# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Abbasi, Alireza' 'Geranmayeh, Shokoofeh' 'Skripkin, Mikhail' 'Eriksson, Lars' _publ_contact_author_name 'Abbasi, Alireza' _publ_contact_author_email aabbasi@khayam.ut.ac.ir _publ_section_title ; Potassium ion-mediated non-covalent bonded metal organic frameworks ; # Attachment '- cif.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 835359' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H12 Cl4 K O2 Rh S2' _chemical_formula_sum 'C4 H12 Cl4 K O2 Rh S2' _chemical_formula_weight 440.07 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.36232(10) _cell_length_b 9.50201(10) _cell_length_c 16.9992(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1350.74(3) _cell_formula_units_Z 4 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 8805 _cell_measurement_theta_min 4.04 _cell_measurement_theta_max 25.67 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 2.646 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6447 _exptl_absorpt_correction_T_max 0.6902 _exptl_absorpt_process_details 'X-red (STOE, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(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 'X-calibur-II with Sapphire-III CCD' _diffrn_measurement_method '\w-scans at different \f' _diffrn_detector_area_resol_mean 12 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% . _diffrn_reflns_number 8805 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0156 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 25.67 _reflns_number_total 2564 _reflns_number_gt 2515 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_data_reduction 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg, 2001)' _computing_publication_material 'PLATON (Spek, 2009)' _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^)+(0.0244P)^2^+0.6521P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(3) _refine_ls_number_reflns 2564 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0201 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0452 _refine_ls_wR_factor_gt 0.0450 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.27913(2) 0.01015(2) 0.112082(12) 0.01758(7) Uani 1 1 d . . . S2 S 0.17132(8) -0.01617(9) 0.23462(4) 0.02441(16) Uani 1 1 d . . . S3 S 0.22195(9) -0.22181(7) 0.09292(4) 0.02093(15) Uani 1 1 d . . . Cl1 Cl 0.52869(9) -0.02870(9) 0.17169(5) 0.03133(19) Uani 1 1 d . . . Cl2 Cl 0.03434(9) 0.05171(9) 0.04751(5) 0.03214(19) Uani 1 1 d . . . Cl3 Cl 0.41347(9) 0.03304(8) -0.01038(4) 0.02708(17) Uani 1 1 d . . . Cl4 Cl 0.31005(11) 0.25757(9) 0.12646(5) 0.0384(2) Uani 1 1 d . . . K1 K 0.18397(9) 0.26954(9) -0.07377(5) 0.0410(2) Uani 1 1 d . . . O1 O 0.0619(3) -0.2596(2) 0.12146(13) 0.0299(5) Uani 1 1 d . . . O2 O 0.2076(4) -0.1504(3) 0.27301(13) 0.0402(6) Uani 1 1 d . . . C1 C -0.0377(4) 0.0078(4) 0.2365(2) 0.0371(8) Uani 1 1 d . . . H1A H -0.0874 -0.0588 0.2018 0.056 Uiso 1 1 calc R . . H1B H -0.0630 0.1016 0.2196 0.056 Uiso 1 1 calc R . . H1C H -0.0765 -0.0064 0.2890 0.056 Uiso 1 1 calc R . . C2 C 0.2386(5) 0.1187(5) 0.2983(2) 0.0453(10) Uani 1 1 d . . . H2A H 0.1955 0.1038 0.3500 0.068 Uiso 1 1 calc R . . H2B H 0.2034 0.2083 0.2788 0.068 Uiso 1 1 calc R . . H2C H 0.3532 0.1173 0.3007 0.068 Uiso 1 1 calc R . . C3 C 0.2340(4) -0.2697(4) -0.00769(19) 0.0343(7) Uani 1 1 d . . . H3A H 0.1936 -0.3635 -0.0144 0.051 Uiso 1 1 calc R . . H3B H 0.3434 -0.2660 -0.0246 0.051 Uiso 1 1 calc R . . H3C H 0.1713 -0.2055 -0.0386 0.051 Uiso 1 1 calc R . . C4 C 0.3618(4) -0.3392(4) 0.1362(2) 0.0362(8) Uani 1 1 d . . . H4A H 0.3634 -0.3254 0.1922 0.054 Uiso 1 1 calc R . . H4B H 0.4664 -0.3213 0.1151 0.054 Uiso 1 1 calc R . . H4C H 0.3313 -0.4345 0.1248 0.054 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 0.01686(10) 0.01798(10) 0.01788(10) -0.00030(9) -0.00008(8) 0.00036(9) S2 0.0235(3) 0.0296(4) 0.0201(3) -0.0042(3) 0.0026(3) 0.0003(3) S3 0.0206(3) 0.0228(3) 0.0193(3) 0.0001(3) 0.0019(3) -0.0008(3) Cl1 0.0208(3) 0.0422(5) 0.0309(4) 0.0016(3) -0.0059(3) -0.0004(3) Cl2 0.0232(4) 0.0369(5) 0.0363(4) 0.0089(4) -0.0069(3) 0.0041(3) Cl3 0.0304(4) 0.0290(4) 0.0219(3) 0.0029(3) 0.0050(3) 0.0013(3) Cl4 0.0433(5) 0.0222(4) 0.0496(5) -0.0067(4) 0.0084(4) -0.0030(4) K1 0.0378(4) 0.0373(4) 0.0478(5) 0.0100(4) 0.0016(4) 0.0072(3) O1 0.0245(11) 0.0329(12) 0.0322(12) -0.0015(11) 0.0051(9) -0.0062(10) O2 0.0520(16) 0.0459(14) 0.0226(12) 0.0074(10) 0.0077(12) 0.0106(14) C1 0.0255(16) 0.044(2) 0.0421(19) -0.0074(19) 0.0111(13) -0.0007(18) C2 0.045(2) 0.064(3) 0.0271(19) -0.0202(16) 0.0066(17) -0.016(2) C3 0.0376(18) 0.0375(19) 0.0278(16) -0.0072(14) 0.0058(15) -0.0064(16) C4 0.0337(19) 0.0306(19) 0.044(2) 0.0088(16) 0.0024(15) 0.0102(15) _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 S3 2.2788(7) . ? Rh1 S2 2.2836(7) . ? Rh1 Cl1 2.3491(7) . ? Rh1 Cl2 2.3560(8) . ? Rh1 Cl3 2.3755(7) . ? Rh1 Cl4 2.3777(8) . ? S2 O2 1.464(3) . ? S2 C1 1.763(3) . ? S2 C2 1.770(3) . ? S3 O1 1.468(2) . ? S3 C3 1.773(3) . ? S3 C4 1.776(4) . ? O2 K1 2.981(2) 2 ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? 