Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _audit_creation_method Xtal3.6 _audit_creation_date 01-11-08 _audit_update_record ? _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bruce, M. I.' 'Skelton, Brian W.' 'White, Allan H.' 'Zaitseva, Natasha N.' _publ_contact_author_name 'Prof M I Bruce' _publ_contact_author_address ; Department of Chemistry University of Adelaide Adelaide 5005 AUSTRALIA ; _publ_contact_author_email MBRUCE@CHEMISTRY.ADELAIDE.EDU.AU _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_section_title ; Some Reactions of Allenylidene-Ruthenium Cluster Carbonyls with Alkynes ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_br563 _database_code_CSD 175557 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C39 H22 O8 Ru3' _chemical_formula_moiety ? _chemical_formula_weight 921.81 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 17.990(4) _cell_length_b 17.483(7) _cell_length_c 13.184(5) _cell_angle_alpha 107.88(3) _cell_angle_beta 103.46(2) _cell_angle_gamma 108.70(2) _cell_volume 3477(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 15.8 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.34 _exptl_crystal_description rod _exptl_crystal_size_max .2 _exptl_crystal_size_mid .09 _exptl_crystal_size_min .07 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min .85 _exptl_absorpt_correction_T_max .92 _diffrn_reflns_number 12220 _reflns_number_total 12220 _reflns_Friedel_coverage ? _reflns_number_gt 5695 _reflns_threshold_expression 'I > 3.0sig(I )' _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .042 _refine_ls_wR_factor_ref .038 _refine_ls_goodness_of_fit_ref 1.241 _refine_ls_number_reflns 5699 _refine_ls_number_parameters 901 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .012 _refine_diff_density_min -.493 _refine_diff_density_max .629 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction 'xtal ADDREF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 156 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 32 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 88 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 12 -1.42 .835999 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru11 .54769(5) .19788(6) .17695(7) .0411(4) Uani ? ? 1.00000 ? ? Ru12 .39499(5) .13203(6) .20821(7) .0373(4) Uani ? ? 1.00000 ? ? Ru13 .53456(5) .27632(6) .39055(7) .0428(4) Uani ? ? 1.00000 ? ? C111 .5924(8) .1277(9) .2439(11) .067(7) Uani ? ? 1.00000 ? ? O111 .6189(7) .0848(7) .2737(9) .116(7) Uani ? ? 1.00000 ? ? C112 .6526(8) .2896(8) .2117(10) .059(6) Uani ? ? 1.00000 ? ? O112 .7144(5) .3464(6) .2338(9) .098(5) Uani ? ? 1.00000 ? ? C113 .5424(7) .1365(9) .0284(11) .065(6) Uani ? ? 1.00000 ? ? O113 .5400(6) .0971(6) -.0602(8) .094(5) Uani ? ? 1.00000 ? ? C121 .3728(8) .0132(8) .2064(10) .062(6) Uani ? ? 1.00000 ? ? O121 .3573(6) -.0573(6) .1970(8) .095(5) Uani ? ? 1.00000 ? ? C122 .2848(7) .1248(7) .1795(10) .056(5) Uani ? ? 1.00000 ? ? O122 .2217(6) .1278(6) .1659(8) .092(5) Uani ? ? 1.00000 ? ? C123 .3775(7) .0770(8) .0457(11) .057(6) Uani ? ? 1.00000 ? ? O123 .3541(5) .0376(6) -.0500(7) .084(4) Uani ? ? 1.00000 ? ? C131 .5947(8) .2306(8) .4674(11) .071(7) Uani ? ? 1.00000 ? ? O131 .6373(6) .2084(7) .5224(8) .104(6) Uani ? ? 1.00000 ? ? C132 .6366(9) .3763(10) .4512(11) .081(7) Uani ? ? 1.00000 ? ? O132 .7003(6) .4386(7) .4919(9) .118(6) Uani ? ? 1.00000 ? ? C11 .4526(6) .2830(7) .0343(9) .044(5) Uani ? ? 1.00000 ? ? C1111 .3830(7) .3097(7) .0124(9) .047(5) Uani ? ? 1.00000 ? ? C1112 .3084(8) .2696(7) .0234(9) .056(6) Uani ? ? 1.00000 ? ? C1113 .2456(8) .2987(10) .0080(11) .077(7) Uani ? ? 1.00000 ? ? C1114 .2583(9) .3716(11) -.0178(13) .087(8) Uani ? ? 1.00000 ? ? C1115 .3299(10) .4120(9) -.0298(11) .082(8) Uani ? ? 1.00000 ? ? C1116 .3943(7) .3831(8) -.0159(10) .064(6) Uani ? ? 1.00000 ? ? C1121 .4972(7) .2789(7) -.0471(10) .045(5) Uani ? ? 1.00000 ? ? C1122 .5841(8) .3312(8) -.0100(10) .066(6) Uani ? ? 1.00000 ? ? C1123 .6250(8) .3265(10) -.0863(13) .084(7) Uani ? ? 1.00000 ? ? C1124 .5834(10) .2678(10) -.1972(12) .079(8) Uani ? ? 1.00000 ? ? C1125 .4984(9) .2167(9) -.2375(10) .076(7) Uani ? ? 1.00000 ? ? C1126 .4581(7) .2231(8) -.1608(11) .065(6) Uani ? ? 1.00000 ? ? C12 .4738(6) .2605(6) .1230(9) .037(4) Uani ? ? 1.00000 ? ? C13 .4442(6) .2573(7) .2133(9) .040(4) Uani ? ? 1.00000 ? ? C14 .4593(6) .3387(7) .3042(8) .045(5) Uani ? ? 1.00000 ? ? C141 .4878(7) .4248(7) .2910(9) .048(5) Uani ? ? 1.00000 ? ? C142 .4341(8) .4664(8) .2879(10) .061(6) Uani ? ? 1.00000 ? ? C143 .4552(9) .5436(9) .2707(10) .069(7) Uani ? ? 1.00000 ? ? C144 .5285(10) .5815(8) .2600(11) .072(7) Uani ? ? 1.00000 ? ? C145 .5840(8) .5413(9) .2614(10) .072(7) Uani ? ? 1.00000 ? ? C146 .5648(7) .4637(8) .2799(10) .062(6) Uani ? ? 1.00000 ? ? C15 .4461(7) .3439(7) .4067(9) .050(5) Uani ? ? 1.00000 ? ? C16 .4220(6) .2739(7) .4419(8) .045(5) Uani ? ? 1.00000 ? ? C17 .4098(6) .1862(7) .3819(9) .046(5) Uani ? ? 1.00000 ? ? C171 .3825(7) .1235(7) .4354(9) .051(5) Uani ? ? 1.00000 ? ? C172 .4241(8) .0719(8) .4532(10) .064(6) Uani ? ? 1.00000 ? ? C173 .3970(8) .0149(9) .5018(11) .075(7) Uani ? ? 1.00000 ? ? C174 .3283(9) .0068(9) .5327(11) .080(7) Uani ? ? 1.00000 ? ? C175 .2849(8) .0576(10) .5136(12) .085(8) Uani ? ? 1.00000 ? ? C176 .3136(7) .1165(8) .4668(10) .066(6) Uani ? ? 1.00000 ? ? Ru21 .09827(5) .85083(6) .87043(8) .0419(4) Uani ? ? 1.00000 ? ? Ru22 -.06321(5) .80063(6) .71920(7) .0403(4) Uani ? ? 1.00000 ? ? Ru23 .05012(5) .75481(6) .63062(8) .0433(4) Uani ? ? 1.00000 ? ? C211 .1409(8) .9624(9) .8552(11) .069(6) Uani ? ? 1.00000 ? ? O211 .1656(6) 1.0301(6) .8572(9) .101(5) Uani ? ? 1.00000 ? ? C212 .1993(8) .8365(8) .8965(10) .059(6) Uani ? ? 1.00000 ? ? O212 .2609(5) .8300(6) .9124(8) .090(5) Uani ? ? 1.00000 ? ? C213 .1206(8) .9075(8) 1.0283(12) .066(6) Uani ? ? 1.00000 ? ? O213 .1360(6) .9429(6) 1.1242(8) .084(5) Uani ? ? 1.00000 ? ? C221 -.0636(8) .9105(8) .7088(10) .061(6) Uani ? ? 1.00000 ? ? O221 -.0646(7) .9732(7) .7035(9) .110(6) Uani ? ? 1.00000 ? ? C222 -.1812(8) .7320(8) .6649(10) .057(6) Uani ? ? 1.00000 ? ? O222 -.2510(5) .6855(7) .6333(9) .105(6) Uani ? ? 1.00000 ? ? C223 -.0535(7) .8529(8) .8767(11) .062(6) Uani ? ? 1.00000 ? ? O223 -.0603(5) .8814(7) .9635(7) .085(5) Uani ? ? 1.00000 ? ? C231 .1099(8) .8565(9) .6180(11) .071(7) Uani ? ? 1.00000 ? ? O231 .1517(6) .9173(7) .6065(9) .107(6) Uani ? ? 1.00000 ? ? C232 .1405(7) .7259(8) .6161(10) .063(6) Uani ? ? 1.00000 ? ? O232 .1960(6) .7117(7) .6028(8) .101(6) Uani ? ? 1.00000 ? ? C21 .0025(6) .6934(7) .9392(9) .042(5) Uani ? ? 1.00000 ? ? C2111 -.0752(7) .6088(7) .8997(10) .049(5) Uani ? ? 1.00000 ? ? C2112 -.1497(7) .5878(8) .8148(10) .057(5) Uani ? ? 1.00000 ? ? C2113 -.2172(7) .5068(9) .7739(10) .066(6) Uani ? ? 1.00000 ? ? C2114 -.2101(8) .4467(9) .8194(12) .075(7) Uani ? ? 1.00000 ? ? C2115 -.1378(9) .4680(8) .9059(12) .075(7) Uani ? ? 1.00000 ? ? C2116 -.0730(7) .5483(8) .9466(10) .062(6) Uani ? ? 1.00000 ? ? C2121 .0589(8) .7325(7) 1.0603(10) .056(6) Uani ? ? 1.00000 ? ? C2122 .1445(9) .7466(8) 1.0888(12) .075(7) Uani ? ? 1.00000 ? ? C2123 .1950(11) .7831(11) 1.2039(17) .109(9) Uani ? ? 1.00000 ? ? C2124 .1654(15) .8051(12) 1.2866(16) .126(11) Uani ? ? 1.00000 ? ? C2125 .0823(14) .7914(11) 1.2607(14) .111(9) Uani ? ? 1.00000 ? ? C2126 .0315(9) .7542(9) 1.1482(13) .078(7) Uani ? ? 1.00000 ? ? C22 .0180(6) .7285(6) .8635(9) .038(5) Uani ? ? 1.00000 ? ? C23 -.0228(6) .7082(7) .7477(9) .041(5) Uani ? ? 1.00000 ? ? C24 -.0239(6) .6336(7) .6610(10) .046(5) Uani ? ? 1.00000 ? ? C241 .0031(8) .5674(8) .6939(10) .052(5) Uani ? ? 1.00000 ? ? C242 -.0585(8) .4825(8) .6576(10) .061(6) Uani ? ? 1.00000 ? ? C243 -.0371(10) .4243(9) .6926(12) .078(7) Uani ? ? 1.00000 ? ? C244 .0426(11) .4450(9) .7603(12) .072(7) Uani ? ? 1.00000 ? ? C245 .1058(8) .5295(10) .7925(11) .072(7) Uani ? ? 1.00000 ? ? C246 .0853(8) .5903(7) .7598(10) .060(6) Uani ? ? 1.00000 ? ? C25 -.0519(7) .6125(8) .5420(10) .053(6) Uani ? ? 1.00000 ? ? C26 -.0784(7) .6622(8) .4896(10) .060(6) Uani ? ? 1.00000 ? ? C27 -.0764(6) .7475(8) .5479(9) .052(5) Uani ? ? 1.00000 ? ? C271 -.1073(8) .7834(8) .4666(10) .057(6) Uani ? ? 1.00000 ? ? C272 -.0585(10) .8560(13) .4550(15) .121(11) Uani ? ? 1.00000 ? ? C273 -.0939(13) .8828(14) .374(2) .140(13) Uani ? ? 1.00000 ? ? C274 -.1744(13) .8420(13) .3085(13) .102(10) Uani ? ? 1.00000 ? ? C275 -.2235(10) .7721(12) .3214(14) .117(10) Uani ? ? 1.00000 ? ? C276 -.1915(9) .7431(9) .3998(13) .094(8) Uani ? ? 1.00000 ? ? H1112 .29911 .21742 .04195 .07000 Uiso ? ? 1.00000 ? ? H1113 .19207 .26824 .01499 .08600 Uiso ? ? 1.00000 ? ? H1114 .21568 .39466 -.02530 .10300 Uiso ? ? 1.00000 ? ? H1115 .34010 .46462 -.04719 .09700 Uiso ? ? 1.00000 ? ? H1116 .44669 .41244 -.02633 .07500 Uiso ? ? 1.00000 ? ? H1122 .61640 .37056 .07156 .07500 Uiso ? ? 1.00000 ? ? H1123 .68442 .36711 -.06079 .09200 Uiso ? ? 1.00000 ? ? H1124 .61605 .26356 -.24695 .09100 Uiso ? ? 1.00000 ? ? H1125 .46845 .17671 -.31910 .08900 Uiso ? ? 1.00000 ? ? H1126 .39750 .18661 -.18904 .07900 Uiso ? ? 1.00000 ? ? H142 .38101 .44076 .29802 .07400 Uiso ? ? 1.00000 ? ? H143 .41606 .57272 .26831 .08000 Uiso ? ? 1.00000 ? ? H144 .54411 .63687 .25120 .08400 Uiso ? ? 1.00000 ? ? H145 .63667 .56680 .24925 .08300 Uiso ? ? 1.00000 ? ? H146 .60547 .43719 .28683 .07500 Uiso ? ? 1.00000 ? ? H15 .45446 .40281 .45976 .06000 Uiso ? ? 1.00000 ? ? H16 .42199 .29623 .52463 .05100 Uiso ? ? 1.00000 ? ? H172 .47246 .07531 .42860 .07200 Uiso ? ? 1.00000 ? ? H173 .42734 -.02143 .51481 .09000 Uiso ? ? 1.00000 ? ? H174 .31114 -.03415 .56901 .09700 Uiso ? ? 1.00000 ? ? H175 .23346 .05027 .53160 .10100 Uiso ? ? 1.00000 ? ? H176 .28409 .15358 .45214 .08000 Uiso ? ? 1.00000 ? ? H2112 -.15463 .63096 .78266 .07100 Uiso ? ? 1.00000 ? ? H2113 -.27034 .49179 .71454 .07500 Uiso ? ? 1.00000 ? ? H2114 -.25702 .38894 .78869 .08300 Uiso ? ? 1.00000 ? ? H2115 -.13421 .42376 .93526 .08500 Uiso ? ? 1.00000 ? ? H2116 -.02203 .56524 1.01304 .07800 Uiso ? ? 1.00000 ? ? H2122 .16684 .73107 1.02662 .09000 Uiso ? ? 1.00000 ? ? H2123 .25416 .78935 1.21998 .13800 Uiso ? ? 1.00000 ? ? H2124 .20809 .83267 1.36595 .16700 Uiso ? ? 1.00000 ? ? H2125 .06565 .81006 1.32483 .13000 Uiso ? ? 1.00000 ? ? H2126 -.02846 .74105 1.13106 .08900 Uiso ? ? 1.00000 ? ? H242 -.11579 .46518 .60704 .07200 Uiso ? ? 1.00000 ? ? H243 -.08001 .36599 .66826 .09300 Uiso ? ? 1.00000 ? ? H244 .05506 .40222 .78511 .08400 Uiso ? ? 1.00000 ? ? H245 .16478 .54509 .83789 .08100 Uiso ? ? 1.00000 ? ? H246 .12929 .65106 .78525 .06800 Uiso ? ? 1.00000 ? ? H25 -.05289 .55658 .49077 .06700 Uiso ? ? 1.00000 ? ? H26 -.08988 .63751 .41491 .06800 Uiso ? ? 1.00000 ? ? H272 .00255 .89123 .50739 .14000 Uiso ? ? 1.00000 ? ? H273 -.06009 .93601 .36465 .16200 Uiso ? ? 1.00000 ? ? H274 -.20207 .85775 .24944 .12400 Uiso ? ? 1.00000 ? ? H275 -.28523 .73993 .27429 .13000 Uiso ? ? 1.00000 ? ? H276 -.23001 .69176 .40826 .10400 Uiso ? ? 1.00000 ? ? 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 Ru11 .0360(5) .0482(6) .0448(6) .0202(5) .0200(5) .0202(5) Ru12 .0379(5) .0352(5) .0412(6) .0147(4) .0198(4) .0159(5) Ru13 .0440(6) .0456(6) .0368(5) .0165(5) .0147(5) .0172(5) C111 .075(10) .065(10) .066(9) .033(8) .029(8) .027(8) O111 .140(10) .127(10) .110(9) .098(8) .029(7) .054(8) C112 .058(8) .072(10) .061(8) .036(7) .024(7) .035(8) O112 .042(5) .084(7) .139(9) .004(5) .021(6) .045(7) C113 .057(8) .096(11) .064(9) .041(8) .034(7) .042(8) O113 .105(8) .115(8) .076(7) .061(6) .059(6) .023(6) C121 .084(9) .052(8) .069(9) .040(8) .048(8) .024(7) O121 .148(9) .050(6) .116(8) .048(6) .081(7) .040(6) C122 .051(8) .044(7) .064(8) .011(7) .025(7) .016(6) O122 .066(6) .091(7) .136(9) .045(6) .050(6) .044(6) C123 .047(8) .065(9) .051(8) .016(7) .011(7) .027(7) O123 .069(6) .090(7) .049(6) .009(5) .011(5) .008(5) C131 .073(10) .065(9) .067(9) .021(8) .012(8) .034(8) O131 .092(8) .130(9) .096(8) .055(7) .015(6) .063(7) C132 .089(11) .084(11) .059(9) .032(9) .014(9) .031(9) O132 .089(8) .094(8) .098(8) -.019(6) .000(7) .034(7) C11 .036(6) .039(7) .052(7) .011(5) .019(6) .014(6) C1111 .058(8) .039(7) .045(7) .016(6) .024(6) .019(6) C1112 .064(8) .056(8) .062(8) .031(7) .029(7) .030(7) C1113 .068(10) .097(12) .089(11) .045(9) .046(8) .046(9) C1114 .071(10) .108(13) .106(12) .056(10) .031(9) .056(11) C1115 .113(13) .086(11) .079(10) .068(11) .041(10) .043(9) C1116 .070(9) .067(9) .070(9) .029(7) .035(7) .038(8) C1121 .052(8) .042(7) .050(8) .024(6) .021(6) .024(6) C1122 .070(9) .074(9) .044(8) .014(8) .019(7) .029(7) C1123 .062(9) .101(12) .081(11) .011(8) .041(9) .042(10) C1124 .100(12) .089(11) .071(10) .052(10) .054(10) .031(9) C1125 .076(10) .083(10) .054(9) .016(8) .030(8) .024(8) C1126 .065(9) .067(9) .060(9) .023(7) .032(8) .024(8) C12 .032(6) .029(6) .046(7) .008(5) .014(5) .016(5) C13 .033(6) .044(7) .041(7) .016(5) .014(5) .015(6) C14 .047(7) .049(7) .034(6) .013(6) .017(5) .015(6) C141 .054(8) .037(7) .042(7) .018(6) .012(6) .009(6) C142 .081(9) .061(9) .069(9) .041(8) .040(7) .039(7) C143 .084(10) .063(9) .063(9) .029(8) .025(8) .031(8) C144 .101(12) .033(8) .068(9) .021(8) .031(9) .010(7) C145 .087(10) .059(9) .067(9) .013(8) .037(8) .034(8) C146 .049(8) .052(8) .073(9) .018(7) .015(7) .018(7) C15 .063(8) .049(7) .042(7) .029(6) .023(6) .016(6) C16 .055(7) .049(7) .027(6) .016(6) .021(5) .013(6) C17 .048(7) .049(7) .047(7) .022(6) .023(6) .021(6) C171 .073(9) .040(7) .054(8) .028(6) .030(7) .029(6) C172 .087(10) .070(9) .062(9) .041(8) .041(8) .044(8) C173 .082(10) .091(11) .078(10) .045(9) .040(8) .050(9) C174 .090(11) .087(11) .074(10) .027(9) .030(9) .059(9) C175 .073(10) .105(12) .098(12) .031(9) .048(9) .063(10) C176 .050(8) .083(10) .082(9) .026(7) .039(7) .046(8) Ru21 .0369(5) .0370(6) .0502(6) .0130(4) .0167(5) .0186(5) Ru22 .0402(5) .0443(6) .0469(6) .0238(5) .0227(5) .0207(5) Ru23 .0440(6) .0495(6) .0497(6) .0250(5) .0268(5) .0247(5) C211 .058(9) .058(9) .076(10) .011(7) .017(7) .027(8) O211 .109(8) .056(7) .120(9) .011(6) .035(7) .047(7) C212 .057(8) .062(9) .060(8) .022(7) .026(7) .029(7) O212 .050(6) .097(8) .117(8) .036(6) .029(6) .035(6) C213 .061(9) .050(9) .085(11) .018(7) .028(8) .032(8) O213 .107(8) .066(7) .058(6) .021(6) .030(6) .017(5) C221 .088(10) .065(9) .068(9) .052(8) .038(7) .047(8) O221 .170(10) .100(8) .139(9) .093(8) .093(8) .083(8) C222 .066(9) .073(10) .057(8) .049(8) .029(7) .032(7) O222 .046(6) .108(9) .140(9) .025(6) .025(6) .042(7) C223 .050(8) .068(9) .053(9) .015(7) .010(7) .021(8) O223 .082(7) .131(9) .052(6) .061(6) .033(5) .028(6) C231 .073(10) .083(11) .081(10) .039(9) .044(8) .045(9) O231 .098(8) .103(9) .143(10) .036(7) .058(7) .077(8) C232 .054(8) .076(9) .063(9) .029(7) .027(7) .030(7) O232 .071(7) .148(10) .116(8) .070(7) .052(6) .056(7) C21 .044(7) .039(7) .056(8) .024(6) .027(6) .021(6) C2111 .040(7) .042(7) .064(8) .009(6) .034(6) .019(6) C2112 .046(8) .064(9) .056(8) .011(7) .022(7) .030(7) C2113 .039(7) .093(11) .051(8) .011(7) .017(6) .029(8) C2114 .056(9) .074(10) .080(10) .000(8) .040(8) .029(9) C2115 .067(9) .058(9) .100(11) .010(8) .030(9) .047(9) C2116 .068(9) .051(8) .069(9) .018(7) .026(7) .031(7) C2121 .065(9) .037(7) .046(8) .013(6) .004(7) .014(6) C2122 .070(10) .054(9) .086(11) .016(7) .007(9) .034(8) C2123 .087(13) .084(13) .107(16) .004(10) -.017(12) .051(13) C2124 .15(2) .070(12) .076(14) -.002(13) -.013(15) .023(11) C2125 .170(18) .074(12) .052(11) .019(13) .040(13) .013(9) C2126 .096(11) .066(10) .059(10) .023(8) .028(9) .023(8) C22 .034(6) .038(6) .056(8) .024(5) .022(6) .021(6) C23 .040(7) .036(7) .051(7) .017(5) .024(6) .018(6) C24 .035(6) .051(8) .053(8) .019(6) .022(6) .019(6) C241 .067(9) .048(8) .060(8) .034(7) .037(7) .024(7) C242 .078(9) .047(8) .064(9) .032(7) .040(7) .015(7) C243 .106(12) .064(10) .096(12) .050(9) .059(10) .045(9) C244 .125(13) .068(10) .076(10) .065(10) .058(10) .054(9) C245 .080(10) .094(11) .075(10) .056(9) .038(8) .050(9) C246 .061(9) .047(8) .079(9) .027(7) .022(7) .032(7) C25 .056(8) .061(8) .049(8) .029(7) .021(6) .027(7) C26 .060(8) .061(9) .050(8) .022(7) .024(7) .013(7) C27 .043(7) .063(9) .047(7) .022(6) .017(6) .020(7) C271 .069(9) .065(9) .054(8) .040(8) .032(7) .027(7) C272 .096(13) .20(2) .144(16) .073(13) .068(12) .132(16) C273 .130(17) .20(2) .18(2) .082(17) .080(16) .16(2) C274 .148(18) .113(15) .083(13) .078(15) .043(13) .061(12) C275 .096(13) .129(16) .105(14) .035(12) -.009(10) .069(13) C276 .074(11) .088(11) .097(12) .017(9) .002(9) .049(10) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ru11 Ru12 . . 2.7986(15) ? Ru11 Ru13 . . 2.8308(17) ? Ru11 C111 . . 1.975(17) ? Ru11 C112 . . 1.884(12) ? Ru11 C113 . . 1.884(14) ? Ru11 C12 . . 2.107(12) ? Ru11 C13 . . 2.475(12) ? Ru12 Ru13 . . 2.8021(11) ? Ru12 C121 . . 1.977(15) ? Ru12 C122 . . 1.884(14) ? Ru12 C123 . . 1.960(13) ? Ru12 C13 . . 2.055(12) ? Ru12 C17 . . 2.106(11) ? Ru13 C131 . . 1.837(17) ? Ru13 C132 . . 1.861(13) ? Ru13 C13 . . 2.371(11) ? Ru13 C14 . . 2.304(13) ? Ru13 C15 . . 2.276(14) ? Ru13 C16 . . 2.272(13) ? Ru13 C17 . . 2.244(11) ? C111 O111 . . 1.13(2) ? C112 O112 . . 1.127(15) ? C113 O113 . . 1.143(17) ? C121 O121 . . 1.133(18) ? C122 O122 . . 1.129(18) ? C123 O123 . . 1.130(15) ? C131 O131 . . 1.17(2) ? C132 O132 . . 1.158(15) ? C11 C1111 . . 1.469(19) ? C11 C1121 . . 1.48(2) ? C11 C12 . . 1.358(18) ? C1111 C1112 . . 1.365(18) ? C1111 C1116 . . 1.41(2) ? C1112 C1113 . . 1.38(2) ? C1112 H1112 . . .990 ? C1113 C1114 . . 1.38(3) ? C1113 H1113 . . .981 ? C1114 C1115 . . 1.33(2) ? C1114 H1114 . . .97 ? C1115 C1116 . . 1.40(3) ? C1115 H1115 . . .986 ? C1116 H1116 . . .982 ? C1121 C1122 . . 1.403(16) ? C1121 C1126 . . 1.366(15) ? C1122 C1123 . . 1.38(2) ? C1122 H1122 . . .983 ? C1123 C1124 . . 1.352(18) ? C1123 H1123 . . .979 ? C1124 C1125 . . 1.37(2) ? C1124 H1124 . . .979 ? C1125 C1126 . . 1.37(2) ? C1125 H1125 . . .982 ? C1126 H1126 . . .976 ? C12 C13 . . 1.421(17) ? C13 C14 . . 1.446(15) ? C14 C141 . . 1.505(18) ? C14 C15 . . 1.407(17) ? C141 C142 . . 1.38(2) ? C141 C146 . . 1.400(18) ? C142 C143 . . 1.38(2) ? C142 H142 . . .976 ? C143 C144 . . 1.33(2) ? C143 H143 . . .992 ? C144 C145 . . 1.39(2) ? C144 H144 . . .969 ? C145 C146 . . 1.40(2) ? C145 H145 . . .983 ? C146 H146 . . .985 ? C15 C16 . . 1.415(19) ? C15 H15 . . .991 ? C16 C17 . . 1.408(17) ? C16 H16 . . 1.039 ? C17 C171 . . 1.494(19) ? C171 C172 . . 1.38(2) ? C171 C176 . . 1.38(2) ? C172 C173 . . 1.37(2) ? C172 H172 . . .988 ? C173 C174 . . 1.37(2) ? C173 H173 . . .989 ? C174 C175 . . 1.40(3) ? C174 H174 . . .987 ? C175 C176 . . 1.38(2) ? C175 H175 . . .987 ? C176 H176 . . .995 ? Ru21 Ru22 . . 2.7891(14) ? Ru21 Ru23 . . 2.8458(16) ? Ru21 C211 . . 1.945(16) ? Ru21 C212 . . 1.880(15) ? Ru21 C213 . . 1.888(15) ? Ru21 C22 . . 2.122(11) ? Ru21 C23 . . 2.445(8) ? Ru22 Ru23 . . 2.7827(16) ? Ru22 C221 . . 1.969(16) ? Ru22 C222 . . 1.895(12) ? Ru22 C223 . . 1.935(13) ? Ru22 C23 . . 2.068(13) ? Ru22 C27 . . 2.084(12) ? Ru23 C231 . . 1.840(16) ? Ru23 C232 . . 1.883(15) ? Ru23 C23 . . 2.408(13) ? Ru23 C24 . . 2.320(13) ? Ru23 C25 . . 2.283(10) ? Ru23 C26 . . 2.275(9) ? Ru23 C27 . . 2.226(12) ? C211 O211 . . 1.113(19) ? C212 O212 . . 1.129(18) ? C213 O213 . . 1.141(17) ? C221 O221 . . 1.13(2) ? C222 O222 . . 1.142(15) ? C223 O223 . . 1.152(17) ? C231 O231 . . 1.16(2) ? C232 O232 . . 1.14(2) ? C21 C2111 . . 1.508(13) ? C21 C2121 . . 1.475(15) ? C21 C22 . . 1.360(19) ? C2111 C2112 . . 1.384(16) ? C2111 C2116 . . 1.39(2) ? C2112 C2113 . . 1.376(16) ? C2112 H2112 . . .990 ? C2113 C2114 . . 1.39(2) ? C2113 H2113 . . .979 ? C2114 C2115 . . 1.37(2) ? C2114 H2114 . . .970 ? C2115 C2116 . . 1.348(16) ? C2115 H2115 . . .978 ? C2116 H2116 . . .994 ? C2121 C2122 . . 1.41(2) ? C2121 C2126 . . 1.36(2) ? C2122 C2123 . . 1.39(2) ? C2122 H2122 . . .997 ? C2123 C2124 . . 1.33(3) ? C2123 H2123 . . 