# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1218 data_global # Synthesis of the Homoleptic Rhodium(III) Complex [Rh(C6Cl5)3]. # Molecular # Structures of [Rh(C6Cl5)3] and [Rh(C6Cl4-C6Cl4)(C6Cl5)(SC4H8)2]. # # by Maria P. Garcia, M. Victoria Jimenez, Fernando J. Lahoz, Jose A. # Lopez and Luis A. Oro. # # to be submitted to Dalton Transactions. # #---------------------------------------------------------------------- # # Person for contact _publ_contact_author ; Dr. Fernando J. Lahoz Departamento de Qu\'imica Inorg\'anica - I.C.M.A. Facultad de Ciencias Universidad de Zaragoza - C.S.I.C. 50009 Zaragoza, Spain ; _publ_contact_author_email lahoz@posta.unizar.es #---------------------------------------------------------------------- #Publication details loop_ _publ_author_name 'Garc\'ia, M.P.' 'Jim\'enez, M.V.' 'Lahoz, F.J.' 'L\'opez, J.A.' 'Oro, L.A.' _journal_name_full 'Dalton Transactions' _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? #---------------------------------------------------------------------- # Data for compound 1 data_compound1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(pentachlorophenyl)-rhodium(III) dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C18 Cl15 Rh), 0.5(C H2 Cl2)' _chemical_formula_sum 'C18.50 H Cl16 Rh' _chemical_formula_weight 893.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.8207(11) _cell_length_b 10.8539(15) _cell_length_c 14.0152(15) _cell_angle_alpha 108.608(5) _cell_angle_beta 102.214(4) _cell_angle_gamma 106.976(6) _cell_volume 1405.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 58 _cell_measurement_theta_min 10 _cell_measurement_theta_max 20 _exptl_crystal_description 'prismatic block' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 858 _exptl_absorpt_coefficient_mu 2.142 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.8146 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; Azimuthal psi-scans of 7 reflections at 10\% intervals. Data corrected with the program: XPREP, SHELXTL v. 5 (Siemens) ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal focus Mo sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Siemens-Stoe AED2' _diffrn_measurement_method '\w-2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 55 _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 4173 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 23.02 _reflns_number_total 3925 _reflns_number_gt 3261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIF4 (Stoe)' _computing_cell_refinement 'DIF4 (Stoe)' _computing_data_reduction 'REDU4 (Stoe)' _computing_structure_solution 'SIR92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v.5 (Siemens)' _computing_publication_material 'CIFTAB (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. A disordered solvent was found close to an inversion centre. A molecule of dichloromethane per unit cell was introduced as two superimposed models, with refined occupancy factors but restrained to sum 1/2. The geometry in each model was restrained, refining in the full-matrix procedure one isotropic displacement factor for the chlorine atoms and a second one for the carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+3.6004P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3925 _refine_ls_number_parameters 329 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1306 _refine_ls_wR_factor_gt 0.1215 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.743 _refine_diff_density_min -0.992 _refine_diff_density_rms 0.135 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.02 _diffrn_measured_fraction_theta_full 1.000 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 Rh Rh 0.22619(5) 0.07425(5) 0.20962(4) 0.02667(19) Uani 1 1 d . . . Cl2 Cl 0.16479(18) 0.13324(18) 0.04302(12) 0.0354(4) Uani 1 1 d . . . Cl3 Cl 0.0864(3) 0.3850(2) 0.01718(15) 0.0661(7) Uani 1 1 d . . . Cl4 Cl 0.0914(3) 0.6188(2) 0.22064(17) 0.0608(6) Uani 1 1 d . . . Cl5 Cl 0.14123(19) 0.58325(19) 0.43518(14) 0.0429(5) Uani 1 1 d . . . Cl6 Cl 0.2187(2) 0.3396(2) 0.45573(14) 0.0545(6) Uani 1 1 d . . . Cl8 Cl 0.30340(18) -0.12925(18) 0.13115(14) 0.0385(4) Uani 1 1 d . . . Cl9 Cl 0.5783(2) -0.1268(2) 0.08259(17) 0.0572(6) Uani 1 1 d . . . Cl10 Cl 0.8188(2) 0.1652(2) 0.15576(18) 0.0583(6) Uani 1 1 d . . . Cl11 Cl 0.7792(2) 0.4412(2) 0.2657(2) 0.0647(6) Uani 1 1 d . . . Cl12 Cl 0.5059(2) 0.4321(2) 0.30594(18) 