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 S3 Rh1 S2 86.65(3) . . ? S3 Rh1 Cl1 95.51(3) . . ? S2 Rh1 Cl1 86.56(3) . . ? S3 Rh1 Cl2 85.02(3) . . ? S2 Rh1 Cl2 95.76(3) . . ? Cl1 Rh1 Cl2 177.65(3) . . ? S3 Rh1 Cl3 93.58(3) . . ? S2 Rh1 Cl3 174.97(3) . . ? Cl1 Rh1 Cl3 88.41(3) . . ? Cl2 Rh1 Cl3 89.27(3) . . ? S3 Rh1 Cl4 173.65(3) . . ? S2 Rh1 Cl4 93.29(3) . . ? Cl1 Rh1 Cl4 90.83(3) . . ? Cl2 Rh1 Cl4 88.66(3) . . ? Cl3 Rh1 Cl4 87.03(3) . . ? S3 Rh1 K1 130.92(2) . 4 ? S2 Rh1 K1 122.38(2) . 4 ? Cl1 Rh1 K1 53.52(2) . 4 ? Cl2 Rh1 K1 124.55(2) . 4 ? Cl3 Rh1 K1 54.13(2) . 4 ? Cl4 Rh1 K1 53.99(2) . 4 ? S3 Rh1 K1 115.61(2) . . ? S2 Rh1 K1 134.00(2) . . ? Cl1 Rh1 K1 126.97(2) . . ? Cl2 Rh1 K1 50.90(2) . . ? Cl3 Rh1 K1 50.15(2) . . ? Cl4 Rh1 K1 60.27(3) . . ? K1 Rh1 K1 74.067(12) 4 . ? O2 S2 C1 108.06(19) . . ? O2 S2 C2 107.00(19) . . ? C1 S2 C2 102.2(2) . . ? O2 S2 Rh1 114.84(10) . . ? C1 S2 Rh1 113.18(12) . . ? C2 S2 Rh1 110.69(14) . . ? O1 S3 C3 107.92(15) . . ? O1 S3 C4 108.04(15) . . ? C3 S3 C4 101.61(18) . . ? O1 S3 Rh1 112.38(10) . . ? C3 S3 Rh1 111.98(12) . . ? C4 S3 Rh1 114.22(13) . . ? Rh1 Cl1 K1 90.86(3) . 4 ? Rh1 Cl2 K1 93.97(3) . . ? Rh1 Cl2 K1 140.15(4) . 4_455 ? K1 Cl2 K1 95.66(2) . 4_455 ? Rh1 Cl3 K1 94.42(3) . . ? Rh1 Cl3 K1 89.79(3) . 4 ? K1 Cl3 K1 99.33(2) . 4 ? Rh1 Cl4 K1 89.88(3) . 4 ? Rh1 Cl4 K1 84.33(3) . . ? K1 Cl4 K1 91.37(2) 4 . ? O2 K1 Cl3 80.93(5) 2_554 . ? O2 K1 Cl2 116.05(6) 2_554 . ? Cl3 K1 Cl2 63.43(2) . . ? O2 K1 Cl1 87.81(5) 2_554 4_455 ? Cl3 K1 Cl1 164.25(3) . 4_455 ? Cl2 K1 Cl1 132.05(3) . 4_455 ? O2 K1 Cl4 91.24(7) 2_554 4_455 ? Cl3 K1 Cl4 128.49(4) . 4_455 ? Cl2 K1 Cl4 75.48(3) . 4_455 ? Cl1 K1 Cl4 62.32(2) 4_455 4_455 ? O2 K1 Cl3 144.18(6) 2_554 4_455 ? Cl3 K1 Cl3 133.03(3) . 4_455 ? Cl2 K1 Cl3 79.48(3) . 4_455 ? Cl1 K1 Cl3 60.78(2) 4_455 4_455 ? Cl4 K1 Cl3 60.15(2) 4_455 4_455 ? O2 K1 Cl2 92.42(7) 2_554 4 ? Cl3 K1 Cl2 77.71(3) . 4 ? Cl2 K1 Cl2 125.22(3) . 4 ? Cl1 K1 Cl2 91.89(3) 4_455 4 ? Cl4 K1 Cl2 153.78(3) 4_455 4 ? Cl3 K1 Cl2 104.54(3) 4_455 4 ? O2 K1 Cl4 137.06(6) 2_554 . ? Cl3 K1 Cl4 57.98(2) . . ? Cl2 K1 Cl4 58.42(2) . . ? Cl1 K1 Cl4 129.24(3) 4_455 . ? Cl4 K1 Cl4 122.89(3) 4_455 . ? Cl3 K1 Cl4 78.76(3) 4_455 . ? Cl2 K1 Cl4 68.74(2) 4 . ? O2 K1 Rh1 108.14(6) 2_554 4_455 ? Cl3 K1 Rh1 159.76(3) . 4_455 ? Cl2 K1 Rh1 96.45(2) . 4_455 ? Cl1 K1 Rh1 35.617(15) 4_455 4_455 ? Cl4 K1 Rh1 36.123(17) 4_455 4_455 ? Cl3 K1 Rh1 36.085(15) 4_455 4_455 ? Cl2 K1 Rh1 118.88(3) 4 4_455 ? Cl4 K1 Rh1 114.77(3) . 4_455 ? O2 K1 Rh1 112.78(5) 2_554 . ? Cl3 K1 Rh1 35.434(16) . . ? Cl2 K1 Rh1 35.123(16) . . ? Cl1 K1 Rh1 158.89(3) 4_455 . ? Cl4 K1 Rh1 110.57(3) 4_455 . ? Cl3 K1 Rh1 98.20(2) 4_455 . ? Cl2 K1 Rh1 91.83(2) 4 . ? Cl4 K1 Rh1 35.393(15) . . ? Rh1 K1 Rh1 126.98(2) 4_455 . ? O2 K1 K1 99.16(6) 2_554 4 ? Cl3 K1 K1 41.265(19) . 4 ? Cl2 K1 K1 87.39(3) . 4 ? Cl1 K1 K1 131.54(3) 4_455 4 ? Cl4 K1 K1 162.60(3) 4_455 4 ? Cl3 K1 K1 114.26(3) 4_455 4 ? Cl2 K1 K1 40.300(16) 4 4 ? Cl4 K1 K1 41.84(2) . 4 ? Rh1 K1 K1 147.14(3) 4_455 4 ? Rh1 K1 K1 52.481(18) . 4 ? O2 K1 K1 132.79(7) 2_554 4_455 ? Cl3 K1 K1 106.96(3) . 4_455 ? Cl2 K1 K1 44.04(2) . 4_455 ? Cl1 K1 K1 88.77(2) 4_455 4_455 ? Cl4 K1 K1 46.792(18) 4_455 4_455 ? Cl3 K1 K1 39.403(18) 4_455 4_455 ? Cl2 K1 K1 134.76(4) 4 4_455 ? Cl4 K1 K1 76.16(3) . 4_455 ? Rh1 K1 K1 53.452(10) 4_455 4_455 ? Rh1 K1 K1 73.98(2) . 4_455 ? K1 K1 K1 117.54(3) 4 4_455 ? S2 O2 K1 141.55(14) . 2 ? S2 C1 H1A 109.5 . . ? S2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S2 C2 H2A 109.5 . . ? S2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? S2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? S3 C3 H3A 109.5 . . ? S3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? S3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? S3 C4 H4A 109.5 . . ? S3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? 