Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Grachova, Elena V.' ; Department of Chemistry St. Petersburg State University Universitetskii pr. 2 St. Petersburg 198504 Russia ; 'Jutzi, Peter' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; 'Neumann, Beate' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; 'Schebaum, Lars O.' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; 'Stammler, Hans-Georg' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; 'Tunik, Sergey P.' ; Department of Chemistry St. Petersburg State University Universitetskii pr. 2 St. Petersburg 198504 Russia ; _publ_contact_author_name 'Prof Sergey Tunik' _publ_contact_author_address ; Chemical St.Petersburg State University Universitetskii pr., 2 St.Petersburg 198504 RUSSIAN FEDERATION ; _publ_requested_journal 'Dalton Transactions' # 1. SUBMISSION DETAILS _publ_contact_author_phone '49 521 1066165' _publ_contact_author_fax '49 521 1066146' _publ_contact_author_email georg.stammler@uni-bielefeld.de _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for deposition To: DALTON@RSC.ORG Subject: Depositing Crystal Structure Data Dear Madam or Sir, please find enclosed the crystallographic data of compound1 'C25 H15 Ga O15 Rh6' compound2 'C34 H30 Ga2 O14 Rh6' compound3 'C45 H49 Cl4 Ga3 O13 Rh6' for deposition in your data file. With kind regards Beate Neumann ; # 3. TITLE AND AUTHOR LIST _publ_section_title ; Unusual Selective Substitution of Triply Bridging Carbonyl Ligands for GaCp* in Rh~6~(CO)~16~. Synthesis and Structural Characterization of the Rh~6~(\m^3^- CO)~4-x~(\m^3^-GaCp*)~x~(CO)~12~ clusters, x=1-4. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. #========================================================================= data_compound1 _database_code_CSD 172643 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H15 Ga O15 Rh6' _chemical_formula_sum 'C25 H15 Ga O15 Rh6' _chemical_formula_weight 1242.55 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' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5540(3) _cell_length_b 15.5970(4) _cell_length_c 17.1100(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.2290(11) _cell_angle_gamma 90.00 _cell_volume 3315.72(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9576 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 30.034 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 3.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4641 _exptl_absorpt_correction_T_max 0.9283 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'CCD; rotation images; thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68198 _diffrn_reflns_av_R_equivalents 0.090 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 29.99 _reflns_number_total 9563 _reflns_number_gt 6281 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0398P)^2^+9.0941P] 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 9563 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.0986 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.79318(3) 0.17132(2) 0.18707(2) 0.01731(10) Uani 1 1 d . . . Rh2 Rh 0.77636(3) 0.34976(2) 0.14949(2) 0.01664(10) Uani 1 1 d . . . Rh3 Rh 0.74073(3) 0.22588(2) 0.02859(2) 0.01685(10) Uani 1 1 d . . . Rh4 Rh 0.58881(3) 0.14882(3) 0.10896(2) 0.01838(10) Uani 1 1 d . . . Rh5 Rh 0.62680(3) 0.27072(3) 0.22652(2) 0.01781(10) Uani 1 1 d . . . Rh6 Rh 0.57213(3) 0.32051(3) 0.07065(2) 0.01785(10) Uani 1 1 d . . . Ga1 Ga 0.92844(5) 0.25247(4) 0.11521(3) 0.02020(13) Uani 1 1 d . . . O1 O 0.8764(3) 0.0025(2) 0.1328(2) 0.0310(10) Uani 1 1 d . . . O2 O 0.9227(4) 0.1612(3) 0.3511(2) 0.0357(10) Uani 1 1 d . . . O3 O 0.9163(3) 0.4155(2) 0.2965(2) 0.0294(9) Uani 1 1 d . . . O4 O 0.8242(4) 0.4976(3) 0.0450(2) 0.0389(11) Uani 1 1 d . . . O5 O 0.7864(3) 0.3498(3) -0.0989(2) 0.0324(10) Uani 1 1 d . . . O6 O 0.8022(4) 0.0705(3) -0.0629(2) 0.0373(11) Uani 1 1 d . . . O7 O 0.6340(3) 0.0819(2) 0.2824(2) 0.0252(9) Uani 1 1 d . . . O8 O 0.5965(3) 0.4666(2) 0.1939(2) 0.0249(9) Uani 1 1 d . . . O9 O 0.5156(3) 0.1901(2) -0.0667(2) 0.0240(8) Uani 1 1 d . . . O10 O 0.6265(3) -0.0265(2) 0.0408(2) 0.0311(10) Uani 1 1 d . . . O11 O 0.3530(4) 0.1173(3) 0.1230(3) 0.0501(13) Uani 1 1 d . . . O12 O 0.7429(3) 0.3108(3) 0.3915(2) 0.0321(10) Uani 1 1 d . . . O13 O 0.4033(4) 0.2780(4) 0.2743(3) 0.0605(15) Uani 1 1 d . . . O14 O 0.5840(3) 0.4597(2) -0.0525(2) 0.0302(9) Uani 1 1 d . . . O15 O 0.3297(4) 0.3370(3) 0.0665(3) 0.0472(12) Uani 1 1 d . . . C1 C 0.8470(5) 0.0654(3) 0.1551(3) 0.0231(12) Uani 1 1 d . . . C2 C 0.8777(5) 0.1685(3) 0.2889(3) 0.0246(12) Uani 1 1 d . . . C3 C 0.8639(4) 0.3908(3) 0.2412(3) 0.0196(11) Uani 1 1 d . . . C4 C 0.8096(4) 0.4417(4) 0.0856(3) 0.0233(12) Uani 1 1 d . . . C5 C 0.7707(5) 0.3024(3) -0.0509(3) 0.0238(12) Uani 1 1 d . . . C6 C 0.7812(5) 0.1277(4) -0.0269(3) 0.0231(12) Uani 1 1 d . . . C7 C 0.6494(5) 0.1324(3) 0.2343(3) 0.0247(12) Uani 1 1 d . . . C8 C 0.6241(5) 0.3997(4) 0.1732(3) 0.0237(12) Uani 1 1 d . . . C9 C 0.5666(4) 0.2087(3) -0.0069(3) 0.0201(11) Uani 1 1 d . . . C10 C 0.6110(5) 0.0374(3) 0.0686(3) 0.0227(12) Uani 1 1 d . . . C11 C 0.4410(5) 0.1292(4) 0.1176(3) 0.0301(14) Uani 1 1 d . . . C12 C 0.6992(4) 0.2969(3) 0.3296(3) 0.0219(11) Uani 1 1 d . . . C13 C 0.4857(5) 0.2754(4) 0.2554(4) 0.0326(14) Uani 1 1 d . . . C14 C 0.5780(4) 0.4073(3) -0.0074(3) 0.0232(12) Uani 1 1 d . . . C15 C 0.4201(5) 0.3307(4) 0.0678(3) 0.0264(13) Uani 1 1 d . . . C16 C 1.0661(4) 0.2844(3) 0.0501(3) 0.0216(11) Uani 1 1 d . . . C17 C 1.0761(4) 0.1953(4) 0.0720(3) 0.0252(12) Uani 1 1 d . . . C18 C 1.0994(5) 0.1920(4) 0.1556(3) 0.0261(12) Uani 1 1 d . . . C19 C 1.1044(4) 0.2770(4) 0.1854(3) 0.0256(12) Uani 1 1 d . . . C20 C 1.0843(4) 0.3345(4) 0.1201(3) 0.0258(13) Uani 1 1 d . . . C21 C 1.0516(5) 0.3188(4) -0.0330(3) 0.0291(13) Uani 1 1 d . . . H21A H 1.0105 0.3724 -0.0353 0.044 Uiso 1 1 calc R . . H21B H 1.0127 0.2767 -0.0688 0.044 Uiso 1 1 calc R . . H21C H 1.1223 0.3298 -0.0489 0.044 Uiso 1 1 calc R . . C22 C 1.0713(5) 0.1213(4) 0.0157(3) 0.0260(12) Uani 1 1 d . . . H22A H 1.1444 0.1053 0.0078 0.039 Uiso 1 1 calc R . . H22B H 1.0299 0.1379 -0.0350 0.039 Uiso 1 1 calc R . . H22C H 1.0363 0.0724 0.0375 0.039 Uiso 1 1 calc R . . C23 C 1.1217(5) 0.1124(4) 0.2049(4) 0.0344(15) Uani 1 1 d . . . H23A H 1.1950 0.1149 0.2336 0.052 Uiso 1 1 calc R . . H23B H 1.1145 0.0619 0.1704 0.052 Uiso 1 1 calc R . . H23C H 1.0702 0.1084 0.2426 0.052 Uiso 1 1 calc R . . C24 C 1.1320(5) 0.3022(4) 0.2708(3) 0.0351(15) Uani 1 1 d . . . H24A H 1.0909 0.2667 0.3031 0.053 Uiso 1 1 calc R . . H24B H 1.1138 0.3627 0.2771 0.053 Uiso 1 1 calc R . . H24C H 1.2091 0.2937 0.2878 0.053 Uiso 1 1 calc R . . C25 C 1.0892(5) 0.4310(4) 0.1251(4) 0.0327(14) Uani 1 1 d . . . H25A H 1.1645 0.4494 0.1359 0.049 Uiso 1 1 calc R . . H25B H 1.0507 0.4505 0.1677 0.049 Uiso 1 1 calc R . . H25C H 1.0556 0.4556 0.0749 0.049 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 Rh1 0.0229(2) 0.0157(2) 0.01240(19) -0.00005(15) -0.00092(16) 0.00088(16) Rh2 0.0215(2) 0.0149(2) 0.01295(19) -0.00015(14) 0.00047(16) -0.00086(16) Rh3 0.0216(2) 0.0159(2) 0.01242(19) -0.00035(14) 0.00033(16) 0.00025(16) Rh4 0.0227(2) 0.0173(2) 0.0141(2) -0.00004(15) -0.00082(16) -0.00322(16) Rh5 0.0216(2) 0.0184(2) 0.01316(19) -0.00051(15) 