# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_718200-718203 _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _audit_creation_date 2008-12-30 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Prof Kiyoshi Isobe' _publ_contact_author_email isobe@cacheibm.s.kanazawa-u.ac.jp _publ_contact_author_fax +81-76-264-5742 _publ_contact_author_phone +81-76-264-5697 _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category ? _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Nakai Hidetaka' . ; Department of Chemistry, Graduate School of Natural Science & Technology, Kanazawa University, Kakuma-machi, Kanazawa 920-1192, Japan ; M.Hatake . ; Department of Chemistry, Graduate School of Natural Science & Technology, Kanazawa University, Kakuma-machi, Kanazawa 920-1192, Japan ; Y.Miyano . ; Department of Chemistry, Graduate School of Natural Science & Technology, Kanazawa University, Kakuma-machi, Kanazawa 920-1192, Japan ; K.Isobe . ; Department of Chemistry, Graduate School of Natural Science & Technology, Kanazawa University, Kakuma-machi, Kanazawa 920-1192, Japan ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2006). CrystalStructure (Version 3.8). Single Crystal Structure Analysis Software. Rigaku/MSC, 9009 TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Sheldrick, G.M. (1997). SHELXL97. University of Gottingen, Germany. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data___(P)-1Pro _database_code_depnum_ccdc_archive 'CCDC 718200' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C26 H42 O4 Rh2 S2 ' _chemical_formula_moiety 'C26 H42 O4 Rh2 S2 ' _chemical_formula_weight 688.55 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2+X,1/2-Y,-Z 3 -X,1/2+Y,1/2-Z 4 1/2-X,-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.0091(11) _cell_length_b 13.4618(18) _cell_length_c 22.202(3) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 2692.6(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8511 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange-brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408.00 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type Empirical _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_T_max 0.845 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 29347 _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6134 _reflns_number_gt 5815 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0878 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6134 _refine_ls_number_parameters 308 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0373P)^2^+1.6021P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.92 _refine_diff_density_min -0.99 _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 -0.01(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Rh Rh -1.118 0.919 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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(1) Rh 0.33077(4) 0.36677(3) 0.365396(16) 0.01305(8) Uani 1.00 1 d . . . Rh(2) Rh 0.28457(4) 0.54045(3) 0.415479(16) 0.01310(8) Uani 1.00 1 d . . . S(1) S 0.57605(13) 0.39228(9) 0.38711(5) 0.0176(2) Uani 1.00 1 d . . . S(2) S 0.53442(13) 0.54695(10) 0.43059(5) 0.0171(2) Uani 1.00 1 d . . . O(1) O 0.6356(4) 0.3253(2) 0.43292(17) 0.0269(8) Uani 1.00 1 d . . . O(2) O 0.6727(4) 0.4068(2) 0.33484(16) 0.0262(8) Uani 1.00 1 d . . . O(3) O 0.5779(3) 0.5417(2) 0.49383(16) 0.0237(7) Uani 1.00 1 d . . . O(4) O 0.6130(3) 0.6227(2) 0.39550(16) 0.0245(8) Uani 1.00 1 d . . . C(1) C 0.1412(5) 0.2541(3) 0.3636(2) 0.0148(9) Uani 1.00 1 d . . . C(2) C 0.2815(5) 0.2067(3) 0.3737(2) 0.0182(9) Uani 1.00 1 d . . . C(3) C 0.3717(5) 0.2229(3) 0.3208(2) 0.0159(10) Uani 1.00 1 d . . . C(4) C 0.2910(5) 0.2834(3) 0.2799(2) 0.0169(10) Uani 1.00 1 d . . . C(5) C 0.1494(5) 0.3025(3) 0.3061(2) 0.0145(9) Uani 1.00 1 d . . . C(6) C 0.0088(5) 0.2447(3) 0.4029(2) 0.0191(10) Uani 1.00 1 d . . . C(7) C 0.3258(6) 0.1462(3) 0.4278(2) 0.0231(11) Uani 1.00 1 d . . . C(8) C 0.5206(5) 0.1790(4) 0.3089(2) 0.0243(11) Uani 1.00 1 d . . . C(9) C 0.3419(6) 0.3131(4) 0.2177(2) 0.0228(11) Uani 1.00 1 d . . . C(10) C 0.0240(5) 0.3594(3) 0.2764(2) 0.0209(10) Uani 1.00 1 d . . . C(11) C -0.0668(6) 0.1416(4) 0.3938(2) 0.0253(11) Uani 1.00 1 d . . . C(12) C -0.0978(6) 0.1155(4) 0.3289(2) 0.0298(12) Uani 1.00 1 d . . . C(13) C 0.2001(5) 0.6936(3) 0.4042(2) 0.0180(10) Uani 1.00 1 d . . . C(14) C 0.0778(5) 0.6277(3) 0.3923(2) 0.0150(9) Uani 1.00 1 d . . . C(15) C 0.0473(5) 0.5705(3) 0.4445(2) 0.0176(10) Uani 1.00 1 d . . . C(16) C 0.1500(5) 0.6020(3) 0.4909(2) 0.0155(9) Uani 1.00 1 d . . . C(17) C 0.2412(5) 0.6793(3) 0.4665(2) 0.0161(10) Uani 1.00 1 d . . . C(18) C 0.2671(5) 0.7682(3) 0.3617(2) 0.0206(10) Uani 1.00 1 d . . . C(19) C -0.0099(5) 0.6255(4) 0.3348(2) 0.0223(11) Uani 1.00 1 d . . . C(20) C -0.0716(5) 0.4955(3) 0.4524(2) 0.0193(10) Uani 1.00 1 d . . . C(21) C 0.1513(6) 0.5672(3) 0.5555(2) 0.0219(11) Uani 1.00 1 d . . . C(22) C 0.3527(6) 0.7371(4) 0.5010(2) 0.0259(12) Uani 1.00 1 d . . . C(23) C 0.1946(5) 0.8710(3) 0.3667(2) 0.0200(9) Uani 1.00 1 d . . . C(24) C 0.2674(6) 0.9441(3) 0.3230(2) 0.0250(11) Uani 1.00 1 d . . . C(25) C 0.3011(5) 0.4017(3) 0.4539(2) 0.0164(10) Uani 1.00 1 d . . . C(26) C 0.3389(6) 0.5063(3) 0.3281(2) 0.0179(10) Uani 1.00 1 d . . . H(1) H -0.0628 0.2981 0.3932 0.023 Uiso 1.00 1 c R . . H(2) H 0.0388 0.2523 0.4455 0.023 Uiso 1.00 1 c R . . H(3) H 0.4249 0.1181 0.4213 0.028 Uiso 1.00 1 c R . . H(4) H 0.2542 0.0923 0.4337 0.028 Uiso 1.00 1 c R . . H(5) H 0.3271 0.1888 0.4636 0.028 Uiso 1.00 1 c R . . H(6) H 0.5558 0.2005 0.2692 0.029 Uiso 1.00 1 c R . . H(7) H 0.5135 0.1064 0.3098 0.029 Uiso 1.00 1 c R . . H(8) H 0.5905 0.2013 0.3399 0.029 Uiso 1.00 1 c R . . H(9) H 0.2655 0.3541 0.1985 0.027 Uiso 1.00 1 c R . . H(10) H 0.3588 0.2533 0.1934 0.027 Uiso 1.00 1 c R . . H(11) H 0.4344 0.3510 0.2207 0.027 Uiso 1.00 1 c R . . H(12) H -0.0619 0.3611 0.3035 0.025 Uiso 1.00 1 c R . . H(13) H -0.0037 0.3265 0.2387 0.025 Uiso 1.00 1 c R . . H(14) H 0.0566 0.4274 0.2679 0.025 Uiso 1.00 1 c R . . H(15) H -0.0020 0.0896 0.4113 0.030 Uiso 1.00 1 c R . . H(16) H -0.1616 0.1408 0.4164 0.030 Uiso 1.00 1 c R . . H(17) H -0.1974 0.1385 0.3179 0.036 Uiso 1.00 1 c R . . H(18) H -0.0917 0.0434 0.3236 0.036 Uiso 1.00 1 c R . . H(19) H -0.0242 0.1479 0.3029 0.036 Uiso 1.00 1 c R . . H(20) H 0.2563 0.7438 0.3199 0.025 Uiso 1.00 1 c R . . H(21) H 0.3745 0.7744 0.3704 0.025 Uiso 1.00 1 c R . . H(22) H 0.0295 0.6754 0.3069 0.027 Uiso 1.00 1 c R . . H(23) H -0.1142 0.6402 0.3435 0.027 Uiso 1.00 1 c R . . H(24) H -0.0021 0.5595 0.3165 0.027 Uiso 1.00 1 c R . . H(25) H -0.1260 0.4876 0.4145 0.023 Uiso 1.00 1 c R . . H(26) H -0.1401 0.5174 0.4840 0.023 Uiso 1.00 1 c R . . H(27) H -0.0273 0.4317 0.4639 0.023 Uiso 1.00 1 c R . . H(28) H 0.0763 0.5152 0.5609 0.026 Uiso 1.00 1 c R . . H(29) H 0.1289 0.6232 0.5822 0.026 Uiso 1.00 1 c R . . H(30) H 0.2495 0.5405 0.5654 0.026 Uiso 1.00 1 c R . . H(31) H 0.3568 0.7125 0.5425 0.031 Uiso 1.00 1 c R . . H(32) H 0.3246 0.8075 0.5011 0.031 Uiso 1.00 1 c R . . H(33) H 0.4504 0.7297 0.4821 0.031 Uiso 1.00 1 c R . . H(34) H 0.0874 0.8656 0.3575 0.024 Uiso 1.00 1 c R . . H(35) H 0.2051 0.8960 0.4084 0.024 Uiso 1.00 1 c R . . H(36) H 0.3506 0.9773 0.3431 0.030 Uiso 1.00 1 c R . . H(37) H 0.1943 0.9937 0.3103 0.030 Uiso 1.00 1 c R . . H(38) H 0.3040 0.9080 0.2876 0.030 Uiso 1.00 1 c R . . H(39) H 0.3888 0.3913 0.4800 0.020 Uiso 1.00 1 c R . . H(40) H 0.2087 0.3759 0.4723 0.020 Uiso 1.00 1 c R . . H(41) H 0.4385 0.5286 0.3149 0.021 Uiso 1.00 1 c R . . H(42) H 0.2611 0.5208 0.2979 0.021 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.01122(17) 0.01392(17) 0.01400(17) 0.00055(15) -0.00008(14) -0.00101(15) Rh(2) 0.01079(17) 0.01328(17) 0.01524(17) -0.00036(14) 0.00018(14) -0.00085(15) S(1) 0.0107(5) 0.0214(6) 0.0208(6) 0.0006(4) -0.0011(4) -0.0042(4) S(2) 0.0106(5) 0.0194(5) 0.0214(6) -0.0004(5) -0.0003(4) -0.0039(5) O(1) 0.023(2) 0.0280(19) 0.029(2) 0.0049(16) -0.0074(15) -0.0033(16) O(2) 0.0151(18) 0.0329(19) 0.0308(19) 0.0001(16) 0.0083(15) -0.0030(16) O(3) 0.0172(18) 0.0271(18) 0.0268(19) 0.0014(17) -0.0051(14) -0.0062(17) O(4) 0.0144(17) 0.0264(19) 0.033(2) -0.0074(15) 0.0034(14) 0.0011(17) C(1) 0.014(2) 0.016(2) 0.015(2) 0.0017(17) 0.0005(19) -0.008(2) C(2) 0.020(2) 0.013(2) 0.022(2) 0.0034(19) 0.000(2) -0.004(2) C(3) 0.015(2) 0.014(2) 0.018(2) -0.0033(18) 0.0002(18) -0.004(2) C(4) 0.016(2) 0.022(2) 0.013(2) -0.005(2) 0.0041(18) -0.0063(19) C(5) 0.015(2) 0.014(2) 0.015(2) -0.0065(18) -0.0016(18) -0.0005(19) C(6) 0.018(2) 0.024(2) 0.015(2) -0.006(2) 0.0014(19) -0.005(2) C(7) 0.023(2) 0.019(2) 0.027(2) 