51 1 calc PR A 1 O2A O 0.7948(14) -0.0636(11) 0.0038(7) 0.051(4) Uani 0.51 1 d P A 1 C2A C 0.880(2) -0.0158(16) 0.0662(11) 0.075(7) Uani 0.51 1 d P A 1 H2AA H 0.8207 0.0134 0.0985 0.113 Uiso 0.51 1 calc PR A 1 H2AB H 0.9468 0.0377 0.0519 0.113 Uiso 0.51 1 calc PR A 1 H2AC H 0.9315 -0.0654 0.0914 0.113 Uiso 0.51 1 calc PR A 1 C221 C 0.9145(12) -0.2862(8) -0.1316(5) 0.015(4) Uiso 0.49 1 d PG A 2 C222 C 0.9560(10) -0.2858(7) -0.0576(5) 0.043(4) Uiso 0.49 1 d PG A 2 H22A H 1.0214 -0.3292 -0.0394 0.052 Uiso 0.49 1 calc PR A 2 C223 C 0.9018(11) -0.2220(8) -0.0101(4) 0.037(4) Uiso 0.49 1 d PG A 2 H22B H 0.9303 -0.2218 0.0406 0.045 Uiso 0.49 1 calc PR A 2 C224 C 0.8061(12) -0.1587(8) -0.0367(6) 0.043(5) Uiso 0.49 1 d PG A 2 C225 C 0.7646(11) -0.1591(8) -0.1107(6) 0.033(5) Uiso 0.49 1 d PG A 2 H22C H 0.6991 -0.1158 -0.1289 0.039 Uiso 0.49 1 calc PR A 2 C226 C 0.8187(12) -0.2229(9) -0.1582(4) 0.028(4) Uiso 0.49 1 d PG A 2 H22D H 0.7903 -0.2232 -0.2089 0.033 Uiso 0.49 1 calc PR A 2 O2B O 0.7434(16) -0.0901(13) 0.0023(10) 0.059(5) Uiso 0.49 1 d P A 2 C2B C 0.788(2) -0.0889(17) 0.0825(11) 0.074(6) Uiso 0.49 1 d P A 2 H2BA H 0.7558 -0.0308 0.1067 0.111 Uiso 0.49 1 calc PR A 2 H2BB H 0.8904 -0.0840 0.0923 0.111 Uiso 0.49 1 calc PR A 2 H2BC H 0.7463 -0.1512 0.1008 0.111 Uiso 0.49 1 calc PR A 2 C131 C 1.1090(10) -0.4391(8) -0.1476(6) 0.041(12) Uani 0.53 1 d PG A 1 C132 C 1.1556(12) -0.4254(7) -0.0738(6) 0.049(4) Uani 0.53 1 d PG A 1 H13A H 1.1296 -0.3708 -0.0459 0.059 Uiso 0.53 1 calc PR A 1 C133 C 1.2400(12) -0.4917(9) -0.0407(4) 0.049(4) Uani 0.53 1 d PG A 1 H13B H 1.2718 -0.4823 0.0098 0.059 Uiso 0.53 1 calc PR A 1 C134 C 1.2779(12) -0.5716(8) -0.0814(6) 0.050(8) Uani 0.53 1 d PG A 1 C135 C 1.2314(12) -0.5852(8) -0.1552(6) 0.036(4) Uani 0.53 1 d PG A 1 H13C H 1.2573 -0.6398 -0.1830 0.043 Uiso 0.53 1 calc PR A 1 C136 C 1.1469(11) -0.5190(9) -0.1883(4) 0.041(4) Uani 0.53 1 d PG A 1 H13D H 1.1151 -0.5283 -0.2387 0.049 Uiso 0.53 1 calc PR A 1 O3A O 1.3690(14) -0.6389(13) -0.0561(8) 0.038(4) Uani 0.53 1 d P A 1 C3A C 1.4132(17) -0.6289(16) 0.0233(9) 0.070(6) Uani 0.53 1 d P A 1 H3AA H 1.4818 -0.6756 0.0361 0.106 Uiso 0.53 1 calc PR A 1 H3AB H 1.3311 -0.6449 0.0482 0.106 Uiso 0.53 1 calc PR A 1 H3AC H 1.4558 -0.5596 0.0379 0.106 Uiso 0.53 1 calc PR A 1 C231 C 1.1088(10) -0.4398(8) -0.1526(6) 0.021(10) Uiso 0.47 1 d PG A 2 C232 C 1.2064(11) -0.3979(7) -0.0946(6) 0.033(4) Uiso 0.47 1 d PG A 2 H23A H 1.2102 -0.3287 -0.0793 0.040 Uiso 0.47 1 calc PR A 2 C233 C 1.2985(11) -0.4572(9) -0.0591(5) 0.038(4) Uiso 0.47 1 d PG A 2 H23B H 1.3652 -0.4285 -0.0194 0.046 Uiso 0.47 1 calc PR A 2 C234 C 1.2929(12) -0.5585(9) -0.0815(7) 0.034(7) Uiso 0.47 1 d PG A 2 C235 C 1.1953(14) -0.6004(7) -0.1395(7) 0.031(5) Uiso 0.47 1 d PG A 2 H23C H 1.1915 -0.6696 -0.1549 0.037 Uiso 0.47 1 calc PR A 2 C236 C 1.1032(11) -0.5411(9) -0.1751(6) 0.029(4) Uiso 0.47 1 d PG A 2 H23D H 1.0365 -0.5698 -0.2147 0.035 Uiso 0.47 1 calc PR A 2 O3B O 1.382(2) -0.6123(15) -0.0394(11) 0.046(6) Uiso 0.47 1 d P A 2 C3B C 1.371(2) -0.7181(17) -0.0610(11) 0.064(5) Uiso 0.47 1 d P A 2 H3BA H 1.4295 -0.7515 -0.0252 0.096 Uiso 0.47 1 calc PR A 2 H3BB H 1.4033 -0.7267 -0.1083 0.096 Uiso 0.47 1 calc PR A 2 H3BC H 1.2730 -0.7482 -0.0642 0.096 Uiso 0.47 1 calc PR A 2 C41A C 0.944(2) 0.1901(18) -0.2586(14) 0.099(8) Uiso 0.50 1 d PDU B 1 H41A H 0.9506 0.2190 -0.3053 0.149 Uiso 0.50 1 calc PR B 1 H41B H 1.0213 0.1502 -0.2471 0.149 Uiso 0.50 1 calc PR B 1 H41C H 0.9486 0.2446 -0.2208 0.149 Uiso 0.50 1 calc PR B 1 C42A C 0.793(3) 0.117(2) -0.2629(16) 0.133(11) Uiso 0.50 1 d PDU B 1 H42A H 0.7180 0.1329 -0.3003 0.160 Uiso 0.50 1 calc PR B 1 H42B H 0.8007 0.0440 -0.2633 0.160 Uiso 0.50 1 calc PR B 1 C43A C 0.795(5) 0.172(3) -0.1841(19) 0.221(18) Uiso 0.50 1 d PDU B 1 H43A H 0.8930 0.1900 -0.1605 0.265 Uiso 0.50 1 calc PR B 1 H43B H 0.7505 0.2351 -0.1885 0.265 Uiso 0.50 1 calc PR B 1 C44A C 0.718(6) 0.104(3) -0.141(2) 0.26(2) Uiso 0.50 1 d PDU B 1 H44A H 0.7740 0.0498 -0.1250 0.317 Uiso 0.50 1 calc PR B 1 H44B H 0.6281 0.0727 -0.1691 0.317 Uiso 0.50 1 calc PR B 1 C45A C 0.691(4) 0.172(3) -0.075(2) 0.193(17) Uiso 0.50 1 d PDU B 1 H45A H 0.6589 0.2368 -0.0892 0.232 Uiso 0.50 1 calc PR B 1 H45B H 0.7744 0.1855 -0.0372 0.232 Uiso 0.50 1 calc PR B 1 C46A C 0.572(7) 0.099(5) -0.051(3) 0.46(5) Uiso 0.50 1 d PDU B 1 H46A H 0.6130 0.0548 -0.0161 0.694 Uiso 0.50 1 calc PR B 1 H46B H 0.5224 0.0575 -0.0937 0.694 Uiso 0.50 1 calc PR B 1 H46C H 0.5067 0.1372 -0.0292 0.694 Uiso 0.50 1 calc PR B 1 C41B C 0.960(3) 0.262(2) -0.3089(14) 0.119(10) Uiso 0.50 1 d PDU C 2 H41D H 0.9422 0.2718 -0.3608 0.179 Uiso 0.50 1 calc PR C 2 H41E H 1.0525 0.2398 -0.2974 0.179 Uiso 0.50 1 calc PR C 2 H41F H 0.9569 0.3261 -0.2813 0.179 Uiso 0.50 1 calc PR C 2 C42B C 0.846(3) 0.182(3) -0.2888(16) 0.178(15) Uiso 0.50 1 d PDU C 2 H42C H 0.7505 0.1987 -0.3052 0.213 Uiso 0.50 1 calc PR C 2 H42D H 0.8552 0.1141 -0.3108 0.213 Uiso 0.50 1 calc PR C 2 C43B C 0.874(4) 0.184(3) -0.2054(17) 0.218(17) Uiso 0.50 1 d PDU C 2 H43C H 0.8636 0.2501 -0.1813 0.262 Uiso 0.50 1 calc PR C 2 H43D H 0.9650 0.1618 -0.1870 0.262 Uiso 0.50 1 calc PR C 2 C44B C 0.739(3) 0.098(2) -0.2031(16) 0.125(10) Uiso 0.50 1 d PDU C 2 H44C H 0.6674 0.0937 -0.2463 0.151 Uiso 0.50 1 calc PR C 2 H44D H 0.7653 0.0312 -0.1915 0.151 Uiso 0.50 1 calc PR C 2 C45B C 0.704(4) 0.163(2) -0.1370(18) 0.137(12) Uiso 0.50 1 d PDU C 2 H45C H 0.7926 0.1920 -0.1066 0.164 Uiso 0.50 1 calc PR C 2 H45D H 0.6540 0.2190 -0.1544 0.164 Uiso 0.50 1 calc PR C 2 C46B C 0.615(5) 0.100(3) -0.092(2) 0.203(19) Uiso 0.50 1 d PDU C 2 H46D H 0.5531 0.1413 -0.0705 0.305 Uiso 0.50 1 calc PR C 2 H46E H 0.6759 0.0717 -0.0544 0.305 Uiso 0.50 1 calc PR C 2 H46F H 0.5590 0.0443 -0.1235 0.305 Uiso 0.50 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh10 0.0218(3) 0.0252(3) 0.0224(3) 0.0016(2) 0.0001(2) 0.0005(2) Rh20 0.0238(3) 0.0256(3) 0.0252(3) 0.0023(2) -0.0001(2) 0.0036(2) Rh21 0.0254(3) 0.0251(3) 0.0254(3) -0.0001(2) -0.0011(2) 0.0002(2) Rh30 0.0248(3) 0.0275(3) 0.0223(3) 0.0000(2) 0.0000(2) 0.0010(2) Rh31 0.0250(3) 0.0244(3) 0.0288(3) 0.0035(2) -0.0007(2) 0.0026(2) Rh40 0.0244(3) 0.0268(3) 0.0281(3) 0.0034(2) 0.0021(2) -0.0006(2) C10 0.028(3) 0.031(4) 0.027(4) -0.004(3) -0.001(3) 0.005(3) O10 0.033(3) 0.032(3) 0.033(3) -0.001(2) 0.005(2) 0.002(2) C11 0.030(4) 0.034(4) 0.025(4) 0.000(3) 0.006(3) -0.002(3) O11 0.037(3) 0.038(3) 0.034(3) -0.001(2) 0.009(2) 0.007(2) C20 0.028(4) 0.028(4) 0.035(4) 0.003(3) 0.004(3) -0.002(3) O20 0.030(3) 0.041(3) 0.041(3) -0.002(2) -0.002(2) 0.002(2) C30 0.035(4) 0.033(4) 0.035(5) 0.001(3) -0.009(3) 0.008(3) O30 0.041(3) 0.043(3) 0.032(3) 0.007(3) 0.003(2) 0.002(2) C40 0.037(4) 0.023(4) 0.026(4) 0.003(3) 0.010(3) -0.002(3) O40 0.021(2) 0.050(3) 0.044(3) 0.006(3) 0.000(2) -0.001(2) C50 0.037(4) 0.028(4) 0.042(5) 0.005(3) 0.004(3) 0.006(3) O50 0.043(3) 0.067(4) 0.035(3) 0.015(3) -0.004(3) 0.019(3) C51 0.030(4) 0.033(4) 0.045(5) -0.002(4) 0.002(3) 0.004(3) O51 0.052(3) 0.062(4) 0.033(3) 0.013(3) -0.011(3) 0.000(3) C60 0.034(4) 0.029(4) 0.033(4) 0.004(3) -0.008(3) 0.002(3) O60 0.047(3) 0.047(3) 0.048(4) -0.006(3) 0.006(3) 0.023(3) C61 0.038(4) 0.041(5) 0.042(5) 0.001(4) -0.005(3) 0.000(3) O61 0.082(4) 0.035(4) 0.071(5) -0.003(3) -0.019(3) -0.008(3) C70 0.035(4) 0.036(4) 0.031(4) 0.000(3) 0.002(3) 0.005(3) O70 0.031(3) 0.065(4) 0.046(3) -0.010(3) -0.006(2) 0.003(3) C71 0.039(4) 0.026(4) 0.040(5) 0.007(3) 0.006(3) -0.004(3) O71 0.025(3) 0.047(3) 0.078(4) 0.017(3) -0.009(3) 0.003(2) C80 0.035(4) 0.031(4) 0.027(4) -0.002(3) -0.006(3) -0.008(3) O80 0.045(3) 0.061(4) 0.035(3) -0.017(3) 0.001(2) 0.013(3) C81 0.030(4) 0.034(5) 0.041(5) 0.005(4) -0.002(3) 0.010(3) O81 0.051(3) 0.030(3) 0.079(5) 0.014(3) -0.010(3) 0.000(3) C90 0.034(4) 0.037(5) 0.043(5) 0.007(4) 0.001(3) 0.000(3) O90 0.052(4) 0.045(3) 0.053(4) -0.001(3) 0.018(3) 0.004(3) C91 0.040(4) 0.037(5) 0.033(4) 0.002(3) 0.006(3) 0.005(3) O91 0.070(4) 0.036(4) 0.075(5) 0.006(3) 0.021(3) -0.016(3) P 0.0252(9) 0.0289(10) 0.0238(9) 0.0008(8) 0.0015(7) 0.0017(7) C111 0.028(3) 0.023(4) 0.031(4) 0.004(3) 0.002(3) -0.001(3) C112 0.045(4) 0.039(5) 0.032(4) 0.003(4) 0.007(3) 0.000(3) C113 0.041(4) 0.043(5) 0.047(5) 0.016(4) 0.018(4) -0.005(3) C114 0.027(4) 0.025(4) 0.051(5) 0.010(3) 0.002(3) 0.000(3) C115 0.036(4) 0.033(4) 0.039(5) 0.003(3) -0.001(3) -0.005(3) C116 0.032(4) 0.023(4) 0.041(5) -0.003(3) 0.002(3) -0.003(3) O1 0.035(3) 0.044(3) 0.066(4) 0.013(3) 0.006(3) -0.006(2) C1 0.056(6) 0.055(6) 0.096(9) 0.027(6) -0.012(5) -0.019(5) C121 0.025(8) 0.024(8) 0.043(10) 0.008(7) 0.010(6) -0.014(6) C122 0.016(6) 0.050(9) 0.039(9) 0.007(7) 0.018(6) -0.003(6) C123 0.043(9) 0.038(9) 0.027(8) -0.007(7) 0.005(6) -0.008(7) C124 0.051(10) 0.030(9) 0.047(10) -0.029(7) 0.030(8) -0.006(8) C125 0.043(10) 0.034(10) 0.042(11) 0.008(8) 0.008(7) 0.003(7) C126 0.048(9) 0.031(9) 0.024(8) 0.008(8) 0.002(7) 0.011(7) O2A 0.042(8) 0.056(9) 0.051(8) -0.042(7) 0.011(6) 0.008(7) C2A 0.065(13) 0.084(15) 0.070(14) -0.049(12) 0.024(10) -0.013(10) C131 0.043(15) 0.038(14) 0.037(14) 0.006(7) -0.003(6) -0.010(6) C132 0.059(10) 0.051(10) 0.032(9) -0.002(8) -0.005(8) -0.001(8) C133 0.071(11) 0.029(9) 0.038(9) 0.006(7) -0.021(8) -0.001(8) C134 0.029(9) 0.043(11) 0.081(17) 0.041(10) 0.010(8) -0.004(7) C135 0.036(8) 0.041(9) 0.030(9) 0.008(7) 0.008(7) -0.002(7) C136 0.034(8) 0.051(10) 0.032(9) 0.013(8) -0.003(7) -0.016(7) O3A 0.039(7) 0.046(10) 0.028(8) -0.009(7) -0.007(5) 0.021(6) C3A 0.054(10) 0.116(17) 0.036(10) 0.038(11) -0.018(8) -0.001(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 Rh10 C40 1.875(7) . ? Rh10 C11 2.137(7) . ? Rh10 C10 2.143(7) . ? Rh10 P 2.3696(18) . ? Rh10 Rh30 2.7763(7) . ? Rh10 Rh31 2.7933(7) . ? Rh10 Rh20 2.8050(7) . ? Rh10 Rh21 2.8086(7) . ? Rh20 C50 1.907(8) . ? Rh20 C60 1.918(8) . ? Rh20 C10 2.175(7) . ? Rh20 C20 2.241(7) . ? Rh20 Rh21 2.7214(7) . ? Rh20 Rh40 2.7545(7) . ? Rh20 Rh30 2.7728(7) . ? Rh21 C51 1.896(8) . ? Rh21 C61 1.903(8) . ? Rh21 C20 2.174(7) . ? Rh21 C11 2.199(7) . ? Rh21 Rh31 2.7701(7) . ? Rh21 Rh40 2.7747(7) . ? Rh30 C80 1.896(7) . ? Rh30 C70 1.915(7) . ? Rh30 C30 2.175(8) . ? Rh30 C10 2.294(7) . ? Rh30 Rh31 2.7415(7) . ? Rh30 Rh40 2.7579(7) . ? Rh31 C81 1.887(8) . ? Rh31 C71 1.927(7) . ? Rh31 C30 2.167(8) . ? Rh31 C11 2.297(7) . ? Rh31 Rh40 2.7580(7) . ? Rh40 C90 1.893(8) . ? Rh40 C91 1.903(8) . ? Rh40 C20 2.149(7) . ? Rh40 C30 2.209(7) . ? C10 O10 1.155(8) . ? C11 O11 1.155(7) . ? C20 O20 1.154(7) . ? C30 O30 1.147(8) . ? C40 O40 1.130(8) . ? C50 O50 1.125(8) . ? C51 O51 1.126(8) . ? C60 O60 1.128(8) . ? C61 O61 1.143(9) . ? C70 O70 1.118(8) . ? C71 O71 1.127(8) . ? C80 O80 1.131(8) . ? C81 O81 1.139(8) . ? C90 O90 1.142(8) . ? C91 O91 1.128(9) . ? P C221 1.830(8) . ? P C231 1.830(9) . ? P C111 1.837(6) . ? P C121 1.840(7) . ? P C131 1.866(8) . ? C111 C116 1.373(9) . ? C111 C112 1.391(9) . ? C112 C113 1.374(10) . ? C113 C114 1.378(10) . ? C114 C115 1.372(10) . ? C114 O1 1.373(8) . ? C115 C116 1.388(9) . ? O1 C1 1.428(11) . ? C121 C122 1.3900 . ? C121 C126 1.3900 . ? C122 C123 1.3900 . ? C123 C124 1.3900 . ? C124 O2A 1.369(13) . ? C124 C125 1.3900 . ? C125 C126 1.3900 . ? O2A C2A 1.41(2) . ? C221 C222 1.3900 . ? C221 C226 1.3900 . ? C222 C223 1.3900 . ? C223 C224 1.3900 . ? C224 O2B 1.38(2) . ? C224 C225 1.3900 . ? C225 C226 1.3900 . ? O2B C2B 1.50(3) . ? C131 C132 1.3900 . ? C131 C136 1.3900 . ? C132 C133 1.3900 . ? C133 C134 1.3900 . ? C134 C135 1.3900 . ? C134 O3A 1.391(16) . ? C135 C136 1.3900 . ? O3A C3A 1.48(2) . ? C231 C232 1.3900 . ? C231 C236 1.3900 . ? C232 C233 1.3900 . ? C233 C234 1.3900 . ? C234 O3B 1.38(2) . ? C234 C235 1.3900 . ? C235 C236 1.3900 . ? O3B C3B 1.44(3) . ? C41A C42A 1.647(19) . ? C42A C43A 1.607(19) . ? C43A C44A 1.45(3) . ? C44A C45A 1.57(2) . ? C45A C46A 1.55(2) . ? C41B C42B 1.549(18) . ? C42B C43B 1.55(2) . ? C43B C44B 1.640(19) . ? C44B C45B 1.564(19) . ? C45B C46B 1.495(19) . ? 