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 S3 Rh1 S2 O2 38.33(14) . . . . ? Cl1 Rh1 S2 O2 -57.40(14) . . . . ? Cl2 Rh1 S2 O2 122.98(14) . . . . ? Cl4 Rh1 S2 O2 -148.03(14) . . . . ? K1 Rh1 S2 O2 -99.39(14) 4 . . . ? K1 Rh1 S2 O2 161.38(14) . . . . ? S3 Rh1 S2 C1 -86.40(16) . . . . ? Cl1 Rh1 S2 C1 177.86(16) . . . . ? Cl2 Rh1 S2 C1 -1.75(16) . . . . ? Cl4 Rh1 S2 C1 87.23(16) . . . . ? K1 Rh1 S2 C1 135.88(15) 4 . . . ? K1 Rh1 S2 C1 36.64(16) . . . . ? S3 Rh1 S2 C2 159.61(17) . . . . ? Cl1 Rh1 S2 C2 63.88(17) . . . . ? Cl2 Rh1 S2 C2 -115.74(17) . . . . ? Cl4 Rh1 S2 C2 -26.75(17) . . . . ? K1 Rh1 S2 C2 21.89(17) 4 . . . ? K1 Rh1 S2 C2 -77.35(17) . . . . ? S2 Rh1 S3 O1 43.84(11) . . . . ? Cl1 Rh1 S3 O1 130.06(11) . . . . ? Cl2 Rh1 S3 O1 -52.24(11) . . . . ? Cl3 Rh1 S3 O1 -141.20(11) . . . . ? K1 Rh1 S3 O1 175.08(10) 4 . . . ? K1 Rh1 S3 O1 -94.20(10) . . . . ? S2 Rh1 S3 C3 165.50(14) . . . . ? Cl1 Rh1 S3 C3 -108.28(14) . . . . ? Cl2 Rh1 S3 C3 69.42(14) . . . . ? Cl3 Rh1 S3 C3 -19.54(14) . . . . ? K1 Rh1 S3 C3 -63.26(14) 4 . . . ? K1 Rh1 S3 C3 27.46(14) . . . . ? S2 Rh1 S3 C4 -79.70(14) . . . . ? Cl1 Rh1 S3 C4 6.52(14) . . . . ? Cl2 Rh1 S3 C4 -175.78(14) . . . . ? Cl3 Rh1 S3 C4 95.27(14) . . . . ? K1 Rh1 S3 C4 51.55(14) 4 . . . ? K1 Rh1 S3 C4 142.27(14) . . . . ? S3 Rh1 Cl1 K1 138.34(3) . . . 4 ? S2 Rh1 Cl1 K1 -135.36(3) . . . 4 ? Cl3 Rh1 Cl1 K1 44.89(3) . . . 4 ? Cl4 Rh1 Cl1 K1 -42.11(3) . . . 4 ? K1 Rh1 Cl1 K1 10.31(4) . . . 4 ? S3 Rh1 Cl2 K1 -129.03(3) . . . . ? S2 Rh1 Cl2 K1 144.85(3) . . . . ? Cl3 Rh1 Cl2 K1 -35.37(3) . . . . ? Cl4 Rh1 Cl2 K1 51.67(3) . . . . ? K1 Rh1 Cl2 K1 8.56(5) 4 . . . ? S3 Rh1 Cl2 K1 127.23(5) . . . 4_455 ? S2 Rh1 Cl2 K1 41.12(6) . . . 4_455 ? Cl3 Rh1 Cl2 K1 -139.10(5) . . . 4_455 ? Cl4 Rh1 Cl2 K1 -52.06(6) . . . 4_455 ? K1 Rh1 Cl2 K1 -95.18(5) 4 . . 4_455 ? K1 Rh1 Cl2 K1 -103.74(6) . . . 4_455 ? S3 Rh1 Cl3 K1 120.78(3) . . . . ? Cl1 Rh1 Cl3 K1 -143.80(3) . . . . ? Cl2 Rh1 Cl3 K1 35.81(3) . . . . ? Cl4 Rh1 Cl3 K1 -52.89(3) . . . . ? K1 Rh1 Cl3 K1 -99.34(2) 4 . . . ? S3 Rh1 Cl3 K1 -139.88(3) . . . 4 ? Cl1 Rh1 Cl3 K1 -44.45(3) . . . 4 ? Cl2 Rh1 Cl3 K1 135.16(3) . . . 4 ? Cl4 Rh1 Cl3 K1 46.46(3) . . . 4 ? K1 Rh1 Cl3 K1 99.34(2) . . . 4 ? S2 Rh1 Cl4 K1 128.41(3) . . . 4 ? Cl1 Rh1 Cl4 K1 41.80(3) . . . 4 ? Cl2 Rh1 Cl4 K1 -135.90(3) . . . 4 ? Cl3 Rh1 Cl4 K1 -46.56(3) . . . 4 ? K1 Rh1 Cl4 K1 -91.39(2) . . . 4 ? S2 Rh1 Cl4 K1 -140.21(3) . . . . ? Cl1 Rh1 Cl4 K1 133.19(3) . . . . ? Cl2 Rh1 Cl4 K1 -44.52(3) . . . . ? Cl3 Rh1 Cl4 K1 44.82(3) . . . . ? K1 Rh1 Cl4 K1 91.39(2) 4 . . . ? Rh1 Cl3 K1 O2 -154.25(6) . . . 2_554 ? K1 Cl3 K1 O2 115.24(6) 4 . . 2_554 ? Rh1 Cl3 K1 Cl2 -29.01(3) . . . . ? K1 Cl3 K1 Cl2 -119.52(3) 4 . . . ? Rh1 Cl3 K1 Cl1 160.85(13) . . . 4_455 ? K1 Cl3 K1 Cl1 70.34(13) 4 . . 4_455 ? Rh1 Cl3 K1 Cl4 -69.93(5) . . . 4_455 ? K1 Cl3 K1 Cl4 -160.44(5) 4 . . 4_455 ? Rh1 Cl3 K1 Cl3 12.73(5) . . . 4_455 ? K1 Cl3 K1 Cl3 -77.78(6) 4 . . 4_455 ? Rh1 Cl3 K1 Cl2 111.25(3) . . . 4 ? K1 Cl3 K1 Cl2 20.74(2) 4 . . 4 ? Rh1 Cl3 K1 Cl4 38.79(2) . . . . ? K1 Cl3 K1 Cl4 -51.72(3) 4 . . . ? Rh1 Cl3 K1 Rh1 -35.67(10) . . . 4_455 ? K1 Cl3 K1 Rh1 -126.18(10) 4 . . 4_455 ? K1 Cl3 K1 Rh1 -90.51(3) 4 . . . ? Rh1 Cl3 K1 K1 90.51(3) . . . 4 ? Rh1 Cl3 K1 K1 -22.15(4) . . . 4_455 ? K1 Cl3 K1 K1 -112.66(4) 4 . . 4_455 ? Rh1 Cl2 K1 O2 93.11(7) . . . 2_554 ? K1 Cl2 K1 O2 -125.61(7) 4_455 . . 2_554 ? Rh1 Cl2 K1 Cl3 29.26(3) . . . . ? K1 Cl2 K1 Cl3 170.53(4) 4_455 . . . ? Rh1 Cl2 K1 Cl1 -154.33(4) . . . 4_455 ? K1 Cl2 K1 Cl1 -13.06(4) 4_455 . . 4_455 ? Rh1 Cl2 K1 Cl4 177.28(3) . . . 4_455 ? K1 Cl2 K1 Cl4 -41.44(2) 4_455 . . 4_455 ? Rh1 Cl2 K1 Cl3 -121.07(3) . . . 4_455 ? K1 Cl2 K1 Cl3 20.20(2) 4_455 . . 4_455 ? Rh1 Cl2 K1 Cl2 -20.62(4) . . . 4 ? K1 Cl2 K1 Cl2 120.65(5) 4_455 . . 4 ? Rh1 Cl2 K1 Cl4 -37.88(2) . . . . ? K1 Cl2 K1 Cl4 103.40(3) 4_455 . . . ? Rh1 Cl2 K1 Rh1 -153.06(3) . . . 4_455 ? K1 Cl2 K1 Rh1 -11.78(2) 4_455 . . 4_455 ? K1 Cl2 K1 Rh1 141.28(4) 4_455 . . . ? Rh1 Cl2 K1 K1 -5.81(3) . . . 4 ? K1 Cl2 K1 K1 135.47(4) 4_455 . . 4 ? Rh1 Cl2 K1 K1 -141.28(4) . . . 4_455 ? Rh1 Cl4 K1 O2 -57.93(10) . . . 2_554 ? K1 Cl4 K1 O2 31.82(9) 4 . . 2_554 ? Rh1 Cl4 K1 Cl3 -38.84(2) . . . . ? K1 Cl4 K1 Cl3 50.91(2) 4 . . . ? Rh1 Cl4 K1 Cl2 37.58(2) . . . . ? K1 Cl4 K1 Cl2 127.33(3) 4 . . . ? Rh1 Cl4 K1 Cl1 158.45(4) . . . 4_455 ? K1 Cl4 K1 Cl1 -111.81(4) 4 . . 4_455 ? Rh1 Cl4 K1 Cl4 79.18(4) . . . 4_455 ? K1 Cl4 K1 Cl4 168.93(5) 4 . . 4_455 ? Rh1 Cl4 K1 Cl3 122.05(3) . . . 4_455 ? K1 Cl4 K1 Cl3 -148.20(3) 4 . . 4_455 ? Rh1 Cl4 K1 Cl2 -127.34(3) . . . 4 ? K1 Cl4 K1 Cl2 -37.60(2) 4 . . 4 ? Rh1 Cl4 K1 Rh1 119.63(3) . . . 4_455 ? K1 Cl4 K1 Rh1 -150.63(3) 4 . . 4_455 ? K1 Cl4 K1 Rh1 89.75(3) 4 . . . ? Rh1 Cl4 K1 K1 -89.75(3) . . . 4 ? Rh1 Cl4 K1 K1 81.73(3) . . . 4_455 ? K1 Cl4 K1 K1 171.48(4) 4 . . 4_455 ? S3 Rh1 K1 O2 -44.23(7) . . . 2_554 ? S2 Rh1 K1 O2 -156.11(7) . . . 2_554 ? Cl1 Rh1 K1 O2 75.38(8) . . . 2_554 ? Cl2 Rh1 K1 O2 -103.34(8) . . . 2_554 ? Cl3 Rh1 K1 O2 27.73(7) . . . 2_554 ? Cl4 Rh1 K1 O2 141.23(7) . . . 2_554 ? K1 Rh1 K1 O2 83.98(7) 4 . . 