data_globalSupplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof. Wing-Tak Wong' _publ_contact_author_email wtwong@hkucc.hku.hk _publ_contact_author_fax '(852) 2547 2933' _publ_contact_author_phone '(852) 2859 2157' _publ_contact_author_address ; Department of Chemistry The University of Hong Kong Pokfulam Road, Pokfulam, Hong Kong SAR, P. R. CHINA ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category FA loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Po-Kwan Jasmine Lau.' . ; Department of Chemistry The University of Hong Kong Pokfulam Road, Pokfulam, Hong Kong SAR, P. R. CHINA ; 'Wing-Tak Wong.' . ; Department of Chemistry The University of Hong Kong Pokfulam Road, Pokfulam, Hong Kong SAR, P. R. CHINA ; _publ_section_title ; Synthesis and structural characterization of a series of high-hydride content Osmium-Rhodium carbonyl complexes by the hydrogenation of arene-coordinated clusters ; _publ_section_references ; Bruker AXS Inc. (1998) SMART version 5.054, Madison, Wisconsin, USA. Bruker AXS Inc. (1999) SAINT, version 6.02, Madison, Wisconsin, USA. Farrugia, L.J. (1997) Ortep-3 J. Appl. Cryst. 30, 565. Johnson, C. K. (1976) ORTEP-II, A FORTRAN Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Rigaku/MSC and Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Sheldrick, G.M. (1997) SHELXS-97, Gottingen University, Gottingen, Germany. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_exptl_refinement ; All non-H atoms were refined anisotropically. The metal-bound hydrido atoms were placed at their geometrically calculated positions and not refined. ; #============================================================================== # 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 #============================================================================== data__wt0878w _database_code_depnum_ccdc_archive 'CCDC 262816' # JAS002---compound 1 _audit_creation_date 2005-05-12 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? _publ_section_references ; Bruker AXS Inc. (1998) SMART version 5.054, Madison, Wisconsin, USA. Bruker AXS Inc. (1999) SAINT, version 6.02, Madison, Wisconsin, USA. Farrugia, L.J. (1997) Ortep-3 J. Appl. Cryst. 30, 565. Johnson, C. K. (1976) ORTEP-II, A FORTRAN Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Rigaku/MSC and Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Sheldrick, G.M. (1997) SHELXS-97, Gottingen University, Gottingen, Germany. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; The C-bound H atoms were placed at their geometrically calculated positions with C-H = 0.95 \%A and in the riding model with U~iso~(H) = 1.2 U~eq~(C). ; #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C25 H10 O17 Os5 Rh2 ' _chemical_formula_moiety 'C25 H10 O17 Os5 Rh2 ' _chemical_formula_weight 1739.15 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _cell_length_a 9.503(2) _cell_length_b 10.726(2) _cell_length_c 18.029(3) _cell_angle_alpha 89.28(1) _cell_angle_beta 76.51(1) _cell_angle_gamma 67.26(1) _cell_volume 1641.9(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 19382 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 27.6 _cell_measurement_temperature 298(1) #------------------------------------------------------------------------------ _exptl_crystal_description cube _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 3.518 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1532.00 _exptl_absorpt_coefficient_mu 20.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.614 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15012 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.6 _diffrn_measured_fraction_theta_max 0.99 _diffrn_reflns_theta_full 27.6 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7506 _reflns_number_gt 4436 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0420 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 4465 _refine_ls_number_parameters 452 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + 1.0000\s(Fo^2^) + 0.0200]' _refine_ls_shift/su_max 0.0070 _refine_diff_density_max 1.63 _refine_diff_density_min -2.29 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os Os -1.216 7.603 ; 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) ; C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 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) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 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 Os(1) Os 0.13001(8) 0.75628(7) 0.18415(4) 0.0320(2) Uani 1.00 1 d . . . Os(2) Os -0.11940(8) 0.67097(7) 0.20930(4) 0.0315(2) Uani 1.00 1 d . . . Os(3) Os -0.19399(9) 0.74814(7) 0.36682(4) 0.0384(2) Uani 1.00 1 d . . . Os(4) Os 0.11376(8) 0.55855(7) 0.29038(4) 0.0329(2) Uani 1.00 1 d . . . Os(5) Os 0.19206(8) 0.49622(7) 0.12957(4) 0.0385(2) Uani 1.00 1 d . . . Rh(1) Rh 0.0573(2) 0.8297(1) 0.33708(8) 0.0344(4) Uani 1.00 1 d . . . Rh(2) Rh -0.1676(2) 0.93178(13) 0.25697(8) 0.0331(4) Uani 1.00 1 d . . . O(1) O 0.484(2) 0.650(1) 0.1197(9) 0.069(5) Uani 1.00 1 d . . . O(2) O 0.110(2) 0.882(2) 0.0349(8) 0.078(5) Uani 1.00 1 d . . . O(3) O -0.162(2) 0.753(2) 0.0510(8) 0.072(5) Uani 1.00 1 d . . . O(4) O -0.476(2) 0.798(2) 0.2619(8) 0.063(5) Uani 1.00 1 d . . . O(5) O -0.181(2) 0.411(1) 0.2006(9) 0.072(6) Uani 1.00 1 d . . . O(6) O -0.284(2) 0.504(2) 0.4055(9) 0.081(6) Uani 1.00 1 d . . . O(7) O -0.155(2) 0.793(2) 0.5252(8) 0.075(6) Uani 1.00 1 d . . . O(8) O -0.531(2) 0.947(1) 0.4249(8) 0.076(5) Uani 1.00 1 d . . . O(9) O 0.472(2) 0.446(2) 0.2566(9) 0.077(5) Uani 1.00 1 d . . . O(10) O 0.071(2) 0.290(1) 0.2994(9) 0.080(6) Uani 1.00 1 d . . . O(11) O 0.138(2) 0.524(2) 0.4543(8) 0.074(6) Uani 1.00 1 d . . . O(12) O 0.157(2) 0.228(2) 0.1157(9) 0.075(6) Uani 1.00 1 d . . . O(13) O 0.546(2) 0.346(2) 0.0776(11) 0.091(6) Uani 1.00 1 d . . . O(14) O 0.170(2) 0.554(2) -0.0334(8) 0.075(5) Uani 1.00 1 d . . . O(15) O 0.342(2) 0.717(2) 0.4029(9) 0.081(6) Uani 1.00 1 d . . . O(16) O -0.081(2) 1.091(2) 0.4410(11) 0.106(7) Uani 1.00 1 d . . . O(17) O 0.213(2) 0.9878(12) 0.2331(8) 0.057(5) Uani 1.00 1 d . . . C(1) C 0.349(2) 0.681(2) 0.1453(11) 0.052(6) Uani 1.00 1 d . . . C(2) C 0.114(2) 0.834(2) 0.0926(12) 0.051(6) Uani 1.00 1 d . . . C(3) C -0.140(2) 0.720(2) 0.1095(12) 0.048(6) Uani 1.00 1 d . . . C(4) C -0.341(2) 0.758(2) 0.2498(11) 0.045(6) Uani 1.00 1 d . . . C(5) C -0.151(2) 0.509(2) 0.2039(10) 0.043(6) Uani 1.00 1 d . . . C(6) C -0.253(2) 0.596(2) 0.3932(10) 0.048(6) Uani 1.00 1 d . . . C(7) C -0.164(2) 0.781(2) 0.4660(13) 0.060(7) Uani 1.00 1 d . . . C(8) C -0.401(3) 0.875(2) 0.4013(11) 0.053(6) Uani 1.00 1 d . . . C(9) C 0.339(2) 0.486(2) 0.2651(11) 0.055(7) Uani 1.00 1 d . . . C(10) C 0.088(2) 0.391(2) 0.2947(10) 0.048(6) Uani 1.00 1 d . . . C(11) C 0.118(2) 0.548(2) 0.3952(12) 0.051(6) Uani 1.00 1 d . . . C(12) C 0.171(2) 0.327(2) 0.1223(12) 0.056(7) Uani 1.00 1 d . . . C(13) C 0.407(3) 0.406(2) 0.0971(13) 0.070(8) Uani 1.00 1 d . . . C(14) C 0.181(2) 0.534(2) 0.0280(13) 0.058(7) Uani 1.00 1 d . . . C(15) C 0.238(3) 0.757(2) 0.3766(12) 0.058(7) Uani 1.00 1 d . . . C(16) C -0.032(3) 0.994(2) 0.4005(13) 0.063(8) Uani 1.00 1 d . . . C(17) C 0.170(2) 0.898(2) 0.2370(11) 0.052(6) Uani 1.00 1 d . . . C(18) C -0.223(2) 1.065(2) 0.1588(11) 0.054(6) Uani 1.00 1 d . . . C(19) C -0.363(2) 1.055(2) 0.1949(12) 0.052(6) Uani 1.00 1 d . . . C(20) C -0.425(2) 1.096(2) 0.2743(12) 0.051(6) Uani 1.00 1 d . . . C(21) C -0.352(2) 1.149(2) 0.3154(10) 0.047(6) Uani 1.00 1 d . . . C(22) C -0.205(3) 1.156(2) 0.2770(13) 0.059(7) Uani 1.00 1 d . . . C(23) C -0.143(2) 1.113(2) 0.2000(13) 0.056(7) Uani 1.00 1 d . . . C(24) C -0.457(3) 1.021(3) 0.148(2) 0.13(1) Uani 1.00 1 d . . . C(25) C -0.422(3) 1.214(2) 0.398(1) 0.099(10) Uani 1.00 1 d . . . H(1) H -0.181(2) 1.039(2) 0.1054(11) 0.060(7) Uiso 1.00 1 c . . . H(2) H -0.519(2) 1.086(2) 0.3001(12) 0.055(7) Uiso 1.00 1 c . . . H(3) H -0.152(3) 1.190(2) 0.3044(13) 0.069(8) Uiso 1.00 1 c . . . H(4) H -0.045(2) 1.114(2) 0.1749(13) 0.065(8) Uiso 1.00 1 c . . . H(5) H -0.485(3) 1.088(3) 0.113(2) 0.17(2) Uiso 1.00 1 c . . . H(6) H -0.550(3) 1.018(3) 0.180(2) 0.17(2) Uiso 1.00 1 c . . . H(7) H -0.395(3) 0.935(3) 0.120(2) 0.17(2) Uiso 1.00 1 c . . . H(8) H -0.519(3) 1.204(2) 0.417(1) 0.101(10) Uiso 1.00 1 c . . . H(9) H -0.441(3) 1.307(2) 0.400(1) 0.100(10) Uiso 1.00 1 c . . . H(10) H -0.351(3) 1.169(2) 0.428(1) 0.100(10) Uiso 1.00 1 c . . . 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 Os(1) 0.0333(4) 0.0324(4) 0.0306(4) -0.0159(3) -0.0036(3) 0.0072(3) Os(2) 0.0329(4) 0.0324(4) 0.0329(4) -0.0155(3) -0.0108(3) 0.0075(3) Os(3) 0.0391(4) 0.0439(4) 0.0333(4) -0.0209(4) -0.0035(3) 0.0089(3) Os(4) 0.0341(4) 0.0335(4) 0.0338(4) -0.0147(3) -0.0113(3) 0.0125(3) Os(5) 0.0389(4) 0.0350(4) 0.0367(4) -0.0126(3) -0.0037(3) 0.0009(3) Rh(1) 0.0366(8) 0.0383(8) 0.0322(8) -0.0172(6) -0.0117(6) -0.0000(6) Rh(2) 0.0339(8) 0.0284(7) 0.0353(8) -0.0127(6) -0.0050(6) 0.0089(6) O(1) 0.041(9) 0.066(10) 0.092(12) -0.022(7) -0.001(8) -0.004(8) O(2) 0.070(11) 0.096(12) 0.054(10) -0.022(9) -0.010(8) 0.041(9) O(3) 0.085(11) 0.078(11) 0.051(10) -0.026(9) -0.027(9) 0.021(8) O(4) 0.046(9) 0.095(11) 0.054(9) -0.029(8) -0.020(7) 0.007(8) O(5) 0.083(11) 0.063(10) 0.098(12) -0.052(9) -0.032(9) 0.020(9) O(6) 0.109(13) 0.083(12) 0.085(12) -0.070(11) -0.032(10) 0.044(10) O(7) 0.094(12) 0.101(13) 0.040(9) -0.041(10) -0.028(9) -0.007(9) O(8) 0.057(10) 0.063(10) 0.072(11) -0.010(8) 0.026(8) -0.013(8) O(9) 0.035(9) 0.097(12) 0.086(12) -0.016(8) -0.009(8) 0.012(9) O(10) 0.12(1) 0.053(9) 0.093(12) -0.060(10) -0.042(11) 0.021(9) O(11) 0.072(10) 0.114(13) 0.054(10) -0.050(10) -0.024(8) 0.040(9) O(12) 0.101(13) 0.055(10) 0.077(11) -0.046(9) -0.012(9) 0.001(8) O(13) 0.044(9) 0.073(11) 0.13(2) -0.004(9) -0.004(10) -0.011(10) O(14) 0.092(12) 0.091(12) 0.035(9) -0.027(10) -0.018(8) 0.012(8) O(15) 0.059(10) 0.12(1) 0.088(12) -0.052(10) -0.036(9) 0.034(10) O(16) 0.13(2) 0.09(1) 0.09(1) -0.029(12) -0.050(12) -0.031(11) O(17) 0.067(9) 0.047(8) 0.070(10) -0.041(7) -0.007(7) 0.002(7) C(1) 0.042(12) 0.051(12) 0.054(13) -0.011(10) -0.006(10) -0.015(10) C(2) 0.040(11) 0.046(12) 0.06(1) -0.010(9) -0.005(10) 0.004(10) C(3) 0.044(12) 0.042(11) 0.049(13) -0.012(9) -0.005(10) 0.005(10) C(4) 0.039(11) 0.046(11) 0.051(12) -0.018(9) -0.011(9) -0.004(9) C(5) 0.035(10) 0.051(12) 0.048(12) -0.015(9) -0.024(9) 0.008(9) C(6) 0.040(11) 0.057(13) 0.036(11) -0.009(10) -0.009(9) 0.003(10) C(7) 0.055(13) 0.07(2) 0.048(13) -0.028(11) 0.003(11) 0.001(11) C(8) 0.058(13) 0.052(12) 0.046(12) -0.031(11) 0.008(10) -0.009(10) C(9) 0.044(12) 0.07(1) 0.050(13) -0.016(11) -0.012(10) 0.016(11) C(10) 0.063(13) 0.044(11) 0.034(11) -0.018(10) -0.008(9) 0.005(9) C(11) 0.056(12) 0.055(12) 0.06(1) -0.033(10) -0.033(11) 0.039(11) C(12) 0.051(13) 0.046(12) 0.06(1) -0.013(10) 0.001(10) -0.004(10) C(13) 0.08(2) 0.033(12) 0.08(2) -0.003(12) -0.02(1) -0.008(11) C(14) 0.053(13) 0.056(13) 0.06(2) -0.013(11) -0.023(12) -0.001(11) C(15) 0.06(1) 0.07(1) 0.05(1) -0.033(12) -0.015(11) 0.010(11) C(16) 0.07(2) 0.08(2) 0.06(2) -0.041(13) -0.032(12) 0.012(13) C(17) 0.043(11) 0.056(13) 0.051(13) -0.021(10) 0.003(9) 0.003(10) C(18) 0.051(13) 0.057(13) 0.041(12) -0.009(11) -0.010(10) 0.016(10) C(19) 0.046(12) 0.051(12) 0.06(1) -0.017(10) -0.014(11) 0.018(10) C(20) 0.030(10) 0.042(11) 0.07(1) -0.007(9) 0.003(10) 0.019(10) C(21) 0.060(13) 0.030(10) 0.031(10) -0.001(9) -0.003(10) 0.010(8) C(22) 0.07(1) 0.034(11) 0.07(2) -0.015(10) -0.018(12) 0.016(11) C(23) 0.07(1) 0.020(9) 0.08(2) -0.019(9) -0.004(12) 0.021(10) C(24) 0.09(2) 0.12(3) 0.21(4) -0.05(2) -0.06(3) 0.05(3) C(25) 0.10(2) 0.07(2) 0.08(2) 0.01(2) -0.01(2) 0.01(1) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' #============================================================================== # 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 Os(1) Os(2) 2.797(1) yes . . Os(1) Os(4) 2.864(1) yes . . Os(1) Os(5) 2.761(1) yes . . Os(1) Rh(1) 2.728(2) yes . . Os(1) Rh(2) 2.735(1) yes . . Os(1) C(1) 1.87(2) yes . . Os(1) C(2) 1.85(2) yes . . Os(1) C(17) 2.00(2) yes . . Os(2) Os(3) 2.814(1) yes . . Os(2) Os(4) 2.811(1) yes . . Os(2) Os(5) 2.8520(8) yes . . Os(2) Rh(2) 2.768(2) yes . . Os(2) C(3) 1.90(2) yes . . Os(2) C(4) 1.90(2) yes . . Os(2) C(5) 1.88(2) yes . . Os(3) Os(4) 2.8600(8) yes . . Os(3) Rh(1) 2.786(2) yes . . Os(3) Rh(2) 2.814(2) yes . . Os(3) C(6) 1.94(2) yes . . Os(3) C(7) 1.93(2) yes . . Os(3) C(8) 1.87(2) yes . . Os(4) Os(5) 2.840(1) yes . . Os(4) Rh(1) 2.846(2) yes . . Os(4) C(9) 1.91(2) yes . . Os(4) C(10) 1.90(2) yes . . Os(4) C(11) 1.90(2) yes . . Os(5) C(12) 1.91(2) yes . . Os(5) C(13) 1.84(2) yes . . Os(5) C(14) 1.89(2) yes . . Rh(1) Rh(2) 2.729(2) yes . . Rh(1) C(15) 1.90(2) yes . . Rh(1) C(16) 1.89(2) yes . . Rh(1) C(17) 2.15(2) yes . . Rh(2) C(18) 2.29(2) yes . . Rh(2) C(19) 2.34(2) yes . . Rh(2) C(20) 2.35(2) yes . . Rh(2) C(21) 2.37(2) yes . . Rh(2) C(22) 2.31(2) yes . . Rh(2) C(23) 2.25(2) yes . . O(1) C(1) 1.17(2) yes . . O(2) C(2) 1.16(3) yes . . O(3) C(3) 1.15(3) yes . . O(4) C(4) 1.15(2) yes . . O(5) C(5) 1.20(3) yes . . O(6) C(6) 1.14(3) yes . . O(7) C(7) 1.10(3) yes . . O(8) C(8) 1.15(2) yes . . O(9) C(9) 1.14(3) yes . . O(10) C(10) 1.15(3) yes . . O(11) C(11) 1.13(3) yes . . O(12) C(12) 1.13(3) yes . . O(13) C(13) 1.19(3) yes . . O(14) C(14) 1.14(3) yes . . O(15) C(15) 1.13(3) yes . . O(16) C(16) 1.14(3) yes . . O(17) C(17) 1.18(3) yes . . C(18) C(19) 1.39(3) yes . . C(18) C(23) 1.40(4) yes . . C(18) H(1) 0.95(3) no . . C(19) C(20) 1.42(3) yes . . C(19) C(24) 1.50(5) yes . . C(20) C(21) 1.39(3) yes . . C(20) H(2) 0.95(3) no . . C(21) C(22) 1.43(3) yes . . C(21) C(25) 1.53(3) yes . . C(22) C(23) 1.38(3) yes . . C(22) H(3) 0.95(4) no . . C(23) H(4) 0.95(3) no . . C(24) H(5) 0.95(5) no . . C(24) H(6) 0.95(4) no . . C(24) H(7) 0.95(4) no . . C(25) H(8) 0.95(4) no . . C(25) H(9) 0.95(4) no . . C(25) H(10) 0.95(4) no . . 