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 C40 Rh10 C11 96.3(3) . . ? C40 Rh10 C10 101.4(3) . . ? C11 Rh10 C10 157.2(3) . . ? C40 Rh10 P 89.1(2) . . ? C11 Rh10 P 98.87(19) . . ? C10 Rh10 P 95.7(2) . . ? C40 Rh10 Rh30 91.6(2) . . ? C11 Rh10 Rh30 111.87(18) . . ? C10 Rh10 Rh30 53.74(19) . . ? P Rh10 Rh30 148.96(5) . . ? C40 Rh10 Rh31 89.8(2) . . ? C11 Rh10 Rh31 53.54(18) . . ? C10 Rh10 Rh31 111.81(19) . . ? P Rh10 Rh31 152.07(5) . . ? Rh30 Rh10 Rh31 58.974(19) . . ? C40 Rh10 Rh20 147.2(2) . . ? C11 Rh10 Rh20 108.45(17) . . ? C10 Rh10 Rh20 49.99(18) . . ? P Rh10 Rh20 107.42(5) . . ? Rh30 Rh10 Rh20 59.576(18) . . ? Rh31 Rh10 Rh20 87.99(2) . . ? C40 Rh10 Rh21 143.4(2) . . ? C11 Rh10 Rh21 50.61(17) . . ? C10 Rh10 Rh21 107.87(18) . . ? P Rh10 Rh21 108.91(5) . . ? Rh30 Rh10 Rh21 88.40(2) . . ? Rh31 Rh10 Rh21 59.271(18) . . ? Rh20 Rh10 Rh21 57.997(18) . . ? C50 Rh20 C60 91.8(3) . . ? C50 Rh20 C10 106.5(3) . . ? C60 Rh20 C10 95.0(3) . . ? C50 Rh20 C20 88.8(3) . . ? C60 Rh20 C20 101.5(3) . . ? C10 Rh20 C20 157.1(2) . . ? C50 Rh20 Rh21 93.9(2) . . ? C60 Rh20 Rh21 151.5(2) . . ? C10 Rh20 Rh21 109.92(18) . . ? C20 Rh20 Rh21 50.85(17) . . ? C50 Rh20 Rh40 138.5(2) . . ? C60 Rh20 Rh40 97.3(2) . . ? C10 Rh20 Rh40 112.86(19) . . ? C20 Rh20 Rh40 49.66(18) . . ? Rh21 Rh20 Rh40 60.887(19) . . ? C50 Rh20 Rh30 159.7(2) . . ? C60 Rh20 Rh30 93.9(2) . . ? C10 Rh20 Rh30 53.60(19) . . ? C20 Rh20 Rh30 109.01(18) . . ? Rh21 Rh20 Rh30 90.25(2) . . ? Rh40 Rh20 Rh30 59.860(18) . . ? C50 Rh20 Rh10 105.5(2) . . ? C60 Rh20 Rh10 142.9(2) . . ? C10 Rh20 Rh10 48.98(17) . . ? C20 Rh20 Rh10 111.18(17) . . ? Rh21 Rh20 Rh10 61.068(18) . . ? Rh40 Rh20 Rh10 91.04(2) . . ? Rh30 Rh20 Rh10 59.698(18) . . ? C51 Rh21 C61 93.0(3) . . ? C51 Rh21 C20 94.7(3) . . ? C61 Rh21 C20 101.8(3) . . ? C51 Rh21 C11 100.8(3) . . ? C61 Rh21 C11 92.6(3) . . ? C20 Rh21 C11 158.2(3) . . ? C51 Rh21 Rh20 97.0(2) . . ? C61 Rh21 Rh20 153.5(2) . . ? C20 Rh21 Rh20 53.07(18) . . ? C11 Rh21 Rh20 109.43(18) . . ? C51 Rh21 Rh31 154.2(2) . . ? C61 Rh21 Rh31 91.5(2) . . ? C20 Rh21 Rh31 109.18(19) . . ? C11 Rh21 Rh31 53.57(18) . . ? Rh20 Rh21 Rh31 90.16(2) . . ? C51 Rh21 Rh40 144.1(2) . . ? C61 Rh21 Rh40 98.4(2) . . ? C20 Rh21 Rh40 49.68(19) . . ? C11 Rh21 Rh40 112.42(18) . . ? Rh20 Rh21 Rh40 60.147(19) . . ? Rh31 Rh21 Rh40 59.657(19) . . ? C51 Rh21 Rh10 102.1(2) . . ? C61 Rh21 Rh10 140.2(2) . . ? C20 Rh21 Rh10 113.24(18) . . ? C11 Rh21 Rh10 48.66(18) . . ? Rh20 Rh21 Rh10 60.936(18) . . ? Rh31 Rh21 Rh10 60.090(18) . . ? Rh40 Rh21 Rh10 90.55(2) . . ? C80 Rh30 C70 92.8(3) . . ? C80 Rh30 C30 102.1(3) . . ? C70 Rh30 C30 95.5(3) . . ? C80 Rh30 C10 95.0(3) . . ? C70 Rh30 C10 101.2(3) . . ? C30 Rh30 C10 155.5(3) . . ? C80 Rh30 Rh31 151.8(2) . . ? C70 Rh30 Rh31 97.0(2) . . ? C30 Rh30 Rh31 50.7(2) . . ? C10 Rh30 Rh31 108.85(17) . . ? C80 Rh30 Rh40 98.4(2) . . ? C70 Rh30 Rh40 146.7(2) . . ? C30 Rh30 Rh40 51.56(18) . . ? C10 Rh30 Rh40 108.94(17) . . ? Rh31 Rh30 Rh40 60.199(19) . . ? C80 Rh30 Rh20 94.7(2) . . ? C70 Rh30 Rh20 150.5(2) . . ? C30 Rh30 Rh20 110.74(18) . . ? C10 Rh30 Rh20 49.75(16) . . ? Rh31 Rh30 Rh20 89.69(2) . . ? Rh40 Rh30 Rh20 59.740(18) . . ? C80 Rh30 Rh10 143.7(2) . . ? C70 Rh30 Rh10 97.8(2) . . ? C30 Rh30 Rh10 111.3(2) . . ? C10 Rh30 Rh10 48.87(17) . . ? Rh31 Rh30 Rh10 60.823(19) . . ? Rh40 Rh30 Rh10 91.58(2) . . ? Rh20 Rh30 Rh10 60.727(18) . . ? C81 Rh31 C71 92.6(3) . . ? C81 Rh31 C30 95.6(3) . . ? C71 Rh31 C30 99.4(3) . . ? C81 Rh31 C11 102.0(3) . . ? C71 Rh31 C11 96.4(3) . . ? C30 Rh31 C11 155.7(3) . . ? C81 Rh31 Rh30 145.6(2) . . ? C71 Rh31 Rh30 100.2(2) . . ? C30 Rh31 Rh30 51.0(2) . . ? C11 Rh31 Rh30 108.05(18) . . ? C81 Rh31 Rh40 94.2(2) . . ? C71 Rh31 Rh40 150.7(2) . . ? C30 Rh31 Rh40 51.60(17) . . ? C11 Rh31 Rh40 109.90(17) . . ? Rh30 Rh31 Rh40 60.194(18) . . ? C81 Rh31 Rh21 96.7(2) . . ? C71 Rh31 Rh21 146.7(2) . . ? C30 Rh31 Rh21 111.32(18) . . ? C11 Rh31 Rh21 50.40(16) . . ? Rh30 Rh31 Rh21 89.89(2) . . ? Rh40 Rh31 Rh21 60.255(18) . . ? C81 Rh31 Rh10 149.6(2) . . ? C71 Rh31 Rh10 97.2(2) . . ? C30 Rh31 Rh10 110.9(2) . . ? C11 Rh31 Rh10 48.44(17) . . ? Rh30 Rh31 Rh10 60.203(19) . . ? Rh40 Rh31 Rh10 91.22(2) . . ? Rh21 Rh31 Rh10 60.639(18) . . ? C90 Rh40 C91 94.2(3) . . ? C90 Rh40 C20 98.8(3) . . ? C91 Rh40 C20 96.0(3) . . ? C90 Rh40 C30 97.4(3) . . ? C91 Rh40 C30 98.3(3) . . ? C20 Rh40 C30 157.5(3) . . ? C90 Rh40 Rh20 95.4(2) . . ? C91 Rh40 Rh20 148.2(2) . . ? C20 Rh40 Rh20 52.65(18) . . ? C30 Rh40 Rh20 110.3(2) . . ? C90 Rh40 Rh31 146.5(2) . . ? C91 Rh40 Rh31 98.6(2) . . ? C20 Rh40 Rh31 110.40(18) . . ? C30 Rh40 Rh31 50.3(2) . . ? Rh20 Rh40 Rh31 89.73(2) . . ? C90 Rh40 Rh30 94.6(2) . . ? C91 Rh40 Rh30 148.4(2) . . ? C20 Rh40 Rh30 112.50(18) . . ? C30 Rh40 Rh30 50.5(2) . . ? Rh20 Rh40 Rh30 60.400(18) . . ? Rh31 Rh40 Rh30 59.607(18) . . ? C90 Rh40 Rh21 147.4(2) . . ? C91 Rh40 Rh21 99.1(2) . . ? C20 Rh40 Rh21 50.48(18) . . ? C30 Rh40 Rh21 109.8(2) . . ? Rh20 Rh40 Rh21 58.967(19) . . ? Rh31 Rh40 Rh21 60.088(18) . . ? Rh30 Rh40 Rh21 89.46(2) . . ? O10 C10 Rh10 137.1(5) . . ? O10 C10 Rh20 133.2(5) . . ? Rh10 C10 Rh20 81.0(2) . . ? O10 C10 Rh30 128.2(5) . . ? Rh10 C10 Rh30 77.4(2) . . ? Rh20 C10 Rh30 76.6(2) . . ? O11 C11 Rh10 137.8(5) . . ? O11 C11 Rh21 132.2(5) . . ? Rh10 C11 Rh21 80.7(2) . . ? O11 C11 Rh31 128.8(5) . . ? Rh10 C11 Rh31 78.0(2) . . ? Rh21 C11 Rh31 76.0(2) . . ? O20 C20 Rh40 134.7(5) . . ? O20 C20 Rh21 132.8(5) . . ? Rh40 C20 Rh21 79.8(2) . . ? O20 C20 Rh20 132.8(5) . . ? Rh40 C20 Rh20 77.7(2) . . ? Rh21 C20 Rh20 76.1(2) . . ? O30 C30 Rh31 133.9(6) . . ? O30 C30 Rh30 134.5(6) . . ? Rh31 C30 Rh30 78.3(3) . . ? O30 C30 Rh40 131.5(6) . . ? Rh31 C30 Rh40 78.1(2) . . ? Rh30 C30 Rh40 78.0(2) . . ? O40 C40 Rh10 176.9(6) . . ? O50 C50 Rh20 172.3(7) . . ? O51 C51 Rh21 175.4(6) . . ? O60 C60 Rh20 178.7(6) . . ? O61 C61 Rh21 177.2(7) . . ? O70 C70 Rh30 176.8(7) . . ? O71 C71 Rh31 178.3(6) . . ? O80 C80 Rh30 179.1(6) . . ? O81 C81 Rh31 175.8(7) . . ? O90 C90 Rh40 177.9(7) . . ? O91 C91 Rh40 179.0(7) . . ? C221 P C231 109.3(5) . . ? C221 P C111 96.4(4) . . ? C231 P C111 99.1(4) . . ? C221 P C121 10.4(5) . . ? C231 P C121 110.1(5) . . ? C111 P C121 106.2(4) . . ? C221 P C131 106.6(5) . . ? C231 P C131 2.7(6) . . ? C111 P C131 99.3(4) . . ? C121 P C131 107.5(5) . . ? C221 P Rh10 115.8(4) . . ? C231 P Rh10 118.8(4) . . ? C111 P Rh10 114.0(2) . . ? C121 P Rh10 107.8(4) . . ? C131 P Rh10 121.0(4) . . ? C116 C111 C112 117.9(6) . . ? C116 C111 P 123.3(5) . . ? C112 C111 P 118.7(5) . . ? C113 C112 C111 120.3(7) . . ? C112 C113 C114 120.7(7) . . ? C115 C114 O1 123.9(7) . . ? C115 C114 C113 120.0(6) . . ? O1 C114 C113 116.1(7) . . ? C114 C115 C116 118.6(7) . . ? C111 C116 C115 122.3(7) . . ? C114 O1 C1 117.1(6) . . ? C122 C121 C126 120.0 . . ? C122 C121 P 124.8(6) . . ? C126 C121 P 115.2(6) . . ? C121 C122 C123 120.0 . . ? C124 C123 C122 120.0 . . ? O2A C124 C123 123.5(9) . . ? O2A C124 C125 116.3(9) . . ? C123 C124 C125 120.0 . . ? C126 C125 C124 120.0 . . ? C125 C126 C121 120.0 . . ? C124 O2A C2A 120.4(13) . . ? C222 C221 C226 120.0 . . ? C222 C221 P 123.5(6) . . ? C226 C221 P 116.5(6) . . ? C223 C222 C221 120.0 . . ? C222 C223 C224 120.0 . . ? O2B C224 C223 127.8(11) . . ? O2B C224 C225 112.2(11) . . ? C223 C224 C225 120.0 . . ? C226 C225 C224 120.0 . . ? C225 C226 C221 120.0 . . ? C224 O2B C2B 112.7(16) . . ? C132 C131 C136 120.0 . . ? C132 C131 P 125.6(7) . . ? C136 C131 P 114.2(7) . . ? C131 C132 C133 120.0 . . ? C134 C133 C132 120.0 . . ? C133 C134 C135 120.0 . . ? C133 C134 O3A 125.7(10) . . ? C135 C134 O3A 114.2(10) . . ? C134 C135 C136 120.0 . . ? C135 C136 C131 120.0 . . ? C134 O3A C3A 114.8(14) . . ? C232 C231 C236 120.0 . . ? C232 C231 P 121.2(7) . . ? C236 C231 P 118.7(7) . . ? C233 C232 C231 120.0 . . ? C234 C233 C232 120.0 . . ? O3B C234 C233 115.4(11) . . ? O3B C234 C235 124.5(11) . . ? C233 C234 C235 120.0 . . ? C236 C235 C234 120.0 . . ? C235 C236 C231 120.0 . . ? C234 O3B C3B 115.1(17) . . ? C43A C42A C41A 81.7(15) . . ? C44A C43A C42A 108(2) . . ? C43A C44A C45A 104(2) . . ? C44A C45A C46A 96(2) . . ? C43B C42B C41B 104(2) . . ? C42B C43B C44B 91.5(17) . . ? C45B C44B C43B 87.1(17) . . ? C46B C45B C44B 111(2) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 1.144 _refine_diff_density_min -1.144 _refine_diff_density_rms 0.180 #======END data_k9883 _database_code_CSD 163534 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '6 Rh6(CO)15(P(n-Bu)3)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H27 O15 P Rh6' _chemical_formula_weight 1239.92 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' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7893(2) _cell_length_b 23.4579(5) _cell_length_c 15.6844(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.9790(10) _cell_angle_gamma 90.00 _cell_volume 3582.12(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 7123 _cell_measurement_theta_min 4.11 _cell_measurement_theta_max 26.37 _exptl_crystal_description 'flat needle' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 2.810 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Denzo-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 26451 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7123 _reflns_number_gt 5672 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'Bruker SHELXTL V5.1' _computing_structure_refinement 'Bruker SHELXTL V5.1' _computing_molecular_graphics 'Bruker SHELXTL V5.1' _computing_publication_material 'Bruker SHELXTL V5.1' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0560P)^2^+3.8855P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7123 _refine_ls_number_parameters 518 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.005 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 Rh10 Rh 0.01118(4) 0.694507(17) 0.65915(2) 0.02894(11) Uani 1 1 d . A . Rh20 Rh 0.22240(4) 0.672096(18) 0.78767(2) 0.02988(11) Uani 1 1 d . . . Rh21 Rh 0.28246(4) 0.675229(17) 0.62114(2) 0.02964(11) Uani 1 1 d . . . Rh30 Rh 0.02129(4) 0.590466(17) 0.74370(3) 0.02915(11) Uani 1 1 d . . . Rh31 Rh 0.07979(4) 0.594893(18) 0.57720(2) 0.02998(11) Uani 1 1 d . . . Rh40 Rh 0.28596(4) 0.572497(18) 0.70655(2) 0.02973(11) Uani 1 1 d . . . C10 C -0.0022(5) 0.6794(2) 0.7918(3) 0.0323(11) Uani 1 1 d . . . O10 O -0.0648(4) 0.69638(17) 0.8452(2) 0.0369(8) Uani 1 1 d . . . C11 C 0.0925(5) 0.6926(2) 0.5410(3) 0.0371(12) Uani 1 1 d . . . O11 O 0.0713(4) 0.71392(19) 0.4737(2) 0.0462(10) Uani 1 1 d . . . C20 C 0.4132(5) 0.6474(2) 0.7365(3) 0.0344(11) Uani 1 1 d . . . O20 O 0.5278(4) 0.65463(17) 0.7599(2) 0.0406(9) Uani 1 1 d . . . C30 C 0.0967(5) 0.5238(2) 0.6636(3) 0.0333(11) Uani 1 1 d . . . O30 O 0.0751(4) 0.47521(17) 0.6575(2) 0.0424(9) Uani 1 1 d . . . C40 C -0.1757(6) 0.6886(2) 0.6230(3) 0.0393(13) Uani 1 1 d . . . O40 O -0.2899(4) 0.6833(2) 0.6014(3) 0.0523(11) Uani 1 1 d . . . C50 C 0.2648(6) 0.7482(3) 0.8218(4) 0.0423(14) Uani 1 1 d . . . O50 O 0.2902(6) 0.7927(2) 0.8456(3) 0.0734(15) Uani 1 1 d . . . C51 C 0.3706(6) 0.7472(3) 0.6190(4) 0.0442(14) Uani 1 1 d . . . O51 O 0.4354(5) 0.7870(2) 0.6149(4) 0.0722(15) Uani 1 1 d . . . C60 C 0.2614(7) 0.6450(3) 0.9009(4) 0.0505(16) Uani 1 1 d . . . O60 O 0.2872(7) 0.6301(3) 0.9698(3) 0.0873(19) Uani 1 1 d . . . C61 C 0.3902(6) 0.6467(3) 0.5360(3) 0.0399(13) Uani 1 1 d . . . O61 O 0.4573(4) 0.6286(2) 0.4876(3) 0.0537(11) Uani 1 1 d . . . C70 C -0.1692(6) 0.5747(2) 0.7198(4) 0.0394(12) Uani 1 1 d . . . O70 O -0.2821(4) 0.5640(2) 0.7042(3) 0.0558(12) Uani 1 1 d . . . C71 C -0.1019(6) 0.5825(3) 0.5244(3) 0.0397(13) Uani 1 1 d . . . O71 O -0.2103(4) 0.5749(2) 0.4941(3) 0.0550(12) Uani 1 1 d . . . C80 C 0.0374(6) 0.5531(3) 0.8525(4) 0.0406(13) Uani 1 1 d . . . O80 O 0.0480(5) 0.5306(2) 0.9164(3) 0.0627(13) Uani 1 1 d . . . C81 C 0.1629(5) 0.5649(3) 0.4818(3) 0.0384(13) Uani 1 1 d . . . O81 O 0.2130(4) 0.5474(2) 0.4257(3) 0.0606(13) Uani 1 1 d . . . C90 C 0.3355(6) 0.5291(3) 0.8066(4) 0.0453(14) Uani 1 1 d . . . O90 O 0.3619(6) 0.5021(2) 0.8655(3) 0.0779(17) Uani 1 1 d . . . C91 C 0.4039(6) 0.5308(2) 0.6381(4) 0.0391(12) Uani 1 1 d . . . O91 O 0.4697(4) 0.5057(2) 0.5970(3) 0.0551(12) Uani 1 1 d . . . P P -0.02346(16) 0.79335(7) 0.66127(10) 0.0426(4) Uani 1 1 d D . . C111 C 0.1293(16) 0.8373(6) 0.656(2) 0.061(10) Uani 0.596(9) 1 d PD A 1 H11A H 0.2050 0.8206 0.6923 0.073 Uiso 0.596(9) 1 calc PR A 1 H11B H 0.1537 0.8370 0.5975 0.073 Uiso 0.596(9) 1 calc PR A 1 C112 C 0.1104(16) 0.8994(5) 0.6838(11) 0.071(4) Uani 0.596(9) 1 d PD A 1 H11C H 0.0239 0.9140 0.6565 0.085 Uiso 0.596(9) 1 calc PR A 1 H11D H 0.1073 0.9009 0.7453 0.085 Uiso 0.596(9) 1 calc PR A 1 C113 C 0.2288(19) 0.9368(6) 0.6589(13) 0.104(6) Uani 0.596(9) 1 d PD A 1 H11E H 0.2365 0.9325 0.5981 0.124 Uiso 0.596(9) 1 calc PR A 1 H11F H 0.2085 0.9764 0.6697 0.124 Uiso 0.596(9) 1 calc PR A 1 C114 C 0.3524(18) 0.9225(9) 0.7043(17) 0.23(3) Uani 0.596(9) 1 d PD A 1 H11G H 0.4056 0.9000 0.6687 0.345 Uiso 0.596(9) 1 calc PR A 1 H11H H 0.3357 0.9009 0.7542 0.345 Uiso 0.596(9) 1 calc PR A 1 H11I H 0.4020 0.9566 0.7215 0.345 Uiso 0.596(9) 1 calc PR A 1 C121 C 0.128(2) 0.8391(11) 0.665(3) 0.057(13) Uiso 0.404(9) 1 d PD A 