1.00 ? C2124 C2125 . . 1.38(4) ? C2124 H2124 . . .998 ? C2125 C2126 . . 1.36(2) ? C2125 H2125 . . .96 ? C2126 H2126 . . .982(15) ? C22 C23 . . 1.405(16) ? C23 C24 . . 1.438(16) ? C24 C241 . . 1.53(2) ? C24 C25 . . 1.417(17) ? C241 C242 . . 1.386(16) ? C241 C246 . . 1.381(18) ? C242 C243 . . 1.36(2) ? C242 H242 . . .977 ? C243 C244 . . 1.36(2) ? C243 H243 . . .958 ? C244 C245 . . 1.40(2) ? C244 H244 . . .971 ? C245 C246 . . 1.38(2) ? C245 H245 . . .989 ? C246 H246 . . .993 ? C25 C26 . . 1.39(2) ? C25 H25 . . .995 ? C26 C27 . . 1.436(19) ? C26 H26 . . .886 ? C27 C271 . . 1.49(2) ? C271 C272 . . 1.37(3) ? C271 C276 . . 1.371(18) ? C272 C273 . . 1.40(4) ? C272 H272 . . 1.007 ? C273 C274 . . 1.32(3) ? C273 H273 . . 1.00 ? C274 C275 . . 1.34(3) ? C274 H274 . . .98 ? C275 C276 . . 1.38(3) ? C275 H275 . . .999 ? C276 H276 . . .999 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Ru12 Ru11 Ru13 . . . 59.70(4) ? Ru12 Ru11 C111 . . . 92.7(4) ? Ru12 Ru11 C112 . . . 152.2(4) ? Ru12 Ru11 C113 . . . 113.3(4) ? Ru12 Ru11 C12 . . . 71.7(3) ? Ru12 Ru11 C13 . . . 45.4(3) ? Ru13 Ru11 C111 . . . 86.1(4) ? Ru13 Ru11 C112 . . . 94.9(4) ? Ru13 Ru11 C113 . . . 173.0(3) ? Ru13 Ru11 C12 . . . 83.6(3) ? Ru13 Ru11 C13 . . . 52.6(2) ? C111 Ru11 C112 . . . 97.0(6) ? C111 Ru11 C113 . . . 94.8(7) ? C111 Ru11 C12 . . . 164.1(6) ? C111 Ru11 C13 . . . 130.3(6) ? C112 Ru11 C113 . . . 91.8(5) ? C112 Ru11 C12 . . . 95.9(6) ? C112 Ru11 C13 . . . 111.3(5) ? C113 Ru11 C12 . . . 94.0(6) ? C113 Ru11 C13 . . . 123.0(5) ? C12 Ru11 C13 . . . 35.0(4) ? Ru11 Ru12 Ru13 . . . 60.72(4) ? Ru11 Ru12 C121 . . . 108.8(4) ? Ru11 Ru12 C122 . . . 147.0(4) ? Ru11 Ru12 C123 . . . 70.3(3) ? Ru11 Ru12 C13 . . . 59.0(3) ? Ru11 Ru12 C17 . . . 111.7(3) ? Ru13 Ru12 C121 . . . 117.0(3) ? Ru13 Ru12 C122 . . . 121.8(3) ? Ru13 Ru12 C123 . . . 130.1(3) ? Ru13 Ru12 C13 . . . 55.9(3) ? Ru13 Ru12 C17 . . . 52.1(3) ? C121 Ru12 C122 . . . 98.7(6) ? C121 Ru12 C123 . . . 86.0(6) ? C121 Ru12 C13 . . . 167.4(5) ? C121 Ru12 C17 . . . 92.0(5) ? C122 Ru12 C123 . . . 94.3(5) ? C122 Ru12 C13 . . . 93.9(5) ? C122 Ru12 C17 . . . 84.6(5) ? C123 Ru12 C13 . . . 91.8(5) ? C123 Ru12 C17 . . . 177.6(5) ? C13 Ru12 C17 . . . 90.4(5) ? Ru11 Ru13 Ru12 . . . 59.58(4) ? Ru11 Ru13 C131 . . . 96.4(5) ? Ru11 Ru13 C132 . . . 95.8(5) ? Ru11 Ru13 C13 . . . 56.0(3) ? Ru11 Ru13 C14 . . . 86.9(3) ? Ru11 Ru13 C15 . . . 121.1(3) ? Ru11 Ru13 C16 . . . 132.3(2) ? Ru11 Ru13 C17 . . . 106.4(3) ? Ru12 Ru13 C131 . . . 107.1(3) ? Ru12 Ru13 C132 . . . 152.9(5) ? Ru12 Ru13 C13 . . . 45.9(3) ? Ru12 Ru13 C14 . . . 75.0(2) ? Ru12 Ru13 C15 . . . 86.1(2) ? Ru12 Ru13 C16 . . . 75.0(2) ? Ru12 Ru13 C17 . . . 47.8(3) ? C131 Ru13 C132 . . . 85.3(7) ? C131 Ru13 C13 . . . 147.1(5) ? C131 Ru13 C14 . . . 176.7(5) ? C131 Ru13 C15 . . . 141.2(6) ? C131 Ru13 C16 . . . 110.9(6) ? C131 Ru13 C17 . . . 94.0(6) ? C132 Ru13 C13 . . . 112.5(6) ? C132 Ru13 C14 . . . 93.8(6) ? C132 Ru13 C15 . . . 99.3(6) ? C132 Ru13 C16 . . . 123.8(6) ? C132 Ru13 C17 . . . 157.7(6) ? C13 Ru13 C14 . . . 36.0(4) ? C13 Ru13 C15 . . . 65.6(4) ? C13 Ru13 C16 . . . 82.8(4) ? C13 Ru13 C17 . . . 79.5(4) ? C14 Ru13 C15 . . . 35.8(4) ? C14 Ru13 C16 . . . 67.0(5) ? C14 Ru13 C17 . . . 85.5(4) ? C15 Ru13 C16 . . . 36.3(5) ? C15 Ru13 C17 . . . 67.6(4) ? C16 Ru13 C17 . . . 36.3(4) ? Ru11 C111 O111 . . . 174.1(13) ? Ru11 C112 O112 . . . 177.7(14) ? Ru11 C113 O113 . . . 177.4(16) ? Ru12 C121 O121 . . . 175.1(11) ? Ru12 C122 O122 . . . 174.4(10) ? Ru12 C123 O123 . . . 168.6(11) ? Ru13 C131 O131 . . . 174.6(9) ? Ru13 C132 O132 . . . 178.1(14) ? C1111 C11 C1121 . . . 117.1(11) ? C1111 C11 C12 . . . 121.7(12) ? C1121 C11 C12 . . . 121.1(12) ? C11 C1111 C1112 . . . 123.3(12) ? C11 C1111 C1116 . . . 119.1(11) ? C1112 C1111 C1116 . . . 117.5(13) ? C1111 C1112 C1113 . . . 122.2(14) ? C1111 C1112 H1112 . . . 118.5 ? C1113 C1112 H1112 . . . 119.2 ? C1112 C1113 C1114 . . . 119.5(14) ? C1112 C1113 H1113 . . . 120.9 ? C1114 C1113 H1113 . . . 119.6 ? C1113 C1114 C1115 . . . 120.0(18) ? C1113 C1114 H1114 . . . 120.5 ? C1115 C1114 H1114 . . . 119 ? C1114 C1115 C1116 . . . 121.6(17) ? C1114 C1115 H1115 . . . 121 ? C1116 C1115 H1115 . . . 117.6 ? C1111 C1116 C1115 . . . 119.2(13) ? C1111 C1116 H1116 . . . 119.4 ? C1115 C1116 H1116 . . . 121.3 ? C11 C1121 C1122 . . . 121.2(9) ? C11 C1121 C1126 . . . 122.9(10) ? C1122 C1121 C1126 . . . 115.9(13) ? C1121 C1122 C1123 . . . 120.7(10) ? C1121 C1122 H1122 . . . 119.8 ? C1123 C1122 H1122 . . . 119.5 ? C1122 C1123 C1124 . . . 120.6(12) ? C1122 C1123 H1123 . . . 119.8 ? C1124 C1123 H1123 . . . 119.6 ? C1123 C1124 C1125 . . . 120.6(16) ? C1123 C1124 H1124 . . . 117.7 ? C1125 C1124 H1124 . . . 121.8 ? C1124 C1125 C1126 . . . 118.1(11) ? C1124 C1125 H1125 . . . 119.6 ? C1126 C1125 H1125 . . . 122.3 ? C1121 C1126 C1125 . . . 124.0(11) ? C1121 C1126 H1126 . . . 117.6 ? C1125 C1126 H1126 . . . 118.4 ? Ru11 C12 C11 . . . 138.0(9) ? Ru11 C12 C13 . . . 86.8(8) ? C11 C12 C13 . . . 134.6(11) ? Ru11 C13 Ru12 . . . 75.7(4) ? Ru11 C13 Ru13 . . . 71.4(3) ? Ru11 C13 C12 . . . 58.2(6) ? Ru11 C13 C14 . . . 128.0(6) ? Ru12 C13 Ru13 . . . 78.2(4) ? Ru12 C13 C12 . . . 113.4(7) ? Ru12 C13 C14 . . . 126.3(9) ? Ru13 C13 C12 . . . 121.1(7) ? Ru13 C13 C14 . . . 69.5(6) ? C12 C13 C14 . . . 119.9(10) ? Ru13 C14 C13 . . . 74.5(7) ? Ru13 C14 C141 . . . 131.2(7) ? Ru13 C14 C15 . . . 71.0(8) ? C13 C14 C141 . . . 120.3(11) ? C13 C14 C15 . . . 124.1(11) ? C141 C14 C15 . . . 115.5(10) ? C14 C141 C142 . . . 118.0(11) ? C14 C141 C146 . . . 123.3(13) ? C142 C141 C146 . . . 118.7(12) ? C141 C142 C143 . . . 120.6(13) ? C141 C142 H142 . . . 119.3 ? C143 C142 H142 . . . 120.1 ? C142 C143 C144 . . . 121.3(16) ? C142 C143 H143 . . . 119.9 ? C144 C143 H143 . . . 118.8 ? C143 C144 C145 . . . 119.9(14) ? C143 C144 H144 . . . 121.2 ? C145 C144 H144 . . . 118.9 ? C144 C145 C146 . . . 120.0(13) ? C144 C145 H145 . . . 120.6 ? C146 C145 H145 . . . 119.4 ? C141 C146 C145 . . . 119.4(14) ? C141 C146 H146 . . . 119.9 ? C145 C146 H146 . . . 120.8 ? Ru13 C15 C14 . . . 73.2(8) ? Ru13 C15 C16 . . . 71.7(8) ? Ru13 C15 H15 . . . 132.5 ? C14 C15 C16 . . . 126.9(10) ? C14 C15 H15 . . . 116.4 ? C16 C15 H15 . . . 116.6 ? Ru13 C16 C15 . . . 72.1(7) ? Ru13 C16 C17 . . . 70.8(7) ? Ru13 C16 H16 . . . 127.1 ? C15 C16 C17 . . . 126.0(11) ? C15 C16 H16 . . . 111.8 ? C17 C16 H16 . . . 121.8 ? Ru12 C17 Ru13 . . . 80.1(4) ? Ru12 C17 C16 . . . 123.8(10) ? Ru12 C17 C171 . . . 117.9(7) ? Ru13 C17 C16 . . . 72.9(6) ? Ru13 C17 C171 . . . 135.0(8) ? C16 C17 C171 . . . 116.0(11) ? C17 C171 C172 . . . 121.7(12) ? C17 C171 C176 . . . 119.0(13) ? C172 C171 C176 . . . 119.3(13) ? C171 C172 C173 . . . 120.0(14) ? C171 C172 H172 . . . 119.6 ? C173 C172 H172 . . . 120.4 ? C172 C173 C174 . . . 121.3(16) ? C172 C173 H173 . . . 119.6 ? C174 C173 H173 . . . 119.1 ? C173 C174 C175 . . . 119.2(16) ? C173 C174 H174 . . . 119.1 ? C175 C174 H174 . . . 121.7 ? C174 C175 C176 . . . 119.3(15) ? C174 C175 H175 . . . 120.3 ? C176 C175 H175 . . . 120.4 ? C171 C176 C175 . . . 120.8(15) ? C171 C176 H176 . . . 117.9 ? C175 C176 H176 . . . 121.3 ? Ru22 Ru21 Ru23 . . . 59.18(4) ? Ru22 Ru21 C211 . . . 91.5(4) ? Ru22 Ru21 C212 . . . 148.1(3) ? Ru22 Ru21 C213 . . . 117.0(4) ? Ru22 Ru21 C22 . . . 72.4(3) ? Ru22 Ru21 C23 . . . 46.0(3) ? Ru23 Ru21 C211 . . . 90.4(4) ? Ru23 Ru21 C212 . . . 89.9(4) ? Ru23 Ru21 C213 . . . 174.8(4) ? Ru23 Ru21 C22 . . . 84.7(3) ? Ru23 Ru21 C23 . . . 53.5(3) ? C211 Ru21 C212 . . . 96.9(6) ? C211 Ru21 C213 . . . 93.3(6) ? C211 Ru21 C22 . . . 163.5(5) ? C211 Ru21 C23 . . . 132.8(5) ? C212 Ru21 C213 . . . 93.3(6) ? C212 Ru21 C22 . . . 98.9(5) ? C212 Ru21 C23 . . . 110.6(4) ? C213 Ru21 C22 . . . 90.7(5) ? C213 Ru21 C23 . . . 121.4(5) ? C22 Ru21 C23 . . . 34.9(4) ? Ru21 Ru22 Ru23 . . . 61.43(4) ? Ru21 Ru22 C221 . . . 105.2(3) ? Ru21 Ru22 C222 . . . 149.1(5) ? Ru21 Ru22 C223 . . . 68.9(4) ? Ru21 Ru22 C23 . . . 58.2(2) ? Ru21 Ru22 C27 . . . 112.9(3) ? Ru23 Ru22 C221 . . . 110.7(4) ? Ru23 Ru22 C222 . . . 126.5(4) ? Ru23 Ru22 C223 . . . 129.9(4) ? Ru23 Ru22 C23 . . . 57.3(4) ? Ru23 Ru22 C27 . . . 52.1(3) ? C221 Ru22 C222 . . . 99.0(6) ? C221 Ru22 C223 . . . 87.2(6) ? C221 Ru22 C23 . . . 162.1(4) ? C221 Ru22 C27 . . . 90.7(6) ? C222 Ru22 C223 . . . 93.8(5) ? C222 Ru22 C23 . . . 98.9(6) ? C222 Ru22 C27 . . . 85.4(5) ? C223 Ru22 C23 . . . 91.9(6) ? C223 Ru22 C27 . . . 177.6(6) ? C23 Ru22 C27 . . . 90.5(5) ? Ru21 Ru23 Ru22 . . . 59.40(4) ? Ru21 Ru23 C231 . . . 90.9(4) ? Ru21 Ru23 C232 . . . 104.6(3) ? Ru21 Ru23 C23 . . . 54.70(19) ? Ru21 Ru23 C24 . . . 84.7(3) ? Ru21 Ru23 C25 . . . 119.3(3) ? Ru21 Ru23 C26 . . . 131.6(4) ? Ru21 Ru23 C27 . . . 106.5(3) ? Ru22 Ru23 C231 . . . 101.8(5) ? Ru22 Ru23 C232 . . . 162.4(4) ? Ru22 Ru23 C23 . . . 46.3(3) ? Ru22 Ru23 C24 . . . 75.1(3) ? Ru22 Ru23 C25 . . . 86.8(4) ? Ru22 Ru23 C26 . . . 75.7(4) ? Ru22 Ru23 C27 . . . 47.6(3) ? C231 Ru23 C232 . . . 84.8(7) ? C231 Ru23 C23 . . . 140.3(5) ? C231 Ru23 C24 . . . 175.5(5) ? C231 Ru23 C25 . . . 148.1(5) ? C231 Ru23 C26 . . . 116.5(6) ? C231 Ru23 C27 . . . 95.3(6) ? C232 Ru23 C23 . . . 119.8(6) ? C232 Ru23 C24 . . . 97.3(5) ? C232 Ru23 C25 . . . 96.3(5) ? C232 Ru23 C26 . . . 116.3(5) ? C232 Ru23 C27 . . . 149.0(5) ? C23 Ru23 C24 . . . 35.3(4) ? C23 Ru23 C25 . . . 65.3(4) ? C23 Ru23 C26 . . . 82.0(4) ? C23 Ru23 C27 . . . 78.9(4) ? C24 Ru23 C25 . . . 35.8(4) ? C24 Ru23 C26 . . . 66.2(5) ? C24 Ru23 C27 . . . 85.1(5) ? C25 Ru23 C26 . . . 35.6(5) ? C25 Ru23 C27 . . . 67.9(5) ? C26 Ru23 C27 . . . 37.2(5) ? Ru21 C211 O211 . . . 173.1(13) ? Ru21 C212 O212 . . . 178.3(12) ? Ru21 C213 O213 . . . 178.4(11) ? Ru22 C221 O221 . . . 179.2(14) ? Ru22 C222 O222 . . . 174.7(15) ? Ru22 C223 O223 . . . 169.7(11) ? Ru23 C231 O231 . . . 174.2(15) ? Ru23 C232 O232 . . . 175.2(14) ? C2111 C21 C2121 . . . 116.7(11) ? C2111 C21 C22 . . . 119.7(9) ? C2121 C21 C22 . . . 123.6(9) ? C21 C2111 C2112 . . . 122.1(12) ? C21 C2111 C2116 . . . 120.1(10) ? C2112 C2111 C2116 . . . 117.9(10) ? C2111 C2112 C2113 . . . 120.6(14) ? C2111 C2112 H2112 . . . 120.0 ? C2113 C2112 H2112 . . . 119.4 ? C2112 C2113 C2114 . . . 119.2(11) ? C2112 C2113 H2113 . . . 121.0 ? C2114 C2113 H2113 . . . 119.8 ? C2113 C2114 C2115 . . . 120.7(11) ? C2113 C2114 H2114 . . . 119.1 ? C2115 C2114 H2114 . . . 120.2 ? C2114 C2115 C2116 . . . 119.3(16) ? C2114 C2115 H2115 . . . 118.8 ? C2116 C2115 H2115 . . . 121.8 ? C2111 C2116 C2115 . . . 122.2(12) ? C2111 C2116 H2116 . . . 118.7 ? C2115 C2116 H2116 . . . 119.1 ? C21 C2121 C2122 . . . 120.3(13) ? C21 C2121 C2126 . . . 122.4(13) ? C2122 C2121 C2126 . . . 117.3(12) ? C2121 C2122 C2123 . . . 118.2(16) ? C2121 C2122 H2122 . . . 119.7 ? C2123 C2122 H2122 . . . 122.1 ? C2122 C2123 C2124 . . . 122.0(19) ? C2122 C2123 H2123 . . . 116 ? C2124 C2123 H2123 . . . 122 ? C2123 C2124 C2125 . . . 120.7(17) ? C2123 C2124 H2124 . . . 115 ? C2125 C2124 H2124 . . . 124 ? C2124 C2125 C2126 . . . 118(2) ? C2124 C2125 H2125 . . . 116.1 ? C2126 C2125 H2125 . . . 126 ? C2121 C2126 C2125 . . . 123.7(17) ? C2121 C2126 H2126 . . . 119.2 ? C2125 C2126 H2126 . . . 117.0 ? Ru21 C22 C21 . . . 137.2(6) ? Ru21 C22 C23 . . . 85.2(7) ? C21 C22 C23 . . . 136.5(8) ? Ru21 C23 Ru22 . . . 75.8(3) ? Ru21 C23 Ru23 . . . 71.8(3) ? Ru21 C23 C22 . . . 59.9(5) ? Ru21 C23 C24 . . . 126.8(8) ? Ru22 C23 Ru23 . . . 76.5(4) ? Ru22 C23 C22 . . . 115.0(8) ? Ru22 C23 C24 . . . 125.7(9) ? Ru23 C23 C22 . . . 123.4(7) ? Ru23 C23 C24 . . . 69.0(7) ? C22 C23 C24 . . . 118.9(12) ? Ru23 C24 C23 . . . 75.7(7) ? Ru23 C24 C241 . . . 131.1(8) ? Ru23 C24 C25 . . . 70.7(7) ? C23 C24 C241 . . . 120.0(11) ? C23 C24 C25 . . . 125.2(13) ? C241 C24 C25 . . . 114.8(11) ? C24 C241 C242 . . . 117.7(11) ? C24 C241 C246 . . . 122.2(10) ? C242 C241 C246 . . . 120.1(14) ? C241 C242 C243 . . . 118.7(12) ? C241 C242 H242 . . . 120.1 ? C243 C242 H242 . . . 121.2 ? C242 C243 C244 . . . 123.0(13) ? C242 C243 H243 . . . 118.4 ? C244 C243 H243 . . . 118.6 ? C243 C244 C245 . . . 118.3(17) ? C243 C244 H244 . . . 120.6 ? C245 C244 H244 . . . 121.2 ? C244 C245 C246 . . . 119.7(13) ? C244 C245 H245 . . . 119.9 ? C246 C245 H245 . . . 120.4 ? C241 C246 C245 . . . 120.1(11) ? C241 C246 H246 . . . 119.8 ? C245 C246 H246 . . . 120.0 ? Ru23 C25 C24 . . . 73.5(6) ? Ru23 C25 C26 . . . 71.9(6) ? Ru23 C25 H25 . . . 131.5 ? C24 C25 C26 . . . 126.4(12) ? C24 C25 H25 . . . 116.8 ? C26 C25 H25 . . . 116.8 ? Ru23 C26 C25 . . . 72.5(6) ? Ru23 C26 C27 . . . 69.6(5) ? Ru23 C26 H26 . . . 127.4 ? C25 C26 C27 . . . 125.7(11) ? C25 C26 H26 . . . 110.0 ? C27 C26 H26 . . . 123.7 ? Ru22 C27 Ru23 . . . 80.3(4) ? Ru22 C27 C26 . . . 124.4(10) ? Ru22 C27 C271 . . . 121.7(10) ? Ru23 C27 C26 . . . 73.2(7) ? Ru23 C27 C271 . . . 132.8(9) ? C26 C27 C271 . . . 112.0(10) ? C27 C271 C272 . . . 125.0(12) ? C27 C271 C276 . . . 118.4(13) ? C272 C271 C276 . . . 116.5(16) ? C271 C272 C273 . . . 120.2(14) ? C271 C272 H272 . . . 119 ? C273 C272 H272 . . . 120 ? C272 C273 C274 . . . 122(2) ? C272 C273 H273 . . . 121.9 ? C274 C273 H273 . . . 116 ? C273 C274 C275 . . . 118(2) ? C273 C274 H274 . . . 125 ? C275 C274 H274 . . . 116.6 ? C274 C275 C276 . . . 121.7(15) ? C274 C275 H275 . . . 120 ? C276 C275 H275 . . . 117.8 ? C271 C276 C275 . . . 121.1(15) ? C271 C276 H276 . . . 119.3 ? C275 C276 H276 . . . 119.6 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1808 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 21 _reflns_limit_k_min -20 _reflns_limit_k_max 19 _reflns_limit_l_min -15 _reflns_limit_l_max 15 _reflns_number_observed ? _reflns_d_resolution_high .842 _reflns_d_resolution_low 15.072 _diffrn_reflns_av_sigmaI/netI .069 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .124 _refine_ls_wR_factor_all .056 _refine_ls_goodness_of_fit_all 1.199 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_br569 _database_code_CSD 175558 _audit_creation_method Xtal3.6 _audit_creation_date 01-08-26 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C33 H30 O8 Ru3 Si2' _chemical_formula_moiety ? _chemical_formula_weight 913.98 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 11.847(7) _cell_length_b 19.100(5) _cell_length_c 17.467(7) _cell_angle_alpha 90.00000 _cell_angle_beta 112.49(4) _cell_angle_gamma 90.00000 _cell_volume 3652(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 18.1 _cell_measurement_theta_max 20.5 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.336 _exptl_crystal_description fragment _exptl_crystal_size_max .38 _exptl_crystal_size_mid .36 _exptl_crystal_size_min .21 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min .63 _exptl_absorpt_correction_T_max .74 _diffrn_reflns_number 6413 _reflns_number_total 6413 _reflns_Friedel_coverage ? _reflns_number_gt 5104 _reflns_threshold_expression 'I > 2sig(I )' _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .036 _refine_ls_wR_factor_ref .038 _refine_ls_goodness_of_fit_ref 1.623 _refine_ls_number_reflns 5109 _refine_ls_number_parameters 416 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .01 _refine_diff_density_min -.457 _refine_diff_density_max .518 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 635(81) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction 'xtal ADDREF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 132 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' Si ? 0 8 .072022 .070984 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 32 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 120 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 12 -1.42 .835999 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 1.07180(4) .50365(2) .72471(3) .0516(2) Uani ? ? 1.00000 ? ? Ru2 .90438(3) .53531(2) .79656(2) .0429(2) Uani ? ? 1.00000 ? ? Ru3 .82115(4) .46280(2) .64755(3) .0517(2) Uani ? ? 1.00000 ? ? C11 1.0296(5) .5875(3) .6570(4) .078(4) Uani ? ? 1.00000 ? ? O11 1.0118(5) .6390(3) .6215(3) .122(4) Uani ? ? 1.00000 ? ? C12 1.1168(6) .4506(4) .6527(4) .086(4) Uani ? ? 1.00000 ? ? O12 1.1426(5) .4184(3) .6059(4) .135(4) Uani ? ? 1.00000 ? ? C13 1.2343(5) .5330(3) .7847(4) .070(3) Uani ? ? 1.00000 ? ? O13 1.3310(4) .5516(2) .8206(3) .093(3) Uani ? ? 1.00000 ? ? C21 .8752(5) .6357(3) .7752(4) .068(3) Uani ? ? 1.00000 ? ? O21 .8755(4) .6945(2) .7649(3) .107(3) Uani ? ? 1.00000 ? ? C22 1.0691(5) .5605(3) .8710(3) .057(3) Uani ? ? 1.00000 ? ? O22 1.1575(3) .5780(2) .9227(2) .074(2) Uani ? ? 1.00000 ? ? C23 .8526(5) .5229(3) .8851(4) .066(3) Uani ? ? 1.00000 ? ? O23 .8217(4) .5111(2) .9381(3) .096(3) Uani ? ? 1.00000 ? ? C31 .7749(5) .5356(3) .5724(4) .073(3) Uani ? ? 1.00000 ? ? O31 .7440(5) .5791(3) .5225(3) .105(3) Uani ? ? 1.00000 ? ? C32 .8321(6) .4109(4) .5601(4) .092(4) Uani ? ? 1.00000 ? ? O32 .8363(5) .3807(3) .5043(3) .144(4) Uani ? ? 1.00000 ? ? C1 1.1716(4) .3842(3) .8699(3) .057(3) Uani ? ? 1.00000 ? ? C111 1.1419(4) .3404(2) .9302(3) .057(3) Uani ? ? 1.00000 ? ? C112 1.0384(5) .3520(3) .9484(4) .069(3) Uani ? ? 1.00000 ? ? C113 1.0089(6) .3088(3) 1.0007(4) .076(4) Uani ? ? 1.00000 ? ? C114 1.0826(6) .2530(3) 1.0381(4) .077(4) Uani ? ? 1.00000 ? ? C115 1.1848(6) .2411(3) 1.0218(4) .081(4) Uani ? ? 1.00000 ? ? C116 1.2146(5) .2834(3) .9697(4) .071(3) Uani ? ? 1.00000 ? ? C121 1.3020(5) .3830(3) .8761(4) .062(3) Uani ? ? 1.00000 ? ? C122 1.3312(5) .3590(4) .8125(4) .088(4) Uani ? ? 1.00000 ? ? C123 1.4523(7) .3594(5) .8191(6) .119(6) Uani ? ? 1.00000 ? ? C124 1.5420(7) .3838(5) .8890(7) .121(6) Uani ? ? 1.00000 ? ? C125 1.5154(6) .4078(4) .9525(5) .105(5) Uani ? ? 1.00000 ? ? C126 1.3956(5) .4070(3) .9477(4) .078(4) Uani ? ? 1.00000 ? ? C2 1.0879(4) .4241(2) .8121(3) .053(3) Uani ? ? 1.00000 ? ? C3 .9608(4) .4347(2) .7891(3) .051(2) Uani ? ? 1.00000 ? ? C4 .8833(5) .3775(2) .7469(3) .059(3) Uani ? ? 1.00000 ? ? C5 .7550(4) .3750(3) .7107(3) .059(3) Uani ? ? 1.00000 ? ? Si5 .68606(16) .28507(9) .67775(14) .0854(11) Uani ? ? 1.00000 ? ? C501 .7696(9) .2389(4) .6239(8) .183(8) Uani ? ? 1.00000 ? ? C502 .7075(7) .2388(3) .7763(5) .126(5) Uani ? ? 1.00000 ? ? C503 .5210(6) .2926(4) .6107(5) .107(5) Uani ? ? 1.00000 ? ? C6 .6816(4) .4360(3) .7017(3) .060(3) Uani ? ? 1.00000 ? ? C7 .7209(4) .5059(3) .7201(3) .053(3) Uani ? ? 1.00000 ? ? Si7 .59211(14) .57202(9) .69911(11) .0692(9) Uani ? ? 1.00000 ? ? C701 .5907(7) .6440(4) .6282(5) .135(6) Uani ? ? 1.00000 ? ? C702 .5976(6) .6108(4) .7977(4) .107(5) Uani ? ? 1.00000 ? ? C703 .4411(6) .5273(4) .6518(5) .123(5) Uani ? ? 1.00000 ? ? H112 .98421 .39170 .92165 .08200 Uiso ? ? 1.00000 ? ? H113 .93416 .31820 1.01086 .09100 Uiso ? ? 1.00000 ? ? H114 1.06329 .22328 1.07737 .09000 Uiso ? ? 1.00000 ? ? H115 1.23737 .20223 1.04850 .09100 Uiso ? ? 1.00000 ? ? H116 1.28670 .27345 .95814 .08000 Uiso ? ? 1.00000 ? ? H122 1.26518 .34219 .76175 .10700 Uiso ? ? 1.00000 ? ? H123 1.47877 .34314 .77644 .15400 Uiso ? ? 1.00000 ? ? H124 1.62716 .38776 .89744 .13500 Uiso ? ? 1.00000 ? ? H125 1.57789 .42595 1.00470 .11500 Uiso ? ? 1.00000 ? ? H126 1.37575 .42349 .99556 .08500 Uiso ? ? 1.00000 ? ? H4 .91711 .33750 .72670 .06900 Uiso ? ? 1.00000 ? ? H501a .74974 .26039 .56957 .25500 Uiso ? ? 1.00000 ? ? H501b .85706 .24773 .65374 .25500 Uiso ? ? 1.00000 ? ? H501c .76526 .18985 .61304 .25500 Uiso ? ? 1.00000 ? ? H502a .78698 .24943 .81840 .15700 Uiso ? ? 1.00000 ? ? H502b .64782 .25463 .79811 .15700 Uiso ? ? 1.00000 ? ? H502c .70026 .18999 .76901 .15700 Uiso ? ? 1.00000 ? ? H503a .46985 .31082 .63878 .13000 Uiso ? ? 1.00000 ? ? H503b .50223 .31999 .56130 .13000 Uiso ? ? 1.00000 ? ? H503c .51012 .24420 .60077 .13000 Uiso ? ? 1.00000 ? ? H6 .58295 .42399 .67503 .07000 Uiso ? ? 1.00000 ? ? H701a .66736 .66869 .65088 .17200 Uiso ? ? 1.00000 ? ? H701b .58456 .62443 .57598 .17200 Uiso ? ? 1.00000 ? ? H701c .52769 .67754 .61706 .17200 Uiso ? ? 1.00000 ? ? H702a .58946 .57382 .83471 .14000 Uiso ? ? 1.00000 ? ? H702b .67487 .63286 .82763 .14000 Uiso ? ? 1.00000 ? ? H702c .53437 .64330 .79009 .14000 Uiso ? ? 