0.003(2) -0.004(2) 0.001(2) C(8) 0.017(2) 0.024(2) 0.032(3) -0.001(2) 0.002(2) -0.010(2) C(9) 0.023(2) 0.026(2) 0.020(2) -0.010(2) 0.003(2) -0.002(2) C(10) 0.017(2) 0.020(2) 0.025(2) 0.003(2) -0.000(2) 0.001(2) C(11) 0.024(2) 0.027(2) 0.025(2) -0.015(2) 0.010(2) -0.004(2) C(12) 0.025(2) 0.033(3) 0.032(3) -0.005(2) 0.002(2) -0.003(2) C(13) 0.016(2) 0.010(2) 0.028(2) -0.0008(18) 0.004(2) -0.0043(19) C(14) 0.018(2) 0.010(2) 0.018(2) 0.003(2) -0.0005(18) -0.0010(19) C(15) 0.011(2) 0.016(2) 0.026(2) 0.0065(18) 0.0047(19) -0.001(2) C(16) 0.016(2) 0.015(2) 0.016(2) 0.0024(19) -0.0001(18) -0.0031(18) C(17) 0.014(2) 0.013(2) 0.022(2) 0.0004(18) 0.0027(19) -0.0030(19) C(18) 0.019(2) 0.022(2) 0.021(2) -0.003(2) 0.005(2) -0.007(2) C(19) 0.016(2) 0.027(2) 0.024(2) 0.003(2) -0.001(2) 0.002(2) C(20) 0.013(2) 0.022(2) 0.023(2) -0.000(2) -0.002(2) 0.002(2) C(21) 0.027(2) 0.018(2) 0.020(2) 0.004(2) 0.002(2) -0.002(2) C(22) 0.022(2) 0.026(2) 0.030(2) 0.001(2) 0.000(2) -0.007(2) C(23) 0.024(2) 0.015(2) 0.021(2) -0.002(2) 0.001(2) -0.001(2) C(24) 0.029(2) 0.021(2) 0.025(2) -0.001(2) -0.004(2) 0.004(2) C(25) 0.024(2) 0.015(2) 0.011(2) 0.001(2) 0.0011(19) -0.0009(18) C(26) 0.024(2) 0.015(2) 0.015(2) -0.005(2) 0.004(2) -0.0006(19) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rh(1) Rh(2) 2.6222(5) yes . . Rh(1) S(1) 2.2877(12) yes . . Rh(1) C(1) 2.285(4) yes . . Rh(1) C(2) 2.208(4) yes . . Rh(1) C(3) 2.206(4) yes . . Rh(1) C(4) 2.234(4) yes . . Rh(1) C(5) 2.269(4) yes . . Rh(1) C(25) 2.038(4) yes . . Rh(1) C(26) 2.054(4) yes . . Rh(2) S(2) 2.2775(12) yes . . Rh(2) C(13) 2.212(4) yes . . Rh(2) C(14) 2.262(4) yes . . Rh(2) C(15) 2.269(4) yes . . Rh(2) C(16) 2.226(4) yes . . Rh(2) C(17) 2.220(4) yes . . Rh(2) C(25) 2.059(4) yes . . Rh(2) C(26) 2.052(4) yes . . S(1) S(2) 2.3255(17) yes . . S(1) O(1) 1.461(3) yes . . S(1) O(2) 1.464(3) yes . . S(2) O(3) 1.459(3) yes . . S(2) O(4) 1.466(3) yes . . C(1) C(2) 1.434(6) yes . . C(1) C(5) 1.434(6) yes . . C(1) C(6) 1.483(6) yes . . C(2) C(3) 1.445(6) yes . . C(2) C(7) 1.505(6) yes . . C(3) C(4) 1.420(6) yes . . C(3) C(8) 1.489(7) yes . . C(4) C(5) 1.426(6) yes . . C(4) C(9) 1.510(6) yes . . C(5) C(10) 1.516(6) yes . . C(6) C(11) 1.559(7) yes . . C(11) C(12) 1.510(7) yes . . C(13) C(14) 1.438(6) yes . . C(13) C(17) 1.446(7) yes . . C(13) C(18) 1.504(6) yes . . C(14) C(15) 1.419(6) yes . . C(14) C(19) 1.502(6) yes . . C(15) C(16) 1.447(6) yes . . C(15) C(20) 1.483(6) yes . . C(16) C(17) 1.432(6) yes . . C(16) C(21) 1.510(6) yes . . C(17) C(22) 1.484(7) yes . . C(18) C(23) 1.533(6) yes . . C(23) C(24) 1.530(7) yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Rh(2) Rh(1) S(1) 85.99(3) yes . . . Rh(2) Rh(1) C(1) 118.74(11) yes . . . Rh(2) Rh(1) C(2) 143.42(13) yes . . . Rh(2) Rh(1) C(3) 178.31(12) yes . . . Rh(2) Rh(1) C(4) 141.52(12) yes . . . Rh(2) Rh(1) C(5) 118.13(11) yes . . . Rh(2) Rh(1) C(25) 50.57(12) yes . . . Rh(2) Rh(1) C(26) 50.28(13) yes . . . S(1) Rh(1) C(1) 145.64(11) yes . . . S(1) Rh(1) C(2) 108.84(13) yes . . . S(1) Rh(1) C(3) 93.72(12) yes . . . S(1) Rh(1) C(4) 114.17(13) yes . . . S(1) Rh(1) C(5) 151.04(12) yes . . . S(1) Rh(1) C(25) 83.62(14) yes . . . S(1) Rh(1) C(26) 85.02(16) yes . . . C(1) Rh(1) C(2) 37.18(17) yes . . . C(1) Rh(1) C(3) 62.24(17) yes . . . C(1) Rh(1) C(4) 62.06(17) yes . . . C(1) Rh(1) C(5) 36.71(16) yes . . . C(1) Rh(1) C(25) 94.12(18) yes . . . C(1) Rh(1) C(26) 128.82(19) yes . . . C(2) Rh(1) C(3) 38.20(18) yes . . . C(2) Rh(1) C(4) 63.13(17) yes . . . C(2) Rh(1) C(5) 62.06(17) yes . . . C(2) Rh(1) C(25) 96.79(17) yes . . . C(2) Rh(1) C(26) 158.98(18) yes . . . C(3) Rh(1) C(4) 37.29(17) yes . . . C(3) Rh(1) C(5) 61.68(17) yes . . . C(3) Rh(1) C(25) 131.06(17) yes . . . C(3) Rh(1) C(26) 128.04(18) yes . . . C(4) Rh(1) C(5) 36.90(17) yes . . . C(4) Rh(1) C(25) 156.05(18) yes . . . C(4) Rh(1) C(26) 97.08(17) yes . . . C(5) Rh(1) C(25) 123.53(18) yes . . . C(5) Rh(1) C(26) 98.11(18) yes . . . C(25) Rh(1) C(26) 100.50(18) yes . . . Rh(1) Rh(2) S(2) 86.55(3) yes . . . Rh(1) Rh(2) C(13) 146.88(13) yes . . . Rh(1) Rh(2) C(14) 119.83(11) yes . . . Rh(1) Rh(2) C(15) 115.41(12) yes . . . Rh(1) Rh(2) C(16) 137.47(12) yes . . . Rh(1) Rh(2) C(17) 174.21(12) yes . . . Rh(1) Rh(2) C(25) 49.86(12) yes . . . Rh(1) Rh(2) C(26) 50.34(12) yes . . . S(2) Rh(2) C(13) 108.72(13) yes . . . S(2) Rh(2) C(14) 145.84(12) yes . . . S(2) Rh(2) C(15) 151.93(13) yes . . . S(2) Rh(2) C(16) 114.40(12) yes . . . S(2) Rh(2) C(17) 93.81(12) yes . . . S(2) Rh(2) C(25) 84.40(14) yes . . . S(2) Rh(2) C(26) 84.96(15) yes . . . C(13) Rh(2) C(14) 37.49(17) yes . . . C(13) Rh(2) C(15) 62.74(17) yes . . . C(13) Rh(2) C(16) 63.34(17) yes . . . C(13) Rh(2) C(17) 38.07(18) yes . . . C(13) Rh(2) C(25) 156.57(18) yes . . . C(13) Rh(2) C(26) 100.57(18) yes . . . C(14) Rh(2) C(15) 36.51(17) yes . . . C(14) Rh(2) C(16) 61.93(16) yes . . . C(14) Rh(2) C(17) 62.21(17) yes . . . C(14) Rh(2) C(25) 128.70(18) yes . . . C(14) Rh(2) C(26) 95.60(18) yes . . . C(15) Rh(2) C(16) 37.54(17) yes . . . C(15) Rh(2) C(17) 62.55(17) yes . . . C(15) Rh(2) C(25) 96.44(18) yes . . . C(15) Rh(2) C(26) 122.2(2) yes . . . C(16) Rh(2) C(17) 37.57(17) yes . . . C(16) Rh(2) C(25) 93.75(17) yes . . . C(16) Rh(2) C(26) 157.45(19) yes . . . C(17) Rh(2) C(25) 124.41(17) yes . . . C(17) Rh(2) C(26) 135.45(17) yes . . . C(25) Rh(2) C(26) 99.85(18) yes . . . Rh(1) S(1) S(2) 93.79(5) yes . . . Rh(1) S(1) O(1) 114.14(16) yes . . . Rh(1) S(1) O(2) 115.31(15) yes . . . S(2) S(1) O(1) 108.81(16) yes . . . S(2) S(1) O(2) 107.77(16) yes . . . O(1) S(1) O(2) 114.6(2) yes . . . Rh(2) S(2) S(1) 93.66(5) yes . . . Rh(2) S(2) O(3) 113.90(14) yes . . . Rh(2) S(2) O(4) 115.21(15) yes . . . S(1) S(2) O(3) 108.23(16) yes . . . S(1) S(2) O(4) 108.93(15) yes . . . O(3) S(2) O(4) 114.5(2) yes . . . Rh(1) C(1) C(2) 68.5(2) yes . . . Rh(1) C(1) C(5) 71.1(2) yes . . . Rh(1) C(1) C(6) 130.3(3) yes . . . C(2) C(1) C(5) 107.2(4) yes . . . C(2) C(1) C(6) 125.4(4) yes . . . C(5) C(1) C(6) 127.1(4) yes . . . Rh(1) C(2) C(1) 74.3(2) yes . . . Rh(1) C(2) C(3) 70.8(2) yes . . . Rh(1) C(2) C(7) 122.8(3) yes . . . C(1) C(2) C(3) 107.6(4) yes . . . C(1) C(2) C(7) 126.8(4) yes . . . C(3) C(2) C(7) 125.6(4) yes . . . Rh(1) C(3) C(2) 71.0(2) yes . . . Rh(1) C(3) C(4) 72.4(2) yes . . . Rh(1) C(3) C(8) 125.3(3) yes . . . C(2) C(3) C(4) 108.6(4) yes . . . C(2) C(3) C(8) 126.2(4) yes . . . C(4) C(3) C(8) 125.1(4) yes . . . Rh(1) C(4) C(3) 70.3(2) yes . . . Rh(1) C(4) C(5) 72.9(2) yes . . . Rh(1) C(4) C(9) 126.6(3) yes . . . C(3) C(4) C(5) 107.5(4) yes . . . C(3) C(4) C(9) 125.5(4) yes . . . C(5) C(4) C(9) 126.7(4) yes . . . Rh(1) C(5) C(1) 72.2(2) yes . . . Rh(1) C(5) C(4) 70.2(2) yes . . . Rh(1) C(5) C(10) 126.6(3) yes . . . C(1) C(5) C(4) 109.1(4) yes . . . C(1) C(5) C(10) 125.3(4) yes . . . C(4) C(5) C(10) 125.5(4) yes . . . C(1) C(6) C(11) 110.5(4) yes . . . C(6) C(11) C(12) 114.2(4) yes . . . Rh(2) C(13) C(14) 73.1(2) yes . . . Rh(2) C(13) C(17) 71.3(2) yes . . . Rh(2) C(13) C(18) 123.8(3) yes . . . C(14) C(13) C(17) 106.8(4) yes . . . C(14) C(13) C(18) 127.2(4) yes . . . C(17) C(13) C(18) 125.9(4) yes . . . Rh(2) C(14) C(13) 69.4(2) yes . . . Rh(2) C(14) C(15) 72.0(2) yes . . . Rh(2) C(14) C(19) 128.1(3) yes . . . C(13) C(14) C(15) 109.5(4) yes . . . C(13) C(14) C(19) 124.8(4) yes . . . C(15) C(14) C(19) 125.6(4) yes . . . Rh(2) C(15) C(14) 71.5(2) yes . . . Rh(2) C(15) C(16) 69.6(2) yes . . . Rh(2) C(15) C(20) 126.3(3) yes . . . C(14) C(15) C(16) 107.3(4) yes . . . C(14) C(15) C(20) 127.3(4) yes . . . C(16) C(15) C(20) 125.3(4) yes . . . Rh(2) C(16) C(15) 72.8(2) yes . . . Rh(2) C(16) C(17) 71.0(2) yes . . . Rh(2) C(16) C(21) 126.5(3) yes . . . C(15) C(16) C(17) 108.1(4) yes . . . C(15) C(16) C(21) 126.1(4) yes . . . C(17) C(16) C(21) 125.5(4) yes . . . Rh(2) C(17) C(13) 70.6(2) yes . . . Rh(2) C(17) C(16) 71.4(2) yes . . . Rh(2) C(17) C(22) 125.9(3) yes . . . C(13) C(17) C(16) 108.1(4) yes . . . C(13) C(17) C(22) 126.7(4) yes . . . C(16) C(17) C(22) 125.1(4) yes . . . C(13) C(18) C(23) 112.7(4) yes . . . C(18) C(23) C(24) 110.6(4) yes . . . Rh(1) C(25) Rh(2) 79.58(15) yes . . . Rh(1) C(26) Rh(2) 79.38(16) yes . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(1) C(6) 3.595(6) ? . 1_655 O(1) C(7) 3.556(6) ? . 2_556 O(1) C(20) 3.520(6) ? . 1_655 O(2) C(10) 3.479(6) ? . 1_655 O(2) C(24) 3.581(6) ? . 3_645 O(3) C(20) 3.347(6) ? . 1_655 O(3) C(23) 3.474(6) ? . 2_566 O(4) C(20) 3.550(6) ? . 1_655 C(6) O(1) 3.595(6) ? . 1_455 C(7) O(1) 3.556(6) ? . 2_456 C(7) C(20) 3.401(7) ? . 2_556 C(8) C(12) 3.570(7) ? . 1_655 C(10) O(2) 3.479(6) ? . 1_455 C(12) C(8) 3.570(7) ? . 1_455 C(15) C(22) 3.353(7) ? . 