2 H12A H 0.2072 0.8149 0.6801 0.068 Uiso 0.404(9) 1 calc PR A 2 H12B H 0.1346 0.8522 0.6069 0.068 Uiso 0.404(9) 1 calc PR A 2 C122 C 0.145(2) 0.8919(9) 0.7233(14) 0.065(7) Uiso 0.404(9) 1 d PD A 2 H12C H 0.0668 0.9166 0.7095 0.077 Uiso 0.404(9) 1 calc PR A 2 H12D H 0.1437 0.8795 0.7821 0.077 Uiso 0.404(9) 1 calc PR A 2 C123 C 0.277(2) 0.9273(11) 0.7178(17) 0.084(7) Uiso 0.404(9) 1 d PD A 2 H12E H 0.2624 0.9468 0.6630 0.100 Uiso 0.404(9) 1 calc PR A 2 H12F H 0.2741 0.9566 0.7612 0.100 Uiso 0.404(9) 1 calc PR A 2 C124 C 0.411(3) 0.909(2) 0.724(4) 0.23(3) Uiso 0.404(9) 1 d PD A 2 H12G H 0.4334 0.8961 0.6694 0.339 Uiso 0.404(9) 1 calc PR A 2 H12H H 0.4227 0.8779 0.7646 0.339 Uiso 0.404(9) 1 calc PR A 2 H12I H 0.4709 0.9396 0.7440 0.339 Uiso 0.404(9) 1 calc PR A 2 C211 C -0.1101(12) 0.8163(8) 0.7530(9) 0.036(5) Uani 0.596(9) 1 d PD A 1 H21A H -0.0624 0.8007 0.8051 0.044 Uiso 0.596(9) 1 calc PR A 1 H21B H -0.1065 0.8575 0.7571 0.044 Uiso 0.596(9) 1 calc PR A 1 C212 C -0.2611(10) 0.7967(5) 0.7448(7) 0.041(3) Uani 0.596(9) 1 d PD A 1 H21C H -0.3075 0.8107 0.6912 0.049 Uiso 0.596(9) 1 calc PR A 1 H21D H -0.2645 0.7554 0.7436 0.049 Uiso 0.596(9) 1 calc PR A 1 C213 C -0.3365(10) 0.8186(5) 0.8196(6) 0.044(3) Uani 0.596(9) 1 d PD A 1 H21E H -0.4242 0.7993 0.8192 0.053 Uiso 0.596(9) 1 calc PR A 1 H21F H -0.2825 0.8102 0.8735 0.053 Uiso 0.596(9) 1 calc PR A 1 C214 C -0.358(2) 0.8767(6) 0.8123(14) 0.157(11) Uani 0.596(9) 1 d PD A 1 H21G H -0.4433 0.8863 0.8334 0.236 Uiso 0.596(9) 1 calc PR A 1 H21H H -0.3602 0.8877 0.7532 0.236 Uiso 0.596(9) 1 calc PR A 1 H21I H -0.2841 0.8964 0.8453 0.236 Uiso 0.596(9) 1 calc PR A 1 C221 C -0.108(3) 0.8210(17) 0.751(2) 0.080(18) Uiso 0.404(9) 1 d PD A 2 H22A H -0.0395 0.8199 0.8004 0.096 Uiso 0.404(9) 1 calc PR A 2 H22B H -0.1258 0.8610 0.7386 0.096 Uiso 0.404(9) 1 calc PR A 2 C222 C -0.241(2) 0.7971(12) 0.7819(13) 0.076(8) Uiso 0.404(9) 1 d PD A 2 H22C H -0.2447 0.7569 0.7677 0.091 Uiso 0.404(9) 1 calc PR A 2 H22D H -0.3172 0.8152 0.7480 0.091 Uiso 0.404(9) 1 calc PR A 2 C223 C -0.267(2) 0.8027(11) 0.8768(13) 0.088(7) Uiso 0.404(9) 1 d PD A 2 H22E H -0.1855 0.7908 0.9133 0.105 Uiso 0.404(9) 1 calc PR A 2 H22F H -0.2857 0.8421 0.8898 0.105 Uiso 0.404(9) 1 calc PR A 2 C224 C -0.376(3) 0.7691(12) 0.8923(18) 0.116(10) Uiso 0.404(9) 1 d PD A 2 H22G H -0.4014 0.7769 0.9487 0.174 Uiso 0.404(9) 1 calc PR A 2 H22H H -0.3515 0.7297 0.8883 0.174 Uiso 0.404(9) 1 calc PR A 2 H22I H -0.4528 0.7773 0.8506 0.174 Uiso 0.404(9) 1 calc PR A 2 C311 C -0.1243(16) 0.8184(5) 0.5641(6) 0.041(3) Uani 0.596(9) 1 d PD A 1 H31A H -0.0810 0.8051 0.5149 0.049 Uiso 0.596(9) 1 calc PR A 1 H31B H -0.2148 0.8012 0.5611 0.049 Uiso 0.596(9) 1 calc PR A 1 C312 C -0.1415(13) 0.8835(4) 0.5572(6) 0.049(3) Uani 0.596(9) 1 d PD A 1 H31C H -0.0534 0.9012 0.5516 0.059 Uiso 0.596(9) 1 calc PR A 1 H31D H -0.1761 0.8982 0.6086 0.059 Uiso 0.596(9) 1 calc PR A 1 C313 C -0.2429(10) 0.8976(6) 0.4783(7) 0.062(4) Uani 0.596(9) 1 d PD A 1 H31E H -0.2380 0.9382 0.4672 0.075 Uiso 0.596(9) 1 calc PR A 1 H31F H -0.2132 0.8779 0.4291 0.075 Uiso 0.596(9) 1 calc PR A 1 C314 C -0.3789(12) 0.8833(6) 0.4852(9) 0.070(4) Uani 0.596(9) 1 d PD A 1 H31G H -0.4353 0.8967 0.4354 0.105 Uiso 0.596(9) 1 calc PR A 1 H31H H -0.4083 0.9007 0.5355 0.105 Uiso 0.596(9) 1 calc PR A 1 H31I H -0.3871 0.8427 0.4892 0.105 Uiso 0.596(9) 1 calc PR A 1 C321 C -0.152(3) 0.8081(10) 0.5713(17) 0.090(14) Uiso 0.404(9) 1 d PD A 2 H32A H -0.1203 0.7894 0.5219 0.108 Uiso 0.404(9) 1 calc PR A 2 H32B H -0.2346 0.7880 0.5834 0.108 Uiso 0.404(9) 1 calc PR A 2 C322 C -0.200(2) 0.8678(9) 0.5408(12) 0.064(6) Uiso 0.404(9) 1 d PD A 2 H32C H -0.1182 0.8897 0.5320 0.076 Uiso 0.404(9) 1 calc PR A 2 H32D H -0.2414 0.8859 0.5872 0.076 Uiso 0.404(9) 1 calc PR A 2 C323 C -0.301(2) 0.8735(7) 0.4592(12) 0.060(6) Uiso 0.404(9) 1 d PD A 2 H32E H -0.2590 0.8581 0.4106 0.072 Uiso 0.404(9) 1 calc PR A 2 H32F H -0.3831 0.8518 0.4658 0.072 Uiso 0.404(9) 1 calc PR A 2 C324 C -0.334(2) 0.9302(7) 0.4442(14) 0.077(6) Uiso 0.404(9) 1 d PD A 2 H32G H -0.3994 0.9331 0.3942 0.115 Uiso 0.404(9) 1 calc PR A 2 H32H H -0.2530 0.9513 0.4352 0.115 Uiso 0.404(9) 1 calc PR A 2 H32I H -0.3739 0.9455 0.4928 0.115 Uiso 0.404(9) 1 calc PR A 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 Rh10 0.0265(2) 0.0308(2) 0.0300(2) -0.00136(15) 0.00540(16) -0.00028(16) Rh20 0.0297(2) 0.0340(2) 0.0263(2) -0.00460(15) 0.00480(16) -0.00600(16) Rh21 0.0260(2) 0.0351(2) 0.0285(2) 0.00118(16) 0.00624(16) -0.00266(16) Rh30 0.0273(2) 0.0302(2) 0.0309(2) -0.00242(15) 0.00721(16) -0.00412(15) Rh31 0.0254(2) 0.0372(2) 0.0273(2) -0.00720(16) 0.00270(16) -0.00051(16) Rh40 0.0268(2) 0.0327(2) 0.0296(2) -0.00076(15) 0.00291(16) 0.00093(16) C10 0.034(3) 0.027(3) 0.038(3) -0.003(2) 0.011(2) -0.006(2) O10 0.037(2) 0.040(2) 0.035(2) -0.0095(16) 0.0116(17) -0.0035(16) C11 0.030(3) 0.047(3) 0.035(3) 0.000(2) 0.005(2) 0.006(2) O11 0.041(2) 0.062(3) 0.037(2) 0.0062(19) 0.0077(18) 0.010(2) C20 0.030(3) 0.041(3) 0.032(3) 0.002(2) 0.003(2) -0.001(2) O20 0.032(2) 0.050(2) 0.039(2) -0.0020(17) 0.0031(16) -0.0052(17) C30 0.025(2) 0.040(3) 0.035(3) -0.004(2) 0.005(2) -0.003(2) O30 0.043(2) 0.034(2) 0.051(2) -0.0108(17) 0.0113(18) -0.0048(17) C40 0.038(3) 0.044(3) 0.036(3) -0.001(2) 0.009(2) 0.004(2) O40 0.030(2) 0.069(3) 0.057(3) -0.003(2) 0.0011(19) 0.0040(19) C50 0.041(3) 0.049(4) 0.038(3) -0.006(3) 0.010(2) -0.009(3) O50 0.093(4) 0.051(3) 0.079(3) -0.029(3) 0.021(3) -0.028(3) C51 0.035(3) 0.043(4) 0.054(4) 0.000(3) 0.006(3) -0.004(3) O51 0.057(3) 0.048(3) 0.114(4) 0.009(3) 0.019(3) -0.012(2) C60 0.053(4) 0.064(4) 0.035(3) -0.002(3) 0.002(3) -0.015(3) O60 0.116(5) 0.108(5) 0.035(3) 0.008(3) -0.005(3) -0.029(4) C61 0.032(3) 0.054(4) 0.034(3) 0.005(2) 0.003(2) -0.008(3) O61 0.044(2) 0.074(3) 0.046(2) -0.010(2) 0.019(2) 0.001(2) C70 0.039(3) 0.035(3) 0.045(3) -0.001(2) 0.011(2) -0.003(2) O70 0.030(2) 0.052(3) 0.087(3) -0.007(2) 0.010(2) -0.0100(19) C71 0.036(3) 0.051(4) 0.032(3) -0.011(2) 0.007(2) 0.002(3) O71 0.029(2) 0.071(3) 0.063(3) -0.026(2) -0.003(2) -0.003(2) C80 0.040(3) 0.039(3) 0.044(3) 0.000(3) 0.012(3) -0.003(2) O80 0.074(3) 0.067(3) 0.049(3) 0.022(2) 0.015(2) -0.003(3) C81 0.030(3) 0.048(3) 0.036(3) -0.012(2) 0.000(2) -0.004(2) O81 0.046(2) 0.090(4) 0.049(3) -0.032(2) 0.017(2) -0.005(2) C90 0.044(3) 0.047(4) 0.044(3) -0.001(3) 0.004(3) 0.006(3) O90 0.084(4) 0.091(4) 0.059(3) 0.035(3) 0.008(3) 0.027(3) C91 0.034(3) 0.038(3) 0.044(3) -0.003(2) -0.001(2) 0.000(2) O91 0.043(2) 0.066(3) 0.057(3) -0.015(2) 0.011(2) 0.016(2) P 0.0466(9) 0.0348(8) 0.0479(9) 0.0043(6) 0.0126(7) 0.0064(6) C111 0.074(13) 0.014(6) 0.101(18) -0.008(5) 0.045(10) -0.002(5) C112 0.106(12) 0.032(6) 0.076(10) -0.013(6) 0.021(9) 0.008(7) C113 0.159(19) 0.045(8) 0.113(14) -0.019(9) 0.043(14) -0.017(11) C114 0.126(18) 0.17(3) 0.43(6) -0.23(4) 0.19(3) -0.11(2) C211 0.045(9) 0.024(6) 0.044(8) -0.004(4) 0.023(5) 0.015(4) C212 0.038(5) 0.056(7) 0.032(6) -0.015(5) 0.018(5) 0.010(5) C213 0.037(5) 0.055(7) 0.043(6) -0.009(5) 0.023(4) 0.010(5) C214 0.097(16) 0.26(3) 0.123(17) -0.05(2) 0.040(13) -0.023(19) C311 0.047(6) 0.040(6) 0.038(6) 0.010(5) 0.012(5) 0.019(5) C312 0.059(8) 0.042(6) 0.048(6) 0.009(5) 0.013(6) 0.010(6) C313 0.060(8) 0.076(9) 0.054(7) 0.023(7) 0.020(6) 0.028(7) C314 0.064(8) 0.066(9) 0.078(9) 0.004(7) 0.001(7) 0.002(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh10 C40 1.864(6) . ? Rh10 C11 2.092(5) . ? Rh10 C10 2.127(5) . ? Rh10 P 2.3441(16) . ? Rh10 Rh30 2.7744(6) . ? Rh10 Rh31 2.7827(6) . ? Rh10 Rh20 2.7833(6) . ? Rh10 Rh21 2.8182(6) . ? Rh20 C60 1.887(6) . ? Rh20 C50 1.898(6) . ? Rh20 C20 2.186(5) . ? Rh20 C10 2.213(5) . ? Rh20 Rh21 2.7373(5) . ? Rh20 Rh40 2.7622(6) . ? Rh20 Rh30 2.7813(6) . ? Rh21 C51 1.899(6) . ? Rh21 C61 1.907(6) . ? Rh21 C11 2.172(5) . ? Rh21 C20 2.203(5) . ? Rh21 Rh40 2.7556(6) . ? Rh21 Rh31 2.7709(6) . ? Rh30 C70 1.900(6) . ? Rh30 C80 1.910(6) . ? Rh30 C30 2.182(5) . ? Rh30 C10 2.238(5) . ? Rh30 Rh31 2.7331(6) . ? Rh30 Rh40 2.7468(6) . ? Rh31 C71 1.904(6) . ? Rh31 C81 1.910(6) . ? Rh31 C30 2.144(5) . ? Rh31 C11 2.368(6) . ? Rh31 Rh40 2.7590(5) . ? Rh40 C90 1.891(6) . ? Rh40 C91 1.924(6) . ? Rh40 C20 2.177(6) . ? Rh40 C30 2.221(5) . ? C10 O10 1.159(6) . ? C11 O11 1.166(6) . ? C20 O20 1.156(6) . ? C30 O30 1.162(6) . ? C40 O40 1.140(7) . ? C50 O50 1.128(7) . ? C51 O51 1.133(7) . ? C60 O60 1.140(7) . ? C61 O61 1.137(7) . ? C70 O70 1.134(7) . ? C71 O71 1.131(7) . ? C80 O80 1.130(7) . ? C81 O81 1.129(6) . ? C90 O90 1.128(7) . ? C91 O91 1.123(7) . ? P C221 1.824(6) . ? P C311 1.825(6) . ? P C211 1.825(5) . ? P C321 1.826(7) . ? P C111 1.826(6) . ? P C121 1.827(6) . ? C111 C112 1.537(7) . ? C112 C113 1.535(7) . ? C113 C114 1.379(11) . ? C121 C122 1.539(7) . ? C122 C123 1.538(7) . ? C123 C124 1.381(11) . ? C211 C212 1.540(7) . ? C212 C213 1.537(7) . ? C213 C214 1.380(11) . ? C221 C222 1.539(7) . ? C222 C223 1.541(7) . ? C223 C224 1.374(11) . ? C311 C312 1.538(7) . ? C312 C313 1.540(7) . ? C313 C314 1.388(11) . ? C321 C322 1.535(7) . ? C322 C323 1.539(7) . ? C323 C324 1.386(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C40 Rh10 C11 100.4(2) . . ? C40 Rh10 C10 97.3(2) . . ? C11 Rh10 C10 158.5(2) . . ? C40 Rh10 P 86.48(18) . . ? C11 Rh10 P 95.88(16) . . ? C10 Rh10 P 97.31(14) . . ? C40 Rh10 Rh30 93.75(18) . . ? C11 Rh10 Rh30 114.01(16) . . ? C10 Rh10 Rh30 52.33(14) . . ? P Rh10 Rh30 149.47(4) . . ? C40 Rh10 Rh31 94.23(18) . . ? C11 Rh10 Rh31 55.99(16) . . ? C10 Rh10 Rh31 110.74(14) . . ? P Rh10 Rh31 151.57(4) . . ? Rh30 Rh10 Rh31 58.920(14) . . ? C40 Rh10 Rh20 146.96(17) . . ? C11 Rh10 Rh20 108.37(15) . . ? C10 Rh10 Rh20 51.48(14) . . ? P Rh10 Rh20 105.92(4) . . ? Rh30 Rh10 Rh20 60.058(14) . . ? Rh31 Rh10 Rh20 88.801(16) . . ? C40 Rh10 Rh21 147.22(17) . . ? C11 Rh10 Rh21 49.87(15) . . ? C10 Rh10 Rh21 109.60(15) . . ? P Rh10 Rh21 107.61(4) . . ? Rh30 Rh10 Rh21 88.423(16) . . ? Rh31 Rh10 Rh21 59.300(14) . . ? Rh20 Rh10 Rh21 58.504(14) . . ? C60 Rh20 C50 92.0(3) . . ? C60 Rh20 C20 99.2(3) . . ? C50 Rh20 C20 100.5(2) . . ? C60 Rh20 C10 95.9(2) . . ? C50 Rh20 C10 96.2(2) . . ? C20 Rh20 C10 156.98(19) . . ? C60 Rh20 Rh21 149.8(2) . . ? C50 Rh20 Rh21 100.46(17) . . ? C20 Rh20 Rh21 51.69(13) . . ? C10 Rh20 Rh21 109.78(14) . . ? C60 Rh20 Rh40 96.6(2) . . ? C50 Rh20 Rh40 150.77(18) . . ? C20 Rh20 Rh40 50.56(15) . . ? C10 Rh20 Rh40 110.55(13) . . ? Rh21 Rh20 Rh40 60.139(14) . . ? C60 Rh20 Rh30 94.04(19) . . ? C50 Rh20 Rh30 147.81(18) . . ? C20 Rh20 Rh30 109.64(14) . . ? C10 Rh20 Rh30 51.73(13) . . ? Rh21 Rh20 Rh30 89.927(16) . . ? Rh40 Rh20 Rh30 59.404(14) . . ? C60 Rh20 Rh10 143.8(2) . . ? C50 Rh20 Rh10 98.68(18) . . ? C20 Rh20 Rh10 112.49(13) . . ? C10 Rh20 Rh10 48.78(13) . . ? Rh21 Rh20 Rh10 61.385(14) . . ? Rh40 Rh20 Rh10 90.695(16) . . ? Rh30 Rh20 Rh10 59.813(14) . . ? C51 Rh21 C61 90.8(3) . . ? C51 Rh21 C11 100.7(2) . . ? C61 Rh21 C11 99.4(2) . . ? C51 Rh21 C20 93.0(2) . . ? C61 Rh21 C20 98.9(2) . . ? C11 Rh21 C20 156.9(2) . . ? C51 Rh21 Rh20 100.58(19) . . ? C61 Rh21 Rh20 147.99(17) . . ? C11 Rh21 Rh20 107.54(14) . . ? C20 Rh21 Rh20 51.15(14) . . ? C51 Rh21 Rh40 143.51(18) . . ? C61 Rh21 Rh40 93.06(18) . . ? C11 Rh21 Rh40 114.34(16) . . ? C20 Rh21 Rh40 50.58(14) . . ? Rh20 Rh21 Rh40 60.378(14) . . ? C51 Rh21 Rh31 156.29(18) . . ? C61 Rh21 Rh31 91.21(17) . . ? C11 Rh21 Rh31 55.67(16) . . ? C20 Rh21 Rh31 110.02(14) . . ? Rh20 Rh21 Rh31 89.982(16) . . ? Rh40 Rh21 Rh31 59.897(14) . . ? C51 Rh21 Rh10 107.50(18) . . ? C61 Rh21 Rh10 143.77(16) . . ? C11 Rh21 Rh10 47.43(14) . . ? C20 Rh21 Rh10 110.70(14) . . ? Rh20 Rh21 Rh10 60.112(14) . . ? Rh40 Rh21 Rh10 90.102(16) . . ? Rh31 Rh21 Rh10 59.712(14) . . ? C70 Rh30 C80 94.3(2) . . ? C70 Rh30 C30 97.5(2) . . ? C80 Rh30 C30 100.6(2) . . ? C70 Rh30 C10 96.6(2) . . ? C80 Rh30 C10 97.4(2) . . ? C30 Rh30 C10 156.15(19) . . ? C70 Rh30 Rh31 96.80(17) . . ? C80 Rh30 Rh31 149.91(18) . . ? C30 Rh30 Rh31 50.20(14) . . ? C10 Rh30 Rh31 109.00(13) . . ? C70 Rh30 Rh40 148.94(17) . . ? C80 Rh30 Rh40 97.32(17) . . ? C30 Rh30 Rh40 52.03(13) . . ? C10 Rh30 Rh40 110.29(13) . . ? Rh31 Rh30 Rh40 60.460(14) . . ? C70 Rh30 Rh10 95.27(18) . . ? C80 Rh30 Rh10 145.68(18) . . ? C30 Rh30 Rh10 110.63(14) . . ? C10 Rh30 Rh10 48.80(13) . . ? Rh31 Rh30 Rh10 60.690(14) . . ? Rh40 Rh30 Rh10 91.206(17) . . ? C70 Rh30 Rh20 146.92(17) . . ? C80 Rh30 Rh20 95.95(17) . . ? C30 Rh30 Rh20 111.28(13) . . ? C10 Rh30 Rh20 50.93(13) . . ? Rh31 Rh30 Rh20 89.852(16) . . ? Rh40 Rh30 Rh20 59.952(14) . . ? Rh10 Rh30 Rh20 60.130(14) . . ? C71 