0.00174(16) -0.00084(16) Rh6 0.0205(2) 0.0177(2) 0.01437(19) 0.00023(15) -0.00076(16) 0.00182(16) Ga1 0.0215(3) 0.0216(3) 0.0172(3) -0.0009(2) 0.0016(2) 0.0005(2) O1 0.043(3) 0.027(2) 0.022(2) -0.0002(17) 0.0010(18) 0.0077(19) O2 0.047(3) 0.031(2) 0.024(2) -0.0032(18) -0.014(2) 0.005(2) O3 0.039(3) 0.027(2) 0.020(2) -0.0003(16) -0.0039(18) -0.0030(18) O4 0.059(3) 0.031(2) 0.024(2) 0.0038(18) -0.002(2) -0.014(2) O5 0.043(3) 0.030(2) 0.023(2) 0.0045(18) 0.0016(19) -0.0026(19) O6 0.054(3) 0.030(2) 0.028(2) -0.0073(18) 0.004(2) 0.010(2) O7 0.036(2) 0.021(2) 0.0183(19) 0.0021(15) 0.0025(17) -0.0017(17) O8 0.034(2) 0.022(2) 0.0175(19) -0.0014(15) 0.0009(17) 0.0031(17) O9 0.030(2) 0.027(2) 0.0143(18) -0.0001(15) 0.0009(16) -0.0042(17) O10 0.043(3) 0.022(2) 0.026(2) -0.0068(17) -0.0006(19) -0.0020(18) O11 0.037(3) 0.067(3) 0.048(3) -0.013(3) 0.014(2) -0.016(3) O12 0.038(3) 0.040(2) 0.019(2) -0.0050(18) 0.0030(18) -0.007(2) O13 0.033(3) 0.109(5) 0.042(3) 0.011(3) 0.014(2) 0.006(3) O14 0.041(3) 0.024(2) 0.024(2) 0.0064(17) 0.0018(19) 0.0028(18) O15 0.028(3) 0.054(3) 0.061(3) 0.005(2) 0.011(2) 0.008(2) C1 0.034(3) 0.018(3) 0.017(3) 0.001(2) 0.000(2) 0.003(2) C2 0.023(3) 0.023(3) 0.026(3) 0.001(2) 0.000(2) -0.002(2) C3 0.026(3) 0.014(3) 0.019(3) 0.003(2) 0.001(2) 0.002(2) C4 0.027(3) 0.028(3) 0.014(3) -0.003(2) -0.002(2) -0.008(2) C5 0.030(3) 0.022(3) 0.018(3) -0.007(2) 0.001(2) 0.000(2) C6 0.025(3) 0.024(3) 0.019(3) 0.003(2) 0.000(2) 0.000(2) C7 0.034(3) 0.020(3) 0.019(3) -0.003(2) -0.001(2) 0.002(2) C8 0.032(3) 0.024(3) 0.013(2) -0.003(2) -0.003(2) -0.004(2) C9 0.024(3) 0.018(3) 0.018(3) 0.003(2) 0.001(2) 0.006(2) C10 0.028(3) 0.022(3) 0.016(3) 0.003(2) -0.005(2) -0.005(2) C11 0.035(4) 0.030(3) 0.026(3) -0.007(2) 0.008(3) -0.006(3) C12 0.023(3) 0.022(3) 0.021(3) -0.002(2) 0.004(2) -0.002(2) C13 0.029(4) 0.046(4) 0.025(3) 0.006(3) 0.009(3) 0.002(3) C14 0.025(3) 0.022(3) 0.021(3) -0.004(2) -0.005(2) 0.000(2) C15 0.023(3) 0.030(3) 0.024(3) -0.002(2) -0.001(2) 0.002(2) C16 0.023(3) 0.022(3) 0.020(3) -0.001(2) 0.005(2) 0.001(2) C17 0.022(3) 0.030(3) 0.025(3) 0.002(2) 0.007(2) 0.000(2) C18 0.022(3) 0.036(3) 0.020(3) 0.002(2) 0.004(2) 0.005(3) C19 0.019(3) 0.035(3) 0.021(3) -0.002(2) 0.000(2) -0.002(2) C20 0.024(3) 0.030(3) 0.024(3) -0.009(2) 0.008(2) -0.004(2) C21 0.040(4) 0.025(3) 0.023(3) -0.003(2) 0.009(3) -0.001(3) C22 0.026(3) 0.025(3) 0.028(3) 0.000(2) 0.009(2) 0.004(2) C23 0.031(4) 0.041(4) 0.032(3) 0.011(3) 0.007(3) 0.012(3) C24 0.030(4) 0.051(4) 0.023(3) -0.004(3) 0.000(3) 0.004(3) C25 0.038(4) 0.029(3) 0.032(3) -0.005(3) 0.006(3) -0.008(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 C1 1.895(5) . ? Rh1 C2 1.906(6) . ? Rh1 C7 2.168(6) . ? Rh1 Ga1 2.5680(7) . ? Rh1 Rh4 2.7404(6) . ? Rh1 Rh5 2.7614(6) . ? Rh1 Rh3 2.8282(5) . ? Rh1 Rh2 2.8574(5) . ? Rh2 C4 1.886(6) . ? Rh2 C3 1.894(5) . ? Rh2 C8 2.155(6) . ? Rh2 Ga1 2.5714(7) . ? Rh2 Rh5 2.7370(6) . ? Rh2 Rh6 2.7588(6) . ? Rh2 Rh3 2.8190(5) . ? Rh3 C5 1.887(6) . ? Rh3 C6 1.909(6) . ? Rh3 C9 2.200(5) . ? Rh3 Ga1 2.6309(7) . ? Rh3 Rh6 2.7589(6) . ? Rh3 Rh4 2.7791(6) . ? Rh4 C10 1.905(6) . ? Rh4 C11 1.907(7) . ? Rh4 C9 2.172(5) . ? Rh4 C7 2.185(5) . ? Rh4 Rh6 2.7577(6) . ? Rh4 Rh5 2.7593(6) . ? Rh5 C13 1.908(6) . ? Rh5 C12 1.909(5) . ? Rh5 C7 2.178(5) . ? Rh5 C8 2.207(5) . ? Rh5 Rh6 2.7681(6) . ? Rh6 C15 1.909(6) . ? Rh6 C14 1.909(6) . ? Rh6 C8 2.168(5) . ? Rh6 C9 2.187(5) . ? Ga1 C16 2.242(5) . ? Ga1 C17 2.273(6) . ? Ga1 C20 2.329(6) . ? Ga1 C18 2.355(6) . ? Ga1 C19 2.390(5) . ? O1 C1 1.134(6) . ? O2 C2 1.137(7) . ? O3 C3 1.139(6) . ? O4 C4 1.146(6) . ? O5 C5 1.143(6) . ? O6 C6 1.136(6) . ? O7 C7 1.174(6) . ? O8 C8 1.170(6) . ? O9 C9 1.163(6) . ? O10 C10 1.134(6) . ? O11 C11 1.137(7) . ? O12 C12 1.142(6) . ? O13 C13 1.127(7) . ? O14 C14 1.135(6) . ? O15 C15 1.135(7) . ? C16 C20 1.419(7) . ? C16 C17 1.440(8) . ? C16 C21 1.507(7) . ? C17 C18 1.420(8) . ? C17 C22 1.499(8) . ? C18 C19 1.419(8) . ? C18 C23 1.504(8) . ? C19 C20 1.426(8) . ? C19 C24 1.504(8) . ? C20 C25 1.508(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 C1 Rh1 C2 93.9(2) . . ? C1 Rh1 C7 102.3(2) . . ? C2 Rh1 C7 92.1(2) . . ? C1 Rh1 Ga1 90.25(17) . . ? C2 Rh1 Ga1 97.43(17) . . ? C7 Rh1 Ga1 163.67(15) . . ? C1 Rh1 Rh4 95.46(17) . . ? C2 Rh1 Rh4 143.37(17) . . ? C7 Rh1 Rh4 51.27(14) . . ? Ga1 Rh1 Rh4 117.82(2) . . ? C1 Rh1 Rh5 150.85(18) . . ? C2 Rh1 Rh5 97.53(17) . . ? C7 Rh1 Rh5 50.70(14) . . ? Ga1 Rh1 Rh5 114.55(2) . . ? Rh4 Rh1 Rh5 60.200(15) . . ? C1 Rh1 Rh3 91.70(16) . . ? C2 Rh1 Rh3 154.95(17) . . ? C7 Rh1 Rh3 110.47(14) . . ? Ga1 Rh1 Rh3 58.119(17) . . ? Rh4 Rh1 Rh3 59.851(14) . . ? Rh5 Rh1 Rh3 89.140(16) . . ? C1 Rh1 Rh2 143.36(16) . . ? C2 Rh1 Rh2 103.99(16) . . ? C7 Rh1 Rh2 108.55(14) . . ? Ga1 Rh1 Rh2 56.278(17) . . ? Rh4 Rh1 Rh2 88.921(16) . . ? Rh5 Rh1 Rh2 58.272(14) . . ? Rh3 Rh1 Rh2 59.444(13) . . ? C4 Rh2 C3 94.2(2) . . ? C4 Rh2 C8 96.3(2) . . ? C3 Rh2 C8 98.4(2) . . ? C4 Rh2 Ga1 94.77(18) . . ? C3 Rh2 Ga1 91.54(16) . . ? C8 Rh2 Ga1 164.46(15) . . ? C4 Rh2 Rh5 147.76(18) . . ? C3 Rh2 Rh5 96.32(16) . . ? C8 Rh2 Rh5 52.00(15) . . ? Ga1 Rh2 Rh5 115.27(2) . . ? C4 Rh2 Rh6 96.30(16) . . ? C3 Rh2 Rh6 148.15(16) . . ? C8 Rh2 Rh6 50.56(14) . . ? Ga1 Rh2 Rh6 117.34(2) . . ? Rh5 Rh2 Rh6 60.485(15) . . ? C4 Rh2 Rh3 96.94(16) . . ? C3 Rh2 Rh3 148.44(15) . . ? C8 Rh2 Rh3 109.50(14) . . ? Ga1 Rh2 Rh3 58.210(17) . . ? Rh5 Rh2 Rh3 89.820(16) . . ? Rh6 Rh2 Rh3 59.279(14) . . ? C4 Rh2 Rh1 148.83(17) . . ? C3 Rh2 Rh1 97.33(15) . . ? C8 Rh2 Rh1 110.40(15) . . ? Ga1 Rh2 Rh1 56.164(18) . . ? Rh5 Rh2 Rh1 59.108(14) . . ? Rh6 Rh2 Rh1 88.997(16) . . ? Rh3 Rh2 Rh1 59.762(14) . . ? C5 Rh3 C6 93.1(2) . . ? C5 Rh3 C9 99.8(2) . . ? C6 Rh3 C9 95.2(2) . . ? C5 Rh3 Ga1 92.97(17) . . ? C6 Rh3 Ga1 97.22(17) . . ? C9 Rh3 Ga1 161.67(14) . . ? C5 Rh3 Rh6 95.12(17) . . ? C6 Rh3 Rh6 145.88(17) . . ? C9 Rh3 Rh6 50.81(13) . . ? Ga1 Rh3 Rh6 115.31(2) . . ? C5 Rh3 Rh4 148.39(18) . . ? C6 Rh3 Rh4 98.61(17) . . ? C9 Rh3 Rh4 50.10(13) . . ? Ga1 Rh3 Rh4 114.35(2) . . ? Rh6 Rh3 Rh4 59.729(15) . . ? C5 Rh3 Rh2 93.94(16) . . ? C6 Rh3 Rh2 152.78(16) . . ? C9 Rh3 Rh2 109.46(14) . . ? Ga1 Rh3 Rh2 56.178(17) . . ? Rh6 Rh3 Rh2 59.274(14) . . ? Rh4 Rh3 Rh2 88.939(16) . . ? C5 Rh3 Rh1 146.96(16) . . ? C6 Rh3 Rh1 101.15(16) . . ? C9 Rh3 Rh1 108.28(14) . . ? Ga1 Rh3 Rh1 55.981(17) . . ? Rh6 Rh3 Rh1 89.594(16) . . ? Rh4 Rh3 Rh1 58.507(14) . . ? Rh2 Rh3 Rh1 60.794(14) . . ? C10 Rh4 C11 94.4(2) . . ? C10 Rh4 C9 93.8(2) . . ? C11 Rh4 C9 98.1(2) . . ? C10 Rh4 C7 101.6(2) . . ? C11 Rh4 C7 96.3(2) . . ? C9 Rh4 C7 158.0(2) . . ? C10 Rh4 Rh1 96.79(16) . . ? C11 Rh4 Rh1 146.71(18) . . ? C9 Rh4 Rh1 112.27(15) . . ? C7 Rh4 Rh1 50.70(16) . . ? C10 Rh4 Rh6 144.04(15) . . ? C11 Rh4 Rh6 97.61(18) . . ? C9 Rh4 Rh6 50.98(14) . . ? C7 Rh4 Rh6 110.55(14) . . ? Rh1 Rh4 Rh6 91.459(17) . . ? C10 Rh4 Rh5 150.92(15) . . ? C11 Rh4 Rh5 97.02(17) . . ? C9 Rh4 Rh5 110.81(14) . . ? C7 Rh4 Rh5 50.65(14) . . ? Rh1 Rh4 Rh5 60.276(15) . . ? Rh6 Rh4 Rh5 60.230(14) . . ? C10 Rh4 Rh3 93.92(17) . . ? C11 Rh4 Rh3 148.43(19) . . ? C9 Rh4 Rh3 50.98(15) . . ? C7 Rh4 Rh3 111.67(16) . . ? Rh1 Rh4 Rh3 61.642(15) . . ? Rh6 Rh4 Rh3 59.773(14) . . ? Rh5 Rh4 Rh3 90.196(17) . . ? C13 Rh5 C12 95.1(2) . . ? C13 Rh5 C7 98.0(2) . . ? C12 Rh5 C7 96.6(2) . . ? C13 Rh5 