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 Os(2) Os(1) Os(4) 59.52(3) yes . . . Os(2) Os(1) Os(5) 61.74(3) yes . . . Os(2) Os(1) Rh(1) 89.51(4) yes . . . Os(2) Os(1) Rh(2) 60.02(4) yes . . . Os(2) Os(1) C(1) 138.2(7) yes . . . Os(2) Os(1) C(2) 100.6(7) yes . . . Os(2) Os(1) C(17) 133.7(5) yes . . . Os(4) Os(1) Os(5) 60.61(3) yes . . . Os(4) Os(1) Rh(1) 61.11(4) yes . . . Os(4) Os(1) Rh(2) 90.99(4) yes . . . Os(4) Os(1) C(1) 97.1(6) yes . . . Os(4) Os(1) C(2) 154.3(7) yes . . . Os(4) Os(1) C(17) 107.3(6) yes . . . Os(5) Os(1) Rh(1) 121.71(4) yes . . . Os(5) Os(1) Rh(2) 121.73(5) yes . . . Os(5) Os(1) C(1) 76.7(7) yes . . . Os(5) Os(1) C(2) 96.5(7) yes . . . Os(5) Os(1) C(17) 155.2(5) yes . . . Rh(1) Os(1) Rh(2) 59.93(4) yes . . . Rh(1) Os(1) C(1) 109.9(7) yes . . . Rh(1) Os(1) C(2) 140.2(6) yes . . . Rh(1) Os(1) C(17) 51.2(6) yes . . . Rh(2) Os(1) C(1) 161.4(7) yes . . . Rh(2) Os(1) C(2) 92.0(5) yes . . . Rh(2) Os(1) C(17) 77.5(5) yes . . . C(1) Os(1) C(2) 87.9(8) yes . . . C(1) Os(1) C(17) 84.1(9) yes . . . C(2) Os(1) C(17) 98.2(9) yes . . . Os(3) Os(2) Os(4) 61.12(3) yes . . . Os(3) Os(2) Os(5) 121.17(4) yes . . . Os(3) Os(2) Rh(2) 60.54(4) yes . . . Os(3) Os(2) C(3) 148.9(5) yes . . . Os(3) Os(2) C(4) 68.7(6) yes . . . Os(3) Os(2) C(5) 105.0(5) yes . . . Os(3) Os(2) Os(1) 90.22(4) yes . . . Os(4) Os(2) Os(5) 60.19(2) yes . . . Os(4) Os(2) Rh(2) 91.44(4) yes . . . Os(4) Os(2) C(3) 140.5(6) yes . . . Os(4) Os(2) C(4) 127.8(6) yes . . . Os(4) Os(2) C(5) 92.7(6) yes . . . Os(4) Os(2) Os(1) 61.42(3) yes . . . Os(5) Os(2) Rh(2) 117.35(4) yes . . . Os(5) Os(2) C(3) 83.5(5) yes . . . Os(5) Os(2) C(4) 166.0(7) yes . . . Os(5) Os(2) C(5) 81.4(5) yes . . . Os(5) Os(2) Os(1) 58.51(3) yes . . . Rh(2) Os(2) C(3) 92.3(6) yes . . . Rh(2) Os(2) C(4) 75.7(7) yes . . . Rh(2) Os(2) C(5) 160.1(5) yes . . . Rh(2) Os(2) Os(1) 58.87(4) yes . . . C(3) Os(2) C(4) 91.1(8) yes . . . C(3) Os(2) C(5) 96.8(9) yes . . . C(3) Os(2) Os(1) 87.5(7) yes . . . C(4) Os(2) C(5) 86.4(8) yes . . . C(4) Os(2) Os(1) 134.4(7) yes . . . C(5) Os(2) Os(1) 139.0(5) yes . . . Os(4) Os(3) Rh(1) 60.51(3) yes . . . Os(4) Os(3) Rh(2) 89.49(3) yes . . . Os(4) Os(3) C(6) 88.6(5) yes . . . Os(4) Os(3) C(7) 101.4(5) yes . . . Os(4) Os(3) C(8) 170.9(6) yes . . . Rh(1) Os(3) Rh(2) 58.32(5) yes . . . Rh(1) Os(3) C(6) 143.8(5) yes . . . Rh(1) Os(3) C(7) 74.6(7) yes . . . Rh(1) Os(3) C(8) 120.6(8) yes . . . Rh(2) Os(3) C(6) 146.3(6) yes . . . Rh(2) Os(3) C(7) 117.7(7) yes . . . Rh(2) Os(3) C(8) 84.3(6) yes . . . C(6) Os(3) C(7) 95(1) yes . . . C(6) Os(3) C(8) 92.9(9) yes . . . C(6) Os(3) Os(2) 91.7(5) yes . . . C(7) Os(3) C(8) 87.4(9) yes . . . C(7) Os(3) Os(2) 159.3(6) yes . . . C(8) Os(3) Os(2) 111.6(7) yes . . . Os(2) Os(3) Os(4) 59.39(2) yes . . . Os(2) Os(3) Rh(1) 88.02(4) yes . . . Os(2) Os(3) Rh(2) 58.92(4) yes . . . Os(5) Os(4) Rh(1) 114.99(4) yes . . . Os(5) Os(4) C(9) 77.7(6) yes . . . Os(5) Os(4) C(10) 83.8(5) yes . . . Os(5) Os(4) C(11) 161.8(5) yes . . . Os(5) Os(4) Os(1) 57.90(3) yes . . . Rh(1) Os(4) C(9) 98.1(7) yes . . . Rh(1) Os(4) C(10) 157.6(5) yes . . . Rh(1) Os(4) C(11) 77.7(6) yes . . . Rh(1) Os(4) Os(1) 57.09(4) yes . . . C(9) Os(4) C(10) 97.9(9) yes . . . C(9) Os(4) C(11) 87.9(8) yes . . . C(9) Os(4) Os(1) 86.8(6) yes . . . C(9) Os(4) Os(2) 135.5(6) yes . . . C(9) Os(4) Os(3) 154.3(7) yes . . . C(10) Os(4) C(11) 87.3(9) yes . . . C(10) Os(4) Os(1) 139.6(6) yes . . . C(10) Os(4) Os(2) 92.6(6) yes . . . C(10) Os(4) Os(3) 102.3(5) yes . . . C(11) Os(4) Os(1) 133.1(7) yes . . . C(11) Os(4) Os(2) 135.9(5) yes . . . C(11) Os(4) Os(3) 77.5(5) yes . . . Os(2) Os(4) Os(5) 60.62(2) yes . . . Os(2) Os(4) Rh(1) 86.91(4) yes . . . Os(2) Os(4) Os(1) 59.06(3) yes . . . Os(2) Os(4) Os(3) 59.49(2) yes . . . Os(3) Os(4) Os(5) 119.99(3) yes . . . Os(3) Os(4) Rh(1) 58.45(4) yes . . . Os(3) Os(4) Os(1) 87.97(3) yes . . . C(12) Os(5) C(13) 89(1) yes . . . C(12) Os(5) C(14) 94(1) yes . . . C(12) Os(5) Os(1) 159.2(5) yes . . . C(12) Os(5) Os(2) 101.4(5) yes . . . C(12) Os(5) Os(4) 102.3(6) yes . . . C(13) Os(5) C(14) 90(1) yes . . . C(13) Os(5) Os(1) 107.6(8) yes . . . C(13) Os(5) Os(2) 164.6(9) yes . . . C(13) Os(5) Os(4) 108.0(8) yes . . . C(14) Os(5) Os(1) 97.0(7) yes . . . C(14) Os(5) Os(2) 99.6(5) yes . . . C(14) Os(5) Os(4) 154.8(5) yes . . . Os(2) Os(5) Os(1) 59.76(3) yes . . . Os(2) Os(5) Os(4) 59.19(2) yes . . . Os(4) Os(5) Os(1) 61.49(3) yes . . . Rh(2) Rh(1) C(15) 170.2(6) yes . . . Rh(2) Rh(1) C(16) 90.2(8) yes . . . Rh(2) Rh(1) C(17) 75.5(6) yes . . . Rh(2) Rh(1) Os(1) 60.16(4) yes . . . C(15) Rh(1) C(16) 94(1) yes . . . C(15) Rh(1) C(17) 95.2(9) yes . . . C(15) Rh(1) Os(1) 111.2(6) yes . . . C(15) Rh(1) Os(3) 126.1(8) yes . . . C(15) Rh(1) Os(4) 87.7(7) yes . . . C(16) Rh(1) C(17) 98.2(9) yes . . . C(16) Rh(1) Os(1) 136.4(7) yes . . . C(16) Rh(1) Os(3) 100.7(8) yes . . . C(16) Rh(1) Os(4) 157.5(8) yes . . . C(17) Rh(1) Os(1) 46.7(6) yes . . . C(17) Rh(1) Os(3) 132.5(6) yes . . . Os(3) Rh(1) Rh(2) 61.35(5) yes . . . Os(3) Rh(1) Os(1) 92.26(6) yes . . . Os(3) Rh(1) Os(4) 61.04(4) yes . . . Os(4) Rh(1) Rh(2) 91.52(6) yes . . . Os(4) Rh(1) C(17) 103.9(5) yes . . . Os(4) Rh(1) Os(1) 61.80(4) yes . . . C(18) Rh(2) C(19) 34.8(8) yes . . . C(18) Rh(2) C(20) 62.6(7) yes . . . C(18) Rh(2) C(21) 74.0(6) yes . . . C(18) Rh(2) C(22) 63.6(8) yes . . . C(18) Rh(2) C(23) 35.8(9) yes . . . C(18) Rh(2) Os(1) 98.2(4) yes . . . C(18) Rh(2) Os(2) 107.8(6) yes . . . C(18) Rh(2) Os(3) 158.4(6) yes . . . C(18) Rh(2) Rh(1) 140.9(6) yes . . . C(19) Rh(2) C(20) 35.2(7) yes . . . C(19) Rh(2) C(21) 62.5(7) yes . . . C(19) Rh(2) C(22) 74.6(8) yes . . . C(19) Rh(2) C(23) 63.5(9) yes . . . C(19) Rh(2) Os(1) 124.7(5) yes . . . C(19) Rh(2) Os(2) 99.5(6) yes . . . C(19) Rh(2) Os(3) 125.2(6) yes . . . C(19) Rh(2) Rh(1) 170.4(6) yes . . . C(20) Rh(2) C(21) 34.1(8) yes . . . C(20) Rh(2) C(22) 62.7(8) yes . . . C(20) Rh(2) C(23) 74.2(7) yes . . . C(20) Rh(2) Os(1) 159.7(5) yes . . . C(20) Rh(2) Os(2) 116.1(6) yes . . . C(20) Rh(2) Os(3) 104.5(5) yes . . . C(20) Rh(2) Rh(1) 139.3(5) yes . . . C(21) Rh(2) C(22) 35.6(8) yes . . . C(21) Rh(2) C(23) 63.3(6) yes . . . C(21) Rh(2) Os(1) 151.8(6) yes . . . C(21) Rh(2) Os(2) 147.0(6) yes . . . C(21) Rh(2) Os(3) 105.5(4) yes . . . C(21) Rh(2) Rh(1) 109.3(5) yes . . . C(22) Rh(2) C(23) 35.3(7) yes . . . C(22) Rh(2) Os(1) 116.5(5) yes . . . C(22) Rh(2) Os(2) 171.1(6) yes . . . C(22) Rh(2) Os(3) 128.3(6) yes . . . C(22) Rh(2) Rh(1) 95.8(6) yes . . . C(23) Rh(2) Os(1) 94.2(4) yes . . . C(23) Rh(2) Os(2) 136.1(5) yes . . . C(23) Rh(2) Os(3) 162.6(6) yes . . . C(23) Rh(2) Rh(1) 109.0(7) yes . . . Os(2) Rh(2) Os(1) 61.11(3) yes . . . Os(2) Rh(2) Os(3) 60.55(4) yes . . . Os(2) Rh(2) Rh(1) 90.12(5) yes . . . Os(3) Rh(2) Os(1) 91.51(4) yes . . . Os(3) Rh(2) Rh(1) 60.32(5) yes . . . Rh(1) Rh(2) Os(1) 59.92(4) yes . . . Os(1) C(1) O(1) 172(1) yes . . . Os(1) C(2) O(2) 177(1) yes . . . Os(2) C(3) O(3) 176(1) yes . . . Os(2) C(4) O(4) 166(1) yes . . . Os(2) C(5) O(5) 176(1) yes . . . Os(3) C(6) O(6) 176(1) yes . . . Os(3) C(7) O(7) 173(2) yes . . . Os(3) C(8) O(8) 175(2) yes . . . Os(4) C(9) O(9) 174(1) yes . . . Os(4) C(10) O(10) 178(1) yes . . . Os(4) C(11) O(11) 170(1) yes . . . Os(5) C(12) O(12) 177(2) yes . . . Os(5) C(13) O(13) 178(1) yes . . . Os(5) C(14) O(14) 176(2) yes . . . Rh(1) C(15) O(15) 177(1) yes . . . Rh(1) C(16) O(16) 176(2) yes . . . Os(1) C(17) O(17) 149(1) yes . . . Rh(1) C(17) Os(1) 82.1(9) yes . . . Rh(1) C(17) O(17) 128(1) yes . . . C(19) C(18) C(23) 120(1) yes . . . C(19) C(18) H(1) 119(2) no . . . C(23) C(18) H(1) 120(2) no . . . H(1) C(18) Rh(2) 127(1) no . . . Rh(2) C(18) C(19) 74(1) yes . . . Rh(2) C(18) C(23) 70(1) yes . . . C(20) C(19) C(24) 121(2) yes . . . C(24) C(19) Rh(2) 135(1) yes . . . C(24) C(19) C(18) 119(2) yes . . . Rh(2) C(19) C(20) 72(1) yes . . . Rh(2) C(19) C(18) 70(1) yes . . . C(18) C(19) C(20) 118(2) yes . . . C(21) C(20) H(2) 119(2) no . . . H(2) C(20) Rh(2) 125(1) no . . . H(2) C(20) C(19) 119(2) no . . . Rh(2) C(20) C(21) 73(1) yes . . . Rh(2) C(20) C(19) 72(1) yes . . . C(19) C(20) C(21) 121(1) yes . . . C(22) C(21) C(25) 116(2) yes . . . C(25) C(21) Rh(2) 134(1) yes . . . C(25) C(21) C(20) 124(2) yes . . . Rh(2) C(21) C(22) 69.9(9) yes . . . Rh(2) C(21) C(20) 72.0(9) yes . . . C(20) C(21) C(22) 118(1) yes . . . C(23) C(22) H(3) 120(2) no . . . H(3) C(22) Rh(2) 126(1) no . . . H(3) C(22) C(21) 120(2) no . . . Rh(2) C(22) C(23) 69(1) yes . . . Rh(2) C(22) C(21) 74(1) yes . . . C(21) C(22) C(23) 119(2) yes . . . H(4) C(23) Rh(2) 122(1) no . . . H(4) C(23) C(18) 119(2) no . . . H(4) C(23) C(22) 119(2) no . . . Rh(2) C(23) C(18) 73(1) yes . . . Rh(2) C(23) C(22) 74(1) yes . . . C(18) C(23) C(22) 121(2) yes . . . H(5) C(24) H(6) 109(3) no . . . H(5) C(24) H(7) 109(4) no . . . H(5) C(24) C(19) 109(3) no . . . H(6) C(24) H(7) 109(4) no . . . H(6) C(24) C(19) 109(3) no . . . H(7) C(24) C(19) 109(3) no . . . H(8) C(25) H(9) 109(2) no . . . H(8) C(25) H(10) 109(3) no . . . H(8) C(25) C(21) 108(3) no . . . H(9) C(25) H(10) 109(3) no . . . H(9) C(25) C(21) 110(2) no . . . H(10) C(25) C(21) 109(2) no . . . 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 Os(1) Os(2) 2.797(1) yes . 55501 Os(1) Os(4) 2.864(1) yes . 55501 Os(1) Os(5) 2.761(1) yes . 55501 Os(1) Rh(1) 2.728(2) yes . 55501 Os(1) Rh(2) 2.735(1) yes . 55501 Os(1) O(1) 3.03(1) yes . 55501 Os(1) O(2) 3.01(2) yes . 55501 Os(1) O(17) 3.08(2) yes . 55501 Os(1) C(3) 3.31(2) yes . 55501 Os(1) C(9) 3.36(2) yes . 55501 Os(1) C(14) 3.53(2) yes . 55501 Os(1) H(4) 3.57(2) no . 55501 Os(2) Os(1) 2.797(1) yes . 55501 Os(2) Os(3) 2.814(1) yes . 55501 Os(2) Os(4) 2.811(1) yes . 55501 Os(2) Os(5) 2.8520(8) yes . 55501 Os(2) Rh(2) 2.768(2) yes . 55501 Os(2) O(3) 3.05(2) yes . 55501 Os(2) O(4) 3.03(1) yes . 55501 Os(2) O(5) 3.08(2) yes . 55501 Os(2) C(6) 3.46(2) yes . 55501 Os(2) C(10) 3.47(2) yes . 55501 Os(3) Os(2) 2.814(1) yes . 55501 Os(3) Os(4) 2.8600(8) yes . 55501 Os(3) Rh(1) 2.786(2) yes . 55501 Os(3) Rh(2) 2.814(2) yes . 55501 Os(3) O(4) 3.50(2) yes . 55501 Os(3) O(6) 3.08(2) yes . 55501 Os(3) O(7) 3.03(2) yes . 55501 Os(3) O(8) 3.02(1) yes . 55501 Os(3) C(4) 2.77(2) yes . 55501 Os(3) C(11) 3.07(2) yes . 55501 Os(4) Os(1) 2.864(1) yes . 55501 Os(4) Os(2) 2.811(1) yes . 55501 Os(4) Os(3) 2.8600(8) yes . 55501 Os(4) Os(5) 2.840(1) yes . 55501 Os(4) Rh(1) 2.846(2) yes . 55501 Os(4) O(9) 3.05(1) yes . 55501 Os(4) O(10) 3.06(2) yes . 55501 Os(4) O(11) 3.02(2) yes . 55501 Os(4) C(5) 3.45(2) yes . 55501 Os(4) C(6) 3.41(2) yes . 55501 Os(4) C(15) 3.36(3) yes . 55501 Os(5) Os(1) 2.761(1) yes . 55501 Os(5) Os(2) 2.8520(8) yes . 55501 Os(5) Os(4) 2.840(1) yes . 55501 Os(5) O(12) 3.04(2) yes . 55501 Os(5) O(13) 3.03(1) yes . 55501 Os(5) O(14) 3.03(1) yes . 55501 Os(5) C(1) 2.96(3) yes . 55501 Os(5) C(2) 3.49(2) yes . 55501 Os(5) C(3) 3.24(2) yes . 55501 Os(5) C(5) 3.17(2) yes . 55501 Os(5) C(9) 3.07(2) yes . 55501 Os(5) C(10) 3.24(2) yes . 55501 Rh(1) Os(1) 2.728(2) yes . 55501 Rh(1) Os(3) 2.786(2) yes . 55501 Rh(1) Os(4) 2.846(2) yes . 55501 Rh(1) Rh(2) 2.729(2) yes . 55501 Rh(1) O(15) 3.02(2) yes . 55501 Rh(1) O(16) 3.04(2) yes . 55501 Rh(1) O(17) 3.02(1) yes . 55501 Rh(1) C(7) 2.94(2) yes . 55501 Rh(1) C(11) 3.07(2) yes . 55501 Rh(1) C(17) 2.15(2) yes . 55501 Rh(2) Os(1) 2.735(1) yes . 55501 Rh(2) Os(2) 2.768(2) yes . 55501 Rh(2) Os(3) 2.814(2) yes . 55501 Rh(2) Rh(1) 2.729(2) yes . 55501 Rh(2) C(2) 3.36(2) yes . 55501 Rh(2) C(3) 3.42(2) yes . 55501 Rh(2) C(4) 2.94(2) yes . 55501 Rh(2) C(8) 3.22(2) yes . 55501 Rh(2) C(16) 3.32(3) yes . 55501 Rh(2) C(17) 3.02(2) yes . 55501 Rh(2) C(18) 2.29(2) yes . 55501 Rh(2) C(19) 2.34(2) yes . 55501 Rh(2) C(20) 2.35(2) yes . 55501 Rh(2) C(21) 2.37(2) yes . 55501 Rh(2) C(22) 2.31(2) yes . 55501 Rh(2) C(23) 2.25(2) yes . 55501 Rh(2) C(24) 3.58(3) yes . 55501 Rh(2) H(1) 2.96(2) no . 55501 Rh(2) H(2) 3.01(2) no . 55501 Rh(2) H(3) 2.98(2) no . 55501 Rh(2) H(4) 2.88(2) no . 55501 O(1) Os(1) 3.03(1) yes . 55501 O(1) O(4) 3.20(2) yes . 65501 O(1) O(9) 3.29(2) yes . 55501 O(1) O(13) 3.15(2) yes . 55501 O(1) O(14) 3.19(2) yes . 66502 O(1) C(2) 3.44(2) yes . 55501 O(1) C(9) 3.45(3) yes . 55501 O(1) C(13) 3.03(3) yes . 55501 O(1) C(14) 3.53(2) yes . 66502 O(1) C(17) 3.39(2) yes . 55501 O(2) Os(1) 3.01(2) yes . 55501 O(2) O(2) 3.07(2) yes . 57502 O(2) O(3) 3.33(3) yes . 55501 O(2) O(13) 3.41(2) yes . 66502 O(2) O(14) 3.53(2) yes . 55501 O(2) C(1) 3.46(3) yes . 55501 O(2) C(3) 3.49(3) yes . 55501 O(2) C(14) 3.53(3) yes . 55501 O(2) C(18) 3.30(2) yes . 55501 O(2) C(18) 3.51(2) yes . 57502 O(2) H(1) 2.63(2) no . 55501 O(2) H(1) 2.67(3) no . 57502 O(2) H(4) 3.21(2) no . 55501 O(3) Os(2) 3.05(2) yes . 55501 O(3) O(2) 3.33(3) yes . 55501 O(3) O(12) 3.00(2) yes . 56502 O(3) O(14) 3.07(2) yes . 55501 O(3) O(14) 3.35(3) yes . 56502 O(3) C(2) 3.30(3) yes . 55501 O(3) C(4) 3.58(2) yes . 55501 O(3) C(12) 3.28(3) yes . 56502 O(3) C(14) 3.12(2) yes . 55501 O(3) C(14) 3.50(3) yes . 56502 O(3) C(24) 3.28(3) yes . 55501 O(3) H(1) 3.16(3) no . 55501 O(3) H(7) 2.39(3) no . 55501 O(4) Os(2) 3.03(1) yes . 55501 O(4) Os(3) 3.50(2) yes . 55501 O(4) O(1) 3.20(2) yes . 45501 O(4) O(8) 3.20(2) yes . 55501 O(4) O(15) 3.04(2) yes . 45501 O(4) O(17) 3.03(2) yes . 45501 O(4) C(1) 3.47(3) yes . 45501 O(4) C(3) 3.51(2) yes . 55501 O(4) C(5) 3.37(2) yes . 55501 O(4) C(8) 2.98(3) yes . 55501 O(4) C(15) 3.18(3) yes . 45501 O(4) C(17) 3.25(3) yes . 45501 O(4) C(19) 3.44(3) yes . 55501 O(4) C(20) 3.43(3) yes . 55501 O(4) C(24) 3.17(4) yes . 55501 O(4) H(2) 3.02(3) no . 55501 O(4) H(6) 2.71(3) no . 55501 O(4) H(7) 3.02(4) no . 55501 O(5) Os(2) 3.08(2) yes . 55501 O(5) O(9) 3.09(2) yes . 45501 O(5) O(10) 3.18(2) yes . 55501 O(5) O(12) 3.07(2) yes . 55501 O(5) O(14) 3.02(2) yes . 56502 O(5) C(4) 3.47(2) yes . 55501 O(5) C(10) 3.33(3) yes . 55501 O(5) C(12) 3.08(2) yes . 55501 O(6) Os(3) 3.08(2) yes . 55501 O(6) O(10) 3.38(2) yes . 55501 O(6) O(15) 3.41(2) yes . 45501 O(6) C(5) 3.57(2) yes . 55501 O(6) C(10) 3.38(2) yes . 55501 O(7) Os(3) 3.03(2) yes . 55501 O(7) O(11) 3.14(2) yes . 55501 O(7) C(8) 3.47(3) yes . 55501 O(7) C(11) 3.34(2) yes . 55501 O(7) C(16) 3.42(3) yes . 55501 O(8) Os(3) 3.02(1) yes . 55501 O(8) O(4) 3.20(2) yes . 55501 O(8) O(15) 3.20(3) yes . 45501 O(8) C(4) 3.46(2) yes . 55501 O(8) C(7) 3.50(3) yes . 55501 O(8) C(20) 3.28(3) yes . 55501 O(8) C(21) 3.56(3) yes . 55501 O(8) C(25) 3.39(3) yes . 55501 O(8) H(2) 2.69(3) no . 55501 O(8) H(8) 2.80(3) no . 55501 O(8) H(10) 3.43(4) no . 55501 O(9) Os(4) 3.05(1) yes . 55501 O(9) O(1) 3.29(2) yes . 55501 O(9) O(5) 3.09(2) yes . 65501 O(9) O(13) 3.24(2) yes . 55501 O(9) O(15) 3.58(2) yes . 55501 O(9) C(1) 3.23(3) yes . 55501 O(9) C(11) 3.47(2) yes . 55501 O(9) C(13) 3.15(3) yes . 55501 O(9) C(15) 3.60(2) yes . 55501 O(10) Os(4) 3.06(2) yes . 55501 O(10) O(5) 3.18(2) yes . 55501 O(10) O(6) 3.38(2) yes . 55501 O(10) O(12) 3.23(2) yes . 55501 O(10) C(5) 3.27(2) yes . 55501 O(10) C(11) 3.50(3) yes . 55501 O(10) C(12) 3.18(3) yes . 55501 O(11) Os(4) 3.02(2) yes . 55501 O(11) O(7) 3.14(2) yes . 55501 O(11) O(15) 3.34(3) yes . 55501 O(11) C(7) 3.07(2) yes . 55501 O(11) C(9) 3.44(2) yes . 55501 O(11) C(10) 3.43(3) yes . 55501 O(11) C(15) 3.20(3) yes . 55501 O(12) Os(5) 3.04(2) yes . 55501 O(12) O(3) 3.00(2) yes . 56502 O(12) O(5) 3.07(2) yes . 55501 O(12) O(10) 3.23(2) yes . 55501 O(12) C(5) 3.37(2) yes . 55501 O(12) C(10) 3.49(2) yes . 55501 O(12) C(13) 3.54(4) yes . 55501 O(13) Os(5) 3.03(1) yes . 55501 O(13) O(1) 3.15(2) yes . 55501 O(13) O(2) 3.41(2) yes . 66502 O(13) O(9) 3.24(2) yes . 55501 O(13) O(14) 3.20(3) yes . 66502 O(13) C(1) 3.43(2) yes . 55501 O(13) C(9) 3.51(2) yes . 55501 O(13) C(12) 3.55(3) yes . 55501 O(13) C(14) 3.59(3) yes . 55501 O(13) C(14) 3.49(3) yes . 66502 O(14) Os(5) 3.03(1) yes . 55501 O(14) O(1) 3.19(2) yes . 66502 O(14) O(2) 3.53(2) yes . 55501 O(14) O(3) 3.07(2) yes . 55501 O(14) O(3) 3.35(3) yes . 56502 O(14) O(5) 3.02(2) yes . 56502 O(14) O(13) 3.20(3) yes . 66502 O(14) C(2) 3.58(3) yes . 55501 O(14) C(3) 3.32(2) yes . 55501 O(14) C(3) 3.39(3) yes . 56502 O(14) C(5) 3.22(3) yes . 56502 O(14) C(13) 3.57(3) yes . 55501 O(15) Rh(1) 3.02(2) yes . 55501 O(15) O(4) 3.04(2) yes . 65501 O(15) O(6) 3.41(2) yes . 65501 O(15) O(8) 3.20(3) yes . 65501 O(15) O(9) 3.58(2) yes . 55501 O(15) O(11) 3.34(3) yes . 55501 O(15) C(6) 3.52(3) yes . 65501 O(15) C(8) 3.46(3) yes . 65501 O(15) C(9) 3.54(3) yes . 55501 O(15) C(11) 3.31(3) yes . 55501 O(16) Rh(1) 3.04(2) yes . 55501 O(16) C(22) 3.40(3) yes . 55501 O(16) C(25) 3.27(3) yes . 55501 O(16) H(3) 2.79(3) no . 55501 O(16) H(9) 3.55(3) no . 55501 O(16) H(10) 2.44(4) no . 55501 O(17) Os(1) 3.08(2) yes . 55501 O(17) Rh(1) 3.02(1) yes . 55501 O(17) O(4) 3.03(2) yes . 65501 O(17) O(10) 3.12(2) yes . 56501 O(17) O(12) 3.28(2) yes . 56501 O(17) C(1) 3.30(2) yes . 55501 O(17) C(2) 3.53(3) yes . 55501 O(17) C(15) 3.54(3) yes . 55501 O(17) C(16) 3.34(3) yes . 55501 O(17) C(22) 3.56(2) yes . 55501 O(17) C(23) 3.32(3) yes . 55501 O(17) C(24) 3.30(3) yes . 65501 O(17) H(2) 3.55(3) no . 65501 O(17) H(3) 3.25(2) no . 55501 O(17) H(4) 2.74(3) no . 55501 O(17) H(6) 2.38(4) no . 65501 C(1) Os(5) 2.96(3) yes . 55501 C(1) O(2) 3.46(3) yes . 55501 C(1) O(4) 3.47(3) yes . 65501 C(1) O(9) 3.23(3) yes . 55501 C(1) O(13) 3.43(2) yes . 55501 C(1) O(17) 3.30(2) yes . 55501 C(1) C(2) 2.58(3) yes . 55501 C(1) C(9) 3.00(3) yes . 55501 C(1) C(13) 2.89(3) yes . 55501 C(1) C(17) 2.60(2) yes . 55501 C(2) Os(5) 3.49(2) yes . 55501 C(2) Rh(2) 3.36(2) yes . 55501 C(2) O(1) 3.44(2) yes . 55501 C(2) O(3) 3.30(3) yes . 55501 C(2) O(14) 3.58(3) yes . 55501 C(2) O(17) 3.53(3) yes . 55501 C(2) C(1) 2.58(3) yes . 55501 C(2) C(3) 3.07(3) yes . 55501 C(2) C(14) 3.20(3) yes . 55501 C(2) C(17) 2.91(3) yes . 55501 C(2) C(18) 3.16(2) yes . 55501 C(2) C(23) 3.31(2) yes . 55501 C(2) H(1) 2.78(2) no . 55501 C(2) H(4) 3.01(2) no . 55501 C(3) Os(1) 3.31(2) yes . 55501 C(3) Os(5) 3.24(2) yes . 55501 C(3) Rh(2) 3.42(2) yes . 55501 C(3) O(2) 3.49(3) yes . 55501 C(3) O(4) 3.51(2) yes . 55501 C(3) O(14) 3.32(2) yes . 55501 C(3) O(14) 3.39(3) yes . 56502 C(3) C(2) 3.07(3) yes . 