Rh31 C81 93.3(2) . . ? C71 Rh31 C30 99.4(2) . . ? C81 Rh31 C30 101.4(2) . . ? C71 Rh31 C11 96.5(2) . . ? C81 Rh31 C11 97.6(2) . . ? C30 Rh31 C11 154.42(19) . . ? C71 Rh31 Rh30 97.49(17) . . ? C81 Rh31 Rh30 152.01(18) . . ? C30 Rh31 Rh30 51.45(14) . . ? C11 Rh31 Rh30 106.71(13) . . ? C71 Rh31 Rh40 150.34(18) . . ? C81 Rh31 Rh40 99.61(16) . . ? C30 Rh31 Rh40 52.04(13) . . ? C11 Rh31 Rh40 107.95(13) . . ? Rh30 Rh31 Rh40 60.016(14) . . ? C71 Rh31 Rh21 145.52(19) . . ? C81 Rh31 Rh21 95.32(16) . . ? C30 Rh31 Rh21 111.44(13) . . ? C11 Rh31 Rh21 49.25(13) . . ? Rh30 Rh31 Rh21 90.232(16) . . ? Rh40 Rh31 Rh21 59.776(14) . . ? C71 Rh31 Rh10 94.01(17) . . ? C81 Rh31 Rh10 144.50(18) . . ? C30 Rh31 Rh10 111.57(14) . . ? C11 Rh31 Rh10 47.09(13) . . ? Rh30 Rh31 Rh10 60.389(14) . . ? Rh40 Rh31 Rh10 90.775(16) . . ? Rh21 Rh31 Rh10 60.988(14) . . ? C90 Rh40 C91 94.1(2) . . ? C90 Rh40 C20 99.4(2) . . ? C91 Rh40 C20 99.7(2) . . ? C90 Rh40 C30 96.2(2) . . ? C91 Rh40 C30 95.7(2) . . ? C20 Rh40 C30 157.1(2) . . ? C90 Rh40 Rh30 94.16(19) . . ? C91 Rh40 Rh30 146.16(16) . . ? C20 Rh40 Rh30 111.19(14) . . ? C30 Rh40 Rh30 50.78(14) . . ? C90 Rh40 Rh21 149.69(19) . . ? C91 Rh40 Rh21 98.71(18) . . ? C20 Rh40 Rh21 51.43(14) . . ? C30 Rh40 Rh21 109.54(14) . . ? Rh30 Rh40 Rh21 90.268(17) . . ? C90 Rh40 Rh31 144.83(19) . . ? C91 Rh40 Rh31 97.02(16) . . ? C20 Rh40 Rh31 111.29(14) . . ? C30 Rh40 Rh31 49.57(14) . . ? Rh30 Rh40 Rh31 59.524(14) . . ? Rh21 Rh40 Rh31 60.327(14) . . ? C90 Rh40 Rh20 97.10(19) . . ? C91 Rh40 Rh20 149.81(17) . . ? C20 Rh40 Rh20 50.88(14) . . ? C30 Rh40 Rh20 110.73(14) . . ? Rh30 Rh40 Rh20 60.644(14) . . ? Rh21 Rh40 Rh20 59.483(14) . . ? Rh31 Rh40 Rh20 89.715(17) . . ? O10 C10 Rh10 137.8(4) . . ? O10 C10 Rh20 130.5(4) . . ? Rh10 C10 Rh20 79.74(17) . . ? O10 C10 Rh30 130.1(4) . . ? Rh10 C10 Rh30 78.87(17) . . ? Rh20 C10 Rh30 77.34(17) . . ? O11 C11 Rh10 138.1(4) . . ? O11 C11 Rh21 131.7(4) . . ? Rh10 C11 Rh21 82.70(19) . . ? O11 C11 Rh31 128.5(4) . . ? Rh10 C11 Rh31 76.92(18) . . ? Rh21 C11 Rh31 75.08(17) . . ? O20 C20 Rh40 134.5(4) . . ? O20 C20 Rh20 133.0(4) . . ? Rh40 C20 Rh20 78.56(18) . . ? O20 C20 Rh21 132.8(4) . . ? Rh40 C20 Rh21 77.98(17) . . ? Rh20 C20 Rh21 77.16(17) . . ? O30 C30 Rh31 135.3(4) . . ? O30 C30 Rh30 132.9(4) . . ? Rh31 C30 Rh30 78.36(19) . . ? O30 C30 Rh40 132.0(4) . . ? Rh31 C30 Rh40 78.40(18) . . ? Rh30 C30 Rh40 77.19(17) . . ? O40 C40 Rh10 178.0(5) . . ? O50 C50 Rh20 177.1(6) . . ? O51 C51 Rh21 172.3(6) . . ? O60 C60 Rh20 178.0(6) . . ? O61 C61 Rh21 177.5(5) . . ? O70 C70 Rh30 178.0(5) . . ? O71 C71 Rh31 179.1(6) . . ? O80 C80 Rh30 179.1(6) . . ? O81 C81 Rh31 179.5(5) . . ? O90 C90 Rh40 177.9(6) . . ? O91 C91 Rh40 178.1(5) . . ? C221 P C311 106.3(17) . . ? C221 P C211 3.7(19) . . ? C311 P C211 107.9(8) . . ? C221 P C321 101(2) . . ? C311 P C321 12.3(15) . . ? C211 P C321 102.3(14) . . ? C221 P C111 105.9(11) . . ? C311 P C111 98.8(13) . . ? C211 P C111 108.7(8) . . ? C321 P C111 111.1(16) . . ? C221 P C121 101.5(12) . . ? C311 P C121 101.8(16) . . ? C211 P C121 104.2(10) . . ? C321 P C121 114.0(18) . . ? C111 P C121 4.7(18) . . ? C221 P Rh10 116.1(15) . . ? C311 P Rh10 111.9(3) . . ? C211 P Rh10 112.5(7) . . ? C321 P Rh10 105.4(8) . . ? C111 P Rh10 116.0(5) . . ? C121 P Rh10 117.6(10) . . ? C112 C111 P 113.5(8) . . ? C113 C112 C111 110.6(10) . . ? C114 C113 C112 112.1(15) . . ? C122 C121 P 122.1(14) . . ? C123 C122 C121 116.3(16) . . ? C124 C123 C122 128(3) . . ? C212 C211 P 111.6(6) . . ? C213 C212 C211 111.8(7) . . ? C214 C213 C212 110.3(12) . . ? C222 C221 P 125.4(16) . . ? C221 C222 C223 120.2(18) . . ? C224 C223 C222 109(2) . . ? C312 C311 P 115.1(7) . . ? C311 C312 C313 109.0(9) . . ? C314 C313 C312 115.4(10) . . ? C322 C321 P 125.1(14) . . ? C321 C322 C323 118.9(13) . . ? C324 C323 C322 110.2(16) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.673 _refine_diff_density_min -1.074 _refine_diff_density_rms 0.161 #======END data_s9508 _database_code_CSD 163535 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '7 Rh6(CO)15(Me2SO)' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H6 O16 Rh6 S' _chemical_formula_weight 1115.74 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.400(2) _cell_length_b 9.841(2) _cell_length_c 14.668(3) _cell_angle_alpha 99.080(10) _cell_angle_beta 96.830(10) _cell_angle_gamma 96.270(10) _cell_volume 1319.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 53 _cell_measurement_theta_min 6.35 _cell_measurement_theta_max 10.02 _exptl_crystal_description 'needle' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.809 _exptl_crystal_density_method none _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 3.820 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.4804 _exptl_absorpt_correction_T_max 0.7546 _exptl_absorpt_process_details 'SHELXTL' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'Less than 2' _diffrn_reflns_number 3695 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.1050 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3443 _reflns_number_observed 1936 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w==1/[\s^2^(Fo^2^)+(0.0367P)^2^] 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 0.00039(14) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3443 _refine_ls_number_parameters 365 _refine_ls_number_restraints 180 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_all 0.0908 _refine_ls_wR_factor_ref 0.0817 _refine_ls_goodness_of_fit_all 0.810 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 0.798 _refine_ls_restrained_S_obs 0.980 _refine_ls_shift/su_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh10 Rh 0.47656(12) 0.75563(12) 0.73023(7) 0.0154(3) Uani 1 d . . Rh20 Rh 0.23454(12) 0.57903(12) 0.64033(7) 0.0170(3) Uani 1 d . . Rh21 Rh 0.20213(12) 0.81912(12) 0.75375(7) 0.0171(3) Uani 1 d . . Rh30 Rh 0.41151(12) 0.50460(12) 0.78256(7) 0.0173(3) Uani 1 d . . Rh31 Rh 0.38024(12) 0.74992(12) 0.89771(7) 0.0168(3) Uani 1 d . . Rh40 Rh 0.14106(12) 0.56825(12) 0.81105(7) 0.0191(3) Uani 1 d . . S S 0.5248(4) 0.8870(4) 0.6173(2) 0.0198(8) Uani 1 d . . C1 C 0.6459(16) 1.0377(15) 0.6651(10) 0.035(4) Uani 1 d . . H1A H 0.6734(73) 1.0855(50) 0.6149(12) 0.042(18) Uiso 1 calc R . H1B H 0.7323(42) 1.0120(17) 0.6990(50) 0.042(18) Uiso 1 calc R . H1C H 0.5992(35) 1.0994(42) 0.7080(47) 0.042(18) Uiso 1 calc R . C2 C 0.6294(16) 0.7998(16) 0.5404(10) 0.034(4) Uani 1 d . . H2A H 0.6546(79) 0.8580(40) 0.4948(38) 0.042(18) Uiso 1 calc R . H2B H 0.5737(38) 0.7120(44) 0.5078(45) 0.042(18) Uiso 1 calc R . H2C H 0.7180(47) 0.7809(81) 0.5759(12) 0.042(18) Uiso 1 calc R . O1 O 0.4019(10) 0.9275(10) 0.5622(7) 0.033(3) Uani 1 d . . C10 C 0.4685(14) 0.5551(13) 0.6475(8) 0.013(3) Uani 1 d U . O10 O 0.5355(10) 0.5036(10) 0.5965(6) 0.024(2) Uani 1 d U . C11 C 0.4140(14) 0.9289(15) 0.8167(9) 0.020(3) Uani 1 d U . O11 O 0.4599(10) 1.0419(10) 0.8414(6) 0.026(3) Uani 1 d U . C20 C 0.0390(16) 0.6435(14) 0.6910(10) 0.025(3) Uani 1 d U . O20 O -0.0792(10) 0.6349(10) 0.6546(7) 0.028(2) Uani 1 d U . C30 C 0.3234(14) 0.5344(15) 0.9143(9) 0.021(3) Uani 1 d U . O30 O 0.3305(10) 0.4814(10) 0.9779(7) 0.029(2) Uani 1 d U . C40 C 0.6725(16) 0.7764(14) 0.7800(9) 0.021(3) Uani 1 d U . O40 O 0.7894(11) 0.7894(12) 0.8103(7) 0.038(3) Uani 1 d U . C50 C 0.2204(16) 0.6424(15) 0.5235(10) 0.026(4) Uani 1 d U . O50 O 0.2110(11) 0.6734(11) 0.4523(7) 0.039(3) Uani 1 d U . C51 C 0.1499(15) 0.9125(14) 0.6526(10) 0.024(3) Uani 1 d U . O51 O 0.1036(11) 0.9643(11) 0.5956(7) 0.038(3) Uani 1 d U . C60 C 0.1530(15) 0.3927(17) 0.5832(9) 0.022(4) Uani 1 d . . O60 O 0.1018(11) 0.2823(11) 0.5530(7) 0.035(3) Uani 1 d . . C61 C 0.1023(15) 0.9305(14) 0.8354(9) 0.022(3) Uani 1 d U . O61 O 0.0455(11) 1.0031(11) 0.8851(7) 0.043(3) Uani 1 d U . C70 C 0.6031(16) 0.4685(15) 0.8160(10) 0.026(4) Uani 1 d U . O70 O 0.7168(12) 0.4415(12) 0.8280(7) 0.041(3) Uani 1 d U . C71 C 0.5687(15) 0.7873(13) 0.9674(8) 0.014(3) Uani 1 d U . O71 O 0.6810(10) 0.8120(10) 1.0090(6) 0.028(2) Uani 1 d U . C80 C 0.3461(16) 0.3150(16) 0.7470(10) 0.030(4) Uani 1 d U . O80 O 0.3047(14) 0.1999(12) 0.7227(8) 0.057(3) Uani 1 d U . C81 C 0.2931(14) 0.8348(14) 0.9989(9) 0.021(3) Uani 1 d U . O81 O 0.2375(11) 0.8813(11) 1.0592(7) 0.036(3) Uani 1 d U . C90 C 0.0404(16) 0.3852(17) 0.7826(10) 0.029(4) Uani 1 d U . O90 O -0.0189(12) 0.2755(11) 0.7680(8) 0.048(3) Uani 1 d U . C91 C 0.0263(14) 0.6226(13) 0.9030(8) 0.015(3) Uani 1 d U . O91 O -0.0394(11) 0.6581(11) 0.9637(7) 0.039(3) Uani 1 d U . 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 Rh10 0.0156(6) 0.0169(7) 0.0138(6) 0.0013(5) 0.0039(5) 0.0021(5) Rh20 0.0186(7) 0.0157(7) 0.0163(6) 0.0017(5) 0.0014(5) 0.0026(5) Rh21 0.0166(6) 0.0160(7) 0.0188(7) 0.0019(5) 0.0024(5) 0.0044(5) Rh30 0.0189(7) 0.0152(7) 0.0186(6) 0.0040(5) 0.0028(5) 0.0039(5) Rh31 0.0180(7) 0.0194(7) 0.0129(6) 0.0012(5) 0.0029(5) 0.0028(5) Rh40 0.0170(7) 0.0197(7) 0.0208(6) 0.0043(5) 0.0046(5) 0.0006(5) S 0.024(2) 0.019(2) 0.018(2) 0.005(2) 0.006(2) 0.004(2) C1 0.033(9) 0.034(10) 0.038(9) 0.009(8) 0.008(8) -0.005(8) C2 0.038(10) 0.038(10) 0.035(9) 0.011(8) 0.028(8) 0.017(8) O1 0.033(6) 0.039(7) 0.036(6) 0.025(5) 0.014(5) 0.006(5) C10 0.017(6) 0.009(6) 0.012(6) 0.004(5) -0.001(5) 0.001(5) O10 0.027(5) 0.028(6) 0.017(5) -0.001(4) 0.012(4) 0.011(5) C11 0.020(6) 0.020(7) 0.018(6) -0.006(6) 0.004(5) 0.006(6) O11 0.020(6) 0.026(6) 0.027(6) -0.003(5) -0.003(4) 0.004(5) C20 0.022(7) 0.013(6) 0.040(7) 0.004(6) 0.000(6) 0.003(6) O20 0.019(6) 0.024(6) 0.037(6) 0.004(5) -0.006(5) -0.004(5) C30 0.019(6) 0.025(7) 0.023(6) 0.005(6) 0.008(5) 0.004(5) O30 0.034(6) 0.027(6) 0.032(6) 0.023(5) 0.007(5) 0.005(5) C40 0.022(7) 0.022(7) 0.020(6) 0.004(5) 0.008(6) 0.005(6) O40 0.018(6) 0.058(7) 0.033(6) 0.003(5) -0.001(5) -0.005(5) C50 0.032(7) 0.020(7) 0.028(7) 0.005(6) 0.003(6) 0.010(6) O50 0.047(7) 0.043(7) 0.027(6) 0.001(5) 0.008(5) 0.014(5) C51 0.022(7) 0.012(6) 0.036(7) -0.007(6) 0.006(6) 0.005(6) O51 0.041(7) 0.039(7) 0.036(6) 0.024(6) -0.008(5) 0.004(5) C60 0.019(8) 0.044(11) 0.009(7) 0.009(7) 0.001(6) 0.024(8) O60 0.042(7) 0.021(6) 0.039(6) -0.003(5) 0.008(5) -0.003(5) C61 0.022(3) 0.022(3) 0.023(3) 0.0034(11) 0.0031(11) 0.0029(11) O61 0.042(3) 0.042(3) 0.043(3) 0.004(2) 0.008(2) 0.007(2) C70 0.021(7) 0.025(7) 0.032(7) 0.011(6) 0.003(6) -0.002(6) O70 0.028(6) 0.057(8) 0.039(6) 0.006(5) 0.008(5) 0.013(6) C71 0.022(7) 0.015(6) 0.009(6) 0.007(5) 0.006(5) 0.005(5) O71 0.022(6) 0.033(6) 0.025(5) -0.001(5) 0.000(5) 0.005(5) C80 0.035(7) 0.023(7) 0.031(7) 0.011(6) -0.005(6) 0.006(6) O80 0.074(8) 0.021(7) 0.070(8) 0.002(6) -0.016(7) 0.012(6) C81 0.020(3) 0.021(3) 0.021(3) 0.0033(11) 0.0031(11) 0.0028(11) O81 0.036(3) 0.038(3) 0.034(3) 0.002(2) 0.008(2) 0.006(2) C90 0.028(7) 0.039(8) 0.024(7) 0.014(6) 0.012(6) -0.001(6) O90 0.055(7) 0.027(7) 0.061(7) 0.003(6) 0.018(6) -0.010(6) C91 0.015(3) 0.016(3) 0.015(3) 0.0030(11) 0.0024(11) 0.0018(11) O91 0.039(3) 0.041(3) 0.039(3) 0.005(2) 0.008(2) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh10 C40 1.875(15) . ? Rh10 C10 2.136(13) . ? Rh10 C11 2.140(13) . ? Rh10 S 2.312(3) . ? Rh10 Rh31 2.724(2) . ? Rh10 Rh30 2.729(2) . ? Rh10 Rh20 2.763(2) . ? Rh10 Rh21 2.768(2) . ? Rh20 C50 1.91(2) . ? Rh20 C60 1.93(2) . ? Rh20 C20 2.183(14) . ? Rh20 C10 2.229(13) . ? Rh20 Rh21 2.735(2) . ? Rh20 Rh30 2.753(2) . ? Rh20 Rh40 2.764(2) . ? Rh21 C51 1.91(2) . ? Rh21 C61 1.896(14) . ? Rh21 C11 2.183(14) . ? Rh21 C20 2.184(14) . ? Rh21 Rh31 2.755(2) . ? Rh21 Rh40 2.755(2) . ? Rh30 C80 1.87(2) . ? Rh30 C70 1.90(2) . ? Rh30 C30 2.182(13) . ? Rh30 C10 2.228(12) . ? Rh30 Rh40 2.747(2) . ? Rh30 Rh31 2.785(2) . ? Rh31 C81 1.902(13) . ? Rh31 C71 1.904(14) . ? Rh31 C30 2.188(15) . ? Rh31 C11 2.290(15) . ? Rh31 Rh40 2.755(2) . ? Rh40 C91 1.875(12) . ? Rh40 C90 1.90(2) . ? Rh40 C20 2.176(15) . ? Rh40 C30 2.238(14) . ? S O1 1.459(10) . ? S C1 1.760(14) . ? S C2 1.766(13) . ? C10 O10 1.129(14) . ? C11 O11 1.133(15) . ? C20 O20 1.16(2) . ? C30 O30 1.14(2) . ? C40 O40 1.12(2) . ? C50 O50 1.13(2) . ? C51 O51 1.12(2) . ? C60 O60 1.14(2) . ? C61 O61 1.16(2) . ? C70 O70 1.13(2) . ? C71 O71 1.136(15) . ? C80 O80 1.14(2) . ? C81 O81 1.140(15) . ? C90 O90 1.14(2) . ? C91 O91 1.173(14) . ? 