0.0551(5) Uani 1 1 d . . . Cl14 Cl -0.00204(17) -0.07871(18) 0.21947(13) 0.0367(4) Uani 1 1 d . . . Cl15 Cl -0.0615(2) -0.1965(2) 0.39282(16) 0.0478(5) Uani 1 1 d . . . Cl16 Cl 0.1795(3) -0.0888(2) 0.60836(16) 0.0585(6) Uani 1 1 d . . . Cl17 Cl 0.4669(3) 0.1275(3) 0.64421(16) 0.0656(6) Uani 1 1 d . . . Cl18 Cl 0.5190(2) 0.2245(2) 0.46689(16) 0.0555(5) Uani 1 1 d . . . C1 C 0.1906(6) 0.2501(7) 0.2451(5) 0.0280(14) Uani 1 1 d . . . C2 C 0.1595(6) 0.2673(6) 0.1517(5) 0.0279(15) Uani 1 1 d . . . C3 C 0.1259(7) 0.3755(7) 0.1385(5) 0.0366(17) Uani 1 1 d . . . C4 C 0.1267(7) 0.4767(7) 0.2301(5) 0.0356(16) Uani 1 1 d . . . C5 C 0.1518(7) 0.4619(7) 0.3255(5) 0.0303(15) Uani 1 1 d . . . C6 C 0.1859(6) 0.3507(7) 0.3335(5) 0.0285(15) Uani 1 1 d . . . C7 C 0.4202(7) 0.1477(7) 0.2148(5) 0.0318(15) Uani 1 1 d . . . C8 C 0.4433(7) 0.0292(7) 0.1671(5) 0.0318(15) Uani 1 1 d . . . C9 C 0.5616(7) 0.0275(7) 0.1449(5) 0.0342(16) Uani 1 1 d . . . C10 C 0.6654(7) 0.1568(8) 0.1767(5) 0.0381(17) Uani 1 1 d . . . C11 C 0.6468(7) 0.2817(8) 0.2264(5) 0.0385(17) Uani 1 1 d . . . C12 C 0.5234(7) 0.2763(7) 0.2445(5) 0.0341(16) Uani 1 1 d . . . C13 C 0.2515(7) 0.0546(7) 0.3484(5) 0.0290(15) Uani 1 1 d . . . C14 C 0.1275(7) -0.0314(7) 0.3402(5) 0.0296(15) Uani 1 1 d . . . C15 C 0.1002(7) -0.0810(7) 0.4151(5) 0.0343(16) Uani 1 1 d . . . C16 C 0.2078(8) -0.0339(7) 0.5094(5) 0.0392(18) Uani 1 1 d . . . C17 C 0.3348(8) 0.0599(8) 0.5236(5) 0.0388(18) Uani 1 1 d . . . C18 C 0.3596(8) 0.1053(8) 0.4432(5) 0.0395(17) Uani 1 1 d . . . C50 C 0.618(3) 0.524(10) 0.052(3) 0.108(16) Uiso 0.277(5) 1 d PD . 1 Cl50 Cl 0.468(3) 0.485(4) 0.082(3) 0.169(5) Uiso 0.277(5) 1 d PD . 1 Cl51 Cl 0.576(3) 0.506(3) -0.078(2) 0.169(5) Uiso 0.277(5) 1 d PD . 1 C51 C 0.498(5) 0.496(9) 0.071(4) 0.108(16) Uiso 0.224(5) 1 d PD . 2 Cl52 Cl 0.661(2) 0.623(3) 0.1309(18) 0.169(5) Uiso 0.224(5) 1 d PD . 2 Cl53 Cl 0.414(3) 0.482(5) -0.0525(19) 0.169(5) Uiso 0.224(5) 1 d PD . 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 Rh 0.0305(3) 0.0280(3) 0.0251(3) 0.0107(2) 0.0096(2) 0.0162(2) Cl2 0.0495(10) 0.0387(10) 0.0254(8) 0.0115(7) 0.0137(7) 0.0278(8) Cl3 0.123(2) 0.0723(15) 0.0392(11) 0.0346(11) 0.0314(12) 0.0711(15) Cl4 0.1075(18) 0.0479(12) 0.0616(13) 0.0327(10) 0.0414(13) 0.0562(13) Cl5 0.0522(11) 0.0365(10) 0.0379(10) 0.0048(8) 0.0179(8) 0.0241(9) Cl6 0.0961(16) 0.0633(13) 0.0285(9) 0.0231(9) 0.0282(10) 0.0538(13) Cl8 0.0432(10) 0.0315(9) 0.0475(10) 0.0166(8) 0.0191(8) 0.0202(8) Cl9 0.0679(14) 0.0555(13) 0.0674(13) 0.0219(11) 0.0370(11) 0.0430(11) Cl10 0.0408(11) 0.0792(15) 0.0670(14) 0.0307(12) 0.0307(10) 0.0297(11) Cl11 0.0407(11) 0.0534(13) 0.0827(16) 0.0167(12) 0.0236(11) 0.0050(10) Cl12 0.0467(11) 0.0335(10) 0.0723(14) 0.0065(9) 0.0211(10) 0.0143(9) Cl14 0.0356(9) 0.0407(10) 0.0338(9) 0.0150(8) 0.0106(7) 0.0158(8) Cl15 0.0623(13) 0.0396(10) 0.0627(12) 0.0274(9) 0.0402(10) 0.0274(10) Cl16 0.1066(18) 0.0639(14) 0.0434(11) 0.0372(10) 0.0419(11) 0.0562(13) Cl17 0.0792(16) 0.0861(17) 0.0345(11) 0.0263(11) 0.0045(10) 0.0447(14) Cl18 0.0409(11) 0.0700(14) 0.0447(11) 0.0229(10) 0.0032(9) 0.0152(10) C1 0.023(3) 0.038(4) 0.029(3) 0.015(3) 0.011(3) 0.017(3) C2 0.031(4) 0.028(4) 0.025(3) 0.005(3) 0.011(3) 0.016(3) C3 0.048(4) 0.041(4) 0.034(4) 0.020(3) 0.017(3) 0.027(4) C4 0.047(4) 0.028(4) 0.042(4) 0.016(3) 0.016(3) 0.025(3) C5 0.033(4) 0.025(4) 0.033(4) 0.005(3) 0.018(3) 0.015(3) C6 0.032(4) 0.031(4) 0.023(3) 0.009(3) 0.010(3) 0.014(3) C7 0.038(4) 0.040(4) 0.029(3) 0.016(3) 0.017(3) 0.026(3) C8 0.037(4) 0.033(4) 0.029(3) 0.017(3) 0.007(3) 0.017(3) C9 0.041(4) 0.041(4) 0.030(4) 0.016(3) 0.016(3) 0.023(4) C10 0.035(4) 0.052(5) 0.037(4) 0.022(4) 0.014(3) 0.025(4) C11 0.036(4) 0.042(4) 0.034(4) 0.017(3) 0.010(3) 0.011(3) C12 0.035(4) 0.032(4) 0.040(4) 0.015(3) 0.015(3) 0.017(3) C13 0.040(4) 0.025(3) 0.029(3) 0.013(3) 0.012(3) 0.019(3) C14 0.039(4) 0.030(4) 0.028(3) 0.014(3) 0.011(3) 0.022(3) C15 0.053(4) 0.026(4) 0.042(4) 0.014(3) 0.028(4) 0.029(3) C16 0.073(6) 0.040(4) 0.031(4) 0.021(3) 0.028(4) 0.042(4) C17 0.054(5) 0.052(5) 0.030(4) 0.022(3) 0.014(3) 0.041(4) C18 0.047(4) 0.041(4) 0.037(4) 0.016(3) 0.011(3) 0.029(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 Rh C1 1.986(6) . ? Rh C7 1.993(7) . ? Rh C13 1.994(6) . ? Rh Cl8 2.5889(17) . ? Rh Cl14 2.6020(18) . ? Rh Cl2 2.6171(16) . ? Cl2 C2 1.764(6) . ? Cl3 C3 1.707(7) . ? Cl4 C4 1.731(6) . ? Cl5 C5 1.727(6) . ? Cl6 C6 