55501 C(3) C(4) 2.71(3) yes . 55501 C(3) C(5) 2.83(3) yes . 55501 C(3) C(14) 2.95(2) yes . 55501 C(3) C(18) 3.56(3) yes . 55501 C(3) C(19) 3.54(2) yes . 55501 C(3) C(24) 3.40(3) yes . 55501 C(3) H(1) 3.30(3) no . 55501 C(3) H(7) 2.59(3) no . 55501 C(4) Os(3) 2.77(2) yes . 55501 C(4) Rh(2) 2.94(2) yes . 55501 C(4) O(3) 3.58(2) yes . 55501 C(4) O(5) 3.47(2) yes . 55501 C(4) O(8) 3.46(2) yes . 55501 C(4) C(3) 2.71(3) yes . 55501 C(4) C(5) 2.59(2) yes . 55501 C(4) C(6) 3.19(3) yes . 55501 C(4) C(8) 2.86(3) yes . 55501 C(4) C(19) 3.27(3) yes . 55501 C(4) C(20) 3.40(3) yes . 55501 C(4) C(24) 3.31(4) yes . 55501 C(4) H(2) 3.29(2) no . 55501 C(4) H(6) 3.18(3) no . 55501 C(4) H(7) 3.01(4) no . 55501 C(5) Os(4) 3.45(2) yes . 55501 C(5) Os(5) 3.17(2) yes . 55501 C(5) O(4) 3.37(2) yes . 55501 C(5) O(6) 3.57(2) yes . 55501 C(5) O(10) 3.27(2) yes . 55501 C(5) O(12) 3.37(2) yes . 55501 C(5) O(14) 3.22(3) yes . 56502 C(5) C(3) 2.83(3) yes . 55501 C(5) C(4) 2.59(2) yes . 55501 C(5) C(6) 3.36(3) yes . 55501 C(5) C(10) 2.99(3) yes . 55501 C(5) C(12) 2.95(2) yes . 55501 C(6) Os(2) 3.46(2) yes . 55501 C(6) Os(4) 3.41(2) yes . 55501 C(6) O(15) 3.52(3) yes . 45501 C(6) C(4) 3.19(3) yes . 55501 C(6) C(5) 3.36(3) yes . 55501 C(6) C(7) 2.87(4) yes . 55501 C(6) C(8) 2.76(3) yes . 55501 C(6) C(10) 3.23(2) yes . 55501 C(6) C(11) 3.37(3) yes . 55501 C(7) Rh(1) 2.94(2) yes . 55501 C(7) O(8) 3.50(3) yes . 55501 C(7) O(11) 3.07(2) yes . 55501 C(7) C(6) 2.87(4) yes . 55501 C(7) C(8) 2.63(3) yes . 55501 C(7) C(11) 2.89(2) yes . 55501 C(7) C(16) 3.11(4) yes . 55501 C(8) Rh(2) 3.22(2) yes . 55501 C(8) O(4) 2.98(3) yes . 55501 C(8) O(7) 3.47(3) yes . 55501 C(8) O(15) 3.46(3) yes . 45501 C(8) C(4) 2.86(3) yes . 55501 C(8) C(6) 2.76(3) yes . 55501 C(8) C(7) 2.63(3) yes . 55501 C(8) C(20) 3.25(3) yes . 55501 C(8) C(21) 3.44(3) yes . 55501 C(8) C(25) 3.56(3) yes . 55501 C(8) H(2) 2.93(3) no . 55501 C(8) H(8) 3.25(3) no . 55501 C(8) H(10) 3.42(4) no . 55501 C(9) Os(1) 3.36(2) yes . 55501 C(9) Os(5) 3.07(2) yes . 55501 C(9) O(1) 3.45(3) yes . 55501 C(9) O(11) 3.44(2) yes . 55501 C(9) O(13) 3.51(2) yes . 55501 C(9) O(15) 3.54(3) yes . 55501 C(9) C(1) 3.00(3) yes . 55501 C(9) C(10) 2.88(4) yes . 55501 C(9) C(11) 2.65(3) yes . 55501 C(9) C(13) 3.01(3) yes . 55501 C(9) C(15) 3.24(3) yes . 55501 C(10) Os(2) 3.47(2) yes . 55501 C(10) Os(5) 3.24(2) yes . 55501 C(10) O(5) 3.33(3) yes . 55501 C(10) O(6) 3.38(2) yes . 55501 C(10) O(11) 3.43(3) yes . 55501 C(10) O(12) 3.49(2) yes . 55501 C(10) C(5) 2.99(3) yes . 55501 C(10) C(6) 3.23(2) yes . 55501 C(10) C(9) 2.88(4) yes . 55501 C(10) C(11) 2.63(3) yes . 55501 C(10) C(12) 3.04(3) yes . 55501 C(11) Os(3) 3.07(2) yes . 55501 C(11) Rh(1) 3.07(2) yes . 55501 C(11) O(7) 3.34(2) yes . 55501 C(11) O(9) 3.47(2) yes . 55501 C(11) O(10) 3.50(3) yes . 55501 C(11) O(15) 3.31(3) yes . 55501 C(11) C(6) 3.37(3) yes . 55501 C(11) C(7) 2.89(2) yes . 55501 C(11) C(9) 2.65(3) yes . 55501 C(11) C(10) 2.63(3) yes . 55501 C(11) C(15) 2.87(4) yes . 55501 C(12) O(3) 3.28(3) yes . 56502 C(12) O(5) 3.08(2) yes . 55501 C(12) O(10) 3.18(3) yes . 55501 C(12) O(13) 3.55(3) yes . 55501 C(12) C(5) 2.95(2) yes . 55501 C(12) C(10) 3.04(3) yes . 55501 C(12) C(13) 2.63(4) yes . 55501 C(12) C(14) 2.80(3) yes . 55501 C(13) O(1) 3.03(3) yes . 55501 C(13) O(9) 3.15(3) yes . 55501 C(13) O(12) 3.54(4) yes . 55501 C(13) O(14) 3.57(3) yes . 55501 C(13) C(1) 2.89(3) yes . 55501 C(13) C(9) 3.01(3) yes . 55501 C(13) C(12) 2.63(4) yes . 55501 C(13) C(14) 2.64(3) yes . 55501 C(14) Os(1) 3.53(2) yes . 55501 C(14) O(1) 3.53(2) yes . 66502 C(14) O(2) 3.53(3) yes . 55501 C(14) O(3) 3.12(2) yes . 55501 C(14) O(3) 3.50(3) yes . 56502 C(14) O(13) 3.59(3) yes . 55501 C(14) O(13) 3.49(3) yes . 66502 C(14) C(2) 3.20(3) yes . 55501 C(14) C(3) 2.95(2) yes . 55501 C(14) C(12) 2.80(3) yes . 55501 C(14) C(13) 2.64(3) yes . 55501 C(15) Os(4) 3.36(3) yes . 55501 C(15) O(4) 3.18(3) yes . 65501 C(15) O(9) 3.60(2) yes . 55501 C(15) O(11) 3.20(3) yes . 55501 C(15) O(17) 3.54(3) yes . 55501 C(15) C(9) 3.24(3) yes . 55501 C(15) C(11) 2.87(4) yes . 55501 C(15) C(16) 2.78(3) yes . 55501 C(15) C(17) 2.99(3) yes . 55501 C(16) Rh(2) 3.32(3) yes . 55501 C(16) O(7) 3.42(3) yes . 55501 C(16) O(17) 3.34(3) yes . 55501 C(16) C(7) 3.11(4) yes . 55501 C(16) C(15) 2.78(3) yes . 55501 C(16) C(17) 3.06(3) yes . 55501 C(16) C(21) 3.54(3) yes . 55501 C(16) C(22) 3.17(3) yes . 55501 C(16) C(25) 3.55(3) yes . 55501 C(16) H(3) 2.77(3) no . 55501 C(16) H(10) 2.81(3) no . 55501 C(17) Rh(1) 2.15(2) yes . 55501 C(17) Rh(2) 3.02(2) yes . 55501 C(17) O(1) 3.39(2) yes . 55501 C(17) O(4) 3.25(3) yes . 65501 C(17) C(1) 2.60(2) yes . 55501 C(17) C(2) 2.91(3) yes . 55501 C(17) C(15) 2.99(3) yes . 55501 C(17) C(16) 3.06(3) yes . 55501 C(17) C(22) 3.48(2) yes . 55501 C(17) C(23) 3.20(3) yes . 55501 C(17) H(3) 3.41(2) no . 55501 C(17) H(4) 2.85(3) no . 55501 C(17) H(6) 3.34(4) no . 65501 C(18) Rh(2) 2.29(2) yes . 55501 C(18) O(2) 3.30(2) yes . 55501 C(18) O(2) 3.51(2) yes . 57502 C(18) O(13) 3.51(2) yes . 46501 C(18) C(2) 3.16(2) yes . 55501 C(18) C(3) 3.56(3) yes . 55501 C(18) C(20) 2.41(3) yes . 55501 C(18) C(21) 2.81(3) yes . 55501 C(18) C(22) 2.42(3) yes . 55501 C(18) C(24) 2.50(4) yes . 55501 C(18) H(2) 3.27(3) no . 55501 C(18) H(3) 3.28(3) no . 55501 C(18) H(4) 2.04(4) no . 55501 C(18) H(5) 2.72(4) no . 55501 C(18) H(6) 3.27(4) no . 55501 C(18) H(7) 2.73(5) no . 55501 C(19) Rh(2) 2.34(2) yes . 55501 C(19) O(4) 3.44(3) yes . 55501 C(19) C(3) 3.54(2) yes . 55501 C(19) C(4) 3.27(3) yes . 55501 C(19) C(21) 2.45(3) yes . 55501 C(19) C(22) 2.82(4) yes . 55501 C(19) C(23) 2.42(4) yes . 55501 C(19) H(1) 2.03(3) no . 55501 C(19) H(2) 2.06(3) no . 55501 C(19) H(4) 3.27(3) no . 55501 C(19) H(5) 2.02(4) no . 55501 C(19) H(6) 2.03(4) no . 55501 C(19) H(7) 2.03(4) no . 55501 C(20) Rh(2) 2.35(2) yes . 55501 C(20) O(4) 3.43(3) yes . 55501 C(20) O(8) 3.28(3) yes . 55501 C(20) O(9) 3.53(2) yes . 46501 C(20) C(4) 3.40(3) yes . 55501 C(20) C(8) 3.25(3) yes . 55501 C(20) C(18) 2.41(3) yes . 55501 C(20) C(22) 2.43(3) yes . 55501 C(20) C(23) 2.77(3) yes . 55501 C(20) C(24) 2.55(4) yes . 55501 C(20) C(25) 2.59(4) yes . 55501 C(20) H(1) 3.27(3) no . 55501 C(20) H(3) 3.28(4) no . 55501 C(20) H(5) 3.09(4) no . 55501 C(20) H(6) 2.59(4) no . 55501 C(20) H(7) 3.19(4) no . 55501 C(20) H(8) 2.64(3) no . 55501 C(20) H(9) 3.16(3) no . 55501 C(20) H(10) 3.20(4) no . 55501 C(21) Rh(2) 2.37(2) yes . 55501 C(21) O(8) 3.56(3) yes . 55501 C(21) O(9) 3.28(2) yes . 46501 C(21) C(8) 3.44(3) yes . 55501 C(21) C(16) 3.54(3) yes . 55501 C(21) C(18) 2.81(3) yes . 55501 C(21) C(19) 2.45(3) yes . 55501 C(21) C(23) 2.43(3) yes . 55501 C(21) H(2) 2.03(3) no . 55501 C(21) H(3) 2.08(4) no . 55501 C(21) H(4) 3.29(3) no . 55501 C(21) H(8) 2.05(3) no . 55501 C(21) H(9) 2.07(3) no . 55501 C(21) H(10) 2.05(3) no . 55501 C(22) Rh(2) 2.31(2) yes . 55501 C(22) O(5) 3.11(3) yes . 56501 C(22) O(9) 3.51(2) yes . 46501 C(22) O(10) 3.54(3) yes . 56501 C(22) O(16) 3.40(3) yes . 55501 C(22) O(17) 3.56(2) yes . 55501 C(22) C(16) 3.17(3) yes . 55501 C(22) C(17) 3.48(2) yes . 55501 C(22) C(18) 2.42(3) yes . 55501 C(22) C(19) 2.82(4) yes . 55501 C(22) C(20) 2.43(3) yes . 55501 C(22) C(25) 2.52(3) yes . 55501 C(22) H(1) 3.28(3) no . 55501 C(22) H(2) 3.29(3) no . 55501 C(22) H(4) 2.03(3) no . 55501 C(22) H(8) 3.30(3) no . 55501 C(22) H(9) 2.74(3) no . 55501 C(22) H(10) 2.74(3) no . 55501 C(23) Rh(2) 2.25(2) yes . 55501 C(23) O(5) 3.08(2) yes . 56501 C(23) O(12) 3.56(3) yes . 56501 C(23) O(17) 3.32(3) yes . 55501 C(23) C(2) 3.31(2) yes . 55501 C(23) C(17) 3.20(3) yes . 55501 C(23) C(19) 2.42(4) yes . 55501 C(23) C(20) 2.77(3) yes . 55501 C(23) C(21) 2.43(3) yes . 55501 C(23) H(1) 2.05(3) no . 55501 C(23) H(3) 2.04(3) no . 55501 C(24) Rh(2) 3.58(3) yes . 55501 C(24) O(3) 3.28(3) yes . 55501 C(24) O(4) 3.17(4) yes . 55501 C(24) O(17) 3.30(3) yes . 45501 C(24) C(3) 3.40(3) yes . 55501 C(24) C(4) 3.31(4) yes . 55501 C(24) C(18) 2.50(4) yes . 55501 C(24) C(20) 2.55(4) yes . 55501 C(24) H(1) 2.64(4) no . 55501 C(24) H(2) 2.71(4) no . 55501 C(25) O(8) 3.39(3) yes . 55501 C(25) O(9) 3.58(3) yes . 46501 C(25) O(16) 3.27(3) yes . 55501 C(25) C(8) 3.56(3) yes . 55501 C(25) C(16) 3.55(3) yes . 55501 C(25) C(20) 2.59(4) yes . 55501 C(25) C(22) 2.52(3) yes . 55501 C(25) H(2) 2.76(4) no . 55501 C(25) H(3) 2.65(3) no . 55501 H(1) Rh(2) 2.96(2) no . 55501 H(1) O(2) 2.63(2) no . 55501 H(1) O(2) 2.67(3) no . 57502 H(1) O(3) 3.16(3) no . 55501 H(1) O(13) 3.43(2) no . 46501 H(1) C(2) 2.78(2) no . 55501 H(1) C(3) 3.30(3) no . 55501 H(1) C(19) 2.03(3) no . 55501 H(1) C(20) 3.27(3) no . 55501 H(1) C(22) 3.28(3) no . 55501 H(1) C(23) 2.05(3) no . 55501 H(1) C(24) 2.64(4) no . 55501 H(2) Rh(2) 3.01(2) no . 55501 H(2) O(4) 3.02(3) no . 55501 H(2) O(8) 2.69(3) no . 55501 H(2) O(17) 3.55(3) no . 45501 H(2) C(4) 3.29(2) no . 55501 H(2) C(8) 2.93(3) no . 55501 H(2) C(18) 3.27(3) no . 55501 H(2) C(19) 2.06(3) no . 55501 H(2) C(21) 2.03(3) no . 55501 H(2) C(22) 3.29(3) no . 55501 H(2) C(24) 2.71(4) no . 55501 H(2) C(25) 2.76(4) no . 55501 H(3) Rh(2) 2.98(2) no . 55501 H(3) O(5) 2.97(3) no . 56501 H(3) O(6) 3.47(3) no . 56501 H(3) O(10) 2.70(3) no . 56501 H(3) O(16) 2.79(3) no . 55501 H(3) O(17) 3.25(2) no . 55501 H(3) C(16) 2.77(3) no . 55501 H(3) C(17) 3.41(2) no . 55501 H(3) C(18) 3.28(3) no . 55501 H(3) C(20) 3.28(4) no . 55501 H(3) C(21) 2.08(4) no . 55501 H(3) C(23) 2.04(3) no . 55501 H(3) C(25) 2.65(3) no . 55501 H(4) Os(1) 3.57(2) no . 55501 H(4) Rh(2) 2.88(2) no . 55501 H(4) O(2) 3.21(2) no . 55501 H(4) O(5) 2.93(2) no . 56501 H(4) O(10) 3.56(3) no . 56501 H(4) O(12) 2.67(3) no . 56501 H(4) O(17) 2.74(3) no . 55501 H(4) C(2) 3.01(2) no . 55501 H(4) C(12) 3.60(3) no . 56501 H(4) C(17) 2.85(3) no . 55501 H(4) C(18) 2.04(4) no . 55501 H(4) C(19) 3.27(3) no . 55501 H(4) C(21) 3.29(3) no . 55501 H(4) C(22) 2.03(3) no . 55501 H(5) O(12) 3.13(3) no . 46501 H(5) O(13) 2.94(4) no . 46501 H(5) C(12) 3.25(3) no . 46501 H(5) C(13) 3.19(4) no . 46501 H(5) C(18) 2.72(4) no . 55501 H(5) C(19) 2.02(4) no . 55501 H(5) C(20) 3.09(4) no . 55501 H(6) O(4) 2.71(3) no . 55501 H(6) O(12) 3.28(3) no . 46501 H(6) O(17) 2.38(4) no . 45501 H(6) C(4) 3.18(3) no . 55501 H(6) C(17) 3.34(4) no . 45501 H(6) C(18) 3.27(4) no . 55501 H(6) C(19) 2.03(4) no . 55501 H(6) C(20) 2.59(4) no . 55501 H(7) O(3) 2.39(3) no . 55501 H(7) O(4) 3.02(4) no . 55501 H(7) C(3) 2.59(3) no . 55501 H(7) C(4) 3.01(4) no . 55501 H(7) C(18) 2.73(5) no . 55501 H(7) C(19) 2.03(4) no . 55501 H(7) C(20) 3.19(4) no . 55501 H(8) O(8) 2.80(3) no . 55501 H(8) C(8) 3.25(3) no . 55501 H(8) C(20) 2.64(3) no . 55501 H(8) C(21) 2.05(3) no . 55501 H(8) C(22) 3.30(3) no . 55501 H(9) O(6) 3.03(4) no . 56501 H(9) O(9) 3.08(3) no . 46501 H(9) O(16) 3.55(3) no . 55501 H(9) C(20) 3.16(3) no . 55501 H(9) C(21) 2.07(3) no . 55501 H(9) C(22) 2.74(3) no . 55501 H(10) O(8) 3.43(4) no . 55501 H(10) O(16) 2.44(4) no . 55501 H(10) C(8) 3.42(4) no . 55501 H(10) C(16) 2.81(3) no . 55501 H(10) C(20) 3.20(4) no . 55501 H(10) C(21) 2.05(3) no . 55501 H(10) C(22) 2.74(3) no . 55501 #============================================================================== # 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 #============================================================================== #============================================================================== # 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 #============================================================================== data__wt0911w _database_code_depnum_ccdc_archive 'CCDC 262818' #-JAS006---Compound 5 _audit_creation_date 2005-02-01 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? _publ_section_references ; Bruker AXS Inc. (1998) SMART version 5.054, Madison, Wisconsin, USA. Bruker AXS Inc. (1999) SAINT, version 6.02, Madison, Wisconsin, USA. Farrugia, L.J. (1997) Ortep-3 J. Appl. Cryst. 30, 565. Johnson, C. K. (1976) ORTEP-II, A FORTRAN Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Rigaku/MSC and Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Sheldrick, G.M. (1997) SHELXS-97, Gottingen University, Gottingen, Germany. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_exptl_refinement ; Some non-H atoms were refined anisotropically, while the rest were refined isotropically. The C-bound H atoms and the metal-bound hydrido atoms were placed at their geometrically calculated positions and not refined. ; #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H13 Cl2 O23 Os7 Rh3 ' _chemical_formula_moiety 'C23 H11 O23 Os7 Rh3, C H2 Cl2 ' _chemical_formula_weight 2380.38 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 #------------------------------------------------------------------------------ _cell_length_a 11.792(4) _cell_length_b 24.927(8) _cell_length_c 15.438(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.39(1) _cell_angle_gamma 90.00 _cell_volume 4395.5(25) _cell_formula_units_Z 4 _cell_measurement_reflns_used 27667 _cell_measurement_theta_min 0.8 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 298(1) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 3.597 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4168.00 _exptl_absorpt_coefficient_mu 21.422 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.646 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27667 _diffrn_reflns_av_R_equivalents 0.082 _diffrn_reflns_theta_max 27.51 _diffrn_measured_fraction_theta_max 0.9795 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.9795 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 10152 _reflns_number_gt 6083 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0410 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 6129 _refine_ls_number_parameters 517 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + 1.0000\s(Fo^2^) + 0.0020]' _refine_ls_shift/su_max 0.0040 _refine_diff_density_max 2.98 _refine_diff_density_min -3.90 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os Os -1.216 7.603 ; 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) ; C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 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) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; 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 Os(1) Os 0.42680(5) 0.09381(3) 0.61987(5) 0.0323(2) Uani 1.00 1 d . . . Os(2) Os 0.38557(6) 0.06479(3) 0.78592(5) 0.0395(2) Uani 1.00 1 d . . . Os(3) Os 0.41256(6) 0.17980(3) 0.74563(5) 0.0338(2) Uani 1.00 1 d . . . Os(4) Os 0.78306(6) 0.12759(3) 0.94516(5) 0.0366(2) Uani 1.00 1 d . . . Os(5) Os 0.82104(6) 0.04529(3) 0.82325(5) 0.0355(2) Uani 1.00 1 d . . . Os(6) Os 0.80638(6) 0.17228(3) 0.58978(5) 0.0328(2) Uani 1.00 1 d . . . Os(7) Os 0.80004(6) 0.26162(3) 0.70774(5) 0.0354(2) Uani 1.00 1 d . . . Rh(1) Rh 0.60452(10) 0.11301(5) 0.78222(9) 0.0305(4) Uani 1.00 1 d . . . Rh(2) Rh 0.83474(10) 0.15215(5) 0.78729(9) 0.0305(4) Uani 1.00 1 d . . . Rh(3) Rh 0.61198(11) 0.19089(5) 0.65377(9) 0.0319(4) Uani 1.00 1 d . . . Cl(1) Cl 0.9721(9) 0.0770(4) 0.2332(7) 0.163(4) Uiso 1.00 1 d . . . Cl(2) Cl 0.814(1) 0.1352(7) 0.3350(11) 0.316(9) Uiso 1.00 1 d . . . O(1) O 0.5513(11) -0.0108(5) 0.6023(8) 0.052(4) Uani 1.00 1 d . . . O(2) O 0.1868(12) 0.0457(6) 0.5364(11) 0.083(6) Uani 1.00 1 d . . . O(3) O 0.4247(13) 0.1370(6) 0.4344(9) 0.070(5) Uani 1.00 1 d . . . O(4) O 0.1217(12) 0.0542(7) 0.7253(11) 0.093(6) Uani 1.00 1 d . . . O(5) O 0.432(2) -0.0533(6) 0.7521(13) 0.095(7) Uani 1.00 1 d . . . O(6) O 0.391(1) 0.0474(7) 0.9834(10) 0.091(6) Uani 1.00 1 d . . . O(7) O 0.1695(12) 0.2276(7) 0.7128(11) 0.093(6) Uani 1.00 1 d . . . O(8) O 0.4546(12) 0.2892(5) 0.6710(9) 0.059(5) Uani 1.00 1 d . . . O(9) O 0.5025(12) 0.2273(7) 0.9316(10) 0.082(6) Uani 1.00 1 d . . . O(10) O 0.7704(12) 0.2465(6) 0.9820(11) 0.072(5) Uani 1.00 1 d . . . O(11) O 1.0328(11) 0.1182(6) 1.0616(9) 0.068(5) Uani 1.00 1 d . . . O(12) O 0.671(2) 0.0937(9) 1.0957(12) 0.126(9) Uani 1.00 1 d . . . O(13) O 1.0729(11) 0.0193(6) 0.9203(10) 0.070(5) Uani 1.00 1 d . . . O(14) O 