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 C40 Rh10 C10 97.0(5) . . ? C40 Rh10 C11 98.7(5) . . ? C10 Rh10 C11 161.2(5) . . ? C40 Rh10 S 92.0(4) . . ? C10 Rh10 S 98.0(3) . . ? C11 Rh10 S 91.9(4) . . ? C40 Rh10 Rh31 94.3(4) . . ? C10 Rh10 Rh31 113.8(3) . . ? C11 Rh10 Rh31 54.6(4) . . ? S Rh10 Rh31 146.44(10) . . ? C40 Rh10 Rh30 94.7(4) . . ? C10 Rh10 Rh30 52.8(3) . . ? C11 Rh10 Rh30 115.3(4) . . ? S Rh10 Rh30 150.61(10) . . ? Rh31 Rh10 Rh30 61.42(4) . . ? C40 Rh10 Rh20 147.7(4) . . ? C10 Rh10 Rh20 52.2(3) . . ? C11 Rh10 Rh20 110.1(4) . . ? S Rh10 Rh20 101.27(10) . . ? Rh31 Rh10 Rh20 90.63(5) . . ? Rh30 Rh10 Rh20 60.17(4) . . ? C40 Rh10 Rh21 147.4(4) . . ? C10 Rh10 Rh21 111.3(3) . . ? C11 Rh10 Rh21 50.9(4) . . ? S Rh10 Rh21 99.30(10) . . ? Rh31 Rh10 Rh21 60.21(4) . . ? Rh30 Rh10 Rh21 90.27(5) . . ? Rh20 Rh10 Rh21 59.28(4) . . ? C50 Rh20 C60 92.5(6) . . ? C50 Rh20 C20 100.6(6) . . ? C60 Rh20 C20 97.0(5) . . ? C50 Rh20 C10 95.4(5) . . ? C60 Rh20 C10 99.3(5) . . ? C20 Rh20 C10 156.7(5) . . ? C50 Rh20 Rh21 99.3(4) . . ? C60 Rh20 Rh21 147.5(4) . . ? C20 Rh20 Rh21 51.2(4) . . ? C10 Rh20 Rh21 109.5(3) . . ? C50 Rh20 Rh30 147.0(4) . . ? C60 Rh20 Rh30 95.9(4) . . ? C20 Rh20 Rh30 109.9(4) . . ? C10 Rh20 Rh30 51.8(3) . . ? Rh21 Rh20 Rh30 90.45(5) . . ? C50 Rh20 Rh10 98.5(4) . . ? C60 Rh20 Rh10 147.3(4) . . ? C20 Rh20 Rh10 110.9(4) . . ? C10 Rh20 Rh10 49.3(3) . . ? Rh21 Rh20 Rh10 60.45(4) . . ? Rh30 Rh20 Rh10 59.30(4) . . ? C50 Rh20 Rh40 150.6(4) . . ? C60 Rh20 Rh40 96.1(4) . . ? C20 Rh20 Rh40 50.5(4) . . ? C10 Rh20 Rh40 110.8(3) . . ? Rh21 Rh20 Rh40 60.13(4) . . ? Rh30 Rh20 Rh40 59.73(4) . . ? Rh10 Rh20 Rh40 89.19(5) . . ? C51 Rh21 C61 92.7(6) . . ? C51 Rh21 C11 103.5(6) . . ? C61 Rh21 C11 93.5(5) . . ? C51 Rh21 C20 90.1(6) . . ? C61 Rh21 C20 103.2(6) . . ? C11 Rh21 C20 158.0(5) . . ? C51 Rh21 Rh20 94.0(4) . . ? C61 Rh21 Rh20 153.5(4) . . ? C11 Rh21 Rh20 109.7(3) . . ? C20 Rh21 Rh20 51.2(4) . . ? C51 Rh21 Rh31 156.8(4) . . ? C61 Rh21 Rh31 93.3(4) . . ? C11 Rh21 Rh31 53.8(4) . . ? C20 Rh21 Rh31 110.3(4) . . ? Rh20 Rh21 Rh31 90.58(5) . . ? C51 Rh21 Rh40 140.6(4) . . ? C61 Rh21 Rh40 99.3(4) . . ? C11 Rh21 Rh40 113.0(4) . . ? C20 Rh21 Rh40 50.7(4) . . ? Rh20 Rh21 Rh40 60.46(4) . . ? Rh31 Rh21 Rh40 60.01(4) . . ? C51 Rh21 Rh10 104.1(4) . . ? C61 Rh21 Rh10 141.7(4) . . ? C11 Rh21 Rh10 49.5(3) . . ? C20 Rh21 Rh10 110.8(4) . . ? Rh20 Rh21 Rh10 60.28(4) . . ? Rh31 Rh21 Rh10 59.11(4) . . ? Rh40 Rh21 Rh10 89.28(5) . . ? C80 Rh30 C70 91.5(6) . . ? C80 Rh30 C30 97.2(6) . . ? C70 Rh30 C30 104.2(6) . . ? C80 Rh30 C10 100.2(5) . . ? C70 Rh30 C10 90.2(5) . . ? C30 Rh30 C10 157.1(5) . . ? C80 Rh30 Rh10 148.2(4) . . ? C70 Rh30 Rh10 98.0(4) . . ? C30 Rh30 Rh10 109.6(4) . . ? C10 Rh30 Rh10 49.8(3) . . ? C80 Rh30 Rh40 92.8(5) . . ? C70 Rh30 Rh40 156.7(4) . . ? C30 Rh30 Rh40 52.5(4) . . ? C10 Rh30 Rh40 111.5(3) . . ? Rh10 Rh30 Rh40 90.25(5) . . ? C80 Rh30 Rh20 94.0(4) . . ? C70 Rh30 Rh20 142.1(4) . . ? C30 Rh30 Rh20 112.2(4) . . ? C10 Rh30 Rh20 51.9(3) . . ? Rh10 Rh30 Rh20 60.53(4) . . ? Rh40 Rh30 Rh20 60.34(4) . . ? C80 Rh30 Rh31 145.7(5) . . ? C70 Rh30 Rh31 106.3(4) . . ? C30 Rh30 Rh31 50.5(4) . . ? C10 Rh30 Rh31 108.7(3) . . ? Rh10 Rh30 Rh31 59.20(4) . . ? Rh40 Rh30 Rh31 59.74(4) . . ? Rh20 Rh30 Rh31 89.58(5) . . ? C81 Rh31 C71 93.0(5) . . ? C81 Rh31 C30 97.3(5) . . ? C71 Rh31 C30 99.7(5) . . ? C81 Rh31 C11 101.2(5) . . ? C71 Rh31 C11 94.8(5) . . ? C30 Rh31 C11 155.7(5) . . ? C81 Rh31 Rh10 150.4(4) . . ? C71 Rh31 Rh10 94.4(4) . . ? C30 Rh31 Rh10 109.6(3) . . ? C11 Rh31 Rh10 49.6(3) . . ? C81 Rh31 Rh21 98.4(4) . . ? C71 Rh31 Rh21 144.7(4) . . ? C30 Rh31 Rh21 111.7(4) . . ? C11 Rh31 Rh21 50.2(3) . . ? Rh10 Rh31 Rh21 60.68(4) . . ? C81 Rh31 Rh40 96.9(4) . . ? C71 Rh31 Rh40 151.2(4) . . ? C30 Rh31 Rh40 52.3(4) . . ? C11 Rh31 Rh40 109.5(3) . . ? Rh10 Rh31 Rh40 90.19(5) . . ? Rh21 Rh31 Rh40 60.01(4) . . ? C81 Rh31 Rh30 146.9(4) . . ? C71 Rh31 Rh30 99.0(4) . . ? C30 Rh31 Rh30 50.3(3) . . ? C11 Rh31 Rh30 108.3(3) . . ? Rh10 Rh31 Rh30 59.38(4) . . ? Rh21 Rh31 Rh30 89.39(5) . . ? Rh40 Rh31 Rh30 59.46(4) . . ? C91 Rh40 C90 92.3(6) . . ? C91 Rh40 C20 102.5(5) . . ? C90 Rh40 C20 97.0(6) . . ? C91 Rh40 C30 93.6(5) . . ? C90 Rh40 C30 99.3(6) . . ? C20 Rh40 C30 156.6(5) . . ? C91 Rh40 Rh30 143.8(4) . . ? C90 Rh40 Rh30 98.2(4) . . ? C20 Rh40 Rh30 110.4(4) . . ? C30 Rh40 Rh30 50.7(3) . . ? C91 Rh40 Rh21 99.3(4) . . ? C90 Rh40 Rh21 147.5(4) . . ? C20 Rh40 Rh21 50.9(4) . . ? C30 Rh40 Rh21 110.1(4) . . ? Rh30 Rh40 Rh21 90.15(5) . . ? C91 Rh40 Rh31 94.0(4) . . ? C90 Rh40 Rh31 149.6(5) . . ? C20 Rh40 Rh31 110.5(4) . . ? C30 Rh40 Rh31 50.7(4) . . ? Rh30 Rh40 Rh31 60.80(4) . . ? Rh21 Rh40 Rh31 59.99(4) . . ? C91 Rh40 Rh20 152.2(4) . . ? C90 Rh40 Rh20 98.0(4) . . ? C20 Rh40 Rh20 50.8(4) . . ? C30 Rh40 Rh20 110.0(3) . . ? Rh30 Rh40 Rh20 59.93(4) . . ? Rh21 Rh40 Rh20 59.41(4) . . ? Rh31 Rh40 Rh20 89.95(5) . . ? O1 S C1 108.2(7) . . ? O1 S C2 108.5(7) . . ? C1 S C2 100.5(7) . . ? O1 S Rh10 117.5(4) . . ? C1 S Rh10 111.2(5) . . ? C2 S Rh10 109.6(5) . . ? O10 C10 Rh10 136.4(10) . . ? O10 C10 Rh30 131.3(10) . . ? Rh10 C10 Rh30 77.4(4) . . ? O10 C10 Rh20 133.5(10) . . ? Rh10 C10 Rh20 78.5(4) . . ? Rh30 C10 Rh20 76.3(4) . . ? O11 C11 Rh10 135.6(10) . . ? O11 C11 Rh21 134.9(11) . . ? Rh10 C11 Rh21 79.6(5) . . ? O11 C11 Rh31 130.9(10) . . ? Rh10 C11 Rh31 75.8(5) . . ? Rh21 C11 Rh31 76.0(5) . . ? O20 C20 Rh40 134.4(11) . . ? O20 C20 Rh20 132.0(11) . . ? Rh40 C20 Rh20 78.7(5) . . ? O20 C20 Rh21 133.3(11) . . ? Rh40 C20 Rh21 78.4(5) . . ? Rh20 C20 Rh21 77.6(5) . . ? O30 C30 Rh30 134.4(11) . . ? O30 C30 Rh31 132.2(11) . . ? Rh30 C30 Rh31 79.2(5) . . ? O30 C30 Rh40 134.1(11) . . ? Rh30 C30 Rh40 76.8(5) . . ? Rh31 C30 Rh40 77.0(5) . . ? O40 C40 Rh10 179.5(10) . . ? O50 C50 Rh20 176.6(13) . . ? O51 C51 Rh21 172.0(13) . . ? O60 C60 Rh20 176.8(11) . . ? O61 C61 Rh21 177.2(12) . . ? O70 C70 Rh30 173.9(13) . . ? O71 C71 Rh31 178.8(12) . . ? O80 C80 Rh30 178.0(13) . . ? O81 C81 Rh31 177.5(12) . . ? O90 C90 Rh40 178.2(13) . . ? O91 C91 Rh40 176.7(11) . . ? _refine_diff_density_max 0.975 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.190 #======END data_s9556 _database_code_CSD 163536 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '8 Rh6(CO)15(MeCN)' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H3 N O15 Rh6' _chemical_formula_weight 1078.66 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.099(4) _cell_length_b 9.6260(10) _cell_length_c 17.080(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.390(10) _cell_angle_gamma 90.00 _cell_volume 2563.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 0.55 _cell_measurement_theta_max 10.98 _exptl_crystal_description 'plate' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.795 _exptl_crystal_density_method none _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 3.845 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.3769 _exptl_absorpt_correction_T_max 0.7538 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.85 _diffrn_reflns_number 5777 _diffrn_reflns_av_R_equivalents 0.0817 _diffrn_reflns_av_sigmaI/netI 0.1134 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5580 _reflns_number_gt 2689 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w==1/[\s^2^(Fo^2^)+(0.0607P)^2^] 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 0.00014(7) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5580 _refine_ls_number_parameters 364 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1555 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_all 0.1645 _refine_ls_wR_factor_ref 0.1255 _refine_ls_goodness_of_fit_all 1.010 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.009 _refine_ls_restrained_S_obs 1.142 _refine_ls_shift/su_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh10 Rh 0.73567(9) 0.32856(12) 0.93120(8) 0.0246(3) Uani 1 d . . Rh20 Rh 0.85314(8) 0.1217(2) 0.98829(7) 0.0278(3) Uani 1 d . . Rh21 Rh 0.76705(7) 0.1247(2) 0.82850(6) 0.0245(3) Uani 1 d . . Rh30 Rh 0.69990(8) 0.1303(2) 1.03195(6) 0.0251(3) Uani 1 d . . Rh31 Rh 0.61281(7) 0.13411(15) 0.87058(6) 0.0225(3) Uani 1 d . . Rh40 Rh 0.73022(9) -0.07462(13) 0.92844(8) 0.0249(3) Uani 1 d . . N1 N 0.8204(13) 0.4626(20) 0.9017(9) 0.051(5) Uani 0.70 d P 1 C1 C 0.8632(14) 0.5402(24) 0.8860(13) 0.069(6) Uani 0.70 d PU 1 C2 C 0.9408(20) 0.5865(32) 0.8425(18) 0.061(9) Uani 0.70 d PU 1 H2A H 0.9944(38) 0.5409(167) 0.8702(82) 0.091 Uiso 0.70 calc PR 1 H2B H 0.9483(89) 0.6875(38) 0.8461(108) 0.091 Uiso 0.70 calc PR 1 H2C H 0.9252(65) 0.5584(192) 0.7856(38) 0.091 Uiso 0.70 calc PR 1 C10 C 0.8019(10) 0.2891(20) 1.0532(9) 0.032(4) Uani 1 d . . O10 O 0.8367(8) 0.3552(16) 1.1096(6) 0.045(3) Uani 1 d . . C11 C 0.6697(11) 0.2878(20) 0.8037(9) 0.032(4) Uani 1 d . . O11 O 0.6429(8) 0.3619(14) 0.7507(6) 0.040(3) Uani 1 d . . C20 C 0.8490(10) -0.0358(21) 0.8960(10) 0.036(4) Uani 1 d . . O20 O 0.9001(8) -0.1040(14) 0.8801(7) 0.041(3) Uani 1 d . . C30 C 0.6083(11) -0.0312(17) 0.9606(10) 0.029(4) Uani 1 d . . O30 O 0.5569(7) -0.0956(11) 0.9748(7) 0.034(3) Uani 1 d . . C40 C 0.6589(10) 0.4690(19) 0.9538(9) 0.027(4) Uani 1 d . . O40 O 0.6140(9) 0.5455(15) 0.9649(8) 0.052(4) Uani 1 d . . C50 C 0.9517(12) 0.2241(21) 0.9765(10) 0.037(4) Uani 1 d . . O50 O 1.0071(8) 0.2915(16) 0.9716(7) 0.053(4) Uani 1 d . . C51 C 0.8562(12) 0.2215(23) 0.7920(9) 0.045(5) Uani 0.70 d P 1 O51 O 0.9077(12) 0.2747(18) 0.7725(9) 0.059(5) Uani 0.70 d P 1 C60 C 0.9102(10) 0.0217(20) 1.0817(10) 0.035(4) Uani 1 d U . O60 O 0.9430(9) -0.0421(18) 1.1368(8) 0.063(5) Uani 1 d . . C61 C 0.7292(10) 0.0175(20) 0.7308(10) 0.032(4) Uani 1 d . . O61 O 0.7075(9) -0.0440(15) 0.6743(7) 0.047(4) Uani 1 d . . C70 C 0.6209(11) 0.2391(19) 1.0715(9) 0.031(4) Uani 1 d U . O70 O 0.5741(8) 0.3065(14) 1.0954(7) 0.045(3) Uani 1 d . . C71 C 0.5175(10) 0.2331(17) 0.8858(8) 0.025(4) Uani 1 d . . O71 O 0.4565(8) 0.2883(16) 0.8934(7) 0.051(4) Uani 1 d . . C80 C 0.7344(13) 0.0178(20) 1.1267(10) 0.041(5) Uani 1 d . . O80 O 0.7572(10) -0.0474(16) 1.1823(7) 0.057(4) Uani 1 d . . C81 C 0.5489(12) 0.0438(18) 0.7760(11) 0.037(4) Uani 1 d . . O81 O 0.5089(9) -0.0016(15) 0.7181(7) 0.051(4) Uani 1 d . . C90 C 0.7753(12) -0.2159(18) 1.0110(10) 0.033(4) Uani 1 d . . O90 O 0.7993(11) -0.2932(17) 1.0587(9) 0.068(5) Uani 1 d . . C91 C 0.6809(13) -0.2068(20) 0.8449(11) 0.040(5) Uani 1 d . . O91 O 0.6547(11) -0.2843(15) 0.7996(8) 0.061(4) Uani 1 d . . C3 C 0.8204(13) 0.4626(20) 0.9017(9) 0.051(5) Uani 0.30 d P 2 O3 O 0.8632(14) 0.5402(24) 0.8860(13) 0.069(6) Uani 0.30 d P 2 N2 N 0.8562(12) 0.2215(23) 0.7920(9) 0.045(5) Uani 0.30 d P 2 C4 C 0.9077(12) 0.2747(18) 0.7725(9) 0.059(5) Uani 0.30 d P 2 C5 C 1.0052(55) 0.3422(104) 0.7792(48) 0.082(26) Uani 0.30 d PU 2 H5A H 1.0046(106) 0.4416(156) 0.7913(330) 0.123 Uiso 0.30 calc PR 2 H5B H 1.0208(166) 0.3292(539) 0.7278(131) 0.123 Uiso 0.30 calc PR 2 H5C H 1.0474(77) 0.2952(411) 0.8224(244) 0.123 Uiso 0.30 calc PR 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 Rh10 0.0271(6) 0.0224(7) 0.0240(5) 0.0010(6) 0.0055(5) -0.0042(6) Rh20 0.0229(6) 0.0308(7) 0.0277(6) 0.0045(6) 0.0026(5) -0.0018(6) Rh21 0.0246(6) 0.0261(7) 0.0237(5) 0.0017(6) 0.0079(5) -0.0040(6) Rh30 0.0284(6) 0.0264(7) 0.0213(5) 0.0031(6) 0.0077(5) 0.0032(6) Rh31 0.0217(6) 0.0221(6) 0.0235(5) -0.0008(6) 0.0053(4) -0.0009(6) Rh40 0.0249(6) 0.0219(6) 0.0285(6) 0.0021(6) 0.0076(5) 0.0019(6) N1 0.069(13) 0.039(12) 0.036(9) -0.002(8) -0.006(9) 0.011(10) C1 0.068(9) 0.061(9) 0.077(9) 0.018(8) 0.012(8) -0.025(8) C2 0.073(16) 0.032(14) 0.072(15) -0.002(12) 0.011(13) -0.020(12) C10 0.019(8) 0.044(11) 0.029(8) -0.010(8) -0.001(7) -0.005(8) O10 0.038(7) 0.059(10) 0.033(6) -0.006(7) -0.001(5) -0.001(7) C11 0.035(10) 0.044(11) 0.026(8) -0.010(8) 0.022(7) -0.008(9) O11 0.054(8) 0.038(8) 0.029(5) 0.019(6) 0.011(5) 0.010(7) C20 0.020(8) 0.047(12) 0.043(10) -0.027(9) 0.013(7) -0.009(8) O20 0.036(7) 0.043(9) 0.047(7) 0.007(6) 0.017(6) 0.013(7) C30 0.030(9) 0.022(9) 0.039(9) 0.024(7) 0.015(7) 0.017(8) O30 0.034(7) 0.016(7) 0.056(7) 0.005(5) 0.017(6) -0.006(5) C40 0.019(8) 0.032(10) 0.033(8) -0.009(7) 0.009(7) -0.003(7) O40 0.063(10) 0.042(9) 0.052(8) 0.000(7) 0.015(7) 0.018(8) C50 0.035(11) 0.037(11) 0.038(9) 0.001(8) 0.010(8) -0.001(9) O50 0.035(8) 0.063(10) 0.057(8) 0.004(8) 0.005(7) -0.021(7) C51 0.047(11) 0.065(14) 0.022(8) 0.011(9) 0.011(8) 0.008(10) O51 0.080(13) 0.056(11) 0.049(9) 0.014(8) 0.031(9) -0.009(10) C60 0.019(7) 0.039(8) 0.039(7) -0.002(6) -0.005(6) 0.000(6) O60 0.038(8) 0.093(13) 0.052(8) 0.024(9) 0.002(7) 0.017(8) C61 0.020(8) 0.042(11) 0.033(9) -0.004(8) 0.007(7) -0.016(8) O61 0.052(8) 0.055(9) 0.039(7) -0.014(7) 0.020(6) -0.021(7) C70 0.035(7) 0.026(7) 0.032(7) 0.006(6) 0.009(6) -0.009(6) O70 0.036(7) 0.047(9) 0.049(7) -0.016(7) 0.007(6) 0.002(6) C71 0.034(9) 0.020(8) 0.026(7) 0.003(6) 