1.00000 ? ? H703a .43393 .50493 .60137 .14400 Uiso ? ? 1.00000 ? ? H703b .43472 .49154 .68917 .14400 Uiso ? ? 1.00000 ? ? H703c .37652 .55939 .64166 .14400 Uiso ? ? 1.00000 ? ? 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 Ru1 .0453(2) .0555(3) .0568(3) -.0055(2) .0226(2) -.0038(2) Ru2 .0405(2) .0402(2) .0457(2) .00036(17) .01382(17) -.00057(18) Ru3 .0450(2) .0553(3) .0518(3) -.0025(2) .0151(2) -.0100(2) C11 .062(4) .088(5) .075(4) -.017(3) .017(3) .012(4) O11 .112(4) .115(4) .119(4) -.013(3) .021(3) .058(3) C12 .078(4) .099(5) .094(5) -.026(4) .046(4) -.024(4) O12 .143(5) .155(5) .147(5) -.036(4) .100(4) -.072(4) C13 .063(4) .069(4) .083(4) -.007(3) .036(3) -.005(3) O13 .061(3) .101(3) .109(4) -.022(2) .023(3) -.000(3) C21 .066(4) .061(4) .070(4) .003(3) .018(3) -.001(3) O21 .129(4) .054(3) .126(4) .006(3) .037(3) .012(3) C22 .057(3) .048(3) .064(4) .002(2) .022(3) -.001(3) O22 .060(2) .083(3) .068(3) -.009(2) .013(2) -.011(2) C23 .058(3) .066(4) .067(4) .001(3) .018(3) -.001(3) O23 .109(4) .115(4) .079(3) -.011(3) .053(3) .006(3) C31 .074(4) .084(4) .058(4) -.018(3) .023(3) -.014(3) O31 .121(4) .112(4) .075(3) -.008(3) .030(3) .024(3) C32 .076(4) .104(5) .089(5) .010(4) .024(4) -.024(4) O32 .148(5) .170(6) .105(4) .029(4) .039(4) -.065(4) C1 .048(3) .051(3) .066(4) .000(2) .013(3) -.009(3) C111 .050(3) .045(3) .067(4) -.001(2) .012(3) -.003(3) C112 .067(4) .064(4) .079(4) .013(3) .031(3) .006(3) C113 .084(4) .070(4) .086(4) .005(3) .044(4) .002(4) C114 .088(5) .059(4) .081(4) -.003(3) .029(4) .008(3) C115 .073(4) .054(4) .105(5) .006(3) .022(4) .011(3) C116 .051(3) .059(4) .096(5) .006(3) .020(3) -.003(3) C121 .047(3) .056(3) .084(4) .002(3) .026(3) -.001(3) C122 .061(4) .097(5) .109(5) .005(3) .038(4) -.013(4) C123 .080(5) .142(7) .154(8) .018(5) .064(6) -.011(6) C124 .056(5) .133(7) .177(10) .000(5) .047(6) .003(7) C125 .053(4) .109(6) .128(7) -.006(4) .008(4) -.007(5) C126 .050(3) .084(4) .084(4) -.001(3) .008(3) -.003(3) C2 .045(3) .046(3) .069(3) -.002(2) .021(3) -.007(3) C3 .046(3) .049(3) .053(3) .002(2) .015(2) .001(2) C4 .056(3) .047(3) .076(4) -.004(2) .027(3) -.010(3) C5 .046(3) .054(3) .076(4) -.003(2) .021(3) -.008(3) Si5 .0594(10) .0571(10) .1305(17) -.0115(8) .0261(11) -.0219(11) C501 .156(9) .107(6) .327(14) -.051(6) .140(10) -.126(8) C502 .098(6) .070(4) .171(8) -.013(4) .008(5) .037(5) C503 .072(4) .096(5) .121(6) -.022(4) .002(4) -.008(5) C6 .045(3) .055(3) .077(4) -.001(2) .021(3) -.006(3) C7 .053(3) .053(3) .048(3) -.000(2) .012(2) -.001(2) Si7 .0523(9) .0679(10) .0782(11) .0144(8) .0148(8) -.0003(9) C701 .135(7) .126(7) .146(7) .064(6) .056(6) .075(6) C702 .068(4) .137(6) .113(6) .031(4) .028(4) -.031(5) C703 .056(4) .124(6) .155(7) .025(4) .002(4) -.031(5) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ru1 Ru2 . . 2.7891(13) ? Ru1 Ru3 . . 2.8602(16) ? Ru1 C11 . . 1.940(7) ? Ru1 C12 . . 1.846(8) ? Ru1 C13 . . 1.891(6) ? Ru1 C2 . . 2.110(5) ? Ru1 C3 . . 2.421(6) ? Ru2 Ru3 . . 2.7750(10) ? Ru2 C21 . . 1.959(6) ? Ru2 C22 . . 1.946(5) ? Ru2 C23 . . 1.884(7) ? Ru2 C3 . . 2.055(5) ? Ru2 C7 . . 2.146(5) ? Ru3 C31 . . 1.846(6) ? Ru3 C32 . . 1.867(8) ? Ru3 C3 . . 2.451(4) ? Ru3 C4 . . 2.288(5) ? Ru3 C5 . . 2.304(6) ? Ru3 C6 . . 2.255(6) ? Ru3 C7 . . 2.201(6) ? C11 O11 . . 1.138(8) ? C12 O12 . . 1.153(10) ? C13 O13 . . 1.132(7) ? C21 O21 . . 1.137(7) ? C22 O22 . . 1.141(6) ? C23 O23 . . 1.141(9) ? C31 O31 . . 1.157(8) ? C32 O32 . . 1.150(10) ? C1 C111 . . 1.488(8) ? C1 C121 . . 1.507(8) ? C1 C2 . . 1.348(6) ? C111 C112 . . 1.397(9) ? C111 C116 . . 1.395(7) ? C112 C113 . . 1.372(10) ? C112 H112 . . .989 ? C113 C114 . . 1.373(8) ? C113 H113 . . .984 ? C114 C115 . . 1.364(11) ? C114 H114 . . .983 ? C115 C116 . . 1.362(10) ? C115 H115 . . .967 ? C116 H116 . . .969 ? C121 C122 . . 1.362(11) ? C121 C126 . . 1.395(7) ? C122 C123 . . 1.394(11) ? C122 H122 . . .985 ? C123 C124 . . 1.359(11) ? C123 H123 . . .963 ? C124 C125 . . 1.344(15) ? C124 H124 . . .965 ? C125 C126 . . 1.389(10) ? C125 H125 . . .992 ? C126 H126 . . 1.002 ? C2 C3 . . 1.417(7) ? C3 C4 . . 1.436(6) ? C4 C5 . . 1.407(7) ? C4 H4 . . .988 ? C5 Si5 . . 1.894(5) ? C5 C6 . . 1.425(7) ? Si5 C501 . . 1.831(13) ? Si5 C502 . . 1.863(9) ? Si5 C503 . . 1.861(6) ? C501 H501a . . .977 ? C501 H501b . . .980 ? C501 H501c . . .954 ? C502 H502a . . .969 ? C502 H502b . . .971 ? C502 H502c . . .941 ? C503 H503a . . .978 ? C503 H503b . . .960 ? C503 H503c . . .940 ? C6 C7 . . 1.410(7) ? C6 H6 . . 1.104 ? C7 Si7 . . 1.905(5) ? Si7 C701 . . 1.847(9) ? Si7 C702 . . 1.853(8) ? Si7 C703 . . 1.866(7) ? C701 H701a . . .963 ? C701 H701b . . .962 ? C701 H701c . . .946 ? C702 H702a . . .987 ? C702 H702b . . .960 ? C702 H702c . . .942 ? C703 H703a . . .953 ? C703 H703b . . .968 ? C703 H703c . . .942 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Ru2 Ru1 Ru3 . . . 58.82(4) ? Ru2 Ru1 C11 . . . 91.9(2) ? Ru2 Ru1 C12 . . . 150.0(2) ? Ru2 Ru1 C13 . . . 115.8(2) ? Ru2 Ru1 C2 . . . 73.36(16) ? Ru2 Ru1 C3 . . . 45.79(12) ? Ru3 Ru1 C11 . . . 87.65(17) ? Ru3 Ru1 C12 . . . 92.7(2) ? Ru3 Ru1 C13 . . . 174.5(2) ? Ru3 Ru1 C2 . . . 86.26(12) ? Ru3 Ru1 C3 . . . 54.54(10) ? C11 Ru1 C12 . . . 96.4(3) ? C11 Ru1 C13 . . . 93.7(2) ? C11 Ru1 C2 . . . 165.2(3) ? C11 Ru1 C3 . . . 132.3(2) ? C12 Ru1 C13 . . . 92.4(3) ? C12 Ru1 C2 . . . 97.4(3) ? C12 Ru1 C3 . . . 111.6(3) ? C13 Ru1 C2 . . . 91.2(2) ? C13 Ru1 C3 . . . 121.5(2) ? C2 Ru1 C3 . . . 35.61(17) ? Ru1 Ru2 Ru3 . . . 61.87(3) ? Ru1 Ru2 C21 . . . 103.3(2) ? Ru1 Ru2 C22 . . . 69.5(2) ? Ru1 Ru2 C23 . . . 148.54(16) ? Ru1 Ru2 C3 . . . 57.61(16) ? Ru1 Ru2 C7 . . . 112.87(16) ? Ru3 Ru2 C21 . . . 109.67(17) ? Ru3 Ru2 C22 . . . 131.0(2) ? Ru3 Ru2 C23 . . . 126.65(16) ? Ru3 Ru2 C3 . . . 58.76(12) ? Ru3 Ru2 C7 . . . 51.22(15) ? C21 Ru2 C22 . . . 86.8(2) ? C21 Ru2 C23 . . . 100.9(3) ? C21 Ru2 C3 . . . 160.3(3) ? C21 Ru2 C7 . . . 94.3(2) ? C22 Ru2 C23 . . . 92.3(2) ? C22 Ru2 C3 . . . 90.4(2) ? C22 Ru2 C7 . . . 177.0(2) ? C23 Ru2 C3 . . . 98.7(2) ? C23 Ru2 C7 . . . 84.7(2) ? C3 Ru2 C7 . . . 89.56(18) ? Ru1 Ru3 Ru2 . . . 59.31(2) ? Ru1 Ru3 C31 . . . 95.83(19) ? Ru1 Ru3 C32 . . . 98.4(2) ? Ru1 Ru3 C3 . . . 53.56(13) ? Ru1 Ru3 C4 . . . 82.07(13) ? Ru1 Ru3 C5 . . . 117.08(11) ? Ru1 Ru3 C6 . . . 131.28(12) ? Ru1 Ru3 C7 . . . 108.57(12) ? Ru2 Ru3 C31 . . . 101.1(2) ? Ru2 Ru3 C32 . . . 157.2(2) ? Ru2 Ru3 C3 . . . 45.79(12) ? Ru2 Ru3 C4 . . . 75.42(13) ? Ru2 Ru3 C5 . . . 88.74(14) ? Ru2 Ru3 C6 . . . 76.97(13) ? Ru2 Ru3 C7 . . . 49.46(11) ? C31 Ru3 C32 . . . 85.0(3) ? C31 Ru3 C3 . . . 141.7(2) ? C31 Ru3 C4 . . . 176.5(2) ? C31 Ru3 C5 . . . 145.7(2) ? C31 Ru3 C6 . . . 113.8(3) ? C31 Ru3 C7 . . . 92.8(3) ? C32 Ru3 C3 . . . 118.5(2) ? C32 Ru3 C4 . . . 98.0(3) ? C32 Ru3 C5 . . . 98.5(3) ? C32 Ru3 C6 . . . 120.9(3) ? C32 Ru3 C7 . . . 153.0(2) ? C3 Ru3 C4 . . . 35.07(16) ? C3 Ru3 C5 . . . 65.13(16) ? C3 Ru3 C6 . . . 81.22(18) ? C3 Ru3 C7 . . . 78.81(17) ? C4 Ru3 C5 . . . 35.68(17) ? C4 Ru3 C6 . . . 66.1(2) ? C4 Ru3 C7 . . . 85.3(2) ? C5 Ru3 C6 . . . 36.40(19) ? C5 Ru3 C7 . . . 68.8(2) ? C6 Ru3 C7 . . . 36.87(19) ? Ru1 C11 O11 . . . 175.1(5) ? Ru1 C12 O12 . . . 178.2(5) ? Ru1 C13 O13 . . . 178.9(5) ? Ru2 C21 O21 . . . 170.3(5) ? Ru2 C22 O22 . . . 169.6(6) ? Ru2 C23 O23 . . . 175.8(5) ? Ru3 C31 O31 . . . 176.9(5) ? Ru3 C32 O32 . . . 177.6(6) ? C111 C1 C121 . . . 117.0(4) ? C111 C1 C2 . . . 122.8(5) ? C121 C1 C2 . . . 120.2(5) ? C1 C111 C112 . . . 122.6(4) ? C1 C111 C116 . . . 121.3(5) ? C112 C111 C116 . . . 116.1(6) ? C111 C112 C113 . . . 121.8(5) ? C111 C112 H112 . . . 118.8 ? C113 C112 H112 . . . 119.4 ? C112 C113 C114 . . . 120.3(7) ? C112 C113 H113 . . . 119.1 ? C114 C113 H113 . . . 120.6 ? C113 C114 C115 . . . 118.9(7) ? C113 C114 H114 . . . 120.3 ? C115 C114 H114 . . . 120.7 ? C114 C115 C116 . . . 121.2(5) ? C114 C115 H115 . . . 119.2 ? C116 C115 H115 . . . 119.7 ? C111 C116 C115 . . . 121.7(6) ? C111 C116 H116 . . . 118.5 ? C115 C116 H116 . . . 119.8 ? C1 C121 C122 . . . 121.3(5) ? C1 C121 C126 . . . 120.0(6) ? C122 C121 C126 . . . 118.6(6) ? C121 C122 C123 . . . 120.4(6) ? C121 C122 H122 . . . 118.7 ? C123 C122 H122 . . . 120.9 ? C122 C123 C124 . . . 120.1(10) ? C122 C123 H123 . . . 124.3 ? C124 C123 H123 . . . 115.5 ? C123 C124 C125 . . . 120.6(8) ? C123 C124 H124 . . . 125.2 ? C125 C124 H124 . . . 114.1 ? C124 C125 C126 . . . 120.2(6) ? C124 C125 H125 . . . 123.3 ? C126 C125 H125 . . . 116.4 ? C121 C126 C125 . . . 120.1(7) ? C121 C126 H126 . . . 119.5 ? C125 C126 H126 . . . 120.5 ? Ru1 C2 C1 . . . 141.8(4) ? Ru1 C2 C3 . . . 84.2(3) ? C1 C2 C3 . . . 133.7(6) ? Ru1 C3 Ru2 . . . 76.61(16) ? Ru1 C3 Ru3 . . . 71.90(15) ? Ru1 C3 C2 . . . 60.2(3) ? Ru1 C3 C4 . . . 122.0(4) ? Ru2 C3 Ru3 . . . 75.45(14) ? Ru2 C3 C2 . . . 116.9(3) ? Ru2 C3 C4 . . . 125.8(3) ? Ru3 C3 C2 . . . 123.5(4) ? Ru3 C3 C4 . . . 66.2(3) ? C2 C3 C4 . . . 116.0(4) ? Ru3 C4 C3 . . . 78.7(3) ? Ru3 C4 C5 . . . 72.8(3) ? Ru3 C4 H4 . . . 109.6 ? C3 C4 C5 . . . 128.7(5) ? C3 C4 H4 . . . 120.3 ? C5 C4 H4 . . . 109.3 ? Ru3 C5 C4 . . . 71.5(3) ? Ru3 C5 Si5 . . . 134.5(3) ? Ru3 C5 C6 . . . 69.9(3) ? C4 C5 Si5 . . . 115.7(4) ? C4 C5 C6 . . . 122.1(4) ? Si5 C5 C6 . . . 122.3(4) ? C5 Si5 C501 . . . 109.8(4) ? C5 Si5 C502 . . . 105.0(3) ? C5 Si5 C503 . . . 110.4(3) ? C501 Si5 C502 . . . 109.7(4) ? C501 Si5 C503 . . . 111.0(4) ? C502 Si5 C503 . . . 110.9(4) ? Si5 C501 H501a . . . 108.7 ? Si5 C501 H501b . . . 108.3 ? Si5 C501 H501c . . . 125.3 ? H501a C501 H501b . . . 104.9 ? H501a C501 H501c . . . 104.1 ? H501b C501 H501c . . . 103.9 ? Si5 C502 H502a . . . 110.6 ? Si5 C502 H502b . . . 110.7 ? Si5 C502 H502c . . . 111.9 ? H502a C502 H502b . . . 106.2 ? H502a C502 H502c . . . 108.7 ? H502b C502 H502c . . . 108.6 ? Si5 C503 H503a . . . 114.6 ? Si5 C503 H503b . . . 115.7 ? Si5 C503 H503c . . . 94.5 ? H503a C503 H503b . . . 106.3 ? H503a C503 H503c . . . 112.1 ? H503b C503 H503c . . . 113.7 ? Ru3 C6 C5 . . . 73.7(4) ? Ru3 C6 C7 . . . 69.5(3) ? Ru3 C6 H6 . . . 134.2 ? C5 C6 C7 . . . 127.9(4) ? C5 C6 H6 . . . 112.3 ? C7 C6 H6 . . . 119.7 ? Ru2 C7 Ru3 . . . 79.32(19) ? Ru2 C7 C6 . . . 123.8(3) ? Ru2 C7 Si7 . . . 119.5(2) ? Ru3 C7 C6 . . . 73.6(3) ? Ru3 C7 Si7 . . . 134.9(3) ? C6 C7 Si7 . . . 114.5(4) ? C7 Si7 C701 . . . 115.1(4) ? C7 Si7 C702 . . . 110.2(3) ? C7 Si7 C703 . . . 110.1(3) ? C701 Si7 C702 . . . 108.3(4) ? C701 Si7 C703 . . . 106.4(3) ? C702 Si7 C703 . . . 106.3(4) ? Si7 C701 H701a . . . 108.8 ? Si7 C701 H701b . . . 108.9 ? Si7 C701 H701c . . . 116.4 ? H701a C701 H701b . . . 107.4 ? H701a C701 H701c . . . 107.5 ? H701b C701 H701c . . . 107.5 ? Si7 C702 H702a . . . 110.2 ? Si7 C702 H702b . . . 111.6 ? Si7 C702 H702c . . . 112.9 ? H702a C702 H702b . . . 105.6 ? H702a C702 H702c . . . 107.0 ? H702b C702 H702c . . . 109.2 ? Si7 C703 H703a . . . 110.2 ? Si7 C703 H703b . . . 109.5 ? Si7 C703 H703c . . . 110.9 ? H703a C703 H703b . . . 107.7 ? H703a C703 H703c . . . 109.8 ? H703b C703 H703c . . . 108.6 ? _exptl_crystal_F_000 1808 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 12 -10 -5 -12 10 -5 12 10 5 -12 -10 6 9 8 -6 -9 -8 6 -9 8 -6 9 -8 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min -20 _reflns_limit_l_max 19 _reflns_number_observed ? _reflns_d_resolution_high .84 _reflns_d_resolution_low 12.327 _diffrn_reflns_av_sigmaI/netI .03 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .049 _refine_ls_wR_factor_all .04 _refine_ls_goodness_of_fit_all 1.519 _refine_ls_shift/su_mean .001 data_br570 _database_code_CSD 175559 _audit_creation_method Xtal3.6 _audit_creation_date 01-08-27 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C30 H26 O11 Ru3 Si1' _chemical_formula_moiety ? _chemical_formula_weight 893.83 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 13.398(4) _cell_length_b 13.138(3) _cell_length_c 10.210(4) _cell_angle_alpha 80.98(2) _cell_angle_beta 76.48(3) _cell_angle_gamma 89.61(2) _cell_volume 1724.9(10) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 15.8 _cell_measurement_theta_max 23.4 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.385 _exptl_crystal_description plate _exptl_crystal_size_max .32 _exptl_crystal_size_mid .19 _exptl_crystal_size_min .09 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min .79 _exptl_absorpt_correction_T_max .85 _diffrn_reflns_number 6765 _reflns_number_total 6063 _reflns_Friedel_coverage ? _reflns_number_gt 4326 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 25. _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .077 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .057 _refine_ls_wR_factor_ref .066 _refine_ls_goodness_of_fit_ref 1.63 _refine_ls_number_reflns 4326 _refine_ls_number_parameters 406 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .068 _refine_diff_density_min -1.31 _refine_diff_density_max 1.41 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius software' _computing_cell_refinement 'Enraf Nonius software' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 60 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 22 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 52 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Si ? 0 2 .072 .071 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 6 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 .71356(6) .04438(7) .11457(9) .0434(7) Uani ? ? 1.00000 ? ? Ru2 .68122(6) .19802(7) .27448(8) .0422(7) Uani ? ? 1.00000 ? ? Ru3 .89062(6) .24894(7) .08939(9) .0428(7) Uani ? ? 1.00000 ? ? O0 .8721(5) .0905(5) .0803(6) .043(5) Uani ? ? 1.00000 ? ? C11 .7426(9) -.0755(9) .2333(13) .060(10) Uani ? ? 1.00000 ? ? O11 .7598(8) -.1427(8) .3079(10) .090(9) Uani ? ? 1.00000 ? ? C12 .7347(9) -.0166(10) -.0486(13) .064(11) Uani ? ? 1.00000 ? ? O12 .7425(8) -.0541(11) -.1430(12) .127(13) Uani ? ? 1.00000 ? ? C13 .5717(10) .0139(9) .1568(12) .059(10) Uani ? ? 1.00000 ? ? O13 .4868(7) -.0013(8) .1777(11) .091(10) Uani ? ? 1.00000 ? ? C21 .7452(9) .1110(11) .3996(12) .066(11) Uani ? ? 1.00000 ? ? O21 .7747(8) .0622(9) .4785(10) .106(11) Uani ? ? 1.00000 ? ? O22 .4766(7) .1131(8) .4495(9) .083(8) Uani ? ? 1.00000 ? ? C22 .5533(9) .1452(9) .3788(11) .054(10) Uani ? ? 1.00000 ? ? C23 .6748(9) .3296(11) .3384(12) .060(10) Uani ? ? 1.00000 ? ? O23 .6716(8) .4056(8) .3784(10) .089(9) Uani ? ? 1.00000 ? ? C31 .9239(9) .2207(10) .2622(13) .064(11) Uani ? ? 1.00000 ? ? O31 .9581(8) .2100(9) .3553(9) .094(10) Uani ? ? 1.00000 ? ? C32 .8878(9) .3880(10) .1061(12) .061(11) Uani ? ? 1.00000 ? ? O32 .8835(8) .4724(7) .1176(10) .091(10) Uani ? ? 1.00000 ? ? C33 1.0340(10) .2543(11) -.0086(12) .064(11) Uani ? ? 1.00000 ? ? O33 1.1174(7) .2555(9) -.0556(11) .107(11) Uani ? ? 1.00000 ? ? C1 .5059(7) .2792(8) .0995(10) .040(8) Uani ? ? 1.00000 ? ? C111 .4327(7) .3190(8) .2142(10) .042(8) Uani ? ? 1.00000 ? ? C112 .3450(9) .2738(13) .2785(13) .086(13) Uani ? ? 1.00000 ? ? C113 .2800(8) .3059(10) .3936(13) .062(10) Uani ? ? 1.00000 ? ? C114 .3055(11) .3971(17) .4210(16) .104(17) Uani ? ? 1.00000 ? ? C115 .3918(10) .4478(10) .3602(14) .066(12) Uani ? ? 1.00000 ? ? C116 .4558(8) .4127(9) .2497(12) .057(9) Uani ? ? 1.00000 ? ? C121 .4772(8) .2863(8) -.0347(11) .047(8) Uani ? ? 1.00000 ? ? C122 .3917(9) .3366(10) -.0573(13) .064(11) Uani ? ? 1.00000 ? ? C123 .3688(11) .3472(12) -.1834(17) .086(14) Uani ? ? 1.00000 ? ? C124 .4311(13) .3041(13) -.2873(14) .085(14) Uani ? ? 1.00000 ? ? C125 .5136(12) .2519(12) -.2664(13) .078(13) Uani ? ? 1.00000 ? ? C126 .5385(9) .2413(10) -.1416(11) .058(10) Uani ? ? 1.00000 ? ? C2 .5942(7) .2387(8) .1188(9) .039(7) Uani ? ? 1.00000 ? ? C3 .6846(7) .1976(8) .0558(9) .038(7) Uani ? ? 1.00000 ? ? C4 .7611(7) .2774(8) -.0217(10) .041(8) Uani ? ? 1.00000 ? ? C5 .8512(7) .2678(7) -.1192(9) .037(7) Uani ? ? 1.00000 ? ? Si5 .8999(3) .3706(3) -.2662(3) .054(3) Uani ? ? 1.00000 ? ? C501 1.0383(10) .3597(13) -.3417(14) .097(14) Uani ? ? 1.00000 ? ? C502 .8258(11) .3476(11) -.3936(12) .076(12) Uani ? ? 1.00000 ? ? C503 .8742(10) .5024(10) -.2207(13) .073(12) Uani ? ? 1.00000 ? ? O01 .9875(6) .0386(7) -.1694(8) .078(8) Uani ? ? 1.00000 ? ? C01 .9802(11) .0496(13) -.3065(13) .091(14) Uani ? ? 1.00000 ? ? H0 .90425 .08801 .00000 .06000 Uiso ? ? 1.00000 ? ? H112 .32193 .21422 .24379 .10800 Uiso ? ? 1.00000 ? ? H113 .22017 .26424 .44966 .07900 Uiso ? ? 1.00000 ? ? H114 .25694 .42700 .49017 .12900 Uiso ? ? 1.00000 ? ? H115 .40955 .50842 .39512 .08000 Uiso ? ? 1.00000 ? ? H116 .51574 .45363 .19631 .07200 Uiso ? ? 1.00000 ? ? H122 .34648 .36680 .01644 .08200 Uiso ? ? 1.00000 ? ? H123 .30980 .38430 -.20156 .11000 Uiso ? ? 1.00000 ? ? H124 .41469 .31179 -.37680 .10000 Uiso ? ? 1.00000 ? ? H125 .55529 .22103 -.34078 .09600 Uiso ? ? 1.00000 ? ? H126 .59728 .20105 -.12597 .07400 Uiso ? ? 1.00000 ? ? H4 .73623 .34686 .00000 .05300 Uiso ? ? 1.00000 ? ? H5 .85833 .20860 -.13889 .06200 Uiso ? ? 1.00000 ? ? H501a 1.07764 .36626 -.27615 .14100 Uiso ? ? 1.00000 ? ? H501b 1.06127 .41196 -.41892 .14100 Uiso ? ? 1.00000 ? ? H501c 1.05128 .29374 -.37029 .14100 Uiso ? ? 1.00000 ? ? H502a .84761 .39449 -.47748 .11000 Uiso ? ? 1.00000 ? ? H502b .75354 .35573 -.35942 .11000 Uiso ? ? 1.00000 ? ? H502c .83479 .27858 -.41453 .11000 Uiso ? ? 1.00000 ? ? H503a .89704 .55341 -.29931 .10400 Uiso ? ? 1.00000 ? ? H503b .90905 .51345 -.15272 .10400 Uiso ? ? 1.00000 ? ? H503c .80212 .50899 -.18602 .10400 Uiso ? ? 1.00000 ? ? H01a .96225 .11878 -.34054 .13000 Uiso ? ? 1.00000 ? ? H01b .92987 .00320 -.32085 .13000 Uiso ? ? 1.00000 ? ? H01c 1.06115 .03226 -.36603 .13000 Uiso ? ? 1.00000 ? ? 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 Ru1 .0424(5) .0443(5) .0467(5) .0081(4) -.0108(4) -.0171(4) Ru2 .0404(5) .0554(6) .0352(5) .0134(4) -.0103(4) -.0183(4) Ru3 .0377(5) .0518(6) .0443(5) .0091(4) -.0120(4) -.0201(4) O0 .039(4) .054(5) .040(4) .007(3) -.007(3) -.020(3) C11 .061(8) .044(7) .073(9) .010(6) -.019(7) .002(6) O11 .089(7) .070(7) .107(8) .008(6) -.032(6) .007(6) C12 .050(7) .082(10) .069(8) .011(7) -.018(6) -.032(7) O12 .099(8) .189(13) .124(9) .013(8) -.031(7) -.115(9) C13 .061(8) .052(8) .061(8) -.001(6) -.005(6) -.018(6) O13 .044(5) .092(8) .137(9) -.005(5) -.008(6) -.039(6) C21 .057(8) .094(11) .055(8) .019(7) -.025(6) -.021(7) O21 .112(9) .133(10) .078(7) .038(7) -.050(6) .008(6) O22 .059(6) .098(8) .074(6) .001(5) .005(5) .007(5) C22 .057(8) .065(8) .045(7) .011(6) -.016(6) -.013(6) C23 .062(8) .077(9) .057(7) .022(7) -.030(6) -.033(7) O23 .107(8) .088(7) .097(7) .038(6) -.045(6) -.057(6) C31 .060(8) .076(9) .067(8) .014(7) -.020(7) -.036(7) O31 .105(8) .139(10) .061(6) .023(7) -.048(6) -.041(6) C32 .061(8) .054(8) .073(9) .002(6) -.026(6) -.012(7) O32 .113(8) .059(6) .115(8) .005(6) -.039(6) -.038(6) C33 .062(8) .083(10) .049(7) -.002(7) -.016(6) -.014(7) O33 .042(6) .154(11) .120(9) -.002(6) -.004(6) -.030(7) C1 .032(5) .040(6) .049(6) -.002(5) -.006(5) -.012(5) C111 .035(6) .038(6) .055(7) .007(5) -.014(5) -.012(5) C112 .035(7) .150(15) .072(9) -.008(8) .009(6) -.047(9) C113 .036(7) .071(9) .072(9) .012(6) -.001(6) -.007(7) C114 .051(9) .18(2) .102(12) .055(11) -.030(8) -.089(13) C115 .059(8) .059(8) .096(10) .024(7) -.034(8) -.033(7) C116 .046(7) .049(7) .073(8) .003(6) -.003(6) -.015(6) C121 .044(6) .046(7) .052(7) -.005(5) -.018(5) -.003(5) C122 .048(7) .071(9) .075(9) .007(6) -.022(6) -.004(7) C123 .076(10) .090(11) .104(12) -.010(8) -.065(9) .018(9) C124 .096(12) .101(12) .063(9) -.033(10) -.042(9) .004(8) C125 .093(11) .096(11) .057(8) -.002(9) -.039(8) -.021(7) C126 .063(8) .071(9) .048(7) .010(6) -.024(6) -.015(6) C2 .037(6) .040(6) .041(6) .000(5) -.003(5) -.014(5) C3 .037(6) .047(6) .036(5) .005(5) -.010(4) -.021(5) C4 .039(6) .046(6) .046(6) .014(5) -.016(5) -.019(5) C5 .036(5) .034(6) .042(6) .009(4) -.009(4) -.011(5) Si5 .0500(19) .061(2) .0482(19) .0088(16) -.0067(15) -.0040(16) C501 .061(9) .135(15) .071(9) .007(9) .015(7) .006(9) C502 .093(10) .089(10) .048(7) .012(8) -.022(7) -.013(7) C503 .086(10) .055(8) .080(9) -.002(7) -.023(8) -.011(7) O01 .080(6) .112(8) .047(5) .048(5) -.020(4) -.027(5) C01 .101(11) .124(14) .054(8) .049(10) -.027(8) -.027(8) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ru1 Ru2 . . 