0.728(1) -0.0668(6) 0.8372(12) 0.088(6) Uani 1.00 1 d . . . O(15) O 0.8605(13) 0.0176(6) 0.6411(10) 0.069(5) Uani 1.00 1 d . . . O(16) O 0.6821(12) 0.0752(6) 0.4906(9) 0.063(5) Uani 1.00 1 d . . . O(17) O 0.7569(12) 0.2387(6) 0.4166(10) 0.078(6) Uani 1.00 1 d . . . O(18) O 1.0449(12) 0.1397(7) 0.5662(11) 0.089(6) Uani 1.00 1 d . . . O(19) O 0.7644(12) 0.3374(6) 0.5485(10) 0.072(5) Uani 1.00 1 d . . . O(20) O 1.0297(11) 0.3167(6) 0.7932(10) 0.068(5) Uani 1.00 1 d . . . O(21) O 0.671(1) 0.3260(7) 0.8187(12) 0.098(7) Uani 1.00 1 d . . . O(22) O 1.0911(10) 0.1459(6) 0.8600(9) 0.062(5) Uani 1.00 1 d . . . O(23) O 0.5368(11) 0.2554(5) 0.4880(9) 0.059(5) Uani 1.00 1 d . . . C(1) C 0.502(1) 0.0275(7) 0.6077(11) 0.035(5) Uani 1.00 1 d . . . C(2) C 0.275(2) 0.0651(8) 0.5682(13) 0.056(7) Uani 1.00 1 d . . . C(3) C 0.431(2) 0.1209(7) 0.505(1) 0.049(6) Uani 1.00 1 d . . . C(4) C 0.221(2) 0.0576(8) 0.7477(12) 0.049(6) Uani 1.00 1 d . . . C(5) C 0.415(2) -0.0094(10) 0.7649(12) 0.055(7) Uani 1.00 1 d . . . C(6) C 0.389(2) 0.0552(8) 0.909(2) 0.058(7) Uani 1.00 1 d . . . C(7) C 0.257(2) 0.2098(7) 0.7238(13) 0.048(6) Uani 1.00 1 d . . . C(8) C 0.455(2) 0.2443(8) 0.6909(12) 0.048(6) Uani 1.00 1 d . . . C(9) C 0.470(1) 0.2105(8) 0.861(1) 0.050(6) Uani 1.00 1 d . . . C(10) C 0.774(1) 0.2010(9) 0.9674(11) 0.050(6) Uani 1.00 1 d . . . C(11) C 0.939(2) 0.1231(8) 1.0149(12) 0.048(6) Uani 1.00 1 d . . . C(12) C 0.711(2) 0.1061(9) 1.039(2) 0.071(8) Uani 1.00 1 d . . . C(13) C 0.980(2) 0.0303(7) 0.8861(12) 0.046(6) Uani 1.00 1 d . . . C(14) C 0.763(2) -0.0255(8) 0.833(1) 0.057(7) Uani 1.00 1 d . . . C(15) C 0.847(2) 0.0278(8) 0.710(1) 0.049(6) Uani 1.00 1 d . . . C(16) C 0.727(2) 0.1124(7) 0.5289(13) 0.043(6) Uani 1.00 1 d . . . C(17) C 0.771(1) 0.2141(8) 0.485(2) 0.054(6) Uani 1.00 1 d . . . C(18) C 0.953(2) 0.1506(8) 0.5739(13) 0.051(6) Uani 1.00 1 d . . . C(19) C 0.772(2) 0.3080(7) 0.613(2) 0.055(7) Uani 1.00 1 d . . . C(20) C 0.941(2) 0.2958(7) 0.7609(12) 0.043(6) Uani 1.00 1 d . . . C(21) C 0.717(2) 0.3017(8) 0.7769(13) 0.051(6) Uani 1.00 1 d . . . C(22) C 0.989(2) 0.1474(7) 0.8307(11) 0.038(5) Uani 1.00 1 d . . . C(23) C 0.5704(13) 0.2299(7) 0.5535(12) 0.038(5) Uani 1.00 1 d . . . C(24) C 0.931(3) 0.0886(13) 0.3363(9) 0.18(2) Uiso 1.00 1 d . . . H(1) H 0.3546 0.0454 0.6721 0.0380 Uiso 1.00 1 c . . . H(2) H 0.5804 0.0929 0.6653 0.0380 Uiso 1.00 1 c . . . H(3) H 0.5359 0.0629 0.8390 0.0380 Uiso 1.00 1 c . . . H(4) H 0.3345 0.1327 0.8017 0.0380 Uiso 1.00 1 c . . . H(5) H 0.3788 0.1627 0.6277 0.0380 Uiso 1.00 1 c . . . H(6) H 0.6608 0.0462 0.7685 0.0380 Uiso 1.00 1 c . . . H(7) H 0.6242 0.1315 0.8943 0.0380 Uiso 1.00 1 c . . . H(8) H 0.8471 0.0611 0.9387 0.0380 Uiso 1.00 1 c . . . H(9) H 0.8469 0.2418 0.6095 0.0380 Uiso 1.00 1 c . . . H(10) H 0.8799 0.1292 0.6866 0.0380 Uiso 1.00 1 c . . . H(11) H 0.8721 0.2196 0.8111 0.0380 Uiso 1.00 1 c . . . H(12) H 0.9119 0.0549 0.3574 0.1957 Uiso 1.00 1 c . . . H(13) H 1.0001 0.1021 0.3787 0.1957 Uiso 1.00 1 c . . . 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 Os(1) 0.0282(4) 0.0378(4) 0.0293(4) -0.0001(3) 0.0043(3) -0.0046(3) Os(2) 0.0348(4) 0.0458(4) 0.0404(4) -0.0060(3) 0.0143(3) 0.0000(4) Os(3) 0.0273(4) 0.0396(4) 0.0340(4) 0.0023(3) 0.0067(3) -0.0055(3) Os(4) 0.0315(4) 0.0510(5) 0.0254(4) 0.0005(3) 0.0036(3) 0.0001(3) Os(5) 0.0325(4) 0.0354(4) 0.0360(4) 0.0057(3) 0.0038(3) 0.0053(3) Os(6) 0.0322(4) 0.0379(4) 0.0289(4) -0.0002(3) 0.0086(3) -0.0013(3) Os(7) 0.0322(4) 0.0320(4) 0.0396(4) -0.0008(3) 0.0044(3) -0.0036(3) Rh(1) 0.0249(7) 0.0370(8) 0.0286(7) 0.0016(5) 0.0046(6) 0.0007(6) Rh(2) 0.0266(7) 0.0353(7) 0.0287(7) 0.0007(5) 0.0050(6) -0.0006(6) Rh(3) 0.0298(7) 0.0339(8) 0.0303(8) -0.0005(6) 0.0041(6) 0.0015(6) O(1) 0.063(9) 0.048(8) 0.044(8) 0.014(7) 0.010(7) -0.003(7) O(2) 0.039(8) 0.095(12) 0.10(1) -0.017(8) -0.002(9) -0.036(10) O(3) 0.089(11) 0.086(12) 0.034(9) 0.004(8) 0.010(8) 0.019(8) O(4) 0.043(9) 0.15(2) 0.086(13) -0.020(10) 0.012(9) -0.012(11) O(5) 0.13(2) 0.044(10) 0.13(2) -0.006(10) 0.060(13) 0.002(10) O(6) 0.109(13) 0.14(2) 0.045(10) 0.001(11) 0.047(10) 0.019(10) O(7) 0.035(8) 0.12(1) 0.12(2) 0.034(9) 0.005(9) -0.020(11) O(8) 0.070(9) 0.042(8) 0.067(10) 0.005(7) 0.023(8) -0.003(8) O(9) 0.063(10) 0.12(1) 0.050(10) 0.021(9) -0.006(8) -0.043(10) O(10) 0.057(9) 0.067(10) 0.085(12) -0.004(8) 0.002(8) -0.025(9) O(11) 0.037(8) 0.102(12) 0.056(10) 0.012(8) -0.005(7) 0.005(8) O(12) 0.12(2) 0.20(2) 0.069(13) -0.04(2) 0.053(12) 0.03(1) O(13) 0.033(8) 0.087(11) 0.080(11) 0.014(7) -0.006(8) 0.029(9) O(14) 0.096(12) 0.039(9) 0.13(2) -0.011(8) 0.019(11) 0.023(10) O(15) 0.079(11) 0.070(10) 0.051(10) 0.015(8) 0.006(8) -0.001(8) O(16) 0.064(9) 0.065(10) 0.057(10) -0.005(8) 0.006(8) -0.009(8) O(17) 0.061(10) 0.110(13) 0.061(10) 0.008(9) 0.011(8) 0.051(10) O(18) 0.052(10) 0.11(1) 0.11(1) 0.029(9) 0.040(10) -0.011(11) O(19) 0.072(10) 0.052(10) 0.085(12) 0.005(8) 0.009(9) 0.014(9) O(20) 0.039(8) 0.076(10) 0.084(11) -0.023(7) 0.002(8) -0.023(9) O(21) 0.073(11) 0.11(1) 0.10(1) 0.016(10) 0.006(10) -0.066(12) O(22) 0.025(7) 0.093(11) 0.062(10) 0.003(7) -0.001(7) -0.001(8) O(23) 0.050(8) 0.070(10) 0.053(9) 0.010(7) 0.005(7) 0.021(8) C(1) 0.036(10) 0.041(11) 0.024(9) -0.002(8) -0.003(8) 0.010(8) C(2) 0.056(13) 0.06(1) 0.037(12) 0.013(11) -0.006(10) -0.000(10) C(3) 0.053(12) 0.041(11) 0.046(13) 0.005(9) 0.000(10) -0.004(10) C(4) 0.029(10) 0.08(2) 0.031(11) -0.006(10) 0.000(9) 0.006(10) C(5) 0.051(12) 0.09(2) 0.031(11) -0.022(12) 0.022(10) 0.006(12) C(6) 0.040(11) 0.08(2) 0.06(2) -0.005(10) 0.018(11) 0.002(12) C(7) 0.040(11) 0.050(12) 0.050(13) 0.011(9) 0.004(10) -0.005(10) C(8) 0.049(12) 0.048(12) 0.039(12) 0.011(10) -0.004(9) -0.005(10) C(9) 0.021(9) 0.07(1) 0.05(1) 0.014(9) -0.004(9) -0.002(11) C(10) 0.024(9) 0.10(2) 0.023(10) -0.010(10) 0.002(8) -0.031(11) C(11) 0.050(12) 0.062(13) 0.037(12) 0.005(10) 0.022(10) -0.006(10) C(12) 0.06(1) 0.08(2) 0.06(2) -0.011(12) -0.002(13) 0.009(13) C(13) 0.049(12) 0.057(13) 0.038(11) -0.007(10) 0.023(10) -0.008(10) C(14) 0.07(1) 0.032(11) 0.07(2) 0.009(10) 0.004(11) 0.001(11) C(15) 0.040(11) 0.053(13) 0.048(13) 0.010(9) -0.001(10) -0.007(10) C(16) 0.045(11) 0.040(11) 0.050(13) 0.009(9) 0.023(10) 0.000(10) C(17) 0.024(10) 0.058(13) 0.08(2) -0.012(9) 0.006(10) -0.016(12) C(18) 0.055(13) 0.055(13) 0.048(13) 0.001(10) 0.018(10) -0.011(10) C(19) 0.052(12) 0.032(11) 0.08(2) -0.007(9) 0.020(12) -0.006(11) C(20) 0.048(11) 0.048(12) 0.037(11) 0.002(9) 0.019(10) 0.001(9) C(21) 0.050(12) 0.048(12) 0.049(13) 0.001(10) -0.001(10) -0.006(10) C(22) 0.051(12) 0.039(10) 0.023(9) -0.008(9) 0.010(9) 0.000(8) C(23) 0.019(9) 0.050(12) 0.047(12) 0.000(7) 0.008(8) -0.001(9) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' #============================================================================== # 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 Os(1) Os(2) 2.820(1) yes . . Os(1) Os(3) 2.925(1) yes . . Os(1) Rh(1) 2.880(1) yes . . Os(1) C(1) 1.91(2) yes . . Os(1) C(2) 1.91(2) yes . . Os(1) C(3) 1.91(2) yes . . Os(1) H(1) 1.78 no . . Os(1) H(2) 1.77 no . . Os(1) H(5) 1.82 no . . Os(2) Os(3) 2.967(1) yes . . Os(2) Rh(1) 2.861(1) yes . . Os(2) C(4) 1.89(2) yes . . Os(2) C(5) 1.92(2) yes . . Os(2) C(6) 1.90(2) yes . . Os(2) H(1) 1.77 no . . Os(2) H(3) 1.76 no . . Os(2) H(4) 1.83 no . . Os(3) Rh(1) 2.753(1) yes . . Os(3) C(7) 1.93(2) yes . . Os(3) C(8) 1.94(2) yes . . Os(3) C(9) 1.91(2) yes . . Os(3) H(4) 1.84 no . . Os(3) H(5) 1.82 no . . Os(4) Os(5) 2.893(1) yes . . Os(4) Rh(1) 2.874(1) yes . . Os(4) Rh(2) 2.725(2) yes . . Os(4) C(10) 1.87(2) yes . . Os(4) C(11) 1.89(2) yes . . Os(4) C(12) 1.93(3) yes . . Os(4) H(7) 1.85 no . . Os(4) H(8) 1.83 no . . Os(5) Rh(1) 2.994(1) yes . . Os(5) Rh(2) 2.734(1) yes . . Os(5) C(13) 1.92(2) yes . . Os(5) C(14) 1.91(2) yes . . Os(5) C(15) 1.89(2) yes . . Os(5) H(6) 1.87 no . . Os(5) H(8) 1.78) no . . Os(6) Os(7) 2.889(1) yes . . Os(6) Rh(2) 3.026(2) yes . . Os(6) Rh(3) 2.752(2) yes . . Os(6) C(16) 1.88(2) yes . . Os(6) C(17) 1.88(2) yes . . Os(6) C(18) 1.89(2) yes . . Os(6) H(9) 1.80 no . . Os(6) H(10) 1.87 no . . Os(7) Rh(2) 2.979(1) yes . . Os(7) Rh(3) 2.793(1) yes . . Os(7) C(19) 1.83(2) yes . . Os(7) C(20) 1.87(2) yes . . Os(7) C(21) 1.90(2) yes . . Os(7) H(9) 1.81 no . . Os(7) H(11) 1.92 no . . Rh(1) Rh(2) 2.867(2) yes . . Rh(1) Rh(3) 2.792(2) yes . . Rh(1) H(2) 1.83 no . . Rh(1) H(3) 1.83 no . . Rh(1) H(6) 1.82 no . . Rh(1) H(7) 1.75 no . . Rh(2) Rh(3) 3.064(2) yes . . Rh(2) C(22) 1.78(2) yes . . Rh(2) H(10) 1.85 no . . Rh(2) H(11) 1.75 no . . Rh(3) C(23) 1.79(2) yes . . Cl(1) C(24) 1.80(2) yes . . Cl(2) C(24) 1.80(3) yes . . O(1) C(1) 1.13(2) yes . . O(2) C(2) 1.14(2) yes . . O(3) C(3) 1.15(3) yes . . O(4) C(4) 1.14(2) yes . . O(5) C(5) 1.14(3) yes . . O(6) C(6) 1.16(3) yes . . O(7) C(7) 1.10(2) yes . . O(8) C(8) 1.16(2) yes . . O(9) C(9) 1.13(2) yes . . O(10) C(10) 1.16(3) yes . . O(11) C(11) 1.17(2) yes . . O(12) C(12) 1.14(3) yes . . O(13) C(13) 1.12(2) yes . . O(14) C(14) 1.12(2) yes . . O(15) C(15) 1.15(3) yes . . O(16) C(16) 1.15(2) yes . . O(17) C(17) 1.20(3) yes . . O(18) C(18) 1.15(3) yes . . O(19) C(19) 1.22(3) yes . . O(20) C(20) 1.16(2) yes . . O(21) C(21) 1.12(3) yes . . O(22) C(22) 1.17(2) yes . . O(23) C(23) 1.18(2) yes . . C(24) H(12) 0.95 no . . C(24) H(13) 0.97 no . . 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 Os(2) Os(1) Os(3) 62.17(3) yes . . . Os(2) Os(1) Rh(1) 60.26(3) yes . . . Os(2) Os(1) C(1) 93.3(5) yes . . . Os(2) Os(1) C(2) 85.8(6) yes . . . Os(2) Os(1) C(3) 170.1(6) yes . . . Os(2) Os(1) H(1) 37 no . . . Os(2) Os(1) H(2) 92 no . . . Os(2) Os(1) H(5) 93 no . . . Os(3) Os(1) Rh(1) 56.62(3) yes . . . Os(3) Os(1) C(1) 143.6(4) yes . . . Os(3) Os(1) C(2) 110.4(7) yes . . . Os(3) Os(1) C(3) 112.1(6) yes . . . Os(3) Os(1) H(1) 95 no . . . Os(3) Os(1) H(2) 88 no . . . Os(3) Os(1) H(5) 36 no . . . Rh(1) Os(1) C(1) 88.5(4) yes . . . Rh(1) Os(1) C(2) 146.1(6) yes . . . Rh(1) Os(1) C(3) 124.6(5) yes . . . Rh(1) Os(1) H(1) 93 no . . . Rh(1) Os(1) H(2) 37) no . . . Rh(1) Os(1) H(5) 88 no . . . C(1) Os(1) C(2) 92.6(8) yes . . . C(1) Os(1) C(3) 95.4(8) yes . . . C(1) Os(1) H(1) 75 no . . . C(1) Os(1) H(2) 65 no . . . C(1) Os(1) H(5) 170 no . . . C(2) Os(1) C(3) 89.0(8) yes . . . C(2) Os(1) H(1) 55 no . . . C(2) Os(1) H(2) 157 no . . . C(2) Os(1) H(5) 96 no . . . C(3) Os(1) H(1) 142 no . . . C(3) Os(1) H(2) 96 no . . . C(3) Os(1) H(5) 79 no . . . H(1) Os(1) H(2) 112 no . . . H(1) Os(1) H(5) 115) no . . . H(2) Os(1) H(5) 107 no . . . Os(3) Os(2) Rh(1) 56.33(3) yes . . . Os(3) Os(2) C(4) 100.5(6) yes . . . Os(3) Os(2) C(5) 149.4(7) yes . . . Os(3) Os(2) C(6) 110.7(6) yes . . . Os(3) Os(2) H(1) 94 no . . . Os(3) Os(2) H(3) 89 no . . . Os(3) Os(2) H(4) 36 no . . . Os(3) Os(2) Os(1) 60.65(3) yes . . . Rh(1) Os(2) C(4) 153.5(6) yes . . . Rh(1) Os(2) C(5) 101.6(6) yes . . . Rh(1) Os(2) C(6) 106.2(6) yes . . . Rh(1) Os(2) H(1) 93 no . . . Rh(1) Os(2) H(3) 38 no . . . Rh(1) Os(2) H(4) 87 no . . . Rh(1) Os(2) Os(1) 60.91(3) yes . . . C(4) Os(2) C(5) 93.9(8) yes . . . C(4) Os(2) C(6) 93.6(8) yes . . . C(4) Os(2) H(1) 74 no . . . C(4) Os(2) H(3) 168 no . . . C(4) Os(2) H(4) 77 no . . . C(4) Os(2) Os(1) 97.8(6) yes . . . C(5) Os(2) C(6) 95.0(9) yes . . . C(5) Os(2) H(1) 65 no . . . C(5) Os(2) H(3) 81 no . . . C(5) Os(2) H(4) 171 no . . . C(5) Os(2) Os(1) 90.9(6) yes . . . C(6) Os(2) H(1) 155 no . . . C(6) Os(2) H(3) 76 no . . . C(6) Os(2) H(4) 85 no . . . C(6) Os(2) Os(1) 166.8(6) yes . . . H(1) Os(2) H(3) 113 no . . . H(1) Os(2) H(4) 113 no . . . H(1) Os(2) Os(1) 38 no . . . H(3) Os(2) H(4) 107 no . . . H(3) Os(2) Os(1) 93 no . . . H(4) Os(2) Os(1) 91 no . . . Rh(1) Os(3) C(7) 165.2(6) yes . . . Rh(1) Os(3) C(8) 107.7(6) yes . . . Rh(1) Os(3) C(9) 88.1(5) yes . . . Rh(1) Os(3) H(4) 90 no . . . Rh(1) Os(3) H(5) 92 no . . . Rh(1) Os(3) Os(1) 60.86(3) yes . . . C(7) Os(3) C(8) 86.4(8) yes . . . C(7) Os(3) C(9) 96.4(8) yes . . . C(7) Os(3) H(4) 76 no . . . C(7) Os(3) H(5) 87 no . . . C(7) Os(3) Os(1) 112.1(5) yes . . . C(7) Os(3) Os(2) 105.4(6) yes . . . C(8) Os(3) C(9) 90.3(8) yes . . . C(8) Os(3) H(4) 162) no . . . C(8) Os(3) H(5) 77 no . . . C(8) Os(3) Os(1) 104.8(6) yes . . . C(8) Os(3) Os(2) 161.0(6) yes . . . C(9) Os(3) H(4) 85 no . . . C(9) Os(3) H(5) 166 no . . . C(9) Os(3) Os(1) 148.2(5) yes . . . C(9) Os(3) Os(2) 102.9(6) yes . . . H(4) Os(3) H(5) 108 no . . . H(4) Os(3) Os(1) 88 no . . . H(5) Os(3) Os(1) 37 no . . . Os(2) Os(3) Rh(1) 59.89(3) yes . . . Os(2) Os(3) H(4) 36 no . . . Os(2) Os(3) H(5) 89 no . . . Os(2) Os(3) Os(1) 57.18(3) yes . . . Os(5) Os(4) Rh(1) 62.56(3) yes . . . Os(5) Os(4) Rh(2) 58.15(3) yes . . . Os(5) Os(4) C(10) 147.0(6) yes . . . Os(5) Os(4) C(11) 92.4(6) yes . . . Os(5) Os(4) C(12) 117.5(7) yes . . . Os(5) Os(4) H(7) 94 no . . . Os(5) Os(4) H(8) 36 no . . . Rh(1) Os(4) Rh(2) 61.55(4) yes . . . Rh(1) Os(4) C(10) 102.8(5) yes . . . Rh(1) Os(4) C(11) 152.7(6) yes . . . Rh(1) Os(4) C(12) 105.1(6) yes . . . Rh(1) Os(4) H(7) 36 no . . . Rh(1) Os(4) H(8) 93 no . . . Rh(2) Os(4) C(10) 88.9(6) yes . . . Rh(2) Os(4) C(11) 96.9(6) yes . . . Rh(2) Os(4) C(12) 166.7(6) yes . . . Rh(2) Os(4) H(7) 92 no . . . Rh(2) Os(4) H(8) 88 no . . . C(10) Os(4) C(11) 92.6(7) yes . . . C(10) Os(4) C(12) 94.4(9) yes . . . C(10) Os(4) H(7) 86 no . . . C(10) Os(4) H(8) 160 no . . . C(11) Os(4) C(12) 95.9(9) yes . . . C(11) Os(4) H(7) 171 no . . . C(11) Os(4) H(8) 68 no . . . C(12) Os(4) H(7) 75 no . . . C(12) Os(4) H(8) 93 no . . . H(7) Os(4) H(8) 114 no . . . Rh(1) Os(5) Rh(2) 59.87(4) yes . . . Rh(1) Os(5) C(13) 152.9(6) yes . . . Rh(1) Os(5) C(14) 103.4(6) yes . . . Rh(1) Os(5) C(15) 104.9(5) yes . . . Rh(1) Os(5) H(6) 35 no . . . Rh(1) Os(5) H(8) 91 no . . . Rh(1) Os(5) Os(4) 58.41(3) yes . . . Rh(2) Os(5) C(13) 101.1(6) yes . . . Rh(2) Os(5) C(14) 162.7(6) yes . . . Rh(2) Os(5) C(15) 90.4(6) yes . . . Rh(2) Os(5) H(6) 90 no . . . Rh(2) Os(5) H(8) 89 no . . . Rh(2) Os(5) Os(4) 57.84(4) yes . . . C(13) Os(5) C(14) 96.2(8) yes . . . C(13) Os(5) C(15) 93.5(8) yes . . . C(13) Os(5) H(6) 169 no . . . C(13) Os(5) H(8) 68 no . . . C(13) Os(5) Os(4) 95.7(6) yes . . . C(14) Os(5) C(15) 90.0(9) yes . . . C(14) Os(5) H(6) 73 no . . . C(14) Os(5) H(8) 96 no . . . C(14) Os(5) Os(4) 119.2(7) yes . . . C(15) Os(5) H(6) 88 no . . . C(15) Os(5) H(8) 161 no . . . C(15) Os(5) Os(4) 148.1(6) yes . . . H(6) Os(5) H(8) 111 no . . . H(6) Os(5) Os(4) 89 no . . . H(8) Os(5) Os(4) 37 no . . . Os(7) Os(6) Rh(2) 60.42(3) yes . . . Os(7) Os(6) Rh(3) 59.30(3) yes . . . Os(7) Os(6) C(16) 146.9(6) yes . . . Os(7) Os(6) C(17) 94.5(6) yes . . . Os(7) Os(6) C(18) 118.1(6) yes . . . Os(7) Os(6) H(9) 37 no . . . Os(7) Os(6) H(10) 91 no . . . Rh(2) Os(6) Rh(3) 63.86(4) yes . . . Rh(2) Os(6) C(16) 106.7(6) yes . . . Rh(2) Os(6) C(17) 154.6(7) yes . . . Rh(2) Os(6) C(18) 102.0(6) yes . . . Rh(2) Os(6) H(9) 92 no . . . Rh(2) Os(6) H(10) 35 no . . . Rh(3) Os(6) C(16) 87.6(6) yes . . . Rh(3) Os(6) C(17) 101.0(6) yes . . . Rh(3) Os(6) C(18) 165.5(6) yes . . . Rh(3) Os(6) H(9) 89 no . . . Rh(3) Os(6) H(10) 94 no . . . C(16) Os(6) C(17) 92.0(8) yes . . . C(16) Os(6) C(18) 93.8(8) yes . . . C(16) Os(6) H(9) 157 no . . . C(16) Os(6) H(10) 91 no . . . C(17) Os(6) C(18) 93.4(8) yes . . . C(17) Os(6) H(9) 67 no . . . C(17) Os(6) H(10) 165 no . . . C(18) Os(6) H(9) 95 no . . . C(18) Os(6) H(10) 71 no . . . H(9) Os(6) H(10) 111 no . . . Rh(2) Os(7) Rh(3) 64.04(4) yes . . . Rh(2) Os(7) C(19) 152.6(7) yes . . . Rh(2) Os(7) C(20) 102.8(5) yes . . . Rh(2) Os(7) C(21) 106.7(6) yes . . . Rh(2) Os(7) H(9) 93 no . . . Rh(2) Os(7) H(11) 34 no . . . Rh(2) Os(7) Os(6) 62.05(3) yes . . . Rh(3) Os(7) C(19) 100.7(6) yes . . . Rh(3) Os(7) C(20) 166.8(5) yes . . . Rh(3) Os(7) C(21) 91.0(6) yes . . . Rh(3) Os(7) H(9) 88 no . . . Rh(3) Os(7) H(11) 93 no . . . Rh(3) Os(7) Os(6) 57.89(4) yes . . . C(19) Os(7) C(20) 91.7(8) yes . . . C(19) Os(7) C(21) 95.7(9) yes . . . C(19) Os(7) H(9) 62 no . . . C(19) Os(7) H(11) 164 no . . . C(19) Os(7) Os(6) 90.6(7) yes . . . C(20) Os(7) C(21) 92.3(8) yes . . . C(20) Os(7) H(9) 94 no . . . C(20) Os(7) H(11) 74 no . . . C(20) Os(7) Os(6) 118.0(6) yes . . . C(21) Os(7) H(9) 157 no . . . C(21) Os(7) H(11) 90 no . . . C(21) Os(7) Os(6) 148.9(6) yes . . . H(9) Os(7) H(11) 113 no . . . H(9) Os(7) Os(6) 37 no . . . H(11) Os(7) Os(6) 92 no . . . Rh(2) Rh(1) Rh(3) 65.55(5) yes . . . Rh(2) Rh(1) H(2) 92 no . . . Rh(2) Rh(1) H(3) 138 no . . . Rh(2) Rh(1) H(6) 87 no . . . Rh(2) Rh(1) H(7) 90 no . . . Rh(2) Rh(1) Os(1) 124.03(6) yes . . . Rh(2) Rh(1) Os(2) 174.40(6) yes . . . Rh(2) Rh(1) Os(3) 121.63(5) yes . . . Rh(2) Rh(1) Os(4) 56.66(4) yes . . . Rh(3) Rh(1) H(2) 61 no . . . Rh(3) Rh(1) H(3) 156 no . . . Rh(3) Rh(1) H(6) 118 no . . . Rh(3) Rh(1) H(7) 120 no . . . Rh(3) Rh(1) Os(1) 69.02(4) yes . . . Rh(3) Rh(1) Os(2) 119.61(5) yes . . . Rh(3) Rh(1) Os(3) 66.62(4) yes . . . Rh(3) Rh(1) Os(4) 112.84(5) yes . . . Rh(3) Rh(1) Os(5) 111.50(6) yes . . . H(2) Rh(1) H(3) 108 no . . . H(2) Rh(1) H(6) 67 no . . . H(2) Rh(1) H(7) 179 no . . . H(2) Rh(1) Os(1) 36 no . . . H(2) Rh(1) Os(4) 143 no . . . H(2) Rh(1) Os(5) 88 no . . . H(3) Rh(1) H(6) 69 no . . . H(3) Rh(1) H(7) 71 no . . . H(3) Rh(1) Os(1) 89 no . . . H(3) Rh(1) Os(4) 89 no . . . H(3) Rh(1) Os(5) 88 no . . . H(6) Rh(1) H(7) 113 no . . . H(6) Rh(1) Os(1) 87 no . . . H(6) Rh(1) Os(2) 89 no . . . H(6) Rh(1) Os(3) 146 no . . . H(6) Rh(1) Os(4) 90 no . . . H(7) Rh(1) Os(1) 143 no . . . H(7) Rh(1) Os(2) 89 no . . . H(7) Rh(1) Os(3) 87 no . . . H(7) Rh(1) Os(4) 38 no . . . Os(1) Rh(1) Os(4) 177.70(5) yes . . . Os(1) Rh(1) Os(5) 119.23(5) yes . . . Os(2) Rh(1) H(2) 89 no . . . Os(2) Rh(1) H(3) 36 no . . . Os(2) Rh(1) Os(1) 58.83(3) yes . . . Os(2) Rh(1) Os(3) 63.78(3) yes . . . Os(2) Rh(1) Os(4) 120.27(5) yes . . . Os(2) Rh(1) Os(5) 119.02(5) yes . . . Os(3) Rh(1) H(2) 93 no . . . Os(3) Rh(1) H(3) 94 no . . . Os(3) Rh(1) Os(1) 62.52(3) yes . . . Os(3) Rh(1) Os(4) 119.29(5) yes . . . Os(3) Rh(1) Os(5) 177.11(5) yes . . . Os(5) Rh(1) Rh(2) 55.55(4) yes . . . Os(5) Rh(1) H(6) 36 no . . . Os(5) Rh(1) H(7) 92 no . . . Os(5) Rh(1) Os(4) 59.04(3) yes . . . Rh(3) Rh(2) C(22) 154.0(6) yes . . . Rh(3) Rh(2) H(10) 85 no . . . Rh(3) Rh(2) H(11) 88 no . . . Rh(3) Rh(2) Os(4) 109.12(5) yes . . . Rh(3) Rh(2) Os(5) 111.08(5) yes . . . Rh(3) Rh(2) Os(6) 53.72(4) yes . . . C(22) Rh(2) H(10) 79 no . . . C(22) Rh(2) H(11) 79 no . . . C(22) Rh(2) Os(4) 94.8(6) yes . . . C(22) Rh(2) Os(5) 88.1(5) yes . . . C(22) Rh(2) Os(6) 103.6(6) yes . . . C(22) Rh(2) Os(7) 103.8(5) yes . . . C(22) Rh(2) Rh(1) 149.4(6) yes . . . H(10) Rh(2) H(11) 111 no . . . H(10) Rh(2) Os(4) 149 no . . . H(10) Rh(2) Os(5) 85 no . . . H(10) Rh(2) Os(6) 36 no . . . H(10) Rh(2) Rh(1) 110 no . . . H(11) Rh(2) Os(4) 97 no . . . H(11) Rh(2) Os(5) 156 no . . . H(11) Rh(2) Os(6) 91 no . . . H(11) Rh(2) Rh(1) 121 no . . . Os(4) Rh(2) Os(6) 160.98(5) yes . . . Os(4) Rh(2) Os(7) 122.43(5) yes . . . Os(5) Rh(2) Os(4) 64.01(4) yes . . . Os(5) Rh(2) Os(6) 111.65(5) yes . . . Os(5) Rh(2) Os(7) 165.31(5) yes . . . Os(5) Rh(2) Rh(1) 64.58(4) yes . . . Os(6) Rh(2) Rh(1) 99.33(4) yes . . . Os(7) Rh(2) Rh(3) 55.04(3) yes . . . Os(7) Rh(2) H(10) 89 no . . . Os(7) Rh(2) H(11) 38 no . . . Os(7) Rh(2) Os(6) 57.53(3) yes . . . Os(7) Rh(2) Rh(1) 105.57(5) yes . . . Rh(1) Rh(2) Rh(3) 56.04(4) yes . . . Rh(1) Rh(2) Os(4) 61.79(4) yes . . . C(23) Rh(3) Os(6) 81.6(6) yes . . . C(23) Rh(3) Os(7) 86.7(5) yes . . . C(23) Rh(3) Rh(1) 160.3(5) yes . . . C(23) Rh(3) Rh(2) 139.3(5) yes . . . Os(6) Rh(3) Rh(1) 108.29(5) yes . . . Os(7) Rh(3) Os(6) 62.81(4) yes . . . Os(7) Rh(3) Rh(1) 112.94(5) yes . . . Os(7) Rh(3) Rh(2) 60.92(4) yes . . . Rh(1) Rh(3) Rh(2) 58.41(4) yes . . . Rh(2) Rh(3) Os(6) 62.42(4) yes . . . Os(1) C(1) O(1) 177(1) yes . . . Os(1) C(2) O(2) 176(2) yes . . . Os(1) C(3) O(3) 174(1) yes . . . Os(2) C(4) O(4) 178(1) yes . . . Os(2) C(5) O(5) 179(2) yes . . . Os(2) C(6) O(6) 177(1) yes . . . Os(3) C(7) O(7) 178(1) yes . . . Os(3) C(8) O(8) 158(1) yes . . . Os(3) C(9) O(9) 177(2) yes . . . Os(4) C(10) O(10) 178.9(9) yes . . . Os(4) C(11) O(11) 175(1) yes . . . Os(4) C(12) O(12) 178(1) yes . . . Os(5) C(13) O(13) 176(1) yes . . . Os(5) C(14) O(14) 179(2) yes . . . Os(5) C(15) O(15) 178(1) yes . . . Os(6) C(16) O(16) 177(1) yes . . . Os(6) C(17) O(17) 174(1) yes . . . Os(6) C(18) O(18) 176(1) yes . . . Os(7) C(19) O(19) 172(1) yes . . . Os(7) C(20) O(20) 178(1) yes . . . Os(7) C(21) O(21) 177(1) yes . . . Rh(2) C(22) O(22) 177(1) yes . . . Rh(3) C(23) O(23) 176(1) yes . . . H(12) C(24) H(13) 108 no . . . H(12) C(24) Cl(1) 108 no . . . H(12) C(24) Cl(2) 109 no . . . H(13) C(24) Cl(1) 107 no . . . H(13) C(24) Cl(2) 107 no . . . Cl(1) C(24) Cl(2) 117(1) yes . . . Os(2) H(1) Os(1) 105 no . . . Rh(1) H(2) Os(1) 106 no . . . Os(2) H(3) Rh(1) 106 no . . . Os(2) H(4) Os(3) 108 no . . . Os(3) H(5) Os(1) 107 no . . . Os(5) H(6) Rh(1) 108 no . . . Rh(1) H(7) Os(4) 106 no . . . Os(5) H(8) Os(4) 107 no . . . Os(7) H(9) Os(6) 106 no . . . Rh(2) H(10) Os(6) 109 no . . . Os(7) H(11) Rh(2) 108 no . . . #============================================================================== # 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 #============================================================================== data_wt0912w _database_code_depnum_ccdc_archive 'CCDC 262819' #-JAS005---Compound 4 _audit_creation_date 2005-02-01 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? _publ_section_references ; Bruker AXS Inc. (1998) SMART version 5.054, Madison, Wisconsin, USA. Bruker AXS Inc. (1999) SAINT, version 6.02, Madison, Wisconsin, USA. Farrugia, L.J. (1997) Ortep-3 J. Appl. Cryst. 30, 565. Johnson, C. K. (1976) ORTEP-II, A FORTRAN Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Rigaku/MSC and Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Sheldrick, G.M. (1997) SHELXS-97, Gottingen University, Gottingen, Germany. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; All non-H atoms were refined anisotropically. The C-bound H atoms were placed at their geometrically calculated positions with C-H = 0.95 \%A and in the riding model with U~iso~(H) = 1.2 U~eq~(C). The hydrido atom (H9) was placed at its calculated position and not refined. ; #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C19 H9 O12 Os4 Rh ' _chemical_formula_moiety 'C19 H9 O12 Os4 Rh ' _chemical_formula_weight 1292.98 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 #------------------------------------------------------------------------------ _cell_length_a 8.605(2) _cell_length_b 16.268(5) _cell_length_c 17.416(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.24(1) _cell_angle_gamma 90.00 _cell_volume 2431.3(12) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15317 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 298(1) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 3.532 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272.00 _exptl_absorpt_coefficient_mu 21.539 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.660 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15317 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9722 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9722 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5632 _reflns_number_gt 3947 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0290 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 3964 _refine_ls_number_parameters 333 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + 1.0000\s(Fo^2^) + 0.0001]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.31 _refine_diff_density_min -1.37 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os Os -1.216 7.603 ; 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) ; C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 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) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 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 Os(1) Os 0.09786(4) 0.27242(2) 0.20001(2) 0.02947(10) Uani 1.00 1 d . . . Os(2) Os 0.31257(5) 0.38529(2) 0.15406(2) 0.03400(11) Uani 1.00 1 d . . . Os(3) Os 0.41893(4) 0.23140(2) 0.20505(2) 0.02941(10) Uani 1.00 1 d . . . Os(4) Os 0.19638(4) 0.11751(2) 0.15385(2) 0.03113(11) Uani 1.00 1 d . . . Rh(1) Rh 0.24568(8) 0.25099(5) 0.06751(4) 0.0284(2) Uani 1.00 1 d . . . O(1) O -0.1648(9) 0.3305(6) 0.0867(5) 0.070(3) Uani 1.00 1 d . . . O(2) O -0.1065(10) 0.1540(5) 0.2823(5) 0.069(3) Uani 1.00 1 d . . . O(3) O 0.0391(10) 0.4118(5) 0.3113(4) 0.057(3) Uani 1.00 1 d . . . O(4) O 0.3605(10) 0.5008(5) 0.2904(5) 0.069(3) Uani 1.00 1 d . . . O(5) O 0.0859(11) 0.5045(6) 0.0742(5) 0.081(3) Uani 1.00 1 d . . . O(6) O 0.5809(10) 0.4492(5) 0.0678(5) 0.061(3) Uani 1.00 1 d . . . O(7) O 0.6446(11) 0.3525(6) 0.2865(6) 0.091(4) Uani 1.00 1 d . . . O(8) O 0.6557(10) 0.1690(6) 0.0969(5) 0.069(3) Uani 1.00 1 d . . . O(9) O 0.5102(10) 0.1079(5) 0.3318(4) 0.061(3) Uani 1.00 1 d . . . O(10) O 0.3932(10) -0.0028(6) 0.0713(5) 0.075(3) Uani 1.00 1 d . . . O(11) O -0.0954(9) 0.0459(5) 0.0700(5) 0.055(3) Uani 1.00 1 d . . . O(12) O 0.1842(10) 0.0095(6) 0.2953(5) 0.072(3) Uani 1.00 1 d . . . C(1) C -0.0691(13) 0.3063(7) 0.1289(6) 0.046(3) Uani 1.00 1 d . . . C(2) C -0.0249(13) 0.1936(6) 0.2498(6) 0.044(3) Uani 1.00 1 d . . . C(3) C 0.0639(12) 0.3615(7) 0.2678(6) 0.040(3) Uani 1.00 1 d . . . C(4) C 0.3466(13) 0.4586(6) 0.2373(7) 0.045(3) Uani 1.00 1 d . . . C(5) C 0.1731(13) 0.4592(6) 0.1037(6) 0.042(3) Uani 1.00 1 d . . . C(6) C 0.484(1) 0.4238(7) 0.1009(6) 0.044(3) Uani 1.00 1 d . . . C(7) C 0.554(1) 0.3126(7) 0.2534(7) 0.053(4) Uani 1.00 1 d . . . C(8) C 0.5684(13) 0.1939(7) 0.1379(6) 0.048(3) Uani 1.00 1 d . . . C(9) C 0.4730(12) 0.1521(6) 0.2831(6) 0.039(3) Uani 1.00 1 d . . . C(10) C 0.321(1) 0.0431(7) 0.1033(6) 0.045(3) Uani 1.00 1 d . . . C(11) C 0.0107(13) 0.0749(7) 0.1021(6) 0.040(3) Uani 1.00 1 d . . . C(12) C 0.1856(12) 0.0486(6) 0.2398(7) 0.043(3) Uani 1.00 1 d . . . C(13) C 0.1270(13) 0.3103(7) -0.0415(5) 0.044(3) Uani 1.00 1 d . . . C(14) C 0.285(1) 0.3334(7) -0.0375(6) 0.048(4) Uani 1.00 1 d . . . C(15) C 0.4005(13) 0.2706(7) -0.0327(6) 0.046(3) Uani 1.00 1 d . . . C(16) C 0.354(2) 0.1886(8) -0.0337(6) 0.056(4) Uani 1.00 1 d . . . C(17) C 0.1903(13) 0.1681(7) -0.0397(5) 0.041(3) Uani 1.00 1 d . . . C(18) C 0.0773(13) 0.2294(7) -0.0439(5) 0.044(3) Uani 1.00 1 d . . . C(19) C -0.096(1) 0.2087(9) -0.0554(6) 0.068(4) Uani 1.00 1 d . . . H(1) H 0.0505(13) 0.3524(7) -0.0426(5) 0.053(3) Uiso 1.00 1 c . . . H(2) H 0.314(1) 0.3898(7) -0.0379(6) 0.058(4) Uiso 1.00 1 c . . . H(3) H 0.5080(13) 0.2845(7) -0.0289(6) 0.056(4) Uiso 1.00 1 c . . . H(4) H 0.430(2) 0.1462(8) -0.0305(6) 0.068(4) Uiso 1.00 1 c . . . H(5) H 0.1595(13) 0.1120(7) -0.0408(5) 0.049(3) Uiso 1.00 1 c . . . H(6) H -0.149(1) 0.2315(9) -0.0144(6) 0.081(5) Uiso 1.00 1 c . . . H(7) H -0.138(1) 0.2311(9) -0.1029(6) 0.081(5) Uiso 1.00 1 c . . . H(8) H -0.109(1) 0.1508(9) -0.0560(6) 0.081(5) Uiso 1.00 1 c . . . H(9) H 0.2642 0.2523 0.2647 0.0380 Uiso 1.00 1 c . . . 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 Os(1) 0.0303(2) 0.0290(2) 0.0290(2) 0.0026(2) 0.0016(2) -0.0025(2) Os(2) 0.0415(2) 0.0222(2) 0.0371(2) -0.0028(2) -0.0051(2) 0.0010(2) Os(3) 0.0288(2) 0.0268(2) 0.0319(2) 0.0006(2) -0.0028(2) 0.0023(2) Os(4) 0.0374(2) 0.0228(2) 0.0330(2) -0.0026(2) 0.0013(2) 0.0004(2) Rh(1) 0.0331(4) 0.0268(4) 0.0251(4) -0.0001(3) 0.0006(3) 0.0009(3) O(1) 0.057(5) 0.094(7) 0.056(5) 0.036(5) -0.020(4) -0.008(5) O(2) 0.073(6) 0.053(6) 0.085(7) -0.021(5) 0.032(5) -0.002(5) O(3) 0.080(6) 0.045(5) 0.048(5) 0.014(4) 0.007(4) -0.021(4) O(4) 0.095(7) 0.057(6) 0.054(5) -0.020(5) -0.007(5) -0.019(5) O(5) 0.097(7) 0.062(6) 0.080(7) 0.038(5) -0.020(5) -0.000(5) O(6) 0.056(5) 0.054(6) 0.074(6) -0.007(4) 0.006(4) 0.015(4) O(7) 0.080(7) 0.068(7) 0.117(8) -0.021(6) -0.049(6) 0.004(6) O(8) 0.060(6) 0.090(7) 0.061(6) 0.010(5) 0.028(5) 0.007(5) O(9) 0.087(6) 0.052(5) 0.046(5) 0.033(5) 0.011(4) 0.019(4) O(10) 0.085(7) 0.076(7) 0.064(6) 0.030(5) 0.010(5) -0.016(5) O(11) 0.051(5) 0.048(5) 0.062(5) -0.013(4) -0.014(4) 0.003(4) O(12) 0.091(7) 0.071(6) 0.051(5) -0.018(5) -0.009(5) 0.029(5) C(1) 0.044(7) 0.050(7) 0.044(7) 0.008(5) -0.003(5) -0.008(5) C(2) 0.053(7) 0.024(6) 0.056(7) -0.003(5) 0.005(6) -0.006(5) C(3) 0.039(6) 0.043(7) 0.036(6) 0.006(5) -0.001(5) 0.010(5) C(4) 0.057(7) 0.022(5) 0.055(7) -0.003(5) -0.003(5) 0.005(5) C(5) 0.065(8) 0.023(5) 0.039(6) 0.005(5) 0.001(5) -0.005(5) C(6) 0.057(8) 0.040(7) 0.036(6) 0.003(6) -0.002(5) -0.001(5) C(7) 0.055(8) 0.029(6) 0.073(8) -0.006(5) -0.018(6) 0.010(6) C(8) 0.042(7) 0.070(8) 0.029(6) 0.004(6) -0.006(5) 0.003(5) C(9) 0.049(7) 0.030(6) 0.038(6) 0.010(5) -0.002(5) -0.003(5) C(10) 0.064(8) 0.036(6) 0.034(6) 0.004(6) -0.005(5) -0.001(5) C(11) 0.048(7) 0.039(6) 0.034(6) 0.004(5) 0.001(5) 0.004(5) C(12) 0.049(7) 0.026(6) 0.054(7) -0.006(5) 0.002(5) -0.011(5) C(13) 0.053(7) 0.052(7) 0.027(5) 0.003(6) 0.001(5) 0.008(5) C(14) 0.067(8) 0.043(7) 0.035(6) -0.007(6) 0.006(5) 0.008(5) C(15) 0.050(7) 0.058(8) 0.032(6) -0.004(6) 0.013(5) 0.003(5) C(16) 0.085(10) 0.059(8) 0.026(6) 0.017(7) 0.010(6) -0.007(5) C(17) 0.060(7) 0.037(6) 0.026(5) -0.010(5) 0.002(5) -0.004(4) C(18) 0.052(7) 0.052(7) 0.028(5) -0.003(6) -0.004(5) 0.001(5) C(19) 0.068(9) 0.095(11) 0.038(7) -0.011(8) -0.009(6) -0.001(7) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' #============================================================================== # 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 Os(1) Os(2) 2.7648(5) yes . . Os(1) Os(3) 2.8373(5) yes . . Os(1) Os(4) 2.7958(5) yes . . Os(1) Rh(1) 2.7384(8) yes . . Os(1) C(1) 1.91(1) yes . . Os(1) C(2) 1.91(1) yes . . Os(1) C(3) 1.91(1) yes . . Os(1) H(9) 1.79 no . . Os(2) Os(3) 2.7881(5) yes . . Os(2) Rh(1) 2.6923(8) yes . . Os(2) C(4) 1.88(1) yes . . Os(2) C(5) 1.87(1) yes . . Os(2) C(6) 1.90(1) yes . . Os(3) Os(4) 2.7646(5) yes . . Os(3) Rh(1) 2.7448(8) yes . . Os(3) C(7) 1.91(1) yes . . Os(3) C(8) 1.90(1) yes . . Os(3) C(9) 1.91(1) yes . . Os(3) H(9) 1.78 no . . Os(4) Rh(1) 2.6927(8) yes . . Os(4) C(10) 1.88(1) yes . . Os(4) C(11) 1.91(1) yes . . Os(4) C(12) 1.88(1) yes . . Rh(1) C(13) 2.30(1) yes . . Rh(1) C(14) 2.31(1) yes . . Rh(1) C(15) 2.29(1) yes . . Rh(1) C(16) 2.29(1) yes . . Rh(1) C(17) 2.32(1) yes . . Rh(1) C(18) 2.36(1) yes . . O(1) C(1) 1.13(1) yes . . O(2) C(2) 1.13(1) yes . . O(3) C(3) 1.15(1) yes . . O(4) C(4) 1.15(1) yes . . O(5) C(5) 1.15(1) yes . . O(6) C(6) 1.13(1) yes . . O(7) C(7) 1.14(1) yes . . O(8) C(8) 1.15(1) yes . . O(9) C(9) 1.14(1) yes . . O(10) C(10) 1.14(1) yes . . O(11) C(11) 1.14(1) yes . . O(12) C(12) 1.16(1) yes . . C(13) C(14) 1.40(2) yes . . C(13) C(18) 1.38(2) yes . . C(13) H(1) 0.95(2) no . . C(14) C(15) 1.43(2) yes . . C(14) H(2) 0.95(2) no . . C(15) C(16) 1.39(2) yes . . C(15) H(3) 0.95(2) no . . C(16) C(17) 1.44(2) yes . . C(16) H(4) 0.95(2) no . . C(17) C(18) 1.39(2) yes . . C(17) H(5) 0.95(2) no . . C(18) C(19) 1.53(2) yes . . C(19) H(6) 0.95(2) no . . C(19) H(7) 0.95(2) no . . C(19) H(8) 0.95(2) no . . 