1.725(6) . ? Cl8 C8 1.763(7) . ? Cl9 C9 1.706(7) . ? Cl10 C10 1.727(7) . ? Cl11 C11 1.721(7) . ? Cl12 C12 1.721(7) . ? Cl14 C14 1.764(6) . ? Cl15 C15 1.723(7) . ? Cl16 C16 1.724(7) . ? Cl17 C17 1.735(7) . ? Cl18 C18 1.714(8) . ? C1 C2 1.366(9) . ? C1 C6 1.388(9) . ? C2 C3 1.380(9) . ? C3 C4 1.394(9) . ? C4 C5 1.377(9) . ? C5 C6 1.390(9) . ? C7 C8 1.368(9) . ? C7 C12 1.374(10) . ? C8 C9 1.384(10) . ? C9 C10 1.379(10) . ? C10 C11 1.407(10) . ? C11 C12 1.399(10) . ? C13 C14 1.349(9) . ? C13 C18 1.392(9) . ? C14 C15 1.370(9) . ? C15 C16 1.391(10) . ? C16 C17 1.380(11) . ? C17 C18 1.411(10) . ? C50 Cl51 1.718(10) . ? C50 Cl50 1.725(10) . ? C50 Cl50 1.87(5) 2_665 ? C50 Cl51 2.16(5) 2_665 ? Cl50 Cl51 0.51(5) 2_665 ? Cl50 C50 1.87(5) 2_665 ? Cl51 Cl50 0.51(5) 2_665 ? Cl51 C50 2.16(5) 2_665 ? C51 Cl53 1.02(7) 2_665 ? C51 Cl52 1.715(10) . ? C51 Cl53 1.717(10) . ? Cl52 Cl53 1.20(4) 2_665 ? Cl53 C51 1.02(7) 2_665 ? Cl53 Cl52 1.20(4) 2_665 ? Cl53 Cl53 1.95(5) 2_665 ? 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 Rh C7 100.4(3) . . ? C1 Rh C13 100.8(2) . . ? C7 Rh C13 100.8(3) . . ? C1 Rh Cl8 164.56(19) . . ? C7 Rh Cl8 68.64(19) . . ? C13 Rh Cl8 92.17(18) . . ? C1 Rh Cl14 95.66(18) . . ? C7 Rh Cl14 161.84(19) . . ? C13 Rh Cl14 67.6(2) . . ? Cl8 Rh Cl14 96.99(6) . . ? C1 Rh Cl2 67.84(18) . . ? C7 Rh Cl2 86.31(18) . . ? C13 Rh Cl2 167.73(18) . . ? Cl8 Rh Cl2 99.76(5) . . ? Cl14 Rh Cl2 107.70(6) . . ? C2 Cl2 Rh 73.2(2) . . ? C8 Cl8 Rh 73.3(2) . . ? C14 Cl14 Rh 73.4(2) . . ? C2 C1 C6 116.1(6) . . ? C2 C1 Rh 105.8(4) . . ? C6 C1 Rh 138.0(5) . . ? C1 C2 C3 126.0(6) . . ? C1 C2 Cl2 113.1(5) . . ? C3 C2 Cl2 120.9(5) . . ? C2 C3 C4 116.1(6) . . ? C2 C3 Cl3 121.9(5) . . ? C4 C3 Cl3 122.1(5) . . ? C5 C4 C3 120.6(6) . . ? C5 C4 Cl4 120.7(5) . . ? C3 C4 Cl4 118.7(5) . . ? C4 C5 C6 120.4(6) . . ? C4 C5 Cl5 119.3(5) . . ? C6 C5 Cl5 120.4(5) . . ? C1 C6 C5 120.8(6) . . ? C1 C6 Cl6 121.0(5) . . ? C5 C6 Cl6 118.1(5) . . ? C8 C7 C12 117.7(6) . . ? C8 C7 Rh 104.3(5) . . ? C12 C7 Rh 137.9(5) . . ? C7 C8 C9 125.5(7) . . ? C7 C8 Cl8 113.7(5) . . ? C9 C8 Cl8 120.8(5) . . ? C10 C9 C8 116.5(6) . . ? C10 C9 Cl9 121.9(5) . . ? C8 C9 Cl9 121.7(6) . . ? C9 C10 C11 120.1(6) . . ? C9 C10 Cl10 119.8(5) . . ? C11 C10 Cl10 120.1(6) . . ? C12 C11 C10 120.6(7) . . ? C12 C11 Cl11 120.6(6) . . ? C10 C11 Cl11 118.7(6) . . ? C7 C12 C11 119.6(6) . . ? C7 C12 Cl12 121.6(5) . . ? C11 C12 Cl12 118.8(5) . . ? C14 C13 C18 118.0(6) . . ? C14 C13 Rh 105.7(4) . . ? C18 C13 Rh 136.3(5) . . ? C13 C14 C15 125.4(6) . . ? C13 C14 Cl14 113.1(5) . . ? C15 C14 Cl14 121.5(5) . . ? C14 C15 C16 117.4(7) . . ? C14 C15 Cl15 121.0(5) . . ? C16 C15 Cl15 121.6(5) . . ? C17 C16 C15 119.2(6) . . ? C17 C16 Cl16 121.0(5) . . ? C15 C16 Cl16 119.8(6) . . ? C16 C17 C18 121.6(6) . . ? C16 C17 Cl17 119.6(5) . . ? C18 C17 Cl17 118.8(6) . . ? C13 C18 C17 118.3(7) . . ? C13 C18 Cl18 122.4(6) . . ? C17 C18 Cl18 119.3(5) . . ? Cl51 C50 Cl50 107.8(11) . . ? Cl51 C50 Cl50 15.8(19) . 2_665 ? Cl50 C50 Cl50 93(2) . 2_665 ? Cl51 C50 Cl51 102.0(17) . 2_665 ? Cl50 C50 Cl51 8.2(17) . 2_665 ? Cl50 C50 Cl51 87(2) 2_665 2_665 ? Cl51 Cl50 C50 143(7) 2_665 . ? Cl51 Cl50 C50 65(6) 2_665 2_665 ? C50 Cl50 C50 87(2) . 2_665 ? Cl50 Cl51 C50 99(7) 2_665 . ? Cl50 Cl51 C50 29(6) 2_665 2_665 ? C50 Cl51 C50 78.0(17) . 2_665 ? Cl53 C51 Cl52 44(3) 2_665 . ? Cl53 C51 Cl53 87(4) 2_665 . ? Cl52 C51 Cl53 113.9(14) . . ? Cl53 Cl52 C51 36(3) 2_665 . ? C51 Cl53 Cl52 101(5) 2_665 2_665 ? C51 Cl53 C51 93(4) 2_665 . ? Cl52 Cl53 C51 129(4) 2_665 . ? C51 Cl53 Cl53 62(2) 2_665 2_665 ? Cl52 Cl53 Cl53 130(5) 2_665 2_665 ? C51 Cl53 Cl53 32(2) . 2_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Rh Cl2 C2 -0.3(3) . . . . ? C7 Rh Cl2 C2 -103.1(3) . . . . ? C13 Rh Cl2 C2 23.0(10) . . . . ? Cl8 Rh Cl2 C2 -170.7(2) . . . . ? Cl14 Rh Cl2 C2 88.7(2) . . . . ? C1 Rh Cl8 C8 44.7(7) . . . . ? C7 Rh Cl8 C8 -1.9(3) . . . . ? C13 Rh Cl8 C8 -102.7(3) . . . . ? Cl14 Rh Cl8 C8 -170.4(2) . . . . ? Cl2 Rh Cl8 C8 80.2(2) . . . . ? C1 Rh Cl14 C14 -101.4(3) . . . . ? C7 Rh Cl14 C14 50.9(6) . . . . ? C13 Rh Cl14 C14 -2.0(3) . . . . ? Cl8 Rh Cl14 C14 87.4(2) . . . . ? Cl2 Rh Cl14 C14 -169.9(2) . . . . ? C7 Rh C1 C2 82.0(5) . . . . ? C13 Rh C1 C2 -174.8(4) . . . . ? Cl8 Rh C1 C2 38.5(10) . . . . ? Cl14 Rh C1 C2 -106.5(4) . . . . ? Cl2 Rh C1 C2 0.3(4) . . . . ? C7 Rh C1 C6 -100.2(7) . . . . ? C13 Rh C1 C6 3.1(8) . . . . ? Cl8 Rh C1 C6 -143.7(6) . . . . ? Cl14 Rh C1 C6 71.3(7) . . . . ? Cl2 Rh C1 C6 178.2(8) . . . . ? C6 C1 C2 C3 0.9(10) . . . . ? Rh C1 C2 C3 179.2(6) . . . . ? C6 C1 C2 Cl2 -178.9(5) . . . . ? Rh C1 C2 Cl2 -0.5(6) . . . . ? Rh Cl2 C2 C1 0.4(4) . . . . ? Rh Cl2 C2 C3 -179.4(6) . . . . ? C1 C2 C3 C4 1.1(11) . . . . ? Cl2 C2 C3 C4 -179.2(5) . . . . ? C1 C2 C3 Cl3 -179.1(5) . . . . ? Cl2 C2 C3 Cl3 0.6(9) . . . . ? C2 C3 C4 C5 -3.7(11) . . . . ? Cl3 C3 C4 C5 176.5(5) . . . . ? C2 C3 C4 Cl4 177.8(5) . . . . ? Cl3 C3 C4 Cl4 -2.0(9) . . . . ? C3 C4 C5 C6 4.3(11) . . . . ? Cl4 C4 C5 C6 -177.2(5) . . . . ? C3 C4 C5 Cl5 -176.0(6) . . . . ? Cl4 C4 C5 Cl5 2.5(8) . . . . ? C2 C1 C6 C5 -0.3(9) . . . . ? Rh C1 C6 C5 -178.0(5) . . . . ? C2 C1 C6 Cl6 178.4(5) . . . . ? Rh C1 C6 Cl6 0.7(10) . . . . ? C4 C5 C6 C1 -2.3(10) . . . . ? Cl5 C5 C6 C1 178.0(5) . . . . ? C4 C5 C6 Cl6 179.0(5) . . . . ? Cl5 C5 C6 Cl6 -0.7(8) . . . . ? C1 Rh C7 C8 -166.2(4) . . . . ? C13 Rh C7 C8 90.5(4) . . . . ? Cl8 Rh C7 C8 2.4(4) . . . . ? Cl14 Rh C7 C8 41.8(9) . . . . ? Cl2 Rh C7 C8 -99.6(4) . . . . ? C1 Rh C7 C12 8.1(8) . . . . ? C13 Rh C7 C12 -95.2(7) . . . . ? Cl8 Rh C7 C12 176.7(8) . . . . ? Cl14 Rh C7 C12 -143.9(6) . . . . ? Cl2 Rh C7 C12 74.7(7) . . . . ? C12 C7 C8 C9 -0.9(10) . . . . ? Rh C7 C8 C9 174.8(5) . . . . ? C12 C7 C8 Cl8 -179.3(5) . . . . ? Rh C7 C8 Cl8 -3.6(5) . . . . ? Rh Cl8 C8 C7 2.8(4) . . . . ? Rh Cl8 C8 C9 -175.7(6) . . . . ? C7 C8 C9 C10 2.0(10) . . . . ? Cl8 C8 C9 C10 -179.7(5) . . . . ? C7 C8 C9 Cl9 -178.7(5) . . . . ? Cl8 C8 C9 Cl9 -0.4(8) . . . . ? C8 C9 C10 C11 -1.7(10) . . . . ? Cl9 C9 C10 C11 179.0(5) . . . . ? C8 C9 C10 Cl10 178.2(5) . . . . ? Cl9 C9 C10 Cl10 -1.1(8) . . . . ? C9 C10 C11 C12 0.3(10) . . . . ? Cl10 C10 C11 C12 -179.5(5) . . . . ? C9 C10 C11 Cl11 179.6(5) . . . . ? Cl10 C10 C11 Cl11 -0.2(8) . . . . ? C8 C7 C12 C11 -0.6(10) . . . . ? Rh C7 C12 C11 -174.4(5) . . . . ? C8 C7 C12 Cl12 -179.5(5) . . . . ? Rh C7 C12 Cl12 6.7(10) . . . . ? C10 C11 C12 C7 0.9(10) . . . . ? Cl11 C11 C12 C7 -178.4(5) . . . . ? C10 C11 C12 Cl12 179.8(5) . . . . ? Cl11 C11 C12 Cl12 0.5(8) . . . . ? C1 Rh C13 C14 94.4(5) . . . . ? C7 Rh C13 C14 -162.7(4) . . . . ? Cl8 Rh C13 C14 -94.0(4) . . . . ? Cl14 Rh C13 C14 2.7(4) . . . . ? Cl2 Rh C13 C14 72.6(11) . . . . ? C1 Rh C13 C18 -85.9(7) . . . . ? C7 Rh C13 C18 17.0(7) . . . . ? Cl8 Rh C13 C18 85.7(7) . . . . ? Cl14 Rh C13 C18 -177.7(7) . . . . ? Cl2 Rh C13 C18 -107.8(10) . . . . ? C18 C13 C14 C15 -4.4(10) . . . . ? Rh C13 C14 C15 175.3(5) . . . . ? C18 C13 C14 Cl14 176.3(5) . . . . ? Rh C13 C14 Cl14 -4.0(5) . . . . ? Rh Cl14 C14 C13 3.0(4) . . . . ? Rh Cl14 C14 C15 -176.2(6) . . . . ? C13 C14 C15 C16 3.1(10) . . . . ? Cl14 C14 C15 C16 -177.7(5) . . . . ? C13 C14 C15 Cl15 -177.2(5) . . . . ? Cl14 C14 C15 Cl15 1.9(8) . . . . ? C14 C15 C16 C17 0.4(9) . . . . ? Cl15 C15 C16 C17 -179.3(5) . . . . ? C14 C15 C16 Cl16 178.4(5) . . . . ? Cl15 C15 C16 Cl16 -1.2(7) . . . . ? C15 C16 C17 C18 -2.3(10) . . . . ? Cl16 C16 C17 C18 179.7(5) . . . . ? C15 C16 C17 Cl17 176.1(5) . . . . ? Cl16 C16 C17 Cl17 -1.9(8) . . . . ? C14 C13 C18 C17 2.3(9) . . . . ? Rh C13 C18 C17 -177.4(5) . . . . ? C14 C13 C18 Cl18 -175.5(5) . . . . ? Rh C13 C18 Cl18 4.9(10) . . . . ? C16 C17 C18 C13 0.9(10) . . . . ? Cl17 C17 C18 C13 -177.5(5) . . . . ? C16 C17 C18 Cl18 178.8(5) . . . . ? Cl17 C17 C18 Cl18 0.3(8) . . . . ? Cl51 C50 Cl50 Cl51 -46(16) . . . 2_665 ? Cl50 C50 Cl50 Cl51 -39(14) 2_665 . . 2_665 ? Cl51 C50 Cl50 C50 -7(3) . . . 2_665 ? Cl50 C50 Cl50 C50 0.000(3) 2_665 . . 2_665 ? Cl51 C50 Cl50 C50 39(14) 2_665 . . 2_665 ? Cl50 C50 Cl51 Cl50 26(10) . . . 2_665 ? Cl51 C50 Cl51 Cl50 20(8) 2_665 . . 2_665 ? Cl50 C50 Cl51 C50 6(3) . . . 2_665 ? Cl50 C50 Cl51 C50 -20(8) 2_665 . . 2_665 ? Cl51 C50 Cl51 C50 0.000(3) 2_665 . . 2_665 ? Cl53 C51 Cl52 Cl53 -57(6) . . . 2_665 ? Cl53 C51 Cl53 C51 0.000(5) 2_665 . . 2_665 ? Cl52 C51 Cl53 C51 35(4) . . . 2_665 ? Cl53 C51 Cl53 Cl52 106(6) 2_665 . . 2_665 ? Cl52 C51 Cl53 Cl52 141(4) . . . 2_665 ? Cl52 C51 Cl53 Cl53 35(4) . . . 2_665 ? #=END #---------------------------------------------------------------------- # Data for compound 2 data_compound2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (octachloro-2,2'-biphenylene)-(pentachlorophenyl)- bis(tetrahidrothiophene)-rhodium(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H16 Cl13 Rh S2' _chemical_formula_sum 'C26 H16 Cl13 Rh S2' _chemical_formula_weight 956.27 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 9.2192(5) _cell_length_b 32.660(2) _cell_length_c 11.3747(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.805(6) _cell_angle_gamma 90.00 _cell_volume 3295.