2.7602(15) ? Ru1 O0 . . 2.146(7) ? Ru1 C11 . . 1.927(12) ? Ru1 C12 . . 1.921(14) ? Ru1 C13 . . 1.879(13) ? Ru1 C3 . . 2.069(10) ? Ru2 Ru3 . . 3.0067(13) ? Ru2 C21 . . 1.927(13) ? Ru2 C22 . . 1.867(11) ? Ru2 C23 . . 1.935(14) ? Ru2 C2 . . 2.183(10) ? Ru2 C3 . . 2.223(10) ? Ru3 O0 . . 2.117(7) ? Ru3 C31 . . 1.900(14) ? Ru3 C32 . . 1.861(14) ? Ru3 C33 . . 1.943(12) ? Ru3 C4 . . 2.283(11) ? Ru3 C5 . . 2.288(10) ? O0 H0 . . .838 ? C11 O11 . . 1.132(16) ? C12 O12 . . 1.13(2) ? C13 O13 . . 1.121(16) ? C21 O21 . . 1.095(17) ? O22 C22 . . 1.148(14) ? C23 O23 . . 1.134(18) ? C31 O31 . . 1.137(17) ? C32 O32 . . 1.132(17) ? C33 O33 . . 1.107(16) ? C1 C111 . . 1.502(14) ? C1 C121 . . 1.498(16) ? C1 C2 . . 1.337(14) ? C111 C112 . . 1.301(15) ? C111 C116 . . 1.392(17) ? C112 C113 . . 1.410(18) ? C112 H112 . . .987 ? C113 C114 . . 1.34(3) ? C113 H113 . . .981 ? C114 C115 . . 1.31(2) ? C114 H114 . . .972 ? C115 C116 . . 1.389(17) ? C115 H115 . . .974 ? C116 H116 . . .970 ? C121 C122 . . 1.367(17) ? C121 C126 . . 1.411(16) ? C122 C123 . . 1.38(2) ? C122 H122 . . .984 ? C123 C124 . . 1.38(2) ? C123 H123 . . .965 ? C124 C125 . . 1.34(2) ? C124 H124 . . .978 ? C125 C126 . . 1.377(19) ? C125 H125 . . .974 ? C126 H126 . . .976 ? C2 C3 . . 1.381(13) ? C3 C4 . . 1.467(13) ? C4 C5 . . 1.393(12) ? C4 H4 . . 1.009 ? C5 Si5 . . 1.849(9) ? C5 H5 . . .833 ? Si5 C501 . . 1.849(14) ? Si5 C502 . . 1.870(15) ? Si5 C503 . . 1.871(14) ? C501 H501a . . .957 ? C501 H501b . . .953 ? C501 H501c . . .959 ? C502 H502a . . .958 ? C502 H502b . . .961 ? C502 H502c . . .965 ? C503 H503a . . .952 ? C503 H503b . . .951 ? C503 H503c . . .956 ? O01 C01 . . 1.411(16) ? C01 H01a . . .970 ? C01 H01b . . .963 ? C01 H01c . . 1.153 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Ru2 Ru1 O0 . . . 83.70(19) ? Ru2 Ru1 C11 . . . 104.7(4) ? Ru2 Ru1 C12 . . . 157.7(4) ? Ru2 Ru1 C13 . . . 90.5(4) ? Ru2 Ru1 C3 . . . 52.5(3) ? O0 Ru1 C11 . . . 87.2(4) ? O0 Ru1 C12 . . . 93.9(4) ? O0 Ru1 C13 . . . 174.2(4) ? O0 Ru1 C3 . . . 87.4(3) ? C11 Ru1 C12 . . . 97.2(6) ? C11 Ru1 C13 . . . 93.9(5) ? C11 Ru1 C3 . . . 157.0(5) ? C12 Ru1 C13 . . . 91.7(5) ? C12 Ru1 C3 . . . 105.4(5) ? C13 Ru1 C3 . . . 89.3(4) ? Ru1 Ru2 Ru3 . . . 75.49(3) ? Ru1 Ru2 C21 . . . 87.1(4) ? Ru1 Ru2 C22 . . . 95.1(4) ? Ru1 Ru2 C23 . . . 164.0(3) ? Ru1 Ru2 C2 . . . 73.8(3) ? Ru1 Ru2 C3 . . . 47.6(3) ? Ru3 Ru2 C21 . . . 88.6(3) ? Ru3 Ru2 C22 . . . 170.4(4) ? Ru3 Ru2 C23 . . . 92.6(3) ? Ru3 Ru2 C2 . . . 96.6(2) ? Ru3 Ru2 C3 . . . 66.9(2) ? C21 Ru2 C22 . . . 89.0(5) ? C21 Ru2 C23 . . . 103.5(6) ? C21 Ru2 C2 . . . 158.1(5) ? C21 Ru2 C3 . . . 131.5(5) ? C22 Ru2 C23 . . . 97.0(5) ? C22 Ru2 C2 . . . 82.3(4) ? C22 Ru2 C3 . . . 108.3(5) ? C23 Ru2 C2 . . . 97.5(5) ? C23 Ru2 C3 . . . 118.1(4) ? C2 Ru2 C3 . . . 36.5(3) ? Ru2 Ru3 O0 . . . 78.22(16) ? Ru2 Ru3 C31 . . . 79.1(3) ? Ru2 Ru3 C32 . . . 94.4(3) ? Ru2 Ru3 C33 . . . 167.6(4) ? Ru2 Ru3 C4 . . . 67.0(2) ? Ru2 Ru3 C5 . . . 100.5(2) ? O0 Ru3 C31 . . . 92.7(4) ? O0 Ru3 C32 . . . 172.3(4) ? O0 Ru3 C33 . . . 93.0(4) ? O0 Ru3 C4 . . . 87.0(3) ? O0 Ru3 C5 . . . 82.3(3) ? C31 Ru3 C32 . . . 88.2(6) ? C31 Ru3 C33 . . . 92.7(5) ? C31 Ru3 C4 . . . 145.4(4) ? C31 Ru3 C5 . . . 175.0(5) ? C32 Ru3 C33 . . . 94.6(5) ? C32 Ru3 C4 . . . 87.8(5) ? C32 Ru3 C5 . . . 96.8(5) ? C33 Ru3 C4 . . . 121.9(4) ? C33 Ru3 C5 . . . 86.9(4) ? C4 Ru3 C5 . . . 35.5(3) ? Ru1 O0 Ru3 . . . 112.1(3) ? Ru1 O0 H0 . . . 111.7 ? Ru3 O0 H0 . . . 101.0 ? Ru1 C11 O11 . . . 176.5(12) ? Ru1 C12 O12 . . . 176.8(11) ? Ru1 C13 O13 . . . 177.2(11) ? Ru2 C21 O21 . . . 174.3(11) ? Ru2 C22 O22 . . . 176.1(12) ? Ru2 C23 O23 . . . 178.4(11) ? Ru3 C31 O31 . . . 169.6(10) ? Ru3 C32 O32 . . . 178.3(11) ? Ru3 C33 O33 . . . 174.9(12) ? C111 C1 C121 . . . 118.3(9) ? C111 C1 C2 . . . 120.0(10) ? C121 C1 C2 . . . 121.7(9) ? C1 C111 C112 . . . 123.7(11) ? C1 C111 C116 . . . 119.0(8) ? C112 C111 C116 . . . 117.2(11) ? C111 C112 C113 . . . 123.9(15) ? C111 C112 H112 . . . 118.1 ? C113 C112 H112 . . . 118.0 ? C112 C113 C114 . . . 115.3(11) ? C112 C113 H113 . . . 122.4 ? C114 C113 H113 . . . 122.3 ? C113 C114 C115 . . . 123.7(15) ? C113 C114 H114 . . . 117.7 ? C115 C114 H114 . . . 119 ? C114 C115 C116 . . . 119.1(15) ? C114 C115 H115 . . . 118.8 ? C116 C115 H115 . . . 122.1 ? C111 C116 C115 . . . 119.7(10) ? C111 C116 H116 . . . 120.0 ? C115 C116 H116 . . . 120.3 ? C1 C121 C122 . . . 121.1(10) ? C1 C121 C126 . . . 120.5(10) ? C122 C121 C126 . . . 118.4(11) ? C121 C122 C123 . . . 120.6(12) ? C121 C122 H122 . . . 120.0 ? C123 C122 H122 . . . 119.4 ? C122 C123 C124 . . . 119.9(14) ? C122 C123 H123 . . . 121.5 ? C124 C123 H123 . . . 118.5 ? C123 C124 C125 . . . 120.4(15) ? C123 C124 H124 . . . 119.8 ? C125 C124 H124 . . . 119.8 ? C124 C125 C126 . . . 120.6(13) ? C124 C125 H125 . . . 118.7 ? C126 C125 H125 . . . 120.7 ? C121 C126 C125 . . . 120.0(12) ? C121 C126 H126 . . . 119.8 ? C125 C126 H126 . . . 120.2 ? Ru2 C2 C1 . . . 142.4(7) ? Ru2 C2 C3 . . . 73.3(6) ? C1 C2 C3 . . . 144.3(10) ? Ru1 C3 Ru2 . . . 79.9(3) ? Ru1 C3 C2 . . . 119.7(6) ? Ru1 C3 C4 . . . 125.8(7) ? Ru2 C3 C2 . . . 70.1(6) ? Ru2 C3 C4 . . . 105.9(7) ? C2 C3 C4 . . . 112.4(9) ? Ru3 C4 C3 . . . 101.8(6) ? Ru3 C4 C5 . . . 72.4(6) ? Ru3 C4 H4 . . . 102.7 ? C3 C4 C5 . . . 129.2(9) ? C3 C4 H4 . . . 109.0 ? C5 C4 H4 . . . 121.6 ? Ru3 C5 C4 . . . 72.1(6) ? Ru3 C5 Si5 . . . 126.8(5) ? Ru3 C5 H5 . . . 102.6 ? C4 C5 Si5 . . . 122.0(7) ? C4 C5 H5 . . . 113.0 ? Si5 C5 H5 . . . 113.5 ? C5 Si5 C501 . . . 112.2(6) ? C5 Si5 C502 . . . 103.9(5) ? C5 Si5 C503 . . . 112.1(5) ? C501 Si5 C502 . . . 108.9(6) ? C501 Si5 C503 . . . 109.9(7) ? C502 Si5 C503 . . . 109.6(7) ? Si5 C501 H501a . . . 110.5 ? Si5 C501 H501b . . . 110.8 ? Si5 C501 H501c . . . 110.3 ? H501a C501 H501b . . . 108.6 ? H501a C501 H501c . . . 108.1 ? H501b C501 H501c . . . 108.5 ? Si5 C502 H502a . . . 111.6 ? Si5 C502 H502b . . . 111.3 ? Si5 C502 H502c . . . 111.0 ? H502a C502 H502b . . . 107.9 ? H502a C502 H502c . . . 107.6 ? H502b C502 H502c . . . 107.3 ? Si5 C503 H503a . . . 110.1 ? Si5 C503 H503b . . . 110.2 ? Si5 C503 H503c . . . 109.7 ? H503a C503 H503b . . . 109.2 ? H503a C503 H503c . . . 108.7 ? H503b C503 H503c . . . 108.9 ? O01 C01 H01a . . . 112.3 ? O01 C01 H01b . . . 113.3 ? O01 C01 H01c . . . 104.5 ? H01a C01 H01b . . . 106.7 ? H01a C01 H01c . . . 109.7 ? H01b C01 H01c . . . 110.3 ? _exptl_crystal_F_000 880 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 9 8 6 -9 -8 -6 10 0 0 -10 0 0 0 13 0 0 -13 0 0 0 11 0 0 -11 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 11 _reflns_number_observed 4026 _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min ? _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .080 _refine_ls_wR_factor_all .070 _refine_ls_goodness_of_fit_all 1.29 _refine_ls_shift/su_mean .002 data_br781 _database_code_CSD 175560 _audit_creation_method Xtal3.6 _audit_creation_date 01-08-27 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C34 H30 O10 Ru3 Si2' _chemical_formula_moiety ? _chemical_formula_weight 957.99 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 12.1663(6) _cell_length_b 18.6509(9) _cell_length_c 16.5147(8) _cell_angle_alpha 90.00000 _cell_angle_beta 96.1710(10) _cell_angle_gamma 90.00000 _cell_volume 3725.7(3) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6057 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 21.0 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 1.318 _exptl_crystal_description prism _exptl_crystal_size_max .13 _exptl_crystal_size_mid .13 _exptl_crystal_size_min .08 _exptl_crystal_size_rad ? _exptl_crystal_colour red _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .71 _exptl_absorpt_correction_T_max .86 _diffrn_reflns_number 78142 _reflns_number_total 9909 _reflns_Friedel_coverage 0 _reflns_number_gt 6826 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 28.99 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .11 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .033 _refine_ls_wR_factor_ref .029 _refine_ls_goodness_of_fit_ref 1.09 _refine_ls_number_reflns 6826 _refine_ls_number_parameters 562 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .041 _refine_diff_density_min -.879 _refine_diff_density_max .872 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 136 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 120 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 40 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 12 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' Si ? 0 8 .072 .071 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 .46252(2) .193184(16) .148919(18) .01895(15) Uani ? ? 1.00000 ? ? Ru2 .38134(2) .218481(16) -.009794(18) .01911(15) Uani ? ? 1.00000 ? ? Ru3 .25373(2) .092479(16) .03909(2) .02078(15) Uani ? ? 1.00000 ? ? O0 .4048(3) .08866(18) .1138(2) .0258(17) Uani ? ? 1.00000 ? ? C11 .6126(3) .1564(2) .1441(2) .026(2) Uani ? ? 1.00000 ? ? O11 .6990(2) .13560(16) .14009(19) .0419(18) Uani ? ? 1.00000 ? ? C12 .4569(3) .1848(2) .2641(3) .030(2) Uani ? ? 1.00000 ? ? O12 .4536(3) .18685(19) .33242(18) .056(2) Uani ? ? 1.00000 ? ? C13 .5104(3) .2875(2) .1655(2) .024(2) Uani ? ? 1.00000 ? ? O13 .5386(2) .34576(15) .17683(17) .0333(16) Uani ? ? 1.00000 ? ? C21 .4940(3) .1517(2) -.0341(2) .026(2) Uani ? ? 1.00000 ? ? O21 .5667(2) .11547(15) -.04559(17) .0350(16) Uani ? ? 1.00000 ? ? C22 .4752(3) .2979(2) -.0200(2) .024(2) Uani ? ? 1.00000 ? ? O22 .5319(2) .34575(14) -.02686(17) .0336(16) Uani ? ? 1.00000 ? ? C23 .2904(3) .2275(2) -.1131(3) .029(2) Uani ? ? 1.00000 ? ? O23 .2380(3) .23257(16) -.17429(18) .0451(19) Uani ? ? 1.00000 ? ? C31 .3222(3) .0586(2) -.0533(3) .033(2) Uani ? ? 1.00000 ? ? O31 .3526(3) .03225(16) -.1087(2) .050(2) Uani ? ? 1.00000 ? ? C32 .1259(3) .1097(2) -.0335(2) .025(2) Uani ? ? 1.00000 ? ? O32 .0515(2) .12032(15) -.07997(17) .0362(17) Uani ? ? 1.00000 ? ? C33 .2056(3) -.0017(2) .0676(2) .026(2) Uani ? ? 1.00000 ? ? O33 .1776(2) -.05808(15) .07914(18) .0363(17) Uani ? ? 1.00000 ? ? C1 .2621(3) .36024(18) .0624(2) .0177(17) Uani ? ? 1.00000 ? ? C111 .2682(3) .40821(19) -.0100(2) .0201(18) Uani ? ? 1.00000 ? ? C112 .3379(3) .4668(2) -.0077(3) .024(2) Uani ? ? 1.00000 ? ? C113 .3453(4) .5076(2) -.0763(3) .031(2) Uani ? ? 1.00000 ? ? C114 .2824(4) .4918(2) -.1485(3) .033(2) Uani ? ? 1.00000 ? ? C115 .2110(4) .4347(2) -.1513(3) .034(2) Uani ? ? 1.00000 ? ? C116 .2031(3) .3929(2) -.0820(2) .026(2) Uani ? ? 1.00000 ? ? C121 .2078(3) .38865(18) .1332(2) .0202(18) Uani ? ? 1.00000 ? ? C122 .1382(3) .4477(2) .1235(3) .025(2) Uani ? ? 1.00000 ? ? C123 .0776(3) .4707(2) .1858(3) .032(2) Uani ? ? 1.00000 ? ? C124 .0866(4) .4343(2) .2587(3) .032(2) Uani ? ? 1.00000 ? ? C125 .1590(4) .3774(2) .2707(3) .029(2) Uani ? ? 1.00000 ? ? C126 .2191(3) .3547(2) .2090(2) .024(2) Uani ? ? 1.00000 ? ? C2 .2967(3) .29267(18) .0619(2) .0187(18) Uani ? ? 1.00000 ? ? C3 .3044(3) .22962(18) .1074(2) .0176(17) Uani ? ? 1.00000 ? ? C4 .2002(3) .19068(19) .1125(2) .0199(18) Uani ? ? 1.00000 ? ? C5 .1904(3) .1282(2) .1589(2) .0204(19) Uani ? ? 1.00000 ? ? Si5 .05921(8) .09586(6) .19927(7) .0248(5) Uani ? ? 1.00000 ? ? C501 .0975(5) .0172(3) .2646(4) .045(3) Uani ? ? 1.00000 ? ? C502 .0122(4) .1693(3) .2633(3) .037(3) Uani ? ? 1.00000 ? ? C503 -.0490(4) .0700(3) .1174(3) .032(2) Uani ? ? 1.00000 ? ? C6 .0997(3) .22595(18) .0796(2) .0188(18) Uani ? ? 1.00000 ? ? C7 .0138(3) .25645(18) .0585(2) .0215(19) Uani ? ? 1.00000 ? ? Si7 -.12243(8) .30072(6) .03858(7) .0235(5) Uani ? ? 1.00000 ? ? C701 -.1789(4) .3098(3) .1383(3) .039(3) Uani ? ? 1.00000 ? ? C702 -.2105(4) .2425(3) -.0317(4) .037(3) Uani ? ? 1.00000 ? ? C703 -.1076(4) .3914(2) -.0049(3) .034(3) Uani ? ? 1.00000 ? ? H0 .402(4) .067(2) .136(3) .009(14) Uiso ? ? 1.00000 ? ? H112 .381(3) .4760(17) .034(2) .014(10) Uiso ? ? 1.00000 ? ? H113 .386(3) .542(2) -.071(2) .025(12) Uiso ? ? 1.00000 ? ? H114 .283(3) .5203(19) -.189(2) .022(10) Uiso ? ? 1.00000 ? ? H115 .165(3) .4233(18) -.199(2) .025(10) Uiso ? ? 1.00000 ? ? H116 .153(3) .3540(18) -.085(2) .017(9) Uiso ? ? 1.00000 ? ? H122 .129(3) .4713(19) .081(2) .022(11) Uiso ? ? 1.00000 ? ? H123 .035(3) .5098(18) .182(2) .016(10) Uiso ? ? 1.00000 ? ? H124 .051(3) .451(2) .295(3) .043(14) Uiso ? ? 1.00000 ? ? H125 .169(3) .355(2) .315(2) .028(12) Uiso ? ? 1.00000 ? ? H126 .272(3) .315(2) .223(2) .038(12) Uiso ? ? 1.00000 ? ? H5 .253(3) .1137(17) .190(2) .012(9) Uiso ? ? 1.00000 ? ? H501a .036(4) .002(2) .289(3) .049(14) Uiso ? ? 1.00000 ? ? H501b .154(4) .027(2) .305(3) .065(18) Uiso ? ? 1.00000 ? ? H501c .113(4) -.020(2) .236(3) .051(17) Uiso ? ? 1.00000 ? ? H502a -.048(4) .159(2) .285(3) .054(15) Uiso ? ? 1.00000 ? ? H502b -.005(4) .212(2) .233(3) .057(15) Uiso ? ? 1.00000 ? ? H502c .071(4) .175(2) .304(3) .054(15) Uiso ? ? 1.00000 ? ? H503a -.110(4) .049(2) .144(3) .056(14) Uiso ? ? 1.00000 ? ? H503b -.029(3) .031(2) .085(3) .047(13) Uiso ? ? 1.00000 ? ? H503c -.073(3) .106(2) .085(2) .021(11) Uiso ? ? 1.00000 ? ? H701a -.246(4) .335(2) .131(3) .062(16) Uiso ? ? 1.00000 ? ? H701b -.125(4) .336(2) .175(3) .058(16) Uiso ? ? 1.00000 ? ? H701c -.186(3) .265(2) .161(3) .047(14) Uiso ? ? 1.00000 ? ? H702a -.274(4) .260(2) -.050(2) .035(12) Uiso ? ? 1.00000 ? ? H702b -.224(3) .194(3) -.016(3) .052(14) Uiso ? ? 1.00000 ? ? H702c -.175(5) .233(3) -.067(4) .09(2) Uiso ? ? 1.00000 ? ? H703a -.175(4) .399(3) -.029(3) .072(18) Uiso ? ? 1.00000 ? ? H703b -.053(4) .393(2) -.038(3) .058(16) Uiso ? ? 1.00000 ? ? H703c -.083(4) .423(2) .036(3) .058(16) Uiso ? ? 1.00000 ? ? 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 Ru1 .01657(14) .02211(16) .01874(16) .00156(12) .00447(12) .00215(13) Ru2 .02048(15) .02172(16) .01616(16) -.00095(12) .00666(12) .00002(12) Ru3 .01990(15) .01943(15) .02393(17) -.00067(12) .00653(13) -.00062(13) O0 .0236(16) .0227(17) .032(2) .0015(13) .0064(13) .0075(16) C11 .027(2) .027(2) .025(2) .0006(17) .0049(18) .0072(17) O11 .0251(16) .048(2) .054(2) .0097(14) .0127(15) .0077(16) C12 .026(2) .036(2) .029(2) .0100(18) .0055(18) .008(2) O12 .069(2) .081(3) .0201(17) .017(2) .0141(17) .0102(17) C13 .0169(18) .034(2) .021(2) .0040(16) .0045(15) .0034(17) O13 .0313(16) .0307(17) .0379(18) -.0024(13) .0037(13) -.0037(14) C21 .029(2) .030(2) .022(2) -.0071(18) .0088(18) -.0023(17) O21 .0329(17) .0366(17) .0381(18) .0046(13) .0154(14) -.0074(14) C22 .027(2) .031(2) .016(2) .0037(17) .0059(16) -.0007(16) O22 .0366(17) .0313(16) .0356(18) -.0082(13) .0165(14) -.0023(13) C23 .031(2) .031(2) .026(2) -.0002(18) .0087(19) -.0014(18) O23 .051(2) .059(2) .0238(17) -.0004(16) -.0029(15) -.0014(15) C31 .028(2) .030(2) .042(3) -.0085(18) .008(2) -.008(2) O31 .053(2) .049(2) .052(2) -.0141(16) .0281(17) -.0266(17) C32 .027(2) .023(2) .027(2) -.0028(16) .0102(18) -.0041(17) O32 .0348(17) .0402(17) .0327(18) -.0004(14) -.0002(14) -.0018(14) C33 .022(2) .025(2) .030(2) .0011(16) .0049(17) -.0009(18) O33 .0351(17) .0269(16) .047(2) -.0049(13) .0029(14) .0039(14) C1 .0165(17) .0196(19) .018(2) .0001(14) .0045(15) .0035(14) C111 .0217(19) .0215(19) .0181(19) .0047(15) .0062(15) .0012(15) C112 .024(2) .025(2) .024(2) -.0021(16) .0043(18) .0003(17) C113 .035(2) .023(2) .038(3) -.006(2) .011(2) .003(2) C114 .047(3) .031(2) .024(2) .008(2) .013(2) .013(2) C115 .043(3) .040(3) .018(2) .007(2) .001(2) .0024(19) C116 .026(2) .026(2) .026(2) -.0022(17) .0001(18) .0005(17) C121 .023(2) .0185(19) .019(2) -.0043(15) .0015(16) .0003(15) C122 .029(2) .024(2) .024(2) .0033(16) .0063(18) .0057(18) C123 .034(2) .027(2) .035(3) .0088(19) .011(2) -.000(2) C124 .039(3) .029(2) .030(3) -.003(2) .014(2) -.010(2) C125 .041(3) .028(2) .019(2) -.0009(19) .008(2) -.0013(18) C126 .028(2) .023(2) .021(2) .0003(16) .0016(17) -.0010(16) C2 .0168(17) .024(2) .0160(18) -.0033(14) .0068(14) -.0010(15) C3 .0206(18) .021(2) .0121(18) -.0008(14) .0064(15) -.0027(14) C4 .0209(18) .0221(19) .0174(19) .0023(15) .0053(15) -.0017(15) C5 .0172(19) .023(2) .021(2) .0034(15) .0046(16) .0018(16) Si5 .0214(5) .0270(6) .0275(6) .0022(4) .0089(5) .0093(5) C501 .038(3) .042(3) .058(4) .006(2) .018(3) .028(3) C502 .037(3) .050(3) .027(3) .007(2) .013(2) .007(2) C503 .026(2) .027(2) .044(3) -.0014(19) .009(2) .004(2) C6 .0239(19) .0143(18) .019(2) -.0052(15) .0073(16) .0011(15) C7 .024(2) .020(2) .022(2) -.0006(15) .0062(16) .0013(15) Si7 .0196(5) .0232(6) .0282(6) .0037(4) .0051(5) .0037(5) C701 .036(3) .042(3) .041(3) .008(2) .019(2) .009(2) C702 .025(2) .037(3) .047(3) -.001(2) -.003(2) .002(2) C703 .035(3) .032(3) .036(3) .004(2) .009(2) .004(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ru1 Ru2 . . 2.7407(4) ? Ru1 Ru3 . . 3.5042(4) ? Ru1 O0 . . 2.131(3) ? Ru1 C11 . . 1.961(4) ? Ru1 C12 . . 1.917(4) ? Ru1 C13 . . 1.865(4) ? Ru1 C3 . . 2.085(3) ? Ru2 Ru3 . . 2.9756(4) ? Ru2 C21 . . 1.926(4) ? Ru2 C22 . . 1.888(4) ? Ru2 C23 . . 1.938(4) ? Ru2 C2 . . 2.153(4) ? Ru2 C3 . . 2.249(4) ? Ru3 O0 . . 2.102(3) ? Ru3 C31 . . 1.923(5) ? Ru3 C32 . . 1.886(4) ? Ru3 C33 . . 1.925(4) ? Ru3 C4 . . 2.327(4) ? Ru3 C5 . . 2.298(4) ? O0 H0 . . .54(4) ? C11 O11 . . 1.129(5) ? C12 O12 . . 1.134(5) ? C13 O13 . . 1.148(5) ? C21 O21 . . 1.145(5) ? C22 O22 . . 1.142(5) ? C23 O23 . . 1.139(5) ? C31 O31 . . 1.135(6) ? C32 O32 . . 1.139(5) ? C33 O33 . . 1.128(5) ? C1 C111 . . 1.501(5) ? C1 C121 . . 1.500(5) ? C1 C2 . . 1.329(5) ? C111 C112 . . 1.381(5) ? C111 C116 . . 1.386(5) ? C112 C113 . . 1.376(6) ? C112 H112 . . .84(3) ? C113 C114 . . 1.378(6) ? C113 H113 . . .80(4) ? C114 C115 . . 1.371(6) ? C114 H114 . . .85(4) ? C115 C116 . . 1.396(6) ? C115 H115 . . .94(4) ? C116 H116 . . .94(3) ? C121 C122 . . 1.388(5) ? C121 C126 . . 1.396(5) ? C122 C123 . . 1.395(6) ? C122 H122 . . .83(4) ? C123 C124 . . 1.376(6) ? C123 H123 . . .90(3) ? C124 C125 . . 1.379(6) ? C124 H124 . . .84(4) ? C125 C126 . . 1.383(6) ? C125 H125 . . .85(4) ? C126 H126 . . 1.00(4) ? C2 C3 . . 1.394(5) ? C3 C4 . . 1.470(5) ? C4 C5 . . 1.408(5) ? C4 C6 . . 1.443(5) ? C5 Si5 . . 1.893(4) ? C5 H5 . . .91(3) ? Si5 C501 . . 1.850(6) ? Si5 C502 . . 1.858(5) ? Si5 C503 . . 1.847(5) ? C501 H501a . . .94(5) ? C501 H501b . . .92(5) ? C501 H501c . . .87(5) ? C502 H502a . . .88(5) ? C502 H502b . . .95(5) ? C502 H502c . . .93(4) ? C503 H503a . . .98(5) ? C503 H503b . . .95(4) ? C503 H503c . . .88(4) ? C6 C7 . . 1.207(5) ? C7 Si7 . . 1.850(4) ? Si7 C701 . . 1.860(5) ? Si7 C702 . . 1.845(5) ? Si7 C703 . . 1.855(5) ? C701 H701a . . .93(5) ? C701 H701b . . .97(4) ? C701 H701c . . .92(4) ? C702 H702a . . .87(4) ? C702 H702b . . .96(5) ? C702 H702c . . .78(6) ? C703 H703a . . .89(5) ? C703 H703b . . .90(5) ? C703 H703c . . .92(5) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Ru2 Ru1 Ru3 . . . 55.293(10) ? Ru2 Ru1 O0 . . . 79.79(9) ? Ru2 Ru1 C11 . . . 105.23(11) ? Ru2 Ru1 C12 . . . 156.26(12) ? Ru2 Ru1 C13 . . . 93.04(11) ? Ru2 Ru1 C3 . . . 53.48(10) ? Ru3 Ru1 O0 . . . 33.85(8) ? Ru3 Ru1 C11 . . . 114.71(11) ? Ru3 Ru1 C12 . . . 111.66(12) ? Ru3 Ru1 C13 . . . 141.24(11) ? Ru3 Ru1 C3 . . . 54.04(9) ? O0 Ru1 C11 . . . 87.15(14) ? O0 Ru1 C12 . . . 98.63(15) ? O0 Ru1 C13 . . . 172.67(15) ? O0 Ru1 C3 . . . 86.74(12) ? C11 Ru1 C12 . . . 98.32(16) ? C11 Ru1 C13 . . . 93.33(15) ? C11 Ru1 C3 . . . 158.61(15) ? C12 Ru1 C13 . . . 88.54(17) ? C12 Ru1 C3 . . . 102.86(15) ? C13 Ru1 C3 . . . 90.21(14) ? Ru1 Ru2 Ru3 . . . 75.491(11) ? Ru1 Ru2 C21 . . . 84.08(11) ? Ru1 Ru2 C22 . . . 93.50(11) ? Ru1 Ru2 C23 . . . 165.85(13) ? Ru1 Ru2 C2 . . . 74.30(9) ? Ru1 Ru2 C3 . . . 48.18(8) ? Ru3 Ru2 C21 . . . 87.12(12) ? Ru3 Ru2 C22 . . . 168.98(11) ? Ru3 Ru2 C23 . . . 92.43(12) ? Ru3 Ru2 C2 . . . 93.68(9) ? Ru3 Ru2 C3 . . . 