0.015(7) 0.014(7) O71 0.041(8) 0.074(11) 0.043(7) 0.009(7) 0.017(6) 0.031(8) C80 0.053(13) 0.032(11) 0.039(10) 0.007(9) 0.013(9) 0.011(10) O80 0.079(11) 0.062(10) 0.032(7) 0.021(7) 0.017(7) 0.024(9) C81 0.043(11) 0.017(9) 0.047(10) 0.008(8) 0.005(9) 0.002(8) O81 0.050(9) 0.055(10) 0.042(7) -0.015(7) 0.000(6) -0.018(7) C90 0.045(11) 0.016(9) 0.038(9) 0.009(7) 0.011(8) -0.006(8) O90 0.076(12) 0.055(11) 0.074(10) 0.024(9) 0.022(9) 0.013(9) C91 0.051(12) 0.024(11) 0.046(10) 0.014(9) 0.016(9) 0.010(9) O91 0.092(13) 0.034(9) 0.056(8) -0.018(7) 0.019(8) -0.027(8) C3 0.069(13) 0.039(12) 0.036(9) -0.002(8) -0.006(9) 0.011(10) O3 0.068(9) 0.061(9) 0.077(9) 0.018(8) 0.012(8) -0.025(8) N2 0.047(11) 0.065(14) 0.022(8) 0.011(9) 0.011(8) 0.008(10) C4 0.080(13) 0.056(11) 0.049(9) 0.014(8) 0.031(9) -0.009(10) C5 0.084(31) 0.079(32) 0.082(30) -0.001(19) 0.019(19) 0.009(19) _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 Rh10 C40 1.93(2) . ? Rh10 C3 2.03(2) . ? Rh10 N1 2.03(2) . ? Rh10 C10 2.13(2) . ? Rh10 C11 2.21(2) . ? Rh10 Rh30 2.726(2) . ? Rh10 Rh31 2.733(2) . ? Rh10 Rh20 2.752(2) . ? Rh10 Rh21 2.761(2) . ? Rh20 C60 1.89(2) . ? Rh20 C50 1.92(2) . ? Rh20 C20 2.18(2) . ? Rh20 C10 2.23(2) . ? Rh20 Rh21 2.737(2) . ? Rh20 Rh40 2.744(2) . ? Rh20 Rh30 2.750(2) . ? Rh21 C61 1.93(2) . ? Rh21 N2 1.94(2) . ? Rh21 C51 1.94(2) . ? Rh21 C20 2.17(2) . ? Rh21 C11 2.18(2) . ? Rh21 Rh40 2.729(2) . ? Rh21 Rh31 2.753(2) . ? Rh30 C70 1.90(2) . ? Rh30 C80 1.91(2) . ? Rh30 C10 2.21(2) . ? Rh30 C30 2.28(2) . ? Rh30 Rh31 2.765(2) . ? Rh30 Rh40 2.772(2) . ? Rh31 C71 1.878(15) . ? Rh31 C81 1.90(2) . ? Rh31 C11 2.20(2) . ? Rh31 C30 2.226(15) . ? Rh31 Rh40 2.767(2) . ? Rh40 C91 1.93(2) . ? Rh40 C90 1.96(2) . ? Rh40 C20 2.15(2) . ? Rh40 C30 2.21(2) . ? N1 C1 1.09(3) . ? C1 C2 1.66(3) . ? C10 O10 1.17(2) . ? C11 O11 1.15(2) . ? C20 O20 1.14(2) . ? C30 O30 1.11(2) . ? C40 O40 1.08(2) . ? C50 O50 1.12(2) . ? C51 O51 1.09(2) . ? C60 O60 1.14(2) . ? C61 O61 1.11(2) . ? C70 O70 1.14(2) . ? C71 O71 1.15(2) . ? C80 O80 1.12(2) . ? C81 O81 1.13(2) . ? C90 O90 1.10(2) . ? C91 O91 1.08(2) . ? C3 O3 1.09(3) . ? N2 C4 1.09(2) . ? C4 C5 1.68(9) . ? 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 C40 Rh10 C3 96.1(7) . . ? C40 Rh10 N1 96.1(7) . . ? C40 Rh10 C10 96.8(7) . . ? C3 Rh10 C10 98.8(7) . . ? N1 Rh10 C10 98.8(7) . . ? C40 Rh10 C11 98.4(7) . . ? C3 Rh10 C11 93.3(6) . . ? N1 Rh10 C11 93.3(6) . . ? C10 Rh10 C11 159.4(7) . . ? C40 Rh10 Rh30 96.8(5) . . ? C3 Rh10 Rh30 149.6(5) . . ? N1 Rh10 Rh30 149.6(5) . . ? C10 Rh10 Rh30 52.3(5) . . ? C11 Rh10 Rh30 111.9(5) . . ? C40 Rh10 Rh31 96.7(5) . . ? C3 Rh10 Rh31 144.0(5) . . ? N1 Rh10 Rh31 144.0(5) . . ? C10 Rh10 Rh31 112.8(5) . . ? C11 Rh10 Rh31 51.6(5) . . ? Rh30 Rh10 Rh31 60.86(5) . . ? C40 Rh10 Rh20 148.4(5) . . ? C3 Rh10 Rh20 95.9(5) . . ? N1 Rh10 Rh20 95.9(5) . . ? C10 Rh10 Rh20 52.4(5) . . ? C11 Rh10 Rh20 109.9(5) . . ? Rh30 Rh10 Rh20 60.27(5) . . ? Rh31 Rh10 Rh20 90.44(5) . . ? C40 Rh10 Rh21 148.3(4) . . ? C3 Rh10 Rh21 93.1(5) . . ? N1 Rh10 Rh21 93.1(5) . . ? C10 Rh10 Rh21 111.7(5) . . ? C11 Rh10 Rh21 50.7(5) . . ? Rh30 Rh10 Rh21 90.23(5) . . ? Rh31 Rh10 Rh21 60.13(5) . . ? Rh20 Rh10 Rh21 59.52(5) . . ? C60 Rh20 C50 96.2(7) . . ? C60 Rh20 C20 100.2(8) . . ? C50 Rh20 C20 99.2(7) . . ? C60 Rh20 C10 96.3(7) . . ? C50 Rh20 C10 95.7(7) . . ? C20 Rh20 C10 156.4(6) . . ? C60 Rh20 Rh21 149.8(6) . . ? C50 Rh20 Rh21 96.7(5) . . ? C20 Rh20 Rh21 50.8(5) . . ? C10 Rh20 Rh21 109.3(4) . . ? C60 Rh20 Rh40 96.8(5) . . ? C50 Rh20 Rh40 148.5(5) . . ? C20 Rh20 Rh40 50.3(4) . . ? C10 Rh20 Rh40 111.2(4) . . ? Rh21 Rh20 Rh40 59.74(5) . . ? C60 Rh20 Rh30 93.8(5) . . ? C50 Rh20 Rh30 146.4(6) . . ? C20 Rh20 Rh30 110.4(4) . . ? C10 Rh20 Rh30 51.3(4) . . ? Rh21 Rh20 Rh30 90.23(5) . . ? Rh40 Rh20 Rh30 60.60(5) . . ? C60 Rh20 Rh10 144.4(5) . . ? C50 Rh20 Rh10 96.0(6) . . ? C20 Rh20 Rh10 110.6(5) . . ? C10 Rh20 Rh10 49.2(4) . . ? Rh21 Rh20 Rh10 60.40(5) . . ? Rh40 Rh20 Rh10 89.88(5) . . ? Rh30 Rh20 Rh10 59.39(5) . . ? C61 Rh21 N2 94.5(7) . . ? C61 Rh21 C51 94.5(7) . . ? C61 Rh21 C20 95.7(7) . . ? N2 Rh21 C20 96.5(7) . . ? C51 Rh21 C20 96.5(7) . . ? C61 Rh21 C11 99.2(7) . . ? N2 Rh21 C11 98.3(7) . . ? C51 Rh21 C11 98.3(7) . . ? C20 Rh21 C11 158.1(6) . . ? C61 Rh21 Rh40 95.4(5) . . ? N2 Rh21 Rh40 146.3(5) . . ? C51 Rh21 Rh40 146.3(5) . . ? C20 Rh21 Rh40 50.5(4) . . ? C11 Rh21 Rh40 111.7(4) . . ? C61 Rh21 Rh20 146.2(6) . . ? N2 Rh21 Rh20 95.4(5) . . ? C51 Rh21 Rh20 95.4(5) . . ? C20 Rh21 Rh20 51.1(4) . . ? C11 Rh21 Rh20 111.2(4) . . ? Rh40 Rh21 Rh20 60.26(5) . . ? C61 Rh21 Rh31 97.6(5) . . ? N2 Rh21 Rh31 148.8(6) . . ? C51 Rh21 Rh31 148.8(6) . . ? C20 Rh21 Rh31 110.7(4) . . ? C11 Rh21 Rh31 51.4(4) . . ? Rh40 Rh21 Rh31 60.63(5) . . ? Rh20 Rh21 Rh31 90.35(5) . . ? C61 Rh21 Rh10 149.5(5) . . ? N2 Rh21 Rh10 97.4(6) . . ? C51 Rh21 Rh10 97.4(6) . . ? C20 Rh21 Rh10 110.6(4) . . ? C11 Rh21 Rh10 51.4(4) . . ? Rh40 Rh21 Rh10 89.99(5) . . ? Rh20 Rh21 Rh10 60.08(5) . . ? Rh31 Rh21 Rh10 59.43(5) . . ? C70 Rh30 C80 95.2(7) . . ? C70 Rh30 C10 95.5(7) . . ? C80 Rh30 C10 101.8(8) . . ? C70 Rh30 C30 99.5(6) . . ? C80 Rh30 C30 94.6(7) . . ? C10 Rh30 C30 156.6(6) . . ? C70 Rh30 Rh10 96.0(5) . . ? C80 Rh30 Rh10 150.3(6) . . ? C10 Rh30 Rh10 49.7(4) . . ? C30 Rh30 Rh10 110.5(4) . . ? C70 Rh30 Rh20 147.1(5) . . ? C80 Rh30 Rh20 97.0(6) . . ? C10 Rh30 Rh20 52.0(5) . . ? C30 Rh30 Rh20 109.9(4) . . ? Rh10 Rh30 Rh20 60.34(5) . . ? C70 Rh30 Rh31 97.4(5) . . ? C80 Rh30 Rh31 145.1(6) . . ? C10 Rh30 Rh31 109.1(4) . . ? C30 Rh30 Rh31 51.3(4) . . ? Rh10 Rh30 Rh31 59.70(5) . . ? Rh20 Rh30 Rh31 89.82(5) . . ? C70 Rh30 Rh40 149.3(5) . . ? C80 Rh30 Rh40 94.4(6) . . ? C10 Rh30 Rh40 110.9(4) . . ? C30 Rh30 Rh40 50.7(4) . . ? Rh10 Rh30 Rh40 89.84(5) . . ? Rh20 Rh30 Rh40 59.58(5) . . ? Rh31 Rh30 Rh40 59.98(5) . . ? C71 Rh31 C81 93.5(7) . . ? C71 Rh31 C11 100.9(7) . . ? C81 Rh31 C11 94.2(7) . . ? C71 Rh31 C30 95.7(6) . . ? C81 Rh31 C30 99.0(7) . . ? C11 Rh31 C30 158.0(6) . . ? C71 Rh31 Rh10 98.0(5) . . ? C81 Rh31 Rh10 145.6(5) . . ? C11 Rh31 Rh10 51.8(4) . . ? C30 Rh31 Rh10 111.9(5) . . ? C71 Rh31 Rh21 150.9(5) . . ? C81 Rh31 Rh21 95.5(6) . . ? C11 Rh31 Rh21 50.9(5) . . ? C30 Rh31 Rh21 110.1(4) . . ? Rh10 Rh31 Rh21 60.44(5) . . ? C71 Rh31 Rh30 95.6(4) . . ? C81 Rh31 Rh30 151.2(5) . . ? C11 Rh31 Rh30 110.7(4) . . ? C30 Rh31 Rh30 53.0(5) . . ? Rh10 Rh31 Rh30 59.44(5) . . ? Rh21 Rh31 Rh30 89.60(5) . . ? C71 Rh31 Rh40 145.9(4) . . ? C81 Rh31 Rh40 98.6(5) . . ? C11 Rh31 Rh40 109.8(5) . . ? C30 Rh31 Rh40 51.0(4) . . ? Rh10 Rh31 Rh40 89.78(5) . . ? Rh21 Rh31 Rh40 59.26(5) . . ? Rh30 Rh31 Rh40 60.14(5) . . ? C91 Rh40 C90 94.9(7) . . ? C91 Rh40 C20 98.8(7) . . ? C90 Rh40 C20 96.5(8) . . ? C91 Rh40 C30 94.6(8) . . ? C90 Rh40 C30 98.3(6) . . ? C20 Rh40 C30 159.1(6) . . ? C91 Rh40 Rh21 96.6(5) . . ? C90 Rh40 Rh21 146.8(5) . . ? C20 Rh40 Rh21 51.1(5) . . ? C30 Rh40 Rh21 111.6(4) . . ? C91 Rh40 Rh20 148.9(6) . . ? C90 Rh40 Rh20 96.1(5) . . ? C20 Rh40 Rh20 51.1(4) . . ? C30 Rh40 Rh20 112.4(5) . . ? Rh21 Rh40 Rh20 60.01(5) . . ? C91 Rh40 Rh31 95.5(5) . . ? C90 Rh40 Rh31 149.0(5) . . ? C20 Rh40 Rh31 110.7(6) . . ? C30 Rh40 Rh31 51.7(4) . . ? Rh21 Rh40 Rh31 60.10(5) . . ? Rh20 Rh40 Rh31 89.90(5) . . ? C91 Rh40 Rh30 146.7(6) . . ? C90 Rh40 Rh30 97.3(5) . . ? C20 Rh40 Rh30 110.5(5) . . ? C30 Rh40 Rh30 53.0(5) . . ? Rh21 Rh40 Rh30 89.93(5) . . ? Rh20 Rh40 Rh30 59.82(5) . . ? Rh31 Rh40 Rh30 59.88(4) . . ? C1 N1 Rh10 176.4(21) . . ? N1 C1 C2 151.8(26) . . ? O10 C10 Rh10 136.7(16) . . ? O10 C10 Rh30 134.1(13) . . ? Rh10 C10 Rh30 77.9(5) . . ? O10 C10 Rh20 129.8(13) . . ? Rh10 C10 Rh20 78.4(5) . . ? Rh30 C10 Rh20 76.7(6) . . ? O11 C11 Rh21 135.2(12) . . ? O11 C11 Rh31 134.6(14) . . ? Rh21 C11 Rh31 77.7(6) . . ? O11 C11 Rh10 131.4(15) . . ? Rh21 C11 Rh10 77.9(6) . . ? Rh31 C11 Rh10 76.6(5) . . ? O20 C20 Rh40 134.7(16) . . ? O20 C20 Rh21 131.8(14) . . ? Rh40 C20 Rh21 78.4(6) . . ? O20 C20 Rh20 132.9(13) . . ? Rh40 C20 Rh20 78.7(5) . . ? Rh21 C20 Rh20 78.1(6) . . ? O30 C30 Rh40 135.1(14) . . ? O30 C30 Rh31 134.9(13) . . ? Rh40 C30 Rh31 77.3(5) . . ? O30 C30 Rh30 133.2(14) . . ? Rh40 C30 Rh30 76.4(6) . . ? Rh31 C30 Rh30 75.7(5) . . ? O40 C40 Rh10 177.8(16) . . ? O50 C50 Rh20 175.3(18) . . ? O51 C51 Rh21 178.6(18) . . ? O60 C60 Rh20 177.8(18) . . ? O61 C61 Rh21 179.7(11) . . ? O70 C70 Rh30 178.8(15) . . ? O71 C71 Rh31 176.6(17) . . ? O80 C80 Rh30 177.9(19) . . ? O81 C81 Rh31 175.5(16) . . ? O90 C90 Rh40 178.0(17) . . ? O91 C91 Rh40 177.6(17) . . ? O3 C3 Rh10 176.4(21) . . ? C4 N2 Rh21 178.6(18) . . ? N2 C4 C5 158.1(33) . . ? _refine_diff_density_max 1.386 _refine_diff_density_min -1.204 _refine_diff_density_rms 0.255 #======END data_s9612 _database_code_CSD 163537 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '9 Rh6(CO)15(C8H14)' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C23 H14 O15 Rh6' _chemical_formula_weight 1147.80 _chemical_melting_point ? _chemical_compound_source ? 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' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.466(2) _cell_length_b 9.832(3) _cell_length_c 16.608(4) _cell_angle_alpha 103.07(2) _cell_angle_beta 94.50(3) _cell_angle_gamma 98.62(3) _cell_volume 1478.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 0.44 _cell_measurement_theta_max 9.92 _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.578 _exptl_crystal_density_method ? _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 3.341 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.382 _exptl_absorpt_correction_T_max 0.782 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 13.93 _diffrn_reflns_number 6809 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.1353 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6411 _reflns_number_gt 3257 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w==1/[\s^2^(Fo^2^)+(0.0700P)^2^] 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 6411 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1318 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_all 0.1579 _refine_ls_wR_factor_ref 0.1300 _refine_ls_goodness_of_fit_all 0.885 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 0.885 _refine_ls_restrained_S_obs 1.050 _refine_ls_shift/su_max -0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh10 Rh 0.53463(11) -0.23143(11) 0.25047(7) 0.0195(3) Uani 1 d . . Rh20 Rh 0.80905(12) -0.28658(11) 0.21685(7) 0.0204(3) Uani 1 d . . Rh21 Rh 0.78612(12) -0.03444(11) 0.31825(7) 0.0208(3) Uani 1 d . . Rh30 Rh 0.61881(11) -0.24013(12) 0.09425(7) 0.0205(3) Uani 1 d . . Rh31 Rh 0.59645(12) 0.01631(11) 0.19816(7) 0.0210(3) Uani 1 d . . Rh40 Rh 0.86236(12) -0.04327(12) 0.15990(7) 0.0218(3) Uani 1 d . . C1 C 0.4837(17) -0.4046(17) 0.3248(10) 0.037(4) Uani 1 d . . H1A H 0.5709(17) -0.4373(17) 0.3464(10) 0.179(95) Uiso 1 calc R . C2 C 0.4621(17) -0.2784(16) 0.3707(9) 0.031(3) Uani 1 d . . H2A H 0.5377(17) -0.2382(16) 0.4193(9) 0.179(95) Uiso 1 calc R . C3 C 0.3128(19) -0.2452(20) 0.3907(11) 0.048(5) Uani 1 d . . H3A H 0.3163(19) -0.1415(20) 0.4010(11) 0.134(32) Uiso 1 calc R . H3B H 0.2421(19) -0.2907(20) 0.3412(11) 0.134(32) Uiso 1 calc R . C4 C 0.2590(28) -0.2944(23) 0.4659(11) 0.072(7) Uani 1 d . . H4A H 0.1781(28) -0.2462(23) 0.4837(11) 0.134(32) Uiso 1 calc R . H4B H 0.3374(28) -0.2662(23) 0.5126(11) 0.134(32) Uiso 1 calc R . C5 C 0.2088(31) -0.4556(26) 0.4468(18) 0.099(10) Uani 1 d . . H5A H 0.1552(31) -0.4734(26) 0.4933(18) 0.134(32) Uiso 1 calc R . H5B H 0.1373(31) -0.4799(26) 0.3968(18) 0.134(32) Uiso 1 calc R . C6 C 0.2987(38) -0.5553(29) 0.4336(20) 0.118(12) Uani 1 d . . H6A H 0.2565(38) -0.6347(29) 0.4566(20) 0.134(32) Uiso 1 calc R . H6B H 0.3912(38) -0.5115(29) 0.4683(20) 0.134(32) Uiso 1 calc R . C7 C 0.3358(22) -0.6221(23) 0.3455(15) 0.063(6) Uani 1 d . . H7A H 0.2566(22) -0.7009(23) 0.3184(15) 0.134(32) Uiso 1 calc R . H7B H 0.4235(22) -0.6639(23) 0.3522(15) 0.134(32) Uiso 1 calc R . C8 C 0.3612(19) -0.5232(16) 0.2853(10) 0.040(4) Uani 1 d . . H8A H 0.3847(19) -0.5772(16) 0.2316(10) 0.134(32) Uiso 1 calc R . H8B H 0.2730(19) -0.4841(16) 0.2745(10) 0.134(32) Uiso 1 calc R . C10 C 0.5946(15) -0.4064(16) 0.1645(8) 0.026(3) Uani 1 d . . O10 O 0.5525(10) -0.5283(10) 0.1395(6) 0.028(2) Uani 1 d . . C11 C 0.5564(15) -0.0177(15) 0.3236(9) 0.025(3) Uani 1 d . . O11 O 0.4977(11) 0.0507(10) 0.3744(6) 0.030(2) Uani 1 d . . C20 C 0.9766(15) -0.0979(16) 0.2636(8) 0.027(3) Uani 1 d . . O20 O 1.0951(10) -0.0801(10) 0.2907(6) 0.028(2) Uani 1 d . . C30 C 0.6711(15) -0.0266(13) 0.0766(9) 