2_466 C(16) C(22) 3.449(7) ? . 2_466 C(20) O(1) 3.520(6) ? . 1_455 C(20) O(3) 3.347(6) ? . 1_455 C(20) O(4) 3.550(6) ? . 1_455 C(20) C(7) 3.401(7) ? . 2_456 C(22) C(15) 3.353(7) ? . 2_566 C(22) C(16) 3.449(7) ? . 2_566 C(23) O(3) 3.474(6) ? . 2_466 C(24) O(2) 3.581(6) ? . 3_655 #============================================================================== data___(M)-1Pro _database_code_depnum_ccdc_archive 'CCDC 718201' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C26 H42 O4 Rh2 S2 ' _chemical_formula_moiety 'C26 H42 O4 Rh2 S2 ' _chemical_formula_weight 688.55 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2+X,1/2-Y,-Z 3 -X,1/2+Y,1/2-Z 4 1/2-X,-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.0049(7) _cell_length_b 13.4615(11) _cell_length_c 22.2113(18) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 2692.4(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8866 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408.00 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type Empirical _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.759 _exptl_absorpt_correction_T_max 0.869 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 29815 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6122 _reflns_number_gt 5619 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0664 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6122 _refine_ls_number_parameters 308 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0274P)^2^+0.6413P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.65 _refine_diff_density_min -0.57 _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 -0.02(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Rh Rh -1.118 0.919 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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(1) Rh 0.78486(3) 0.45957(2) 0.415481(14) 0.01120(7) Uani 1.00 1 d . . . Rh(2) Rh 0.83108(3) 0.63326(2) 0.365377(14) 0.01106(7) Uani 1.00 1 d . . . S(1) S 1.03520(11) 0.45289(8) 0.43062(5) 0.0153(2) Uani 1.00 1 d . . . S(2) S 1.07671(11) 0.60769(7) 0.38719(5) 0.0160(2) Uani 1.00 1 d . . . O(1) O 1.0791(3) 0.4587(2) 0.49373(13) 0.0211(6) Uani 1.00 1 d . . . O(2) O 1.1139(3) 0.3775(2) 0.39562(13) 0.0232(6) Uani 1.00 1 d . . . O(3) O 1.1363(3) 0.6742(2) 0.43315(13) 0.0228(7) Uani 1.00 1 d . . . O(4) O 1.1739(3) 0.5932(2) 0.33461(13) 0.0230(6) Uani 1.00 1 d . . . C(1) C 0.6997(4) 0.3064(2) 0.40456(18) 0.0150(8) Uani 1.00 1 d . . . C(2) C 0.5770(4) 0.3717(3) 0.39245(17) 0.0132(8) Uani 1.00 1 d . . . C(3) C 0.5489(4) 0.4302(2) 0.44466(19) 0.0145(9) Uani 1.00 1 d . . . C(4) C 0.6501(4) 0.3982(2) 0.49091(18) 0.0140(8) Uani 1.00 1 d . . . C(5) C 0.7414(4) 0.3211(2) 0.46674(19) 0.0156(8) Uani 1.00 1 d . . . C(6) C 0.7662(4) 0.2323(2) 0.36204(19) 0.0192(8) Uani 1.00 1 d . . . C(7) C 0.4898(4) 0.3748(3) 0.33483(19) 0.0211(9) Uani 1.00 1 d . . . C(8) C 0.4286(4) 0.5041(2) 0.4526(2) 0.0182(9) Uani 1.00 1 d . . . C(9) C 0.6509(5) 0.4330(3) 0.55548(18) 0.0206(9) Uani 1.00 1 d . . . C(10) C 0.8523(4) 0.2627(3) 0.5010(2) 0.0225(10) Uani 1.00 1 d . . . C(11) C 0.6938(4) 0.1289(2) 0.36670(19) 0.0199(8) Uani 1.00 1 d . . . C(12) C 0.7664(5) 0.0563(2) 0.32319(19) 0.0229(9) Uani 1.00 1 d . . . C(13) C 0.6424(4) 0.7453(2) 0.36358(18) 0.0132(8) Uani 1.00 1 d . . . C(14) C 0.6492(4) 0.6973(2) 0.30570(17) 0.0111(8) Uani 1.00 1 d . . . C(15) C 0.7917(4) 0.7163(2) 0.27956(17) 0.0148(8) Uani 1.00 1 d . . . C(16) C 0.8714(4) 0.7775(3) 0.32060(19) 0.0149(9) Uani 1.00 1 d . . . C(17) C 0.7817(4) 0.7934(2) 0.37340(18) 0.0143(8) Uani 1.00 1 d . . . C(18) C 0.5093(4) 0.7563(3) 0.40303(19) 0.0171(9) Uani 1.00 1 d . . . C(19) C 0.5244(4) 0.6413(3) 0.27652(18) 0.0181(9) Uani 1.00 1 d . . . C(20) C 0.8413(5) 0.6859(3) 0.21805(19) 0.0230(9) Uani 1.00 1 d . . . C(21) C 1.0227(4) 0.8211(3) 0.3092(2) 0.0230(10) Uani 1.00 1 d . . . C(22) C 0.8270(4) 0.8540(2) 0.42729(18) 0.0205(9) Uani 1.00 1 d . . . C(23) C 0.4334(4) 0.8585(3) 0.39378(19) 0.0235(9) Uani 1.00 1 d . . . C(24) C 0.4021(5) 0.8851(3) 0.3289(2) 0.0274(10) Uani 1.00 1 d . . . C(25) C 0.8020(4) 0.5975(2) 0.45422(17) 0.0139(8) Uani 1.00 1 d . . . C(26) C 0.8409(4) 0.4938(2) 0.32823(17) 0.0146(8) Uani 1.00 1 d . . . H(1) H 0.8737 0.2261 0.3706 0.023 Uiso 1.00 1 c R . . H(2) H 0.7552 0.2571 0.3203 0.023 Uiso 1.00 1 c R . . H(3) H 0.4121 0.4255 0.3379 0.025 Uiso 1.00 1 c R . . H(4) H 0.4441 0.3098 0.3277 0.025 Uiso 1.00 1 c R . . H(5) H 0.5563 0.3911 0.3013 0.025 Uiso 1.00 1 c R . . H(6) H 0.4299 0.5291 0.4941 0.022 Uiso 1.00 1 c R . . H(7) H 0.3325 0.4727 0.4444 0.022 Uiso 1.00 1 c R . . H(8) H 0.4438 0.5595 0.4247 0.022 Uiso 1.00 1 c R . . H(9) H 0.7259 0.3958 0.5782 0.025 Uiso 1.00 1 c R . . H(10) H 0.5529 0.4218 0.5734 0.025 Uiso 1.00 1 c R . . H(11) H 0.6745 0.5041 0.5568 0.025 Uiso 1.00 1 c R . . H(12) H 0.8969 0.2127 0.4746 0.027 Uiso 1.00 1 c R . . H(13) H 0.8034 0.2298 0.5350 0.027 Uiso 1.00 1 c R . . H(14) H 0.9300 0.3072 0.5162 0.027 Uiso 1.00 1 c R . . H(15) H 0.7040 0.1037 0.4084 0.024 Uiso 1.00 1 c R . . H(16) H 0.5866 0.1343 0.3574 0.024 Uiso 1.00 1 c R . . H(17) H 0.7144 0.0585 0.2844 0.028 Uiso 1.00 1 c R . . H(18) H 0.7607 -0.0111 0.3398 0.028 Uiso 1.00 1 c R . . H(19) H 0.8707 0.0747 0.3173 0.028 Uiso 1.00 1 c R . . H(20) H 0.5396 0.7494 0.4457 0.021 Uiso 1.00 1 c R . . H(21) H 0.4375 0.7027 0.3939 0.021 Uiso 1.00 1 c R . . H(22) H 0.5560 0.6179 0.2367 0.022 Uiso 1.00 1 c R . . H(23) H 0.4382 0.6851 0.2721 0.022 Uiso 1.00 1 c R . . H(24) H 0.4975 0.5842 0.3016 0.022 Uiso 1.00 1 c R . . H(25) H 0.9402 0.7134 0.2101 0.028 Uiso 1.00 1 c R . . H(26) H 0.7710 0.7111 0.1880 0.028 Uiso 1.00 1 c R . . H(27) H 0.8454 0.6133 0.2157 0.028 Uiso 1.00 1 c R . . H(28) H 1.0520 0.8623 0.3436 0.028 Uiso 1.00 1 c R . . H(29) H 1.0198 0.8620 0.2728 0.028 Uiso 1.00 1 c R . . H(30) H 1.0950 0.7673 0.3039 0.028 Uiso 1.00 1 c R . . H(31) H 0.7474 0.8527 0.4573 0.025 Uiso 1.00 1 c R . . H(32) H 0.8454 0.9228 0.4149 0.025 Uiso 1.00 1 c R . . H(33) H 0.9178 0.8261 0.4448 0.025 Uiso 1.00 1 c R . . H(34) H 0.3385 0.8589 0.4163 0.028 Uiso 1.00 1 c R . . H(35) H 0.4977 0.9106 0.4114 0.028 Uiso 1.00 1 c R . . H(36) H 0.4885 0.9193 0.3118 0.033 Uiso 1.00 1 c R . . H(37) H 0.3153 0.9290 0.3270 0.033 Uiso 1.00 1 c R . . H(38) H 0.3823 0.8244 0.3059 0.033 Uiso 1.00 1 c R . . H(39) H 0.7097 0.6231 0.4728 0.017 Uiso 1.00 1 c R . . H(40) H 0.8900 0.6075 0.4802 0.017 Uiso 1.00 1 c R . . H(41) H 0.9409 0.4718 0.3154 0.018 Uiso 1.00 1 c R . . H(42) H 0.7638 0.4790 0.2977 0.018 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.00919(15) 0.01185(14) 0.01256(15) -0.00008(12) 0.00039(12) 0.00080(13) Rh(2) 0.01012(15) 0.01204(14) 0.01101(15) -0.00056(13) 0.00026(12) 0.00085(13) S(1) 0.0098(4) 0.0177(5) 0.0184(5) 0.0004(4) 0.0001(3) 0.0029(4) S(2) 0.0098(4) 0.0201(5) 0.0182(5) -0.0016(4) -0.0009(4) 0.0040(4) O(1) 0.0145(14) 0.0272(15) 0.0217(16) 0.0005(14) -0.0056(12) 0.0098(14) O(2) 0.0161(14) 0.0243(16) 0.0292(17) 0.0054(13) 0.0047(12) 0.0016(14) O(3) 0.0168(16) 0.0260(15) 0.0256(18) -0.0037(12) -0.0057(12) 0.0010(13) O(4) 0.0105(14) 0.0346(16) 0.0237(16) -0.0018(13) 0.0057(12) 0.0055(13) C(1) 0.012(2) 0.0134(18) 0.020(2) -0.0028(16) 0.0031(17) 0.0024(16) C(2) 0.0136(19) 0.0117(19) 0.014(2) -0.0050(18) 0.0004(15) 0.0004(17) C(3) 0.0085(19) 0.012(2) 0.023(2) -0.0045(15) 0.0058(16) -0.0007(17) C(4) 0.014(2) 0.0142(19) 0.014(2) -0.0072(16) 0.0023(16) 0.0037(16) C(5) 0.013(2) 0.0152(19) 0.019(2) -0.0027(16) 0.0006(16) 0.0049(16) C(6) 0.024(2) 0.0166(19) 0.017(2) 0.0019(17) 0.0045(19) 0.0049(18) C(7) 0.021(2) 0.020(2) 0.023(2) -0.0009(19) -0.0014(18) -0.003(2) C(8) 0.014(2) 0.017(2) 0.024(2) 0.0009(17) 0.0038(18) -0.0029(18) C(9) 0.028(2) 0.019(2) 0.015(2) -0.0058(18) 0.0020(19) -0.0000(17) C(10) 0.021(2) 0.024(2) 0.022(2) -0.0013(19) -0.0027(19) 0.0063(19) C(11) 0.023(2) 0.0116(18) 0.025(2) -0.0029(18) 0.0021(19) -0.0007(19) C(12) 0.027(2) 0.016(2) 0.025(2) -0.0026(19) -0.0016(19) -0.0024(18) C(13) 0.017(2) 0.0106(18) 0.0119(19) -0.0003(15) -0.0008(17) 0.0096(16) C(14) 0.015(2) 0.0081(17) 0.0101(19) 0.0039(15) -0.0010(15) 0.0031(15) C(15) 0.016(2) 0.021(2) 0.0081(19) 0.0076(17) -0.0008(16) 0.0056(16) C(16) 0.014(2) 0.014(2) 0.017(2) -0.0008(16) -0.0002(16) 0.0046(17) C(17) 0.0150(19) 0.0095(17) 0.018(2) 0.0010(16) -0.0000(17) 0.0027(16) C(18) 0.015(2) 0.019(2) 0.018(2) 0.0046(16) 0.0015(17) 0.0023(17) C(19) 0.017(2) 0.022(2) 0.015(2) 0.0054(19) -0.0034(16) -0.0016(19) C(20) 0.028(2) 0.025(2) 0.017(2) 0.004(2) 0.0074(19) 0.0019(18) C(21) 0.018(2) 0.021(2) 0.031(2) -0.0027(18) 0.0042(19) 0.010(2) C(22) 0.022(2) 0.019(2) 0.021(2) 0.0007(19) -0.0035(18) 0.0002(17) C(23) 