64.01(9) ? C21 Ru2 C22 . . . 92.17(16) ? C21 Ru2 C23 . . . 102.93(16) ? C21 Ru2 C2 . . . 157.39(14) ? C21 Ru2 C3 . . . 127.65(14) ? C22 Ru2 C23 . . . 98.44(16) ? C22 Ru2 C2 . . . 82.78(15) ? C22 Ru2 C3 . . . 108.41(14) ? C23 Ru2 C2 . . . 99.61(15) ? C23 Ru2 C3 . . . 119.93(15) ? C2 Ru2 C3 . . . 36.84(12) ? Ru1 Ru3 Ru2 . . . 49.216(8) ? Ru1 Ru3 O0 . . . 34.40(9) ? Ru1 Ru3 C31 . . . 103.59(12) ? Ru1 Ru3 C32 . . . 137.74(11) ? Ru1 Ru3 C33 . . . 125.82(11) ? Ru1 Ru3 C4 . . . 62.38(8) ? Ru1 Ru3 C5 . . . 71.97(9) ? Ru2 Ru3 O0 . . . 74.76(9) ? Ru2 Ru3 C31 . . . 76.14(12) ? Ru2 Ru3 C32 . . . 96.42(12) ? Ru2 Ru3 C33 . . . 165.44(11) ? Ru2 Ru3 C4 . . . 72.72(9) ? Ru2 Ru3 C5 . . . 103.76(9) ? O0 Ru3 C31 . . . 91.63(15) ? O0 Ru3 C32 . . . 171.13(15) ? O0 Ru3 C33 . . . 95.49(14) ? O0 Ru3 C4 . . . 89.82(12) ? O0 Ru3 C5 . . . 81.80(13) ? C31 Ru3 C32 . . . 87.09(17) ? C31 Ru3 C33 . . . 93.65(17) ? C31 Ru3 C4 . . . 147.26(15) ? C31 Ru3 C5 . . . 173.16(15) ? C32 Ru3 C33 . . . 93.35(15) ? C32 Ru3 C4 . . . 86.54(14) ? C32 Ru3 C5 . . . 99.69(15) ? C33 Ru3 C4 . . . 118.76(15) ? C33 Ru3 C5 . . . 85.12(15) ? C4 Ru3 C5 . . . 35.43(13) ? Ru1 O0 Ru3 . . . 111.75(15) ? Ru1 O0 H0 . . . 122(4) ? Ru3 O0 H0 . . . 107(5) ? Ru1 C11 O11 . . . 179.0(4) ? Ru1 C12 O12 . . . 173.4(4) ? Ru1 C13 O13 . . . 178.7(3) ? Ru2 C21 O21 . . . 174.8(3) ? Ru2 C22 O22 . . . 179.4(3) ? Ru2 C23 O23 . . . 179.3(4) ? Ru3 C31 O31 . . . 171.4(4) ? Ru3 C32 O32 . . . 177.1(4) ? Ru3 C33 O33 . . . 175.6(4) ? C111 C1 C121 . . . 118.2(3) ? C111 C1 C2 . . . 121.1(3) ? C121 C1 C2 . . . 120.5(3) ? C1 C111 C112 . . . 122.2(3) ? C1 C111 C116 . . . 119.2(3) ? C112 C111 C116 . . . 118.6(3) ? C111 C112 C113 . . . 120.7(4) ? C111 C112 H112 . . . 121(2) ? C113 C112 H112 . . . 118(2) ? C112 C113 C114 . . . 121.0(4) ? C112 C113 H113 . . . 117(3) ? C114 C113 H113 . . . 122(3) ? C113 C114 C115 . . . 119.1(4) ? C113 C114 H114 . . . 120(2) ? C115 C114 H114 . . . 121(2) ? C114 C115 C116 . . . 120.4(4) ? C114 C115 H115 . . . 122(2) ? C116 C115 H115 . . . 118(2) ? C111 C116 C115 . . . 120.3(4) ? C111 C116 H116 . . . 120(2) ? C115 C116 H116 . . . 120(2) ? C1 C121 C122 . . . 120.3(3) ? C1 C121 C126 . . . 121.9(3) ? C122 C121 C126 . . . 117.6(4) ? C121 C122 C123 . . . 121.5(4) ? C121 C122 H122 . . . 123(3) ? C123 C122 H122 . . . 115(3) ? C122 C123 C124 . . . 119.7(4) ? C122 C123 H123 . . . 123(2) ? C124 C123 H123 . . . 117(2) ? C123 C124 C125 . . . 119.6(4) ? C123 C124 H124 . . . 117(3) ? C125 C124 H124 . . . 124(3) ? C124 C125 C126 . . . 120.6(4) ? C124 C125 H125 . . . 123(3) ? C126 C125 H125 . . . 117(3) ? C121 C126 C125 . . . 120.8(4) ? C121 C126 H126 . . . 123(2) ? C125 C126 H126 . . . 116(2) ? Ru2 C2 C1 . . . 141.6(3) ? Ru2 C2 C3 . . . 75.3(2) ? C1 C2 C3 . . . 143.0(4) ? Ru1 C3 Ru2 . . . 78.34(12) ? Ru1 C3 C2 . . . 117.3(2) ? Ru1 C3 C4 . . . 126.2(2) ? Ru2 C3 C2 . . . 67.8(2) ? Ru2 C3 C4 . . . 116.4(2) ? C2 C3 C4 . . . 116.1(3) ? Ru3 C4 C3 . . . 93.9(2) ? Ru3 C4 C5 . . . 71.1(2) ? Ru3 C4 C6 . . . 115.8(2) ? C3 C4 C5 . . . 124.3(3) ? C3 C4 C6 . . . 117.0(3) ? C5 C4 C6 . . . 117.7(3) ? Ru3 C5 C4 . . . 73.4(2) ? Ru3 C5 Si5 . . . 125.76(18) ? Ru3 C5 H5 . . . 93(2) ? C4 C5 Si5 . . . 125.4(3) ? C4 C5 H5 . . . 116(2) ? Si5 C5 H5 . . . 113(2) ? C5 Si5 C501 . . . 106.8(2) ? C5 Si5 C502 . . . 106.7(2) ? C5 Si5 C503 . . . 112.8(2) ? C501 Si5 C502 . . . 109.1(3) ? C501 Si5 C503 . . . 109.6(2) ? C502 Si5 C503 . . . 111.7(2) ? Si5 C501 H501a . . . 109(3) ? Si5 C501 H501b . . . 113(3) ? Si5 C501 H501c . . . 112(3) ? H501a C501 H501b . . . 108(4) ? H501a C501 H501c . . . 102(4) ? H501b C501 H501c . . . 111(4) ? Si5 C502 H502a . . . 114(3) ? Si5 C502 H502b . . . 113(3) ? Si5 C502 H502c . . . 103(3) ? H502a C502 H502b . . . 104(4) ? H502a C502 H502c . . . 110(4) ? H502b C502 H502c . . . 114(4) ? Si5 C503 H503a . . . 107(3) ? Si5 C503 H503b . . . 114(2) ? Si5 C503 H503c . . . 114(2) ? H503a C503 H503b . . . 102(4) ? H503a C503 H503c . . . 110(3) ? H503b C503 H503c . . . 109(4) ? C4 C6 C7 . . . 174.6(4) ? C6 C7 Si7 . . . 173.2(3) ? C7 Si7 C701 . . . 107.0(2) ? C7 Si7 C702 . . . 107.3(2) ? C7 Si7 C703 . . . 110.7(2) ? C701 Si7 C702 . . . 111.5(2) ? C701 Si7 C703 . . . 108.7(2) ? C702 Si7 C703 . . . 111.5(2) ? Si7 C701 H701a . . . 109(3) ? Si7 C701 H701b . . . 108(3) ? Si7 C701 H701c . . . 110(3) ? H701a C701 H701b . . . 110(4) ? H701a C701 H701c . . . 113(4) ? H701b C701 H701c . . . 107(4) ? Si7 C702 H702a . . . 116(3) ? Si7 C702 H702b . . . 119(3) ? Si7 C702 H702c . . . 106(4) ? H702a C702 H702b . . . 106(4) ? H702a C702 H702c . . . 111(5) ? H702b C702 H702c . . . 96(5) ? Si7 C703 H703a . . . 101(3) ? Si7 C703 H703b . . . 111(3) ? Si7 C703 H703c . . . 110(3) ? H703a C703 H703b . . . 116(5) ? H703a C703 H703c . . . 117(4) ? H703b C703 H703c . . . 103(4) ? _exptl_crystal_F_000 1896 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min -22 _reflns_limit_l_max 22 _reflns_number_observed ? _reflns_d_resolution_high .733 _reflns_d_resolution_low 12.294 _diffrn_reflns_av_sigmaI/netI .105 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .065 _refine_ls_wR_factor_all .032 _refine_ls_goodness_of_fit_all .993 _refine_ls_shift/su_mean .001 data_br789 _database_code_CSD 175561 _audit_creation_method Xtal3.6 _audit_creation_date 01-08-27 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C40 H36 O10 Ru3 Si2' _chemical_formula_moiety ? _chemical_formula_weight 1036.1 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 10.1882(8) _cell_length_b 13.1780(10) _cell_length_c 16.074(2) _cell_angle_alpha 85.469(3) _cell_angle_beta 89.050(3) _cell_angle_gamma 77.973(3) _cell_volume 2104.1(3) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 20.1 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 1.174 _exptl_crystal_description prism _exptl_crystal_size_max .15 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .04 _exptl_crystal_size_rad ? _exptl_crystal_colour orange _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .86 _exptl_absorpt_correction_T_max .89 _diffrn_reflns_number 44024 _reflns_number_total 14196 _reflns_Friedel_coverage 0 _reflns_number_gt 9853 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.55 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .045 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .039 _refine_ls_wR_factor_ref .039 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_number_reflns 9853 _refine_ls_number_parameters 640 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .01 _refine_diff_density_min -.946 _refine_diff_density_max 2.034 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 80 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 72 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 20 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 6 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' Si ? 0 4 .072 .071 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 .33498(3) .95615(2) .860800(10) .01973(16) Uani ? ? 1.00000 ? ? Ru2 .06783(3) .95634(2) .813070(10) .01825(15) Uani ? ? 1.00000 ? ? Ru3 .18145(3) 1.02959(2) .667350(10) .01816(15) Uani ? ? 1.00000 ? ? O0 .3598(2) 1.01006(17) .73696(13) .0223(14) Uani ? ? 1.00000 ? ? C11 .2795(4) 1.0982(3) .8864(2) .029(2) Uani ? ? 1.00000 ? ? O11 .2509(3) 1.1831(2) .90027(17) .042(2) Uani ? ? 1.00000 ? ? C12 .5261(4) .9310(3) .8849(2) .029(2) Uani ? ? 1.00000 ? ? O12 .6362(3) .9125(2) .90261(18) .043(2) Uani ? ? 1.00000 ? ? C13 .2973(4) .9149(3) .97228(19) .026(2) Uani ? ? 1.00000 ? ? O13 .2737(3) .89676(19) 1.04128(14) .0338(17) Uani ? ? 1.00000 ? ? C21 -.0108(4) 1.1020(3) .8195(2) .029(2) Uani ? ? 1.00000 ? ? O21 -.0562(3) 1.1874(2) .82610(16) .040(2) Uani ? ? 1.00000 ? ? C22 .0147(4) .9091(3) .92270(19) .024(2) Uani ? ? 1.00000 ? ? O22 -.0267(3) .8832(2) .98513(15) .0358(18) Uani ? ? 1.00000 ? ? C23 -.0873(4) .9223(3) .7672(2) .025(2) Uani ? ? 1.00000 ? ? O23 -.1776(3) .8982(2) .73965(17) .038(2) Uani ? ? 1.00000 ? ? C31 .1464(3) 1.1812(3) .67251(19) .024(2) Uani ? ? 1.00000 ? ? O31 .1264(3) 1.26792(19) .67977(17) .0395(19) Uani ? ? 1.00000 ? ? C32 .0217(4) 1.0311(2) .61145(19) .024(2) Uani ? ? 1.00000 ? ? O32 -.0763(3) 1.0297(2) .57843(15) .0320(17) Uani ? ? 1.00000 ? ? C33 .2850(4) 1.0247(3) .5656(2) .025(2) Uani ? ? 1.00000 ? ? O33 .3414(3) 1.0226(2) .50456(15) .039(2) Uani ? ? 1.00000 ? ? C1 .3547(3) .7772(2) .82657(17) .0203(19) Uani ? ? 1.00000 ? ? C111 .3553(3) .7178(2) .91008(17) .0203(19) Uani ? ? 1.00000 ? ? C112 .4757(4) .6815(3) .9540(2) .026(2) Uani ? ? 1.00000 ? ? C113 .4762(4) .6270(3) 1.0314(2) .032(2) Uani ? ? 1.00000 ? ? C114 .3590(5) .6079(3) 1.0663(2) .035(3) Uani ? ? 1.00000 ? ? C115 .2411(5) .6404(3) 1.0230(2) .030(2) Uani ? ? 1.00000 ? ? C116 .2387(4) .6938(3) .9445(2) .025(2) Uani ? ? 1.00000 ? ? C121 .4560(3) .7279(2) .76352(18) .022(2) Uani ? ? 1.00000 ? ? C122 .4723(4) .6217(3) .7562(2) .029(2) Uani ? ? 1.00000 ? ? C123 .5508(4) .5744(3) .6927(3) .037(3) Uani ? ? 1.00000 ? ? C124 .6147(5) .6340(3) .6369(2) .039(3) Uani ? ? 1.00000 ? ? C125 .6014(5) .7377(4) .6450(2) .040(3) Uani ? ? 1.00000 ? ? C126 .5215(4) .7856(3) .7077(2) .031(2) Uani ? ? 1.00000 ? ? C2 .2432(3) .8478(2) .79313(17) .0181(18) Uani ? ? 1.00000 ? ? C3 .1937(3) .8774(2) .71114(17) .0177(18) Uani ? ? 1.00000 ? ? C4 .1601(3) .7902(2) .66584(17) .0180(18) Uani ? ? 1.00000 ? ? C5 .1779(3) .7822(2) .58295(18) .022(2) Uani ? ? 1.00000 ? ? Si5 .14251(11) .67276(7) .52462(5) .0251(6) Uani ? ? 1.00000 ? ? C501 -.0411(5) .6768(4) .5302(3) .039(3) Uani ? ? 1.00000 ? ? C502 .1963(5) .6912(3) .4139(2) .036(3) Uani ? ? 1.00000 ? ? C503 .2387(6) .5445(3) .5689(3) .041(3) Uani ? ? 1.00000 ? ? C6 .1112(3) .7111(2) .71671(18) .021(2) Uani ? ? 1.00000 ? ? C7 .0664(4) .6463(2) .75896(19) .024(2) Uani ? ? 1.00000 ? ? Si7 -.01052(11) .55069(7) .81994(6) .0259(6) Uani ? ? 1.00000 ? ? C701 -.0882(5) .4784(3) .7468(3) .041(3) Uani ? ? 1.00000 ? ? C702 -.1397(7) .6259(4) .8862(3) .052(4) Uani ? ? 1.00000 ? ? C703 .1215(6) .4584(4) .8805(3) .050(4) Uani ? ? 1.00000 ? ? C01 .4386(5) 1.2728(4) .6277(4) .052(4) Uani ? ? 1.00000 ? ? C02 .4441(6) 1.3010(4) .7080(4) .066(5) Uani ? ? 1.00000 ? ? C03 .5297(6) 1.2364(4) .7660(3) .056(4) Uani ? ? 1.00000 ? ? C04 .6087(5) 1.1448(3) .7426(3) .041(3) Uani ? ? 1.00000 ? ? C05 .6014(4) 1.1181(3) .6616(2) .035(3) Uani ? ? 1.00000 ? ? C06 .5166(4) 1.1824(3) .6050(3) .039(3) Uani ? ? 1.00000 ? ? H0 .396(4) 1.056(3) .733(2) .026(10) Uiso ? ? 1.00000 ? ? H112 .554(4) .695(3) .933(2) .021(10) Uiso ? ? 1.00000 ? ? H113 .554(4) .600(3) 1.058(2) .030(10) Uiso ? ? 1.00000 ? ? H114 .360(4) .571(3) 1.116(3) .042(12) Uiso ? ? 1.00000 ? ? H115 .157(4) .632(3) 1.043(2) .033(11) Uiso ? ? 1.00000 ? ? H116 .161(4) .715(3) .916(2) .022(9) Uiso ? ? 1.00000 ? ? H122 .430(4) .583(3) .794(2) .027(10) Uiso ? ? 1.00000 ? ? H123 .554(5) .506(4) .687(3) .061(15) Uiso ? ? 1.00000 ? ? H124 .658(4) .608(3) .596(3) .036(11) Uiso ? ? 1.00000 ? ? H125 .648(4) .773(3) .612(3) .048(13) Uiso ? ? 1.00000 ? ? H126 .513(4) .853(3) .708(2) .032(10) Uiso ? ? 1.00000 ? ? H5 .198(3) .841(3) .555(2) .022(9) Uiso ? ? 1.00000 ? ? H501a -.063(5) .634(4) .504(3) .074(17) Uiso ? ? 1.00000 ? ? H501b -.069(5) .662(4) .585(3) .056(14) Uiso ? ? 1.00000 ? ? H501c -.090(4) .746(3) .514(2) .029(10) Uiso ? ? 1.00000 ? ? H502a .181(5) .634(4) .386(3) .062(14) Uiso ? ? 1.00000 ? ? H502b .152(5) .752(4) .393(3) .063(16) Uiso ? ? 1.00000 ? ? H502c .295(6) .691(4) .412(3) .077(18) Uiso ? ? 1.00000 ? ? H503a .211(5) .495(4) .544(3) .077(17) Uiso ? ? 1.00000 ? ? H503b .334(5) .543(4) .565(3) .067(17) Uiso ? ? 1.00000 ? ? H503c .219(5) .529(4) .626(3) .057(14) Uiso ? ? 1.00000 ? ? H701a -.127(4) .424(3) .774(2) .038(11) Uiso ? ? 1.00000 ? ? H701b -.163(5) .521(4) .717(3) .063(15) Uiso ? ? 1.00000 ? ? H701c -.020(5) .453(4) .705(3) .060(15) Uiso ? ? 1.00000 ? ? H702a -.189(5) .586(4) .917(3) .078(17) Uiso ? ? 1.00000 ? ? H702b -.101(5) .673(4) .920(3) .070(16) Uiso ? ? 1.00000 ? ? H702c -.203(6) .667(5) .858(4) .10(3) Uiso ? ? 1.00000 ? ? H703a .082(5) .410(4) .909(3) .068(16) Uiso ? ? 1.00000 ? ? H703b .179(5) .422(4) .845(3) .070(19) Uiso ? ? 1.00000 ? ? H703c .170(5) .488(4) .912(3) .072(17) Uiso ? ? 1.00000 ? ? H01 .387(4) 1.321(4) .590(3) .050(13) Uiso ? ? 1.00000 ? ? H02 .391(5) 1.361(4) .714(3) .061(16) Uiso ? ? 1.00000 ? ? H03 .529(5) 1.248(4) .821(3) .071(16) Uiso ? ? 1.00000 ? ? H04 .670(4) 1.097(3) .783(3) .049(13) Uiso ? ? 1.00000 ? ? H05 .652(4) 1.056(3) .647(3) .046(13) Uiso ? ? 1.00000 ? ? H06 .516(4) 1.163(3) .551(2) .033(10) Uiso ? ? 1.00000 ? ? 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 Ru1 .02440(18) .02146(11) .01576(10) -.00922(11) -.00002(10) -.00433(8) Ru2 .02002(18) .01982(11) .01544(10) -.00474(10) .00390(10) -.00387(8) Ru3 .02170(18) .01869(11) .01508(10) -.00636(10) .00200(10) -.00207(8) O0 .0255(16) .0251(11) .0196(9) -.0125(10) .0012(9) -.0032(8) C11 .039(3) .0286(16) .0226(14) -.0128(16) .0014(15) -.0041(12) O11 .057(2) .0285(13) .0435(15) -.0099(13) .0087(14) -.0112(12) C12 .034(3) .0298(16) .0251(15) -.0132(16) -.0025(16) -.0052(13) O12 .033(2) .0563(18) .0444(16) -.0165(14) -.0087(14) -.0059(14) C13 .034(2) .0252(15) .0221(14) -.0097(15) -.0023(14) -.0068(12) O13 .0502(19) .0363(13) .0184(10) -.0163(12) .0034(11) -.0047(9) C21 .034(3) .0288(16) .0228(15) -.0064(16) .0061(15) -.0013(12) O21 .047(2) .0284(13) .0397(15) .0022(13) .0125(13) -.0057(11) C22 .027(2) .0251(15) .0222(14) -.0049(14) .0039(14) -.0073(12) O22 .043(2) .0389(14) .0262(12) -.0099(13) .0148(12) -.0028(11) C23 .019(2) .0327(17) .0233(14) -.0063(15) .0106(14) -.0049(12) O23 .0262(18) .0483(16) .0433(15) -.0126(13) -.0031(13) -.0053(13) C31 .024(2) .0258(15) .0223(14) -.0058(14) .0015(14) -.0019(12) O31 .046(2) .0251(12) .0481(16) -.0069(12) .0012(14) -.0066(11) C32 .026(2) .0239(14) .0213(13) -.0043(14) .0036(14) -.0022(11) O32 .0234(17) .0419(15) .0299(12) -.0048(12) -.0017(11) -.0038(11) C33 .025(2) .0278(15) .0246(15) -.0113(14) .0020(15) -.0045(12) O33 .044(2) .0543(17) .0262(12) -.0228(14) .0142(13) -.0140(12) C1 .024(2) .0213(13) .0180(12) -.0080(13) .0008(13) -.0045(10) C111 .025(2) .0198(13) .0166(12) -.0059(13) .0026(13) -.0033(10) C112 .025(3) .0274(16) .0234(14) -.0031(15) -.0022(15) -.0033(12) C113 .035(3) .0313(17) .0245(15) .0026(17) -.0080(17) -.0011(13) C114 .052(3) .0319(18) .0207(15) -.0071(18) -.0030(17) .0024(13) C115 .041(3) .0284(17) .0238(15) -.0132(17) .0038(16) .0003(13) C116 .030(2) .0237(15) .0220(14) -.0084(15) -.0013(15) -.0013(11) C121 .018(2) .0280(15) .0192(13) -.0027(14) -.0007(13) -.0049(11) C122 .025(2) .0332(18) .0305(17) -.0063(16) .0040(16) -.0075(14) C123 .031(3) .039(2) .040(2) -.0020(18) .0031(18) -.0181(17) C124 .033(3) .050(2) .0285(18) .007(2) .0067(19) -.0125(17) C125 .033(3) .050(2) .0309(19) .002(2) .0167(19) .0013(17) C126 .030(3) .0319(18) .0308(17) -.0031(17) .0093(17) -.0015(14) C2 .020(2) .0202(13) .0160(11) -.0092(12) .0048(12) -.0043(10) C3 .020(2) .0172(12) .0173(12) -.0055(12) .0027(12) -.0035(10) C4 .018(2) .0190(13) .0177(12) -.0046(12) .0024(12) -.0036(10) C5 .025(2) .0222(14) .0192(13) -.0080(14) .0006(13) -.0034(11) Si5 .0301(7) .0281(4) .0209(4) -.0118(4) .0015(4) -.0096(3) C501 .038(3) .054(3) .0310(19) -.022(2) -.0003(19) -.0082(18) C502 .042(3) .042(2) .0276(17) -.018(2) .0054(18) -.0140(16) C503 .052(4) .031(2) .040(2) -.005(2) -.002(2) -.0136(17) C6 .020(2) .0239(14) .0197(13) -.0048(13) -.0012(13) -.0070(11) C7 .027(2) .0236(14) .0213(13) -.0075(14) .0009(14) -.0036(11) Si7 .0315(7) .0227(4) .0256(4) -.0108(4) -.0003(4) .0002(3) C701 .044(3) .036(2) .049(2) -.018(2) -.012(2) -.0038(18) C702 .064(4) .042(2) .052(3) -.016(3) .028(3) -.003(2) C703 .061(4) .038(2) .053(3) -.018(2) -.024(3) .012(2) C01 .038(3) .043(3) .074(3) -.007(2) -.002(3) .004(2) C02 .049(4) .042(3) .109(5) -.010(3) .031(3) -.028(3) C03 .060(4) .069(3) .050(3) -.030(3) .020(3) -.029(3) C04 .043(3) .049(2) .038(2) -.023(2) .002(2) -.0068(18) C05 .033(3) .038(2) .037(2) -.0141(19) .0090(18) -.0071(16) C06 .035(3) .043(2) .041(2) -.016(2) .0009(19) -.0027(17) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ru1 Ru2 . . 2.8396(5) ? Ru1 Ru3 . . 3.4796(5) ? Ru1 O0 . . 2.089(2) ? Ru1 C11 . . 1.915(3) ? Ru1 C12 . . 1.946(4) ? Ru1 C13 . . 1.888(3) ? Ru1 C1 . . 2.431(3) ? Ru1 C2 . . 2.220(3) ? Ru2 Ru3 . . 2.7886(4) ? Ru2 C21 . . 1.930(3) ? Ru2 C22 . . 1.929(3) ? Ru2 C23 . . 1.905(4) ? Ru2 C2 . . 2.081(3) ? Ru2 C3 . . 2.248(3) ? Ru3 O0 . . 2.108(2) ? Ru3 C31 . . 1.963(3) ? Ru3 C32 . . 1.868(4) ? Ru3 C33 . . 1.929(3) ? Ru3 C3 . . 2.052(3) ? O0 H0 . . .77(4) ? C11 O11 . . 1.134(4) ? C12 O12 . . 1.134(5) ? C13 O13 . . 1.148(4) ? C21 O21 . . 1.136(4) ? C22 O22 . . 1.137(4) ? C23 O23 . . 1.141(5) ? C31 O31 . . 1.134(4) ? C32 O32 . . 1.143(5) ? C33 O33 . . 1.128(4) ? C1 C111 . . 1.499(4) ? C1 C121 . . 1.518(4) ? C1 C2 . . 1.395(4) ? C111 C112 . . 1.400(5) ? C111 C116 . . 1.387(5) ? C112 C113 . . 1.387(5) ? C112 H112 . . .91(4) ? C113 C114 . . 1.372(6) ? C113 H113 . . .90(4) ? C114 C115 . . 1.370(6) ? C114 H114 . . .89(4) ? C115 C116 . . 1.393(4) ? C115 H115 . . .93(4) ? C116 H116 . . .91(3) ? C121 C122 . . 1.388(5) ? C121 C126 . . 1.384(5) ? C122 C123 . . 1.392(5) ? C122 H122 . . .92(4) ? C123 C124 . . 1.388(6) ? C123 H123 . . .91(5) ? C124 C125 . . 1.361(7) ? C124 H124 . . .84(4) ? C125 C126 . . 1.391(6) ? C125 H125 . . .88(5) ? C126 H126 . . .88(4) ? C2 C3 . . 1.415(4) ? C3 C4 . . 1.507(4) ? C4 C5 . . 1.351(4) ? C4 C6 . . 1.439(4) ? C5 Si5 . . 1.879(4) ? C5 H5 . . .93(4) ? Si5 C501 . . 1.861(5) ? Si5 C502 . . 1.866(4) ? Si5 C503 . . 1.862(4) ? C501 H501a . . .80(6) ? C501 H501b . . .94(5) ? C501 H501c . . .96(4) ? C502 H502a . . .96(5) ? C502 H502b . . .88(5) ? C502 H502c . . 1.00(6) ? C503 H503a . . .89(6) ? C503 H503b . . .97(6) ? C503 H503c . . .95(5) ? C6 C7 . . 1.209(5) ? C7 Si7 . . 1.831(4) ? Si7 C701 . . 1.854(5) ? Si7 C702 . . 1.851(6) ? Si7 C703 . . 1.846(5) ? C701 H701a . . .97(4) ? C701 H701b . . .96(5) ? C701 H701c . . .99(5) ? C702 H702a . . .92(6) ? C702 H702b . . 1.00(6) ? C702 H702c . . .86(6) ? C703 H703a . . .91(6) ? C703 H703b . . .90(5) ? C703 H703c . . .88(6) ? C01 C02 . . 1.376(9) ? C01 C06 . . 1.360(6) ? C01 H01 . . .92(4) ? C02 C03 . . 1.395(8) ? C02 H02 . . .88(5) ? C03 C04 . . 1.380(7) ? C03 H03 . . .91(5) ? C04 C05 . . 1.381(6) ? C04 H04 . . 1.00(4) ? C05 C06 . . 1.375(5) ? C05 H05 . . .92(4) ? C06 H06 . . .93(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Ru2 Ru1 Ru3 . . . 51.155(7) ? Ru2 Ru1 O0 . . . 85.33(7) ? Ru2 Ru1 C11 . . . 89.57(12) ? Ru2 Ru1 C12 . . . 169.37(11) ? Ru2 Ru1 C13 . . . 90.69(12) ? Ru2 Ru1 C1 . . . 78.54(8) ? Ru2 Ru1 C2 . . . 46.60(8) ? Ru3 Ru1 O0 . . . 34.19(7) ? Ru3 Ru1 C11 . . . 87.57(10) ? Ru3 Ru1 C12 . . . 126.96(10) ? Ru3 Ru1 C13 . . . 141.67(11) ? Ru3 Ru1 C1 . . . 86.85(7) ? Ru3 Ru1 C2 . . . 58.09(7) ? O0 Ru1 C11 . . . 88.11(11) ? O0 Ru1 C12 . . . 93.30(12) ? O0 Ru1 C13 . . . 174.95(12) ? O0 Ru1 C1 . . . 93.30(9) ? O0 Ru1 C2 . . . 78.92(10) ? C11 Ru1 C12 . . . 100.93(16) ? C11 Ru1 C13 . . . 88.75(14) ? C11 Ru1 C1 . . . 167.86(15) ? C11 Ru1 C2 . . . 134.72(14) ? C12 Ru1 C13 . . . 91.18(15) ? C12 Ru1 C1 . . . 91.03(13) ? C12 Ru1 C2 . . . 122.79(13) ? C13 Ru1 C1 . . . 88.94(12) ? C13 Ru1 C2 . . . 100.58(14) ? C1 Ru1 C2 . . . 34.54(10) ? Ru1 Ru2 Ru3 . . . 76.370(11) ? Ru1 Ru2 C21 . . . 99.50(12) ? Ru1 Ru2 C22 . . . 94.57(11) ? Ru1 Ru2 C23 . . . 164.01(10) ? Ru1 Ru2 C2 . . . 50.83(9) ? Ru1 Ru2 C3 . . . 76.19(9) ? Ru3 Ru2 C21 . . . 82.82(10) ? Ru3 Ru2 C22 . . . 170.75(11) ? Ru3 Ru2 C23 . . . 99.63(10) ? Ru3 Ru2 C2 . . . 73.81(8) ? Ru3 Ru2 C3 . . . 46.57(7) ? C21 Ru2 C22 . . . 97.02(13) ? C21 Ru2 C23 . . . 95.29(16) ? C21 Ru2 C2 . . . 145.46(16) ? C21 Ru2 C3 . . . 129.15(12) ? C22 Ru2 C23 . . . 89.60(15) ? C22 Ru2 C2 . . . 102.08(12) ? C22 Ru2 C3 . . . 133.66(11) ? C23 Ru2 C2 . . . 113.19(14) ? C23 Ru2 C3 . . . 