0.025(3) Uani 1 d . . O30 O 0.6617(11) 0.0191(12) 0.0192(6) 0.035(3) Uani 1 d . . C40 C 0.3435(15) -0.2620(16) 0.2058(9) 0.031(4) Uani 1 d . . O40 O 0.2270(11) -0.2846(13) 0.1756(7) 0.045(3) Uani 1 d . . C50 C 0.8505(15) -0.3677(16) 0.3079(9) 0.028(3) Uani 1 d . . O50 O 0.8808(14) -0.4096(12) 0.3647(7) 0.052(3) Uani 1 d . . C51 C 0.8171(17) -0.0841(18) 0.4229(10) 0.036(4) Uani 1 d . . O51 O 0.8398(14) -0.1062(14) 0.4858(7) 0.055(4) Uani 1 d . . C60 C 0.9097(15) -0.4073(16) 0.1417(9) 0.028(3) Uani 1 d . . O60 O 0.9584(12) -0.4837(12) 0.0960(7) 0.044(3) Uani 1 d . . C61 C 0.8771(17) 0.1574(16) 0.3603(9) 0.034(4) Uani 1 d . . O61 O 0.9445(15) 0.2704(13) 0.3796(8) 0.058(4) Uani 1 d . . C70 C 0.4293(15) -0.2863(13) 0.0353(9) 0.024(3) Uani 1 d . . O70 O 0.3172(10) -0.3141(11) -0.0004(6) 0.033(3) Uani 1 d . . C71 C 0.4012(16) 0.0374(16) 0.1704(9) 0.030(3) Uani 1 d . . O71 O 0.2870(12) 0.0569(14) 0.1588(7) 0.050(3) Uani 1 d . . C80 C 0.7033(15) -0.3325(15) 0.0013(9) 0.025(3) Uani 1 d . . O80 O 0.7542(12) -0.3868(12) -0.0534(7) 0.043(3) Uani 1 d . . C81 C 0.6629(18) 0.2157(16) 0.2264(9) 0.033(4) Uani 1 d . . O81 O 0.7049(14) 0.3315(11) 0.2470(9) 0.062(4) Uani 1 d . . C90 C 0.9776(15) -0.1134(16) 0.0759(9) 0.027(3) Uani 1 d . . O90 O 1.0429(12) -0.1584(12) 0.0249(7) 0.045(3) Uani 1 d . . C91 C 0.9586(15) 0.1453(17) 0.1755(10) 0.031(4) Uani 1 d . . O91 O 1.0178(13) 0.2586(12) 0.1858(8) 0.049(3) Uani 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 Rh10 0.0204(5) 0.0183(5) 0.0193(6) 0.0030(4) 0.0030(5) 0.0031(4) Rh20 0.0203(5) 0.0187(5) 0.0222(6) 0.0046(5) 0.0000(5) 0.0052(4) Rh21 0.0230(6) 0.0184(5) 0.0190(6) 0.0026(5) -0.0006(5) 0.0021(5) Rh30 0.0196(5) 0.0234(6) 0.0169(6) 0.0022(5) 0.0005(4) 0.0041(4) Rh31 0.0217(6) 0.0182(6) 0.0230(6) 0.0050(5) 0.0014(5) 0.0043(5) Rh40 0.0204(6) 0.0233(6) 0.0218(6) 0.0068(5) 0.0018(5) 0.0024(5) C1 0.037(9) 0.043(10) 0.044(10) 0.030(8) 0.013(8) 0.014(8) C2 0.034(8) 0.031(8) 0.023(8) 0.006(6) 0.001(7) -0.001(7) C3 0.046(10) 0.051(11) 0.042(11) -0.005(9) 0.021(9) 0.009(9) C4 0.121(21) 0.069(15) 0.025(10) 0.009(10) 0.026(12) 0.007(14) C5 0.118(23) 0.062(16) 0.116(23) 0.001(15) 0.079(19) 0.015(16) C6 0.164(32) 0.062(18) 0.116(26) 0.013(17) -0.022(24) 0.021(20) C7 0.049(12) 0.061(13) 0.094(18) 0.035(13) 0.022(12) 0.017(10) C8 0.055(11) 0.027(8) 0.037(10) 0.001(7) 0.018(8) 0.007(8) C10 0.027(7) 0.034(8) 0.018(7) 0.000(6) 0.006(6) 0.018(6) O10 0.029(6) 0.023(5) 0.032(6) 0.006(5) 0.008(5) 0.001(4) C11 0.024(7) 0.026(7) 0.023(8) 0.009(6) -0.001(6) -0.006(6) O11 0.035(6) 0.026(5) 0.028(6) 0.004(5) 0.013(5) 0.001(5) C20 0.027(8) 0.038(8) 0.018(7) 0.013(6) -0.002(6) 0.009(6) O20 0.021(5) 0.032(6) 0.029(6) 0.014(5) -0.001(4) -0.007(4) C30 0.027(7) 0.015(6) 0.028(8) -0.003(6) -0.006(6) 0.008(6) O30 0.038(6) 0.047(7) 0.023(6) 0.021(5) -0.008(5) 0.004(5) C40 0.020(7) 0.034(8) 0.030(8) -0.005(7) 0.004(6) 0.003(6) O40 0.026(6) 0.055(8) 0.046(7) 0.001(6) -0.006(5) 0.009(5) C50 0.018(6) 0.034(8) 0.029(8) 0.003(7) -0.005(6) 0.006(6) O50 0.071(9) 0.038(7) 0.044(8) 0.017(6) -0.018(7) 0.003(6) C51 0.038(9) 0.046(10) 0.027(9) 0.014(8) 0.003(7) 0.011(8) O51 0.066(9) 0.062(9) 0.034(7) 0.022(6) -0.013(6) -0.005(7) C60 0.025(7) 0.038(9) 0.020(7) 0.005(7) -0.001(6) 0.004(7) O60 0.040(6) 0.050(7) 0.038(7) -0.013(6) 0.014(5) 0.024(6) C61 0.041(9) 0.027(8) 0.026(8) -0.001(7) 0.000(7) -0.001(7) O61 0.075(10) 0.035(7) 0.049(8) -0.001(6) 0.012(7) -0.020(7) C70 0.028(7) 0.013(6) 0.025(8) -0.005(6) 0.006(6) 0.000(6) O70 0.022(5) 0.039(6) 0.030(6) -0.005(5) -0.006(5) 0.002(5) C71 0.035(8) 0.035(8) 0.013(7) -0.007(6) -0.001(6) 0.009(7) O71 0.033(6) 0.076(9) 0.040(7) 0.001(6) -0.003(5) 0.033(6) C80 0.026(7) 0.031(8) 0.019(7) 0.009(6) 0.011(6) 0.001(6) O80 0.038(6) 0.051(7) 0.031(6) -0.007(6) 0.011(5) 0.005(6) C81 0.052(10) 0.035(9) 0.018(8) 0.016(7) 0.002(7) 0.014(8) O81 0.065(9) 0.013(6) 0.099(11) 0.014(6) -0.021(8) -0.002(6) C90 0.028(8) 0.032(8) 0.023(8) 0.007(6) 0.002(6) 0.008(6) O90 0.044(7) 0.043(7) 0.044(7) 0.000(6) 0.022(6) 0.006(6) C91 0.017(7) 0.038(9) 0.035(9) 0.004(7) 0.002(6) 0.008(6) O91 0.054(8) 0.038(7) 0.047(8) 0.016(6) 0.005(6) -0.022(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh10 C40 1.855(14) . ? Rh10 C11 2.147(14) . ? Rh10 C10 2.151(13) . ? Rh10 C2 2.28(2) . ? Rh10 C1 2.335(15) . ? Rh10 Rh30 2.760(2) . ? Rh10 Rh31 2.764(2) . ? Rh10 Rh20 2.805(2) . ? Rh10 Rh21 2.810(2) . ? Rh20 C50 1.90(2) . ? Rh20 C60 1.931(15) . ? Rh20 C10 2.192(15) . ? Rh20 C20 2.198(15) . ? Rh20 Rh21 2.713(2) . ? Rh20 Rh40 2.759(2) . ? Rh20 Rh30 2.773(2) . ? Rh21 C61 1.900(15) . ? Rh21 C51 1.92(2) . ? Rh21 C20 2.191(15) . ? Rh21 C11 2.213(14) . ? Rh21 Rh31 2.758(2) . ? Rh21 Rh40 2.767(2) . ? Rh30 C80 1.905(14) . ? Rh30 C70 1.913(14) . ? Rh30 C30 2.175(14) . ? Rh30 C10 2.209(15) . ? Rh30 Rh40 2.750(2) . ? Rh30 Rh31 2.762(2) . ? Rh31 C81 1.90(2) . ? Rh31 C71 1.923(15) . ? Rh31 C30 2.16(2) . ? Rh31 C11 2.235(14) . ? Rh31 Rh40 2.758(2) . ? Rh40 C91 1.89(2) . ? Rh40 C90 1.91(2) . ? Rh40 C20 2.173(13) . ? Rh40 C30 2.240(13) . ? C1 C2 1.36(2) . ? C1 C8 1.50(2) . ? C2 C3 1.54(2) . ? C3 C4 1.53(2) . ? C4 C5 1.54(3) . ? C5 C6 1.38(3) . ? C6 C7 1.55(4) . ? C7 C8 1.55(2) . ? C10 O10 1.17(2) . ? C11 O11 1.18(2) . ? C20 O20 1.15(2) . ? C30 O30 1.14(2) . ? C40 O40 1.14(2) . ? C50 O50 1.14(2) . ? C51 O51 1.13(2) . ? C60 O60 1.12(2) . ? C61 O61 1.16(2) . ? C70 O70 1.14(2) . ? C71 O71 1.13(2) . ? C80 O80 1.13(2) . ? C81 O81 1.11(2) . ? C90 O90 1.14(2) . ? C91 O91 1.14(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C40 Rh10 C11 100.2(6) . . ? C40 Rh10 C10 96.4(6) . . ? C11 Rh10 C10 156.5(6) . . ? C40 Rh10 C2 89.4(6) . . ? C11 Rh10 C2 81.1(5) . . ? C10 Rh10 C2 115.6(6) . . ? C40 Rh10 C1 90.9(7) . . ? C11 Rh10 C1 114.3(6) . . ? C10 Rh10 C1 81.6(6) . . ? C2 Rh10 C1 34.1(5) . . ? C40 Rh10 Rh30 89.9(5) . . ? C11 Rh10 Rh30 111.7(4) . . ? C10 Rh10 Rh30 51.7(4) . . ? C2 Rh10 Rh30 167.0(4) . . ? C1 Rh10 Rh30 133.0(4) . . ? C40 Rh10 Rh31 92.2(5) . . ? C11 Rh10 Rh31 52.3(4) . . ? C10 Rh10 Rh31 110.9(4) . . ? C2 Rh10 Rh31 133.0(4) . . ? C1 Rh10 Rh31 166.7(4) . . ? Rh30 Rh10 Rh31 60.00(5) . . ? C40 Rh10 Rh20 144.0(4) . . ? C11 Rh10 Rh20 108.5(4) . . ? C10 Rh10 Rh20 50.4(4) . . ? C2 Rh10 Rh20 115.7(4) . . ? C1 Rh10 Rh20 96.4(4) . . ? Rh30 Rh10 Rh20 59.76(5) . . ? Rh31 Rh10 Rh20 88.61(5) . . ? C40 Rh10 Rh21 147.4(5) . . ? C11 Rh10 Rh21 50.9(4) . . ? C10 Rh10 Rh21 107.9(4) . . ? C2 Rh10 Rh21 98.8(4) . . ? C1 Rh10 Rh21 113.4(4) . . ? Rh30 Rh10 Rh21 88.65(5) . . ? Rh31 Rh10 Rh21 59.30(4) . . ? Rh20 Rh10 Rh21 57.78(4) . . ? C50 Rh20 C60 94.3(6) . . ? C50 Rh20 C10 101.5(6) . . ? C60 Rh20 C10 94.6(5) . . ? C50 Rh20 C20 94.3(6) . . ? C60 Rh20 C20 101.1(6) . . ? C10 Rh20 C20 156.8(5) . . ? C50 Rh20 Rh21 92.9(4) . . ? C60 Rh20 Rh21 152.3(5) . . ? C10 Rh20 Rh21 110.0(3) . . ? C20 Rh20 Rh21 51.7(4) . . ? C50 Rh20 Rh40 143.9(4) . . ? C60 Rh20 Rh40 99.6(5) . . ? C10 Rh20 Rh40 110.3(4) . . ? C20 Rh20 Rh40 50.5(3) . . ? Rh21 Rh20 Rh40 60.76(5) . . ? C50 Rh20 Rh30 151.5(4) . . ? C60 Rh20 Rh30 95.8(4) . . ? C10 Rh20 Rh30 51.2(4) . . ? C20 Rh20 Rh30 109.7(3) . . ? Rh21 Rh20 Rh30 90.39(5) . . ? Rh40 Rh20 Rh30 59.63(5) . . ? C50 Rh20 Rh10 98.0(4) . . ? C60 Rh20 Rh10 143.4(4) . . ? C10 Rh20 Rh10 49.1(3) . . ? C20 Rh20 Rh10 112.2(4) . . ? Rh21 Rh20 Rh10 61.21(5) . . ? Rh40 Rh20 Rh10 90.39(5) . . ? Rh30 Rh20 Rh10 59.32(4) . . ? C61 Rh21 C51 94.3(7) . . ? C61 Rh21 C20 93.3(6) . . ? C51 Rh21 C20 99.1(6) . . ? C61 Rh21 C11 101.8(6) . . ? C51 Rh21 C11 96.6(6) . . ? C20 Rh21 C11 157.3(5) . . ? C61 Rh21 Rh20 144.5(5) . . ? C51 Rh21 Rh20 98.1(5) . . ? C20 Rh21 Rh20 51.9(4) . . ? C11 Rh21 Rh20 109.7(4) . . ? C61 Rh21 Rh31 96.0(5) . . ? C51 Rh21 Rh31 148.4(5) . . ? C20 Rh21 Rh31 110.0(3) . . ? C11 Rh21 Rh31 52.0(4) . . ? Rh20 Rh21 Rh31 90.64(5) . . ? C61 Rh21 Rh40 93.2(5) . . ? C51 Rh21 Rh40 148.9(5) . . ? C20 Rh21 Rh40 50.3(3) . . ? C11 Rh21 Rh40 111.2(4) . . ? Rh20 Rh21 Rh40 60.44(5) . . ? Rh31 Rh21 Rh40 59.89(5) . . ? C61 Rh21 Rh10 148.9(5) . . ? C51 Rh21 Rh10 98.6(5) . . ? C20 Rh21 Rh10 112.2(4) . . ? C11 Rh21 Rh10 48.9(4) . . ? Rh20 Rh21 Rh10 61.01(5) . . ? Rh31 Rh21 Rh10 59.52(5) . . ? Rh40 Rh21 Rh10 90.10(5) . . ? C80 Rh30 C70 93.4(6) . . ? C80 Rh30 C30 96.8(6) . . ? C70 Rh30 C30 97.2(5) . . ? C80 Rh30 C10 100.5(5) . . ? C70 Rh30 C10 97.4(6) . . ? C30 Rh30 C10 156.6(5) . . ? C80 Rh30 Rh40 94.4(4) . . ? C70 Rh30 Rh40 149.5(4) . . ? C30 Rh30 Rh40 52.5(3) . . ? C10 Rh30 Rh40 110.1(4) . . ? C80 Rh30 Rh10 149.7(4) . . ? C70 Rh30 Rh10 96.4(4) . . ? C30 Rh30 Rh10 110.3(4) . . ? C10 Rh30 Rh10 49.8(3) . . ? Rh40 Rh30 Rh10 91.51(5) . . ? C80 Rh30 Rh31 145.9(4) . . ? C70 Rh30 Rh31 99.0(4) . . ? C30 Rh30 Rh31 50.3(4) . . ? C10 Rh30 Rh31 109.1(3) . . ? Rh40 Rh30 Rh31 60.05(5) . . ? Rh10 Rh30 Rh31 60.07(5) . . ? C80 Rh30 Rh20 97.0(4) . . ? C70 Rh30 Rh20 147.7(4) . . ? C30 Rh30 Rh20 111.7(3) . . ? C10 Rh30 Rh20 50.7(4) . . ? Rh40 Rh30 Rh20 59.93(5) . . ? Rh10 Rh30 Rh20 60.91(5) . . ? Rh31 Rh30 Rh20 89.30(5) . . ? C81 Rh31 C71 92.7(7) . . ? C81 Rh31 C30 96.7(6) . . ? C71 Rh31 C30 101.4(5) . . ? C81 Rh31 C11 100.2(6) . . ? C71 Rh31 C11 93.4(6) . . ? C30 Rh31 C11 157.0(5) . . ? C81 Rh31 Rh21 94.3(4) . . ? C71 Rh31 Rh21 144.7(5) . . ? C30 Rh31 Rh21 112.1(3) . . ? C11 Rh31 Rh21 51.3(4) . . ? C81 Rh31 Rh40 92.9(5) . . ? C71 Rh31 Rh40 153.7(4) . . ? C30 Rh31 Rh40 52.5(3) . . ? C11 Rh31 Rh40 110.8(4) . . ? Rh21 Rh31 Rh40 60.23(5) . . ? C81 Rh31 Rh30 145.5(5) . . ? C71 Rh31 Rh30 103.6(4) . . ? C30 Rh31 Rh30 50.6(3) . . ? C11 Rh31 Rh30 108.8(4) . . ? Rh21 Rh31 Rh30 89.67(5) . . ? Rh40 Rh31 Rh30 59.76(5) . . ? C81 Rh31 Rh10 148.4(4) . . ? C71 Rh31 Rh10 97.3(5) . . ? C30 Rh31 Rh10 110.4(3) . . ? C11 Rh31 Rh10 49.5(4) . . ? Rh21 Rh31 Rh10 61.18(5) . . ? Rh40 Rh31 Rh10 91.25(5) . . ? Rh30 Rh31 Rh10 59.93(5) . . ? C91 Rh40 C90 92.4(6) . . ? C91 Rh40 C20 98.8(6) . . ? C90 Rh40 C20 98.1(6) . . ? C91 Rh40 C30 97.0(5) . . ? C90 Rh40 C30 98.3(5) . . ? C20 Rh40 C30 156.7(6) . . ? C91 Rh40 Rh30 147.2(4) . . ? C90 Rh40 Rh30 95.7(4) . . ? C20 Rh40 Rh30 111.4(4) . . ? C30 Rh40 Rh30 50.4(4) . . ? C91 Rh40 Rh31 97.9(4) . . ? C90 Rh40 Rh31 147.5(4) . . ? C20 Rh40 Rh31 110.5(4) . . ? C30 Rh40 Rh31 50.0(4) . . ? Rh30 Rh40 Rh31 60.19(5) . . ? C91 Rh40 Rh20 149.6(5) . . ? C90 Rh40 Rh20 96.8(5) . . ? C20 Rh40 Rh20 51.3(4) . . ? C30 Rh40 Rh20 110.1(4) . . ? Rh30 Rh40 Rh20 60.44(5) . . ? Rh31 Rh40 Rh20 89.68(6) . . ? C91 Rh40 Rh21 100.0(5) . . ? C90 Rh40 Rh21 147.9(4) . . ? C20 Rh40 Rh21 50.9(4) . . ? C30 Rh40 Rh21 109.3(4) . . ? Rh30 Rh40 Rh21 89.73(6) . . ? Rh31 Rh40 Rh21 59.88(5) . . ? Rh20 Rh40 Rh21 58.80(5) . . ? C2 C1 C8 122.2(14) . . ? C2 C1 Rh10 70.8(9) . . ? C8 C1 Rh10 115.6(11) . . ? C1 C2 C3 123.7(14) . . ? C1 C2 Rh10 75.1(9) . . ? C3 C2 Rh10 116.0(11) . . ? C4 C3 C2 114.9(17) . . ? C3 C4 C5 112.6(17) . . ? C6 C5 C4 124.9(27) . . ? C5 C6 C7 122.3(26) . . ? C6 C7 C8 117.4(18) . . ? C1 C8 C7 108.6(15) . . ? O10 C10 Rh10 137.3(12) . . ? O10 C10 Rh20 131.6(10) . . ? Rh10 C10 Rh20 80.4(5) . . ? O10 C10 Rh30 128.7(10) . . ? Rh10 C10 Rh30 78.5(5) . . ? Rh20 C10 Rh30 78.1(5) . . ? O11 C11 Rh10 139.4(11) . . ? O11 C11 Rh21 131.3(10) . . ? Rh10 C11 Rh21 80.2(5) . . ? O11 C11 Rh31 127.7(11) . . ? Rh10 C11 Rh31 78.2(5) . . ? Rh21 C11 Rh31 76.6(5) . . ? O20 C20 Rh40 134.6(12) . . ? O20 C20 Rh21 131.8(11) . . ? Rh40 C20 Rh21 78.7(4) . . ? O20 C20 Rh20 134.1(11) . . ? Rh40 C20 Rh20 78.3(4) . . ? Rh21 C20 Rh20 76.3(5) . . ? O30 C30 Rh31 135.7(11) . . ? O30 C30 Rh30 132.8(11) . . ? Rh31 C30 Rh30 79.1(5) . . ? O30 C30 Rh40 131.8(12) . . ? Rh31 C30 Rh40 77.5(5) . . ? Rh30 C30 Rh40 77.1(4) . . ? O40 C40 Rh10 177.3(13) . . ? O50 C50 Rh20 176.2(13) . . ? O51 C51 Rh21 176.3(15) . . ? O60 C60 Rh20 174.8(13) . . ? O61 C61 Rh21 172.0(15) . . ? O70 C70 Rh30 179.4(13) . . ? O71 C71 Rh31 175.4(12) . . ? O80 C80 Rh30 179.5(12) . . ? O81 C81 Rh31 176.2(13) . . ? O90 C90 Rh40 177.9(14) . . ? O91 C91 Rh40 179.0(12) . . ? _refine_diff_density_max 1.340 _refine_diff_density_min -1.997 _refine_diff_density_rms 0.284 #======END data_k9958 _database_code_CSD 163538 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '10 Rh6(CO)16)' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 O16 Rh6' _chemical_formula_weight 1065.62 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.113(3) _cell_length_b 9.550(2) _cell_length_c 17.013(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.89(3) _cell_angle_gamma 90.00 _cell_volume 2530.