0.022(2) 0.027(2) 0.021(2) 0.011(2) 0.0043(17) -0.001(2) C(24) 0.028(2) 0.027(2) 0.027(2) 0.003(2) 0.005(2) 0.009(2) C(25) 0.016(2) 0.0159(18) 0.0101(19) 0.0009(17) 0.0018(16) 0.0035(15) C(26) 0.017(2) 0.0169(19) 0.0100(19) -0.0013(17) 0.0022(17) 0.0034(16) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rh(1) Rh(2) 2.6227(3) yes . . Rh(1) S(1) 2.2810(10) yes . . Rh(1) C(1) 2.213(3) yes . . Rh(1) C(2) 2.272(3) yes . . Rh(1) C(3) 2.256(3) yes . . Rh(1) C(4) 2.228(3) yes . . Rh(1) C(5) 2.219(3) yes . . Rh(1) C(25) 2.052(3) yes . . Rh(1) C(26) 2.055(3) yes . . Rh(2) S(2) 2.2903(10) yes . . Rh(2) C(13) 2.272(3) yes . . Rh(2) C(14) 2.277(3) yes . . Rh(2) C(15) 2.238(3) yes . . Rh(2) C(16) 2.212(4) yes . . Rh(2) C(17) 2.209(3) yes . . Rh(2) C(25) 2.048(3) yes . . Rh(2) C(26) 2.053(3) yes . . S(1) S(2) 2.3265(14) yes . . S(1) O(1) 1.458(3) yes . . S(1) O(2) 1.461(3) yes . . S(2) O(3) 1.460(3) yes . . S(2) O(4) 1.472(3) yes . . C(1) C(2) 1.437(5) yes . . C(1) C(5) 1.445(5) yes . . C(1) C(6) 1.499(5) yes . . C(2) C(3) 1.424(5) yes . . C(2) C(7) 1.502(5) yes . . C(3) C(4) 1.439(5) yes . . C(3) C(8) 1.482(5) yes . . C(4) C(5) 1.428(5) yes . . C(4) C(9) 1.509(5) yes . . C(5) C(10) 1.482(5) yes . . C(6) C(11) 1.540(5) yes . . C(11) C(12) 1.522(5) yes . . C(13) C(14) 1.440(5) yes . . C(13) C(17) 1.429(5) yes . . C(13) C(18) 1.492(5) yes . . C(14) C(15) 1.432(5) yes . . C(14) C(19) 1.501(5) yes . . C(15) C(16) 1.423(5) yes . . C(15) C(20) 1.495(5) yes . . C(16) C(17) 1.440(5) yes . . C(16) C(21) 1.505(5) yes . . C(17) C(22) 1.505(5) yes . . C(18) C(23) 1.550(6) yes . . C(23) C(24) 1.511(6) yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Rh(2) Rh(1) S(1) 86.61(2) yes . . . Rh(2) Rh(1) C(1) 147.04(10) yes . . . Rh(2) Rh(1) C(2) 119.94(10) yes . . . Rh(2) Rh(1) C(3) 115.31(9) yes . . . Rh(2) Rh(1) C(4) 137.42(9) yes . . . Rh(2) Rh(1) C(5) 174.02(10) yes . . . Rh(2) Rh(1) C(25) 50.17(10) yes . . . Rh(2) Rh(1) C(26) 50.29(10) yes . . . S(1) Rh(1) C(1) 108.77(10) yes . . . S(1) Rh(1) C(2) 145.76(10) yes . . . S(1) Rh(1) C(3) 151.81(10) yes . . . S(1) Rh(1) C(4) 114.39(10) yes . . . S(1) Rh(1) C(5) 93.77(10) yes . . . S(1) Rh(1) C(25) 84.24(11) yes . . . S(1) Rh(1) C(26) 84.56(12) yes . . . C(1) Rh(1) C(2) 37.36(14) yes . . . C(1) Rh(1) C(3) 62.75(13) yes . . . C(1) Rh(1) C(4) 63.13(14) yes . . . C(1) Rh(1) C(5) 38.05(14) yes . . . C(1) Rh(1) C(25) 156.18(14) yes . . . C(1) Rh(1) C(26) 100.98(14) yes . . . C(2) Rh(1) C(3) 36.66(14) yes . . . C(2) Rh(1) C(4) 61.80(13) yes . . . C(2) Rh(1) C(5) 62.16(14) yes . . . C(2) Rh(1) C(25) 128.84(15) yes . . . C(2) Rh(1) C(26) 96.11(15) yes . . . C(3) Rh(1) C(4) 37.44(14) yes . . . C(3) Rh(1) C(5) 62.56(14) yes . . . C(3) Rh(1) C(25) 96.24(14) yes . . . C(3) Rh(1) C(26) 122.78(16) yes . . . C(4) Rh(1) C(5) 37.46(14) yes . . . C(4) Rh(1) C(25) 93.51(14) yes . . . C(4) Rh(1) C(26) 157.85(15) yes . . . C(5) Rh(1) C(25) 123.91(14) yes . . . C(5) Rh(1) C(26) 135.69(14) yes . . . C(25) Rh(1) C(26) 100.04(14) yes . . . Rh(1) Rh(2) S(2) 85.96(2) yes . . . Rh(1) Rh(2) C(13) 118.72(9) yes . . . Rh(1) Rh(2) C(14) 118.07(9) yes . . . Rh(1) Rh(2) C(15) 141.42(10) yes . . . Rh(1) Rh(2) C(16) 178.32(10) yes . . . Rh(1) Rh(2) C(17) 143.52(10) yes . . . Rh(1) Rh(2) C(25) 50.29(9) yes . . . Rh(1) Rh(2) C(26) 50.35(10) yes . . . S(2) Rh(2) C(13) 145.65(9) yes . . . S(2) Rh(2) C(14) 151.03(10) yes . . . S(2) Rh(2) C(15) 114.09(10) yes . . . S(2) Rh(2) C(16) 93.92(10) yes . . . S(2) Rh(2) C(17) 108.91(10) yes . . . S(2) Rh(2) C(25) 83.36(11) yes . . . S(2) Rh(2) C(26) 84.61(12) yes . . . C(13) Rh(2) C(14) 36.91(13) yes . . . C(13) Rh(2) C(15) 62.29(14) yes . . . C(13) Rh(2) C(16) 62.11(13) yes . . . C(13) Rh(2) C(17) 37.15(13) yes . . . C(13) Rh(2) C(25) 94.44(14) yes . . . C(13) Rh(2) C(26) 129.21(15) yes . . . C(14) Rh(2) C(15) 36.96(14) yes . . . C(14) Rh(2) C(16) 61.57(13) yes . . . C(14) Rh(2) C(17) 62.12(13) yes . . . C(14) Rh(2) C(25) 123.92(14) yes . . . C(14) Rh(2) C(26) 98.25(14) yes . . . C(15) Rh(2) C(16) 37.29(14) yes . . . C(15) Rh(2) C(17) 63.20(14) yes . . . C(15) Rh(2) C(25) 156.61(14) yes . . . C(15) Rh(2) C(26) 96.98(14) yes . . . C(16) Rh(2) C(17) 38.03(14) yes . . . C(16) Rh(2) C(25) 131.37(14) yes . . . C(16) Rh(2) C(26) 127.97(15) yes . . . C(17) Rh(2) C(25) 97.25(14) yes . . . C(17) Rh(2) C(26) 159.06(15) yes . . . C(25) Rh(2) C(26) 100.22(14) yes . . . Rh(1) S(1) S(2) 93.57(4) yes . . . Rh(1) S(1) O(1) 114.04(12) yes . . . Rh(1) S(1) O(2) 115.34(12) yes . . . S(2) S(1) O(1) 107.90(13) yes . . . S(2) S(1) O(2) 108.87(12) yes . . . O(1) S(1) O(2) 114.63(17) yes . . . Rh(2) S(2) S(1) 93.85(4) yes . . . Rh(2) S(2) O(3) 114.25(12) yes . . . Rh(2) S(2) O(4) 115.22(12) yes . . . S(1) S(2) O(3) 108.56(13) yes . . . S(1) S(2) O(4) 107.80(12) yes . . . O(3) S(2) O(4) 114.67(17) yes . . . Rh(1) C(1) C(2) 73.6(2) yes . . . Rh(1) C(1) C(5) 71.2(2) yes . . . Rh(1) C(1) C(6) 123.5(2) yes . . . C(2) C(1) C(5) 107.1(3) yes . . . C(2) C(1) C(6) 126.6(3) yes . . . C(5) C(1) C(6) 126.2(3) yes . . . Rh(1) C(2) C(1) 69.1(2) yes . . . Rh(1) C(2) C(3) 71.1(2) yes . . . Rh(1) C(2) C(7) 127.5(2) yes . . . C(1) C(2) C(3) 108.8(3) yes . . . C(1) C(2) C(7) 125.3(3) yes . . . C(3) C(2) C(7) 125.8(3) yes . . . Rh(1) C(3) C(2) 72.3(2) yes . . . Rh(1) C(3) C(4) 70.2(2) yes . . . Rh(1) C(3) C(8) 127.2(2) yes . . . C(2) C(3) C(4) 107.6(3) yes . . . C(2) C(3) C(8) 126.8(3) yes . . . C(4) C(3) C(8) 125.4(3) yes . . . Rh(1) C(4) C(3) 72.3(2) yes . . . Rh(1) C(4) C(5) 70.9(2) yes . . . Rh(1) C(4) C(9) 126.6(2) yes . . . C(3) C(4) C(5) 108.3(3) yes . . . C(3) C(4) C(9) 126.0(3) yes . . . C(5) C(4) C(9) 125.5(3) yes . . . Rh(1) C(5) C(1) 70.8(2) yes . . . Rh(1) C(5) C(4) 71.6(2) yes . . . Rh(1) C(5) C(10) 126.2(2) yes . . . C(1) C(5) C(4) 108.0(3) yes . . . C(1) C(5) C(10) 126.4(3) yes . . . C(4) C(5) C(10) 125.4(3) yes . . . C(1) C(6) C(11) 113.0(3) yes . . . C(6) C(11) C(12) 110.9(3) yes . . . Rh(2) C(13) C(14) 71.7(2) yes . . . Rh(2) C(13) C(17) 69.0(2) yes . . . Rh(2) C(13) C(18) 131.0(2) yes . . . C(14) C(13) C(17) 107.6(3) yes . . . C(14) C(13) C(18) 127.1(3) yes . . . C(17) C(13) C(18) 124.8(3) yes . . . Rh(2) C(14) C(13) 71.4(2) yes . . . Rh(2) C(14) C(15) 70.1(2) yes . . . Rh(2) C(14) C(19) 126.8(2) yes . . . C(13) C(14) C(15) 108.7(3) yes . . . C(13) C(14) C(19) 125.4(3) yes . . . C(15) C(14) C(19) 125.9(3) yes . . . Rh(2) C(15) C(14) 73.0(2) yes . . . Rh(2) C(15) C(16) 70.3(2) yes . . . Rh(2) C(15) C(20) 126.5(2) yes . . . C(14) C(15) C(16) 107.2(3) yes . . . C(14) C(15) C(20) 126.1(3) yes . . . C(16) C(15) C(20) 126.4(3) yes . . . Rh(2) C(16) C(15) 72.4(2) yes . . . Rh(2) C(16) C(17) 70.9(2) yes . . . Rh(2) C(16) C(21) 124.5(2) yes . . . C(15) C(16) C(17) 108.9(3) yes . . . C(15) C(16) C(21) 125.1(3) yes . . . C(17) C(16) C(21) 125.9(3) yes . . . Rh(2) C(17) C(13) 73.8(2) yes . . . Rh(2) C(17) C(16) 71.1(2) yes . . . Rh(2) C(17) C(22) 122.6(2) yes . . . C(13) C(17) C(16) 107.5(3) yes . . . C(13) C(17) C(22) 127.3(3) yes . . . C(16) C(17) C(22) 125.2(3) yes . . . C(13) C(18) C(23) 111.4(3) yes . . . C(18) C(23) C(24) 114.8(3) yes . . . Rh(1) C(25) Rh(2) 79.54(13) yes . . . Rh(1) C(26) Rh(2) 79.36(13) yes . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(1) C(8) 3.334(4) ? . 1_655 O(1) C(11) 3.474(5) ? . 2_556 O(2) C(8) 3.542(4) ? . 1_655 O(3) C(8) 3.515(4) ? . 1_655 O(3) C(18) 3.599(4) ? . 1_655 O(3) C(22) 3.564(4) ? . 2_566 O(4) C(12) 3.581(5) ? . 3_755 O(4) C(19) 3.471(4) ? . 1_655 C(3) C(10) 3.367(5) ? . 2_456 C(4) C(10) 3.452(5) ? . 2_456 C(8) O(1) 3.334(4) ? . 1_455 C(8) O(2) 3.542(4) ? . 1_455 C(8) O(3) 3.515(4) ? . 1_455 C(8) C(22) 3.405(5) ? . 2_466 C(10) C(3) 3.367(5) ? . 2_556 C(10) C(4) 3.452(5) ? . 2_556 C(11) O(1) 3.474(5) ? . 2_456 C(12) O(4) 3.581(5) ? . 3_745 C(18) O(3) 3.599(4) ? . 1_455 C(19) O(4) 3.471(4) ? . 1_455 C(21) C(24) 3.551(6) ? . 1_655 C(22) O(3) 3.564(4) ? . 2_466 C(22) C(8) 3.405(5) ? . 2_566 C(24) C(21) 3.551(6) ? . 