2_554 ? S3 Rh1 K1 Cl3 -71.96(4) . . . . ? S2 Rh1 K1 Cl3 176.16(4) . . . . ? Cl1 Rh1 K1 Cl3 47.65(4) . . . . ? Cl2 Rh1 K1 Cl3 -131.07(4) . . . . ? Cl4 Rh1 K1 Cl3 113.50(4) . . . . ? K1 Rh1 K1 Cl3 56.26(3) 4 . . . ? S3 Rh1 K1 Cl2 59.11(4) . . . . ? S2 Rh1 K1 Cl2 -52.77(4) . . . . ? Cl1 Rh1 K1 Cl2 178.72(4) . . . . ? Cl3 Rh1 K1 Cl2 131.07(4) . . . . ? Cl4 Rh1 K1 Cl2 -115.43(4) . . . . ? K1 Rh1 K1 Cl2 -172.68(4) 4 . . . ? S3 Rh1 K1 Cl1 122.36(8) . . . 4_455 ? S2 Rh1 K1 Cl1 10.47(10) . . . 4_455 ? Cl1 Rh1 K1 Cl1 -118.03(7) . . . 4_455 ? Cl2 Rh1 K1 Cl1 63.25(8) . . . 4_455 ? Cl3 Rh1 K1 Cl1 -165.68(9) . . . 4_455 ? Cl4 Rh1 K1 Cl1 -52.18(8) . . . 4_455 ? K1 Rh1 K1 Cl1 -109.43(9) 4 . . 4_455 ? S3 Rh1 K1 Cl4 56.30(4) . . . 4_455 ? S2 Rh1 K1 Cl4 -55.59(4) . . . 4_455 ? Cl1 Rh1 K1 Cl4 175.90(3) . . . 4_455 ? Cl2 Rh1 K1 Cl4 -2.81(3) . . . 4_455 ? Cl3 Rh1 K1 Cl4 128.26(4) . . . 4_455 ? Cl4 Rh1 K1 Cl4 -118.24(4) . . . 4_455 ? K1 Rh1 K1 Cl4 -175.49(4) 4 . . 4_455 ? S3 Rh1 K1 Cl3 117.41(3) . . . 4_455 ? S2 Rh1 K1 Cl3 5.52(4) . . . 4_455 ? Cl1 Rh1 K1 Cl3 -122.98(3) . . . 4_455 ? Cl2 Rh1 K1 Cl3 58.30(3) . . . 4_455 ? Cl3 Rh1 K1 Cl3 -170.63(4) . . . 4_455 ? Cl4 Rh1 K1 Cl3 -57.13(3) . . . 4_455 ? K1 Rh1 K1 Cl3 -114.38(3) 4 . . 4_455 ? S3 Rh1 K1 Cl2 -137.62(3) . . . 4 ? S2 Rh1 K1 Cl2 110.50(4) . . . 4 ? Cl1 Rh1 K1 Cl2 -18.01(4) . . . 4 ? Cl2 Rh1 K1 Cl2 163.27(3) . . . 4 ? Cl3 Rh1 K1 Cl2 -65.66(3) . . . 4 ? Cl4 Rh1 K1 Cl2 47.84(3) . . . 4 ? K1 Rh1 K1 Cl2 -9.406(17) 4 . . 4 ? S3 Rh1 K1 Cl4 174.54(3) . . . . ? S2 Rh1 K1 Cl4 62.65(4) . . . . ? Cl1 Rh1 K1 Cl4 -65.86(4) . . . . ? Cl2 Rh1 K1 Cl4 115.43(4) . . . . ? Cl3 Rh1 K1 Cl4 -113.50(4) . . . . ? K1 Rh1 K1 Cl4 -57.25(3) 4 . . . ? S3 Rh1 K1 Rh1 93.41(3) . . . 4_455 ? S2 Rh1 K1 Rh1 -18.47(5) . . . 4_455 ? Cl1 Rh1 K1 Rh1 -146.98(3) . . . 4_455 ? Cl2 Rh1 K1 Rh1 34.30(3) . . . 4_455 ? Cl3 Rh1 K1 Rh1 165.37(4) . . . 4_455 ? Cl4 Rh1 K1 Rh1 -81.12(4) . . . 4_455 ? K1 Rh1 K1 Rh1 -138.37(4) 4 . . 4_455 ? S3 Rh1 K1 K1 -128.21(3) . . . 4 ? S2 Rh1 K1 K1 119.90(3) . . . 4 ? Cl1 Rh1 K1 K1 -8.61(4) . . . 4 ? Cl2 Rh1 K1 K1 172.68(4) . . . 4 ? Cl3 Rh1 K1 K1 -56.26(3) . . . 4 ? Cl4 Rh1 K1 K1 57.25(3) . . . 4 ? S3 Rh1 K1 K1 86.01(3) . . . 4_455 ? S2 Rh1 K1 K1 -25.87(4) . . . 4_455 ? Cl1 Rh1 K1 K1 -154.38(3) . . . 4_455 ? Cl2 Rh1 K1 K1 26.90(3) . . . 4_455 ? Cl3 Rh1 K1 K1 157.97(4) . . . 4_455 ? Cl4 Rh1 K1 K1 -88.53(3) . . . 4_455 ? K1 Rh1 K1 K1 -145.78(3) 4 . . 4_455 ? C1 S2 O2 K1 -99.0(3) . . . 2 ? C2 S2 O2 K1 10.4(3) . . . 2 ? Rh1 S2 O2 K1 133.6(2) . . . 2 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.67 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.369 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.075 #========================================END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 835360' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H28 Cl8 K2 O6 Rh2 S4, H2 O' _chemical_formula_sum 'C8 H30 Cl8 K2 O7 Rh2 S4' _chemical_formula_weight 934.22 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9314(2) _cell_length_b 8.93130(10) _cell_length_c 27.9106(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.9070(10) _cell_angle_gamma 90.00 _cell_volume 3049.59(7) _cell_formula_units_Z 4 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 12846 _cell_measurement_theta_min 3.73 _cell_measurement_theta_max 25.62 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.035 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 2.357 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6770 _exptl_absorpt_correction_T_max 0.7204 _exptl_absorpt_process_details 'X-red (STOE, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(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 'X-calibur-II with Sapphire-III CCD' _diffrn_measurement_method '\w-scans at different \f' _diffrn_detector_area_resol_mean 12 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% . _diffrn_reflns_number 12846 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.62 _reflns_number_total 5765 _reflns_number_gt 4395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_data_reduction 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg, 2001)' _computing_publication_material 'PLATON (Spek, 2009)' _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^)+(0.0275P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5765 _refine_ls_number_parameters 307 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0553 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.257322(18) 0.19427(2) -0.263286(8) 0.01880(6) Uani 1 1 d . . . Rh2 Rh 0.26697(2) -0.19749(3) -0.481009(8) 0.02496(7) Uani 1 1 d . . . K1 K 0.44575(7) -0.00865(10) -0.34594(3) 0.0470(2) Uani 1 1 d . . . K2 K 0.08911(8) -0.01112(10) -0.39942(3) 0.0520(2) Uani 1 1 d . . . Cl1 Cl 0.06855(6) 0.16665(9) -0.29855(3) 0.0353(2) Uani 1 1 d . . . Cl2 Cl 0.28051(8) -0.05783(8) -0.28251(3) 0.0405(2) Uani 1 1 d . . . Cl3 Cl 0.44825(6) 0.21712(9) -0.23085(3) 0.03480(19) Uani 1 1 d . . . Cl4 Cl 0.26243(7) 0.25675(9) -0.34574(3) 0.03244(18) Uani 1 1 d . . . Cl5 Cl 0.07582(7) -0.18995(10) -0.50307(3) 0.0432(2) Uani 1 1 d . . . Cl6 Cl 0.27211(9) 0.05705(9) -0.45541(3) 0.0492(2) Uani 1 1 d . . . Cl7 Cl 0.45764(7) -0.18969(11) -0.45775(3) 0.0489(2) Uani 1 1 d . . . Cl8 Cl 0.27904(8) -0.26779(10) -0.39772(3) 0.0458(2) Uani 1 1 d . . . S1 S 0.23425(7) 0.12864(9) -0.18900(3) 0.02755(18) Uani 1 1 d . . . S2 S 0.25158(6) 0.44066(8) -0.24212(3) 0.02659(18) Uani 1 1 d . . . S3 S 0.26533(7) -0.44733(9) -0.49895(3) 0.03208(19) Uani 1 1 d . . . S4 S 0.24929(7) -0.13143(10) -0.56269(3) 0.0328(2) Uani 1 1 d . . . O1 O 0.1595(2) 0.2294(3) -0.17454(8) 0.0441(6) Uani 1 1 d . . . O2 O 0.32065(19) 0.4757(2) -0.18992(8) 0.0409(6) Uani 1 1 d . . . O3 O 0.2660(3) -0.4843(3) -0.54968(9) 0.0632(8) Uani 1 1 d . . . O4 O 0.1516(2) -0.1886(4) -0.60110(9) 0.0662(9) Uani 1 1 d . . . O5 O 0.5230(3) 0.3078(4) -0.33167(12) 0.0680(9) Uani 1 1 d D . . H5A H 0.4558(18) 0.300(6) -0.3378(18) 0.102 Uiso 1 1 d D . . H5B H 0.571(3) 0.313(6) -0.3036(11) 0.102 Uiso 1 1 d D . . O6 O -0.0162(3) -0.0664(3) -0.10983(12) 0.0628(8) Uani 1 1 d D . . H6A H 0.039(3) -0.115(5) -0.1096(19) 0.094 Uiso 1 1 d D . . H6B H -0.069(3) -0.124(5) -0.1168(18) 0.094 Uiso 1 1 d D . . O7 O -0.0073(3) -0.2537(4) -0.37953(16) 0.0860(12) Uani 1 1 d D . . H7A H 0.000(5) -0.341(3) -0.388(2) 0.129 Uiso 1 1 d D . . H7B H -0.039(4) -0.256(7) -0.3579(17) 0.129 Uiso 1 1 d D . . C11 C 0.1854(3) -0.0572(4) -0.18922(14) 0.0453(9) Uani 1 1 d . . . H11A H 0.1183 -0.0690 -0.2168 0.068 Uiso 1 1 calc R . . H11B H 0.1725 -0.0768 -0.1578 0.068 Uiso 1 1 calc R . . H11C H 0.2388 -0.1264 -0.1932 0.068 Uiso 1 1 calc R . . C12 C 0.3587(3) 0.1190(4) -0.13842(12) 0.0454(9) Uani 1 1 d . . . H12A H 0.3929 0.2157 -0.1332 0.068 Uiso 1 1 calc R . . H12B H 0.4062 0.0477 -0.1464 0.068 Uiso 1 1 calc R . . H12C H 0.3445 0.0882 -0.1082 0.068 Uiso 1 1 calc R . . C21 C 0.1188(3) 0.5084(4) -0.25063(15) 0.0474(10) Uani 1 1 d . . . H21A H 0.0888 0.4577 -0.2278 0.071 Uiso 1 1 calc R . . H21B H 0.0732 0.4904 -0.2849 0.071 Uiso 1 1 calc R . . H21C H 0.1219 0.6140 -0.2439 0.071 Uiso 1 1 calc R . . C22 C 0.2921(3) 0.5585(4) -0.28324(14) 0.0480(10) Uani 1 1 d . . . H22A H 0.3652 0.5336 -0.2819 0.072 Uiso 1 1 calc R . . H22B H 0.2897 0.6608 -0.2731 0.072 Uiso 1 1 calc R . . H22C H 0.2434 0.5454 -0.3172 0.072 Uiso 1 1 calc R . . C31 C 0.1535(3) -0.5406(4) -0.48892(15) 0.0527(10) Uani 1 1 d . . . H31A H 0.0867 -0.5081 -0.5138 0.079 Uiso 1 1 calc R . . H31B H 0.1513 -0.5176 -0.4557 0.079 Uiso 1 1 calc R . . H31C H 0.1615 -0.6467 -0.4919 0.079 Uiso 1 1 calc R . . C32 C 0.3772(3) -0.5411(4) -0.45523(17) 0.0641(12) Uani 1 1 d . . . H32A H 0.4444 -0.5002 -0.4572 0.096 Uiso 1 1 calc R . . H32B H 0.3737 -0.6459 -0.4633 0.096 Uiso 1 1 calc R . . H32C H 0.3742 -0.5279 -0.4216 0.096 Uiso 1 1 calc R . . C41 C 0.3627(3) -0.1813(4) -0.58076(14) 0.0501(10) Uani 1 1 d . . . H41A H 0.3743 -0.2874 -0.5769 0.075 Uiso 1 1 calc R . . H41B H 0.4264 -0.1298 -0.5597 0.075 Uiso 1 1 calc R . . H41C H 0.3495 -0.1540 -0.6155 0.075 Uiso 1 1 calc R . . C42 C 0.2514(3) 0.0637(4) -0.57096(14) 0.0550(11) Uani 1 1 d . . . H42A H 0.1932 0.1088 -0.5617 0.083 Uiso 1 1 calc R . . H42B H 0.2419 0.0857 -0.6058 0.083 Uiso 1 1 calc R . . H42C H 0.3202 0.1031 -0.5499 0.083 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 0.01961(13) 0.01787(12) 0.02001(12) -0.00070(10) 0.00793(9) -0.00026(10) Rh2 0.03205(15) 0.02237(13) 0.01992(12) 0.00161(10) 0.00769(10) -0.00184(11) K1 0.0408(5) 0.0483(5) 0.0484(5) 0.0069(4) 0.0098(4) 0.0031(4) K2 0.0622(6) 0.0501(5) 0.0453(5) -0.0097(4) 0.0197(4) -0.0148(4) Cl1 0.0224(4) 0.0455(5) 0.0348(4) 0.0014(4) 0.0048(3) -0.0077(4) Cl2 0.0619(6) 0.0197(4) 0.0440(5) -0.0044(4) 0.0227(4) 0.0030(4) Cl3 0.0204(4) 0.0446(5) 0.0393(4) -0.0019(4) 0.0093(3) 0.0017(4) Cl4 0.0390(5) 0.0360(4) 0.0256(4) 0.0016(3) 0.0149(3) -0.0007(4) Cl5 0.0353(5) 0.0477(5) 0.0486(5) -0.0018(4) 0.0165(4) 0.0056(4) Cl6 0.0815(7) 0.0254(5) 0.0391(5) -0.0033(4) 0.0174(5) -0.0037(4) Cl7 0.0329(5) 0.0614(6) 0.0435(5) 0.0072(5) 0.0002(4) -0.0087(5) Cl8 0.0742(7) 0.0399(5) 0.0245(4) 0.0035(4) 0.0177(4) -0.0061(5) S1 0.0308(5) 0.0311(4) 0.0227(4) 0.0025(3) 0.0115(3) -0.0010(3) S2 0.0284(5) 0.0215(4) 0.0317(4) -0.0052(3) 0.0123(3) 0.0010(3) S3 0.0410(5) 0.0254(4) 0.0322(4) -0.0026(3) 0.0151(4) -0.0004(4) S4 0.0333(5) 0.0428(5) 0.0193(4) 0.0041(4) 0.0045(3) -0.0081(4) O1 0.0540(16) 0.0495(15) 0.0400(14) 0.0036(12) 