89.77(13) ? C2 Ru2 C3 . . . 37.91(10) ? Ru1 Ru3 Ru2 . . . 52.474(10) ? Ru1 Ru3 O0 . . . 33.84(6) ? Ru1 Ru3 C31 . . . 98.78(9) ? Ru1 Ru3 C32 . . . 141.11(10) ? Ru1 Ru3 C33 . . . 121.28(10) ? Ru1 Ru3 C3 . . . 64.05(9) ? Ru2 Ru3 O0 . . . 86.30(6) ? Ru2 Ru3 C31 . . . 104.64(9) ? Ru2 Ru3 C32 . . . 88.80(10) ? Ru2 Ru3 C33 . . . 158.33(10) ? Ru2 Ru3 C3 . . . 52.72(8) ? O0 Ru3 C31 . . . 91.71(12) ? O0 Ru3 C32 . . . 173.10(11) ? O0 Ru3 C33 . . . 89.72(12) ? O0 Ru3 C3 . . . 82.08(11) ? C31 Ru3 C32 . . . 94.24(14) ? C31 Ru3 C33 . . . 96.76(14) ? C31 Ru3 C3 . . . 156.67(12) ? C32 Ru3 C33 . . . 93.05(15) ? C32 Ru3 C3 . . . 91.08(13) ? C33 Ru3 C3 . . . 105.64(13) ? Ru1 O0 Ru3 . . . 111.97(11) ? Ru1 O0 H0 . . . 112(3) ? Ru3 O0 H0 . . . 116(3) ? Ru1 C11 O11 . . . 177.5(4) ? Ru1 C12 O12 . . . 176.1(3) ? Ru1 C13 O13 . . . 175.3(3) ? Ru2 C21 O21 . . . 177.7(3) ? Ru2 C22 O22 . . . 174.6(3) ? Ru2 C23 O23 . . . 177.5(3) ? Ru3 C31 O31 . . . 176.5(3) ? Ru3 C32 O32 . . . 178.2(3) ? Ru3 C33 O33 . . . 177.6(3) ? Ru1 C1 C111 . . . 103.67(19) ? Ru1 C1 C121 . . . 122.2(2) ? Ru1 C1 C2 . . . 64.44(17) ? C111 C1 C121 . . . 116.0(2) ? C111 C1 C2 . . . 123.8(3) ? C121 C1 C2 . . . 115.6(2) ? C1 C111 C112 . . . 120.3(3) ? C1 C111 C116 . . . 121.3(3) ? C112 C111 C116 . . . 118.3(3) ? C111 C112 C113 . . . 120.3(4) ? C111 C112 H112 . . . 121(2) ? C113 C112 H112 . . . 119(2) ? C112 C113 C114 . . . 120.6(4) ? C112 C113 H113 . . . 121(2) ? C114 C113 H113 . . . 118(2) ? C113 C114 C115 . . . 119.6(3) ? C113 C114 H114 . . . 120(3) ? C115 C114 H114 . . . 120(3) ? C114 C115 C116 . . . 120.6(4) ? C114 C115 H115 . . . 125(2) ? C116 C115 H115 . . . 114(2) ? C111 C116 C115 . . . 120.4(3) ? C111 C116 H116 . . . 119(2) ? C115 C116 H116 . . . 121(2) ? C1 C121 C122 . . . 118.0(3) ? C1 C121 C126 . . . 122.7(3) ? C122 C121 C126 . . . 118.9(3) ? C121 C122 C123 . . . 120.6(4) ? C121 C122 H122 . . . 119(2) ? C123 C122 H122 . . . 120(2) ? C122 C123 C124 . . . 119.4(4) ? C122 C123 H123 . . . 119(3) ? C124 C123 H123 . . . 122(3) ? C123 C124 C125 . . . 120.1(4) ? C123 C124 H124 . . . 121(3) ? C125 C124 H124 . . . 119(3) ? C124 C125 C126 . . . 120.7(4) ? C124 C125 H125 . . . 119(3) ? C126 C125 H125 . . . 120(3) ? C121 C126 C125 . . . 120.2(4) ? C121 C126 H126 . . . 123(2) ? C125 C126 H126 . . . 116(2) ? Ru1 C2 Ru2 . . . 82.57(10) ? Ru1 C2 C1 . . . 81.0(2) ? Ru1 C2 C3 . . . 120.0(2) ? Ru2 C2 C1 . . . 148.6(2) ? Ru2 C2 C3 . . . 77.49(17) ? C1 C2 C3 . . . 133.9(3) ? Ru2 C3 Ru3 . . . 80.71(10) ? Ru2 C3 C2 . . . 64.61(16) ? Ru2 C3 C4 . . . 124.5(2) ? Ru3 C3 C2 . . . 117.2(2) ? Ru3 C3 C4 . . . 128.1(2) ? C2 C3 C4 . . . 114.6(2) ? C3 C4 C5 . . . 123.5(3) ? C3 C4 C6 . . . 116.1(2) ? C5 C4 C6 . . . 120.4(3) ? C4 C5 Si5 . . . 124.9(3) ? C4 C5 H5 . . . 113(2) ? Si5 C5 H5 . . . 122(2) ? C5 Si5 C501 . . . 108.1(2) ? C5 Si5 C502 . . . 108.7(2) ? C5 Si5 C503 . . . 111.38(19) ? C501 Si5 C502 . . . 110.4(2) ? C501 Si5 C503 . . . 110.6(2) ? C502 Si5 C503 . . . 107.7(2) ? Si5 C501 H501a . . . 113(4) ? Si5 C501 H501b . . . 112(3) ? Si5 C501 H501c . . . 110(2) ? H501a C501 H501b . . . 104(5) ? H501a C501 H501c . . . 112(4) ? H501b C501 H501c . . . 105(3) ? Si5 C502 H502a . . . 108(3) ? Si5 C502 H502b . . . 108(3) ? Si5 C502 H502c . . . 110(3) ? H502a C502 H502b . . . 114(4) ? H502a C502 H502c . . . 108(4) ? H502b C502 H502c . . . 109(5) ? Si5 C503 H503a . . . 108(3) ? Si5 C503 H503b . . . 110(3) ? Si5 C503 H503c . . . 113(3) ? H503a C503 H503b . . . 115(4) ? H503a C503 H503c . . . 103(5) ? H503b C503 H503c . . . 107(4) ? C4 C6 C7 . . . 178.1(3) ? C6 C7 Si7 . . . 176.8(3) ? C7 Si7 C701 . . . 108.49(19) ? C7 Si7 C702 . . . 106.2(2) ? C7 Si7 C703 . . . 108.9(2) ? C701 Si7 C702 . . . 110.8(3) ? C701 Si7 C703 . . . 109.0(2) ? C702 Si7 C703 . . . 113.3(2) ? Si7 C701 H701a . . . 113(2) ? Si7 C701 H701b . . . 114(3) ? Si7 C701 H701c . . . 108(3) ? H701a C701 H701b . . . 102(4) ? H701a C701 H701c . . . 113(4) ? H701b C701 H701c . . . 107(4) ? Si7 C702 H702a . . . 114(3) ? Si7 C702 H702b . . . 111(3) ? Si7 C702 H702c . . . 113(4) ? H702a C702 H702b . . . 113(5) ? H702a C702 H702c . . . 100(6) ? H702b C702 H702c . . . 105(5) ? Si7 C703 H703a . . . 108(3) ? Si7 C703 H703b . . . 110(3) ? Si7 C703 H703c . . . 115(3) ? H703a C703 H703b . . . 105(5) ? H703a C703 H703c . . . 113(5) ? H703b C703 H703c . . . 106(5) ? C02 C01 C06 . . . 120.0(5) ? C02 C01 H01 . . . 117(3) ? C06 C01 H01 . . . 123(3) ? C01 C02 C03 . . . 119.8(5) ? C01 C02 H02 . . . 110(3) ? C03 C02 H02 . . . 130(3) ? C02 C03 C04 . . . 119.9(5) ? C02 C03 H03 . . . 123(3) ? C04 C03 H03 . . . 117(3) ? C03 C04 C05 . . . 119.3(4) ? C03 C04 H04 . . . 121(3) ? C05 C04 H04 . . . 119(3) ? C04 C05 C06 . . . 120.3(4) ? C04 C05 H05 . . . 119(3) ? C06 C05 H05 . . . 121(3) ? C01 C06 C05 . . . 120.7(4) ? C01 C06 H06 . . . 121(2) ? C05 C06 H06 . . . 118(2) ? _exptl_crystal_F_000 1032 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 13 _reflns_limit_k_min -21 _reflns_limit_k_max 22 _reflns_limit_l_min -27 _reflns_limit_l_max 27 _reflns_number_observed ? _reflns_d_resolution_high .583 _reflns_d_resolution_low 12.817 _diffrn_reflns_av_sigmaI/netI .095 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .069 _refine_ls_wR_factor_all .043 _refine_ls_goodness_of_fit_all 1.064 _refine_ls_shift/su_mean .001 data_br800 _database_code_CSD 175562 _audit_creation_method Xtal3.6 _audit_creation_date 01-08-28 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C50 H34 O10 Ru3' _chemical_formula_moiety ? _chemical_formula_weight 1098.02 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 10.8403(10) _cell_length_b 11.3445(10) _cell_length_c 19.726(2) _cell_angle_alpha 82.429(2) _cell_angle_beta 88.921(2) _cell_angle_gamma 68.909(2) _cell_volume 2242.6(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 20.2 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 1.056 _exptl_crystal_description prism _exptl_crystal_size_max .24 _exptl_crystal_size_mid .23 _exptl_crystal_size_min .2 _exptl_crystal_size_rad ? _exptl_crystal_colour orange _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .66 _exptl_absorpt_correction_T_max .83 _diffrn_reflns_number 46051 _reflns_number_total 11802 _reflns_Friedel_coverage 0 _reflns_number_gt 9191 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 28.9 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .036 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .033 _refine_ls_wR_factor_ref .038 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_number_reflns 9191 _refine_ls_number_parameters 568 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .008 _refine_diff_density_min -.709 _refine_diff_density_max 1.582 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 100 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 68 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 20 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 6 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 .96504(2) .11730(2) .702952(11) .02269(15) Uani ? ? 1.00000 ? ? Ru2 .97264(2) .36252(2) .660932(11) .02459(16) Uani ? ? 1.00000 ? ? Ru3 .73514(2) .37331(2) .603672(11) .02823(17) Uani ? ? 1.00000 ? ? C11 1.0404(3) .0698(3) .61779(15) .035(2) Uani ? ? 1.00000 ? ? O11 1.0824(3) .0379(3) .56734(12) .057(2) Uani ? ? 1.00000 ? ? C12 1.1381(3) .0604(3) .74238(14) .029(2) Uani ? ? 1.00000 ? ? O12 1.2444(2) .0207(2) .76289(12) .0391(18) Uani ? ? 1.00000 ? ? C13 .9480(3) -.0424(3) .74180(15) .031(2) Uani ? ? 1.00000 ? ? O13 .9484(2) -.1390(2) .76450(13) .047(2) Uani ? ? 1.00000 ? ? C21 1.0248(4) .3436(3) .56826(16) .040(3) Uani ? ? 1.00000 ? ? O21 1.0613(3) .3308(3) .51418(12) .061(3) Uani ? ? 1.00000 ? ? C22 .9566(3) .5369(3) .65197(15) .034(2) Uani ? ? 1.00000 ? ? O22 .9495(3) .6396(2) .65046(13) .049(2) Uani ? ? 1.00000 ? ? C23 1.1474(3) .3156(3) .70147(16) .033(2) Uani ? ? 1.00000 ? ? O23 1.2508(2) .2944(2) .72234(13) .048(2) Uani ? ? 1.00000 ? ? C31 .7786(4) .3115(3) .51498(16) .044(3) Uani ? ? 1.00000 ? ? O31 .8133(3) .2689(3) .46575(13) .070(3) Uani ? ? 1.00000 ? ? C32 .7048(3) .5417(3) .56651(15) .038(2) Uani ? ? 1.00000 ? ? O32 .6881(3) .6443(2) .54389(13) .053(2) Uani ? ? 1.00000 ? ? C33 .5495(3) .4020(3) .59829(16) .039(2) Uani ? ? 1.00000 ? ? O33 .4385(3) .4255(3) .59221(14) .057(2) Uani ? ? 1.00000 ? ? C1 .8795(2) .2225(2) .80138(13) .0204(17) Uani ? ? 1.00000 ? ? C111 .9965(3) .1836(3) .85032(13) .0234(18) Uani ? ? 1.00000 ? ? C112 1.0671(3) .2627(3) .85660(14) .029(2) Uani ? ? 1.00000 ? ? C113 1.1755(3) .2237(4) .90238(17) .040(3) Uani ? ? 1.00000 ? ? C114 1.2118(3) .1070(4) .94189(16) .044(3) Uani ? ? 1.00000 ? ? C115 1.1406(3) .0282(3) .93814(15) .040(2) Uani ? ? 1.00000 ? ? C116 1.0328(3) .0669(3) .89283(14) .030(2) Uani ? ? 1.00000 ? ? C121 .7555(3) .2151(2) .83452(13) .0220(18) Uani ? ? 1.00000 ? ? C122 .6632(3) .1803(3) .80201(14) .028(2) Uani ? ? 1.00000 ? ? C123 .5501(3) .1776(3) .83513(17) .034(2) Uani ? ? 1.00000 ? ? C124 .5265(3) .2101(3) .90061(17) .034(2) Uani ? ? 1.00000 ? ? C125 .6161(3) .2458(3) .93285(15) .035(2) Uani ? ? 1.00000 ? ? C126 .7305(3) .2484(3) .90037(14) .029(2) Uani ? ? 1.00000 ? ? C2 .8674(3) .3060(2) .74112(13) .0208(18) Uani ? ? 1.00000 ? ? C3 .7659(3) .4051(2) .70213(13) .0219(18) Uani ? ? 1.00000 ? ? C4 .6872(3) .5175(2) .73677(13) .0212(17) Uani ? ? 1.00000 ? ? C41 .5425(3) .5752(3) .71901(14) .0243(19) Uani ? ? 1.00000 ? ? C42 .4907(3) .6934(3) .67874(15) .032(2) Uani ? ? 1.00000 ? ? C43 .3552(3) .7497(3) .66441(17) .046(3) Uani ? ? 1.00000 ? ? C44 .2711(3) .6897(4) .6900(2) .051(3) Uani ? ? 1.00000 ? ? C45 .3216(3) .5729(4) .7296(2) .047(3) Uani ? ? 1.00000 ? ? C46 .4567(3) .5149(3) .74401(17) .037(2) Uani ? ? 1.00000 ? ? C5 .7434(3) .5640(3) .78167(13) .0233(18) Uani ? ? 1.00000 ? ? C51 .6825(3) .6691(2) .82281(13) .0231(18) Uani ? ? 1.00000 ? ? C52 .5493(3) .7155(3) .83969(15) .030(2) Uani ? ? 1.00000 ? ? C53 .5010(3) .8145(3) .87891(15) .033(2) Uani ? ? 1.00000 ? ? C54 .5836(3) .8694(3) .90229(15) .034(2) Uani ? ? 1.00000 ? ? C55 .7154(3) .8250(3) .88624(17) .037(3) Uani ? ? 1.00000 ? ? C56 .7647(3) .7252(3) .84776(14) .028(2) Uani ? ? 1.00000 ? ? O0 .7790(2) .18591(18) .65402(10) .0280(14) Uani ? ? 1.00000 ? ? C101 .7093(4) .5123(3) 1.0114(2) .048(3) Uani ? ? 1.00000 ? ? C102 .8379(4) .4681(3) .99078(17) .044(3) Uani ? ? 1.00000 ? ? C103 .9295(3) .3612(4) 1.02582(18) .044(3) Uani ? ? 1.00000 ? ? C104 .8939(3) .2966(3) 1.08185(17) .040(3) Uani ? ? 1.00000 ? ? C105 .7653(4) .3404(4) 1.10282(19) .050(3) Uani ? ? 1.00000 ? ? C106 .6725(4) .4485(4) 1.0675(2) .053(3) Uani ? ? 1.00000 ? ? C201 .6605(6) .0260(5) .5478(2) .067(4) Uani ? ? 1.00000 ? ? C202 .7328(4) -.0653(4) .5960(3) .058(4) Uani ? ? 1.00000 ? ? C203 .6857(6) -.0839(5) .6569(2) .070(5) Uani ? ? 1.00000 ? ? C204 .5667(8) -.0102(7) .6732(3) .098(7) Uani ? ? 1.00000 ? ? C205 .4870(6) .0858(7) .6270(6) .126(8) Uani ? ? 1.00000 ? ? C206 .5362(7) .1032(5) .5612(4) .098(6) Uani ? ? 1.00000 ? ? H112 1.04134 .34398 .83099 .02800 Uiso ? ? 1.00000 ? ? H113 1.22313 .27941 .90518 .06400 Uiso ? ? 1.00000 ? ? H114 1.28428 .07934 .96978 .04900 Uiso ? ? 1.00000 ? ? H115 1.16393 -.05230 .96557 .03900 Uiso ? ? 1.00000 ? ? H116 .98783 .01557 .88862 .01700 Uiso ? ? 1.00000 ? ? H122 .67935 .15551 .76040 .02400 Uiso ? ? 1.00000 ? ? H123 .48744 .15361 .81426 .03600 Uiso ? ? 1.00000 ? ? H124 .44829 .21289 .92273 .02600 Uiso ? ? 1.00000 ? ? H125 .60088 .27990 .97632 .04500 Uiso ? ? 1.00000 ? ? H126 .79218 .27207 .92415 .03200 Uiso ? ? 1.00000 ? ? H42 .55280 .73320 .66169 .03900 Uiso ? ? 1.00000 ? ? H43 .32109 .82463 .64128 .05600 Uiso ? ? 1.00000 ? ? H44 .18109 .72565 .67713 .05400 Uiso ? ? 1.00000 ? ? H45 .26915 .53292 .74938 .06700 Uiso ? ? 1.00000 ? ? H46 .49186 .43666 .77110 .04400 Uiso ? ? 1.00000 ? ? H5 .83204 .52983 .78674 .03000 Uiso ? ? 1.00000 ? ? H52 .49326 .68035 .82401 .03400 Uiso ? ? 1.00000 ? ? H53 .41866 .84550 .89285 .05600 Uiso ? ? 1.00000 ? ? H54 .54473 .93705 .92933 .03100 Uiso ? ? 1.00000 ? ? H55 .77689 .86096 .90036 .04800 Uiso ? ? 1.00000 ? ? H56 .85350 .70066 .83788 .02300 Uiso ? ? 1.00000 ? ? H0 .74128 .13713 .63598 .00100 Uiso ? ? 1.00000 ? ? H101 .65008 .58724 .98977 .05400 Uiso ? ? 1.00000 ? ? H102 .86516 .50544 .95164 .05100 Uiso ? ? 1.00000 ? ? H103 1.01205 .32830 1.01407 .04500 Uiso ? ? 1.00000 ? ? H104 .95737 .22737 1.10476 .05100 Uiso ? ? 1.00000 ? ? H105 .74610 .29715 1.13597 .04100 Uiso ? ? 1.00000 ? ? H106 .58736 .47535 1.08455 .07300 Uiso ? ? 1.00000 ? ? H201 .69615 .03683 .50405 .11000 Uiso ? ? 1.00000 ? ? H202 .82002 -.11795 .58624 .09300 Uiso ? ? 1.00000 ? ? H203 .73949 -.15274 .68953 .10400 Uiso ? ? 1.00000 ? ? H204 .53806 -.02601 .71826 .11600 Uiso ? ? 1.00000 ? ? H205 .40303 .13894 .63978 .14700 Uiso ? ? 1.00000 ? ? H206 .48308 .16702 .52676 .13800 Uiso ? ? 1.00000 ? ? 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 Ru1 .02701(11) .01968(11) .01843(10) -.00527(9) .00023(8) -.00143(8) Ru2 .02978(12) .02301(11) .01903(11) -.00834(9) .00515(8) -.00001(8) Ru3 .03701(13) .02522(12) .01664(11) -.00470(10) -.00582(9) -.00056(8) C11 .0423(18) .0295(15) .0271(15) -.0055(13) .0019(13) -.0046(12) O11 .0743(19) .0526(16) .0315(13) -.0053(14) .0144(12) -.0134(12) C12 .0324(16) .0258(14) .0259(14) -.0078(12) .0060(12) -.0048(11) O12 .0271(11) .0427(13) .0414(13) -.0054(10) .0006(9) -.0054(10) C13 .0292(15) .0319(16) .0315(15) -.0096(13) -.0005(12) -.0051(12) O13 .0514(15) .0288(12) .0601(16) -.0173(11) -.0011(12) .0074(11) C21 .053(2) .0390(18) .0293(16) -.0174(16) .0124(14) -.0047(13) O21 .084(2) .075(2) .0288(13) -.0331(17) .0248(13) -.0115(13) C22 .0390(17) .0317(16) .0288(15) -.0122(13) .0059(13) .0009(12) O22 .0624(17) .0289(13) .0557(16) -.0193(12) .0038(13) .0010(11) C23 .0324(16) .0297(15) .0345(16) -.0113(13) .0092(13) -.0013(12) O23 .0322(13) .0537(16) .0601(16) -.0190(12) .0023(11) -.0027(13) C31 .061(2) .0407(19) .0214(15) -.0060(17) -.0109(15) -.0034(13) O31 .092(2) .078(2) .0280(13) -.0097(17) -.0047(14) -.0197(14) C32 .051(2) .0348(17) .0213(14) -.0076(15) -.0033(13) .0012(12) O32 .0777(19) .0319(13) .0409(14) -.0139(13) .0020(13) .0073(11) C33 .045(2) .0302(16) .0325(16) -.0023(14) -.0140(14) -.0056(13) O33 .0419(15) .0622(17) .0593(17) -.0059(13) -.0179(12) -.0205(14) C1 .0220(12) .0198(12) .0179(12) -.0063(10) -.0019(10) -.0010(9) C111 .0199(12) .0315(14) .0156(11) -.0056(11) .0008(9) -.0028(10) C112 .0235(13) .0362(16) .0268(14) -.0099(12) .0021(11) -.0087(12) C113 .0252(15) .060(2) .0392(18) -.0139(15) -.0010(13) -.0197(16) C114 .0245(15) .068(2) .0285(16) -.0018(16) -.0068(12) -.0113(16) C115 .0306(16) .0461(19) .0249(15) .0046(14) -.0030(12) .0035(13) C116 .0262(14) .0348(16) .0235(14) -.0065(12) -.0010(11) .0032(12) C121 .0213(12) .0191(12) .0222(13) -.0053(10) -.0016(10) .0038(10) C122 .0283(14) .0300(15) .0280(14) -.0125(12) -.0046(11) -.0007(11) C123 .0260(15) .0333(16) .0464(18) -.0155(13) -.0043(13) .0002(14) C124 .0226(14) .0342(16) .0422(18) -.0088(12) .0063(12) .0041(13) C125 .0296(15) .0409(17) .0296(15) -.0089(13) .0054(12) -.0017(13) C126 .0262(14) .0345(16) .0257(14) -.0111(12) -.0002(11) -.0023(12) C2 .0230(13) .0213(12) .0185(12) -.0083(10) .0015(10) -.0034(10) C3 .0258(13) .0210(12) .0185(12) -.0082(10) .0003(10) -.0009(10) C4 .0234(13) .0193(12) .0187(12) -.0062(10) -.0000(10) .0013(9) C41 .0241(13) .0224(13) .0262(13) -.0070(11) -.0024(10) -.0062(11) C42 .0331(16) .0291(15) .0286(15) -.0039(12) -.0035(12) -.0046(12) C43 .0403(19) .043(2) .0360(18) .0062(16) -.0117(15) -.0057(15) C44 .0268(16) .071(3) .049(2) -.0015(17) -.0091(15) -.028(2) C45 .0313(17) .060(2) .061(2) -.0238(17) .0066(16) -.026(2) C46 .0324(16) .0347(17) .048(2) -.0154(14) .0032(14) -.0128(14) C5 .0231(13) .0229(13) .0213(12) -.0061(11) -.0003(10) -.0008(10) C51 .0277(14) .0219(13) .0185(12) -.0084(11) .0003(10) .0001(10) C52 .0283(14) .0362(16) .0264(14) -.0106(12) .0018(11) -.0081(12) C53 .0296(15) .0370(16) .0240(14) -.0033(13) .0020(11) -.0048(12) C54 .0469(18) .0255(15) .0261(14) -.0081(13) .0050(13) -.0074(12) C55 .048(2) .0350(17) .0381(17) -.0229(15) .0023(14) -.0106(14) C56 .0302(15) .0280(14) .0273(14) -.0116(12) .0015(11) -.0051(11) O0 .0357(11) .0228(10) .0250(10) -.0095(8) -.0074(8) -.0030(8) C101 .050(2) .0350(18) .048(2) -.0058(16) -.0066(17) .0033(15) C102 .055(2) .045(2) .0303(17) -.0181(17) .0005(15) .0065(14) C103 .0350(17) .051(2) .043(2) -.0122(16) .0054(15) -.0029(16) C104 .0415(18) .0351(17) .0377(18) -.0095(14) -.0061(14) .0045(14) C105 .052(2) .052(2) .043(2) -.0201(18) .0086(17) .0106(17) C106 .038(2) .054(2) .056(2) -.0074(17) .0085(17) .0018(19) C201 .107(4) .062(3) .038(2) -.037(3) .008(2) -.010(2) C202 .050(2) .041(2) .083(3) -.0165(18) -.001(2) -.011(2) C203 .102(4) .069(3) .057(3) -.056(3) -.024(3) .008(2) C204 .161(7) .099(4) .089(4) -.098(5) .074(4) -.065(4) C205 .061(3) .085(4) .260(11) -.032(3) .068(5) -.109(6) C206 .094(4) .043(3) .133(5) .003(3) -.066(4) -.000(3) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ru1 Ru2 . . 2.8262(4) ? Ru1 Ru3 . . 3.4579(3) ? Ru1 C11 . . 1.910(3) ? Ru1 C12 . . 1.895(3) ? Ru1 C13 . . 1.942(3) ? Ru1 C1 . . 2.409(3) ? Ru1 C2 . . 2.244(3) ? Ru1 O0 . . 2.086(2) ? Ru2 Ru3 . . 2.7867(4) ? Ru2 C21 . . 1.919(3) ? Ru2 C22 . . 1.907(3) ? Ru2 C23 . . 1.932(3) ? Ru2 C2 . . 2.099(3) ? Ru2 C3 . . 2.274(3) ? Ru3 C31 . . 1.957(3) ? Ru3 C32 . . 1.866(3) ? Ru3 C33 . . 1.922(4) ? Ru3 C3 . . 2.076(3) ? Ru3 O0 . . 2.1134(19) ? C11 O11 . . 1.135(4) ? C12 O12 . . 1.136(4) ? C13 O13 . . 1.127(4) ? C21 O21 . . 1.140(4) ? C22 O22 . . 1.136(4) ? C23 O23 . . 1.132(4) ? C31 O31 . . 1.139(4) ? C32 O32 . . 1.140(4) ? C33 O33 . . 1.139(5) ? C1 C111 . . 1.505(4) ? C1 C121 . . 1.508(4) ? C1 C2 . . 1.396(3) ? C111 C112 . . 1.391(5) ? C111 C116 . . 1.398(4) ? C112 C113 . . 1.398(4) ? C112 H112 . . .938 ? C113 C114 . . 1.371(5) ? C113 H113 . . .956 ? C114 C115 . . 1.384(6) ? C114 H114 . . .901 ? C115 C116 . . 1.387(4) ? C115 H115 . . .948 ? C116 H116 . . .896 ? C121 C122 . . 1.394(5) ? C121 C126 . . 1.395(4) ? C122 C123 . . 1.386(5) ? C122 H122 . . .896 ? C123 C124 . . 1.384(5) ? C123 H123 . . .937 ? C124 C125 . . 1.373(5) ? C124 H124 . . .939 ? C125 C126 . . 1.393(5) ? C125 H125 . . .974 ? C126 H126 . . .956 ? C2 C3 . . 1.406(3) ? C3 C4 . . 1.499(4) ? C4 C41 . . 1.494(4) ? C4 C5 . . 1.345(4) ? C41 C42 . . 1.392(4) ? C41 C46 . . 1.388(5) ? C42 C43 . . 1.392(4) ? C42 H42 . . .970 ? C43 C44 . . 1.374(6) ? C43 H43 . . .863 ? C44 C45 . . 1.374(5) ? C44 H44 . . .937 ? C45 C46 . . 1.390(4) ? C45 H45 . . .901 ? C46 H46 . . .927 ? C5 C51 . . 1.478(4) ? C5 H5 . . .900 ? C51 C52 . . 1.398(4) ? C51 C56 . . 1.396(5) ? C52 C53 . . 1.387(4) ? C52 H52 . . .915 ? C53 C54 . . 1.376(5) ? C53 H53 . . .887 ? C54 C55 . . 1.379(5) ? C54 H54 . . .958 ? C55 C56 . . 1.385(4) ? C55 H55 . . .959 ? C56 H56 . . .925 ? O0 H0 . . .906 ? C101 C102 . . 1.375(5) ? C101 C106 . . 1.374(6) ? C101 H101 . . .916 ? C102 C103 . . 1.368(4) ? C102 H102 . . .926 ? C103 C104 . . 1.372(5) ? C103 H103 . . .877 ? C104 C105 . . 1.377(5) ? C104 H104 . . .907 ? C105 C106 . . 1.384(5) ? C105 H105 . . .834 ? C106 H106 . . .933 ? C201 C202 . . 1.333(6) ? C201 C206 . . 1.360(8) ? C201 H201 . . .950 ? C202 C203 . . 1.318(7) ? C202 H202 . . .951 ? C203 C204 . . 1.321(9) ? C203 H203 . . .959 ? C204 C205 . . 1.362(10) ? C204 H204 . . .952 ? C205 C206 . . 1.411(13) ? C205 H205 . . .945 ? C206 H206 . . .950 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Ru2 Ru1 Ru3 . . . 51.456(9) ? Ru2 Ru1 C11 . . . 87.97(10) ? Ru2 Ru1 C12 . . . 91.07(10) ? Ru2 Ru1 C13 . . . 172.76(9) ? Ru2 Ru1 C1 . . . 78.64(7) ? Ru2 Ru1 C2 . . . 47.21(7) ? Ru2 Ru1 O0 . . . 86.17(6) ? Ru3 Ru1 C11 . . . 85.03(8) ? Ru3 Ru1 C12 . . . 142.16(10) ? Ru3 Ru1 C13 . . . 128.03(9) ? Ru3 Ru1 C1 . . . 87.84(5) ? Ru3 Ru1 C2 . . . 58.14(6) ? Ru3 Ru1 O0 . . . 34.83(6) ? C11 Ru1 C12 . . . 89.04(13) ? C11 Ru1 C13 . . . 