C8 96.5(2) . . ? C12 Rh5 C8 99.4(2) . . ? C7 Rh5 C8 157.3(2) . . ? C13 Rh5 Rh2 146.54(19) . . ? C12 Rh5 Rh2 94.59(16) . . ? C7 Rh5 Rh2 112.55(16) . . ? C8 Rh5 Rh2 50.30(15) . . ? C13 Rh5 Rh4 98.35(19) . . ? C12 Rh5 Rh4 146.19(16) . . ? C7 Rh5 Rh4 50.90(14) . . ? C8 Rh5 Rh4 109.62(13) . . ? Rh2 Rh5 Rh4 91.044(17) . . ? C13 Rh5 Rh1 148.0(2) . . ? C12 Rh5 Rh1 93.99(16) . . ? C7 Rh5 Rh1 50.39(16) . . ? C8 Rh5 Rh1 112.20(15) . . ? Rh2 Rh5 Rh1 62.621(15) . . ? Rh4 Rh5 Rh1 59.524(15) . . ? C13 Rh5 Rh6 97.34(18) . . ? C12 Rh5 Rh6 148.16(16) . . ? C7 Rh5 Rh6 110.43(14) . . ? C8 Rh5 Rh6 50.13(13) . . ? Rh2 Rh5 Rh6 60.148(15) . . ? Rh4 Rh5 Rh6 59.857(14) . . ? Rh1 Rh5 Rh6 90.796(17) . . ? C15 Rh6 C14 93.5(2) . . ? C15 Rh6 C8 99.1(2) . . ? C14 Rh6 C8 97.2(2) . . ? C15 Rh6 C9 96.1(2) . . ? C14 Rh6 C9 98.2(2) . . ? C8 Rh6 C9 157.7(2) . . ? C15 Rh6 Rh4 97.40(17) . . ? C14 Rh6 Rh4 147.67(16) . . ? C8 Rh6 Rh4 110.92(14) . . ? C9 Rh6 Rh4 50.53(13) . . ? C15 Rh6 Rh2 148.73(17) . . ? C14 Rh6 Rh2 95.64(16) . . ? C8 Rh6 Rh2 50.14(16) . . ? C9 Rh6 Rh2 112.04(14) . . ? Rh4 Rh6 Rh2 90.617(17) . . ? C15 Rh6 Rh3 147.08(17) . . ? C14 Rh6 Rh3 95.09(17) . . ? C8 Rh6 Rh3 111.25(16) . . ? C9 Rh6 Rh3 51.25(14) . . ? Rh4 Rh6 Rh3 60.499(15) . . ? Rh2 Rh6 Rh3 61.447(15) . . ? C15 Rh6 Rh5 99.06(17) . . ? C14 Rh6 Rh5 147.48(16) . . ? C8 Rh6 Rh5 51.39(14) . . ? C9 Rh6 Rh5 110.04(13) . . ? Rh4 Rh6 Rh5 59.913(14) . . ? Rh2 Rh6 Rh5 59.368(14) . . ? Rh3 Rh6 Rh5 90.433(17) . . ? C16 Ga1 C17 37.19(19) . . ? C16 Ga1 C20 36.11(18) . . ? C17 Ga1 C20 60.5(2) . . ? C16 Ga1 C18 60.02(19) . . ? C17 Ga1 C18 35.69(19) . . ? C20 Ga1 C18 58.9(2) . . ? C16 Ga1 C19 59.40(19) . . ? C17 Ga1 C19 59.2(2) . . ? C20 Ga1 C19 35.16(19) . . ? C18 Ga1 C19 34.8(2) . . ? C16 Ga1 Rh1 163.14(14) . . ? C17 Ga1 Rh1 126.03(14) . . ? C20 Ga1 Rh1 149.68(14) . . ? C18 Ga1 Rh1 107.41(14) . . ? C19 Ga1 Rh1 117.74(14) . . ? C16 Ga1 Rh2 129.22(14) . . ? C17 Ga1 Rh2 166.41(14) . . ? C20 Ga1 Rh2 108.38(14) . . ? C18 Ga1 Rh2 147.58(14) . . ? C19 Ga1 Rh2 116.99(14) . . ? Rh1 Ga1 Rh2 67.557(19) . . ? C16 Ga1 Rh3 116.57(14) . . ? C17 Ga1 Rh3 117.46(14) . . ? C20 Ga1 Rh3 141.89(15) . . ? C18 Ga1 Rh3 143.84(15) . . ? C19 Ga1 Rh3 175.94(14) . . ? Rh1 Ga1 Rh3 65.900(19) . . ? Rh2 Ga1 Rh3 65.612(19) . . ? O1 C1 Rh1 176.9(5) . . ? O2 C2 Rh1 174.1(5) . . ? O3 C3 Rh2 179.8(6) . . ? O4 C4 Rh2 176.3(5) . . ? O5 C5 Rh3 178.2(5) . . ? O6 C6 Rh3 176.8(5) . . ? O7 C7 Rh1 132.7(5) . . ? O7 C7 Rh5 132.4(4) . . ? Rh1 C7 Rh5 78.91(19) . . ? O7 C7 Rh4 134.2(4) . . ? Rh1 C7 Rh4 78.03(19) . . ? Rh5 C7 Rh4 78.46(18) . . ? O8 C8 Rh2 133.5(4) . . ? O8 C8 Rh6 133.2(4) . . ? Rh2 C8 Rh6 79.30(19) . . ? O8 C8 Rh5 132.5(4) . . ? Rh2 C8 Rh5 77.70(19) . . ? Rh6 C8 Rh5 78.48(18) . . ? O9 C9 Rh4 132.7(4) . . ? O9 C9 Rh6 134.3(4) . . ? Rh4 C9 Rh6 78.49(17) . . ? O9 C9 Rh3 132.3(4) . . ? Rh4 C9 Rh3 78.92(17) . . ? Rh6 C9 Rh3 77.94(18) . . ? O10 C10 Rh4 175.9(5) . . ? O11 C11 Rh4 179.7(7) . . ? O12 C12 Rh5 178.5(5) . . ? O13 C13 Rh5 178.4(6) . . ? O14 C14 Rh6 178.1(5) . . ? O15 C15 Rh6 179.6(6) . . ? C20 C16 C17 108.3(5) . . ? C20 C16 C21 125.7(5) . . ? C17 C16 C21 125.7(5) . . ? C20 C16 Ga1 75.3(3) . . ? C17 C16 Ga1 72.6(3) . . ? C21 C16 Ga1 123.4(4) . . ? C18 C17 C16 107.1(5) . . ? C18 C17 C22 127.1(5) . . ? C16 C17 C22 125.6(5) . . ? C18 C17 Ga1 75.3(3) . . ? C16 C17 Ga1 70.2(3) . . ? C22 C17 Ga1 123.5(4) . . ? C19 C18 C17 108.7(5) . . ? C19 C18 C23 125.2(5) . . ? C17 C18 C23 126.1(5) . . ? C19 C18 Ga1 73.9(3) . . ? C17 C18 Ga1 69.0(3) . . ? C23 C18 Ga1 125.7(4) . . ? C18 C19 C20 108.2(5) . . ? C18 C19 C24 125.8(5) . . ? C20 C19 C24 126.0(5) . . ? C18 C19 Ga1 71.3(3) . . ? C20 C19 Ga1 70.1(3) . . ? C24 C19 Ga1 126.7(4) . . ? C16 C20 C19 107.7(5) . . ? C16 C20 C25 126.7(5) . . ? C19 C20 C25 125.5(5) . . ? C16 C20 Ga1 68.6(3) . . ? C19 C20 Ga1 74.7(3) . . ? C25 C20 Ga1 125.2(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.548 _refine_diff_density_min -1.472 _refine_diff_density_rms 0.219 #===END data_compound2 _database_code_CSD 172644 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H30 Ga2 O14 Rh6' _chemical_formula_sum 'C34 H30 Ga2 O14 Rh6' _chemical_formula_weight 1419.48 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' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 11.3400(3) _cell_length_b 15.2260(5) _cell_length_c 12.6640(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.1911(13) _cell_angle_gamma 90.00 _cell_volume 1994.58(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6032 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 30.034 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 3.811 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4492 _exptl_absorpt_correction_T_max 0.9277 _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'CCD; rotation images; thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36192 _diffrn_reflns_av_R_equivalents 0.080 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3646 _reflns_number_gt 2627 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0318P)^2^+1.7970P] 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 3646 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0653 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh -0.13434(6) 0.2500 -0.89072(5) 0.01472(15) Uani 1 2 d S . . Rh2 Rh -0.37024(4) 0.34329(3) -0.96596(4) 0.01467(12) Uani 1 1 d . . . Rh3 Rh -0.20581(4) 0.34291(3) -0.73415(4) 0.01458(12) Uani 1 1 d . . . Rh4 Rh -0.43458(6) 0.2500 -0.81031(5) 0.01531(15) Uani 1 2 d S . . Ga1 Ga -0.30001(8) 0.2500 -1.10188(7) 0.0192(2) Uani 1 2 d S . . Ga2 Ga -0.00013(9) 0.2500 -0.67234(8) 0.0238(2) Uani 1 2 d S . . O1 O 0.0134(4) 0.4001(3) -0.9370(4) 0.0346(11) Uani 1 1 d . . . O2 O -0.2680(4) 0.5153(2) -1.0172(3) 0.0261(10) Uani 1 1 d . . . O3 O -0.6457(4) 0.3642(2) -1.1474(3) 0.0297(10) Uani 1 1 d . . . O4 O -0.0711(4) 0.5136(2) -0.7417(3) 0.0312(10) Uani 1 1 d . . . O5 O -0.1823(4) 0.3634(3) -0.4877(4) 0.0394(11) Uani 1 1 d . . . O6 O -0.7245(6) 0.2500 -0.9548(5) 0.0360(16) Uani 1 2 d S . . O7 O -0.4545(6) 0.2500 -0.5784(5) 0.0368(16) Uani 1 2 d S . . O8 O -0.4534(3) 0.4532(2) -0.8038(3) 0.0227(9) Uani 1 1 d . . . C1 C -0.0400(5) 0.3431(4) -0.9194(5) 0.0229(13) Uani 1 1 d . . . C2 C -0.3072(5) 0.4502(4) -1.0011(5) 0.0201(13) Uani 1 1 d . . . C3 C -0.5413(6) 0.3575(3) -1.0808(5) 0.0181(12) Uani 1 1 d . . . C4 C -0.1198(5) 0.4487(4) -0.7375(5) 0.0209(13) Uani 1 1 d . . . C5 C -0.1886(5) 0.3558(3) -0.5784(5) 0.0211(13) Uani 1 1 d . . . C6 C -0.6160(9) 0.2500 -0.9015(7) 0.026(2) Uani 1 2 d S . . C7 C -0.4483(8) 0.2500 -0.6638(8) 0.0232(19) Uani 1 2 d S . . C8 C -0.4019(5) 0.3902(4) -0.8195(5) 0.0212(13) Uani 1 1 d . . . C9 C -0.1731(8) 0.2500 -1.2121(7) 0.028(2) Uani 1 2 d S . . C10 C -0.2553(6) 0.3251(4) -1.2411(5) 0.0285(15) Uani 1 1 d . . . C11 C -0.3850(6) 0.2968(4) -1.2876(5) 0.0258(14) Uani 1 1 d . . . C12 C -0.0286(9) 0.2500 -1.1650(9) 0.053(3) Uani 1 2 d S . . H12A H -0.0015 0.2500 -1.2292 0.080 Uiso 1 2 calc SR . . H12B H 0.0051 0.1974 -1.1174 0.080 Uiso 0.50 1 calc PR . . H12C H 0.0051 0.3026 -1.1174 0.080 Uiso 0.50 1 calc PR . . C13 C -0.2127(7) 0.4194(4) -1.2345(6) 0.0445(19) Uani 1 1 d . . . H13A H -0.1319 0.4277 -1.1656 0.067 Uiso 1 1 calc R . . H13B H -0.2797 0.4578 -1.2297 0.067 Uiso 1 1 calc R . . H13C H -0.1988 0.4341 -1.3039 0.067 Uiso 1 1 calc R . . C14 C -0.5042(7) 0.3543(4) -1.3416(5) 0.0449(19) Uani 1 1 d . . . H14A H -0.5145 0.3726 -1.4190 0.067 Uiso 1 1 calc R . . H14B H -0.4945 0.4063 -1.2931 0.067 Uiso 1 1 calc R . . H14C H -0.5807 0.3210 -1.3474 0.067 Uiso 1 1 calc R . . C15 C 0.2095(5) 0.2972(3) -0.6108(5) 0.0238(14) Uani 1 1 d . . . C16 C 0.1676(5) 0.3261(3) -0.5249(5) 0.0263(14) Uani 1 1 d . . . C17 C 0.1439(7) 0.2500 -0.4707(7) 0.026(2) Uani 1 2 d S . . C18 C 0.2536(6) 0.3549(4) -0.6836(6) 0.0337(16) Uani 1 1 d . . . H18A H 0.3430 0.3734 -0.6383 0.051 Uiso 1 1 calc R . . H18B H 0.1977 0.4068 -0.7083 0.051 Uiso 1 1 calc R . . H18C H 0.2488 0.3223 -0.7520 0.051 Uiso 1 1 calc R . . C19 C 0.1613(6) 0.4190(4) -0.4895(5) 0.0355(16) Uani 1 1 d . . . H19A H 0.0835 0.4272 -0.4749 0.053 Uiso 1 1 calc R . . H19B H 0.1582 0.4587 -0.5515 0.053 Uiso 1 1 calc R . . H19C H 0.2381 0.4322 -0.4188 0.053 Uiso 1 1 calc R . . C20 C 0.1052(8) 0.2500 -0.3711(8) 0.035(2) Uani 1 2 d S . . H20A H 0.1829 0.2500 -0.2982 0.052 Uiso 1 2 calc SR . . H20B H 0.0538 0.1974 -0.3749 0.052 Uiso 0.50 1 calc PR . . H20C H 0.0538 0.3026 -0.3749 0.052 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0176(3) 0.0120(3) 0.0170(4) 0.000 0.0094(3) 0.000 Rh2 0.0178(2) 0.0116(2) 0.0147(3) 0.00137(17) 0.00671(19) 0.00148(18) Rh3 0.0185(2) 0.0111(2) 0.0143(2) -0.00127(17) 0.00689(19) -0.00086(18) Rh4 0.0161(3) 0.0154(3) 0.0161(4) 0.000 0.0083(3) 0.000 Ga1 0.0246(5) 0.0170(4) 0.0173(5) 0.000 0.0100(4) 0.000 Ga2 0.0248(5) 0.0209(5) 0.0261(6) 0.000 0.0109(5) 0.000 O1 0.035(3) 0.032(2) 0.042(3) 0.006(2) 0.020(2) -0.011(2) O2 0.028(2) 0.019(2) 0.032(3) 0.0058(18) 0.013(2) -0.0030(19) O3 0.027(2) 0.028(2) 0.025(3) 0.0048(19) 0.002(2) 0.002(2) O4 0.039(3) 0.021(2) 0.033(3) -0.0023(19) 0.014(2) -0.013(2) O5 0.060(3) 0.035(3) 0.026(3) -0.007(2) 0.020(2) -0.004(2) O6 0.023(4) 0.049(4) 0.035(4) 0.000 0.011(3) 0.000 O7 0.035(4) 0.051(4) 0.029(4) 0.000 0.018(3) 0.000 O8 0.026(2) 0.021(2) 0.024(2) 0.0023(18) 0.0124(19) 0.0082(18) C1 0.021(3) 0.028(3) 0.022(3) 0.000(3) 0.011(3) 0.001(3) C2 0.021(3) 0.026(3) 0.010(3) -0.004(2) 0.004(3) 0.007(3) C3 0.025(3) 0.014(3) 0.018(3) 0.003(2) 0.012(3) -0.001(3) C4 0.025(3) 0.023(3) 0.013(3) -0.002(2) 0.006(3) -0.001(3) C5 0.030(3) 0.014(3) 0.020(3) -0.008(3) 0.011(3) -0.002(3) C6 0.033(6) 0.027(5) 0.025(5) 0.000 0.019(5) 0.000 C7 0.024(5) 0.021(4) 0.030(6) 0.000 0.017(4) 0.000 C8 0.018(3) 0.024(3) 0.019(3) 0.000(3) 0.005(3) -0.002(3) C9 0.037(5) 0.035(5) 0.014(5) 0.000 0.014(4) 0.000 C10 0.048(4) 0.024(3) 0.018(3) -0.004(3) 0.017(3) -0.005(3) C11 0.034(4) 0.029(3) 0.014(3) 0.004(2) 0.010(3) 0.007(3) C12 0.045(7) 0.079(8) 0.041(7) 0.000 0.023(6) 0.000 C13 0.080(5) 0.027(4) 0.041(4) -0.001(3) 0.041(4) -0.017(4) C14 0.067(5) 0.050(4) 0.021(4) 0.007(3) 0.021(4) 0.026(4) C15 0.018(3) 0.023(3) 0.026(4) 0.001(3) 0.004(3) 0.005(3) C16 0.023(3) 0.019(3) 0.033(4) 0.000(3) 0.007(3) 0.002(3) C17 0.014(4) 0.034(5) 0.025(5) 0.000 0.005(4) 0.000 C18 0.034(4) 0.025(3) 0.047(4) 0.009(3) 0.021(3) 0.002(3) C19 0.040(4) 0.028(4) 0.036(4) -0.004(3) 0.013(3) 0.000(3) C20 0.024(5) 0.043(6) 0.033(6) 0.000 0.008(4) 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 Rh1 C1 1.898(6) . ? Rh1 C1 1.898(6) 4_565 ? Rh1 Ga2 2.5524(11) . ? Rh1 Ga1 2.5618(10) . ? Rh1 Rh3 2.8119(7) . ? Rh1 Rh3 2.8119(7) 4_565 ? Rh1 Rh2 2.8271(6) 4_565 ? Rh1 Rh2 2.8271(6) . ? Rh2 C3 1.901(6) . ? Rh2 C2 1.902(6) . ? Rh2 C8 2.150(6) . ? Rh2 Ga1 2.5958(8) . ? Rh2 Rh3 2.7584(6) . ? Rh2 Rh4 2.7592(7) . ? Rh2 Rh2 2.8407(8) 4_565 ? Rh3 C4 1.893(6) . ? Rh3 C5 1.910(6) . ? Rh3 C8 2.159(5) . ? Rh3 Ga2 2.5608(8) . ? Rh3 Rh4 2.7588(7) . ? Rh3 Rh3 2.8293(8) 4_565 ? Rh4 C6 1.902(9) . ? Rh4 C7 1.924(9) . ? Rh4 C8 2.178(5) . ? Rh4 C8 2.178(5) 4_565 ? Rh4 Rh3 2.7588(7) 4_565 ? Rh4 Rh2 2.7593(7) 4_565 ? Ga1 C11 2.261(5) 4_565 ? Ga1 C11 2.261(5) . ? Ga1 C10 2.326(6) . ? Ga1 C10 2.326(6) 4_565 ? Ga1 C9 2.380(8) . ? Ga1 Rh2 2.5957(8) 4_565 ? Ga2 C15 2.293(5) 4_565 ? Ga2 C15 2.293(5) . ? Ga2 C16 2.353(6) 4_565 ? Ga2 C16 2.353(6) . ? Ga2 C17 2.402(8) . ? Ga2 Rh3 2.5608(9) 4_565 ? O1 C1 1.131(6) . ? O2 C2 1.139(6) . ? O3 C3 1.142(6) . ? O4 C4 1.144(6) . ? O5 C5 1.127(6) . ? O6 C6 1.135(9) . ? O7 C7 1.113(9) . ? O8 C8 1.181(6) . ? C9 C10 1.425(8) . ? C9 C10 1.425(8) 4_565 ? C9 C12 1.497(12) . ? C10 C11 1.409(8) . ? C10 C13 1.507(8) . ? C11 C11 1.425(11) 4_565 ? C11 C14 1.518(8) . ? C15 C16 1.424(8) . ? C15 C15 1.439(10) 4_565 ? C15 C18 1.500(8) . ? C16 C17 1.427(7) . ? C16 C19 1.495(7) . ? C17 C16 1.427(7) 4_565 ? C17 C20 1.496(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 C1 Rh1 C1 96.6(3) . 4_565 ? C1 Rh1 Ga2 94.29(17) . . ? C1 Rh1 Ga2 94.29(17) 4_565 . ? C1 Rh1 Ga1 91.72(17) . . ? C1 Rh1 Ga1 91.72(17) 4_565 . ? Ga2 Rh1 Ga1 170.96(4) . . ? C1 Rh1 Rh3 96.17(16) . . ? C1 Rh1 Rh3 149.15(17) 4_565 . ? Ga2 Rh1 Rh3 56.78(2) . . ? Ga1 Rh1 Rh3 115.85(3) . . ? C1 Rh1 Rh3 149.15(17) . 4_565 ? C1 Rh1 Rh3 96.17(16) 4_565 4_565 ? Ga2 Rh1 Rh3 56.78(2) . 4_565 ? Ga1 Rh1 Rh3 115.85(3) . 4_565 ? Rh3 Rh1 Rh3 60.41(2) . 4_565 ? C1 Rh1 Rh2 147.17(17) . 4_565 ? C1 Rh1 Rh2 95.18(16) 4_565 4_565 ? Ga2 Rh1 Rh2 115.27(3) . 4_565 ? Ga1 Rh1 Rh2 57.34(2) . 4_565 ? Rh3 Rh1 Rh2 89.09(2) . 4_565 ? Rh3 Rh1 Rh2 58.571(16) 4_565 4_565 ? C1 Rh1 Rh2 95.18(16) . . ? C1 Rh1 Rh2 147.17(17) 4_565 . ? Ga2 Rh1 Rh2 115.27(3) . . ? Ga1 Rh1 Rh2 57.34(2) . . ? Rh3 Rh1 Rh2 58.570(16) . . ? Rh3 Rh1 Rh2 89.09(2) 4_565 . ? Rh2 Rh1 Rh2 60.32(2) 4_565 . ? C3 Rh2 C2 95.0(2) . . ? C3 Rh2 C8 98.2(2) . . ? C2 Rh2 C8 97.4(2) . . ? C3 Rh2 Ga1 92.82(16) . . ? C2 Rh2 Ga1 93.79(16) . . ? C8 Rh2 Ga1 163.47(15) . . ? C3 Rh2 Rh3 147.93(16) . . ? C2 Rh2 Rh3 95.49(16) . . ? C8 Rh2 Rh3 50.34(15) . . ? Ga1 Rh2 Rh3 116.57(2) . . ? C3 Rh2 Rh4 96.85(16) . . ? C2 Rh2 Rh4 147.38(16) . . ? C8 Rh2 Rh4 50.85(14) . . ? Ga1 Rh2 Rh4 115.772(19) . . ? Rh3 Rh2 Rh4 59.999(17) . . ? C3 Rh2 Rh1 147.46(16) . . ? C2 Rh2 Rh1 96.55(16) . . ? C8 Rh2 Rh1 110.21(15) . . ? Ga1 Rh2 Rh1 56.19(2) . . ? Rh3 Rh2 Rh1 60.439(17) . . ? Rh4 Rh2 Rh1 89.501(19) . . ? C3 Rh2 Rh2 96.52(15) . 4_565 ? C2 Rh2 Rh2 148.81(16) . 4_565 ? C8 Rh2 Rh2 109.41(15) . 4_565 ? Ga1 Rh2 Rh2 56.825(14) . 4_565 ? Rh3 Rh2 Rh2 89.881(11) . 4_565 ? Rh4 Rh2 Rh2 59.019(11) . 4_565 ? Rh1 Rh2 Rh2 59.840(10) . 4_565 ? C4 Rh3 C5 95.8(2) . . ? C4 Rh3 C8 98.0(2) . . ? C5 Rh3 C8 97.5(2) . . ? C4 Rh3 Ga2 93.65(17) . . ? C5 Rh3 Ga2 92.65(17) . . ? C8 Rh3 Ga2 163.64(15) . . ? C4 Rh3 Rh2 95.97(16) . . ? C5 Rh3 Rh2 146.82(17) . . ? C8 Rh3 Rh2 50.07(15) . . ? Ga2 Rh3 Rh2 117.40(3) . . ? C4 Rh3 Rh4 147.99(16) . . ? C5 Rh3 Rh4 95.59(16) . . ? C8 Rh3 Rh4 50.81(14) . . ? Ga2 Rh3 Rh4 115.58(2) . . ? Rh2 Rh3 Rh4 60.016(17) . . ? C4 Rh3 Rh1 96.43(16) . . ? C5 Rh3 Rh1 147.40(16) . . ? C8 Rh3 Rh1 110.49(15) . . ? Ga2 Rh3 Rh1 56.50(2) . . ? Rh2 Rh3 Rh1 60.991(17) . . ? Rh4 Rh3 Rh1 89.825(19) . . ? C4 Rh3 Rh3 148.33(17) . 4_565 ? C5 Rh3 Rh3 95.90(15) . 4_565 ? C8 Rh3 Rh3 109.49(14) . 4_565 ? Ga2 Rh3 Rh3 56.467(14) . 4_565 ? Rh2 Rh3 Rh3 90.120(11) . 4_565 ? Rh4 Rh3 Rh3 59.151(11) . 4_565 ? Rh1 Rh3 Rh3 59.795(10) . 4_565 ? C6 Rh4 C7 95.2(3) . . ? C6 Rh4 C8 97.65(15) . . ? C7 Rh4 C8 97.72(15) . . ? C6 Rh4 C8 97.65(15) . 4_565 ? C7 Rh4 C8 97.72(15) . 4_565 ? C8 Rh4 C8 157.1(3) . 