0.0309(12) 0.0110(12) O2 0.0446(15) 0.0352(14) 0.0397(13) -0.0145(11) 0.0093(11) -0.0032(11) O3 0.113(2) 0.0468(16) 0.0437(15) -0.0162(13) 0.0438(16) -0.0113(16) O4 0.0535(17) 0.109(3) 0.0287(14) 0.0026(15) 0.0022(12) -0.0389(17) O5 0.061(2) 0.084(2) 0.068(2) 0.0049(19) 0.0333(18) -0.009(2) O6 0.065(2) 0.0471(19) 0.0682(19) -0.0072(15) 0.0103(18) -0.0024(14) O7 0.107(3) 0.0521(19) 0.139(3) -0.003(2) 0.095(3) -0.0039(19) C11 0.046(2) 0.041(2) 0.051(2) 0.0128(18) 0.0191(19) -0.0103(18) C12 0.047(2) 0.058(2) 0.0283(19) 0.0082(17) 0.0074(17) -0.0058(19) C21 0.037(2) 0.038(2) 0.067(3) -0.0035(19) 0.0163(19) 0.0172(17) C22 0.067(3) 0.0243(19) 0.060(2) 0.0040(17) 0.031(2) -0.0091(17) C31 0.055(3) 0.034(2) 0.073(3) 0.0022(19) 0.026(2) -0.0092(18) C32 0.054(3) 0.033(2) 0.089(3) 0.009(2) 0.002(2) 0.0144(19) C41 0.059(3) 0.057(3) 0.042(2) 0.0017(19) 0.0269(19) 0.000(2) C42 0.073(3) 0.051(3) 0.046(2) 0.0202(19) 0.026(2) 0.010(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 Rh1 S1 2.2654(7) . ? Rh1 S2 2.2860(8) . ? Rh1 Cl1 2.3305(8) . ? Rh1 Cl3 2.3470(8) . ? Rh1 Cl2 2.3562(8) . ? Rh1 Cl4 2.3896(7) . ? Rh2 S3 2.2854(8) . ? Rh2 S4 2.2935(8) . ? Rh2 Cl7 2.3385(9) . ? Rh2 Cl5 2.3467(9) . ? Rh2 Cl8 2.3638(8) . ? Rh2 Cl6 2.3775(8) . ? S1 O1 1.469(2) . ? S1 C12 1.765(3) . ? S1 C11 1.776(3) . ? S2 O2 1.475(2) . ? S2 C22 1.757(3) . ? S2 C21 1.763(3) . ? S3 O3 1.457(2) . ? S3 C31 1.768(4) . ? S3 C32 1.772(4) . ? S4 O4 1.459(2) . ? S4 C41 1.756(4) . ? S4 C42 1.759(4) . ? O5 H5A 0.83(2) . ? O5 H5B 0.83(2) . ? O6 H6A 0.83(2) . ? O6 H6B 0.83(2) . ? O7 H7A 0.83(2) . ? O7 H7B 0.83(2) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? 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 S1 Rh1 S2 89.29(3) . . ? S1 Rh1 Cl1 85.91(3) . . ? S2 Rh1 Cl1 95.38(3) . . ? S1 Rh1 Cl3 95.94(3) . . ? S2 Rh1 Cl3 86.26(3) . . ? Cl1 Rh1 Cl3 177.55(3) . . ? S1 Rh1 Cl2 91.46(3) . . ? S2 Rh1 Cl2 174.85(3) . . ? Cl1 Rh1 Cl2 89.76(3) . . ? Cl3 Rh1 Cl2 88.59(3) . . ? S1 Rh1 Cl4 174.12(3) . . ? S2 Rh1 Cl4 92.15(3) . . ? Cl1 Rh1 Cl4 88.28(3) . . ? Cl3 Rh1 Cl4 89.84(3) . . ? Cl2 Rh1 Cl4 87.63(3) . . ? S3 Rh2 S4 92.44(3) . . ? S3 Rh2 Cl7 91.38(3) . . ? S4 Rh2 Cl7 91.42(3) . . ? S3 Rh2 Cl5 92.08(3) . . ? S4 Rh2 Cl5 88.54(3) . . ? Cl7 Rh2 Cl5 176.54(4) . . ? S3 Rh2 Cl8 87.08(3) . . ? S4 Rh2 Cl8 178.11(3) . . ? Cl7 Rh2 Cl8 90.41(3) . . ? Cl5 Rh2 Cl8 89.65(3) . . ? S3 Rh2 Cl6 175.42(3) . . ? S4 Rh2 Cl6 92.11(3) . . ? Cl7 Rh2 Cl6 87.92(4) . . ? Cl5 Rh2 Cl6 88.62(3) . . ? Cl8 Rh2 Cl6 88.39(3) . . ? O1 S1 C12 108.69(16) . . ? O1 S1 C11 107.95(16) . . ? C12 S1 C11 100.84(18) . . ? O1 S1 Rh1 112.72(10) . . ? C12 S1 Rh1 112.86(11) . . ? C11 S1 Rh1 113.02(12) . . ? O2 S2 C22 107.75(16) . . ? O2 S2 C21 108.19(16) . . ? C22 S2 C21 100.95(19) . . ? O2 S2 Rh1 113.56(10) . . ? C22 S2 Rh1 111.48(13) . . ? C21 S2 Rh1 114.03(13) . . ? O3 S3 C31 108.06(18) . . ? O3 S3 C32 107.5(2) . . ? C31 S3 C32 101.3(2) . . ? O3 S3 Rh2 115.56(11) . . ? C31 S3 Rh2 112.03(13) . . ? C32 S3 Rh2 111.28(14) . . ? O4 S4 C41 107.78(18) . . ? O4 S4 C42 107.27(19) . . ? C41 S4 C42 99.44(18) . . ? O4 S4 Rh2 115.08(10) . . ? C41 S4 Rh2 113.37(13) . . ? C42 S4 Rh2 112.60(13) . . ? H5A O5 H5B 128(5) . . ? H6A O6 H6B 109(5) . . ? H7A O7 H7B 109(5) . . ? S1 C11 H11A 109.5 . . ? S1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? S1 C12 H12A 109.5 . . ? S1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? S2 C21 H21A 109.5 . . ? S2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? S2 C22 H22A 109.5 . . ? S2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? S3 C31 H31A 109.5 . . ? S3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S3 C32 H32A 109.5 . . ? S3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? S4 C41 H41A 109.5 . . ? S4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? S4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? S4 C42 H42A 109.5 . . ? S4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? S4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? 