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 7346 _cell_measurement_theta_min 4.19 _cell_measurement_theta_max 30.03 _exptl_crystal_description 'block' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.798 _exptl_crystal_density_method none _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 3.896 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Denzo-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method '\f scan and \w scans with \k offsets' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 23768 _diffrn_reflns_av_R_equivalents 0.0800 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.19 _diffrn_reflns_theta_max 30.03 _reflns_number_total 7346 _reflns_number_gt 3908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'Bruker SHELXTL V5.1' _computing_structure_refinement 'Bruker SHELXTL V5.1' _computing_molecular_graphics 'Bruker SHELXTL V5.1' _computing_publication_material 'Bruker SHELXTL V5.1' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w==1/[\s^2^(Fo^2^)+(0.0552P)^2^] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00007(8) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7346 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_all 0.1179 _refine_ls_wR_factor_ref 0.1034 _refine_ls_goodness_of_fit_all 0.942 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 0.942 _refine_ls_restrained_S_obs 1.154 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh1 Rh 0.26624(3) 0.87255(6) 0.32881(3) 0.02277(13) Uani 1 d . . Rh2 Rh 0.11224(3) 0.86510(5) 0.37044(3) 0.02126(12) Uani 1 d . . Rh3 Rh 0.23525(3) 0.66788(6) 0.43210(3) 0.02292(13) Uani 1 d . . Rh4 Rh 0.35304(3) 0.87619(6) 0.49005(3) 0.02587(13) Uani 1 d . . Rh5 Rh 0.23023(3) 1.07477(6) 0.42877(3) 0.02323(13) Uani 1 d . . Rh6 Rh 0.19976(3) 0.86999(6) 0.53281(3) 0.02349(13) Uani 1 d . . C1 C 0.1684(4) 0.7073(8) 0.3044(4) 0.0273(15) Uani 1 d . . O1 O 0.1404(3) 0.6360(5) 0.2502(3) 0.0304(11) Uani 1 d . . C2 C 0.3508(4) 1.0337(8) 0.3961(4) 0.031(2) Uani 1 d . . O2 O 0.4014(3) 1.1072(5) 0.3804(3) 0.0347(12) Uani 1 d . . C3 C 0.1118(4) 1.0259(7) 0.4615(4) 0.0253(14) Uani 1 d . . O3 O 0.0585(3) 1.0971(5) 0.4743(3) 0.0341(11) Uani 1 d . . C4 C 0.3035(4) 0.7135(8) 0.5561(4) 0.031(2) Uani 1 d . . O4 O 0.3352(3) 0.6448(6) 0.6112(3) 0.0385(13) Uani 1 d . . C5 C 0.2293(4) 0.9781(8) 0.2301(4) 0.031(2) Uani 1 d . . O5 O 0.2078(3) 1.0443(6) 0.1738(3) 0.0363(12) Uani 1 d . . C6 C 0.3521(4) 0.7702(8) 0.2931(4) 0.036(2) Uani 1 d . . O6 O 0.4041(4) 0.7132(8) 0.2745(3) 0.069(2) Uani 1 d . . C7 C 0.0136(4) 0.7671(8) 0.3847(4) 0.030(2) Uani 1 d . . O7 O -0.0455(3) 0.7122(6) 0.3941(3) 0.0362(12) Uani 1 d . . C8 C 0.0459(4) 0.9541(8) 0.2744(4) 0.031(2) Uani 1 d . . O8 O 0.0078(3) 1.0003(6) 0.2153(3) 0.0400(13) Uani 1 d . . C9 C 0.1590(4) 0.5318(8) 0.4541(4) 0.033(2) Uani 1 d . . O9 O 0.1124(3) 0.4488(6) 0.4670(3) 0.0386(12) Uani 1 d . . C10 C 0.3139(4) 0.5306(8) 0.4062(4) 0.033(2) Uani 1 d . . O10 O 0.3585(4) 0.4543(7) 0.3905(4) 0.076(2) Uani 1 d . . C11 C 0.4502(4) 0.7733(9) 0.4793(4) 0.034(2) Uani 1 d . . O11 O 0.5071(3) 0.7081(6) 0.4722(3) 0.0465(14) Uani 1 d . . C12 C 0.4119(4) 0.9833(9) 0.5835(4) 0.036(2) Uani 1 d . . O12 O 0.4437(3) 1.0444(7) 0.6390(3) 0.059(2) Uani 1 d . . C13 C 0.1802(4) 1.2074(8) 0.3462(4) 0.031(2) Uani 1 d . . O13 O 0.1511(3) 1.2867(6) 0.2982(3) 0.0435(13) Uani 1 d . . C14 C 0.2743(4) 1.2124(8) 0.5117(4) 0.029(2) Uani 1 d . . O14 O 0.3007(3) 1.2947(7) 0.5578(3) 0.052(2) Uani 1 d . . C15 C 0.1199(4) 0.7604(8) 0.5736(4) 0.029(2) Uani 1 d . . O15 O 0.0755(3) 0.6898(6) 0.5972(3) 0.0358(12) Uani 1 d . . C16 C 0.2352(4) 0.9788(8) 0.6296(4) 0.033(2) Uani 1 d . . O16 O 0.2578(3) 1.0499(6) 0.6844(3) 0.0476(15) Uani 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 0.0237(2) 0.0235(3) 0.0219(2) -0.0007(2) 0.0073(2) 0.0024(2) Rh2 0.0216(2) 0.0199(3) 0.0218(2) 0.0007(2) 0.0046(2) 0.0006(2) Rh3 0.0257(2) 0.0207(3) 0.0223(2) -0.0006(2) 0.0061(2) 0.0037(2) Rh4 0.0220(2) 0.0294(3) 0.0247(3) -0.0032(2) 0.0032(2) 0.0012(2) Rh5 0.0251(2) 0.0192(3) 0.0259(3) -0.0025(2) 0.0075(2) -0.0011(2) Rh6 0.0273(2) 0.0245(3) 0.0194(2) -0.0027(2) 0.0072(2) -0.0020(2) C1 0.031(3) 0.028(4) 0.023(3) 0.004(3) 0.008(3) 0.004(3) O1 0.041(3) 0.029(3) 0.021(2) 0.003(2) 0.008(2) -0.004(2) C2 0.024(3) 0.031(4) 0.039(4) -0.002(3) 0.011(3) -0.001(3) O2 0.022(2) 0.039(3) 0.043(3) 0.001(2) 0.007(2) -0.003(2) C3 0.031(3) 0.022(4) 0.025(3) -0.002(3) 0.012(3) 0.003(3) O3 0.037(3) 0.026(3) 0.046(3) -0.005(2) 0.021(2) -0.001(2) C4 0.025(3) 0.040(5) 0.027(4) -0.004(3) 0.007(3) -0.004(3) O4 0.033(2) 0.049(4) 0.029(2) 0.009(3) -0.001(2) -0.002(2) C5 0.029(3) 0.035(4) 0.031(4) -0.004(3) 0.012(3) 0.000(3) O5 0.044(3) 0.037(3) 0.031(3) 0.008(2) 0.013(2) 0.010(2) C6 0.049(4) 0.036(5) 0.030(4) -0.007(3) 0.023(3) 0.008(3) O6 0.088(5) 0.077(6) 0.050(4) 0.003(4) 0.032(3) 0.013(4) C7 0.038(4) 0.032(4) 0.019(3) 0.001(3) 0.007(3) -0.003(3) O7 0.034(2) 0.043(3) 0.034(3) -0.007(2) 0.013(2) -0.016(2) C8 0.024(3) 0.026(4) 0.041(4) 0.006(3) 0.004(3) 0.001(3) O8 0.038(3) 0.045(4) 0.036(3) 0.014(3) 0.007(2) 0.013(2) C9 0.042(4) 0.027(4) 0.028(4) -0.003(3) 0.004(3) 0.008(3) O9 0.038(3) 0.029(3) 0.048(3) 0.002(2) 0.011(2) 0.001(2) C10 0.038(4) 0.021(4) 0.035(4) 0.005(3) 0.000(3) 0.008(3) O10 0.082(5) 0.047(5) 0.088(5) -0.013(4) 0.001(4) 0.025(4) C11 0.029(4) 0.041(5) 0.031(4) -0.003(3) 0.007(3) 0.001(3) O11 0.034(3) 0.050(4) 0.055(3) -0.001(3) 0.010(2) 0.011(3) C12 0.026(3) 0.040(5) 0.038(4) -0.012(4) 0.002(3) 0.000(3) O12 0.039(3) 0.078(5) 0.059(4) -0.023(4) 0.011(3) -0.008(3) C13 0.037(4) 0.020(4) 0.037(4) -0.010(3) 0.011(3) 0.000(3) O13 0.055(3) 0.026(3) 0.049(3) 0.008(3) 0.013(3) 0.004(3) C14 0.035(4) 0.018(4) 0.038(4) -0.001(3) 0.018(3) -0.005(3) O14 0.056(3) 0.048(4) 0.056(4) -0.019(3) 0.024(3) -0.010(3) C15 0.031(3) 0.030(4) 0.022(3) -0.010(3) 0.003(3) 0.001(3) O15 0.036(3) 0.041(3) 0.031(3) 0.004(2) 0.010(2) -0.004(2) C16 0.036(4) 0.039(5) 0.031(4) -0.002(3) 0.019(3) -0.007(3) O16 0.065(4) 0.047(4) 0.032(3) -0.012(3) 0.016(3) -0.025(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 Rh1 C6 1.917(7) . ? Rh1 C5 1.918(7) . ? Rh1 C2 2.175(7) . ? Rh1 C1 2.193(7) . ? Rh1 Rh5 2.7324(8) . ? Rh1 Rh4 2.7406(11) . ? Rh1 Rh2 2.7509(8) . ? Rh1 Rh3 2.7585(8) . ? Rh2 C8 1.907(7) . ? Rh2 C7 1.913(7) . ? Rh2 C3 2.182(6) . ? Rh2 C1 2.208(7) . ? Rh2 Rh3 2.7402(9) . ? Rh2 Rh6 2.7604(11) . ? Rh2 Rh5 2.7640(9) . ? Rh3 C9 1.891(8) . ? Rh3 C10 1.951(7) . ? Rh3 C4 2.158(6) . ? Rh3 C1 2.195(6) . ? Rh3 Rh6 2.7371(8) . ? Rh3 Rh4 2.7514(9) . ? Rh4 C11 1.896(7) . ? Rh4 C12 1.924(7) . ? Rh4 C4 2.184(7) . ? Rh4 C2 2.188(7) . ? Rh4 Rh5 2.7458(9) . ? Rh4 Rh6 2.7488(9) . ? Rh5 C13 1.910(8) . ? Rh5 C14 1.926(7) . ? Rh5 C3 2.172(6) . ? Rh5 C2 2.189(6) . ? Rh5 Rh6 2.7650(8) . ? Rh6 C16 1.907(7) . ? Rh6 C15 1.921(7) . ? Rh6 C3 2.194(7) . ? Rh6 C4 2.201(7) . ? C1 O1 1.143(8) . ? C2 O2 1.159(8) . ? C3 O3 1.159(7) . ? C4 O4 1.151(8) . ? C5 O5 1.126(8) . ? C6 O6 1.110(8) . ? C7 O7 1.133(7) . ? C8 O8 1.124(7) . ? C9 O9 1.151(8) . ? C10 O10 1.103(8) . ? C11 O11 1.140(8) . ? C12 O12 1.115(8) . ? C13 O13 1.124(8) . ? C14 O14 1.114(8) . ? C15 O15 1.130(8) . ? C16 O16 1.135(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Rh1 C5 94.4(3) . . ? C6 Rh1 C2 97.0(3) . . ? C5 Rh1 C2 95.8(3) . . ? C6 Rh1 C1 96.6(3) . . ? C5 Rh1 C1 99.6(3) . . ? C2 Rh1 C1 158.6(2) . . ? C6 Rh1 Rh5 147.6(2) . . ? C5 Rh1 Rh5 96.1(2) . . ? C2 Rh1 Rh5 51.5(2) . . ? C1 Rh1 Rh5 111.7(2) . . ? C6 Rh1 Rh4 95.7(2) . . ? C5 Rh1 Rh4 146.5(2) . . ? C2 Rh1 Rh4 51.3(2) . . ? C1 Rh1 Rh4 110.8(2) . . ? Rh5 Rh1 Rh4 60.22(2) . . ? C6 Rh1 Rh2 147.3(2) . . ? C5 Rh1 Rh2 98.1(2) . . ? C2 Rh1 Rh2 111.5(2) . . ? C1 Rh1 Rh2 51.6(2) . . ? Rh5 Rh1 Rh2 60.54(2) . . ? Rh4 Rh1 Rh2 90.27(3) . . ? C6 Rh1 Rh3 96.0(2) . . ? C5 Rh1 Rh3 149.8(2) . . ? C2 Rh1 Rh3 110.9(2) . . ? C1 Rh1 Rh3 51.1(2) . . ? Rh5 Rh1 Rh3 90.12(3) . . ? Rh4 Rh1 Rh3 60.04(2) . . ? Rh2 Rh1 Rh3 59.65(2) . . ? C8 Rh2 C7 91.4(3) . . ? C8 Rh2 C3 101.0(3) . . ? C7 Rh2 C3 95.7(3) . . ? C8 Rh2 C1 94.7(3) . . ? C7 Rh2 C1 101.1(3) . . ? C3 Rh2 C1 156.6(2) . . ? C8 Rh2 Rh3 145.6(2) . . ? C7 Rh2 Rh3 99.1(2) . . ? C3 Rh2 Rh3 110.2(2) . . ? C1 Rh2 Rh3 51.3(2) . . ? C8 Rh2 Rh1 96.5(2) . . ? C7 Rh2 Rh1 151.5(2) . . ? C3 Rh2 Rh1 109.4(2) . . ? C1 Rh2 Rh1 51.1(2) . . ? Rh3 Rh2 Rh1 60.31(2) . . ? C8 Rh2 Rh6 151.6(2) . . ? C7 Rh2 Rh6 96.3(2) . . ? C3 Rh2 Rh6 51.1(2) . . ? C1 Rh2 Rh6 110.5(2) . . ? Rh3 Rh2 Rh6 59.68(3) . . ? Rh1 Rh2 Rh6 89.69(3) . . ? C8 Rh2 Rh5 99.6(2) . . ? C7 Rh2 Rh5 145.7(2) . . ? C3 Rh2 Rh5 50.4(2) . . ? C1 Rh2 Rh5 110.1(2) . . ? Rh3 Rh2 Rh5 89.85(3) . . ? Rh1 Rh2 Rh5 59.40(2) . . ? Rh6 Rh2 Rh5 60.07(2) . . ? C9 Rh3 C10 94.4(3) . . ? C9 Rh3 C4 98.0(3) . . ? C10 Rh3 C4 99.1(3) . . ? C9 Rh3 C1 97.8(3) . . ? C10 Rh3 C1 94.2(3) . . ? C4 Rh3 C1 158.4(3) . . ? C9 Rh3 Rh6 96.3(2) . . ? C10 Rh3 Rh6 150.2(2) . . ? C4 Rh3 Rh6 51.8(2) . . ? C1 Rh3 Rh6 111.7(2) . . ? C9 Rh3 Rh2 96.0(2) . . ? C10 Rh3 Rh2 145.4(2) . . ? C4 Rh3 Rh2 111.9(2) . . ? C1 Rh3 Rh2 51.7(2) . . ? Rh6 Rh3 Rh2 60.53(3) . . ? C9 Rh3 Rh4 148.2(2) . . ? C10 Rh3 Rh4 98.0(2) . . ? C4 Rh3 Rh4 51.1(2) . . ? C1 Rh3 Rh4 110.4(2) . . ? Rh6 Rh3 Rh4 60.11(2) . . ? Rh2 Rh3 Rh4 90.27(3) . . ? C9 Rh3 Rh1 147.8(2) . . ? C10 Rh3 Rh1 95.6(2) . . ? C4 Rh3 Rh1 110.4(2) . . ? C1 Rh3 Rh1 51.0(2) . . ? Rh6 Rh3 Rh1 90.01(3) . . ? Rh2 Rh3 Rh1 60.04(2) . . ? Rh4 Rh3 Rh1 59.66(3) . . ? C11 Rh4 C12 96.4(3) . . ? C11 Rh4 C4 95.8(3) . . ? C12 Rh4 C4 96.9(3) . . ? C11 Rh4 C2 98.3(3) . . ? C12 Rh4 C2 98.7(3) . . ? C4 Rh4 C2 157.6(2) . . ? C11 Rh4 Rh1 96.8(2) . . ? C12 Rh4 Rh1 148.3(3) . . ? C4 Rh4 Rh1 110.2(2) . . ? C2 Rh4 Rh1 50.9(2) . . ? C11 Rh4 Rh5 148.6(2) . . ? C12 Rh4 Rh5 95.8(2) . . ? C4 Rh4 Rh5 111.3(2) . . ? C2 Rh4 Rh5 51.2(2) . . ? Rh1 Rh4 Rh5 59.74(3) . . ? C11 Rh4 Rh6 146.6(2) . . ? C12 Rh4 Rh6 94.5(2) . . ? C4 Rh4 Rh6 51.5(2) . . ? C2 Rh4 Rh6 111.1(2) . . ? Rh1 Rh4 Rh6 90.14(3) . . ? Rh5 Rh4 Rh6 60.43(2) . . ? C11 Rh4 Rh3 95.8(2) . . ? C12 Rh4 Rh3 146.0(2) . . ? C4 Rh4 Rh3 50.3(2) . . ? C2 Rh4 Rh3 110.8(2) . . ? Rh1 Rh4 Rh3 60.30(3) . . ? Rh5 Rh4 Rh3 89.99(3) . . ? Rh6 Rh4 Rh3 59.69(2) . . ? C13 Rh5 C14 95.3(3) . . ? C13 Rh5 C3 95.6(3) . . ? C14 Rh5 C3 98.2(2) . . ? C13 Rh5 C2 99.6(3) . . ? C14 Rh5 C2 97.1(3) . . ? C3 Rh5 C2 157.2(3) . . ? C13 Rh5 Rh1 97.4(2) . . ? C14 Rh5 Rh1 147.3(2) . . ? C3 Rh5 Rh1 110.4(2) . . ? C2 Rh5 Rh1 51.0(2) . . ? C13 Rh5 Rh4 149.8(2) . . ? C14 Rh5 Rh4 95.7(2) . . ? C3 Rh5 Rh4 110.4(2) . . ? C2 Rh5 Rh4 51.1(2) . . ? Rh1 Rh5 Rh4 60.04(3) . . ? C13 Rh5 Rh2 95.4(2) . . ? C14 Rh5 Rh2 148.0(2) . . ? C3 Rh5 Rh2 50.8(2) . . ? C2 Rh5 Rh2 110.6(2) . . ? Rh1 Rh5 Rh2 60.06(2) . . ? Rh4 Rh5 Rh2 89.89(3) . . ? C13 Rh5 Rh6 146.0(2) . . ? C14 Rh5 Rh6 96.1(2) . . ? C3 Rh5 Rh6 51.1(2) . . ? C2 Rh5 Rh6 110.5(2) . . ? Rh1 Rh5 Rh6 89.97(3) . . ? Rh4 Rh5 Rh6 59.84(2) . . ? Rh2 Rh5 Rh6 59.90(3) . . ? C16 Rh6 C15 93.7(3) . . ? C16 Rh6 C3 96.6(3) . . ? C15 Rh6 C3 99.9(3) . . ? C16 Rh6 C4 99.8(3) . . ? C15 Rh6 C4 96.5(3) . . ? C3 Rh6 C4 155.9(2) . . ? C16 Rh6 Rh3 149.4(2) . . ? C15 Rh6 Rh3 96.2(2) . . ? C3 Rh6 Rh3 110.0(2) . . ? C4 Rh6 Rh3 50.4(2) . . ? C16 Rh6 Rh4 97.3(2) . . ? C15 Rh6 Rh4 146.9(2) . . ? C3 Rh6 Rh4 109.6(2) . . ? C4 Rh6 Rh4 50.9(2) . . ? Rh3 Rh6 Rh4 60.20(2) . . ? C16 Rh6 Rh2 146.7(2) . . ? C15 Rh6 Rh2 97.7(2) . . ? C3 Rh6 Rh2 50.7(2) . . ? C4 Rh6 Rh2 109.7(2) . . ? Rh3 Rh6 Rh2 59.79(2) . . ? Rh4 Rh6 Rh2 89.90(3) . . ? C16 Rh6 Rh5 96.0(2) . . ? C15 Rh6 Rh5 149.6(2) . . ? C3 Rh6 Rh5 50.3(2) . . ? C4 Rh6 Rh5 110.1(2) . . ? Rh3 Rh6 Rh5 89.89(3) . . ? Rh4 Rh6 Rh5 59.73(2) . . ? Rh2 Rh6 Rh5 60.03(2) . . ? O1 C1 Rh1 134.2(5) . . ? O1 C1 Rh3 133.5(6) . . ? Rh1 C1 Rh3 77.9(2) . . ? O1 C1 Rh2 133.6(5) . . ? Rh1 C1 Rh2 77.4(2) . . ? Rh3 C1 Rh2 77.0(2) . . ? O2 C2 Rh1 133.7(5) . . ? O2 C2 Rh4 134.8(5) . . ? Rh1 C2 Rh4 77.8(2) . . ? O2 C2 Rh5 132.3(6) . . ? Rh1 C2 Rh5 77.5(2) . . ? Rh4 C2 Rh5 77.7(2) . . ? O3 C3 Rh5 131.6(5) . . ? O3 C3 Rh2 133.2(5) . . ? Rh5 C3 Rh2 78.8(2) . . ? O3 C3 Rh6 134.3(5) . . ? Rh5 C3 Rh6 78.6(2) . . ? Rh2 C3 Rh6 78.2(2) . . ? O4 C4 Rh3 133.6(6) . . ? O4 C4 Rh4 132.9(5) . . ? Rh3 C4 Rh4 78.6(2) . . ? O4 C4 Rh6 133.7(5) . . ? Rh3 C4 Rh6 77.8(2) . . ? Rh4 C4 Rh6 77.6(3) . . ? O5 C5 Rh1 177.5(7) . . ? O6 C6 Rh1 177.5(7) . . ? O7 C7 Rh2 178.1(6) . . ? O8 C8 Rh2 176.0(7) . . ? O9 C9 Rh3 179.5(6) . . ? O10 C10 Rh3 178.8(7) . . ? O11 C11 Rh4 178.0(7) . . ? O12 C12 Rh4 177.5(6) . . ? O13 C13 Rh5 179.2(6) . . ? O14 C14 Rh5 177.7(6) . . ? O15 C15 Rh6 176.3(6) . . ? O16 C16 Rh6 175.8(6) . . ? _refine_diff_density_max 1.720 _refine_diff_density_min -1.598 _refine_diff_density_rms 0.214 #======END