4_565 ? C6 Rh4 Rh3 147.18(8) . . ? C7 Rh4 Rh3 95.7(2) . . ? C8 Rh4 Rh3 50.19(14) . . ? C8 Rh4 Rh3 111.41(14) 4_565 . ? C6 Rh4 Rh3 147.18(8) . 4_565 ? C7 Rh4 Rh3 95.7(2) . 4_565 ? C8 Rh4 Rh3 111.41(14) . 4_565 ? C8 Rh4 Rh3 50.19(14) 4_565 4_565 ? Rh3 Rh4 Rh3 61.70(2) . 4_565 ? C6 Rh4 Rh2 95.9(2) . . ? C7 Rh4 Rh2 146.95(8) . . ? C8 Rh4 Rh2 49.96(15) . . ? C8 Rh4 Rh2 111.45(15) 4_565 . ? Rh3 Rh4 Rh2 59.985(16) . . ? Rh3 Rh4 Rh2 91.59(2) 4_565 . ? C6 Rh4 Rh2 95.9(2) . 4_565 ? C7 Rh4 Rh2 146.95(8) . 4_565 ? C8 Rh4 Rh2 111.45(15) . 4_565 ? C8 Rh4 Rh2 49.96(15) 4_565 4_565 ? Rh3 Rh4 Rh2 91.59(2) . 4_565 ? Rh3 Rh4 Rh2 59.986(16) 4_565 4_565 ? Rh2 Rh4 Rh2 61.96(2) . 4_565 ? C11 Ga1 C11 36.7(3) 4_565 . ? C11 Ga1 C10 59.89(19) 4_565 . ? C11 Ga1 C10 35.8(2) . . ? C11 Ga1 C10 35.8(2) 4_565 4_565 ? C11 Ga1 C10 59.89(19) . 4_565 ? C10 Ga1 C10 58.9(3) . 4_565 ? C11 Ga1 C9 59.5(2) 4_565 . ? C11 Ga1 C9 59.5(2) . . ? C10 Ga1 C9 35.22(18) . . ? C10 Ga1 C9 35.23(18) 4_565 . ? C11 Ga1 Rh1 154.64(15) 4_565 . ? C11 Ga1 Rh1 154.64(15) . . ? C10 Ga1 Rh1 119.81(15) . . ? C10 Ga1 Rh1 119.81(15) 4_565 . ? C9 Ga1 Rh1 104.6(2) . . ? C11 Ga1 Rh2 113.68(14) 4_565 4_565 ? C11 Ga1 Rh2 138.29(16) . 4_565 ? C10 Ga1 Rh2 173.44(15) . 4_565 ? C10 Ga1 Rh2 117.08(14) 4_565 4_565 ? C9 Ga1 Rh2 144.33(7) . 4_565 ? Rh1 Ga1 Rh2 66.48(2) . 4_565 ? C11 Ga1 Rh2 138.29(16) 4_565 . ? C11 Ga1 Rh2 113.68(14) . . ? C10 Ga1 Rh2 117.08(14) . . ? C10 Ga1 Rh2 173.44(15) 4_565 . ? C9 Ga1 Rh2 144.33(7) . . ? Rh1 Ga1 Rh2 66.48(2) . . ? Rh2 Ga1 Rh2 66.35(3) 4_565 . ? C15 Ga2 C15 36.6(3) 4_565 . ? C15 Ga2 C16 35.67(19) 4_565 4_565 ? C15 Ga2 C16 59.77(19) . 4_565 ? C15 Ga2 C16 59.77(19) 4_565 . ? C15 Ga2 C16 35.67(19) . . ? C16 Ga2 C16 59.0(3) 4_565 . ? C15 Ga2 C17 58.7(2) 4_565 . ? C15 Ga2 C17 58.7(2) . . ? C16 Ga2 C17 34.90(17) 4_565 . ? C16 Ga2 C17 34.90(17) . . ? C15 Ga2 Rh1 116.29(15) 4_565 . ? C15 Ga2 Rh1 116.29(15) . . ? C16 Ga2 Rh1 142.11(15) 4_565 . ? C16 Ga2 Rh1 142.11(15) . . ? C17 Ga2 Rh1 174.60(19) . . ? C15 Ga2 Rh3 128.18(13) 4_565 4_565 ? C15 Ga2 Rh3 164.74(13) . 4_565 ? C16 Ga2 Rh3 108.01(13) 4_565 4_565 ? C16 Ga2 Rh3 148.57(16) . 4_565 ? C17 Ga2 Rh3 117.55(15) . 4_565 ? Rh1 Ga2 Rh3 66.72(3) . 4_565 ? C15 Ga2 Rh3 164.74(13) 4_565 . ? C15 Ga2 Rh3 128.18(13) . . ? C16 Ga2 Rh3 148.57(16) 4_565 . ? C16 Ga2 Rh3 108.02(13) . . ? C17 Ga2 Rh3 117.55(15) . . ? Rh1 Ga2 Rh3 66.72(3) . . ? Rh3 Ga2 Rh3 67.07(3) 4_565 . ? O1 C1 Rh1 178.0(5) . . ? O2 C2 Rh2 176.9(5) . . ? O3 C3 Rh2 177.5(5) . . ? O4 C4 Rh3 178.0(5) . . ? O5 C5 Rh3 178.0(5) . . ? O6 C6 Rh4 179.3(7) . . ? O7 C7 Rh4 179.1(8) . . ? O8 C8 Rh2 133.1(4) . . ? O8 C8 Rh3 131.7(4) . . ? Rh2 C8 Rh3 79.60(19) . . ? O8 C8 Rh4 132.9(4) . . ? Rh2 C8 Rh4 79.20(19) . . ? Rh3 C8 Rh4 79.00(19) . . ? C10 C9 C10 106.8(7) . 4_565 ? C10 C9 C12 126.6(4) . . ? C10 C9 C12 126.6(4) 4_565 . ? C10 C9 Ga1 70.3(4) . . ? C10 C9 Ga1 70.3(4) 4_565 . ? C12 C9 Ga1 126.3(6) . . ? C11 C10 C9 108.8(5) . . ? C11 C10 C13 124.8(6) . . ? C9 C10 C13 126.1(6) . . ? C11 C10 Ga1 69.6(3) . . ? C9 C10 Ga1 74.5(4) . . ? C13 C10 Ga1 126.2(4) . . ? C10 C11 C11 107.8(3) . 4_565 ? C10 C11 C14 126.6(6) . . ? C11 C11 C14 125.2(4) 4_565 . ? C10 C11 Ga1 74.6(3) . . ? C11 C11 Ga1 71.63(14) 4_565 . ? C14 C11 Ga1 124.8(4) . . ? C16 C15 C15 108.0(3) . 4_565 ? C16 C15 C18 126.1(5) . . ? C15 C15 C18 125.9(3) 4_565 . ? C16 C15 Ga2 74.4(3) . . ? C15 C15 Ga2 71.72(13) 4_565 . ? C18 C15 Ga2 122.3(4) . . ? C15 C16 C17 107.7(5) . . ? C15 C16 C19 126.4(5) . . ? C17 C16 C19 125.7(6) . . ? C15 C16 Ga2 69.9(3) . . ? C17 C16 Ga2 74.4(4) . . ? C19 C16 Ga2 125.6(4) . . ? C16 C17 C16 108.6(7) . 4_565 ? C16 C17 C20 125.7(4) . . ? C16 C17 C20 125.7(4) 4_565 . ? C16 C17 Ga2 70.7(4) . . ? C16 C17 Ga2 70.7(4) 4_565 . ? C20 C17 Ga2 126.1(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.994 _refine_diff_density_min -0.986 _refine_diff_density_rms 0.140 #===END data_compound3 _database_code_CSD 172645 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H49 Cl4 Ga3 O13 Rh6' _chemical_formula_sum 'C45 H49 Cl4 Ga3 O13 Rh6' _chemical_formula_weight 1766.26 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' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.43400(10) _cell_length_b 17.4920(2) _cell_length_c 24.9780(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5432.60(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6827 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3416 _exptl_absorpt_coefficient_mu 3.492 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6596 _exptl_absorpt_correction_T_max 0.8730 _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'CCD; rotation images' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72288 _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.49 _reflns_number_total 12394 _reflns_number_gt 10778 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0125P)^2^+11.5821P] 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 0.00022(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.313(10) _refine_ls_number_reflns 12394 _refine_ls_number_parameters 657 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0615 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.89961(3) 0.18820(2) 0.308769(15) 0.01640(9) Uani 1 1 d . . . Rh2 Rh 0.91497(3) 0.19060(2) 0.199001(14) 0.01645(9) Uani 1 1 d . . . Rh3 Rh 0.72419(3) 0.147457(18) 0.247205(16) 0.01558(8) Uani 1 1 d . . . Rh4 Rh 0.91025(3) 0.330406(18) 0.255700(16) 0.01672(8) Uani 1 1 d . . . Rh5 Rh 0.73339(3) 0.28717(2) 0.191372(15) 0.01574(9) Uani 1 1 d . . . Rh6 Rh 0.71739(3) 0.28549(2) 0.304907(15) 0.01614(9) Uani 1 1 d . . . Ga1 Ga 0.88958(4) 0.31785(3) 0.35687(2) 0.01921(12) Uani 1 1 d . . . Ga2 Ga 0.91657(4) 0.32147(3) 0.15411(2) 0.01970(12) Uani 1 1 d . . . Ga3 Ga 0.56648(4) 0.24422(3) 0.24101(2) 0.01817(12) Uani 1 1 d . . . O1 O 0.9083(2) 0.03225(16) 0.25166(15) 0.0201(6) Uani 1 1 d . . . O2 O 0.8301(3) 0.0986(2) 0.40687(16) 0.0331(9) Uani 1 1 d . . . O3 O 1.1397(3) 0.1696(2) 0.32520(15) 0.0311(9) Uani 1 1 d . . . O4 O 1.1570(3) 0.1731(2) 0.19573(15) 0.0322(9) Uani 1 1 d . . . O5 O 0.8799(3) 0.1118(2) 0.09265(15) 0.0341(10) Uani 1 1 d . . . O6 O 0.6471(3) 0.0508(2) 0.15414(15) 0.0336(10) Uani 1 1 d . . . O7 O 0.6214(3) 0.0538(2) 0.33577(15) 0.0295(9) Uani 1 1 d . . . O8 O 1.1532(3) 0.3409(2) 0.26401(15) 0.0309(9) Uani 1 1 d . . . O9 O 0.8545(3) 0.49889(17) 0.25258(18) 0.0280(8) Uani 1 1 d . . . O10 O 0.6570(3) 0.2225(2) 0.08529(14) 0.0288(9) Uani 1 1 d . . . O11 O 0.6471(3) 0.4476(2) 0.17762(16) 0.0289(9) Uani 1 1 d . . . O12 O 0.6119(3) 0.2171(2) 0.40329(14) 0.0295(9) Uani 1 1 d . . . O13 O 0.6319(3) 0.4460(2) 0.31943(16) 0.0315(9) Uani 1 1 d . . . C1 C 0.8803(3) 0.0961(2) 0.2511(2) 0.0190(9) Uani 1 1 d . . . C2 C 0.8565(4) 0.1331(3) 0.3711(2) 0.0220(12) Uani 1 1 d . . . C3 C 1.0496(4) 0.1779(3) 0.3199(2) 0.0223(11) Uani 1 1 d . . . C4 C 1.0670(4) 0.1797(3) 0.19687(19) 0.0216(11) Uani 1 1 d . . . C5 C 0.8928(4) 0.1415(3) 0.1324(2) 0.0223(11) Uani 1 1 d . . . C6 C 0.6737(4) 0.0874(3) 0.1895(2) 0.0244(12) Uani 1 1 d . . . C7 C 0.6583(4) 0.0900(3) 0.3019(2) 0.0200(11) Uani 1 1 d . . . C8 C 1.0617(4) 0.3392(3) 0.26087(19) 0.0223(11) Uani 1 1 d . . . C9 C 0.8777(3) 0.4358(3) 0.2542(2) 0.0212(10) Uani 1 1 d . . . C10 C 0.6849(4) 0.2479(3) 0.1252(2) 0.0201(11) Uani 1 1 d . . . C11 