1_455 #============================================================================== data___(P)-2Pro _database_code_depnum_ccdc_archive 'CCDC 718202' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C26 H42 O4 Rh2 S2 ' _chemical_formula_moiety 'C26 H42 O4 Rh2 S2 ' _chemical_formula_weight 688.55 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2+X,1/2-Y,-Z 3 -X,1/2+Y,1/2-Z 4 1/2-X,-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.1949(11) _cell_length_b 13.8240(16) _cell_length_c 21.119(3) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 2684.5(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7437 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange-brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408.00 _exptl_absorpt_coefficient_mu 1.413 _exptl_absorpt_correction_type Empirical _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.710 _exptl_absorpt_correction_T_max 0.844 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 28299 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6121 _reflns_number_gt 5930 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1085 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6121 _refine_ls_number_parameters 326 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0485P)^2^+7.8671P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 1.43 _refine_diff_density_min -1.09 _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 -0.03(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Rh Rh -1.118 0.919 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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(1) Rh 0.81920(4) 0.36638(3) 0.36543(2) 0.01954(11) Uani 1.00 1 d . . . Rh(2) Rh 0.78902(4) 0.54073(3) 0.41286(2) 0.01933(11) Uani 1.00 1 d . . . S(1) S 1.06558(17) 0.36366(13) 0.37882(10) 0.0429(4) Uani 1.00 1 d . . . S(2) S 1.03208(17) 0.56061(12) 0.42858(10) 0.0412(4) Uani 1.00 1 d . . . O(1) O 1.1053(5) 0.3060(5) 0.4334(2) 0.0508(15) Uani 0.98 1 d P . . O(2) O 1.1612(15) 0.3860(13) 0.3432(7) 0.041(4) Uani 0.29 1 d P . . O(3) O 1.0811(6) 0.5446(4) 0.4889(2) 0.0356(12) Uani 0.77 1 d P . . O(4) O 1.0928(5) 0.6423(4) 0.3968(2) 0.0508(14) Uani 0.99 1 d P . . O(5) O 1.0982(16) 0.4487(11) 0.4499(7) 0.025(3) Uani 0.26 1 d P . . O(6) O 1.1194(5) 0.4784(4) 0.3790(2) 0.0284(13) Uani 0.72 1 d P . . C(1) C 0.6271(6) 0.2600(3) 0.3664(2) 0.0208(10) Uani 1.00 1 d . . . C(2) C 0.7618(5) 0.2110(3) 0.3728(2) 0.0209(11) Uani 1.00 1 d . . . C(3) C 0.8416(6) 0.2260(4) 0.3149(2) 0.0260(12) Uani 1.00 1 d . . . C(4) C 0.7605(6) 0.2886(4) 0.2759(2) 0.0258(12) Uani 1.00 1 d . . . C(5) C 0.6267(6) 0.3096(4) 0.3076(2) 0.0251(12) Uani 1.00 1 d . . . C(6) C 0.4966(6) 0.2477(3) 0.4098(2) 0.0225(11) Uani 1.00 1 d . . . C(7) C 0.8088(6) 0.1474(4) 0.4270(2) 0.0281(12) Uani 1.00 1 d . . . C(8) C 0.9836(7) 0.1784(4) 0.2968(3) 0.0329(14) Uani 1.00 1 d . . . C(9) C 0.7987(8) 0.3195(4) 0.2091(2) 0.0364(14) Uani 1.00 1 d . . . C(10) C 0.5012(6) 0.3666(4) 0.2805(2) 0.0305(12) Uani 1.00 1 d . . . C(11) C 0.3860(7) 0.1772(4) 0.3799(3) 0.0323(14) Uani 1.00 1 d . . . C(12) C 0.4459(7) 0.0781(4) 0.3657(3) 0.0384(14) Uani 1.00 1 d . . . C(13) C 0.7105(6) 0.6911(3) 0.4004(2) 0.0232(11) Uani 1.00 1 d . . . C(14) C 0.7462(6) 0.6773(3) 0.4662(2) 0.0219(11) Uani 1.00 1 d . . . C(15) C 0.6510(6) 0.6043(3) 0.4901(2) 0.0213(11) Uani 1.00 1 d . . . C(16) C 0.5553(6) 0.5745(4) 0.4386(2) 0.0233(11) Uani 1.00 1 d . . . C(17) C 0.5911(6) 0.6301(4) 0.3849(2) 0.0225(11) Uani 1.00 1 d . . . C(18) C 0.7846(7) 0.7632(4) 0.3578(2) 0.0270(11) Uani 1.00 1 d . . . C(19) C 0.8512(7) 0.7328(4) 0.5055(3) 0.0321(13) Uani 1.00 1 d . . . C(20) C 0.6409(7) 0.5711(4) 0.5575(3) 0.0329(14) Uani 1.00 1 d . . . C(21) C 0.4320(6) 0.5060(4) 0.4471(2) 0.0272(12) Uani 1.00 1 d . . . C(22) C 0.5113(6) 0.6297(4) 0.3232(3) 0.0321(13) Uani 1.00 1 d . . . C(23) C 0.7197(7) 0.8674(3) 0.3639(2) 0.0290(11) Uani 1.00 1 d . . . C(24) C 0.7949(7) 0.9358(4) 0.3179(3) 0.0320(13) Uani 1.00 1 d . . . C(25) C 0.8022(7) 0.4077(3) 0.4567(2) 0.0255(11) Uani 1.00 1 d . . . C(26) C 0.8392(6) 0.4981(4) 0.3229(2) 0.0248(12) Uani 1.00 1 d . . . H(1) H 0.4498 0.3112 0.4170 0.027 Uiso 1.00 1 c R . . H(2) H 0.5291 0.2222 0.4513 0.027 Uiso 1.00 1 c R . . H(3) H 0.9023 0.1172 0.4167 0.034 Uiso 1.00 1 c R . . H(4) H 0.7356 0.0970 0.4340 0.034 Uiso 1.00 1 c R . . H(5) H 0.8191 0.1865 0.4654 0.034 Uiso 1.00 1 c R . . H(6) H 1.0129 0.2004 0.2545 0.039 Uiso 1.00 1 c R . . H(7) H 0.9712 0.1080 0.2965 0.039 Uiso 1.00 1 c R . . H(8) H 1.0588 0.1961 0.3276 0.039 Uiso 1.00 1 c R . . H(9) H 0.7216 0.3612 0.1924 0.044 Uiso 1.00 1 c R . . H(10) H 0.8086 0.2622 0.1822 0.044 Uiso 1.00 1 c R . . H(11) H 0.8908 0.3552 0.2096 0.044 Uiso 1.00 1 c R . . H(12) H 0.4219 0.3690 0.3115 0.037 Uiso 1.00 1 c R . . H(13) H 0.4668 0.3353 0.2417 0.037 Uiso 1.00 1 c R . . H(14) H 0.5335 0.4325 0.2708 0.037 Uiso 1.00 1 c R . . H(15) H 0.3023 0.1703 0.4091 0.039 Uiso 1.00 1 c R . . H(16) H 0.3494 0.2060 0.3401 0.039 Uiso 1.00 1 c R . . H(17) H 0.4864 0.0774 0.3228 0.046 Uiso 1.00 1 c R . . H(18) H 0.3676 0.0302 0.3688 0.046 Uiso 1.00 1 c R . . H(19) H 0.5224 0.0624 0.3963 0.046 Uiso 1.00 1 c R . . H(20) H 0.7754 0.7414 0.3133 0.032 Uiso 1.00 1 c R . . H(21) H 0.8895 0.7653 0.3683 0.032 Uiso 1.00 1 c R . . H(22) H 0.8477 0.7091 0.5493 0.038 Uiso 1.00 1 c R . . H(23) H 0.8254 0.8015 0.5047 0.038 Uiso 1.00 1 c R . . H(24) H 0.9496 0.7243 0.4886 0.038 Uiso 1.00 1 c R . . H(25) H 0.5638 0.5225 0.5613 0.040 Uiso 1.00 1 c R . . H(26) H 0.6184 0.6264 0.5848 0.040 Uiso 1.00 1 c R . . H(27) H 0.7339 0.5426 0.5704 0.040 Uiso 1.00 1 c R . . H(28) H 0.3815 0.4973 0.4067 0.033 Uiso 1.00 1 c R . . H(29) H 0.3640 0.5322 0.4785 0.033 Uiso 1.00 1 c R . . H(30) H 0.4692 0.4435 0.4619 0.033 Uiso 1.00 1 c R . . H(31) H 0.5538 0.6781 0.2949 0.038 Uiso 1.00 1 c R . . H(32) H 0.4086 0.6451 0.3306 0.038 Uiso 1.00 1 c R . . H(33) H 0.5190 0.5655 0.3038 0.038 Uiso 1.00 1 c R . . H(34) H 0.6142 0.8657 0.3547 0.035 Uiso 1.00 1 c R . . H(35) H 0.7329 0.8912 0.4077 0.035 Uiso 1.00 1 c R . . H(36) H 0.8795 0.9652 0.3386 0.038 Uiso 1.00 1 c R . . H(37) H 0.7269 0.9867 0.3050 0.038 Uiso 1.00 1 c R . . H(38) H 0.8268 0.8996 0.2805 0.038 Uiso 1.00 1 c R . . H(39) H 0.8904 0.3973 0.4827 0.031 Uiso 1.00 1 c R . . H(40) H 0.7126 0.3863 0.4785 0.031 Uiso 1.00 1 c R . . H(41) H 0.7646 0.5129 0.2905 0.030 Uiso 1.00 1 c R . . H(42) H 0.9385 0.5148 0.3085 0.030 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.0171(2) 0.01610(19) 0.0254(2) 0.00001(16) 0.00315(16) -0.00100(17) Rh(2) 0.0148(2) 0.01603(19) 0.0272(2) 0.00000(15) -0.00192(17) -0.00219(17) S(1) 0.0168(7) 0.0285(7) 0.0833(13) 0.0044(6) -0.0013(7) -0.0040(8) S(2) 0.0168(7) 0.0266(7) 0.0800(13) -0.0011(5) -0.0097(7) -0.0057(8) O(1) 0.028(2) 0.088(4) 0.037(2) 0.012(2) -0.002(2) -0.005(2) O(2) 0.016(7) 0.062(11) 0.044(8) 0.003(7) 0.018(6) 0.010(8) O(3) 0.021(2) 0.040(3) 0.045(3) 0.002(2) -0.004(2) -0.005(2) O(4) 0.026(2) 0.073(3) 0.053(3) -0.021(2) 0.005(2) -0.002(2) O(5) 0.023(7) 0.029(8) 0.022(7) 0.009(6) -0.012(6) -0.007(6) O(6) 0.011(2) 0.038(3) 0.036(3) -0.000(2) 0.002(2) -0.010(2) C(1) 0.027(2) 0.017(2) 0.019(2) 0.005(2) -0.004(2) -0.005(2) C(2) 0.021(2) 0.011(2) 0.030(2) -0.0009(18) -0.001(2) -0.005(2) C(3) 0.029(3) 0.024(2) 0.025(2) -0.002(2) 0.008(2) -0.003(2) C(4) 0.026(3) 0.029(2) 0.023(2) -0.007(2) 0.010(2) -0.004(2) C(5) 0.029(3) 0.021(2) 0.025(2) -0.005(2) -0.003(2) 0.003(2) C(6) 0.022(2) 0.020(2) 0.025(2) 0.004(2) 0.001(2) -0.001(2) C(7) 0.027(2) 0.024(2) 0.033(2) 0.003(2) -0.001(2) -0.001(2) C(8) 0.040(3) 0.026(2) 0.033(3) 0.004(2) 0.008(2) -0.009(2) C(9) 0.047(4) 0.037(3) 0.025(2) -0.000(3) 0.009(3) 0.000(2) C(10) 0.031(3) 0.028(2) 0.032(3) 0.004(2) -0.004(2) 0.006(2) C(11) 0.026(3) 0.038(3) 0.033(3) -0.002(2) 0.007(2) -0.001(2) C(12) 0.037(3) 0.032(3) 0.047(3) -0.006(2) 0.006(3) -0.009(3) C(13) 0.026(2) 0.015(2) 0.029(2) -0.001(2) 0.005(2) -0.000(2) C(14) 0.020(2) 0.019(2) 0.027(2) 0.004(2) -0.001(2) -0.007(2) C(15) 0.022(2) 0.018(2) 0.024(2) -0.001(2) 0.002(2) -0.005(2) C(16) 0.014(2) 0.019(2) 0.037(3) 0.004(2) 0.001(2) -0.001(2) C(17) 0.020(2) 0.014(2) 0.033(2) 0.003(2) -0.001(2) -0.003(2) C(18) 0.031(3) 0.023(2) 0.027(2) -0.001(2) 0.004(2) -0.002(2) C(19) 0.032(3) 0.027(3) 0.037(3) -0.002(2) -0.000(2) -0.012(2) C(20) 0.037(3) 0.030(3) 0.031(3) 0.006(2) 0.007(2) -0.000(2) C(21) 0.024(2) 0.022(2) 0.035(3) 0.001(2) 0.006(2) -0.009(2) C(22) 0.027(3) 0.033(3) 0.036(3) 0.006(2) -0.009(2) -0.002(2) C(23) 0.037(3) 0.014(2) 0.036(3) -0.004(2) -0.003(2) -0.001(2) C(24) 0.034(3) 0.020(2) 0.042(3) 0.000(2) -0.003(2) 0.005(2) C(25) 0.032(3) 0.022(2) 0.023(2) 0.001(2) -0.008(2) 0.000(2) C(26) 0.028(3) 0.021(2) 0.026(2) -0.001(2) 0.011(2) -0.002(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rh(1) Rh(2) 2.6248(5) yes . . Rh(1) S(1) 2.2833(16) yes . . Rh(1) C(1) 2.299(5) yes . . Rh(1) C(2) 2.217(4) yes . . Rh(1) C(3) 2.225(5) yes . . Rh(1) C(4) 2.241(5) yes . . Rh(1) C(5) 2.289(5) yes . . Rh(1) C(25) 2.016(5) yes . . Rh(1) C(26) 2.039(5) yes . . Rh(2) S(2) 2.2761(16) yes . . Rh(2) C(13) 2.216(5) yes . . Rh(2) C(14) 2.232(5) yes . . Rh(2) C(15) 2.245(5) yes . . Rh(2) C(16) 2.265(5) yes . . Rh(2) C(17) 2.278(5) yes . . Rh(2) C(25) 2.062(5) yes . . Rh(2) C(26) 2.043(5) yes . . S(1) O(1) 1.448(6) yes . . S(1) O(2) 1.198(15) yes . . S(1) O(5) 