99.23(14) ? C11 Ru1 C1 . . . 166.51(13) ? C11 Ru1 C2 . . . 133.12(11) ? C11 Ru1 O0 . . . 88.27(11) ? C12 Ru1 C13 . . . 89.81(13) ? C12 Ru1 C1 . . . 89.58(11) ? C12 Ru1 C2 . . . 102.57(12) ? C12 Ru1 O0 . . . 176.21(11) ? C13 Ru1 C1 . . . 94.18(11) ? C13 Ru1 C2 . . . 125.64(11) ? C13 Ru1 O0 . . . 93.26(11) ? C1 Ru1 C2 . . . 34.68(8) ? C1 Ru1 O0 . . . 92.40(8) ? C2 Ru1 O0 . . . 77.41(9) ? Ru1 Ru2 Ru3 . . . 76.056(10) ? Ru1 Ru2 C21 . . . 99.19(12) ? Ru1 Ru2 C22 . . . 166.55(9) ? Ru1 Ru2 C23 . . . 92.27(10) ? Ru1 Ru2 C2 . . . 51.68(7) ? Ru1 Ru2 C3 . . . 76.84(7) ? Ru3 Ru2 C21 . . . 80.46(12) ? Ru3 Ru2 C22 . . . 103.44(10) ? Ru3 Ru2 C23 . . . 167.56(10) ? Ru3 Ru2 C2 . . . 73.26(7) ? Ru3 Ru2 C3 . . . 47.10(7) ? C21 Ru2 C22 . . . 93.93(15) ? C21 Ru2 C23 . . . 97.48(14) ? C21 Ru2 C2 . . . 144.39(16) ? C21 Ru2 C3 . . . 127.18(13) ? C22 Ru2 C23 . . . 88.92(14) ? C22 Ru2 C2 . . . 115.05(12) ? C22 Ru2 C3 . . . 92.89(12) ? C23 Ru2 C2 . . . 103.02(12) ? C23 Ru2 C3 . . . 134.98(11) ? C2 Ru2 C3 . . . 37.25(8) ? Ru1 Ru3 Ru2 . . . 52.488(9) ? Ru1 Ru3 C31 . . . 97.75(9) ? Ru1 Ru3 C32 . . . 141.07(12) ? Ru1 Ru3 C33 . . . 124.12(9) ? Ru1 Ru3 C3 . . . 65.15(6) ? Ru1 Ru3 O0 . . . 34.31(6) ? Ru2 Ru3 C31 . . . 105.95(12) ? Ru2 Ru3 C32 . . . 88.59(12) ? Ru2 Ru3 C33 . . . 157.50(10) ? Ru2 Ru3 C3 . . . 53.37(8) ? Ru2 Ru3 O0 . . . 86.68(6) ? C31 Ru3 C32 . . . 92.72(14) ? C31 Ru3 C33 . . . 96.53(16) ? C31 Ru3 C3 . . . 158.25(13) ? C31 Ru3 O0 . . . 91.54(12) ? C32 Ru3 C33 . . . 91.43(15) ? C32 Ru3 C3 . . . 93.28(12) ? C32 Ru3 O0 . . . 174.35(12) ? C33 Ru3 C3 . . . 104.19(12) ? C33 Ru3 O0 . . . 91.76(11) ? C3 Ru3 O0 . . . 81.42(9) ? Ru1 C11 O11 . . . 177.0(4) ? Ru1 C12 O12 . . . 175.4(3) ? Ru1 C13 O13 . . . 174.7(3) ? Ru2 C21 O21 . . . 177.0(3) ? Ru2 C22 O22 . . . 176.1(3) ? Ru2 C23 O23 . . . 175.5(3) ? Ru3 C31 O31 . . . 174.5(3) ? Ru3 C32 O32 . . . 179.1(3) ? Ru3 C33 O33 . . . 175.7(3) ? Ru1 C1 C111 . . . 104.90(15) ? Ru1 C1 C121 . . . 121.3(2) ? Ru1 C1 C2 . . . 66.20(14) ? C111 C1 C121 . . . 113.9(2) ? C111 C1 C2 . . . 122.2(3) ? C121 C1 C2 . . . 118.7(2) ? C1 C111 C112 . . . 121.9(2) ? C1 C111 C116 . . . 119.5(3) ? C112 C111 C116 . . . 118.6(3) ? C111 C112 C113 . . . 120.5(3) ? C111 C112 H112 . . . 120.5 ? C113 C112 H112 . . . 119.0 ? C112 C113 C114 . . . 119.7(4) ? C112 C113 H113 . . . 118.8 ? C114 C113 H113 . . . 121.5 ? C113 C114 C115 . . . 120.8(3) ? C113 C114 H114 . . . 120.2 ? C115 C114 H114 . . . 118.9 ? C114 C115 C116 . . . 119.5(3) ? C114 C115 H115 . . . 121.7 ? C116 C115 H115 . . . 118.8 ? C111 C116 C115 . . . 120.8(3) ? C111 C116 H116 . . . 118.6 ? C115 C116 H116 . . . 120.5 ? C1 C121 C122 . . . 123.4(2) ? C1 C121 C126 . . . 118.1(3) ? C122 C121 C126 . . . 118.5(3) ? C121 C122 C123 . . . 120.3(3) ? C121 C122 H122 . . . 119.7 ? C123 C122 H122 . . . 119.9 ? C122 C123 C124 . . . 120.7(3) ? C122 C123 H123 . . . 121.5 ? C124 C123 H123 . . . 117.8 ? C123 C124 C125 . . . 119.5(3) ? C123 C124 H124 . . . 121.6 ? C125 C124 H124 . . . 118.9 ? C124 C125 C126 . . . 120.5(3) ? C124 C125 H125 . . . 123.9 ? C126 C125 H125 . . . 115.3 ? C121 C126 C125 . . . 120.5(3) ? C121 C126 H126 . . . 120.5 ? C125 C126 H126 . . . 119.0 ? Ru1 C2 Ru2 . . . 81.11(8) ? Ru1 C2 C1 . . . 79.11(15) ? Ru1 C2 C3 . . . 120.7(2) ? Ru2 C2 C1 . . . 144.22(18) ? Ru2 C2 C3 . . . 78.14(16) ? C1 C2 C3 . . . 137.6(3) ? Ru2 C3 Ru3 . . . 79.54(9) ? Ru2 C3 C2 . . . 64.61(15) ? Ru2 C3 C4 . . . 126.9(2) ? Ru3 C3 C2 . . . 115.52(18) ? Ru3 C3 C4 . . . 127.09(16) ? C2 C3 C4 . . . 117.3(2) ? C3 C4 C41 . . . 116.5(3) ? C3 C4 C5 . . . 121.9(2) ? C41 C4 C5 . . . 121.6(2) ? C4 C41 C42 . . . 120.1(3) ? C4 C41 C46 . . . 121.1(2) ? C42 C41 C46 . . . 118.8(3) ? C41 C42 C43 . . . 120.3(3) ? C41 C42 H42 . . . 117.1 ? C43 C42 H42 . . . 122.6 ? C42 C43 C44 . . . 120.5(3) ? C42 C43 H43 . . . 121.4 ? C44 C43 H43 . . . 118.1 ? C43 C44 C45 . . . 119.6(3) ? C43 C44 H44 . . . 119.5 ? C45 C44 H44 . . . 120.7 ? C44 C45 C46 . . . 120.7(4) ? C44 C45 H45 . . . 122.1 ? C46 C45 H45 . . . 117.2 ? C41 C46 C45 . . . 120.3(3) ? C41 C46 H46 . . . 118.2 ? C45 C46 H46 . . . 121.5 ? C4 C5 C51 . . . 129.9(2) ? C4 C5 H5 . . . 116.8 ? C51 C5 H5 . . . 113.2 ? C5 C51 C52 . . . 125.1(3) ? C5 C51 C56 . . . 117.5(2) ? C52 C51 C56 . . . 117.3(3) ? C51 C52 C53 . . . 121.1(3) ? C51 C52 H52 . . . 119.1 ? C53 C52 H52 . . . 119.9 ? C52 C53 C54 . . . 120.6(3) ? C52 C53 H53 . . . 125.2 ? C54 C53 H53 . . . 114.2 ? C53 C54 C55 . . . 119.3(3) ? C53 C54 H54 . . . 116.8 ? C55 C54 H54 . . . 123.9 ? C54 C55 C56 . . . 120.4(4) ? C54 C55 H55 . . . 122.8 ? C56 C55 H55 . . . 116.8 ? C51 C56 C55 . . . 121.3(3) ? C51 C56 H56 . . . 122.1 ? C55 C56 H56 . . . 116.5 ? Ru1 O0 Ru3 . . . 110.86(11) ? Ru1 O0 H0 . . . 124.84 ? Ru3 O0 H0 . . . 116.82 ? C102 C101 C106 . . . 119.8(3) ? C102 C101 H101 . . . 120.0 ? C106 C101 H101 . . . 120.1 ? C101 C102 C103 . . . 120.4(3) ? C101 C102 H102 . . . 122.2 ? C103 C102 H102 . . . 117.3 ? C102 C103 C104 . . . 120.4(3) ? C102 C103 H103 . . . 123.8 ? C104 C103 H103 . . . 115.8 ? C103 C104 C105 . . . 119.5(3) ? C103 C104 H104 . . . 118.3 ? C105 C104 H104 . . . 122.2 ? C104 C105 C106 . . . 120.3(4) ? C104 C105 H105 . . . 117.1 ? C106 C105 H105 . . . 122.6 ? C101 C106 C105 . . . 119.7(3) ? C101 C106 H106 . . . 123.5 ? C105 C106 H106 . . . 116.8 ? C202 C201 C206 . . . 120.1(5) ? C202 C201 H201 . . . 119.6 ? C206 C201 H201 . . . 120.2 ? C201 C202 C203 . . . 121.2(4) ? C201 C202 H202 . . . 119.4 ? C203 C202 H202 . . . 119.4 ? C202 C203 C204 . . . 121.3(5) ? C202 C203 H203 . . . 118.6 ? C204 C203 H203 . . . 120.0 ? C203 C204 C205 . . . 121.1(7) ? C203 C204 H204 . . . 118.2 ? C205 C204 H204 . . . 120.7 ? C204 C205 C206 . . . 117.5(6) ? C204 C205 H205 . . . 120.1 ? C206 C205 H205 . . . 122.4 ? C201 C206 C205 . . . 118.8(5) ? C201 C206 H206 . . . 120.7 ? C205 C206 H206 . . . 120.5 ? _exptl_crystal_F_000 1092 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min -13 _reflns_limit_k_max 15 _reflns_limit_l_min -26 _reflns_limit_l_max 26 _reflns_number_observed ? _reflns_d_resolution_high .735 _reflns_d_resolution_low 10.467 _diffrn_reflns_av_sigmaI/netI .058 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .054 _refine_ls_wR_factor_all .041 _refine_ls_goodness_of_fit_all 1.078 _refine_ls_shift/su_mean .0003 data_br802 _database_code_CSD 175563 _audit_creation_method Xtal3.6 _audit_creation_date 01-05-01 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C54 H36 Fe2 O9 Ru3' _chemical_formula_moiety ? _chemical_formula_weight 1243.78 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 16.8890(14) _cell_length_b 18.2350(10) _cell_length_c 15.5780(10) _cell_angle_alpha 90.00000 _cell_angle_beta 104.117(2) _cell_angle_gamma 90.00000 _cell_volume 4652.7(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.776 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8171 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 22.1 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 1.619 _exptl_crystal_description rhomb _exptl_crystal_size_max .4 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .3 _exptl_crystal_size_rad ? _exptl_crystal_colour dark_red _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .67 _exptl_absorpt_correction_T_max .83 _diffrn_reflns_number 94806 _reflns_number_total 24348 _reflns_Friedel_coverage 0 _reflns_number_gt 17036 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.7 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .037 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .034 _refine_ls_wR_factor_ref .04 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_number_reflns 17036 _refine_ls_number_parameters 733 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .008 _refine_diff_density_min -.825 _refine_diff_density_max 1.45 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 216 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 144 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Fe ? 0 8 .301 .845 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 36 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 12 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 .285456(9) 1.189350(8) .221101(10) .01668(6) Uani ? ? 1.00000 ? ? Ru2 .181631(9) 1.132030(9) .322572(10) .01717(6) Uani ? ? 1.00000 ? ? Ru3 .114430(9) 1.029970(10) .413652(10) .01949(6) Uani ? ? 1.00000 ? ? Fe5 .365597(18) .981129(16) .60202(2) .01973(11) Uani ? ? 1.00000 ? ? Fe7 .04202(2) .892570(19) .13615(2) .02466(13) Uani ? ? 1.00000 ? ? C11 .23731(13) 1.28537(12) .23349(14) .0230(8) Uani ? ? 1.00000 ? ? O11 .20755(11) 1.33939(9) .24266(12) .0328(8) Uani ? ? 1.00000 ? ? C12 .19354(13) 1.16548(12) .12273(14) .0239(8) Uani ? ? 1.00000 ? ? O12 .13907(11) 1.15123(11) .06686(11) .0351(8) Uani ? ? 1.00000 ? ? C13 .36012(13) 1.21744(12) .14940(15) .0248(9) Uani ? ? 1.00000 ? ? O13 .40420(12) 1.23840(10) .11072(13) .0373(9) Uani ? ? 1.00000 ? ? C14 .36731(13) 1.20449(11) .33307(15) .0244(8) Uani ? ? 1.00000 ? ? O14 .41340(11) 1.21498(10) .39784(12) .0358(8) Uani ? ? 1.00000 ? ? C21 .08736(14) 1.17709(14) .25537(16) .0293(10) Uani ? ? 1.00000 ? ? O21 .02917(12) 1.20353(13) .21295(14) .0496(11) Uani ? ? 1.00000 ? ? C22 .20090(14) 1.20951(13) .40261(15) .0266(9) Uani ? ? 1.00000 ? ? O22 .21493(13) 1.25589(11) .45380(13) .0434(10) Uani ? ? 1.00000 ? ? C31 .10368(13) 1.08917(14) .51529(14) .0271(9) Uani ? ? 1.00000 ? ? O31 .09303(12) 1.12883(12) .56753(12) .0415(10) Uani ? ? 1.00000 ? ? C32 .11577(15) .93427(14) .46018(15) .0300(10) Uani ? ? 1.00000 ? ? O32 .11979(15) .87551(12) .48540(15) .0507(12) Uani ? ? 1.00000 ? ? O33 -.07292(11) 1.04793(14) .34980(12) .0465(10) Uani ? ? 1.00000 ? ? C33 -.00411(14) 1.03947(15) .37211(14) .0308(10) Uani ? ? 1.00000 ? ? C1 .35079(12) 1.02907(11) .18116(13) .0199(8) Uani ? ? 1.00000 ? ? C111 .36524(13) .94950(11) .20048(15) .0227(8) Uani ? ? 1.00000 ? ? C112 .38363(14) .92249(12) .28742(16) .0260(9) Uani ? ? 1.00000 ? ? C113 .40050(17) .84859(13) .30514(19) .0343(11) Uani ? ? 1.00000 ? ? C114 .3998(2) .80053(14) .2359(2) .0433(14) Uani ? ? 1.00000 ? ? C115 .3816(2) .82591(14) .1495(2) .0425(14) Uani ? ? 1.00000 ? ? C116 .36442(17) .89931(13) .13153(18) .0324(11) Uani ? ? 1.00000 ? ? C121 .37860(14) 1.05636(11) .10276(15) .0246(9) Uani ? ? 1.00000 ? ? C122 .32155(19) 1.07473(14) .02451(17) .0353(12) Uani ? ? 1.00000 ? ? C123 .3462(2) 1.09797(17) -.0498(2) .0500(16) Uani ? ? 1.00000 ? ? C124 .4263(2) 1.10328(16) -.0481(2) .0543(17) Uani ? ? 1.00000 ? ? C125 .4841(2) 1.08405(18) .0268(2) .0501(17) Uani ? ? 1.00000 ? ? C126 .46079(17) 1.06007(15) .1026(2) .0364(12) Uani ? ? 1.00000 ? ? C2 .31310(12) 1.07385(10) .22804(12) .0171(7) Uani ? ? 1.00000 ? ? C3 .26381(12) 1.04795(10) .28863(12) .0173(7) Uani ? ? 1.00000 ? ? C4 .28868(11) 1.05714(11) .38300(12) .0175(7) Uani ? ? 1.00000 ? ? C5 .24000(11) 1.04774(11) .44405(12) .0174(7) Uani ? ? 1.00000 ? ? C501 .28572(12) 1.05881(10) .53786(12) .0181(7) Uani ? ? 1.00000 ? ? C502 .26173(13) 1.03193(12) .61473(13) .0218(8) Uani ? ? 1.00000 ? ? C503 .32628(14) 1.04581(12) .69105(14) .0240(8) Uani ? ? 1.00000 ? ? C504 .39000(14) 1.08162(12) .66293(14) .0242(8) Uani ? ? 1.00000 ? ? C505 .36622(13) 1.08952(11) .56963(14) .0204(8) Uani ? ? 1.00000 ? ? C501' .35714(16) .89456(13) .51634(17) .0310(10) Uani ? ? 1.00000 ? ? C502' .33804(18) .87165(13) .5963(2) .0343(11) Uani ? ? 1.00000 ? ? C503' .40700(19) .88591(14) .6665(2) .0373(12) Uani ? ? 1.00000 ? ? C504' .46862(16) .91782(14) .6312(2) .0359(11) Uani ? ? 1.00000 ? ? C505' .43781(15) .92324(13) .53770(18) .0311(10) Uani ? ? 1.00000 ? ? C6 .18389(12) 1.02311(11) .24707(13) .0196(7) Uani ? ? 1.00000 ? ? C7 .11957(12) 1.00579(12) .28637(13) .0209(8) Uani ? ? 1.00000 ? ? C701 .04568(13) .97890(13) .22189(14) .0247(9) Uani ? ? 1.00000 ? ? C702 .01664(13) 1.00186(13) .13149(14) .0233(8) Uani ? ? 1.00000 ? ? C703 -.05504(14) .96192(14) .09258(15) .0287(10) Uani ? ? 1.00000 ? ? C704 -.07111(15) .91314(17) .15668(16) .0352(11) Uani ? ? 1.00000 ? ? C705 -.01025(15) .92311(16) .23611(16) .0338(11) Uani ? ? 1.00000 ? ? C701' .15495(17) .84425(16) .1628(2) .0398(13) Uani ? ? 1.00000 ? ? C702' .13530(17) .87241(16) .0765(2) .0374(12) Uani ? ? 1.00000 ? ? C703' .06235(19) .83718(18) .0296(2) .0436(14) Uani ? ? 1.00000 ? ? C704' .0379(2) .78766(17) .0873(2) .0492(15) Uani ? ? 1.00000 ? ? C705' .0947(2) .79226(17) .1699(2) .0486(15) Uani ? ? 1.00000 ? ? C01 .2605(2) .7195(2) .4009(3) .061(2) Uani ? ? 1.00000 ? ? C02 .1800(3) .6990(2) .3808(3) .064(2) Uani ? ? 1.00000 ? ? C03 .1607(2) .6269(2) .3490(3) .065(2) Uani ? ? 1.00000 ? ? C04 .2203(2) .5777(2) .3389(3) .062(2) Uani ? ? 1.00000 ? ? C05 .2998(3) .6041(2) .3607(3) .068(2) Uani ? ? 1.00000 ? ? C06 .3185(3) .6756(2) .3888(3) .069(2) Uani ? ? 1.00000 ? ? H112 .3861(16) .9560(14) .3393(18) .025(7) Uiso ? ? 1.00000 ? ? H113 .4143(16) .8312(15) .3644(18) .025(7) Uiso ? ? 1.00000 ? ? H114 .404(2) .756(2) .250(3) .076(13) Uiso ? ? 1.00000 ? ? H115 .3775(19) .7980(18) .106(2) .042(9) Uiso ? ? 1.00000 ? ? H116 .3538(16) .9134(15) .0716(18) .028(7) Uiso ? ? 1.00000 ? ? H122 .2615(18) 1.0755(16) .0189(19) .035(8) Uiso ? ? 1.00000 ? ? H123 .3158(17) 1.112(2) -.088(2) .070(14) Uiso ? ? 1.00000 ? ? H124 .4418(10) 1.119(2) -.093(2) .078(13) Uiso ? ? 1.00000 ? ? H125 .533(2) 1.084(2) .0268(10) .060(11) Uiso ? ? 1.00000 ? ? H126 .5003(15) 1.0501(13) .1553(16) .015(6) Uiso ? ? 1.00000 ? ? H4 .3456(14) 1.0707(13) .4056(15) .012(5) Uiso ? ? 1.00000 ? ? H502 .2142(14) 1.0108(13) .6169(15) .011(5) Uiso ? ? 1.00000 ? ? H503 .3275(18) 1.0314(16) .753(2) .038(8) Uiso ? ? 1.00000 ? ? H504 .4355(17) 1.0953(15) .6919(18) .029(7) Uiso ? ? 1.00000 ? ? H505 .3954(17) 1.1118(15) .5335(18) .029(7) Uiso ? ? 1.00000 ? ? H501' .3203(18) .8950(16) .460(2) .034(8) Uiso ? ? 1.00000 ? ? H502' .2898(18) .8554(16) .5972(19) .031(7) Uiso ? ? 1.00000 ? ? H503' .410(2) .880(2) .725(3) .072(13) Uiso ? ? 1.00000 ? ? H504' .526(2) .937(2) .668(2) .062(11) Uiso ? ? 1.00000 ? ? H505' .469(2) .9413(18) .493(2) .056(10) Uiso ? ? 1.00000 ? ? H6 .1711(17) 1.0199(15) .1864(19) .031(7) Uiso ? ? 1.00000 ? ? H702 .0429(17) 1.0352(15) .1053(18) .030(7) Uiso ? ? 1.00000 ? ? H703 -.0879(16) .9673(14) .0343(18) .025(7) Uiso ? ? 1.00000 ? ? H704 -.116(2) .8751(17) .146(2) .046(9) Uiso ? ? 1.00000 ? ? H705 -.0052(18) .8980(17) .282(2) .036(8) Uiso ? ? 1.00000 ? ? H701' .196(2) .8592(18) .199(2) .048(10) Uiso ? ? 1.00000 ? ? H702' .1656(18) .9103(17) .061(2) .035(8) Uiso ? ? 1.00000 ? ? H703' .045(2) .841(2) -.022(3) .072(13) Uiso ? ? 1.00000 ? ? H704' -.011(2) .7525(19) .071(2) .054(10) Uiso ? ? 1.00000 ? ? H705' .092(2) .769(2) .221(2) .053(10) Uiso ? ? 1.00000 ? ? H01 .27533 .76738 .42572 .07400 Uiso ? ? 1.00000 ? ? H02 .13732 .73305 .38750 .08000 Uiso ? ? 1.00000 ? ? H03 .10399 .61167 .33380 .08200 Uiso ? ? 1.00000 ? ? H04 .20750 .52729 .31999 .07000 Uiso ? ? 1.00000 ? ? H05 .34432 .57154 .35529 .08400 Uiso ? ? 1.00000 ? ? H06 .37400 .69340 .39988 .08500 Uiso ? ? 1.00000 ? ? 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 Ru1 .01797(6) .01541(6) .01786(7) -.00002(5) .00667(5) -.00055(5) Ru2 .01590(6) .02093(7) .01580(6) .00185(5) .00602(5) -.00034(5) Ru3 .01698(6) .02946(8) .01327(6) -.00294(6) .00611(5) -.00087(6) Fe5 .02163(13) .01521(12) .02076(13) .00189(10) .00210(10) .00021(10) Fe7 .02424(14) .02856(16) .01971(13) -.00691(12) .00251(11) -.00139(12) C11 .0239(9) .0243(9) .0219(9) .0016(8) .0073(7) .0017(7) O11 .0411(10) .0242(8) .0354(9) .0102(7) .0139(8) .0028(7) C12 .0277(10) .0244(10) .0207(9) -.0013(8) .0081(8) .0019(7) O12 .0341(9) .0449(11) .0247(8) -.0097(8) .0039(7) .0015(7) C13 .0285(10) .0186(9) .0306(10) -.0011(8) .0138(8) -.0014(8) O13 .0471(10) .0246(8) .0503(11) -.0066(7) .0315(9) -.0003(8) C14 .0256(9) .0171(9) .0308(11) .0028(7) .0077(8) -.0012(8) O14 .0354(9) .0278(8) .0364(9) .0010(7) -.0065(7) -.0042(7) C21 .0247(10) .0370(13) .0272(10) .0067(9) .0080(8) .0032(9) O21 .0321(10) .0698(15) .0426(11) .0236(10) .0008(8) .0048(10) C22 .0287(10) .0258(10) .0271(10) .0066(8) .0102(8) .0014(8) O22 .0570(13) .0336(10) .0415(11) .0023(9) .0159(9) -.0152(8) C31 .0198(9) .0427(13) .0191(9) .0037(9) .0057(7) .0009(9) O31 .0384(10) .0597(13) .0260(8) .0149(9) .0069(7) -.0135(8) C32 .0301(11) .0375(13) .0232(10) -.0076(9) .0081(8) -.0000(9) O32 .0656(15) .0394(12) .0488(13) -.0120(10) .0171(11) .0096(9) O33 .0206(8) .0900(17) .0291(9) .0004(9) .0062(7) .0013(10) C33 .0228(9) .0546(16) .0164(9) -.0044(10) .0075(7) -.0012(9) C1 .0220(8) .0180(8) .0229(9) -.0012(7) .0117(7) -.0025(7) C111 .0272(9) .0169(8) .0286(10) -.0008(7) .0155(8) -.0020(7) C112 .0298(10) .0191(9) .0311(11) .0012(8) .0114(9) -.0021(8) C113 .0455(14) .0205(10) .0387(13) .0055(10) .0140(11) .0040(9) C114 .065(2) .0161(11) .0552(18) .0038(11) .0264(15) -.0013(10) C115 .070(2) .0211(11) .0445(15) -.0047(12) .0305(15) -.0110(10) C116 .0507(15) .0196(10) .0345(12) -.0039(10) .0252(11) -.0049(9) C121 .0340(11) .0163(8) .0313(10) .0003(8) .0231(9) -.0032(8) C122 .0527(16) .0304(12) .0284(11) .0085(11) .0208(11) .0021(9) C123 .088(3) .0366(15) .0353(15) .0196(16) .0351(17) .0093(12) C124 .100(3) .0309(14) .0520(18) .0102(16) .058(2) .0091(13) C125 .0591(19) .0441(16) .065(2) -.0066(14) .0501(18) -.0065(15) C126 .0387(13) .0321(12) .0475(15) -.0024(10) .0283(12) -.0052(11) C2 .0207(8) .0153(8) .0170(8) -.0012(6) .0083(6) -.0001(6) C3 .0194(8) .0163(8) .0178(8) -.0013(6) .0076(6) -.0009(6) C4 .0174(8) .0189(8) .0167(8) .0009(6) .0049(6) -.0007(6) C5 .0185(8) .0181(8) .0162(7) .0011(6) .0053(6) -.0001(6) C501 .0205(8) .0169(8) .0161(8) .0029(6) .0029(6) -.0001(6) C502 .0235(9) .0240(9) .0185(8) .0030(7) .0062(7) .0011(7) C503 .0309(10) .0238(10) .0160(8) .0045(8) .0033(7) .0005(7) C504 .0270(10) .0197(9) .0217(9) .0006(8) -.0019(8) -.0035(7) C505 .0232(9) .0153(8) .0215(9) -.0003(7) .0028(7) -.0012(7) C501' .0377(12) .0187(10) .0340(12) .0024(9) .0036(10) -.0073(9) C502' .0406(14) .0162(9) .0459(15) -.0036(9) .0102(11) -.0002(9) C503' .0517(16) .0203(10) .0356(13) .0072(10) .0024(12) .0071(9) C504' .0302(11) .0243(11) .0474(15) .0107(9) -.0021(10) -.0024(10) C505' .0319(11) .0221(10) .0402(13) .0068(9) .0102(10) -.0050(9) C6 .0215(8) .0238(9) .0148(7) -.0056(7) .0067(6) -.0019(7) C7 .0211(8) .0260(9) .0163(8) -.0057(7) .0062(7) -.0025(7) C701 .0229(9) .0352(11) .0181(8) -.0089(8) .0091(7) -.0045(8) C702 .0217(9) .0302(11) .0192(9) -.0021(8) .0070(7) -.0029(8) C703 .0221(9) .0412(13) .0219(10) -.0030(9) .0036(8) -.0077(9) C704 .0248(10) .0543(16) .0279(11) -.0169(11) .0092(9) -.0114(11) C705 .0313(11) .0515(16) .0205(10) -.0199(11) .0097(9) -.0029(10) C701' .0308(12) .0366(14) .0447(15) .0015(11) -.0053(11) -.0035(12) C702' .0371(13) .0378(14) .0408(14) .0062(11) .0162(11) -.0034(11) C703' .0432(15) .0505(17) .0329(14) .0145(13) .0007(12) -.0165(12) C704' .0410(15) .0303(13) .069(2) -.0032(12) -.0011(14) -.0125(14) C705' .0450(16) .0347(15) .060(2) -.0036(12) .0013(14) .0140(14) C01 .065(2) .0397(18) .075(3) -.0184(16) .0144(19) -.0062(17) C02 .067(2) .055(2) .076(3) .0035(18) .029(2) .0066(19) C03 .056(2) .064(2) .076(3) -.0135(18) .016(2) -.009(2) C04 .0367(15) .072(2) .077(3) -.0090(16) .0121(16) -.033(2) C05 .062(2) .064(2) .080(3) -.004(2) .022(2) -.019(2) C06 .063(2) .056(2) .091(3) -.0175(19) .022(2) .001(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ru1 Ru2 . . 2.8316(3) ? Ru1 C11 . . 1.960(2) ? Ru1 C12 . . 1.946(2) ? Ru1 C13 . . 1.946(3) ? Ru1 C14 . . 1.963(2) ? Ru1 C2 . . 2.1544(19) ? Ru1 C3 . . 2.842(2) ? Ru2 Ru3 . . 2.7478(3) ? Ru2 C21 . . 1.869(2) ? Ru2 C22 . . 1.860(2) ? Ru2 C3 . . 2.217(2) ? Ru2 C4 . . 2.2780(18) ? Ru2 C5 . . 2.4506(18) ? Ru2 C6 . . 2.313(2) ? Ru2 C7 . . 2.535(2) ? Ru3 C31 . . 1.961(2) ? Ru3 C32 . . 1.888(3) ? Ru3 C33 . . 1.956(2) ? Ru3 C5 . . 2.0825(19) ? Ru3 C7 . . 2.054(2) ? Fe5 C501 . . 2.0415(18) ? Fe5 C502 . . 