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 S2 Rh1 S1 O1 37.17(12) . . . . ? Cl1 Rh1 S1 O1 -58.27(12) . . . . ? Cl3 Rh1 S1 O1 123.34(12) . . . . ? Cl2 Rh1 S1 O1 -147.93(12) . . . . ? S2 Rh1 S1 C12 -86.44(14) . . . . ? Cl1 Rh1 S1 C12 178.12(14) . . . . ? Cl3 Rh1 S1 C12 -0.27(14) . . . . ? Cl2 Rh1 S1 C12 88.46(14) . . . . ? S2 Rh1 S1 C11 159.93(14) . . . . ? Cl1 Rh1 S1 C11 64.48(14) . . . . ? Cl3 Rh1 S1 C11 -113.91(14) . . . . ? Cl2 Rh1 S1 C11 -25.17(14) . . . . ? S1 Rh1 S2 O2 46.84(11) . . . . ? Cl1 Rh1 S2 O2 132.66(11) . . . . ? Cl3 Rh1 S2 O2 -49.16(11) . . . . ? Cl4 Rh1 S2 O2 -138.86(11) . . . . ? S1 Rh1 S2 C22 168.77(15) . . . . ? Cl1 Rh1 S2 C22 -105.41(15) . . . . ? Cl3 Rh1 S2 C22 72.77(15) . . . . ? Cl4 Rh1 S2 C22 -16.93(15) . . . . ? S1 Rh1 S2 C21 -77.71(15) . . . . ? Cl1 Rh1 S2 C21 8.11(14) . . . . ? Cl3 Rh1 S2 C21 -173.72(14) . . . . ? Cl4 Rh1 S2 C21 96.58(14) . . . . ? S4 Rh2 S3 O3 6.04(15) . . . . ? Cl7 Rh2 S3 O3 -85.44(15) . . . . ? Cl5 Rh2 S3 O3 94.67(15) . . . . ? Cl8 Rh2 S3 O3 -175.78(15) . . . . ? S4 Rh2 S3 C31 -118.32(15) . . . . ? Cl7 Rh2 S3 C31 150.20(15) . . . . ? Cl5 Rh2 S3 C31 -29.69(15) . . . . ? Cl8 Rh2 S3 C31 59.86(15) . . . . ? S4 Rh2 S3 C32 129.07(17) . . . . ? Cl7 Rh2 S3 C32 37.59(17) . . . . ? Cl5 Rh2 S3 C32 -142.30(17) . . . . ? Cl8 Rh2 S3 C32 -52.76(17) . . . . ? S3 Rh2 S4 O4 59.07(16) . . . . ? Cl7 Rh2 S4 O4 150.51(16) . . . . ? Cl5 Rh2 S4 O4 -32.95(16) . . . . ? Cl6 Rh2 S4 O4 -121.52(16) . . . . ? S3 Rh2 S4 C41 -65.65(15) . . . . ? Cl7 Rh2 S4 C41 25.79(15) . . . . ? Cl5 Rh2 S4 C41 -157.67(15) . . . . ? Cl6 Rh2 S4 C41 113.77(15) . . . . ? S3 Rh2 S4 C42 -177.57(16) . . . . ? Cl7 Rh2 S4 C42 -86.13(16) . . . . ? Cl5 Rh2 S4 C42 90.40(16) . . . . ? Cl6 Rh2 S4 C42 1.84(16) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.62 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.723 _refine_diff_density_min -0.723 _refine_diff_density_rms 0.086 #===============================================END data_Compound3 _database_code_depnum_ccdc_archive 'CCDC 835361' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H12 Cl4 K O2.25 Rh S2' _chemical_formula_sum 'C4 H12 Cl4 K O2.25 Rh S2' _chemical_formula_weight 444.09 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7053(3) _cell_length_b 7.82170(10) _cell_length_c 15.2964(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.421(2) _cell_angle_gamma 90.00 _cell_volume 1415.10(5) _cell_formula_units_Z 4 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 8780 _cell_measurement_theta_min 3.78 _cell_measurement_theta_max 25.62 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 2.528 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8752 _exptl_absorpt_correction_T_max 0.9102 _exptl_absorpt_process_details 'X-red (STOE, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(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 'X-calibur-II with Sapphire-III CCD' _diffrn_measurement_method '\w-scans at different \f' _diffrn_detector_area_resol_mean 12 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% . _diffrn_reflns_number 8780 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 25.62 _reflns_number_total 2666 _reflns_number_gt 2272 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_data_reduction 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg, 2001)' _computing_publication_material 'PLATON (Spek, 2009)' _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^)+(0.0368P)^2^+0.9900P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2666 _refine_ls_number_parameters 143 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0666 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.5000 0.5000 0.5000 0.01957(10) Uani 1 2 d S . . Rh2 Rh 0.0000 0.0000 0.5000 0.02513(10) Uani 1 2 d S . . K1 K 0.31472(6) -0.02897(9) 0.46548(6) 0.0411(2) Uani 1 1 d . . . Cl1 Cl 0.46522(7) 0.25130(9) 0.40768(5) 0.03095(18) Uani 1 1 d . . . Cl4 Cl 0.30818(6) 0.56866(10) 0.43643(6) 0.03321(19) Uani 1 1 d . . . Cl2 Cl 0.16152(7) -0.15958(12) 0.58356(6) 0.0427(2) Uani 1 1 d . . . Cl3 Cl 0.11461(8) 0.20997(11) 0.47083(7) 0.0461(2) Uani 1 1 d . . . S2 S 0.52326(7) 0.64562(9) 0.37628(5) 0.02835(18) Uani 1 1 d . . . S1 S 0.00043(7) -0.15092(11) 0.36904(6) 0.0358(2) Uani 1 1 d . . . O2 O 0.5334(2) 0.8320(3) 0.38653(17) 0.0493(7) Uani 1 1 d . . . O1 O 0.0933(2) -0.1087(4) 0.33703(18) 0.0551(7) Uani 1 1 d . . . O3 O 0.2205(13) -0.063(2) 0.2516(10) 0.089(4) Uani 0.25 1 d P . . C3 C 0.4114(3) 0.6016(5) 0.2682(2) 0.0404(8) Uani 1 1 d . . . H7 H 0.3429 0.6530 0.2685 0.061 Uiso 1 1 calc R . . H8 H 0.4012 0.4801 0.2604 0.061 Uiso 1 1 calc R . . H9 H 0.4297 0.6478 0.2173 0.061 Uiso 1 1 calc R . . C4 C 0.6404(3) 0.5663(6) 0.3510(3) 0.0485(9) Uani 1 1 d . . . H10 H 0.6384 0.6127 0.2923 0.073 Uiso 1 1 calc R . . H11 H 0.6364 0.4439 0.3469 0.073 Uiso 1 1 calc R . . H12 H 0.7095 0.5997 0.4001 0.073 Uiso 1 1 calc R . . C1 C -0.1278(3) -0.1252(6) 0.2723(3) 0.0582(11) Uani 1 1 d . . . H1 H -0.1375 -0.0070 0.2541 0.087 Uiso 1 1 calc R . . H2 H -0.1897 -0.1615 0.2896 0.087 Uiso 1 1 calc R . . H3 H -0.1258 -0.1930 0.2206 0.087 Uiso 1 1 calc R . . C2 C 0.0024(4) -0.3757(5) 0.3869(3) 0.0615(12) Uani 1 1 d . . . H4 H 0.0010 -0.4334 0.3311 0.092 Uiso 1 1 calc R . . H5 H -0.0626 -0.4085 0.4008 0.092 Uiso 1 1 calc R . . H6 H 0.0699 -0.4066 0.4385 0.092 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 