1.930(15) yes . . S(1) O(6) 1.661(6) yes . . S(2) O(3) 1.369(6) yes . . S(2) O(4) 1.427(6) yes . . S(2) O(5) 1.722(16) yes . . S(2) O(6) 1.742(6) yes . . O(2) O(6) 1.533(18) yes . . O(3) O(5) 1.569(17) yes . . O(5) O(6) 1.565(16) yes . . C(1) C(2) 1.418(7) yes . . C(1) C(5) 1.419(7) yes . . C(1) C(6) 1.520(7) yes . . C(2) C(3) 1.442(8) yes . . C(2) C(7) 1.506(7) yes . . C(3) C(4) 1.408(8) yes . . C(3) C(8) 1.511(9) yes . . C(4) C(5) 1.430(8) yes . . C(4) C(9) 1.515(8) yes . . C(5) C(10) 1.509(8) yes . . C(6) C(11) 1.543(8) yes . . C(11) C(12) 1.507(9) yes . . C(13) C(14) 1.441(7) yes . . C(13) C(17) 1.421(8) yes . . C(13) C(18) 1.507(8) yes . . C(14) C(15) 1.428(7) yes . . C(14) C(19) 1.488(8) yes . . C(15) C(16) 1.458(8) yes . . C(15) C(20) 1.499(8) yes . . C(16) C(17) 1.409(8) yes . . C(16) C(21) 1.487(8) yes . . C(17) C(22) 1.496(8) yes . . C(18) C(23) 1.564(7) yes . . C(23) C(24) 1.521(8) yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Rh(2) Rh(1) S(1) 94.17(4) yes . . . Rh(2) Rh(1) C(1) 120.19(13) yes . . . Rh(2) Rh(1) C(2) 146.87(14) yes . . . Rh(2) Rh(1) C(3) 173.73(14) yes . . . Rh(2) Rh(1) C(4) 137.47(15) yes . . . Rh(2) Rh(1) C(5) 115.89(14) yes . . . Rh(2) Rh(1) C(25) 50.72(15) yes . . . Rh(2) Rh(1) C(26) 50.05(16) yes . . . S(1) Rh(1) C(1) 138.66(14) yes . . . S(1) Rh(1) C(2) 102.21(14) yes . . . S(1) Rh(1) C(3) 87.32(16) yes . . . S(1) Rh(1) C(4) 109.62(16) yes . . . S(1) Rh(1) C(5) 145.85(15) yes . . . S(1) Rh(1) C(25) 87.89(19) yes . . . S(1) Rh(1) C(26) 88.85(18) yes . . . C(1) Rh(1) C(2) 36.55(19) yes . . . C(1) Rh(1) C(3) 61.1(2) yes . . . C(1) Rh(1) C(4) 61.0(2) yes . . . C(1) Rh(1) C(5) 36.02(19) yes . . . C(1) Rh(1) C(25) 96.5(2) yes . . . C(1) Rh(1) C(26) 130.1(2) yes . . . C(2) Rh(1) C(3) 37.9(2) yes . . . C(2) Rh(1) C(4) 62.5(2) yes . . . C(2) Rh(1) C(5) 61.4(2) yes . . . C(2) Rh(1) C(25) 100.9(2) yes . . . C(2) Rh(1) C(26) 156.6(2) yes . . . C(3) Rh(1) C(4) 36.8(2) yes . . . C(3) Rh(1) C(5) 61.1(2) yes . . . C(3) Rh(1) C(25) 135.5(2) yes . . . C(3) Rh(1) C(26) 124.0(2) yes . . . C(4) Rh(1) C(5) 36.8(2) yes . . . C(4) Rh(1) C(25) 157.5(2) yes . . . C(4) Rh(1) C(26) 94.5(2) yes . . . C(5) Rh(1) C(25) 123.2(2) yes . . . C(5) Rh(1) C(26) 98.1(2) yes . . . C(25) Rh(1) C(26) 100.1(2) yes . . . Rh(1) Rh(2) S(2) 93.60(4) yes . . . Rh(1) Rh(2) C(13) 148.23(14) yes . . . Rh(1) Rh(2) C(14) 170.88(14) yes . . . Rh(1) Rh(2) C(15) 134.12(13) yes . . . Rh(1) Rh(2) C(16) 112.38(14) yes . . . Rh(1) Rh(2) C(17) 118.95(14) yes . . . Rh(1) Rh(2) C(25) 49.16(14) yes . . . Rh(1) Rh(2) C(26) 49.91(15) yes . . . S(2) Rh(2) C(13) 102.95(16) yes . . . S(2) Rh(2) C(14) 89.86(14) yes . . . S(2) Rh(2) C(15) 113.70(15) yes . . . S(2) Rh(2) C(16) 150.66(15) yes . . . S(2) Rh(2) C(17) 139.18(14) yes . . . S(2) Rh(2) C(25) 89.11(19) yes . . . S(2) Rh(2) C(26) 87.07(18) yes . . . C(13) Rh(2) C(14) 37.8(2) yes . . . C(13) Rh(2) C(15) 62.31(19) yes . . . C(13) Rh(2) C(16) 61.7(2) yes . . . C(13) Rh(2) C(17) 36.8(2) yes . . . C(13) Rh(2) C(25) 155.4(2) yes . . . C(13) Rh(2) C(26) 103.5(2) yes . . . C(14) Rh(2) C(15) 37.20(19) yes . . . C(14) Rh(2) C(16) 62.5(2) yes . . . C(14) Rh(2) C(17) 62.0(2) yes . . . C(14) Rh(2) C(25) 122.6(2) yes . . . C(14) Rh(2) C(26) 138.8(2) yes . . . C(15) Rh(2) C(16) 37.7(2) yes . . . C(15) Rh(2) C(17) 61.6(2) yes . . . C(15) Rh(2) C(25) 93.2(2) yes . . . C(15) Rh(2) C(26) 156.4(2) yes . . . C(16) Rh(2) C(17) 36.1(2) yes . . . C(16) Rh(2) C(25) 97.6(2) yes . . . C(16) Rh(2) C(26) 119.8(2) yes . . . C(17) Rh(2) C(25) 130.3(2) yes . . . C(17) Rh(2) C(26) 95.5(2) yes . . . C(25) Rh(2) C(26) 98.4(2) yes . . . Rh(1) S(1) O(1) 111.0(2) yes . . . Rh(1) S(1) O(2) 130.3(7) yes . . . Rh(1) S(1) O(5) 103.9(4) yes . . . Rh(1) S(1) O(6) 106.3(2) yes . . . O(1) S(1) O(2) 117.1(8) yes . . . O(1) S(1) O(5) 71.2(5) yes . . . O(1) S(1) O(6) 116.7(3) yes . . . O(2) S(1) O(5) 102.6(9) yes . . . O(2) S(1) O(6) 62.4(8) yes . . . O(5) S(1) O(6) 51.0(5) yes . . . Rh(2) S(2) O(3) 116.1(2) yes . . . Rh(2) S(2) O(4) 114.3(2) yes . . . Rh(2) S(2) O(5) 106.0(5) yes . . . Rh(2) S(2) O(6) 106.6(2) yes . . . O(3) S(2) O(4) 115.9(3) yes . . . O(3) S(2) O(5) 59.7(5) yes . . . O(3) S(2) O(6) 107.6(3) yes . . . O(4) S(2) O(5) 134.1(5) yes . . . O(4) S(2) O(6) 93.1(3) yes . . . O(5) S(2) O(6) 53.7(5) yes . . . S(1) O(2) O(6) 73.8(8) yes . . . S(2) O(3) O(5) 71.4(6) yes . . . S(1) O(5) S(2) 106.8(7) yes . . . S(1) O(5) O(3) 155.1(10) yes . . . S(1) O(5) O(6) 55.6(5) yes . . . S(2) O(5) O(3) 48.9(5) yes . . . S(2) O(5) O(6) 63.8(6) yes . . . O(3) O(5) O(6) 107.0(10) yes . . . S(1) O(6) S(2) 119.2(3) yes . . . S(1) O(6) O(2) 43.8(6) yes . . . S(1) O(6) O(5) 73.4(6) yes . . . S(2) O(6) O(2) 162.9(7) yes . . . S(2) O(6) O(5) 62.5(6) yes . . . O(2) O(6) O(5) 106.5(9) yes . . . Rh(1) C(1) C(2) 68.6(2) yes . . . Rh(1) C(1) C(5) 71.6(3) yes . . . Rh(1) C(1) C(6) 133.1(3) yes . . . C(2) C(1) C(5) 108.5(4) yes . . . C(2) C(1) C(6) 125.3(4) yes . . . C(5) C(1) C(6) 125.5(5) yes . . . Rh(1) C(2) C(1) 74.9(2) yes . . . Rh(1) C(2) C(3) 71.3(3) yes . . . Rh(1) C(2) C(7) 123.5(3) yes . . . C(1) C(2) C(3) 107.1(4) yes . . . C(1) C(2) C(7) 127.0(5) yes . . . C(3) C(2) C(7) 125.6(4) yes . . . Rh(1) C(3) C(2) 70.8(3) yes . . . Rh(1) C(3) C(4) 72.2(3) yes . . . Rh(1) C(3) C(8) 125.5(4) yes . . . C(2) C(3) C(4) 108.3(5) yes . . . C(2) C(3) C(8) 126.3(5) yes . . . C(4) C(3) C(8) 125.3(5) yes . . . Rh(1) C(4) C(3) 71.0(3) yes . . . Rh(1) C(4) C(5) 73.5(3) yes . . . Rh(1) C(4) C(9) 126.5(4) yes . . . C(3) C(4) C(5) 107.9(4) yes . . . C(3) C(4) C(9) 126.4(5) yes . . . C(5) C(4) C(9) 125.3(5) yes . . . Rh(1) C(5) C(1) 72.4(3) yes . . . Rh(1) C(5) C(4) 69.8(3) yes . . . Rh(1) C(5) C(10) 127.9(4) yes . . . C(1) C(5) C(4) 108.0(5) yes . . . C(1) C(5) C(10) 125.8(5) yes . . . C(4) C(5) C(10) 125.9(5) yes . . . C(1) C(6) C(11) 110.1(4) yes . . . C(6) C(11) C(12) 114.5(5) yes . . . Rh(2) C(13) C(14) 71.7(3) yes . . . Rh(2) C(13) C(17) 73.9(3) yes . . . Rh(2) C(13) C(18) 123.0(4) yes . . . C(14) C(13) C(17) 108.6(4) yes . . . C(14) C(13) C(18) 124.1(5) yes . . . C(17) C(13) C(18) 127.2(5) yes . . . Rh(2) C(14) C(13) 70.5(3) yes . . . Rh(2) C(14) C(15) 71.9(3) yes . . . Rh(2) C(14) C(19) 127.1(4) yes . . . C(13) C(14) C(15) 107.2(4) yes . . . C(13) C(14) C(19) 128.2(5) yes . . . C(15) C(14) C(19) 124.4(5) yes . . . Rh(2) C(15) C(14) 70.9(3) yes . . . Rh(2) C(15) C(16) 71.9(3) yes . . . Rh(2) C(15) C(20) 127.2(4) yes . . . C(14) C(15) C(16) 107.8(4) yes . . . C(14) C(15) C(20) 126.2(5) yes . . . C(16) C(15) C(20) 125.8(5) yes . . . Rh(2) C(16) C(15) 70.4(3) yes . . . Rh(2) C(16) C(17) 72.4(3) yes . . . Rh(2) C(16) C(21) 128.4(3) yes . . . C(15) C(16) C(17) 107.7(4) yes . . . C(15) C(16) C(21) 123.3(5) yes . . . C(17) C(16) C(21) 128.6(5) yes . . . Rh(2) C(17) C(13) 69.2(3) yes . . . Rh(2) C(17) C(16) 71.5(3) yes . . . Rh(2) C(17) C(22) 128.0(4) yes . . . C(13) C(17) C(16) 108.7(4) yes . . . C(13) C(17) C(22) 125.6(5) yes . . . C(16) C(17) C(22) 125.7(5) yes . . . C(13) C(18) C(23) 112.8(4) yes . . . C(18) C(23) C(24) 110.3(4) yes . . . Rh(1) C(25) Rh(2) 80.12(19) yes . . . Rh(1) C(26) Rh(2) 80.0(2) yes . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(1) C(6) 3.538(7) ? . 2_556 O(1) C(7) 3.553(7) ? . 2_556 O(1) C(11) 3.332(8) ? . 1_655 O(2) C(10) 3.406(15) ? . 1_655 O(2) C(24) 3.495(17) ? . 3_745 O(3) C(21) 3.387(8) ? . 1_655 O(3) C(23) 3.575(8) ? . 2_566 O(4) C(9) 3.465(8) ? . 3_755 O(4) C(19) 3.589(8) ? . 2_566 O(5) C(7) 3.504(16) ? . 2_556 O(5) C(21) 3.171(16) ? . 1_655 O(6) C(21) 3.237(8) ? . 1_655 C(6) O(1) 3.538(7) ? . 2_456 C(7) O(1) 3.553(7) ? . 2_456 C(7) O(5) 3.504(16) ? . 2_456 C(7) C(21) 3.585(8) ? . 2_556 C(9) O(4) 3.465(8) ? . 3_745 C(9) C(20) 3.585(8) ? . 4_664 C(10) O(2) 3.406(15) ? . 1_455 C(10) C(24) 3.557(9) ? . 3_645 C(11) O(1) 3.332(8) ? . 1_455 C(15) C(19) 3.561(8) ? . 2_466 C(16) C(19) 3.466(8) ? . 2_466 C(19) O(4) 3.589(8) ? . 2_466 C(19) C(15) 3.561(8) ? . 2_566 C(19) C(16) 3.466(8) ? . 2_566 C(20) C(9) 3.585(8) ? . 4_665 C(21) O(3) 3.387(8) ? . 1_455 C(21) O(5) 3.171(16) ? . 1_455 C(21) O(6) 3.237(8) ? . 1_455 C(21) C(7) 3.585(8) ? . 2_456 C(23) O(3) 3.575(8) ? . 2_466 C(24) O(2) 3.495(17) ? . 3_755 C(24) C(10) 3.557(9) ? . 