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 58 _cell_measurement_theta_min 10 _cell_measurement_theta_max 18 _exptl_crystal_description 'prismatic block' _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.927 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 1.721 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.5147 _exptl_absorpt_correction_T_max 0.5625 _exptl_absorpt_process_details ; Azimuthal psi-scans of 12 reflections at 10\% intervals. Data corrected with the program: XPREP, SHELXTL v. 5 (Siemens) ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal focus Mo sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Siemens-Stoe AED2' _diffrn_measurement_method '\w-2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 55 _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 6264 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5795 _reflns_number_gt 4613 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIF4 (Stoe)' _computing_cell_refinement 'DIF4 (Stoe)' _computing_data_reduction 'REDU4 (Stoe)' _computing_structure_solution 'SIR92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v.5 (Siemens)' _computing_publication_material 'CIFTAB (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. One tetrahydrothiophene ligand presents a two-fold disorder affecting two carbons. This group was refined with anisotropic displacement parameters but with some restrictions in the geometry; the refined occupancy factors were constrained to sum the unity. The hidrogens of this ligand were not introduced in the refinement. The hydrogens of the non-disordered tetrahydrothiophene group were introduced geometrically and refined riding on the corresponding carbon atoms, with a common, but refined, isotropic displacement parameter. ; _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^)+(0.0334P)^2^+4.3269P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5795 _refine_ls_number_parameters 399 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0913 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.452 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.077 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 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 Rh Rh 0.40573(3) 0.116604(10) 0.79082(3) 0.03277(10) Uani 1 1 d . . . S1 S 0.30268(14) 0.18084(4) 0.83927(11) 0.0495(3) Uani 1 1 d D A . S2 S 0.34040(12) 0.09368(4) 0.97978(10) 0.0427(3) Uani 1 1 d . . . C1 C 0.4459(5) 0.05995(14) 0.7297(4) 0.0433(10) Uani 1 1 d . . . C2 C 0.3115(6) 0.03822(14) 0.6930(4) 0.0498(12) Uani 1 1 d . . . C3 C 0.2994(8) -0.00224(17) 0.6553(4) 0.0668(16) Uani 1 1 d . . . C4 C 0.4284(9) -0.02179(16) 0.6446(5) 0.0742(19) Uani 1 1 d . . . C5 C 0.5627(8) -0.00083(17) 0.6719(4) 0.0660(16) Uani 1 1 d . . . C6 C 0.5709(6) 0.03929(15) 0.7156(4) 0.0502(12) Uani 1 1 d . . . Cl2 Cl 0.14832(15) 0.06529(5) 0.69433(12) 0.0637(4) Uani 1 1 d . . . Cl3 Cl 0.1291(2) -0.02735(6) 0.62230(17) 0.1101(7) Uani 1 1 d . . . Cl4 Cl 0.4171(3) -0.07140(5) 0.59481(18) 0.1305(9) Uani 1 1 d . . . Cl5 Cl 0.7213(2) -0.02500(6) 0.65149(15) 0.1035(7) Uani 1 1 d . . . Cl6 Cl 0.74738(16) 0.06259(5) 0.75005(14) 0.0682(4) Uani 1 1 d . . . C7 C 0.6185(5) 0.13237(13) 0.8696(4) 0.0356(9) Uani 1 1 d . . . C8 C 0.7057(5) 0.12361(14) 0.9879(4) 0.0436(11) Uani 1 1 d . . . C9 C 0.8271(5) 0.14863(16) 1.0447(4) 0.0459(11) Uani 1 1 d . . . C10 C 0.8669(5) 0.18099(15) 0.9819(4) 0.0466(11) Uani 1 1 d . . . C11 C 0.7955(5) 0.18610(14) 0.8584(4) 0.0436(10) Uani 1 1 d . . . C12 C 0.6806(4) 0.15920(13) 0.7992(4) 0.0357(9) Uani 1 1 d . . . C13 C 0.6018(4) 0.15740(12) 0.6680(4) 0.0342(9) Uani 1 1 d . . . C14 C 0.6649(5) 0.16446(13) 0.5705(4) 0.0394(10) Uani 1 1 d . . . C15 C 0.5717(5) 0.16611(13) 0.4519(4) 0.0403(10) Uani 1 1 d . . . C16 C 0.4187(5) 0.15889(13) 0.4307(4) 0.0379(10) Uani 1 1 d . . . C17 C 0.3626(5) 0.14590(13) 0.5261(4) 0.0388(10) Uani 1 1 d . . . C18 C 0.4546(5) 0.14240(12) 0.6448(3) 0.0340(9) Uani 1 1 d . . . Cl8 Cl 0.67612(14) 0.08005(5) 1.06449(11) 0.0633(4) Uani 1 1 d . . . Cl9 Cl 0.92624(14) 0.13963(5) 1.19428(11) 0.0690(4) Uani 1 1 d . . . Cl10 Cl 1.00459(15) 0.21530(5) 1.05672(13) 