C 0.6793(4) 0.3879(3) 0.1822(2) 0.0197(11) Uani 1 1 d . . . C12 C 0.6492(4) 0.2440(3) 0.3661(2) 0.0204(11) Uani 1 1 d . . . C13 C 0.6632(4) 0.3854(3) 0.3136(2) 0.0207(11) Uani 1 1 d . . . C14 C 0.9121(4) 0.4273(3) 0.40639(19) 0.0243(12) Uani 1 1 d . . . C15 C 0.8409(4) 0.3801(3) 0.4359(2) 0.0240(12) Uani 1 1 d . . . C16 C 0.8976(4) 0.3136(3) 0.45125(19) 0.0227(11) Uani 1 1 d . . . C17 C 1.0062(4) 0.3188(4) 0.4313(2) 0.0276(12) Uani 1 1 d . . . C18 C 1.0154(4) 0.3912(3) 0.4038(2) 0.0269(13) Uani 1 1 d . . . C19 C 0.8875(5) 0.5070(3) 0.3862(2) 0.0321(14) Uani 1 1 d . . . H19A H 0.8112 0.5104 0.3765 0.048 Uiso 1 1 calc R . . H19B H 0.9317 0.5179 0.3546 0.048 Uiso 1 1 calc R . . H19C H 0.9035 0.5444 0.4143 0.048 Uiso 1 1 calc R . . C20 C 0.7285(4) 0.3992(3) 0.4518(2) 0.0303(13) Uani 1 1 d . . . H20A H 0.6851 0.3525 0.4525 0.046 Uiso 1 1 calc R . . H20B H 0.6979 0.4353 0.4260 0.046 Uiso 1 1 calc R . . H20C H 0.7288 0.4225 0.4875 0.046 Uiso 1 1 calc R . . C21 C 0.8566(5) 0.2493(4) 0.4865(2) 0.0329(14) Uani 1 1 d . . . H21A H 0.8592 0.2652 0.5241 0.049 Uiso 1 1 calc R . . H21B H 0.9018 0.2040 0.4815 0.049 Uiso 1 1 calc R . . H21C H 0.7822 0.2371 0.4767 0.049 Uiso 1 1 calc R . . C22 C 1.0934(5) 0.2631(4) 0.4418(2) 0.0375(15) Uani 1 1 d . . . H22A H 1.1168 0.2676 0.4792 0.056 Uiso 1 1 calc R . . H22B H 1.1542 0.2737 0.4180 0.056 Uiso 1 1 calc R . . H22C H 1.0668 0.2112 0.4353 0.056 Uiso 1 1 calc R . . C23 C 1.1161(4) 0.4230(3) 0.3800(2) 0.0312(13) Uani 1 1 d . . . H23A H 1.0996 0.4470 0.3455 0.047 Uiso 1 1 calc R . . H23B H 1.1682 0.3817 0.3746 0.047 Uiso 1 1 calc R . . H23C H 1.1467 0.4613 0.4043 0.047 Uiso 1 1 calc R . . C24 C 1.0441(4) 0.3790(3) 0.1084(2) 0.0244(12) Uani 1 1 d . . . C25 C 0.9444(4) 0.4211(3) 0.0998(2) 0.0223(11) Uani 1 1 d . . . C26 C 0.8818(4) 0.3773(3) 0.0629(2) 0.0216(11) Uani 1 1 d . . . C27 C 0.9406(4) 0.3112(3) 0.04834(19) 0.0209(11) Uani 1 1 d . . . C28 C 1.0393(4) 0.3122(3) 0.0763(2) 0.0253(12) Uani 1 1 d . . . C29 C 1.1407(4) 0.4085(3) 0.1382(2) 0.0286(13) Uani 1 1 d . . . H29A H 1.1824 0.3652 0.1522 0.043 Uiso 1 1 calc R . . H29B H 1.1170 0.4407 0.1681 0.043 Uiso 1 1 calc R . . H29C H 1.1858 0.4386 0.1139 0.043 Uiso 1 1 calc R . . C30 C 0.9197(5) 0.5003(3) 0.1193(2) 0.0280(13) Uani 1 1 d . . . H30A H 0.9404 0.5376 0.0920 0.042 Uiso 1 1 calc R . . H30B H 0.9600 0.5102 0.1523 0.042 Uiso 1 1 calc R . . H30C H 0.8424 0.5047 0.1265 0.042 Uiso 1 1 calc R . . C31 C 0.7746(4) 0.3999(3) 0.0411(2) 0.0284(13) Uani 1 1 d . . . H31A H 0.7287 0.3545 0.0381 0.043 Uiso 1 1 calc R . . H31B H 0.7839 0.4229 0.0056 0.043 Uiso 1 1 calc R . . H31C H 0.7409 0.4370 0.0652 0.043 Uiso 1 1 calc R . . C32 C 0.9054(4) 0.2517(3) 0.0087(2) 0.0281(12) Uani 1 1 d . . . H32A H 0.9618 0.2129 0.0050 0.042 Uiso 1 1 calc R . . H32B H 0.8923 0.2758 -0.0261 0.042 Uiso 1 1 calc R . . H32C H 0.8390 0.2274 0.0213 0.042 Uiso 1 1 calc R . . C33 C 1.1280(4) 0.2532(3) 0.0704(2) 0.0298(13) Uani 1 1 d . . . H33A H 1.0972 0.2018 0.0733 0.045 Uiso 1 1 calc R . . H33B H 1.1816 0.2606 0.0986 0.045 Uiso 1 1 calc R . . H33C H 1.1624 0.2591 0.0353 0.045 Uiso 1 1 calc R . . C34 C 0.4029(3) 0.1905(2) 0.2452(2) 0.0194(9) Uani 1 1 d . . . C35 C 0.4005(4) 0.2596(3) 0.27520(18) 0.0209(11) Uani 1 1 d . . . C36 C 0.4104(4) 0.3215(3) 0.23854(19) 0.0198(10) Uani 1 1 d . . . C37 C 0.4177(4) 0.2908(3) 0.1856(2) 0.0200(10) Uani 1 1 d . . . C38 C 0.4135(4) 0.2106(3) 0.18951(19) 0.0192(10) Uani 1 1 d . . . C39 C 0.3859(4) 0.1105(3) 0.2661(2) 0.0243(12) Uani 1 1 d . . . H39A H 0.4076 0.1082 0.3038 0.036 Uiso 1 1 calc R . . H39B H 0.4293 0.0746 0.2452 0.036 Uiso 1 1 calc R . . H39C H 0.3097 0.0969 0.2630 0.036 Uiso 1 1 calc R . . C40 C 0.3800(4) 0.2675(3) 0.3338(2) 0.0255(12) Uani 1 1 d . . . H40A H 0.3034 0.2777 0.3398 0.038 Uiso 1 1 calc R . . H40B H 0.4227 0.3100 0.3480 0.038 Uiso 1 1 calc R . . H40C H 0.4003 0.2201 0.3520 0.038 Uiso 1 1 calc R . . C41 C 0.4044(4) 0.4056(2) 0.2532(2) 0.0253(10) Uani 1 1 d . . . H41A H 0.3319 0.4249 0.2458 0.038 Uiso 1 1 calc R . . H41B H 0.4568 0.4343 0.2319 0.038 Uiso 1 1 calc R . . H41C H 0.4207 0.4120 0.2913 0.038 Uiso 1 1 calc R . . C42 C 0.4264(4) 0.3362(3) 0.1347(2) 0.0265(12) Uani 1 1 d . . . H42A H 0.4922 0.3216 0.1157 0.040 Uiso 1 1 calc R . . H42B H 0.4287 0.3908 0.1432 0.040 Uiso 1 1 calc R . . H42C H 0.3638 0.3256 0.1120 0.040 Uiso 1 1 calc R . . C43 C 0.4094(4) 0.1556(3) 0.1434(2) 0.0263(12) Uani 1 1 d . . . H43A H 0.3363 0.1541 0.1289 0.039 Uiso 1 1 calc R . . H43B H 0.4298 0.1045 0.1559 0.039 Uiso 1 1 calc R . . H43C H 0.4595 0.1723 0.1155 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.90011(13) 0.42081(9) 0.57849(6) 0.0387(4) Uani 1 1 d . . . Cl2 Cl 1.00992(13) 0.54521(9) 0.52316(6) 0.0402(4) Uani 1 1 d . . . C44 C 1.0130(5) 0.4477(3) 0.5400(2) 0.0337(14) Uani 1 1 d . . . H44A H 1.0794 0.4367 0.5605 0.040 Uiso 1 1 calc R . . H44B H 1.0149 0.4168 0.5068 0.040 Uiso 1 1 calc R . . Cl3 Cl 0.28282(13) 0.54802(10) 0.49570(7) 0.0476(4) Uani 1 1 d . . . Cl4 Cl 0.45240(18) 0.44663(13) 0.46005(10) 0.0787(7) Uani 1 1 d . . . C45 C 0.4180(6) 0.5408(4) 0.4765(3) 0.0504(17) Uani 1 1 d . . . H45A H 0.4311 0.5742 0.4452 0.061 Uiso 1 1 calc R . . H45B H 0.4644 0.5586 0.5062 0.061 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 Rh1 0.01360(18) 0.0177(2) 0.01788(18) 0.00089(16) -0.00127(16) 0.00099(15) Rh2 0.01248(18) 0.0183(2) 0.01856(19) -0.00055(16) 0.00085(16) 0.00083(16) Rh3 0.01302(17) 0.01545(15) 0.01828(18) -0.00014(18) 0.00021(17) -0.00084(13) Rh4 0.01209(17) 0.01695(16) 0.02112(19) 0.00036(17) -0.00056(17) -0.00155(13) Rh5 0.01257(18) 0.0159(2) 0.01875(19) 0.00100(16) -0.00138(15) 0.00005(15) Rh6 0.01276(17) 0.0166(2) 0.01906(19) -0.00065(16) 0.00070(15) 0.00024(15) Ga1 0.0169(3) 0.0201(3) 0.0206(3) -0.0012(2) -0.0020(2) -0.0010(2) Ga2 0.0158(3) 0.0202(3) 0.0231(3) 0.0026(2) 0.0016(2) -0.0015(2) Ga3 0.0126(2) 0.0196(2) 0.0223(3) 0.0005(2) -0.0001(2) -0.00075(19) O1 0.0168(16) 0.0215(16) 0.0219(16) -0.0010(17) 0.0012(17) 0.0028(13) O2 0.036(2) 0.034(2) 0.030(2) 0.0055(19) 0.0021(18) -0.0006(19) O3 0.016(2) 0.039(2) 0.039(2) 0.0036(19) -0.0038(16) -0.0004(17) O4 0.020(2) 0.042(2) 0.035(2) 0.001(2) -0.0003(17) 0.0011(17) O5 0.041(2) 0.036(2) 0.025(2) -0.0073(19) -0.0048(18) 0.0045(19) O6 0.043(3) 0.031(2) 0.027(2) -0.0051(19) -0.0073(18) -0.0048(19) O7 0.034(2) 0.028(2) 0.026(2) 0.0022(18) 0.0044(17) -0.0076(18) O8 0.0123(18) 0.042(2) 0.038(2) 0.0015(18) -0.0022(16) -0.0024(15) O9 0.0220(18) 0.0207(17) 0.041(2) 0.003(2) 0.0001(19) 0.0023(13) O10 0.028(2) 0.036(2) 0.022(2) -0.0077(18) -0.0018(16) -0.0029(18) O11 0.032(2) 0.019(2) 0.035(2) 0.0034(18) -0.0021(17) 0.0054(17) O12 0.027(2) 0.035(2) 0.026(2) 0.0026(18) 0.0033(17) -0.0021(18) O13 0.033(2) 0.025(2) 0.037(2) -0.0026(19) -0.0023(18) 0.0071(18) C1 0.016(2) 0.023(2) 0.018(2) -0.006(3) -0.002(2) -0.0027(17) C2 0.022(3) 0.021(3) 0.024(3) -0.002(2) 0.001(2) 0.001(2) C3 0.022(3) 0.024(3) 0.020(3) -0.002(2) -0.002(2) 0.002(2) C4 0.014(2) 0.028(3) 0.023(3) 0.003(2) 0.002(2) 0.003(2) C5 0.022(3) 0.019(3) 0.026(3) 0.002(2) 0.001(2) 0.005(2) C6 0.024(3) 0.020(3) 0.029(3) 0.004(3) -0.008(2) -0.002(2) C7 0.019(3) 0.019(3) 0.022(3) -0.005(2) -0.004(2) 0.000(2) C8 0.023(3) 0.022(2) 0.022(3) 0.000(2) -0.002(2) -0.004(2) C9 0.013(2) 0.031(3) 