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(1) Os(4) C(10) 98.0(3) yes . . . Rh(1) Os(4) C(11) 101.0(3) yes . . . Rh(1) Os(4) C(12) 161.0(3) yes . . . Rh(1) Os(4) Os(1) 59.82(2) yes . . . Rh(1) Os(4) Os(3) 60.38(2) yes . . . C(10) Os(4) C(11) 91.8(5) yes . . . C(10) Os(4) C(12) 93.0(5) yes . . . C(10) Os(4) Os(1) 155.6(3) yes . . . C(10) Os(4) Os(3) 100.2(3) yes . . . C(11) Os(4) C(12) 94.0(4) yes . . . C(11) Os(4) Os(1) 101.7(3) yes . . . C(11) Os(4) Os(3) 158.9(3) yes . . . C(12) Os(4) Os(1) 106.0(3) yes . . . C(12) Os(4) Os(3) 102.5(3) yes . . . Os(1) Os(4) Os(3) 61.36(1) yes . . . C(13) Rh(1) C(14) 35.5(4) yes . . . C(13) Rh(1) C(15) 64.0(4) yes . . . C(13) Rh(1) C(16) 74.4(4) yes . . . C(13) Rh(1) C(17) 61.9(4) yes . . . C(13) Rh(1) C(18) 34.5(4) yes . . . C(13) Rh(1) Os(1) 115.9(3) yes . . . C(13) Rh(1) Os(2) 100.7(3) yes . . . C(13) Rh(1) Os(3) 161.5(3) yes . . . C(13) Rh(1) Os(4) 136.1(3) yes . . . C(14) Rh(1) C(15) 36.0(4) yes . . . C(14) Rh(1) C(16) 63.7(4) yes . . . C(14) Rh(1) C(17) 74.6(4) yes . . . C(14) Rh(1) C(18) 63.4(4) yes . . . C(14) Rh(1) Os(1) 134.1(3) yes . . . C(14) Rh(1) Os(2) 86.2(3) yes . . . C(14) Rh(1) Os(3) 131.0(3) yes . . . C(14) Rh(1) Os(4) 161.4(3) yes . . . C(15) Rh(1) C(16) 35.4(4) yes . . . C(15) Rh(1) C(17) 64.3(4) yes . . . C(15) Rh(1) C(18) 75.6(4) yes . . . C(15) Rh(1) Os(1) 162.8(3) yes . . . C(15) Rh(1) Os(2) 101.6(3) yes . . . C(15) Rh(1) Os(3) 111.8(3) yes . . . C(15) Rh(1) Os(4) 131.4(3) yes . . . C(16) Rh(1) C(17) 36.4(4) yes . . . C(16) Rh(1) C(18) 64.0(4) yes . . . C(16) Rh(1) Os(1) 161.0(3) yes . . . C(16) Rh(1) Os(2) 135.1(3) yes . . . C(16) Rh(1) Os(3) 113.3(3) yes . . . C(16) Rh(1) Os(4) 99.3(3) yes . . . C(17) Rh(1) C(18) 34.6(4) yes . . . C(17) Rh(1) Os(1) 132.1(3) yes . . . C(17) Rh(1) Os(2) 160.6(3) yes . . . C(17) Rh(1) Os(3) 134.4(3) yes . . . C(17) Rh(1) Os(4) 87.1(3) yes . . . C(18) Rh(1) Os(1) 114.6(3) yes . . . C(18) Rh(1) Os(2) 132.3(3) yes . . . C(18) Rh(1) Os(3) 163.9(3) yes . . . C(18) Rh(1) Os(4) 103.1(3) yes . . . Os(1) Rh(1) Os(2) 61.20(2) yes . . . Os(1) Rh(1) Os(3) 62.32(2) yes . . . Os(2) Rh(1) Os(3) 61.69(2) yes . . . Os(2) Rh(1) Os(4) 112.19(3) yes . . . Os(4) Rh(1) Os(1) 61.96(2) yes . . . Os(4) Rh(1) Os(3) 61.11(2) yes . . . Os(1) C(1) O(1) 176(1) yes . . . Os(1) C(2) O(2) 172(1) yes . . . Os(1) C(3) O(3) 175.8(9) yes . . . Os(2) C(4) O(4) 175(1) yes . . . Os(2) C(5) O(5) 178(1) yes . . . Os(2) C(6) O(6) 176(1) yes . . . Os(3) C(7) O(7) 171(1) yes . . . Os(3) C(8) O(8) 177(1) yes . . . Os(3) C(9) O(9) 176.2(8) yes . . . Os(4) C(10) O(10) 178.1(9) yes . . . Os(4) C(11) O(11) 176(1) yes . . . Os(4) C(12) O(12) 176.0(9) yes . . . C(14) C(13) C(18) 123(1) yes . . . C(14) C(13) H(1) 118(1) no . . . C(18) C(13) H(1) 118(1) no . . . H(1) C(13) Rh(1) 125.7(9) no . . . Rh(1) C(13) C(14) 72.7(6) yes . . . Rh(1) C(13) C(18) 75.2(6) yes . . . C(15) C(14) H(2) 120(1) no . . . H(2) C(14) Rh(1) 128(1) no . . . H(2) C(14) C(13) 120(1) no . . . Rh(1) C(14) C(15) 71.3(6) yes . . . Rh(1) C(14) C(13) 71.8(6) yes . . . C(13) C(14) C(15) 118(1) yes . . . C(16) C(15) H(3) 120(1) no . . . H(3) C(15) Rh(1) 126.7(9) no . . . H(3) C(15) C(14) 120(1) no . . . Rh(1) C(15) C(16) 72.1(6) yes . . . Rh(1) C(15) C(14) 72.6(6) yes . . . C(14) C(15) C(16) 119(1) yes . . . C(17) C(16) H(4) 119(1) no . . . H(4) C(16) Rh(1) 126(1) no . . . H(4) C(16) C(15) 119(1) no . . . Rh(1) C(16) C(17) 73.1(6) yes . . . Rh(1) C(16) C(15) 72.5(6) yes . . . C(15) C(16) C(17) 120(1) yes . . . C(18) C(17) H(5) 119(1) no . . . H(5) C(17) Rh(1) 127.9(9) no . . . H(5) C(17) C(16) 119(1) no . . . Rh(1) C(17) C(18) 74.2(6) yes . . . Rh(1) C(17) C(16) 70.5(6) yes . . . C(16) C(17) C(18) 120(1) yes . . . C(19) C(18) Rh(1) 132.4(7) yes . . . C(19) C(18) C(13) 120(1) yes . . . C(19) C(18) C(17) 121(1) yes . . . Rh(1) C(18) C(13) 70.3(6) yes . . . Rh(1) C(18) C(17) 71.3(6) yes . . . C(13) C(18) C(17) 117(1) yes . . . H(6) C(19) H(7) 109(1) no . . . H(6) C(19) H(8) 109(1) no . . . H(6) C(19) C(18) 109(1) no . . . H(7) C(19) H(8) 109(1) no . . . H(7) C(19) C(18) 109(1) no . . . H(8) C(19) C(18) 109(1) no . . . Os(1) H(9) Os(3) 105 no . . . #============================================================================== # 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 #============================================================================== data__wt0914w _database_code_depnum_ccdc_archive 'CCDC 262820' #-JAS007---Compound 6 _audit_creation_date 2005-02-03 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? _publ_section_comment ; Bruker AXS Inc. (1998) SMART version 5.054, Madison, Wisconsin, USA. Bruker AXS Inc. (1999) SAINT, version 6.02, Madison, Wisconsin, USA. Farrugia, L.J. (1997) Ortep-3 J. Appl. Cryst. 30, 565. Johnson, C. K. (1976) ORTEP-II, A FORTRAN Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Rigaku/MSC and Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Sheldrick, G.M. (1990) SHELXS-86, Acta Cryst. A46, 467-473. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; Metal (Os and Rh) and Cl(1 and 2) atoms were refined anisotropically, while the rest (C and O atoms) and the solvent molecule (Cl3 and Cl4) were failed to refine anisotropically and thus refined isotropically. The C-bound H atoms and the metal-bound hydrido atoms were placed at their geometrically calculated positions and not refined. ; #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C37 H18 Cl4 O36 Os10 Rh6 ' _chemical_formula_moiety '2(C18 H8 Cl O18 Os5 Rh3), C H2 Cl2 ' _chemical_formula_weight 3699.77 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 #------------------------------------------------------------------------------ _cell_length_a 8.522(2) _cell_length_b 21.992(5) _cell_length_c 37.291(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.15(1) _cell_angle_gamma 90.00 _cell_volume 6987.5(30) _cell_formula_units_Z 4 _cell_measurement_reflns_used 44169 _cell_measurement_theta_min 0.9 _cell_measurement_theta_max 27.6 _cell_measurement_temperature 298.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 3.517 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6504.00 _exptl_absorpt_coefficient_mu 19.693 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.878 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 88340 _diffrn_reflns_av_R_equivalents 0.146 _diffrn_reflns_theta_max 27.56 _diffrn_measured_fraction_theta_max 0.9797 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.9797 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 48 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 16243 _reflns_number_gt 5410 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.0630 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5482 _refine_ls_number_parameters 463 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + 1.0000\s(Fo^2^) + 0.002]' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 2.86 _refine_diff_density_min -2.31 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os Os -1.216 7.603 ; 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) ; C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 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) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; 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 Os(1) Os 0.6057(2) 0.63490(8) -0.03433(5) 0.0349(6) Uani 1.00 1 d . . . Os(2) Os 0.3680(2) 0.66114(8) 0.01735(5) 0.0379(6) Uani 1.00 1 d . . . Os(3) Os 0.7497(2) 0.82747(8) 0.05698(5) 0.0391(6) Uani 1.00 1 d . . . Os(4) Os 0.3531(2) 0.87605(8) -0.04071(5) 0.0401(6) Uani 1.00 1 d . . . Os(5) Os 0.5820(2) 0.82892(8) -0.08818(5) 0.0423(6) Uani 1.00 1 d . . . Os(6) Os 0.9962(2) 0.40610(9) -0.18408(6) 0.0458(6) Uani 1.00 1 d . . . Os(7) Os 1.2332(2) 0.49410(9) -0.16635(6) 0.0455(7) Uani 1.00 1 d . . . Os(8) Os 0.8440(2) 0.64792(9) -0.21058(6) 0.0534(7) Uani 1.00 1 d . . . Os(9) Os 1.1972(2) 0.55264(9) -0.30137(5) 0.0456(6) Uani 1.00 1 d . . . Os(10) Os 0.9589(2) 0.45951(9) -0.30650(5) 0.0459(6) Uani 1.00 1 d . . . Rh(1) Rh 0.4318(4) 0.7457(2) -0.04366(10) 0.0355(11) Uani 1.00 1 d . . . Rh(2) Rh 0.6513(4) 0.7180(2) 0.01783(10) 0.0354(11) Uani 1.00 1 d . . . Rh(3) Rh 0.6443(4) 0.8436(2) -0.01735(10) 0.0366(11) Uani 1.00 1 d . . . Rh(4) Rh 1.1404(4) 0.4657(2) -0.24085(10) 0.0448(12) Uani 1.00 1 d . . . Rh(5) Rh 0.9416(4) 0.5264(2) -0.18753(11) 0.0457(13) Uani 1.00 1 d . . . Rh(6) Rh 0.9189(4) 0.5618(2) -0.26787(10) 0.0430(12) Uani 1.00 1 d . . . Cl(1) Cl 0.8895(12) 0.7856(5) 0.0051(3) 0.045(4) Uani 1.00 1 d . . . Cl(2) Cl 0.6899(13) 0.5549(5) -0.2237(3) 0.052(4) Uani 1.00 1 d . . . Cl(3) Cl 0.580(2) 0.6898(9) 0.1323(6) 0.146(8) Uiso 1.00 1 d . . . Cl(4) Cl 0.292(2) 0.7538(9) 0.1641(6) 0.141(8) Uiso 1.00 1 d . . . O(1) O 0.936(4) 0.657(2) -0.0617(10) 0.083(12) Uiso 1.00 1 d . . . O(2) O 0.510(4) 0.574(2) -0.1037(10) 0.073(11) Uiso 1.00 1 d . . . O(3) O 0.714(4) 0.518(2) 0.0013(10) 0.069(10) Uiso 1.00 1 d . . . O(4) O 0.048(5) 0.603(2) 0.0093(10) 0.089(12) Uiso 1.00 1 d . . . O(5) O 0.451(4) 0.561(2) 0.0705(10) 0.074(11) Uiso 1.00 1 d . . . O(6) O 0.255(4) 0.754(2) 0.0720(11) 0.090(12) Uiso 1.00 1 d . . . O(7) O 0.947(4) 0.758(2) 0.1138(10) 0.079(11) Uiso 1.00 1 d . . . O(8) O 0.525(4) 0.874(2) 0.1090(10) 0.077(11) Uiso 1.00 1 d . . . O(9) O 0.944(4) 0.944(1) 0.0556(8) 0.061(9) Uiso 1.00 1 d . . . O(10) O 0.269(4) 0.887(1) 0.0373(9) 0.065(10) Uiso 1.00 1 d . . . O(11) O 0.425(4) 1.010(2) -0.0500(10) 0.082(11) Uiso 1.00 1 d . . . O(12) O 0.026(5) 0.896(2) -0.0716(12) 0.10(1) Uiso 1.00 1 d . . . O(13) O 0.706(4) 0.948(2) -0.1146(10) 0.079(11) Uiso 1.00 1 d . . . O(14) O 0.479(4) 0.788(2) -0.1596(11) 0.093(13) Uiso 1.00 1 d . . . O(15) O 0.905(4) 0.771(1) -0.0926(9) 0.067(10) Uiso 1.00 1 d . . . O(16) O 0.244(5) 0.699(2) -0.1072(12) 0.10(1) Uiso 1.00 1 d . . . O(17) O 0.785(4) 0.623(2) 0.0653(10) 0.072(11) Uiso 1.00 1 d . . . O(18) O 0.762(4) 0.966(2) -0.0303(10) 0.079(11) Uiso 1.00 1 d . . . O(19) O 0.672(5) 0.385(2) -0.2184(11) 0.093(13) Uiso 1.00 1 d . . . O(20) O 1.085(4) 0.276(2) -0.2001(11) 0.094(13) Uiso 1.00 1 d . . . O(21) O 0.874(4) 0.376(1) -0.1116(10) 0.071(10) Uiso 1.00 1 d . . . O(22) O 1.570(5) 0.451(2) -0.1509(10) 0.089(12) Uiso 1.00 1 d . . . O(23) O 1.187(4) 0.513(2) -0.0857(10) 0.081(11) Uiso 1.00 1 d . . . O(24) O 1.333(4) 0.622(2) -0.1769(10) 0.087(12) Uiso 1.00 1 d . . . O(25) O 0.701(5) 0.674(2) -0.1375(12) 0.10(1) Uiso 1.00 1 d . . . O(26) O 1.087(6) 0.746(2) -0.2016(13) 0.13(2) Uiso 1.00 1 d . . . O(27) O 0.620(5) 0.725(2) -0.2574(11) 0.096(13) Uiso 1.00 1 d . . . O(28) O 1.292(5) 0.666(2) -0.2599(11) 0.097(13) Uiso 1.00 1 d . . . O(29) O 1.113(5) 0.617(2) -0.3709(11) 0.092(13) Uiso 1.00 1 d . . . O(30) O 1.518(5) 0.524(2) -0.3305(12) 0.11(2) Uiso 1.00 1 d . . . O(31) O 0.818(4) 0.499(2) -0.3782(11) 0.088(12) Uiso 1.00 1 d . . . O(32) O 1.086(5) 0.339(2) -0.3355(12) 0.11(2) Uiso 1.00 1 d . . . O(33) O 0.629(5) 0.416(2) -0.2889(12) 0.12(2) Uiso 1.00 1 d . . . O(34) O 1.324(5) 0.354(2) -0.2549(12) 0.12(2) Uiso 1.00 1 d . . . O(35) O 0.843(4) 0.522(2) -0.1121(10) 0.073(11) Uiso 1.00 1 d . . . O(36) O 0.786(5) 0.624(2) -0.3319(12) 0.10(1) Uiso 1.00 1 d . . . C(1) C 0.808(7) 0.651(2) -0.053(2) 0.08(2) Uiso 1.00 1 d . . . C(2) C 0.550(5) 0.598(2) -0.076(1) 0.053(13) Uiso 1.00 1 d . . . C(3) C 0.671(6) 0.561(2) -0.014(2) 0.07(2) Uiso 1.00 1 d . . . C(4) C 0.170(7) 0.623(2) 0.012(2) 0.07(2) Uiso 1.00 1 d . . . C(5) C 0.421(6) 0.604(2) 0.052(1) 0.07(2) Uiso 1.00 1 d . . . C(6) C 0.303(6) 0.716(2) 0.052(1) 0.06(2) Uiso 1.00 1 d . . . C(7) C 0.874(5) 0.784(2) 0.0930(12) 0.042(12) Uiso 1.00 1 d . . . C(8) C 0.619(5) 0.855(2) 0.0918(13) 0.048(13) Uiso 1.00 1 d . . . C(9) C 0.870(6) 0.898(2) 0.057(1) 0.06(2) Uiso 1.00 1 d . . . C(10) C 0.296(5) 0.882(2) 0.0057(12) 0.037(11) Uiso 1.00 1 d . . . C(11) C 0.395(5) 0.959(2) -0.0440(11) 0.040(12) Uiso 1.00 1 d . . . C(12) C 0.145(9) 0.888(3) -0.062(2) 0.11(2) Uiso 1.00 1 d . . . C(13) C 0.649(5) 0.901(2) -0.1072(13) 0.053(13) Uiso 1.00 1 d . . . C(14) C 0.525(7) 0.808(2) -0.127(2) 0.08(2) Uiso 1.00 1 d . . . C(15) C 0.784(5) 0.792(2) -0.0922(12) 0.047(13) Uiso 1.00 1 d . . . C(16) C 0.316(7) 0.721(3) -0.082(2) 0.08(2) Uiso 1.00 1 d . . . C(17) C 0.736(7) 0.662(3) 0.048(2) 0.08(2) Uiso 1.00 1 d . . . C(18) C 0.720(5) 0.916(2) -0.0250(12) 0.047(13) Uiso 1.00 1 d . . . C(19) C 0.804(7) 0.394(2) -0.209(2) 0.08(2) Uiso 1.00 1 d . . . C(20) C 1.056(5) 0.329(2) -0.1923(12) 0.048(12) Uiso 1.00 1 d . . . C(21) C 0.926(6) 0.386(2) -0.139(2) 0.08(2) Uiso 1.00 1 d . . . C(22) C 1.440(7) 0.465(2) -0.157(1) 0.07(2) Uiso 1.00 1 d . . . C(23) C 1.195(5) 0.504(2) -0.119(1) 0.053(13) Uiso 1.00 1 d . . . C(24) C 1.287(6) 0.573(2) -0.172(1) 0.06(2) Uiso 1.00 1 d . . . C(25) C 0.741(7) 0.666(3) -0.165(2) 0.08(2) Uiso 1.00 1 d . . . C(26) C 0.978(9) 0.706(3) -0.205(2) 0.12(3) Uiso 1.00 1 d . . . C(27) C 0.707(6) 0.695(2) -0.2409(13) 0.05(1) Uiso 1.00 1 d . . . C(28) C 1.263(7) 0.620(3) -0.277(2) 0.08(2) Uiso 1.00 1 d . . . C(29) C 1.146(6) 0.593(3) -0.347(2) 0.07(2) Uiso 1.00 1 d . . . C(30) C 1.402(7) 0.534(3) -0.319(2) 0.08(2) Uiso 1.00 1 d . . . C(31) C 0.892(6) 0.481(2) -0.347(2) 0.08(2) Uiso 1.00 1 d . . . C(32) C 1.024(7) 0.383(3) -0.327(2) 0.09(2) Uiso 1.00 1 d . . . C(33) C 0.768(6) 0.433(2) -0.2925(13) 0.06(1) Uiso 1.00 1 d . . . C(34) C 1.249(7) 0.399(3) -0.249(2) 0.08(2) Uiso 1.00 1 d . . . C(35) C 0.876(6) 0.522(2) -0.141(1) 0.06(1) Uiso 1.00 1 d . . . C(36) C 0.843(6) 0.595(3) -0.305(2) 0.07(2) Uiso 1.00 1 d . . . C(37) C 0.498(3) 0.736(3) 0.1671(12) 0.16(3) Uiso 1.00 1 d . . . H(1) H 0.4551 0.6007 -0.0057 0.0375 Uiso 1.00 1 c . . . H(2) H 0.4603 0.6782 -0.0640 0.0380 Uiso 1.00 1 c . . . H(3) H 0.2886 0.6969 -0.0270 0.0380 Uiso 1.00 1 c . . . H(4) H 0.4269 0.8856 -0.0840 0.0375 Uiso 1.00 1 c . . . H(5) H 0.2805 0.7964 -0.0533 0.0380 Uiso 1.00 1 c . . . H(6) H 0.4469 0.7627 -0.0871 0.0380 Uiso 1.00 1 c . . . H(7) H 0.7238 0.7435 0.0601 0.0375 Uiso 1.00 1 c . . . H(8) H 0.7157 0.8841 0.0207 0.0375 Uiso 1.00 1 c . . . H(9) H 1.1573 0.4234 -0.1528 0.0375 Uiso 1.00 1 c . . . H(10) H 1.1240 0.3961 -0.2234 0.0380 Uiso 1.00 1 c . . . H(11) H 1.2965 0.4591 -0.2109 0.0380 Uiso 1.00 1 c . . . H(12) H 1.1055 0.5018 -0.3320 0.0375 Uiso 1.00 1 c . . . H(13) H 1.2800 0.4858 -0.2726 0.0380 Uiso 1.00 1 c . . . H(14) H 1.1070 0.4191 -0.2763 0.0380 Uiso 1.00 1 c . . . H(15) H 0.8819 0.5976 -0.1710 0.0375 Uiso 1.00 1 c . . . H(16) H 0.8569 0.6371 -0.2606 0.0375 Uiso 1.00 1 c . . . H(17) H 0.5156 0.7154 0.1893 0.1773 Uiso 1.00 1 c . . . H(18) H 0.5534 0.7735 0.1675 0.1773 Uiso 1.00 1 c . . . 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 Os(1) 0.0348(11) 0.0313(11) 0.0384(12) 0.0035(8) -0.0041(9) -0.0041(9) Os(2) 0.0334(11) 0.0372(12) 0.0433(13) 0.0005(9) 0.0021(9) 0.0032(10) Os(3) 0.0339(11) 0.0390(11) 0.0443(13) -0.0015(9) -0.0036(9) -0.0069(10) Os(4) 0.0358(11) 0.0323(11) 0.052(1) 0.0075(9) 0.0022(10) 0.0043(10) Os(5) 0.0449(12) 0.0429(12) 0.0393(13) 0.0009(10) 0.0037(10) 0.0064(10) Os(6) 0.0387(12) 0.0474(13) 0.052(1) 0.0011(10) 0.0055(10) 0.0063(11) Os(7) 0.0362(12) 0.0534(13) 0.047(1) 0.0024(10) -0.0040(10) 0.0032(11) Os(8) 0.053(1) 0.0396(13) 0.068(2) 0.0063(10) 0.0026(12) -0.0037(11) Os(9) 0.0391(12) 0.0498(13) 0.048(1) -0.0087(10) 0.0012(10) 0.0063(11) Os(10) 0.0487(13) 0.0461(13) 0.0427(13) -0.0076(10) 0.0003(10) -0.0039(10) Rh(1) 0.029(2) 0.038(2) 0.039(3) 0.002(2) -0.002(2) -0.002(2) Rh(2) 0.030(2) 0.036(2) 0.040(3) -0.000(2) -0.004(2) -0.003(2) Rh(3) 0.032(2) 0.033(2) 0.045(2) 0.001(2) 0.000(2) -0.003(2) Rh(4) 0.040(2) 0.048(3) 0.047(3) 0.004(2) 0.005(2) 0.001(2) Rh(5) 0.043(2) 0.043(2) 0.051(3) 0.009(2) -0.001(2) -0.000(2) Rh(6) 0.039(2) 0.042(2) 0.048(3) 0.000(2) -0.001(2) 0.002(2) Cl(1) 0.023(6) 0.049(7) 0.064(9) 0.003(5) -0.001(6) -0.001(6) Cl(2) 0.048(8) 0.046(7) 0.061(9) -0.001(6) 0.002(7) 0.011(7) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' #============================================================================== # 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 Os(1) Os(2) 2.882(3) yes . . Os(1) Rh(1) 2.869(4) yes . . Os(1) Rh(2) 2.691(4) yes . . Os(1) C(1) 1.90(6) yes . . Os(1) C(2) 1.82(5) yes . . Os(1) C(3) 1.87(5) yes . . Os(1) H(1) 1.85 no . . Os(1) H(2) 1.90 no . . Os(2) Rh(1) 2.996(4) yes . . Os(2) Rh(2) 2.718(4) yes . . Os(2) C(4) 1.89(5) yes . . Os(2) C(5) 1.84(5) yes . . Os(2) C(6) 1.86(5) yes . . Os(2) H(1) 1.76 no . . Os(2) H(3) 1.94 no . . Os(3) Rh(2) 2.930(4) yes . . Os(3) Rh(3) 2.918(4) yes . . Os(3) Cl(1) 2.47(1) yes . . Os(3) C(7) 1.94(4) yes . . Os(3) C(8) 1.83(5) yes . . Os(3) C(9) 1.87(5) yes . . Os(3) H(7) 1.86) no . . Os(3) H(8) 1.86 no . . Os(4) Os(5) 2.855(3) yes . . Os(4) Rh(1) 2.947(4) yes . . Os(4) Rh(3) 2.709(4) yes . . Os(4) C(10) 1.81(4) yes . . Os(4) C(11) 1.85(4) yes . . Os(4) C(12) 1.94(7) yes . . Os(4) H(4) 1.76 no . . Os(4) H(5) 1.91 no . . Os(5) Rh(1) 2.798(4) yes . . Os(5) Rh(3) 2.703(4) yes . . Os(5) C(13) 1.83(5) yes . . Os(5) C(14) 1.60(6) yes . . Os(5) C(15) 1.91(5) yes . . Os(5) H(4) 