0.0695(4) Uani 1 1 d . . . Cl11 Cl 0.83457(16) 0.22954(4) 0.78581(13) 0.0669(4) Uani 1 1 d . . . Cl14 Cl 0.85817(14) 0.16353(4) 0.59246(12) 0.0609(3) Uani 1 1 d . . . Cl15 Cl 0.64431(17) 0.17579(5) 0.33029(11) 0.0706(4) Uani 1 1 d . . . Cl16 Cl 0.30101(15) 0.16259(5) 0.28468(10) 0.0622(4) Uani 1 1 d . . . Cl17 Cl 0.17251(13) 0.13429(5) 0.49501(11) 0.0708(4) Uani 1 1 d . . . C19 C 0.3902(7) 0.19547(18) 0.9990(5) 0.0681(15) Uani 1 1 d D . . C20A C 0.504(2) 0.2290(5) 0.9971(11) 0.078(7) Uani 0.53(3) 1 d PD A 1 C21A C 0.457(4) 0.2538(7) 0.8812(12) 0.092(13) Uani 0.53(3) 1 d PD A 1 C20B C 0.410(3) 0.2404(3) 0.9949(11) 0.069(6) Uani 0.47(3) 1 d PD A 2 C21B C 0.472(4) 0.2493(8) 0.8867(14) 0.085(13) Uani 0.47(3) 1 d PD A 2 C22 C 0.3720(8) 0.22691(17) 0.7764(5) 0.082(2) Uani 1 1 d D . . C23 C 0.3299(6) 0.03838(15) 1.0030(5) 0.0557(13) Uani 1 1 d . . . H23A H 0.3615 0.0236 0.9402 0.072(6) Uiso 1 1 calc R . . H23B H 0.3951 0.0306 1.0821 0.072(6) Uiso 1 1 calc R . . C24 C 0.1662(6) 0.02847(16) 0.9960(5) 0.0636(14) Uani 1 1 d . . . H24A H 0.1120 0.0209 0.9132 0.072(6) Uiso 1 1 calc R . . H24B H 0.1612 0.0058 1.0498 0.072(6) Uiso 1 1 calc R . . C25 C 0.0975(6) 0.06654(17) 1.0350(5) 0.0655(15) Uani 1 1 d . . . H25A H -0.0114 0.0640 1.0138 0.072(6) Uiso 1 1 calc R . . H25B H 0.1344 0.0702 1.1227 0.072(6) Uiso 1 1 calc R . . C26 C 0.1413(5) 0.10281(16) 0.9699(5) 0.0539(12) Uani 1 1 d . . . H26A H 0.1286 0.1282 1.0101 0.072(6) Uiso 1 1 calc R . . H26B H 0.0813 0.1039 0.8855 0.072(6) 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 Rh 0.02914(17) 0.04091(19) 0.02905(16) 0.00243(14) 0.00928(12) 0.00198(14) S1 0.0500(7) 0.0545(7) 0.0457(6) -0.0020(5) 0.0158(5) 0.0112(6) S2 0.0388(6) 0.0520(7) 0.0406(6) 0.0081(5) 0.0165(5) 0.0028(5) C1 0.057(3) 0.042(2) 0.032(2) 0.0025(18) 0.014(2) 0.004(2) C2 0.066(3) 0.046(3) 0.035(2) 0.004(2) 0.010(2) -0.006(2) C3 0.106(5) 0.048(3) 0.035(3) 0.003(2) 0.001(3) -0.014(3) C4 0.135(6) 0.043(3) 0.038(3) -0.001(2) 0.012(3) 0.010(4) C5 0.105(5) 0.057(3) 0.037(3) 0.007(2) 0.021(3) 0.032(3) C6 0.066(3) 0.050(3) 0.036(2) 0.006(2) 0.017(2) 0.016(2) Cl2 0.0480(7) 0.0830(10) 0.0564(7) -0.0011(7) 0.0077(6) -0.0096(7) Cl3 0.1337(17) 0.0799(12) 0.0934(13) -0.0017(10) -0.0087(11) -0.0511(12) Cl4 0.241(3) 0.0481(9) 0.0890(13) -0.0186(9) 0.0217(15) 0.0115(13) Cl5 0.1526(18) 0.0964(12) 0.0678(10) 0.0065(9) 0.0406(10) 0.0754(13) Cl6 0.0567(8) 0.0803(10) 0.0738(9) 0.0047(7) 0.0284(7) 0.0234(7) C7 0.032(2) 0.043(2) 0.033(2) 0.0006(18) 0.0107(17) 0.0043(18) C8 0.035(2) 0.061(3) 0.036(2) 0.005(2) 0.0126(19) 0.008(2) C9 0.035(2) 0.069(3) 0.032(2) -0.005(2) 0.0063(19) 0.009(2) C10 0.034(2) 0.058(3) 0.046(3) -0.017(2) 0.008(2) -0.003(2) C11 0.038(2) 0.043(2) 0.050(3) -0.004(2) 0.011(2) -0.001(2) C12 0.030(2) 0.042(2) 0.033(2) -0.0014(18) 0.0046(17) 0.0043(18) C13 0.033(2) 0.037(2) 0.034(2) 0.0034(17) 0.0113(17) 0.0026(17) C14 0.037(2) 0.038(2) 0.047(2) -0.0007(19) 0.017(2) -0.0073(19) C15 0.050(3) 0.041(2) 0.035(2) 0.0022(18) 0.020(2) -0.008(2) C16 0.046(3) 0.040(2) 0.028(2) 0.0018(17) 0.0104(18) 0.0014(19) C17 0.031(2) 0.049(3) 0.035(2) 0.0027(19) 0.0086(18) -0.0009(19) C18 0.038(2) 0.034(2) 0.031(2) -0.0020(17) 0.0111(18) 0.0016(18) Cl8 0.0444(7) 0.0916(10) 0.0518(7) 0.0304(7) 0.0094(5) 0.0049(7) Cl9 0.0468(7) 0.1199(12) 0.0336(6) -0.0041(7) -0.0007(5) 0.0062(7) Cl10 0.0529(8) 0.0785(9) 0.0684(8) -0.0302(7) 0.0016(6) -0.0124(7) Cl11 0.0698(9) 0.0510(7) 0.0743(9) 0.0020(6) 0.0102(7) -0.0201(7) Cl14 0.0387(6) 0.0851(10) 0.0637(8) 0.0028(7) 0.0223(6) -0.0083(6) Cl15 0.0756(9) 0.0996(11) 0.0457(7) 0.0028(7) 0.0324(7) -0.0245(8) Cl16 0.0630(8) 0.0875(10) 0.0301(6) 0.0107(6) 0.0026(5) -0.0101(7) Cl17 0.0335(6) 0.1300(13) 0.0452(7) 0.0188(7) 0.0044(5) -0.0091(7) C19 0.086(4) 0.073(4) 0.046(3) -0.013(3) 0.019(3) -0.004(3) C20A 0.102(15) 0.052(8) 0.071(8) -0.010(6) 0.010(8) 0.000(9) C21A 0.11(2) 0.09(2) 0.083(19) 0.007(12) 0.032(15) 0.010(15) C20B 0.088(14) 0.047(8) 0.068(8) -0.017(6) 0.016(8) 0.024(7) C21B 0.088(19) 0.030(10) 0.15(3) -0.025(13) 0.059(19) -0.004(10) C22 0.144(6) 0.046(3) 0.065(4) 0.013(3) 0.046(4) 0.013(4) C23 0.054(3) 0.053(3) 0.063(3) 0.016(2) 0.020(2) 0.011(2) C24 0.059(3) 0.062(3) 0.075(4) 0.019(3) 0.028(3) -0.007(3) C25 0.049(3) 0.082(4) 0.074(4) 0.015(3) 0.031(3) 0.001(3) C26 0.044(3) 0.064(3) 0.060(3) 0.007(2) 0.026(2) 0.009(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 Rh C7 