0.020(2) 0.000(3) -0.001(2) -0.0034(19) C10 0.009(2) 0.019(3) 0.032(3) 0.005(2) -0.002(2) 0.001(2) C11 0.019(3) 0.022(3) 0.019(3) 0.000(2) 0.000(2) -0.003(2) C12 0.015(3) 0.019(3) 0.027(3) -0.003(2) 0.000(2) 0.001(2) C13 0.022(3) 0.023(3) 0.017(3) 0.001(2) -0.004(2) -0.002(2) C14 0.025(3) 0.028(3) 0.020(3) -0.005(2) -0.009(2) -0.002(2) C15 0.024(3) 0.026(3) 0.022(3) -0.004(2) -0.003(2) -0.003(2) C16 0.025(3) 0.026(3) 0.017(2) -0.002(2) -0.003(2) -0.008(2) C17 0.030(3) 0.034(3) 0.019(3) -0.008(3) -0.005(2) 0.003(3) C18 0.023(3) 0.037(3) 0.021(3) -0.009(3) 0.000(2) -0.005(2) C19 0.039(4) 0.024(3) 0.033(3) 0.002(2) -0.007(3) -0.007(3) C20 0.026(3) 0.034(3) 0.031(3) -0.004(3) -0.001(2) -0.001(3) C21 0.042(4) 0.033(3) 0.024(3) -0.006(3) 0.000(2) 0.000(3) C22 0.038(3) 0.048(4) 0.026(3) -0.009(3) -0.005(3) 0.012(3) C23 0.026(3) 0.034(3) 0.034(3) -0.006(3) -0.002(3) -0.006(3) C24 0.025(3) 0.025(3) 0.023(3) 0.001(2) 0.005(2) -0.007(2) C25 0.020(3) 0.023(3) 0.024(3) 0.000(2) 0.005(2) -0.006(2) C26 0.024(3) 0.020(3) 0.021(3) 0.007(2) 0.003(2) -0.004(2) C27 0.021(3) 0.021(3) 0.021(2) 0.005(2) 0.006(2) 0.001(2) C28 0.025(3) 0.024(3) 0.027(3) 0.003(2) 0.009(2) -0.003(2) C29 0.029(3) 0.028(3) 0.028(3) -0.001(3) 0.002(2) -0.006(2) C30 0.031(3) 0.025(3) 0.028(3) 0.004(2) 0.006(3) -0.002(3) C31 0.027(3) 0.031(3) 0.028(3) 0.004(2) -0.001(2) -0.001(2) C32 0.032(3) 0.029(3) 0.023(3) -0.006(2) 0.000(2) -0.006(3) C33 0.026(3) 0.031(3) 0.033(3) 0.001(3) 0.009(2) 0.008(2) C34 0.012(2) 0.020(2) 0.027(3) 0.000(2) -0.001(2) 0.0005(17) C35 0.011(2) 0.024(3) 0.027(3) 0.004(2) 0.001(2) 0.001(2) C36 0.010(2) 0.020(2) 0.030(3) 0.001(2) 0.000(2) -0.0018(19) C37 0.010(2) 0.021(3) 0.029(3) 0.007(2) -0.001(2) 0.000(2) C38 0.011(2) 0.023(2) 0.024(2) 0.000(2) -0.001(2) 0.0034(19) C39 0.017(3) 0.022(2) 0.034(3) 0.004(2) -0.002(2) -0.001(2) C40 0.019(3) 0.028(3) 0.030(3) 0.003(2) 0.003(2) 0.001(2) C41 0.019(2) 0.022(2) 0.035(3) 0.003(3) -0.001(3) 0.0027(18) C42 0.017(3) 0.032(3) 0.030(3) 0.004(2) -0.002(2) 0.001(2) C43 0.019(3) 0.032(3) 0.028(3) -0.001(2) -0.003(2) -0.001(2) Cl1 0.0495(10) 0.0360(8) 0.0305(7) 0.0032(6) 0.0023(7) 0.0016(7) Cl2 0.0470(9) 0.0353(8) 0.0382(8) 0.0007(7) 0.0026(7) -0.0031(7) C44 0.037(3) 0.034(3) 0.030(3) -0.005(3) 0.000(3) 0.005(3) Cl3 0.0431(9) 0.0536(10) 0.0462(9) -0.0016(8) -0.0106(8) 0.0085(8) Cl4 0.0678(14) 0.0694(14) 0.0987(17) 0.0261(13) 0.0242(12) 0.0298(12) C45 0.048(4) 0.064(5) 0.039(4) 0.001(3) -0.007(3) -0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C3 1.895(5) . ? Rh1 C2 1.908(6) . ? Rh1 C1 2.174(5) . ? Rh1 Ga1 2.5696(7) . ? Rh1 Rh2 2.7488(5) . ? Rh1 Rh3 2.7623(5) . ? Rh1 Rh4 2.8218(5) . ? Rh1 Rh6 2.8354(5) . ? Rh2 C5 1.892(5) . ? Rh2 C4 1.900(5) . ? Rh2 C1 2.148(5) . ? Rh2 Ga2 2.5492(7) . ? Rh2 Rh3 2.7653(5) . ? Rh2 Rh5 2.8261(5) . ? Rh2 Rh4 2.8266(5) . ? Rh3 C7 1.884(5) . ? Rh3 C6 1.891(6) . ? Rh3 C1 2.141(4) . ? Rh3 Ga3 2.5949(6) . ? Rh3 Rh6 2.8133(5) . ? Rh3 Rh5 2.8160(5) . ? Rh4 C9 1.888(5) . ? Rh4 C8 1.893(5) . ? Rh4 Ga2 2.5436(7) . ? Rh4 Ga1 2.5496(7) . ? Rh4 Rh6 2.8068(5) . ? Rh4 Rh5 2.8266(5) . ? Rh5 C10 1.889(5) . ? Rh5 C11 1.900(6) . ? Rh5 Ga3 2.5316(6) . ? Rh5 Ga2 2.5326(6) . ? Rh5 Rh6 2.8430(5) . ? Rh6 C13 1.886(6) . ? Rh6 C12 1.891(5) . ? Rh6 Ga3 2.5670(6) . ? Rh6 Ga1 2.5669(6) . ? Ga1 C14 2.297(5) . ? Ga1 C15 2.333(5) . ? Ga1 C18 2.338(5) . ? Ga1 C17 2.358(5) . ? Ga1 C16 2.361(5) . ? Ga2 C24 2.198(5) . ? Ga2 C25 2.236(5) . ? Ga2 C28 2.476(5) . ? Ga2 C26 2.517(5) . ? Ga3 C34 2.243(4) . ? Ga3 C35 2.250(5) . ? Ga3 C36 2.367(4) . ? Ga3 C38 2.371(5) . ? Ga3 C37 2.450(5) . ? O1 C1 1.170(5) . ? O2 C2 1.127(6) . ? O3 C3 1.138(6) . ? O4 C4 1.126(6) . ? O5 C5 1.132(6) . ? O6 C6 1.140(6) . ? O7 C7 1.151(6) . ? O8 C8 1.142(6) . ? O9 C9 1.141(5) . ? O10 C10 1.145(6) . ? O11 C11 1.124(6) . ? O12 C12 1.141(6) . ? O13 C13 1.139(6) . ? C14 C15 1.418(7) . ? C14 C18 1.433(8) . ? C14 C19 1.515(8) . ? C15 C16 1.413(7) . ? C15 C20 1.491(7) . ? C16 C17 1.442(7) . ? C16 C21 1.517(8) . ? C17 C18 1.445(8) . ? C17 C22 1.481(8) . ? C18 C23 1.494(8) . ? C24 C28 1.418(8) . ? C24 C25 1.458(7) . ? C24 C29 1.505(7) . ? C25 C26 1.429(7) . ? C25 C30 1.500(7) . ? C26 C27 1.415(7) . ? C26 C31 1.493(7) . ? C27 C28 1.413(7) . ? C27 C32 1.503(7) . ? C28 C33 1.518(7) . ? C34 C35 1.423(7) . ? C34 C38 1.440(7) . ? C34 C39 1.509(6) . ? C35 C36 1.423(7) . ? C35 C40 1.492(7) . ? C36 C37 1.430(7) . ? C36 C41 1.517(6) . ? C37 C38 1.408(7) . ? C37 C42 1.502(7) . ? C38 C43 1.501(7) . ? Cl1 C44 1.765(6) . ? Cl2 C44 1.757(6) . ? Cl3 C45 1.752(7) . ? Cl4 C45 1.750(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 C3 Rh1 C2 96.3(2) . . ? C3 Rh1 C1 97.8(2) . . ? C2 Rh1 C1 97.8(2) . . ? C3 Rh1 Ga1 93.65(16) . . ? C2 Rh1 Ga1 92.89(16) . . ? C1 Rh1 Ga1 163.40(13) . . ? C3 Rh1 Rh2 94.53(15) . . ? C2 Rh1 Rh2 147.27(16) . . ? C1 Rh1 Rh2 50.08(14) . . ? Ga1 Rh1 Rh2 117.15(2) . . ? C3 Rh1 Rh3 146.55(16) . . ? C2 Rh1 Rh3 95.86(16) . . ? C1 Rh1 Rh3 49.67(12) . . ? Ga1 Rh1 Rh3 116.72(2) . . ? Rh2 Rh1 Rh3 60.233(14) . . ? C3 Rh1 Rh4 96.13(16) . . ? C2 Rh1 Rh4 147.32(16) . . ? C1 Rh1 Rh4 110.32(14) . . ? Ga1 Rh1 Rh4 56.211(16) . . ? Rh2 Rh1 Rh4 60.968(15) . . ? Rh3 Rh1 Rh4 90.167(15) . . ? C3 Rh1 Rh6 148.11(17) . . ? C2 Rh1 Rh6 96.10(16) . . ? C1 Rh1 Rh6 109.50(12) . . ? Ga1 Rh1 Rh6 56.449(16) . . ? Rh2 Rh1 Rh6 90.711(16) . . ? Rh3 Rh1 Rh6 60.324(13) . . ? Rh4 Rh1 Rh6 59.491(13) . . ? C5 Rh2 C4 94.3(2) . . ? C5 Rh2 C1 98.9(2) . . ? C4 Rh2 C1 98.01(19) . . ? C5 Rh2 Ga2 91.28(16) . . ? C4 Rh2 Ga2 94.03(16) . . ? C1 Rh2 Ga2 163.60(13) . . ? C5 Rh2 Rh1 149.28(16) . . ? C4 Rh2 Rh1 95.48(15) . . ? C1 Rh2 Rh1 50.93(13) . . ? Ga2 Rh2 Rh1 116.94(2) . . ? C5 Rh2 Rh3 97.70(16) . . ? C4 Rh2 Rh3 146.92(15) . . ? C1 Rh2 Rh3 49.74(12) . . ? Ga2 Rh2 Rh3 116.31(2) . . ? Rh1 Rh2 Rh3 60.126(14) . . ? C5 Rh2 Rh5 95.51(15) . . ? C4 Rh2 Rh5 148.52(16) . . ? C1 Rh2 Rh5 109.90(12) . . ? Ga2 Rh2 Rh5 55.933(16) . . ? Rh1 Rh2 Rh5 91.196(16) . . ? Rh3 Rh2 Rh5 60.470(13) . . ? C5 Rh2 Rh4 146.13(16) . . ? C4 Rh2 Rh4 97.00(16) . . ? C1 Rh2 Rh4 110.97(13) . . ? Ga2 Rh2 Rh4 56.194(16) . . ? Rh1 Rh2 Rh4 60.791(15) . . ? Rh3 Rh2 Rh4 90.006(15) . . ? Rh5 Rh2 Rh4 60.004(13) . . ? C7 Rh3 C6 96.4(2) . . ? C7 Rh3 C1 97.9(2) . . ? C6 Rh3 C1 95.9(2) . . ? C7 Rh3 Ga3 93.60(15) . . ? C6 Rh3 Ga3 93.79(16) . . ? C1 Rh3 Ga3 164.04(11) . . ? C7 Rh3 Rh1 94.43(15) . . ? C6 Rh3 Rh1 146.08(16) . . ? C1 Rh3 Rh1 50.73(12) . . ? Ga3 Rh3 Rh1 117.493(19) . . ? C7 Rh3 Rh2 146.56(15) . . ? C6 Rh3 Rh2 96.00(17) . . ? C1 Rh3 Rh2 49.96(13) . . ? Ga3 Rh3 Rh2 116.380(18) . . ? Rh1 Rh3 Rh2 59.641(13) . . ? C7 Rh3 Rh6 94.21(16) . . ? C6 Rh3 Rh6 149.03(16) . . ? C1 Rh3 Rh6 111.34(12) . . ? Ga3 Rh3 Rh6 56.499(15) . . ? Rh1 Rh3 Rh6 61.125(13) . . ? Rh2 Rh3 Rh6 90.838(15) . . ? C7 Rh3 Rh5 147.15(16) . . ? C6 Rh3 Rh5 96.78(16) . . ? C1 Rh3 Rh5 110.48(13) . . ? Ga3 Rh3 Rh5 55.611(15) . . ? Rh1 Rh3 Rh5 91.129(15) . . ? Rh2 Rh3 Rh5 60.835(13) . . ? Rh6 Rh3 Rh5 60.667(12) . . ? C9 Rh4 C8 97.78(19) . . ? C9 Rh4 Ga2 92.72(17) . . ? C8 Rh4 Ga2 92.42(15) . . ? C9 Rh4 Ga1 94.67(17) . . ? C8 Rh4 Ga1 92.27(15) . . ? Ga2 Rh4 Ga1 170.63(2) . . ? C9 Rh4 Rh6 95.65(14) . . ? C8 Rh4 Rh6 147.40(14) . . ? Ga2 Rh4 Rh6 116.492(19) . . ? Ga1 Rh4 Rh6 57.026(16) . . ? C9 Rh4 Rh1 149.30(16) . . ? C8 Rh4 Rh1 94.95(14) . . ? Ga2 