1.83 no . . Os(5) H(6) 1.86 no . . Os(6) Os(7) 2.865(3) yes . . Os(6) Rh(4) 2.796(4) yes . . Os(6) Rh(5) 2.688(4) yes . . Os(6) C(19) 1.88(6) yes . . Os(6) C(20) 1.80(5) yes . . Os(6) C(21) 1.83(6) yes . . Os(6) H(9) 1.82 no . . Os(6) H(10) 1.86 no . . Os(7) Rh(4) 2.940(4) yes . . Os(7) Rh(5) 2.688(4) yes . . Os(7) C(22) 1.91(5) yes . . Os(7) C(23) 1.82(5) yes . . Os(7) C(24) 1.80(5) yes . . Os(7) H(9) 1.76 no . . Os(7) H(11) 1.92 no . . Os(8) Rh(5) 2.923(4) yes . . Os(8) Rh(6) 2.935(4) yes . . Os(8) Cl(2) 2.48(1) yes . . Os(8) C(25) 1.96(6) yes . . Os(8) C(26) 1.72(7) yes . . Os(8) C(27) 1.91(5) yes . . Os(8) H(15) 1.87 no . . Os(8) H(16) 1.89 no . . Os(9) Os(10) 2.888(3) yes . . Os(9) Rh(4) 3.004(4) yes . . Os(9) Rh(6) 2.710(4) yes . . Os(9) C(28) 1.83(6) yes . . Os(9) C(29) 1.95(6) yes . . Os(9) C(30) 1.92(6) yes . . Os(9) H(12) 1.77 no . . Os(9) H(13) 1.94 no . . Os(10) Rh(4) 2.873(4) yes . . Os(10) Rh(6) 2.696(4) yes . . Os(10) C(31) 1.68(6) yes . . Os(10) C(32) 1.93(6) yes . . Os(10) C(33) 1.81(5) yes . . Os(10) H(12) 1.84 no . . Os(10) H(14) 1.90) no . . Rh(1) Rh(2) 2.993(5) yes . . Rh(1) Rh(3) 2.967(5) yes . . Rh(1) C(16) 1.81(6) yes . . Rh(1) H(2) 1.69 no . . Rh(1) H(3) 1.75 no . . Rh(1) H(5) 1.74 no . . Rh(1) H(6) 1.67) no . . Rh(2) Cl(1) 2.57(1) yes . . Rh(2) C(17) 1.81(6) yes . . Rh(2) H(7) 1.77 no . . Rh(3) Cl(1) 2.57(1) yes . . Rh(3) C(18) 1.74(5) yes . . Rh(3) H(8) 1.77 no . . Rh(4) Rh(5) 2.956(5) yes . . Rh(4) Rh(6) 2.994(5) yes . . Rh(4) C(34) 1.76(6) yes . . Rh(4) H(10) 1.67 no . . Rh(4) H(11) 1.73 no . . Rh(4) H(13) 1.75 no . . Rh(4) H(14) 1.69 no . . Rh(5) Cl(2) 2.59(1) yes . . Rh(5) C(35) 1.85(5) yes . . Rh(5) H(15) 1.76 no . . Rh(6) Cl(2) 2.58(1) yes . . Rh(6) C(36) 1.68(6) yes . . Rh(6) H(16) 1.76 no . . Cl(3) C(37) 1.80(6) yes . . Cl(4) C(37) 1.80(3) yes . . O(1) C(1) 1.16(7) yes . . O(2) C(2) 1.19(6) yes . . O(3) C(3) 1.16(6) yes . . O(4) C(4) 1.13(7) yes . . O(5) C(5) 1.20(6) yes . . O(6) C(6) 1.19(6) yes . . O(7) C(7) 1.15(6) yes . . O(8) C(8) 1.11(6) yes . . O(9) C(9) 1.18(6) yes . . O(10) C(10) 1.21(6) yes . . O(11) C(11) 1.18(6) yes . . O(12) C(12) 1.09(9) yes . . O(13) C(13) 1.17(6) yes . . O(14) C(14) 1.33(7) yes . . O(15) C(15) 1.13(6) yes . . O(16) C(16) 1.20(7) yes . . O(17) C(17) 1.15(7) yes . . O(18) C(18) 1.18(6) yes . . O(19) C(19) 1.19(7) yes . . O(20) C(20) 1.22(6) yes . . O(21) C(21) 1.16(7) yes . . O(22) C(22) 1.16(7) yes . . O(23) C(23) 1.25(6) yes . . O(24) C(24) 1.17(6) yes . . O(25) C(25) 1.11(8) yes . . O(26) C(26) 1.29(8) yes . . O(27) C(27) 1.16(6) yes . . O(28) C(28) 1.20(7) yes . . O(29) C(29) 1.08(7) yes . . O(30) C(30) 1.10(8) yes . . O(31) C(31) 1.37(7) yes . . O(32) C(32) 1.16(8) yes . . O(33) C(33) 1.26(7) yes . . O(34) C(34) 1.20(7) yes . . O(35) C(35) 1.11(6) yes . . O(36) C(36) 1.28(7) yes . . C(37) H(17) 0.95 no . . C(37) H(18) 0.95 no . . 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 Os(2) Os(1) Rh(1) 62.80(9) yes . . . Os(2) Os(1) Rh(2) 58.27(9) yes . . . Os(2) Os(1) C(1) 148(1) yes . . . Os(2) Os(1) C(2) 119(1) yes . . . Os(2) Os(1) C(3) 96(1) yes . . . Os(2) Os(1) H(1) 36 no . . . Os(2) Os(1) H(2) 80 no . . . Rh(1) Os(1) Rh(2) 65.0(1) yes . . . Rh(1) Os(1) C(1) 105(1) yes . . . Rh(1) Os(1) C(2) 98(1) yes . . . Rh(1) Os(1) C(3) 159(1) yes . . . Rh(1) Os(1) H(1) 93 no . . . Rh(1) Os(1) H(2) 34 no . . . Rh(2) Os(1) C(1) 90(1) yes . . . Rh(2) Os(1) C(2) 162(1) yes . . . Rh(2) Os(1) C(3) 105(1) yes . . . Rh(2) Os(1) H(1) 87 no . . . Rh(2) Os(1) H(2) 99 no . . . C(1) Os(1) C(2) 89(2) yes . . . C(1) Os(1) C(3) 92(2) yes . . . C(1) Os(1) H(1) 159 no . . . C(1) Os(1) H(2) 106 no . . . C(2) Os(1) C(3) 92(2) yes . . . C(2) Os(1) H(1) 98 no . . . C(2) Os(1) H(2) 64 no . . . C(3) Os(1) H(1) 67 no . . . C(3) Os(1) H(2) 149 no . . . H(1) Os(1) H(2) 95 no . . . Rh(1) Os(2) Rh(2) 62.9(1) yes . . . Rh(1) Os(2) C(4) 111(1) yes . . . Rh(1) Os(2) C(5) 154(1) yes . . . Rh(1) Os(2) C(6) 101(1) yes . . . Rh(1) Os(2) H(1) 91 no . . . Rh(1) Os(2) H(3) 34 no . . . Rh(1) Os(2) Os(1) 58.39(8) yes . . . Rh(2) Os(2) C(4) 174(1) yes . . . Rh(2) Os(2) C(5) 95(1) yes . . . Rh(2) Os(2) C(6) 88(1) yes . . . Rh(2) Os(2) H(1) 88 no . . . Rh(2) Os(2) H(3) 97 no . . . Rh(2) Os(2) Os(1) 57.35(9) yes . . . C(4) Os(2) C(5) 88(2) yes . . . C(4) Os(2) C(6) 94(2) yes . . . C(4) Os(2) H(1) 90 no . . . C(4) Os(2) H(3) 78 no . . . C(4) Os(2) Os(1) 118(1) yes . . . C(5) Os(2) C(6) 91(2) yes . . . C(5) Os(2) H(1) 74 no . . . C(5) Os(2) H(3) 161 no . . . C(5) Os(2) Os(1) 99(1) yes . . . C(6) Os(2) H(1) 165 no . . . C(6) Os(2) H(3) 103 no . . . C(6) Os(2) Os(1) 145(1) yes . . . H(1) Os(2) H(3) 92 no . . . H(1) Os(2) Os(1) 38 no . . . H(3) Os(2) Os(1) 75 no . . . Rh(2) Os(3) Rh(3) 63.0(1) yes . . . Rh(2) Os(3) Cl(1) 56.0(3) yes . . . Rh(2) Os(3) C(7) 95(1) yes . . . Rh(2) Os(3) C(8) 117(1) yes . . . Rh(2) Os(3) C(9) 146(1) yes . . . Rh(2) Os(3) H(7) 35 no . . . Rh(2) Os(3) H(8) 99 no . . . Rh(3) Os(3) Cl(1) 56.3(3) yes . . . Rh(3) Os(3) C(7) 150(1) yes . . . Rh(3) Os(3) C(8) 116(1) yes . . . Rh(3) Os(3) C(9) 93.3(12) yes . . . Rh(3) Os(3) H(7) 98 no . . . Rh(3) Os(3) H(8) 36 no . . . Cl(1) Os(3) C(7) 95(1) yes . . . Cl(1) Os(3) C(8) 171(1) yes . . . Cl(1) Os(3) C(9) 91(1) yes . . . Cl(1) Os(3) H(7) 75 no . . . Cl(1) Os(3) H(8) 76 no . . . C(7) Os(3) C(8) 90(1) yes . . . C(7) Os(3) C(9) 97(2) yes . . . C(7) Os(3) H(7) 62 no . . . C(7) Os(3) H(8) 155 no . . . C(8) Os(3) C(9) 93(2) yes . . . C(8) Os(3) H(7) 102 no . . . C(8) Os(3) H(8) 102 no . . . C(9) Os(3) H(7) 153 no . . . C(9) Os(3) H(8) 61 no . . . H(7) Os(3) H(8) 134 no . . . Os(5) Os(4) Rh(1) 57.64(9) yes . . . Os(5) Os(4) Rh(3) 58.05(9) yes . . . Os(5) Os(4) C(10) 144(1) yes . . . Os(5) Os(4) C(11) 100(1) yes . . . Os(5) Os(4) C(12) 115(2) yes . . . Os(5) Os(4) H(4) 38 no . . . Os(5) Os(4) H(5) 75 no . . . Rh(1) Os(4) Rh(3) 63.1(1) yes . . . Rh(1) Os(4) C(10) 99(1) yes . . . Rh(1) Os(4) C(11) 154(1) yes . . . Rh(1) Os(4) C(12) 109(1) yes . . . Rh(1) Os(4) H(4) 90 no . . . Rh(1) Os(4) H(5) 34 no . . . Rh(3) Os(4) C(10) 88(1) yes . . . Rh(3) Os(4) C(11) 95(1) yes . . . Rh(3) Os(4) C(12) 171(1) yes . . . Rh(3) Os(4) H(4) 89 no . . . Rh(3) Os(4) H(5) 97 no . . . C(10) Os(4) C(11) 92(1) yes . . . C(10) Os(4) C(12) 97(2) yes . . . C(10) Os(4) H(4) 168 no . . . C(10) Os(4) H(5) 102 no . . . C(11) Os(4) C(12) 90(2) yes . . . C(11) Os(4) H(4) 76 no . . . C(11) Os(4) H(5) 160 no . . . C(12) Os(4) H(4) 87 no . . . C(12) Os(4) H(5) 75 no . . . H(4) Os(4) H(5) 90 no . . . Rh(1) Os(5) Rh(3) 65.2(1) yes . . . Rh(1) Os(5) C(13) 161(1) yes . . . Rh(1) Os(5) C(14) 103(2) yes . . . Rh(1) Os(5) C(15) 100(1) yes . . . Rh(1) Os(5) H(4) 93 no . . . Rh(1) Os(5) H(6) 35 no . . . Rh(1) Os(5) Os(4) 62.83(9) yes . . . Rh(3) Os(5) C(13) 102(1) yes . . . Rh(3) Os(5) C(14) 168(1) yes . . . Rh(3) Os(5) C(15) 88(1) yes . . . Rh(3) Os(5) H(4) 88 no . . . Rh(3) Os(5) H(6) 100 no . . . Rh(3) Os(5) Os(4) 58.27(9) yes . . . C(13) Os(5) C(14) 88(2) yes . . . C(13) Os(5) C(15) 92(2) yes . . . C(13) Os(5) H(4) 71 no . . . C(13) Os(5) H(6) 152 no . . . C(13) Os(5) Os(4) 98(1) yes . . . C(14) Os(5) C(15) 94(2) yes . . . C(14) Os(5) H(4) 94 no . . . C(14) Os(5) H(6) 67 no . . . C(14) Os(5) Os(4) 118(2) yes . . . C(15) Os(5) H(4) 162 no . . . C(15) Os(5) H(6) 103 no . . . C(15) Os(5) Os(4) 146(1) yes . . . H(4) Os(5) H(6) 95 no . . . H(4) Os(5) Os(4) 36 no . . . H(6) Os(5) Os(4) 81 no . . . Os(7) Os(6) Rh(4) 62.6(1) yes . . . Os(7) Os(6) Rh(5) 57.8(1) yes . . . Os(7) Os(6) C(19) 143(1) yes . . . Os(7) Os(6) C(20) 118(1) yes . . . Os(7) Os(6) C(21) 100(1) yes . . . Os(7) Os(6) H(9) 36 no . . . Os(7) Os(6) H(10) 81 no . . . Rh(4) Os(6) Rh(5) 65.2(1) yes . . . Rh(4) Os(6) C(19) 94(1) yes . . . Rh(4) Os(6) C(20) 100(1) yes . . . Rh(4) Os(6) C(21) 162(1) yes . . . Rh(4) Os(6) H(9) 93 no . . . Rh(4) Os(6) H(10) 35 no . . . Rh(5) Os(6) C(19) 87(1) yes . . . Rh(5) Os(6) C(20) 165(1) yes . . . Rh(5) Os(6) C(21) 102(1) yes . . . Rh(5) Os(6) H(9) 87 no . . . Rh(5) Os(6) H(10) 101 no . . . C(19) Os(6) C(20) 91(2) yes . . . C(19) Os(6) C(21) 96(2) yes . . . C(19) Os(6) H(9) 168 no . . . C(19) Os(6) H(10) 96 no . . . C(20) Os(6) C(21) 91(2) yes . . . C(20) Os(6) H(9) 95 no . . . C(20) Os(6) H(10) 65 no . . . C(21) Os(6) H(9) 74 no . . . C(21) Os(6) H(10) 154 no . . . H(9) Os(6) H(10) 95 no . . . Rh(4) Os(7) Rh(5) 63.2(1) yes . . . Rh(4) Os(7) C(22) 109(1) yes . . . Rh(4) Os(7) C(23) 153(1) yes . . . Rh(4) Os(7) C(24) 99(1) yes . . . Rh(4) Os(7) H(9) 89 no . . . Rh(4) Os(7) H(11) 34. no . . . Rh(4) Os(7) Os(6) 57.57(9) yes . . . Rh(5) Os(7) C(22) 172(1) yes . . . Rh(5) Os(7) C(23) 94(1) yes . . . Rh(5) Os(7) C(24) 87(1) yes . . . Rh(5) Os(7) H(9) 89 no . . . Rh(5) Os(7) H(11) 97 no . . . Rh(5) Os(7) Os(6) 57.81(9) yes . . . C(22) Os(7) C(23) 92(2) yes . . . C(22) Os(7) C(24) 96(2) yes . . . C(22) Os(7) H(9) 90 no . . . C(22) Os(7) H(11) 75 no . . . C(22) Os(7) Os(6) 117(1) yes . . . C(23) Os(7) C(24) 92(2) yes . . . C(23) Os(7) H(9) 76 no . . . C(23) Os(7) H(11) 162 no . . . C(23) Os(7) Os(6) 99(1) yes . . . C(24) Os(7) H(9) 167 no . . . C(24) Os(7) H(11) 102 no . . . C(24) Os(7) Os(6) 143(1) yes . . . H(9) Os(7) H(11) 90 no . . . H(9) Os(7) Os(6) 38 no . . . H(11) Os(7) Os(6) 75 no . . . Rh(5) Os(8) Rh(6) 63.8(1) yes . . . Rh(5) Os(8) Cl(2) 56.6(3) yes . . . Rh(5) Os(8) C(25) 93(1) yes . . . Rh(5) Os(8) C(26) 117(2) yes . . . Rh(5) Os(8) C(27) 146(1) yes . . . Rh(5) Os(8) H(15) 35 no . . . Rh(5) Os(8) H(16) 99 no . . . Rh(6) Os(8) Cl(2) 56.2(3) yes . . . Rh(6) Os(8) C(25) 150(1) yes . . . Rh(6) Os(8) C(26) 114(2) yes . . . Rh(6) Os(8) C(27) 93(1) yes . . . Rh(6) Os(8) H(15) 99 no . . . Rh(6) Os(8) H(16) 35 no . . . Cl(2) Os(8) C(25) 95(1) yes . . . Cl(2) Os(8) C(26) 169(2) yes . . . Cl(2) Os(8) C(27) 90(1) yes . . . Cl(2) Os(8) H(15) 75 no . . . Cl(2) Os(8) H(16) 75 no . . . C(25) Os(8) C(26) 93(2) yes . . . C(25) Os(8) C(27) 96(2) yes . . . C(25) Os(8) H(15) 61 no . . . C(25) Os(8) H(16) 156 no . . . C(26) Os(8) C(27) 93(2) yes . . . C(26) Os(8) H(15) 104 no . . . C(26) Os(8) H(16) 99 no . . . C(27) Os(8) H(15) 152 no . . . C(27) Os(8) H(16) 62 no . . . H(15) Os(8) H(16) 134 no . . . Os(10) Os(9) Rh(4) 58.33(9) yes . . . Os(10) Os(9) Rh(6) 57.48(9) yes . . . Os(10) Os(9) C(28) 144(1) yes . . . Os(10) Os(9) C(29) 96(1) yes . . . Os(10) Os(9) C(30) 118(1) yes . . . Os(10) Os(9) H(12) 38 no . . . Os(10) Os(9) H(13) 75 no . . . Rh(4) Os(9) Rh(6) 63.0(1) yes . . . Rh(4) Os(9) C(28) 100(1) yes . . . Rh(4) Os(9) C(29) 154(1) yes . . . Rh(4) Os(9) C(30) 106(1) yes . . . Rh(4) Os(9) H(12) 90 no . . . Rh(4) Os(9) H(13) 34 no . . . Rh(6) Os(9) C(28) 89(2) yes . . . Rh(6) Os(9) C(29) 100(1) yes . . . Rh(6) Os(9) C(30) 169(1) yes . . . Rh(6) Os(9) H(12) 88 no . . . Rh(6) Os(9) H(13) 96 no . . . C(28) Os(9) C(29) 97(2) yes . . . C(28) Os(9) C(30) 93(2) yes . . . C(28) Os(9) H(12) 165 no . . . C(28) Os(9) H(13) 104 no . . . C(29) Os(9) C(30) 89(2) yes . . . C(29) Os(9) H(12) 69 no . . . C(29) Os(9) H(13) 153 no . . . C(30) Os(9) H(12) 92 no . . . C(30) Os(9) H(13) 73 no . . . H(12) Os(9) H(13) 92 no . . . Rh(4) Os(10) Rh(6) 65.0(1) yes . . . Rh(4) Os(10) C(31) 157(1) yes . . . Rh(4) Os(10) C(32) 102(1) yes . . . Rh(4) Os(10) C(33) 103(1) yes . . . Rh(4) Os(10) H(12) 93 no . . . Rh(4) Os(10) H(14) 34 no . . . Rh(4) Os(10) Os(9) 62.86(9) yes . . . Rh(6) Os(10) C(31) 102(1) yes . . . Rh(6) Os(10) C(32) 167(1) yes . . . Rh(6) Os(10) C(33) 89(1) yes . . . Rh(6) Os(10) H(12) 87 no . . . Rh(6) Os(10) H(14) 99 no . . . Rh(6) Os(10) Os(9) 57.95(9) yes . . . C(31) Os(10) C(32) 88(2) yes . . . C(31) Os(10) C(33) 93(2) yes . . . C(31) Os(10) H(12) 67 no . . . C(31) Os(10) H(14) 152 no . . . C(31) Os(10) Os(9) 95(1) yes . . . C(32) Os(10) C(33) 95(2) yes . . . C(32) Os(10) H(12) 92 no . . . C(32) Os(10) H(14) 69 no . . . C(32) Os(10) Os(9) 115(1) yes . . . C(33) Os(10) H(12) 159 no . . . C(33) Os(10) H(14) 106 no . . . C(33) Os(10) Os(9) 147(1) yes . . . H(12) Os(10) H(14) 95 no . . . H(12) Os(10) Os(9) 36 no . . . H(14) Os(10) Os(9) 80 no . . . Rh(2) Rh(1) Rh(3) 61.7(1) yes . . . Rh(2) Rh(1) C(16) 150(1) yes . . . Rh(2) Rh(1) H(2) 94 no . . . Rh(2) Rh(1) H(3) 92 no . . . Rh(2) Rh(1) H(5) 138 no . . . Rh(2) Rh(1) H(6) 137 no . . . Rh(2) Rh(1) Os(1) 54.6(1) yes . . . Rh(2) Rh(1) Os(4) 108.0(1) yes . . . Rh(2) Rh(1) Os(5) 107.6(1) yes . . . Rh(3) Rh(1) C(16) 143(1) yes . . . Rh(3) Rh(1) H(2) 134 no . . . Rh(3) Rh(1) H(3) 139 no . . . Rh(3) Rh(1) H(5) 93 no . . . Rh(3) Rh(1) H(6) 96 no . . . Rh(3) Rh(1) Os(1) 105.4(1) yes . . . Rh(3) Rh(1) Os(2) 108.5(1) yes . . . Rh(3) Rh(1) Os(4) 54.53(9) yes . . . C(16) Rh(1) H(2) 57 no . . . C(16) Rh(1) H(3) 74 no . . . C(16) Rh(1) H(5) 69 no . . . C(16) Rh(1) H(6) 49 no . . . C(16) Rh(1) Os(1) 96(1) yes . . . C(16) Rh(1) Os(2) 108(1) yes . . . C(16) Rh(1) Os(4) 101(1) yes . . . C(16) Rh(1) Os(5) 88(1) yes . . . H(2) Rh(1) H(3) 74 no . . . H(2) Rh(1) H(5) 126 no . . . H(2) Rh(1) H(6) 75 no . . . H(2) Rh(1) Os(1) 40 no . . . H(2) Rh(1) Os(4) 155 no . . . H(2) Rh(1) Os(5) 104 no . . . H(3) Rh(1) H(5) 87 no . . . H(3) Rh(1) H(6) 123 no . . . H(3) Rh(1) Os(1) 78 no . . . H(3) Rh(1) Os(4) 115 no . . . H(3) Rh(1) Os(5) 161 no . . . H(5) Rh(1) H(6) 74 no . . . H(5) Rh(1) Os(1) 162 no . . . H(5) Rh(1) Os(2) 114 no . . . H(5) Rh(1) Os(4) 38 no . . . H(6) Rh(1) Os(1) 105 no . . . H(6) Rh(1) Os(2) 153 no . . . H(6) Rh(1) Os(4) 81 no . . . Os(1) Rh(1) Os(4) 159.9(1) yes . . . Os(1) Rh(1) Os(5) 112.7(1) yes . . . Os(2) Rh(1) Rh(2) 54.0(1) yes . . . Os(2) Rh(1) H(2) 80 no . . . Os(2) Rh(1) H(3) 38 no . . . Os(2) Rh(1) Os(1) 58.81(8) yes . . . Os(2) Rh(1) Os(4) 122.0(1) yes . . . Os(2) Rh(1) Os(5) 161.5(1) yes . . . Os(5) Rh(1) Rh(3) 55.8(1) yes . . . Os(5) Rh(1) H(5) 79 no . . . Os(5) Rh(1) H(6) 40 no . . . Os(5) Rh(1) Os(4) 59.53(8) yes . . . Cl(1) Rh(2) C(17) 101(1) yes . . . Cl(1) Rh(2) H(7) 74 no . . . Cl(1) Rh(2) Os(1) 111.3(3) yes . . . Cl(1) Rh(2) Os(2) 165.9(3) yes . . . Cl(1) Rh(2) Os(3) 52.9(3) yes . . . Cl(1) Rh(2) Rh(1) 103.0(3) yes . . . C(17) Rh(2) H(7) 62 no . . . C(17) Rh(2) Os(1) 91(1) yes . . . C(17) Rh(2) Os(2) 91(1) yes . . . C(17) Rh(2) Os(3) 98(1) yes . . . C(17) Rh(2) Rh(1) 148(1) yes . . . H(7) Rh(2) Os(1) 154 no . . . H(7) Rh(2) Os(2) 116 no . . . H(7) Rh(2) Os(3) 37 no . . . H(7) Rh(2) Rh(1) 145 no . . . Os(1) Rh(2) Os(3) 162.5(2) yes . . . Os(2) Rh(2) Os(1) 64.38(9) yes . . . Os(2) Rh(2) Os(3) 128.8(1) yes . . . Os(2) Rh(2) Rh(1) 63.1(1) yes . . . Os(3) Rh(2) Rh(1) 112.5(1) yes . . . Rh(1) Rh(2) Os(1) 60.3(1) yes . . . Cl(1) Rh(3) C(18) 101(1) yes . . . Cl(1) Rh(3) H(8) 74 no . . . Cl(1) Rh(3) Os(3) 53.0(3) yes . . . Cl(1) Rh(3) Os(4) 165.4(3) yes . . . Cl(1) Rh(3) Os(5) 113.6(3) yes . . . Cl(1) Rh(3) Rh(1) 103.6(3) yes . . . C(18) Rh(3) H(8) 63 no . . . C(18) Rh(3) Os(3) 99(1) yes . . . C(18) Rh(3) Os(4) 92(1) yes . . . C(18) Rh(3) Os(5) 90(1) yes . . . C(18) Rh(3) Rh(1) 146(1) yes . . . H(8) Rh(3) Os(3) 37 no . . . H(8) Rh(3) Os(4) 115 no . . . H(8) Rh(3) Os(5) 154 no . . . H(8) Rh(3) Rh(1) 146 no . . . Os(3) Rh(3) Os(4) 126.9(1) yes . . . Os(3) Rh(3) Os(5) 164.7(1) yes . . . Os(3) Rh(3) Rh(1) 113.6(1) yes . . . Os(5) Rh(3) Os(4) 63.7(1) yes . . . Os(5) Rh(3) Rh(1) 58.9(1) yes . . . Rh(1) Rh(3) Os(4) 62.4(1) yes . . . Rh(5) Rh(4) Rh(6) 62.7(1) yes . . . Rh(5) Rh(4) C(34) 143(1) yes . . . Rh(5) Rh(4) H(10) 96 no . . . Rh(5) Rh(4) H(11) 93 no . . . Rh(5) Rh(4) H(13) 138 no . . . Rh(5) Rh(4) H(14) 135 no . . . Rh(5) Rh(4) Os(6) 55.6(1) yes . . . Rh(5) Rh(4) Os(9) 108.8(1) yes . . . Rh(5) Rh(4) Os(10) 106.8(1) yes . . . Rh(6) Rh(4) C(34) 149(1) yes . . . Rh(6) Rh(4) H(10) 136 no . . . Rh(6) Rh(4) H(11) 139 no . . . Rh(6) Rh(4) H(13) 92 no . . . Rh(6) Rh(4) H(14) 94 no . . . Rh(6) Rh(4) Os(6) 107.6(1) yes . . . Rh(6) Rh(4) Os(7) 108.9(1) yes . . . Rh(6) Rh(4) Os(9) 53.7(1) yes . . . C(34) Rh(4) H(10) 50 no . . . C(34) Rh(4) H(11) 69 no . . . C(34) Rh(4) H(13) 74 no . . . C(34) Rh(4) H(14) 56 no . . . C(34) Rh(4) Os(6) 88(1) yes . . . C(34) Rh(4) Os(7) 101(1) yes . . . C(34) Rh(4) Os(9) 