1.990(4) . ? Rh C18 2.020(4) . ? Rh C1 2.046(4) . ? Rh S1 2.4275(12) . ? Rh S2 2.4997(11) . ? Rh Cl2 2.8682(14) . ? S1 C19 1.839(5) . ? S1 C22 1.853(6) . ? S2 C23 1.832(5) . ? S2 C26 1.832(5) . ? C1 C6 1.382(6) . ? C1 C2 1.390(7) . ? C2 C3 1.384(7) . ? C2 Cl2 1.748(5) . ? C3 C4 1.384(9) . ? C3 Cl3 1.720(6) . ? C4 C5 1.375(9) . ? C4 Cl4 1.710(6) . ? C5 C6 1.396(7) . ? C5 Cl5 1.732(6) . ? C6 Cl6 1.741(5) . ? C7 C8 1.396(6) . ? C7 C12 1.410(6) . ? C8 C9 1.394(6) . ? C8 Cl8 1.728(5) . ? C9 C10 1.381(7) . ? C9 Cl9 1.723(4) . ? C10 C11 1.390(6) . ? C10 Cl10 1.733(4) . ? C11 C12 1.399(6) . ? C11 Cl11 1.728(5) . ? C12 C13 1.472(5) . ? C13 C18 1.398(6) . ? C13 C14 1.405(6) . ? C14 C15 1.389(6) . ? C14 Cl14 1.731(4) . ? C15 C16 1.385(6) . ? C15 Cl15 1.722(4) . ? C16 C17 1.389(6) . ? C16 Cl16 1.723(4) . ? C17 C18 1.390(5) . ? C17 Cl17 1.733(4) . ? C19 C20B 1.480(11) . ? C19 C20A 1.522(12) . ? C20A C21A 1.505(15) . ? C21A C22 1.517(13) . ? C20B C21B 1.519(16) . ? C21B C22 1.525(13) . ? C23 C24 1.524(7) . ? C24 C25 1.516(7) . ? C25 C26 1.509(7) . ? 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 C7 Rh C18 81.31(16) . . ? C7 Rh C1 98.02(18) . . ? C18 Rh C1 89.77(16) . . ? C7 Rh S1 94.18(12) . . ? C18 Rh S1 90.86(11) . . ? C1 Rh S1 167.74(14) . . ? C7 Rh S2 97.42(12) . . ? C18 Rh S2 172.76(11) . . ? C1 Rh S2 97.47(12) . . ? S1 Rh S2 82.11(4) . . ? C7 Rh Cl2 159.24(12) . . ? C18 Rh Cl2 106.01(12) . . ? C1 Rh Cl2 63.19(14) . . ? S1 Rh Cl2 104.93(4) . . ? S2 Rh Cl2 77.64(4) . . ? C19 S1 C22 93.8(3) . . ? C19 S1 Rh 110.81(19) . . ? C22 S1 Rh 114.6(2) . . ? C23 S2 C26 94.5(2) . . ? C23 S2 Rh 116.97(17) . . ? C26 S2 Rh 111.75(16) . . ? C6 C1 C2 114.8(4) . . ? C6 C1 Rh 135.7(4) . . ? C2 C1 Rh 109.5(3) . . ? C3 C2 C1 124.7(5) . . ? C3 C2 Cl2 119.3(4) . . ? C1 C2 Cl2 116.0(4) . . ? C4 C3 C2 118.0(6) . . ? C4 C3 Cl3 121.0(5) . . ? C2 C3 Cl3 120.9(5) . . ? C5 C4 C3 119.5(5) . . ? C5 C4 Cl4 121.1(6) . . ? C3 C4 Cl4 119.4(6) . . ? C4 C5 C6 120.4(5) . . ? C4 C5 Cl5 119.0(5) . . ? C6 C5 Cl5 120.6(5) . . ? C1 C6 C5 122.2(5) . . ? C1 C6 Cl6 121.2(4) . . ? C5 C6 Cl6 116.6(4) . . ? C2 Cl2 Rh 71.02(16) . . ? C8 C7 C12 117.3(4) . . ? C8 C7 Rh 128.3(3) . . ? C12 C7 Rh 114.1(3) . . ? C9 C8 C7 120.4(4) . . ? C9 C8 Cl8 117.7(3) . . ? C7 C8 Cl8 121.8(4) . . ? C10 C9 C8 120.1(4) . . ? C10 C9 Cl9 119.8(4) . . ? C8 C9 Cl9 120.1(4) . . ? C9 C10 C11 119.7(4) . . ? C9 C10 Cl10 120.2(4) . . ? C11 C10 Cl10 120.1(4) . . ? C10 C11 C12 119.9(4) . . ? C10 C11 Cl11 118.6(4) . . ? C12 C11 Cl11 121.0(3) . . ? C11 C12 C7 119.2(4) . . ? C11 C12 C13 127.8(4) . . ? C7 C12 C13 112.7(4) . . ? C18 C13 C14 119.8(4) . . ? C18 C13 C12 113.0(3) . . ? C14 C13 C12 126.7(4) . . ? C15 C14 C13 119.6(4) . . ? C15 C14 Cl14 118.8(3) . . ? C13 C14 Cl14 121.0(3) . . ? C16 C15 C14 119.6(4) . . ? C16 C15 Cl15 119.4(3) . . ? C14 C15 Cl15 120.9(3) . . ? C15 C16 C17 119.6(4) . . ? C15 C16 Cl16 120.0(3) . . ? C17 C16 Cl16 120.3(3) . . ? C16 C17 C18 121.7(4) . . ? C16 C17 Cl17 118.6(3) . . ? C18 C17 Cl17 119.7(3) . . ? C17 C18 C13 117.3(4) . . ? C17 C18 Rh 128.3(3) . . ? C13 C18 Rh 114.4(3) . . ? C20B C19 C20A 36.4(6) . . ? C20B C19 S1 104.5(6) . . ? C20A C19 S1 107.0(5) . . ? C21A C20A C19 111.5(12) . . ? C20A C21A C22 109.9(11) . . ? C19 C20B C21B 107.0(13) . . ? C20B C21B C22 107.4(12) . . ? C21A C22 C21B 7(3) . . ? C21A C22 S1 109.1(6) . . ? C21B C22 S1 105.5(7) . . ? C24 C23 S2 107.0(3) . . ? C25 C24 C23 107.3(4) . . ? C26 C25 C24 108.1(4) . . ? C25 C26 S2 103.9(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 Rh S1 C19 -45.6(2) . . . . ? C18 Rh S1 C19 -127.0(2) . . . . ? C1 Rh S1 C19 140.1(6) . . . . ? S2 Rh S1 C19 51.3(2) . . . . ? Cl2 Rh S1 C19 126.2(2) . . . . ? C7 Rh S1 C22 58.9(3) . . . . ? C18 Rh S1 C22 -22.4(3) . . . . ? C1 Rh S1 C22 -115.3(6) . . . . ? S2 Rh S1 C22 155.8(2) . . . . ? Cl2 Rh S1 C22 -129.3(2) . . . . ? C7 Rh S2 C23 -104.1(2) . . . . ? C18 Rh S2 C23 176.5(9) . . . . ? C1 Rh S2 C23 -5.0(2) . . . . ? S1 Rh S2 C23 162.64(19) . . . . ? Cl2 Rh S2 C23 55.38(19) . . . . ? C7 Rh S2 C26 148.6(2) . . . . ? C18 Rh S2 C26 69.2(10) . . . . ? C1 Rh S2 C26 -112.3(2) . . . . ? S1 Rh S2 C26 55.34(19) . . . . ? Cl2 Rh S2 C26 -51.92(19) . . . . ? C7 Rh C1 C6 -13.8(5) . . . . ? C18 Rh C1 C6 67.4(5) . . . . ? S1 Rh C1 C6 160.4(4) . . . . ? S2 Rh C1 C6 -112.4(4) . . . . ? Cl2 Rh C1 C6 175.5(5) . . . . ? C7 Rh C1 C2 167.1(3) . . . . ? C18 Rh C1 C2 -111.7(3) . . . . ? S1 