Rh4 Rh1 114.577(19) . . ? Ga1 Rh4 Rh1 56.890(17) . . ? Rh6 Rh4 Rh1 60.496(13) . . ? C9 Rh4 Rh5 94.79(14) . . ? C8 Rh4 Rh5 146.52(15) . . ? Ga2 Rh4 Rh5 55.979(16) . . ? Ga1 Rh4 Rh5 117.514(19) . . ? Rh6 Rh4 Rh5 60.618(12) . . ? Rh1 Rh4 Rh5 89.695(14) . . ? C9 Rh4 Rh2 147.11(16) . . ? C8 Rh4 Rh2 94.81(14) . . ? Ga2 Rh4 Rh2 56.381(17) . . ? Ga1 Rh4 Rh2 115.100(19) . . ? Rh6 Rh4 Rh2 89.714(14) . . ? Rh1 Rh4 Rh2 58.240(12) . . ? Rh5 Rh4 Rh2 59.989(13) . . ? C10 Rh5 C11 96.8(2) . . ? C10 Rh5 Ga3 93.40(14) . . ? C11 Rh5 Ga3 92.52(15) . . ? C10 Rh5 Ga2 92.94(14) . . ? C11 Rh5 Ga2 93.12(15) . . ? Ga3 Rh5 Ga2 170.96(2) . . ? C10 Rh5 Rh3 96.02(16) . . ? C11 Rh5 Rh3 148.22(15) . . ? Ga3 Rh5 Rh3 57.763(16) . . ? Ga2 Rh5 Rh3 115.10(2) . . ? C10 Rh5 Rh2 95.54(14) . . ? C11 Rh5 Rh2 147.71(15) . . ? Ga3 Rh5 Rh2 116.393(19) . . ? Ga2 Rh5 Rh2 56.491(16) . . ? Rh3 Rh5 Rh2 58.695(13) . . ? C10 Rh5 Rh4 147.46(14) . . ? C11 Rh5 Rh4 95.50(15) . . ? Ga3 Rh5 Rh4 116.03(2) . . ? Ga2 Rh5 Rh4 56.349(16) . . ? Rh3 Rh5 Rh4 88.988(15) . . ? Rh2 Rh5 Rh4 60.007(13) . . ? C10 Rh5 Rh6 147.88(15) . . ? C11 Rh5 Rh6 96.02(15) . . ? Ga3 Rh5 Rh6 56.704(16) . . ? Ga2 Rh5 Rh6 115.59(2) . . ? Rh3 Rh5 Rh6 59.618(14) . . ? Rh2 Rh5 Rh6 88.998(16) . . ? Rh4 Rh5 Rh6 59.347(13) . . ? C13 Rh6 C12 95.9(2) . . ? C13 Rh6 Ga3 94.09(15) . . ? C12 Rh6 Ga3 93.81(15) . . ? C13 Rh6 Ga1 92.02(15) . . ? C12 Rh6 Ga1 92.87(15) . . ? Ga3 Rh6 Ga1 170.44(2) . . ? C13 Rh6 Rh4 95.53(16) . . ? C12 Rh6 Rh4 147.55(15) . . ? Ga3 Rh6 Rh4 115.531(19) . . ? Ga1 Rh6 Rh4 56.436(16) . . ? C13 Rh6 Rh3 149.92(15) . . ? C12 Rh6 Rh3 95.63(16) . . ? Ga3 Rh6 Rh3 57.453(15) . . ? Ga1 Rh6 Rh3 115.04(2) . . ? Rh4 Rh6 Rh3 89.440(15) . . ? C13 Rh6 Rh1 146.92(15) . . ? C12 Rh6 Rh1 95.77(15) . . ? Ga3 Rh6 Rh1 115.876(19) . . ? Ga1 Rh6 Rh1 56.541(17) . . ? Rh4 Rh6 Rh1 60.013(13) . . ? Rh3 Rh6 Rh1 58.551(13) . . ? C13 Rh6 Rh5 97.51(16) . . ? C12 Rh6 Rh5 147.22(15) . . ? Ga3 Rh6 Rh5 55.520(15) . . ? Ga1 Rh6 Rh5 116.34(2) . . ? Rh4 Rh6 Rh5 60.035(14) . . ? Rh3 Rh6 Rh5 59.715(14) . . ? Rh1 Rh6 Rh5 89.094(16) . . ? C14 Ga1 C15 35.65(18) . . ? C14 Ga1 C18 36.01(19) . . ? C15 Ga1 C18 59.60(18) . . ? C14 Ga1 C17 59.61(19) . . ? C15 Ga1 C17 59.28(19) . . ? C18 Ga1 C17 35.8(2) . . ? C14 Ga1 C16 58.89(18) . . ? C15 Ga1 C16 35.02(18) . . ? C18 Ga1 C16 59.22(18) . . ? C17 Ga1 C16 35.58(18) . . ? C14 Ga1 Rh4 116.72(13) . . ? C15 Ga1 Rh4 145.51(14) . . ? C18 Ga1 Rh4 112.47(14) . . ? C17 Ga1 Rh4 135.98(14) . . ? C16 Ga1 Rh4 171.21(13) . . ? C14 Ga1 Rh6 123.92(13) . . ? C15 Ga1 Rh6 108.30(13) . . ? C18 Ga1 Rh6 158.85(15) . . ? C17 Ga1 Rh6 155.94(15) . . ? C16 Ga1 Rh6 122.22(13) . . ? Rh4 Ga1 Rh6 66.538(17) . . ? C14 Ga1 Rh1 169.03(13) . . ? C15 Ga1 Rh1 145.05(14) . . ? C18 Ga1 Rh1 133.31(15) . . ? C17 Ga1 Rh1 110.20(15) . . ? C16 Ga1 Rh1 115.92(14) . . ? Rh4 Ga1 Rh1 66.899(18) . . ? Rh6 Ga1 Rh1 67.010(18) . . ? C24 Ga2 C25 38.38(19) . . ? C24 Ga2 C28 34.67(19) . . ? C25 Ga2 C28 58.62(18) . . ? C24 Ga2 C26 58.37(18) . . ? C25 Ga2 C26 34.34(17) . . ? C28 Ga2 C26 54.60(17) . . ? C24 Ga2 Rh5 161.47(15) . . ? C25 Ga2 Rh5 123.15(13) . . ? C28 Ga2 Rh5 145.83(13) . . ? C26 Ga2 Rh5 105.69(12) . . ? C24 Ga2 Rh4 120.83(14) . . ? C25 Ga2 Rh4 124.23(13) . . ? C28 Ga2 Rh4 143.69(13) . . ? C26 Ga2 Rh4 150.95(12) . . ? Rh5 Ga2 Rh4 67.672(18) . . ? C24 Ga2 Rh2 130.20(15) . . ? C25 Ga2 Rh2 165.51(14) . . ? C28 Ga2 Rh2 106.93(13) . . ? C26 Ga2 Rh2 138.20(12) . . ? Rh5 Ga2 Rh2 67.576(18) . . ? Rh4 Ga2 Rh2 67.425(17) . . ? C34 Ga3 C35 36.92(17) . . ? C34 Ga3 C36 59.78(15) . . ? C35 Ga3 C36 35.81(17) . . ? C34 Ga3 C38 36.25(17) . . ? C35 Ga3 C38 59.98(16) . . ? C36 Ga3 C38 57.97(16) . . ? C34 Ga3 C37 58.72(16) . . ? C35 Ga3 C37 58.79(16) . . ? C36 Ga3 C37 34.48(16) . . ? C38 Ga3 C37 33.92(16) . . ? C34 Ga3 Rh5 152.94(13) . . ? C35 Ga3 Rh5 154.47(13) . . ? C36 Ga3 Rh5 119.34(11) . . ? C38 Ga3 Rh5 117.75(11) . . ? C37 Ga3 Rh5 104.10(11) . . ? C34 Ga3 Rh6 138.75(13) . . ? C35 Ga3 Rh6 113.63(12) . . ? C36 Ga3 Rh6 117.06(11) . . ? C38 Ga3 Rh6 173.60(11) . . ? C37 Ga3 Rh6 144.04(12) . . ? Rh5 Ga3 Rh6 67.776(16) . . ? C34 Ga3 Rh3 114.18(11) . . ? C35 Ga3 Rh3 138.49(12) . . ? C36 Ga3 Rh3 173.78(11) . . ? C38 Ga3 Rh3 118.48(11) . . ? C37 Ga3 Rh3 145.23(12) . . ? Rh5 Ga3 Rh3 66.626(17) . . ? Rh6 Ga3 Rh3 66.048(17) . . ? O1 C1 Rh3 132.1(3) . . ? O1 C1 Rh2 133.0(4) . . ? Rh3 C1 Rh2 80.30(16) . . ? O1 C1 Rh1 131.8(4) . . ? Rh3 C1 Rh1 79.61(15) . . ? Rh2 C1 Rh1 78.99(14) . . ? O2 C2 Rh1 177.7(5) . . ? O3 C3 Rh1 177.5(5) . . ? O4 C4 Rh2 179.8(6) . . ? O5 C5 Rh2 179.7(5) . . ? O6 C6 Rh3 177.5(5) . . ? O7 C7 Rh3 177.7(5) . . ? O8 C8 Rh4 176.8(4) . . ? O9 C9 Rh4 177.6(4) . . ? O10 C10 Rh5 178.3(5) . . ? O11 C11 Rh5 178.9(5) . . ? O12 C12 Rh6 177.1(5) . . ? O13 C13 Rh6 178.8(5) . . ? C15 C14 C18 109.0(5) . . ? C15 C14 C19 125.7(5) . . ? C18 C14 C19 125.0(5) . . ? C15 C14 Ga1 73.6(3) . . ? C18 C14 Ga1 73.6(3) . . ? C19 C14 Ga1 124.3(3) . . ? C16 C15 C14 108.0(5) . . ? C16 C15 C20 125.4(5) . . ? C14 C15 C20 126.4(5) . . ? C16 C15 Ga1 73.6(3) . . ? C14 C15 Ga1 70.8(3) . . ? C20 C15 Ga1 125.1(4) . . ? C15 C16 C17 108.7(5) . . ? C15 C16 C21 126.9(5) . . ? C17 C16 C21 124.2(5) . . ? C15 C16 Ga1 71.4(3) . . ? C17 C16 Ga1 72.1(3) . . ? C21 C16 Ga1 126.1(3) . . ? C16 C17 C18 107.1(5) . . ? C16 C17 C22 125.6(5) . . ? C18 C17 C22 127.0(5) . . ? C16 C17 Ga1 72.3(3) . . ? C18 C17 Ga1 71.3(3) . . ? C22 C17 Ga1 125.8(4) . . ? C14 C18 C17 107.1(5) . . ? C14 C18 C23 127.2(5) . . ? C17 C18 C23 125.7(5) . . ? C14 C18 Ga1 70.4(3) . . ? C17 C18 Ga1 72.8(3) . . ? C23 C18 Ga1 124.5(4) . . ? C28 C24 C25 107.3(5) . . ? C28 C24 C29 126.5(5) . . ? C25 C24 C29 125.4(5) . . ? C28 C24 Ga2 83.5(3) . . ? C25 C24 Ga2 72.2(3) . . ? C29 C24 Ga2 118.4(4) . . ? C26 C25 C24 106.7(5) . . ? C26 C25 C30 126.4(5) . . ? C24 C25 C30 126.3(5) . . ? C26 C25 Ga2 83.7(3) . . ? C24 C25 Ga2 69.4(3) . . ? C30 C25 Ga2 119.3(3) . . ? C27 C26 C25 108.8(5) . . ? C27 C26 C31 125.7(5) . . ? C25 C26 C31 125.4(5) . . ? C27 C26 Ga2 80.0(3) . . ? C25 C26 Ga2 62.0(3) . . ? C31 C26 Ga2 125.9(3) . . ? C26 C27 C28 108.2(5) . . ? C26 C27 C32 125.8(5) . . ? C28 C27 C32 126.0(5) . . ? C27 C28 C24 109.0(5) . . ? C27 C28 C33 125.0(5) . . ? C24 C28 C33 125.9(5) . . ? C27 C28 Ga2 81.6(3) . . ? C24 C28 Ga2 61.9(3) . . ? C33 C28 Ga2 124.7(4) . . ? C35 C34 C38 107.7(4) . . ? C35 C34 C39 127.0(4) . . ? C38 C34 C39 125.0(4) . . ? C35 C34 Ga3 71.8(3) . . ? C38 C34 Ga3 76.7(3) . . ? C39 C34 Ga3 122.1(3) . . ? C34 C35 C36 107.8(4) . . ? C34 C35 C40 126.8(4) . . ? C36 C35 C40 125.1(4) . . ? C34 C35 Ga3 71.3(3) . . ? C36 C35 Ga3 76.6(3) . . ? C40 C35 Ga3 122.7(3) . . ? C35 C36 C37 108.3(4) . . ? C35 C36 C41 125.3(4) . . ? C37 C36 C41 126.1(4) . . ? C35 C36 Ga3 67.6(3) . . ? C37 C36 Ga3 76.0(3) . . ? C41 C36 Ga3 126.0(3) . . ? C38 C37 C36 107.9(4) . . ? C38 C37 C42 126.0(5) . . ? C36 C37 C42 126.1(4) . . ? C38 C37 Ga3 69.9(3) . . ? C36 C37 Ga3 69.5(3) . . ? C42 C37 Ga3 126.8(3) . . ? C37 C38 C34 108.2(4) . . ? C37 C38 C43 126.0(5) . . ? C34 C38 C43 125.5(4) . . ? C37 C38 Ga3 76.1(3) . . ? C34 C38 Ga3 67.0(2) . . ? C43 C38 Ga3 127.0(3) . . ? Cl2 C44 Cl1 111.8(3) . . ? Cl4 C45 Cl3 111.5(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.713 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.121 #===END