0.01780(17) 0.02066(16) 0.01816(17) -0.00339(12) 0.00408(13) 0.00046(11) Rh2 0.01881(18) 0.03126(19) 0.02168(19) 0.00209(13) 0.00308(14) 0.00491(13) K1 0.0325(4) 0.0345(4) 0.0515(5) 0.0001(3) 0.0095(4) -0.0013(3) Cl1 0.0391(4) 0.0244(4) 0.0290(4) -0.0085(3) 0.0119(3) -0.0033(3) Cl4 0.0191(4) 0.0422(4) 0.0335(4) -0.0023(3) 0.0039(3) 0.0049(3) Cl2 0.0317(4) 0.0546(5) 0.0336(5) 0.0053(4) 0.0021(4) 0.0194(4) Cl3 0.0429(5) 0.0369(4) 0.0666(6) 0.0020(4) 0.0296(5) -0.0029(4) S2 0.0340(4) 0.0263(4) 0.0225(4) -0.0009(3) 0.0076(3) -0.0049(3) S1 0.0289(4) 0.0478(5) 0.0263(4) -0.0053(4) 0.0048(4) 0.0081(4) O2 0.081(2) 0.0230(12) 0.0367(14) 0.0000(10) 0.0127(14) -0.0111(12) O1 0.0436(15) 0.085(2) 0.0417(16) -0.0105(14) 0.0212(13) 0.0012(14) O3 0.078(9) 0.127(12) 0.073(10) 0.021(9) 0.040(8) 0.010(9) C3 0.044(2) 0.048(2) 0.0216(17) 0.0023(15) 0.0037(15) -0.0036(16) C4 0.041(2) 0.066(2) 0.045(2) 0.004(2) 0.0240(19) -0.0023(19) C1 0.039(2) 0.089(3) 0.032(2) -0.014(2) -0.0049(17) 0.013(2) C2 0.072(3) 0.046(2) 0.065(3) -0.013(2) 0.023(2) 0.011(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 Rh1 S2 2.3184(8) 3_666 ? Rh1 S2 2.3184(8) . ? Rh1 Cl4 2.3329(7) 3_666 ? Rh1 Cl4 2.3329(7) . ? Rh1 Cl1 2.3490(7) 3_666 ? Rh1 Cl1 2.3490(7) . ? Rh2 S1 2.3268(8) . ? Rh2 S1 2.3268(8) 3_556 ? Rh2 Cl2 2.3425(8) . ? Rh2 Cl2 2.3425(8) 3_556 ? Rh2 Cl3 2.3433(8) 3_556 ? Rh2 Cl3 2.3433(8) . ? S2 O2 1.467(2) . ? S2 C3 1.776(3) . ? S2 C4 1.780(4) . ? S1 O1 1.470(3) . ? S1 C1 1.767(4) . ? S1 C2 1.778(4) . ? C3 H7 0.9600 . ? C3 H8 0.9600 . ? C3 H9 0.9600 . ? C4 H10 0.9600 . ? C4 H11 0.9600 . ? C4 H12 0.9600 . ? C1 H1 0.9600 . ? C1 H2 0.9600 . ? C1 H3 0.9600 . ? C2 H4 0.9600 . ? C2 H5 0.9600 . ? C2 H6 0.9600 . ? 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 S2 Rh1 S2 180.0 3_666 . ? S2 Rh1 Cl4 88.39(3) 3_666 3_666 ? S2 Rh1 Cl4 91.61(3) . 3_666 ? S2 Rh1 Cl4 91.61(3) 3_666 . ? S2 Rh1 Cl4 88.39(3) . . ? Cl4 Rh1 Cl4 180.0 3_666 . ? S2 Rh1 Cl1 88.18(3) 3_666 3_666 ? S2 Rh1 Cl1 91.82(3) . 3_666 ? Cl4 Rh1 Cl1 90.09(3) 3_666 3_666 ? Cl4 Rh1 Cl1 89.91(3) . 3_666 ? S2 Rh1 Cl1 91.82(3) 3_666 . ? S2 Rh1 Cl1 88.18(3) . . ? Cl4 Rh1 Cl1 89.91(3) 3_666 . ? Cl4 Rh1 Cl1 90.09(3) . . ? Cl1 Rh1 Cl1 180.0 3_666 . ? S1 Rh2 S1 180.0 . 3_556 ? S1 Rh2 Cl2 85.55(3) . . ? S1 Rh2 Cl2 94.45(3) 3_556 . ? S1 Rh2 Cl2 94.45(3) . 3_556 ? S1 Rh2 Cl2 85.55(3) 3_556 3_556 ? Cl2 Rh2 Cl2 180.00(4) . 3_556 ? S1 Rh2 Cl3 90.31(3) . 3_556 ? S1 Rh2 Cl3 89.69(3) 3_556 3_556 ? Cl2 Rh2 Cl3 90.24(3) . 3_556 ? Cl2 Rh2 Cl3 89.76(3) 3_556 3_556 ? S1 Rh2 Cl3 89.69(3) . . ? S1 Rh2 Cl3 90.31(3) 3_556 . ? Cl2 Rh2 Cl3 89.76(3) . . ? Cl2 Rh2 Cl3 90.24(3) 3_556 . ? Cl3 Rh2 Cl3 180.00(4) 3_556 . ? O2 S2 C3 107.54(16) . . ? O2 S2 C4 108.80(19) . . ? C3 S2 C4 100.25(19) . . ? O2 S2 Rh1 115.67(11) . . ? C3 S2 Rh1 111.55(12) . . ? C4 S2 Rh1 111.85(14) . . ? O1 S1 C1 107.56(19) . . ? O1 S1 C2 107.8(2) . . ? C1 S1 C2 101.4(2) . . ? O1 S1 Rh2 115.29(12) . . ? C1 S1 Rh2 111.83(14) . . ? C2 S1 Rh2 111.95(15) . . ? S2 C3 H7 109.5 . . ? S2 C3 H8 109.5 . . ? H7 C3 H8 109.5 . . ? S2 C3 H9 109.5 . . ? H7 C3 H9 109.5 . . ? H8 C3 H9 109.5 . . ? S2 C4 H10 109.5 . . ? S2 C4 H11 109.5 . . ? H10 C4 H11 109.5 . . ? S2 C4 H12 109.5 . . ? H10 C4 H12 109.5 . . ? H11 C4 H12 109.5 . . ? S1 C1 H1 109.5 . . ? S1 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? S1 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? S1 C2 H4 109.5 . . ? S1 C2 H5 109.5 . . ? H4 C2 H5 109.5 . . ? S1 C2 H6 109.5 . . ? H4 C2 H6 109.5 . . ? H5 C2 H6 109.5 . . ? 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 Cl4 Rh1 S2 O2 -98.61(14) 3_666 . . . ? Cl4 Rh1 S2 O2 81.39(14) . . . . ? Cl1 Rh1 S2 O2 -8.47(14) 3_666 . . . ? Cl1 Rh1 S2 O2 171.53(14) . . . . ? Cl4 Rh1 S2 C3 138.08(14) 3_666 . . . ? Cl4 Rh1 S2 C3 -41.92(14) . . . . ? Cl1 Rh1 S2 C3 -131.78(14) 3_666 . . . ? Cl1 Rh1 S2 C3 48.22(14) . . . . ? Cl4 Rh1 S2 C4 26.70(15) 3_666 . . . ? Cl4 Rh1 S2 C4 -153.30(15) . . . . ? Cl1 Rh1 S2 C4 116.84(15) 3_666 . . . ? Cl1 Rh1 S2 C4 -63.16(15) . . . . ? Cl2 Rh2 S1 O1 -69.55(14) . . . . ? Cl2 Rh2 S1 O1 110.45(14) 3_556 . . . ? Cl3 Rh2 S1 O1 -159.76(14) 3_556 . . . ? Cl3 Rh2 S1 O1 20.24(14) . . . . ? Cl2 Rh2 S1 C1 167.17(19) . . . . ? Cl2 Rh2 S1 C1 -12.83(19) 3_556 . . . ? Cl3 Rh2 S1 C1 76.96(19) 3_556 . . . ? Cl3 Rh2 S1 C1 -103.04(19) . . . . ? Cl2 Rh2 S1 C2 54.11(17) . . . . ? Cl2 Rh2 S1 C2 -125.89(17) 3_556 . . . ? Cl3 Rh2 S1 C2 -36.11(17) 3_556 . . . ? Cl3 Rh2 S1 C2 143.89(17) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.62 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.748 _refine_diff_density_min -1.233 _refine_diff_density_rms 0.092 #=====================================END