107(1) yes . . . C(34) Rh(4) Os(10) 95(1) yes . . . H(10) Rh(4) H(11) 75 no . . . H(10) Rh(4) H(13) 124 no . . . H(10) Rh(4) H(14) 75 no . . . H(10) Rh(4) Os(6) 40 no . . . H(10) Rh(4) Os(9) 153 no . . . H(10) Rh(4) Os(10) 104 no . . . H(11) Rh(4) H(13) 86 no . . . H(11) Rh(4) H(14) 125 no . . . H(11) Rh(4) Os(6) 79 no . . . H(11) Rh(4) Os(9) 114 no . . . H(11) Rh(4) Os(10) 160 no . . . H(13) Rh(4) H(14) 74 no . . . H(13) Rh(4) Os(6) 161 no . . . H(13) Rh(4) Os(7) 114 no . . . H(13) Rh(4) Os(9) 37 no . . . H(14) Rh(4) Os(6) 104 no . . . H(14) Rh(4) Os(7) 155 no . . . H(14) Rh(4) Os(9) 80 no . . . Os(6) Rh(4) Os(9) 161.3(2) yes . . . Os(6) Rh(4) Os(10) 112.7(1) yes . . . Os(7) Rh(4) Rh(5) 54.2(1) yes . . . Os(7) Rh(4) H(10) 81 no . . . Os(7) Rh(4) H(11) 38 no . . . Os(7) Rh(4) Os(6) 59.87(9) yes . . . Os(7) Rh(4) Os(9) 122.1(1) yes . . . Os(7) Rh(4) Os(10) 161.0(2) yes . . . Os(10) Rh(4) Rh(6) 54.7(1) yes . . . Os(10) Rh(4) H(13) 78 no . . . Os(10) Rh(4) H(14) 39 no . . . Os(10) Rh(4) Os(9) 58.81(9) yes . . . Cl(2) Rh(5) C(35) 104(1) yes . . . Cl(2) Rh(5) H(15) 74 no . . . Cl(2) Rh(5) Os(6) 113.8(3) yes . . . Cl(2) Rh(5) Os(7) 165.6(3) yes . . . Cl(2) Rh(5) Os(8) 53.0(3) yes . . . Cl(2) Rh(5) Rh(4) 103.8(3) yes . . . C(35) Rh(5) H(15) 68 no . . . C(35) Rh(5) Os(6) 87(1) yes . . . C(35) Rh(5) Os(7) 90(1) yes . . . C(35) Rh(5) Os(8) 103(1) yes . . . C(35) Rh(5) Rh(4) 143(1) yes . . . H(15) Rh(5) Os(6) 155 no . . . H(15) Rh(5) Os(7) 114 no . . . H(15) Rh(5) Os(8) 38 no . . . H(15) Rh(5) Rh(4) 144 no . . . Os(6) Rh(5) Os(8) 164.1(2) yes . . . Os(7) Rh(5) Os(6) 64.4(1) yes . . . Os(7) Rh(5) Os(8) 125.7(1) yes . . . Os(7) Rh(5) Rh(4) 62.6(1) yes . . . Os(8) Rh(5) Rh(4) 112.2(2) yes . . . Rh(4) Rh(5) Os(6) 59.2(1) yes . . . Cl(2) Rh(6) C(36) 105(1) yes . . . Cl(2) Rh(6) H(16) 74 no . . . Cl(2) Rh(6) Os(8) 52.8(3) yes . . . Cl(2) Rh(6) Os(9) 165.7(3) yes . . . Cl(2) Rh(6) Os(10) 113.4(3) yes . . . Cl(2) Rh(6) Rh(4) 102.9(3) yes . . . C(36) Rh(6) H(16) 67 no . . . C(36) Rh(6) Os(8) 103(1) yes . . . C(36) Rh(6) Os(9) 89(1) yes . . . C(36) Rh(6) Os(10) 88(1) yes . . . C(36) Rh(6) Rh(4) 144(1) yes . . . H(16) Rh(6) Os(8) 38 no . . . H(16) Rh(6) Os(9) 114 no . . . H(16) Rh(6) Os(10) 155 no . . . H(16) Rh(6) Rh(4) 143 no . . . Os(8) Rh(6) Os(9) 126.0(1) yes . . . Os(8) Rh(6) Os(10) 163.5(2) yes . . . Os(8) Rh(6) Rh(4) 110.8(1) yes . . . Os(10) Rh(6) Os(9) 64.6(1) yes . . . Os(10) Rh(6) Rh(4) 60.4(1) yes . . . Rh(4) Rh(6) Os(9) 63.3(1) yes . . . Rh(2) Cl(1) Os(3) 71.1(3) yes . . . Rh(2) Cl(1) Rh(3) 73.0(3) yes . . . Rh(3) Cl(1) Os(3) 70.7(3) yes . . . Rh(5) Cl(2) Os(8) 70.5(3) yes . . . Rh(5) Cl(2) Rh(6) 73.6(3) yes . . . Rh(6) Cl(2) Os(8) 70.9(3) yes . . . Os(1) C(1) O(1) 173(4) yes . . . Os(1) C(2) O(2) 178(4) yes . . . Os(1) C(3) O(3) 173(4) yes . . . Os(2) C(4) O(4) 176(4) yes . . . Os(2) C(5) O(5) 171(4) yes . . . Os(2) C(6) O(6) 174(4) yes . . . Os(3) C(7) O(7) 178(4) yes . . . Os(3) C(8) O(8) 170(4) yes . . . Os(3) C(9) O(9) 178(4) yes . . . Os(4) C(10) O(10) 175(3) yes . . . Os(4) C(11) O(11) 172(3) yes . . . Os(4) C(12) O(12) 175(5) yes . . . Os(5) C(13) O(13) 169(3) yes . . . Os(5) C(14) O(14) 176(4) yes . . . Os(5) C(15) O(15) 175(3) yes . . . Rh(1) C(16) O(16) 174(4) yes . . . Rh(2) C(17) O(17) 174(5) yes . . . Rh(3) C(18) O(18) 175(4) yes . . . Os(6) C(19) O(19) 167(5) yes . . . Os(6) C(20) O(20) 173(4) yes . . . Os(6) C(21) O(21) 175(4) yes . . . Os(7) C(22) O(22) 175(4) yes . . . Os(7) C(23) O(23) 172(3) yes . . . Os(7) C(24) O(24) 173(4) yes . . . Os(8) C(25) O(25) 170(5) yes . . . Os(8) C(26) O(26) 175(6) yes . . . Os(8) C(27) O(27) 175(4) yes . . . Os(9) C(28) O(28) 173(4) yes . . . Os(9) C(29) O(29) 175(4) yes . . . Os(9) C(30) O(30) 177(6) yes . . . Os(10) C(31) O(31) 172(4) yes . . . Os(10) C(32) O(32) 168(4) yes . . . Os(10) C(33) O(33) 169(4) yes . . . Rh(4) C(34) O(34) 178(5) yes . . . Rh(5) C(35) O(35) 175(2) yes . . . Rh(6) C(36) O(36) 176(4) yes . . . H(17) C(37) H(18) 109 no . . . H(17) C(37) Cl(3) 108 no . . . H(17) C(37) Cl(4) 107 no . . . H(18) C(37) Cl(3) 108 no . . . H(18) C(37) Cl(4) 107 no . . . Cl(3) C(37) Cl(4) 117(2) yes . . . Os(2) H(1) Os(1) 106 no . . . Rh(1) H(2) Os(1) 106 no . . . Os(2) H(3) Rh(1) 109 no . . . Os(5) H(4) Os(4) 106 no . . . Rh(1) H(5) Os(4) 108 no . . . Os(5) H(6) Rh(1) 105 no . . . Rh(2) H(7) Os(3) 107 no . . . Rh(3) H(8) Os(3) 107 no . . . Os(7) H(9) Os(6) 106 no . . . Rh(4) H(10) Os(6) 105 no . . . Os(7) H(11) Rh(4) 107 no . . . Os(10) H(12) Os(9) 106 no . . . Rh(4) H(13) Os(9) 109 no . . . Os(10) H(14) Rh(4) 106 no . . . Rh(5) H(15) Os(8) 107 no . . . Rh(6) H(16) Os(8) 107 no . . . #============================================================================== data_wt0927w _database_code_depnum_ccdc_archive 'CCDC 262821' #-JAS012---compound 7 _audit_creation_date 2005-02-02 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_absolute_configuration ad _chemical_formula_sum 'C18 H5 O18 Os5 Rh ' _chemical_formula_moiety 'C18 H5 O18 Os5 Rh ' _chemical_formula_weight 1563.13 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z #------------------------------------------------------------------------------ _cell_length_a 8.784(4) _cell_length_b 19.500(9) _cell_length_c 9.201(4) _cell_angle_alpha 90 _cell_angle_beta 115.34(1) _cell_angle_gamma 90 _cell_volume 1424.4(11) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8577 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.7 _cell_measurement_temperature 298(1) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 3.644 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1364.00 _exptl_absorpt_coefficient_mu 22.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.236 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8577 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_theta_max 27.74 _diffrn_measured_fraction_theta_max 0.9466 _diffrn_reflns_theta_full 27.74 _diffrn_measured_fraction_theta_full 0.9466 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5996 _reflns_number_gt 5491 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0430 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5507 _refine_ls_number_parameters 379 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0002Fo^2^ + 1.0000\s(Fo^2^) + 0.05]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 4.55 _refine_diff_density_min -3.15 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, 5996 Friedel-pairs' _refine_ls_abs_structure_Flack -0.003(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os Os -1.216 7.603 ; 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) ; C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 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) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 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 Os(1) Os 0.67332(8) 0.07181(7) 0.49919(7) 0.0302(2) Uani 1.00 1 d . . . Os(2) Os 0.56724(9) 0.10891(7) 0.74345(8) 0.0305(2) Uani 1.00 1 d . . . Os(3) Os 0.90225(8) 0.07072(7) 0.83805(7) 0.0313(2) Uani 1.00 1 d . . . Os(4) Os 0.60101(10) -0.13836(7) 0.90238(8) 0.0327(2) Uani 1.00 1 d . . . Os(5) Os 0.70901(10) -0.17161(7) 0.64657(9) 0.0362(2) Uani 1.00 1 d . . . Rh(1) Rh 0.6169(2) -0.02407(9) 0.6862(2) 0.0283(3) Uani 1.00 1 d . . . O(1) O 0.855(2) -0.0361(8) 0.394(2) 0.067(6) Uani 1.00 1 d . . . O(2) O 0.340(2) 0.0411(10) 0.220(2) 0.065(5) Uani 1.00 1 d . . . O(3) O 0.761(3) 0.1882(9) 0.329(2) 0.091(8) Uani 1.00 1 d . . . O(4) O 0.190(2) 0.1292(10) 0.584(2) 0.076(6) Uani 1.00 1 d . . . O(5) O 0.637(3) 0.2539(8) 0.871(2) 0.075(7) Uani 1.00 1 d . . . O(6) O 0.581(2) 0.0590(8) 1.059(2) 0.052(4) Uani 1.00 1 d . . . O(7) O 1.001(3) 0.2217(8) 0.880(3) 0.086(7) Uani 1.00 1 d . . . O(8) O 0.965(2) 0.0572(9) 1.186(2) 0.063(5) Uani 1.00 1 d . . . O(9) O 1.233(2) 0.0064(9) 0.863(2) 0.064(5) Uani 1.00 1 d . . . O(10) O 0.488(2) -0.0933(8) 1.155(2) 0.061(5) Uani 1.00 1 d . . . O(11) O 0.971(2) -0.1102(10) 1.138(2) 0.066(6) Uani 1.00 1 d . . . O(12) O 0.619(3) -0.2906(8) 0.990(2) 0.074(6) Uani 1.00 1 d . . . O(13) O 0.230(2) -0.1498(10) 0.663(2) 0.069(6) Uani 1.00 1 d . . . O(14) O 1.072(2) -0.1353(11) 0.884(2) 0.071(6) Uani 1.00 1 d . . . O(15) O 0.773(3) -0.3222(8) 0.749(2) 0.079(6) Uani 1.00 1 d . . . O(16) O 0.812(3) -0.1951(9) 0.376(2) 0.070(6) Uani 1.00 1 d . . . O(17) O 0.335(3) -0.1898(12) 0.420(2) 0.087(7) Uani 1.00 1 d . . . O(18) O 0.249(2) -0.0248(10) 0.477(2) 0.072(5) Uani 1.00 1 d . . . C(1) C 0.781(3) 0.0044(10) 0.429(2) 0.038(5) Uani 1.00 1 d . . . C(2) C 0.469(3) 0.0535(11) 0.326(2) 0.050(6) Uani 1.00 1 d . . . C(3) C 0.727(3) 0.1452(13) 0.390(3) 0.058(7) Uani 1.00 1 d . . . C(4) C 0.331(3) 0.1196(11) 0.641(3) 0.048(6) Uani 1.00 1 d . . . C(5) C 0.609(3) 0.1998(11) 0.818(2) 0.050(6) Uani 1.00 1 d . . . C(6) C 0.571(2) 0.0799(9) 0.937(2) 0.031(4) Uani 1.00 1 d . . . C(7) C 0.964(3) 0.1653(12) 0.866(3) 0.052(7) Uani 1.00 1 d . . . C(8) C 0.932(2) 0.0624(10) 1.055(3) 0.040(5) Uani 1.00 1 d . . . C(9) C 1.108(3) 0.0311(10) 0.857(2) 0.044(6) Uani 1.00 1 d . . . C(10) C 0.528(3) -0.1083(9) 1.057(2) 0.038(5) Uani 1.00 1 d . . . C(11) C 0.837(3) -0.1195(11) 1.048(2) 0.048(6) Uani 1.00 1 d . . . C(12) C 0.616(3) -0.2354(12) 0.956(3) 0.054(7) Uani 1.00 1 d . . . C(13) C 0.365(3) -0.1462(11) 0.747(3) 0.049(6) Uani 1.00 1 d . . . C(14) C 0.932(2) -0.1461(10) 0.797(2) 0.041(5) Uani 1.00 1 d . . . C(15) C 0.746(4) -0.2653(11) 0.716(3) 0.057(7) Uani 1.00 1 d . . . C(16) C 0.777(3) -0.1860(11) 0.478(3) 0.058(7) Uani 1.00 1 d . . . C(17) C 0.466(3) -0.1830(13) 0.502(3) 0.053(6) Uani 1.00 1 d . . . C(18) C 0.387(2) -0.0243(10) 0.554(2) 0.039(5) Uani 1.00 1 d . . . H(1) H 0.5411 0.1291 0.5400 0.0380 Uiso 1.00 1 c . . . H(2) H 0.8927 0.0866 0.6441 0.0380 Uiso 1.00 1 c . . . H(3) H 0.8405 -0.0152 0.8427 0.0380 Uiso 1.00 1 c . . . H(4) H 0.6888 -0.0808 0.5675 0.0380 Uiso 1.00 1 c . . . H(5) H 0.5670 -0.0434 0.8541 0.0380 Uiso 1.00 1 c . . . 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 Os(1) 0.0368(4) 0.0333(3) 0.0213(3) 0.0023(3) 0.0130(3) 0.0028(3) Os(2) 0.0400(4) 0.0280(3) 0.0265(3) 0.0030(3) 0.0171(3) 0.0013(3) Os(3) 0.0324(3) 0.0337(3) 0.0242(3) -0.0058(3) 0.0086(3) 0.0008(3) Os(4) 0.0435(4) 0.0276(3) 0.0323(3) -0.0009(3) 0.0214(3) 0.0013(3) Os(5) 0.0507(5) 0.0296(3) 0.0338(4) 0.0022(3) 0.0233(4) -0.0018(3) Rh(1) 0.0323(7) 0.0269(6) 0.0245(6) -0.0010(6) 0.0110(5) 0.0007(5) O(1) 0.085(12) 0.057(10) 0.085(12) 0.010(9) 0.060(11) -0.001(9) O(2) 0.061(11) 0.088(12) 0.043(9) 0.001(9) 0.020(8) -0.006(8) O(3) 0.16(2) 0.057(11) 0.083(13) -0.008(12) 0.07(2) 0.020(10) O(4) 0.059(11) 0.09(1) 0.074(12) 0.017(10) 0.023(10) 0.017(10) O(5) 0.12(2) 0.036(8) 0.11(2) -0.018(9) 0.09(1) -0.026(9) O(6) 0.063(9) 0.065(10) 0.038(7) -0.014(8) 0.032(7) 0.004(7) O(7) 0.09(2) 0.040(10) 0.10(1) -0.022(10) 0.013(12) 0.004(9) O(8) 0.079(11) 0.090(13) 0.031(7) -0.002(10) 0.033(8) 0.010(7) O(9) 0.039(9) 0.083(12) 0.073(11) 0.004(8) 0.025(8) 0.005(9) O(10) 0.096(13) 0.053(9) 0.051(9) 0.001(9) 0.049(10) -0.005(7) O(11) 0.064(11) 0.077(12) 0.051(9) -0.001(9) 0.019(9) -0.007(8) O(12) 0.10(2) 0.040(9) 0.11(2) 0.006(9) 0.076(13) 0.023(9) O(13) 0.048(10) 0.09(1) 0.058(10) -0.024(10) 0.016(8) -0.006(9) O(14) 0.050(10) 0.089(13) 0.076(11) -0.005(10) 0.029(9) -0.013(10) O(15) 0.12(2) 0.037(8) 0.072(12) 0.007(10) 0.038(12) 0.007(8) O(16) 0.11(2) 0.063(11) 0.065(11) 0.020(10) 0.059(11) 0.001(8) O(17) 0.072(13) 0.12(2) 0.073(13) -0.021(12) 0.035(11) -0.049(12) O(18) 0.045(10) 0.072(11) 0.075(11) -0.004(9) 0.003(9) 0.012(9) C(1) 0.041(11) 0.040(10) 0.036(10) 0.002(9) 0.021(9) 0.005(8) C(2) 0.07(1) 0.06(1) 0.029(10) 0.021(11) 0.021(10) -0.001(8) C(3) 0.07(2) 0.07(2) 0.032(10) -0.025(13) 0.022(11) 0.000(10) C(4) 0.053(13) 0.047(12) 0.047(11) 0.024(10) 0.024(10) 0.009(9) C(5) 0.08(2) 0.044(12) 0.037(10) 0.005(11) 0.034(11) 0.003(9) C(6) 0.023(7) 0.031(9) 0.038(9) 0.006(7) 0.012(7) -0.001(7) C(7) 0.045(12) 0.053(13) 0.06(1) -0.014(10) 0.027(11) -0.004(10) C(8) 0.022(8) 0.038(10) 0.064(13) -0.001(8) 0.022(8) 0.004(9) C(9) 0.047(12) 0.049(11) 0.033(10) -0.009(10) 0.016(9) 0.003(8) C(10) 0.049(11) 0.032(9) 0.040(10) -0.003(8) 0.025(9) 0.004(8) C(11) 0.052(13) 0.054(13) 0.033(10) -0.015(10) 0.015(10) -0.003(9) C(12) 0.07(2) 0.050(13) 0.07(2) -0.006(11) 0.06(1) 0.000(10) C(13) 0.06(1) 0.047(12) 0.045(12) -0.004(11) 0.029(11) 0.002(9) C(14) 0.037(10) 0.042(10) 0.053(11) -0.012(9) 0.027(9) -0.007(9) C(15) 0.09(2) 0.041(12) 0.046(12) -0.005(12) 0.033(12) -0.009(9) C(16) 0.09(2) 0.038(11) 0.06(1) -0.004(11) 0.05(1) -0.011(10) C(17) 0.038(12) 0.08(2) 0.036(10) -0.007(12) 0.008(10) -0.019(10) C(18) 0.026(9) 0.044(10) 0.039(10) 0.007(8) 0.006(8) 0.010(8) #============================================================================== _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'CRYSTALS (Watkin et al., 1996)' _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' #============================================================================== # 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 Os(1) Os(2) 2.870(1) yes . . Os(1) Os(3) 2.8980(7) yes . . Os(1) Rh(1) 2.726(2) yes . . Os(1) C(1) 1.89(2) yes . . Os(1) C(2) 1.85(2) yes . . Os(1) C(3) 1.92(3) yes . . Os(1) H(1) 1.76 no . . Os(1) H(2) 1.84 no . . Os(2) Os(3) 2.789(1) yes . . Os(2) Rh(1) 2.718(2) yes . . Os(2) C(4) 1.89(2) yes . . Os(2) C(5) 1.88(2) yes . . Os(2) C(6) 1.85(2) yes . . Os(2) H(1) 1.83 no . . Os(3) Rh(1) 2.942(2) yes . . Os(3) C(7) 1.91(2) yes . . Os(3) C(8) 1.91(2) yes . . Os(3) C(9) 1.91(2) yes . . Os(3) H(2) 1.78 no . . Os(3) H(3) 1.77 no . . Os(4) Os(5) 2.962(1) yes . . Os(4) Rh(1) 3.030(2) yes . . Os(4) C(10) 1.89(2) yes . . Os(4) C(11) 1.96(2) yes . . Os(4) C(12) 1.95(2) yes . . Os(4) C(13) 1.95(2) yes . . Os(4) H(5) 1.90 no . . Os(5) Rh(1) 3.053(2) yes . . Os(5) C(14) 1.92(2) yes . . Os(5) C(15) 1.92(2) yes . . Os(5) C(16) 1.90(3) yes . . Os(5) C(17) 1.98(2) yes . . Os(5) H(4) 1.90 no . . Rh(1) C(18) 1.86(2) yes . . Rh(1) H(3) 1.88 no . . Rh(1) H(4) 1.85 no . . Rh(1) H(5) 1.82 no . . O(1) C(1) 1.16(3) yes . . O(2) C(2) 1.16(2) yes . . O(3) C(3) 1.12(4) yes . . O(4) C(4) 1.14(3) yes . . O(5) C(5) 1.14(3) yes . . O(6) C(6) 1.16(2) yes . . O(7) C(7) 1.14(3) yes . . O(8) C(8) 1.11(3) yes . . O(9) C(9) 1.17(3) yes . . O(10) C(10) 1.13(3) yes . . O(11) C(11) 1.13(3) yes . . O(12) C(12) 1.12(3) yes . . O(13) C(13) 1.11(3) yes . . O(14) C(14) 1.16(2) yes . . O(15) C(15) 1.15(3) yes . . O(16) C(16) 1.13(4) yes . . O(17) C(17) 1.08(3) yes . . O(18) C(18) 1.11(2) 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(1) Os(5) C(14) 84.9(6) yes . . . Rh(1) Os(5) C(15) 151.0(9) yes . . . Rh(1) Os(5) C(16) 115.3(6) yes . . . Rh(1) Os(5) C(17) 85.6(7) yes . . . Rh(1) Os(5) H(4) 35 no . . . Rh(1) Os(5) Os(4) 60.48(5) yes . . . C(14) Os(5) C(15) 91.8(9) yes . . . C(14) Os(5) C(16) 92(1) yes . . . C(14) Os(5) C(17) 170(1) yes . . . C(14) Os(5) H(4) 86 no . . . C(14) Os(5) Os(4) 86.9(8) yes . . . C(15) Os(5) C(16) 93(1) yes . . . C(15) Os(5) C(17) 95(1) yes . . . C(15) Os(5) H(4) 174 no . . . C(15) Os(5) Os(4) 90.6(9) yes . . . C(16) Os(5) C(17) 93(1) yes . . . C(16) Os(5) H(4) 81 no . . . C(16) Os(5) Os(4) 175.8(6) yes . . . C(17) Os(5) H(4) 87 no . . . C(17) Os(5) Os(4) 86.6(8) yes . . . H(4) Os(5) Os(4) 95 no . . . Os(1) C(1) O(1) 176(1) yes . . . Os(1) C(2) O(2) 178(2) yes . . . Os(1) C(3) O(3) 178(1) yes . . . Os(2) C(4) O(4) 176(1) yes . . . Os(2) C(5) O(5) 176(2) yes . . . Os(2) C(6) O(6) 175(1) yes . . . Os(3) C(7) O(7) 178(2) yes . . . Os(3) C(8) O(8) 173(1) yes . . . Os(3) C(9) O(9) 178(1) yes . . . Os(4) C(10) O(10) 176(1) yes . . . Os(4) C(11) O(11) 176(2) yes . . . Os(4) C(12) O(12) 176(2) yes . . . Os(4) C(13) O(13) 177(2) yes . . . Os(5) C(14) O(14) 174(2) yes . . . Os(5) C(15) O(15) 174(2) yes . . . Os(5) C(16) O(16) 177(2) yes . . . Os(5) C(17) O(17) 177(2) yes . . . Rh(1) C(18) O(18) 179(2) yes . . . Os(1) H(1) Os(2) 106 no . . . Os(1) H(2) Os(3) 107 no . . . Os(3) H(3) Rh(1) 107 no . . . Os(5) H(4) Rh(1) 109 no . . . Rh(1) H(5) Os(4) 109 no . . .