Rh C1 C2 -18.7(8) . . . . ? S2 Rh C1 C2 68.5(3) . . . . ? Cl2 Rh C1 C2 -3.6(3) . . . . ? C6 C1 C2 C3 5.7(7) . . . . ? Rh C1 C2 C3 -175.0(4) . . . . ? C6 C1 C2 Cl2 -173.5(3) . . . . ? Rh C1 C2 Cl2 5.8(4) . . . . ? C1 C2 C3 C4 -5.0(7) . . . . ? Cl2 C2 C3 C4 174.3(4) . . . . ? C1 C2 C3 Cl3 175.3(4) . . . . ? Cl2 C2 C3 Cl3 -5.5(6) . . . . ? C2 C3 C4 C5 0.4(7) . . . . ? Cl3 C3 C4 C5 -179.9(4) . . . . ? C2 C3 C4 Cl4 -178.5(4) . . . . ? Cl3 C3 C4 Cl4 1.3(6) . . . . ? C3 C4 C5 C6 2.9(8) . . . . ? Cl4 C4 C5 C6 -178.3(4) . . . . ? C3 C4 C5 Cl5 -177.1(4) . . . . ? Cl4 C4 C5 Cl5 1.7(6) . . . . ? C2 C1 C6 C5 -2.2(6) . . . . ? Rh C1 C6 C5 178.8(4) . . . . ? C2 C1 C6 Cl6 177.0(3) . . . . ? Rh C1 C6 Cl6 -2.0(6) . . . . ? C4 C5 C6 C1 -2.0(7) . . . . ? Cl5 C5 C6 C1 178.1(3) . . . . ? C4 C5 C6 Cl6 178.8(4) . . . . ? Cl5 C5 C6 Cl6 -1.1(5) . . . . ? C3 C2 Cl2 Rh 176.6(4) . . . . ? C1 C2 Cl2 Rh -4.1(3) . . . . ? C7 Rh Cl2 C2 -24.1(4) . . . . ? C18 Rh Cl2 C2 84.21(19) . . . . ? C1 Rh Cl2 C2 2.8(2) . . . . ? S1 Rh Cl2 C2 179.53(16) . . . . ? S2 Rh Cl2 C2 -102.24(16) . . . . ? C18 Rh C7 C8 -174.6(4) . . . . ? C1 Rh C7 C8 -86.0(4) . . . . ? S1 Rh C7 C8 95.2(4) . . . . ? S2 Rh C7 C8 12.6(4) . . . . ? Cl2 Rh C7 C8 -62.0(6) . . . . ? C18 Rh C7 C12 12.5(3) . . . . ? C1 Rh C7 C12 101.0(3) . . . . ? S1 Rh C7 C12 -77.7(3) . . . . ? S2 Rh C7 C12 -160.3(3) . . . . ? Cl2 Rh C7 C12 125.1(3) . . . . ? C12 C7 C8 C9 17.4(6) . . . . ? Rh C7 C8 C9 -155.4(3) . . . . ? C12 C7 C8 Cl8 -158.1(3) . . . . ? Rh C7 C8 Cl8 29.1(6) . . . . ? C7 C8 C9 C10 -3.5(7) . . . . ? Cl8 C8 C9 C10 172.2(3) . . . . ? C7 C8 C9 Cl9 175.6(3) . . . . ? Cl8 C8 C9 Cl9 -8.7(5) . . . . ? C8 C9 C10 C11 -6.4(7) . . . . ? Cl9 C9 C10 C11 174.4(3) . . . . ? C8 C9 C10 Cl10 173.2(3) . . . . ? Cl9 C9 C10 Cl10 -5.9(5) . . . . ? C9 C10 C11 C12 1.9(7) . . . . ? Cl10 C10 C11 C12 -177.8(3) . . . . ? C9 C10 C11 Cl11 173.8(4) . . . . ? Cl10 C10 C11 Cl11 -5.8(5) . . . . ? C10 C11 C12 C7 12.3(6) . . . . ? Cl11 C11 C12 C7 -159.4(3) . . . . ? C10 C11 C12 C13 -174.1(4) . . . . ? Cl11 C11 C12 C13 14.2(6) . . . . ? C8 C7 C12 C11 -21.7(6) . . . . ? Rh C7 C12 C11 152.1(3) . . . . ? C8 C7 C12 C13 163.8(4) . . . . ? Rh C7 C12 C13 -22.4(4) . . . . ? C11 C12 C13 C18 -151.5(4) . . . . ? C7 C12 C13 C18 22.4(5) . . . . ? C11 C12 C13 C14 36.2(7) . . . . ? C7 C12 C13 C14 -149.9(4) . . . . ? C18 C13 C14 C15 15.4(6) . . . . ? C12 C13 C14 C15 -172.8(4) . . . . ? C18 C13 C14 Cl14 -154.8(3) . . . . ? C12 C13 C14 Cl14 17.0(6) . . . . ? C13 C14 C15 C16 -3.0(6) . . . . ? Cl14 C14 C15 C16 167.5(3) . . . . ? C13 C14 C15 Cl15 178.6(3) . . . . ? Cl14 C14 C15 Cl15 -10.9(5) . . . . ? C14 C15 C16 C17 -6.7(6) . . . . ? Cl15 C15 C16 C17 171.7(3) . . . . ? C14 C15 C16 Cl16 177.8(3) . . . . ? Cl15 C15 C16 Cl16 -3.8(5) . . . . ? C15 C16 C17 C18 4.2(7) . . . . ? Cl16 C16 C17 C18 179.7(3) . . . . ? C15 C16 C17 Cl17 -176.3(3) . . . . ? Cl16 C16 C17 Cl17 -0.9(5) . . . . ? C16 C17 C18 C13 8.0(6) . . . . ? Cl17 C17 C18 C13 -171.5(3) . . . . ? C16 C17 C18 Rh -170.1(3) . . . . ? Cl17 C17 C18 Rh 10.5(6) . . . . ? C14 C13 C18 C17 -17.7(6) . . . . ? C12 C13 C18 C17 169.5(4) . . . . ? C14 C13 C18 Rh 160.7(3) . . . . ? C12 C13 C18 Rh -12.2(4) . . . . ? C7 Rh C18 C17 178.3(4) . . . . ? C1 Rh C18 C17 80.1(4) . . . . ? S1 Rh C18 C17 -87.6(4) . . . . ? S2 Rh C18 C17 -101.3(9) . . . . ? Cl2 Rh C18 C17 18.2(4) . . . . ? C7 Rh C18 C13 0.2(3) . . . . ? C1 Rh C18 C13 -98.0(3) . . . . ? S1 Rh C18 C13 94.3(3) . . . . ? S2 Rh C18 C13 80.6(10) . . . . ? Cl2 Rh C18 C13 -159.9(3) . . . . ? C22 S1 C19 C20B 22.6(10) . . . . ? Rh S1 C19 C20B 140.8(10) . . . . ? C22 S1 C19 C20A -15.2(11) . . . . ? Rh S1 C19 C20A 103.0(10) . . . . ? C20B C19 C20A C21A -62(2) . . . . ? S1 C19 C20A C21A 29(2) . . . . ? C19 C20A C21A C22 -32(3) . . . . ? C20A C19 C20B C21B 54.8(17) . . . . ? S1 C19 C20B C21B -44.2(19) . . . . ? C19 C20B C21B C22 50(3) . . . . ? C20A C21A C22 C21B -42(10) . . . . ? C20A C21A C22 S1 19(3) . . . . ? C20B C21B C22 C21A 90(14) . . . . ? C20B C21B C22 S1 -30(3) . . . . ? C19 S1 C22 C21A -2.1(17) . . . . ? Rh S1 C22 C21A -117.1(16) . . . . ? C19 S1 C22 C21B 4.6(16) . . . . ? Rh S1 C22 C21B -110.4(16) . . . . ? C26 S2 C23 C24 2.7(4) . . . . ? Rh S2 C23 C24 -114.5(3) . . . . ? S2 C23 C24 C25 -27.3(5) . . . . ? C23 C24 C25 C26 46.2(6) . . . . ? C24 C25 C26 S2 -42.3(5) . . . . ? C23 S2 C26 C25 22.4(4) . . . . ? Rh S2 C26 C25 143.8(3) . . . . ?