3_655 #============================================================================== data___(M)-2Pro _database_code_depnum_ccdc_archive 'CCDC 718203' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C26 H42 O4 Rh2 S2 ' _chemical_formula_moiety 'C26 H42 O4 Rh2 S2 ' _chemical_formula_weight 688.55 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2+X,1/2-Y,-Z 3 -X,1/2+Y,1/2-Z 4 1/2-X,-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.1945(11) _cell_length_b 13.8409(16) _cell_length_c 21.120(3) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 2687.8(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7912 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange-brown _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408.00 _exptl_absorpt_coefficient_mu 1.411 _exptl_absorpt_correction_type Empirical _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 0.868 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 27355 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6108 _reflns_number_gt 5621 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0979 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6108 _refine_ls_number_parameters 326 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0426P)^2^+1.5127P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 1.38 _refine_diff_density_min -1.02 _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 -0.09(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Rh Rh -1.118 0.919 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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(1) Rh 0.21001(4) 0.54094(3) 0.412691(18) 0.01975(10) Uani 1.00 1 d . . . Rh(2) Rh 0.18077(4) 0.36664(3) 0.365295(18) 0.01980(10) Uani 1.00 1 d . . . S(1) S -0.03337(16) 0.56104(11) 0.42789(9) 0.0394(4) Uani 1.00 1 d . . . S(2) S -0.06592(16) 0.36351(11) 0.37793(8) 0.0405(3) Uani 1.00 1 d . . . O(1) O -0.0828(5) 0.5448(4) 0.4888(2) 0.0390(12) Uani 0.80 1 d P . . O(2) O -0.0937(4) 0.6431(3) 0.3968(2) 0.0466(11) Uani 0.99 1 d P . . O(3) O -0.1059(4) 0.3089(4) 0.4333(2) 0.0483(12) Uani 0.98 1 d P . . O(4) O -0.1652(16) 0.3824(13) 0.3437(7) 0.043(4) Uani 0.25 1 d P . . O(5) O -0.0996(17) 0.4497(12) 0.4507(7) 0.026(3) Uani 0.23 1 d P . . O(6) O -0.1209(5) 0.4800(3) 0.3794(2) 0.0283(11) Uani 0.75 1 d P . . C(1) C 0.2881(6) 0.6921(3) 0.4001(2) 0.0239(11) Uani 1.00 1 d . . . C(2) C 0.4083(5) 0.6305(3) 0.3850(2) 0.0229(11) Uani 1.00 1 d . . . C(3) C 0.4434(5) 0.5737(3) 0.4393(2) 0.0209(11) Uani 1.00 1 d . . . C(4) C 0.3487(5) 0.6039(3) 0.4898(2) 0.0221(11) Uani 1.00 1 d . . . C(5) C 0.2521(5) 0.6766(3) 0.4661(2) 0.0220(11) Uani 1.00 1 d . . . C(6) C 0.2153(6) 0.7639(3) 0.3570(2) 0.0256(11) Uani 1.00 1 d . . . C(7) C 0.4875(6) 0.6292(4) 0.3230(2) 0.0319(12) Uani 1.00 1 d . . . C(8) C 0.5674(6) 0.5063(3) 0.4476(2) 0.0288(12) Uani 1.00 1 d . . . C(9) C 0.3572(7) 0.5698(4) 0.5578(2) 0.0357(14) Uani 1.00 1 d . . . C(10) C 0.1482(6) 0.7335(4) 0.5051(2) 0.0299(12) Uani 1.00 1 d . . . C(11) C 0.2776(6) 0.8667(3) 0.3640(2) 0.0317(11) Uani 1.00 1 d . . . C(12) C 0.2054(7) 0.9364(3) 0.3183(2) 0.0340(13) Uani 1.00 1 d . . . C(13) C 0.3725(5) 0.2599(3) 0.3668(2) 0.0217(10) Uani 1.00 1 d . . . C(14) C 0.3750(5) 0.3092(3) 0.3074(2) 0.0226(11) Uani 1.00 1 d . . . C(15) C 0.2405(6) 0.2893(3) 0.2759(2) 0.0267(12) Uani 1.00 1 d . . . C(16) C 0.1606(6) 0.2249(4) 0.3152(2) 0.0290(12) Uani 1.00 1 d . . . C(17) C 0.2382(5) 0.2113(3) 0.3730(2) 0.0216(11) Uani 1.00 1 d . . . C(18) C 0.5019(5) 0.2476(3) 0.4101(2) 0.0209(10) Uani 1.00 1 d . . . C(19) C 0.4992(6) 0.3669(4) 0.2810(2) 0.0296(12) Uani 1.00 1 d . . . C(20) C 0.2012(7) 0.3201(4) 0.2093(2) 0.0369(14) Uani 1.00 1 d . . . C(21) C 0.0158(6) 0.1800(4) 0.2968(2) 0.0343(14) Uani 1.00 1 d . . . C(22) C 0.1900(6) 0.1479(3) 0.4269(2) 0.0266(11) Uani 1.00 1 d . . . C(23) C 0.6131(6) 0.1762(4) 0.3799(2) 0.0343(14) Uani 1.00 1 d . . . C(24) C 0.5539(6) 0.0780(4) 0.3658(3) 0.0376(13) Uani 1.00 1 d . . . C(25) C 0.1965(6) 0.4083(3) 0.4568(2) 0.0248(11) Uani 1.00 1 d . . . C(26) C 0.1614(6) 0.4986(3) 0.3222(2) 0.0275(12) Uani 1.00 1 d . . . H(1) H 0.1099 0.7653 0.3665 0.031 Uiso 1.00 1 c R . . H(2) H 0.2271 0.7424 0.3126 0.031 Uiso 1.00 1 c R . . H(3) H 0.5650 0.5806 0.3245 0.038 Uiso 1.00 1 c R . . H(4) H 0.5302 0.6930 0.3151 0.038 Uiso 1.00 1 c R . . H(5) H 0.4194 0.6133 0.2889 0.038 Uiso 1.00 1 c R . . H(6) H 0.5706 0.4840 0.4916 0.035 Uiso 1.00 1 c R . . H(7) H 0.6584 0.5397 0.4374 0.035 Uiso 1.00 1 c R . . H(8) H 0.5553 0.4508 0.4194 0.035 Uiso 1.00 1 c R . . H(9) H 0.2837 0.6037 0.5831 0.043 Uiso 1.00 1 c R . . H(10) H 0.4541 0.5837 0.5748 0.043 Uiso 1.00 1 c R . . H(11) H 0.3392 0.5001 0.5596 0.043 Uiso 1.00 1 c R . . H(12) H 0.0999 0.7818 0.4784 0.036 Uiso 1.00 1 c R . . H(13) H 0.2011 0.7662 0.5392 0.036 Uiso 1.00 1 c R . . H(14) H 0.0752 0.6901 0.5233 0.036 Uiso 1.00 1 c R . . H(15) H 0.2624 0.8895 0.4079 0.038 Uiso 1.00 1 c R . . H(16) H 0.3836 0.8653 0.3558 0.038 Uiso 1.00 1 c R . . H(17) H 0.2591 0.9368 0.2782 0.041 Uiso 1.00 1 c R . . H(18) H 0.2057 1.0015 0.3365 0.041 Uiso 1.00 1 c R . . H(19) H 0.1049 0.9159 0.3106 0.041 Uiso 1.00 1 c R . . H(20) H 0.4693 0.2223 0.4516 0.025 Uiso 1.00 1 c R . . H(21) H 0.5491 0.3110 0.4172 0.025 Uiso 1.00 1 c R . . H(22) H 0.4747 0.3889 0.2382 0.035 Uiso 1.00 1 c R . . H(23) H 0.5866 0.3264 0.2793 0.035 Uiso 1.00 1 c R . . H(24) H 0.5174 0.4230 0.3082 0.035 Uiso 1.00 1 c R . . H(25) H 0.1080 0.2909 0.1973 0.044 Uiso 1.00 1 c R . . H(26) H 0.2770 0.2986 0.1799 0.044 Uiso 1.00 1 c R . . H(27) H 0.1929 0.3906 0.2076 0.044 Uiso 1.00 1 c R . . H(28) H -0.0185 0.1382 0.3311 0.041 Uiso 1.00 1 c R . . H(29) H 0.0281 0.1416 0.2582 0.041 Uiso 1.00 1 c R . . H(30) H -0.0557 0.2313 0.2892 0.041 Uiso 1.00 1 c R . . H(31) H 0.2623 0.1504 0.4609 0.032 Uiso 1.00 1 c R . . H(32) H 0.1801 0.0812 0.4119 0.032 Uiso 1.00 1 c R . . H(33) H 0.0960 0.1707 0.4429 0.032 Uiso 1.00 1 c R . . H(34) H 0.6497 0.2048 0.3400 0.041 Uiso 1.00 1 c R . . H(35) H 0.6969 0.1693 0.4089 0.041 Uiso 1.00 1 c R . . H(36) H 0.5680 0.0361 0.4027 0.045 Uiso 1.00 1 c R . . H(37) H 0.6051 0.0507 0.3293 0.045 Uiso 1.00 1 c R . . H(38) H 0.4499 0.0829 0.3562 0.045 Uiso 1.00 1 c R . . H(39) H 0.2858 0.3871 0.4790 0.030 Uiso 1.00 1 c R . . H(40) H 0.1080 0.3980 0.4826 0.030 Uiso 1.00 1 c R . . H(41) H 0.2366 0.5133 0.2901 0.033 Uiso 1.00 1 c R . . H(42) H 0.0623 0.5152 0.3075 0.033 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.0162(2) 0.01797(19) 0.0251(2) -0.00012(16) 0.00168(17) -0.00207(15) Rh(2) 0.0189(2) 0.01691(19) 0.0236(2) -0.00018(17) -0.00280(16) -0.00086(15) S(1) 0.0183(7) 0.0277(8) 0.0720(11) 0.0022(6) 0.0083(7) -0.0057(7) S(2) 0.0174(7) 0.0273(7) 0.0768(11) -0.0029(6) 0.0009(7) -0.0055(7) O(1) 0.027(2) 0.044(3) 0.046(3) 0.002(2) 0.001(2) -0.008(2) O(2) 0.028(2) 0.064(3) 0.048(2) 0.016(2) -0.0023(19) -0.005(2) O(3) 0.025(2) 0.083(3) 0.037(2) -0.008(2) 0.0030(19) -0.004(2) O(4) 0.021(8) 0.071(13) 0.038(8) 0.014(8) -0.015(6) 0.011(8) O(5) 0.023(8) 0.033(9) 0.024(8) 0.001(7) 0.006(6) 0.003(7) O(6) 0.015(2) 0.033(2) 0.037(2) 0.000(2) -0.001(2) -0.009(2) C(1) 0.020(2) 0.021(2) 0.030(2) 0.000(2) -0.002(2) -0.006(2) C(2) 0.019(2) 0.018(2) 0.032(2) -0.002(2) 0.006(2) -0.004(2) C(3) 0.013(2) 0.014(2) 0.035(2) -0.008(2) -0.000(2) 0.0011(19) C(4) 0.022(2) 0.020(2) 0.024(2) -0.004(2) -0.000(2) -0.0049(19) C(5) 0.021(2) 0.017(2) 0.027(2) -0.004(2) 0.003(2) -0.0048(19) C(6) 0.029(2) 0.017(2) 0.031(2) 0.003(2) 0.001(2) -0.0001(19) C(7) 0.028(3) 0.029(3) 0.038(3) -0.006(2) 0.014(2) -0.003(2) C(8) 0.022(2) 0.025(2) 0.039(3) 0.004(2) -0.002(2) -0.006(2) C(9) 0.043(3) 0.035(3) 0.029(2) -0.006(2) -0.003(2) -0.005(2) C(10) 0.024(3) 0.032(3) 0.033(3) 0.000(2) -0.001(2) -0.007(2) C(11) 0.042(3) 0.020(2) 0.032(2) 0.001(2) 0.004(2) -0.004(2) C(12) 0.039(3) 0.019(2) 0.044(3) -0.002(2) 0.005(2) 0.003(2) C(13) 0.024(2) 0.022(2) 0.019(2) -0.001(2) 0.000(2) -0.002(2) C(14) 0.027(2) 0.015(2) 0.026(2) 0.003(2) 0.003(2) 0.005(2) C(15) 0.035(3) 0.025(2) 0.020(2) 0.001(2) -0.001(2) -0.005(2) C(16) 0.033(3) 0.027(2) 0.026(2) -0.000(2) -0.008(2) -0.008(2) C(17) 0.021(2) 0.014(2) 0.030(2) -0.007(2) -0.001(2) -0.005(2) C(18) 0.019(2) 0.019(2) 0.025(2) -0.0022(19) -0.003(2) 0.002(2) C(19) 0.030(3) 0.027(2) 0.032(2) 0.002(2) 0.006(2) 0.001(2) C(20) 0.047(4) 0.036(3) 0.027(2) 0.001(3) -0.011(2) 0.000(2) C(21) 0.038(3) 0.032(3) 0.033(3) -0.000(2) -0.009(2) -0.009(2) C(22) 0.026(2) 0.023(2) 0.031(2) -0.010(2) 0.000(2) -0.000(2) C(23) 0.030(3) 0.038(3) 0.035(3) 0.006(2) -0.007(2) -0.002(2) C(24) 0.037(3) 0.033(3) 0.042(3) 0.009(2) -0.004(3) -0.005(2) C(25) 0.027(3) 0.022(2) 0.025(2) -0.009(2) 0.004(2) -0.0030(19) C(26) 0.031(3) 0.025(2) 0.027(2) -0.001(2) -0.010(2) -0.002(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rh(1) Rh(2) 2.6257(5) yes . . Rh(1) S(1) 2.2776(15) yes . . Rh(1) C(1) 2.227(5) yes . . Rh(1) C(2) 2.281(5) yes . . Rh(1) C(3) 2.264(5) yes . . Rh(1) C(4) 2.244(5) yes . . Rh(1) C(5) 2.224(4) yes . . Rh(1) C(25) 2.063(4) yes . . Rh(1) C(26) 2.047(5) yes . . Rh(2) S(2) 2.2842(15) yes . . Rh(2) C(13) 2.300(5) yes . . Rh(2) C(14) 2.306(5) yes . . Rh(2) C(15) 2.239(5) yes . . Rh(2) C(16) 2.236(5) yes . . Rh(2) C(17) 2.220(4) yes . . Rh(2) C(25) 2.022(4) yes . . Rh(2) C(26) 2.048(5) yes . . S(1) O(1) 1.382(5) yes . . S(1) O(2) 1.424(5) yes . . S(1) O(5) 1.726(16) yes . . S(1) O(6) 1.719(5) yes . . S(2) O(3) 1.440(5) yes . . S(2) O(4) 1.193(16) yes . . S(2) O(5) 1.970(16) yes . . S(2) O(6) 1.690(5) yes . . O(1) O(5) 1.550(17) yes . . O(4) O(6) 1.599(19) yes . . O(5) O(6) 1.577(16) yes . . C(1) C(2) 1.432(7) yes . . C(1) C(5) 1.447(7) yes . . C(1) C(6) 1.505(7) yes . . C(2) C(3) 1.428(7) yes . . C(2) C(7) 1.498(7) yes . . C(3) C(4) 1.439(7) yes . . C(3) C(8) 1.483(7) yes . . C(4) C(5) 1.433(7) yes . . C(4) C(9) 1.514(7) yes . . C(5) C(10) 1.486(7) yes . . C(6) C(11) 1.540(7) yes . . C(11) C(12) 1.518(7) yes . . C(13) C(14) 1.428(7) yes . . C(13) C(17) 1.412(7) yes . . C(13) C(18) 1.511(7) yes . . C(14) C(15) 1.432(7) yes . . C(14) C(19) 1.501(7) yes . . C(15) C(16) 1.423(7) yes . . C(15) C(20) 1.513(7) yes . . C(16) C(17) 1.427(7) yes . . C(16) C(21) 1.521(8) yes . . C(17) C(22) 1.503(7) yes . . C(18) C(23) 1.558(7) yes . . C(23) C(24) 1.494(8) yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Rh(2) Rh(1) S(1) 93.74(4) yes . . . Rh(2) Rh(1) C(1) 148.27(13) yes . . . Rh(2) Rh(1) C(2) 118.90(13) yes . . . Rh(2) Rh(1) C(3) 112.07(12) yes . . . Rh(2) Rh(1) C(4) 133.74(12) yes . . . Rh(2) Rh(1) C(5) 170.68(13) yes . . . Rh(2) Rh(1) C(25) 49.33(13) yes . . . Rh(2) Rh(1) C(26) 50.12(14) yes . . . S(1) Rh(1) C(1) 102.63(14) yes . . . S(1) Rh(1) C(2) 139.03(13) yes . . . S(1) Rh(1) C(3) 150.65(13) yes . . . S(1) Rh(1) C(4) 114.11(13) yes . . . S(1) Rh(1) C(5) 89.79(14) yes . . . S(1) Rh(1) C(25) 89.17(17) yes . . . S(1) Rh(1) C(26) 87.24(17) yes . . . C(1) Rh(1) C(2) 37.02(19) yes . . . C(1) Rh(1) C(3) 62.36(18) yes . . . C(1) Rh(1) C(4) 62.54(18) yes . . . C(1) Rh(1) C(5) 37.94(18) yes . . . C(1) Rh(1) C(25) 155.4(2) yes . . . C(1) Rh(1) C(26) 103.20(19) yes . . . C(2) Rh(1) C(3) 36.62(18) yes . . . C(2) Rh(1) C(4) 61.40(18) yes . . . C(2) Rh(1) C(5) 62.12(18) yes . . . C(2) Rh(1) C(25) 130.4(2) yes . . . C(2) Rh(1) C(26) 95.2(2) yes . . . C(3) Rh(1) C(4) 37.22(18) yes . . . C(3) Rh(1) C(5) 62.63(18) yes . . . C(3) Rh(1) C(25) 97.1(2) yes . . . C(3) Rh(1) C(26) 119.7(2) yes . . . C(4) Rh(1) C(5) 37.42(18) yes . . . C(4) Rh(1) C(25) 92.98(19) yes . . . C(4) Rh(1) C(26) 155.8(2) yes . . . C(5) Rh(1) C(25) 122.21(18) yes . . . C(5) Rh(1) C(26) 138.82(19) yes . . . C(25) Rh(1) C(26) 98.82(19) yes . . . Rh(1) Rh(2) S(2) 94.27(4) yes . . . Rh(1) Rh(2) C(13) 120.43(12) yes . . . Rh(1) Rh(2) C(14) 116.09(12) yes . . . Rh(1) Rh(2) C(15) 137.36(13) yes . . . Rh(1) Rh(2) C(16) 174.13(13) yes . . . Rh(1) Rh(2) C(17) 146.86(13) yes . . . Rh(1) Rh(2) C(25) 50.69(13) yes . . . Rh(1) Rh(2) C(26) 50.12(14) yes . . . S(2) Rh(2) C(13) 138.34(13) yes . . . S(2) Rh(2) C(14) 145.54(13) yes . . . S(2) Rh(2) C(15) 109.45(15) yes . . . S(2) Rh(2) C(16) 87.50(16) yes . . . S(2) Rh(2) C(17) 102.08(13) yes . . . S(2) Rh(2) C(25) 87.96(17) yes . . . S(2) Rh(2) C(26) 88.98(17) yes . . . C(13) Rh(2) C(14) 36.12(17) yes . . . C(13) Rh(2) C(15) 61.10(18) yes . . . C(13) Rh(2) C(16) 60.43(19) yes . . . C(13) Rh(2) C(17) 36.35(18) yes . . . C(13) Rh(2) C(25) 96.6(2) yes . . . C(13) Rh(2) C(26) 130.2(2) yes . . . C(14) Rh(2) C(15) 36.68(19) yes . . . C(14) Rh(2) C(16) 60.72(19) yes . . . C(14) Rh(2) C(17) 61.37(18) yes . . . C(14) Rh(2) C(25) 123.4(2) yes . . . C(14) Rh(2) C(26) 98.0(2) yes . . . C(15) Rh(2) C(16) 37.08(19) yes . . . C(15) Rh(2) C(17) 62.68(18) yes . . . C(15) Rh(2) C(25) 157.7(2) yes . . . C(15) Rh(2) C(26) 94.20(19) yes . . . C(16) Rh(2) C(17) 37.34(19) yes . . . C(16) Rh(2) C(25) 135.06(19) yes . . . C(16) Rh(2) C(26) 124.4(2) yes . . . C(17) Rh(2) C(25) 100.86(19) yes . . . C(17) Rh(2) C(26) 156.5(2) yes . . . C(25) Rh(2) C(26) 100.2(2) yes . . . Rh(1) S(1) O(1) 115.8(2) yes . . . Rh(1) S(1) O(2) 114.5(2) yes . . . Rh(1) S(1) O(5) 106.1(5) yes . . . Rh(1) S(1) O(6) 107.23(18) yes . . . O(1) S(1) O(2) 115.5(3) yes . . . O(1) S(1) O(5) 58.6(5) yes . . . O(1) S(1) O(6) 107.1(2) yes . . . O(2) S(1) O(5) 134.7(5) yes . . . O(2) S(1) O(6) 93.6(2) yes . . . O(5) S(1) O(6) 54.5(5) yes . . . Rh(2) S(2) O(3) 110.97(19) yes . . . Rh(2) S(2) O(4) 133.2(7) yes . . . Rh(2) S(2) O(5) 103.6(4) yes . . . Rh(2) S(2) O(6) 106.32(18) yes . . . O(3) S(2) O(4) 114.3(8) yes . . . O(3) S(2) O(5) 69.1(5) yes . . . O(3) S(2) O(6) 114.2(2) yes . . . O(4) S(2) O(5) 102.7(9) yes . . . O(4) S(2) O(6) 64.7(9) yes . . . O(5) S(2) O(6) 50.4(5) yes . . . S(1) O(1) O(5) 71.9(6) yes . . . S(2) O(4) O(6) 72.8(8) yes . . . S(1) O(5) S(2) 105.5(7) yes . . . S(1) O(5) O(1) 49.5(5) yes . . . S(1) O(5) O(6) 62.5(6) yes . . . S(2) O(5) O(1) 154.6(10) yes . . . S(2) O(5) O(6) 55.6(5) yes . . . O(1) O(5) O(6) 106.3(10) yes . . . S(1) O(6) S(2) 119.5(3) yes . . . S(1) O(6) O(4) 162.0(6) yes . . . S(1) O(6) O(5) 63.0(6) yes . . . S(2) O(6) O(4) 42.4(6) yes . . . S(2) O(6) O(5) 74.1(6) yes . . . O(4) O(6) O(5) 104.9(9) yes . . . Rh(1) C(1) C(2) 73.5(2) yes . . . Rh(1) C(1) C(5) 70.9(2) yes . . . Rh(1) C(1) C(6) 123.3(3) yes . . . C(2) C(1) C(5) 107.7(4) yes . . . C(2) C(1) C(6) 126.9(4) yes . . . C(5) C(1) C(6) 125.3(4) yes . . . Rh(1) C(2) C(1) 69.4(2) yes . . . Rh(1) C(2) C(3) 71.0(2) yes . . . Rh(1) C(2) C(7) 127.4(3) yes . . . C(1) C(2) C(3) 108.8(4) yes . . . C(1) C(2) C(7) 125.3(4) yes . . . C(3) C(2) C(7) 125.9(4) yes . . . Rh(1) C(3) C(2) 72.3(2) yes . . . Rh(1) C(3) C(4) 70.6(2) yes . . . Rh(1) C(3) C(8) 129.2(3) yes . . . C(2) C(3) C(4) 107.4(4) yes . . . C(2) C(3) C(8) 127.9(4) yes . . . C(4) C(3) C(8) 124.1(4) yes . . . Rh(1) C(4) C(3) 72.2(2) yes . . . Rh(1) C(4) C(5) 70.5(2) yes . . . Rh(1) C(4) C(9) 126.7(3) yes . . . C(3) C(4) C(5) 108.7(4) yes . . . C(3) C(4) C(9) 125.6(4) yes . . . C(5) C(4) C(9) 125.6(4) yes . . . Rh(1) C(5) C(1) 71.1(2) yes . . . Rh(1) C(5) C(4) 72.0(2) yes . . . Rh(1) C(5) C(10) 128.1(3) yes . . . C(1) C(5) C(4) 107.4(4) yes . . . C(1) C(5) C(10) 127.0(4) yes . . . C(4) C(5) C(10) 125.2(4) yes . . . C(1) C(6) C(11) 112.8(4) yes . . . C(6) C(11) C(12) 111.4(4) yes . . . Rh(2) C(13) C(14) 72.2(2) yes . . . Rh(2) C(13) C(17) 68.7(2) yes . . . Rh(2) C(13) C(18) 133.2(3) yes . . . C(14) C(13) C(17) 108.9(4) yes . . . C(14) C(13) C(18) 124.9(4) yes . . . C(17) C(13) C(18) 125.4(4) yes . . . Rh(2) C(14) C(13) 71.7(2) yes . . . Rh(2) C(14) C(15) 69.1(2) yes . . . Rh(2) C(14) C(19) 127.1(3) yes . . . C(13) C(14) C(15) 107.6(4) yes . . . C(13) C(14) C(19) 126.4(4) yes . . . C(15) C(14) C(19) 125.9(4) yes . . . Rh(2) C(15) C(14) 74.2(2) yes . . . Rh(2) C(15) C(16) 71.3(2) yes . . . Rh(2) C(15) C(20) 126.2(3) yes . . . C(14) C(15) C(16) 107.1(4) yes . . . C(14) C(15) C(20) 125.8(4) yes . . . C(16) C(15) C(20) 126.6(5) yes . . . Rh(2) C(16) C(15) 71.6(3) yes . . . Rh(2) C(16) C(17) 70.7(2) yes . . . Rh(2) C(16) C(21) 123.5(3) yes . . . C(15) C(16) C(17) 108.9(4) yes . . . C(15) C(16) C(21) 123.9(4) yes . . . C(17) C(16) C(21) 127.1(4) yes . . . Rh(2) C(17) C(13) 74.9(2) yes . . . Rh(2) C(17) C(16) 71.9(2) yes . . . Rh(2) C(17) C(22) 123.5(3) yes . . . C(13) C(17) C(16) 107.1(4) yes . . . C(13) C(17) C(22) 127.4(4) yes . . . C(16) C(17) C(22) 125.2(4) yes . . . C(13) C(18) C(23) 109.9(4) yes . . . C(18) C(23) C(24) 114.8(4) yes . . . Rh(1) C(25) Rh(2) 79.99(17) yes . . . Rh(1) C(26) Rh(2) 79.76(19) yes . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(1) C(8) 3.373(7) ? . 1_455 O(1) C(11) 3.581(7) ? . 2_466 O(2) C(10) 3.583(7) ? . 2_466 O(2) C(20) 3.464(7) ? . 3_555 O(3) C(18) 3.540(6) ? . 2_456 O(3) C(22) 3.550(6) ? . 2_456 O(3) C(23) 3.365(7) ? . 1_455 O(4) C(12) 3.521(17) ? . 3_545 O(4) C(19) 3.365(16) ? . 1_455 O(4) C(23) 3.589(19) ? . 1_455 O(5) C(8) 3.162(17) ? . 1_455 O(5) C(22) 3.499(16) ? . 2_456 O(6) C(8) 3.229(7) ? . 1_455 C(3) C(10) 3.471(7) ? . 2_566 C(4) C(10) 3.559(7) ? . 2_566 C(8) O(1) 3.373(7) ? . 1_655 C(8) O(5) 3.162(17) ? . 1_655 C(8) O(6) 3.229(7) ? . 1_655 C(8) C(22) 3.585(7) ? . 2_556 C(9) C(20) 3.583(7) ? . 4_565 C(10) O(2) 3.583(7) ? . 2_566 C(10) C(3) 3.471(7) ? . 2_466 C(10) C(4) 3.559(7) ? . 2_466 C(11) O(1) 3.581(7) ? . 2_566 C(12) O(4) 3.521(17) ? . 3_555 C(12) C(19) 3.563(8) ? . 3_655 C(18) O(3) 3.540(6) ? . 2_556 C(19) O(4) 3.365(16) ? . 1_655 C(19) C(12) 3.563(8) ? . 3_645 C(20) O(2) 3.464(7) ? . 3_545 C(20) C(9) 3.583(7) ? . 4_564 C(22) O(3) 3.550(6) ? . 2_556 C(22) O(5) 3.499(16) ? . 2_556 C(22) C(8) 3.585(7) ? . 2_456 C(23) O(3) 3.365(7) ? . 1_655 C(23) O(4) 3.589(19) ? . 1_655 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================