2.036(2) ? Fe5 C503 . . 2.051(2) ? Fe5 C504 . . 2.059(2) ? Fe5 C505 . . 2.041(2) ? Fe5 C501' . . 2.050(2) ? Fe5 C502' . . 2.047(2) ? Fe5 C503' . . 2.042(3) ? Fe5 C504' . . 2.045(3) ? Fe5 C505' . . 2.050(3) ? Fe7 C701 . . 2.056(2) ? Fe7 C702 . . 2.036(2) ? Fe7 C703 . . 2.051(2) ? Fe7 C704 . . 2.047(3) ? Fe7 C705 . . 2.046(3) ? Fe7 C701' . . 2.049(3) ? Fe7 C702' . . 2.048(3) ? Fe7 C703' . . 2.042(3) ? Fe7 C704' . . 2.054(3) ? Fe7 C705' . . 2.046(3) ? C11 O11 . . 1.131(3) ? C12 O12 . . 1.132(3) ? C13 O13 . . 1.132(3) ? C14 O14 . . 1.130(3) ? C21 O21 . . 1.148(3) ? C22 O22 . . 1.147(3) ? C31 O31 . . 1.135(3) ? C32 O32 . . 1.138(3) ? O33 C33 . . 1.139(3) ? C1 C111 . . 1.490(3) ? C1 C121 . . 1.497(3) ? C1 C2 . . 1.353(3) ? C111 C112 . . 1.403(3) ? C111 C116 . . 1.409(3) ? C112 C113 . . 1.391(3) ? C112 H112 . . 1.01(3) ? C113 C114 . . 1.388(4) ? C113 H113 . . .95(3) ? C114 C115 . . 1.384(4) ? C114 H114 . . .85(4) ? C115 C116 . . 1.384(4) ? C115 H115 . . .84(3) ? C116 H116 . . .94(3) ? C121 C122 . . 1.398(3) ? C121 C126 . . 1.390(4) ? C122 C123 . . 1.388(5) ? C122 H122 . . 1.00(3) ? C123 C124 . . 1.350(6) ? C123 H123 . . .73(3) ? C124 C125 . . 1.371(5) ? C124 H124 . . .86(4) ? C125 C126 . . 1.402(5) ? C125 H125 . . .83(4) ? C126 H126 . . .94(2) ? C2 C3 . . 1.480(3) ? C3 C4 . . 1.437(3) ? C3 C6 . . 1.421(3) ? C4 C5 . . 1.411(3) ? C4 H4 . . .97(2) ? C5 C501 . . 1.491(2) ? C501 C502 . . 1.441(3) ? C501 C505 . . 1.442(3) ? C502 C503 . . 1.426(3) ? C502 H502 . . .90(2) ? C503 C504 . . 1.416(3) ? C503 H503 . . .99(3) ? C504 C505 . . 1.418(3) ? C504 H504 . . .83(3) ? C505 H505 . . .93(3) ? C501' C502' . . 1.424(4) ? C501' C505' . . 1.421(4) ? C501' H501' . . .95(3) ? C502' C503' . . 1.413(4) ? C502' H502' . . .87(3) ? C503' C504' . . 1.415(4) ? C503' H503' . . .91(4) ? C504' C505' . . 1.426(4) ? C504' H504' . . 1.05(3) ? C505' H505' . . 1.02(4) ? C6 C7 . . 1.407(3) ? C6 H6 . . .92(3) ? C7 C701 . . 1.482(3) ? C701 C702 . . 1.436(3) ? C701 C705 . . 1.442(4) ? C702 C703 . . 1.416(3) ? C702 H702 . . .91(3) ? C703 C704 . . 1.412(4) ? C703 H703 . . .95(2) ? C704 C705 . . 1.414(3) ? C704 H704 . . 1.01(3) ? C705 H705 . . .83(3) ? C701' C702' . . 1.402(4) ? C701' C705' . . 1.414(5) ? C701' H701' . . .82(3) ? C702' C703' . . 1.423(4) ? C702' H702' . . .93(3) ? C703' C704' . . 1.405(5) ? C703' H703' . . .78(4) ? C704' C705' . . 1.408(5) ? C704' H704' . . 1.02(3) ? C705' H705' . . .91(4) ? C01 C02 . . 1.371(6) ? C01 C06 . . 1.313(6) ? C01 H01 . . .963 ? C02 C03 . . 1.416(6) ? C02 H02 . . .976 ? C03 C04 . . 1.386(6) ? C03 H03 . . .969 ? C04 C05 . . 1.388(5) ? C04 H04 . . .973 ? C05 C06 . . 1.387(6) ? C05 H05 . . .978 ? C06 H06 . . .967 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Ru2 Ru1 C11 . . . 86.93(7) ? Ru2 Ru1 C12 . . . 82.73(7) ? Ru2 Ru1 C13 . . . 173.59(7) ? Ru2 Ru1 C14 . . . 87.35(7) ? Ru2 Ru1 C2 . . . 76.54(6) ? Ru2 Ru1 C3 . . . 46.00(4) ? C11 Ru1 C12 . . . 90.40(9) ? C11 Ru1 C13 . . . 99.43(10) ? C11 Ru1 C14 . . . 90.35(9) ? C11 Ru1 C2 . . . 163.45(9) ? C11 Ru1 C3 . . . 132.86(8) ? C12 Ru1 C13 . . . 96.37(9) ? C12 Ru1 C14 . . . 169.99(10) ? C12 Ru1 C2 . . . 86.70(8) ? C12 Ru1 C3 . . . 86.48(7) ? C13 Ru1 C14 . . . 93.35(9) ? C13 Ru1 C2 . . . 97.08(9) ? C13 Ru1 C3 . . . 127.67(8) ? C14 Ru1 C2 . . . 89.76(8) ? C14 Ru1 C3 . . . 85.70(7) ? C2 Ru1 C3 . . . 30.71(7) ? Ru1 Ru2 Ru3 . . . 158.166(10) ? Ru1 Ru2 C21 . . . 94.81(8) ? Ru1 Ru2 C22 . . . 93.61(8) ? Ru1 Ru2 C3 . . . 67.24(5) ? Ru1 Ru2 C4 . . . 85.12(5) ? Ru1 Ru2 C5 . . . 118.38(5) ? Ru1 Ru2 C6 . . . 86.78(5) ? Ru1 Ru2 C7 . . . 119.32(5) ? Ru3 Ru2 C21 . . . 100.62(8) ? Ru3 Ru2 C22 . . . 101.25(8) ? Ru3 Ru2 C3 . . . 90.93(5) ? Ru3 Ru2 C4 . . . 76.51(5) ? Ru3 Ru2 C5 . . . 46.80(5) ? Ru3 Ru2 C6 . . . 75.00(5) ? Ru3 Ru2 C7 . . . 45.53(5) ? C21 Ru2 C22 . . . 91.57(10) ? C21 Ru2 C3 . . . 131.90(9) ? C21 Ru2 C4 . . . 167.64(9) ? C21 Ru2 C5 . . . 146.68(9) ? C21 Ru2 C6 . . . 102.13(9) ? C21 Ru2 C7 . . . 91.44(9) ? C22 Ru2 C3 . . . 131.91(8) ? C22 Ru2 C4 . . . 100.77(8) ? C22 Ru2 C5 . . . 89.26(8) ? C22 Ru2 C6 . . . 166.22(8) ? C22 Ru2 C7 . . . 146.53(9) ? C3 Ru2 C4 . . . 37.25(7) ? C3 Ru2 C5 . . . 65.99(7) ? C3 Ru2 C6 . . . 36.49(7) ? C3 Ru2 C7 . . . 64.40(7) ? C4 Ru2 C5 . . . 34.48(7) ? C4 Ru2 C6 . . . 65.51(6) ? C4 Ru2 C7 . . . 77.94(6) ? C5 Ru2 C6 . . . 78.50(6) ? C5 Ru2 C7 . . . 70.66(6) ? C6 Ru2 C7 . . . 33.34(7) ? Ru2 Ru3 C31 . . . 100.09(7) ? Ru2 Ru3 C32 . . . 148.94(8) ? Ru2 Ru3 C33 . . . 106.71(8) ? Ru2 Ru3 C5 . . . 59.07(5) ? Ru2 Ru3 C7 . . . 61.76(6) ? C31 Ru3 C32 . . . 101.17(11) ? C31 Ru3 C33 . . . 85.96(9) ? C31 Ru3 C5 . . . 91.17(8) ? C31 Ru3 C7 . . . 158.71(10) ? C32 Ru3 C33 . . . 97.15(11) ? C32 Ru3 C5 . . . 98.07(9) ? C32 Ru3 C7 . . . 99.96(10) ? C33 Ru3 C5 . . . 164.78(10) ? C33 Ru3 C7 . . . 88.88(9) ? C5 Ru3 C7 . . . 88.42(8) ? C501 Fe5 C502 . . . 41.38(9) ? C501 Fe5 C503 . . . 69.37(8) ? C501 Fe5 C504 . . . 69.03(8) ? C501 Fe5 C505 . . . 41.36(8) ? C501 Fe5 C501' . . . 106.43(8) ? C501 Fe5 C502' . . . 122.64(9) ? C501 Fe5 C503' . . . 159.54(11) ? C501 Fe5 C504' . . . 157.75(11) ? C501 Fe5 C505' . . . 121.26(9) ? C502 Fe5 C503 . . . 40.85(8) ? C502 Fe5 C504 . . . 68.31(9) ? C502 Fe5 C505 . . . 68.89(9) ? C502 Fe5 C501' . . . 119.28(9) ? C502 Fe5 C502' . . . 104.83(11) ? C502 Fe5 C503' . . . 122.61(12) ? C502 Fe5 C504' . . . 160.38(11) ? C502 Fe5 C505' . . . 155.71(8) ? C503 Fe5 C504 . . . 40.33(10) ? C503 Fe5 C505 . . . 68.42(9) ? C503 Fe5 C501' . . . 154.27(10) ? C503 Fe5 C502' . . . 118.86(11) ? C503 Fe5 C503' . . . 106.56(11) ? C503 Fe5 C504' . . . 124.93(10) ? C503 Fe5 C505' . . . 162.99(9) ? C504 Fe5 C505 . . . 40.47(8) ? C504 Fe5 C501' . . . 163.77(11) ? C504 Fe5 C502' . . . 154.97(11) ? C504 Fe5 C503' . . . 121.61(9) ? C504 Fe5 C504' . . . 109.65(9) ? C504 Fe5 C505' . . . 127.42(10) ? C505 Fe5 C501' . . . 126.07(10) ? C505 Fe5 C502' . . . 161.59(9) ? C505 Fe5 C503' . . . 157.43(9) ? C505 Fe5 C504' . . . 123.13(10) ? C505 Fe5 C505' . . . 109.78(10) ? C501' Fe5 C502' . . . 40.67(12) ? C501' Fe5 C503' . . . 68.06(10) ? C501' Fe5 C504' . . . 68.31(10) ? C501' Fe5 C505' . . . 40.56(10) ? C502' Fe5 C503' . . . 40.45(10) ? C502' Fe5 C504' . . . 68.35(11) ? C502' Fe5 C505' . . . 68.44(12) ? C503' Fe5 C504' . . . 40.51(12) ? C503' Fe5 C505' . . . 68.24(12) ? C504' Fe5 C505' . . . 40.76(11) ? C701 Fe7 C702 . . . 41.09(8) ? C701 Fe7 C703 . . . 68.75(9) ? C701 Fe7 C704 . . . 68.87(10) ? C701 Fe7 C705 . . . 41.16(10) ? C701 Fe7 C701' . . . 108.57(10) ? C701 Fe7 C702' . . . 121.86(10) ? C701 Fe7 C703' . . . 157.29(12) ? C701 Fe7 C704' . . . 161.27(12) ? C701 Fe7 C705' . . . 125.14(12) ? C702 Fe7 C703 . . . 40.55(9) ? C702 Fe7 C704 . . . 68.28(11) ? C702 Fe7 C705 . . . 68.56(11) ? C702 Fe7 C701' . . . 127.26(10) ? C702 Fe7 C702' . . . 109.76(11) ? C702 Fe7 C703' . . . 122.07(11) ? C702 Fe7 C704' . . . 155.59(11) ? C702 Fe7 C705' . . . 163.51(11) ? C703 Fe7 C704 . . . 40.32(11) ? C703 Fe7 C705 . . . 68.00(10) ? C703 Fe7 C701' . . . 164.08(12) ? C703 Fe7 C702' . . . 127.00(11) ? C703 Fe7 C703' . . . 108.39(11) ? C703 Fe7 C704' . . . 119.97(11) ? C703 Fe7 C705' . . . 154.03(12) ? C704 Fe7 C705 . . . 40.43(9) ? C704 Fe7 C701' . . . 154.80(12) ? C704 Fe7 C702' . . . 162.59(10) ? C704 Fe7 C703' . . . 124.46(11) ? C704 Fe7 C704' . . . 106.24(13) ? C704 Fe7 C705' . . . 119.19(13) ? C705 Fe7 C701' . . . 121.04(11) ? C705 Fe7 C702' . . . 156.46(10) ? C705 Fe7 C703' . . . 160.48(12) ? C705 Fe7 C704' . . . 123.62(14) ? C705 Fe7 C705' . . . 106.82(14) ? C701' Fe7 C702' . . . 40.02(12) ? C701' Fe7 C703' . . . 67.64(12) ? C701' Fe7 C704' . . . 67.71(12) ? C701' Fe7 C705' . . . 40.40(13) ? C702' Fe7 C703' . . . 40.72(12) ? C702' Fe7 C704' . . . 67.98(13) ? C702' Fe7 C705' . . . 67.76(14) ? C703' Fe7 C704' . . . 40.12(14) ? C703' Fe7 C705' . . . 67.52(14) ? C704' Fe7 C705' . . . 40.17(13) ? Ru1 C11 O11 . . . 177.1(2) ? Ru1 C12 O12 . . . 178.4(2) ? Ru1 C13 O13 . . . 175.1(2) ? Ru1 C14 O14 . . . 178.1(2) ? Ru2 C21 O21 . . . 178.6(2) ? Ru2 C22 O22 . . . 177.6(2) ? Ru3 C31 O31 . . . 172.5(2) ? Ru3 C32 O32 . . . 176.0(3) ? Ru3 C33 O33 . . . 177.0(2) ? C111 C1 C121 . . . 114.84(19) ? C111 C1 C2 . . . 123.6(2) ? C121 C1 C2 . . . 121.48(18) ? C1 C111 C112 . . . 121.6(2) ? C1 C111 C116 . . . 120.5(2) ? C112 C111 C116 . . . 117.8(2) ? C111 C112 C113 . . . 121.2(2) ? C111 C112 H112 . . . 121.2(15) ? C113 C112 H112 . . . 117.6(15) ? C112 C113 C114 . . . 119.7(3) ? C112 C113 H113 . . . 120.5(17) ? C114 C113 H113 . . . 119.8(17) ? C113 C114 C115 . . . 120.1(2) ? C113 C114 H114 . . . 115(3) ? C115 C114 H114 . . . 124(3) ? C114 C115 C116 . . . 120.4(3) ? C114 C115 H115 . . . 123(2) ? C116 C115 H115 . . . 117(2) ? C111 C116 C115 . . . 120.8(2) ? C111 C116 H116 . . . 122.8(17) ? C115 C116 H116 . . . 116.4(17) ? C1 C121 C122 . . . 120.3(2) ? C1 C121 C126 . . . 122.0(2) ? C122 C121 C126 . . . 117.6(3) ? C121 C122 C123 . . . 121.1(3) ? C121 C122 H122 . . . 123.3(17) ? C123 C122 H122 . . . 115.4(17) ? C122 C123 C124 . . . 120.5(3) ? C122 C123 H123 . . . 120(3) ? C124 C123 H123 . . . 119(3) ? C123 C124 C125 . . . 120.0(4) ? C123 C124 H124 . . . 120.8(13) ? C125 C124 H124 . . . 119.2(13) ? C124 C125 C126 . . . 120.6(3) ? C124 C125 H125 . . . 120.2(13) ? C126 C125 H125 . . . 119.2(14) ? C121 C126 C125 . . . 120.1(2) ? C121 C126 H126 . . . 119.0(17) ? C125 C126 H126 . . . 120.7(17) ? Ru1 C2 C1 . . . 133.43(16) ? Ru1 C2 C3 . . . 101.26(13) ? C1 C2 C3 . . . 124.29(18) ? Ru1 C3 Ru2 . . . 66.75(5) ? Ru1 C3 C2 . . . 48.03(10) ? Ru1 C3 C4 . . . 103.95(12) ? Ru1 C3 C6 . . . 108.31(12) ? Ru2 C3 C2 . . . 114.44(13) ? Ru2 C3 C4 . . . 73.69(12) ? Ru2 C3 C6 . . . 75.46(12) ? C2 C3 C4 . . . 123.08(16) ? C2 C3 C6 . . . 115.51(16) ? C4 C3 C6 . . . 120.8(2) ? Ru2 C4 C3 . . . 69.06(10) ? Ru2 C4 C5 . . . 79.47(11) ? Ru2 C4 H4 . . . 127.8(13) ? C3 C4 C5 . . . 127.04(17) ? C3 C4 H4 . . . 114.7(14) ? C5 C4 H4 . . . 118.3(14) ? Ru2 C5 Ru3 . . . 74.13(5) ? Ru2 C5 C4 . . . 66.05(10) ? Ru2 C5 C501 . . . 133.37(13) ? Ru3 C5 C4 . . . 126.45(12) ? Ru3 C5 C501 . . . 119.96(15) ? C4 C5 C501 . . . 113.36(16) ? Fe5 C501 C5 . . . 120.56(14) ? Fe5 C501 C502 . . . 69.10(11) ? Fe5 C501 C505 . . . 69.28(11) ? C5 C501 C502 . . . 125.82(17) ? C5 C501 C505 . . . 127.5(2) ? C502 C501 C505 . . . 106.24(16) ? Fe5 C502 C501 . . . 69.52(12) ? Fe5 C502 C503 . . . 70.13(13) ? Fe5 C502 H502 . . . 127.4(15) ? C501 C502 C503 . . . 108.65(19) ? C501 C502 H502 . . . 127.7(14) ? C503 C502 H502 . . . 123.6(14) ? Fe5 C503 C502 . . . 69.01(13) ? Fe5 C503 C504 . . . 70.13(13) ? Fe5 C503 H503 . . . 124.8(17) ? C502 C503 C504 . . . 107.94(19) ? C502 C503 H503 . . . 126.3(17) ? C504 C503 H503 . . . 125.7(17) ? Fe5 C504 C503 . . . 69.54(12) ? Fe5 C504 C505 . . . 69.09(12) ? Fe5 C504 H504 . . . 125(2) ? C503 C504 C505 . . . 108.50(18) ? C503 C504 H504 . . . 130(2) ? C505 C504 H504 . . . 121(2) ? Fe5 C505 C501 . . . 69.35(11) ? Fe5 C505 C504 . . . 70.45(12) ? Fe5 C505 H505 . . . 127.6(17) ? C501 C505 C504 . . . 108.7(2) ? C501 C505 H505 . . . 124.0(15) ? C504 C505 H505 . . . 127.3(15) ? Fe5 C501' C502' . . . 69.56(14) ? Fe5 C501' C505' . . . 69.73(15) ? Fe5 C501' H501' . . . 121.7(18) ? C502' C501' C505' . . . 108.2(2) ? C502' C501' H501' . . . 125(2) ? C505' C501' H501' . . . 126(2) ? Fe5 C502' C501' . . . 69.77(14) ? Fe5 C502' C503' . . . 69.59(14) ? Fe5 C502' H502' . . . 122(2) ? C501' C502' C503' . . . 107.6(3) ? C501' C502' H502' . . . 121.7(18) ? C503' C502' H502' . . . 130.5(19) ? Fe5 C503' C502' . . . 69.96(14) ? Fe5 C503' C504' . . . 69.85(15) ? Fe5 C503' H503' . . . 122(2) ? C502' C503' C504' . . . 108.7(3) ? C502' C503' H503' . . . 126(3) ? C504' C503' H503' . . . 126(2) ? Fe5 C504' C503' . . . 69.64(15) ? Fe5 C504' C505' . . . 69.81(15) ? Fe5 C504' H504' . . . 124(2) ? C503' C504' C505' . . . 107.8(2) ? C503' C504' H504' . . . 125(2) ? C505' C504' H504' . . . 127(2) ? Fe5 C505' C501' . . . 69.71(16) ? Fe5 C505' C504' . . . 69.43(16) ? Fe5 C505' H505' . . . 129(2) ? C501' C505' C504' . . . 107.7(2) ? C501' C505' H505' . . . 125.5(17) ? C504' C505' H505' . . . 126.7(17) ? Ru2 C6 C3 . . . 68.06(11) ? Ru2 C6 C7 . . . 82.02(13) ? Ru2 C6 H6 . . . 123.2(17) ? C3 C6 C7 . . . 128.44(18) ? C3 C6 H6 . . . 116.6(18) ? C7 C6 H6 . . . 114.9(18) ? Ru2 C7 Ru3 . . . 72.71(6) ? Ru2 C7 C6 . . . 64.64(11) ? Ru2 C7 C701 . . . 133.27(15) ? Ru3 C7 C6 . . . 126.22(14) ? Ru3 C7 C701 . . . 119.91(16) ? C6 C7 C701 . . . 113.04(18) ? Fe7 C701 C7 . . . 125.51(16) ? Fe7 C701 C702 . . . 68.72(13) ? Fe7 C701 C705 . . . 69.05(14) ? C7 C701 C702 . . . 126.7(2) ? C7 C701 C705 . . . 127.2(2) ? C702 C701 C705 . . . 106.06(18) ? Fe7 C702 C701 . . . 70.19(13) ? Fe7 C702 C703 . . . 70.27(14) ? Fe7 C702 H702 . . . 123.4(19) ? C701 C702 C703 . . . 108.8(2) ? C701 C702 H702 . . . 123.3(16) ? C703 C702 H702 . . . 127.9(16) ? Fe7 C703 C702 . . . 69.18(13) ? Fe7 C703 C704 . . . 69.72(14) ? Fe7 C703 H703 . . . 128.0(17) ? C702 C703 C704 . . . 108.2(2) ? C702 C703 H703 . . . 126.7(17) ? C704 C703 H703 . . . 125.1(17) ? Fe7 C704 C703 . . . 69.96(15) ? Fe7 C704 C705 . . . 69.72(15) ? Fe7 C704 H704 . . . 122(2) ? C703 C704 C705 . . . 108.3(2) ? C703 C704 H704 . . . 125.5(18) ? C705 C704 H704 . . . 126.0(18) ? Fe7 C705 C701 . . . 69.79(14) ? Fe7 C705 C704 . . . 69.85(15) ? Fe7 C705 H705 . . . 122(2) ? C701 C705 C704 . . . 108.7(2) ? C701 C705 H705 . . . 126(2) ? C704 C705 H705 . . . 125(2) ? Fe7 C701' C702' . . . 69.94(17) ? Fe7 C701' C705' . . . 69.67(17) ? Fe7 C701' H701' . . . 125(3) ? C702' C701' C705' . . . 108.3(3) ? C702' C701' H701' . . . 120(3) ? C705' C701' H701' . . . 132(3) ? Fe7 C702' C701' . . . 70.04(18) ? Fe7 C702' C703' . . . 69.40(19) ? Fe7 C702' H702' . . . 121(2) ? C701' C702' C703' . . . 107.4(3) ? C701' C702' H702' . . . 120.4(17) ? C703' C702' H702' . . . 132.0(17) ? Fe7 C703' C702' . . . 69.88(18) ? Fe7 C703' C704' . . . 70.4(2) ? Fe7 C703' H703' . . . 134(3) ? C702' C703' C704' . . . 108.4(3) ? C702' C703' H703' . . . 123(3) ? C704' C703' H703' . . . 128(3) ? Fe7 C704' C703' . . . 69.48(18) ? Fe7 C704' C705' . . . 69.61(18) ? Fe7 C704' H704' . . . 129(2) ? C703' C704' C705' . . . 107.7(3) ? C703' C704' H704' . . . 126(2) ? C705' C704' H704' . . . 126.1(19) ? Fe7 C705' C701' . . . 69.93(17) ? Fe7 C705' C704' . . . 70.21(18) ? Fe7 C705' H705' . . . 122(2) ? C701' C705' C704' . . . 108.2(3) ? C701' C705' H705' . . . 125(2) ? C704' C705' H705' . . . 127(2) ? C02 C01 C06 . . . 122.3(4) ? C02 C01 H01 . . . 119.0 ? C06 C01 H01 . . . 118.7 ? C01 C02 C03 . . . 117.6(4) ? C01 C02 H02 . . . 121.4 ? C03 C02 H02 . . . 121.0 ? C02 C03 C04 . . . 122.0(4) ? C02 C03 H03 . . . 118.7 ? C04 C03 H03 . . . 119.3 ? C03 C04 C05 . . . 115.7(4) ? C03 C04 H04 . . . 122.1 ? C05 C04 H04 . . . 122.1 ? C04 C05 C06 . . . 122.4(4) ? C04 C05 H05 . . . 119.1 ? C06 C05 H05 . . . 118.5 ? C01 C06 C05 . . . 119.8(4) ? C01 C06 H06 . . . 119.6 ? C05 C06 H06 . . . 120.5 ? _exptl_crystal_F_000 2464 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 28 _reflns_limit_k_min 0 _reflns_limit_k_max 31 _reflns_limit_l_min -26 _reflns_limit_l_max 25 _reflns_number_observed ? _reflns_d_resolution_high .581 _reflns_d_resolution_low 12.156 _diffrn_reflns_av_sigmaI/netI .088 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .065 _refine_ls_wR_factor_all .045 _refine_ls_goodness_of_fit_all 1.018 _refine_ls_shift/su_mean .0008 data_br803 _database_code_CSD 175564 _audit_creation_method Xtal3.6 _audit_creation_date 01-08-27 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C48 H30 Fe2 O10 Ru3' _chemical_formula_moiety ? _chemical_formula_weight 1181.66 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 17.094(3) _cell_length_b 13.413(2) _cell_length_c 18.535(3) _cell_angle_alpha 90.00000 _cell_angle_beta 92.187(4) _cell_angle_gamma 90.00000 _cell_volume 4246.6(12) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 18.4 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 1.77 _exptl_crystal_description prism _exptl_crystal_size_max .18 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .05 _exptl_crystal_size_rad ? _exptl_crystal_colour dark_red _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .64 _exptl_absorpt_correction_T_max .79 _diffrn_reflns_number 88304 _reflns_number_total 15151 _reflns_Friedel_coverage 0 _reflns_number_gt 8668 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.58 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .091 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .042 _refine_ls_wR_factor_ref .036 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_number_reflns 8668 _refine_ls_number_parameters 564 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .062 _refine_diff_density_min -.713 _refine_diff_density_max 1.394 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 192 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 120 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Fe ? 0 8 .301 .845 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 40 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 12 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 .166256(19) .42404(2) .073844(15) .02175(15) Uani ? ? 1.00000 ? ? Ru2 .305023(19) .40844(2) -.002824(15) .02061(15) Uani ? ? 1.00000 ? ? Ru3 .354617(19) .36383(2) .138112(15) .02168(15) Uani ? ? 1.00000 ? ? Fe5 .40490(3) -.09252(4) .14274(3) .0262(3) Uani ? ? 1.00000 ? ? Fe7 .20198(4) -.12869(4) -.13219(3) .0287(3) Uani ? ? 1.00000 ? ? O0 .23615(15) .38449(17) .16487(12) .0250(14) Uani ? ? 1.00000 ? ? C11 .1955(2) .5602(3) .08796(19) .027(2) Uani ? ? 1.00000 ? ? O11 .21021(17) .64205(19) .09559(15) .0386(17) Uani ? ? 1.00000 ? ? C12 .1074(2) .4686(3) -.0081(2) .027(2) Uani ? ? 1.00000 ? ? O12 .07180(16) .5034(2) -.05490(14) .0388(17) Uani ? ? 1.00000 ? ? C13 .0754(2) .4116(3) .1341(2) .031(2) Uani ? ? 1.00000 ? ? O13 .02601(17) .4029(2) .17229(15) .0425(18) Uani ? ? 1.00000 ? ? C21 .3507(2) .5351(3) .0215(2) .028(2) Uani ? ? 1.00000 ? ? O21 .37643(18) .61151(19) .03451(15) .0389(17) Uani ? ? 1.00000 ? ? C22 .3946(2) .3687(3) -.0547(2) .030(2) Uani ? ? 1.00000 ? ? O22 .44711(17) .3470(2) -.08658(15) .045(2) Uani ? ? 1.00000 ? ? C23 .2512(2) .4477(3) -.0918(2) .027(2) Uani ? ? 1.00000 ? ? O23 .22321(17) .4739(2) -.14547(14) .0401(17) Uani ? ? 1.00000 ? ? C31 .3941(2) .4887(3) .18102(19) .027(2) Uani ? ? 1.00000 ? ? O31 .42186(17) .5597(2) .20304(14) .0372(17) Uani ? ? 1.00000 ? ? C32 .4557(2) .3403(3) .10685(19) .030(2) Uani ? ? 1.00000 ? ? O32 .51738(17) .3266(2) .08788(15) .0414(18) Uani ? ? 1.00000 ? ? C33 .3634(2) .2802(3) .2229(2) .033(2) Uani ? ? 1.00000 ? ? O33 .3667(2) .2277(2) .27086(15) .055(2) Uani ? ? 1.00000 ? ? C1 .1552(2) .2556(2) .02567(17) .022(2) Uani ? ? 1.00000 ? ? C111 .1051(2) .2632(2) -.04251(18) .025(2) Uani ? ? 1.00000 ? ? C112 .1377(2) .2536(3) -.10960(19) .028(2) Uani ? ? 1.00000 ? ? C113 .0903(3) .2520(3) -.1724(2) .042(3) Uani ? ? 1.00000 ? ? C114 .0108(3) .2609(3) -.1688(2) .045(3) Uani ? ? 1.00000 ? ? C115 -.0223(3) .2700(3) -.1037(2) .044(3) Uani ? ? 1.00000 ? ? C116 .0238(2) .2718(3) -.0405(2) .033(2) Uani ? ? 1.00000 ? ? C121 .1337(2) .1705(3) .07457(18) .024(2) Uani ? ? 1.00000 ? ? C122 .1553(2) .1694(3) .1476(2) .031(2) Uani ? ? 1.00000 ? ? C123 .1361(3) .0881(3) .1908(2) .037(2) Uani ? ? 1.00000 ? ? C124 .0959(3) .0081(3) .1618(2) .038(2) Uani ? ? 1.00000 ? ? C125 .0754(3) .0071(3) .0895(2) .039(3) Uani ? ? 1.00000 ? ? C126 .0942(2) .0876(3) .0460(2) .033(2) Uani ? ? 1.00000 ? ? C2 .2312(2) .2935(2) .03194(17) .0205(18) Uani ? ? 1.00000 ? ? C3 .3034(2) .2654(2) .06346(17) .0216(19) Uani ? ? 1.00000 ? ? C4 .3344(2) .1652(2) .04272(18) .0207(19) Uani ? ? 1.00000 ? ? C5 .3923(2) .1211(2) .08246(18) .024(2) Uani ? ? 1.00000 ? ? C501 .4279(2) .0241(3) .07541(19) .025(2) Uani ? ? 1.00000 ? ? C502 .4041(2) -.0611(3) .03431(19) .027(2) Uani ? ? 1.00000 ? ? C503 .4578(2) -.1397(3) .0508(2) .032(2) Uani ? ? 1.00000 ? ? C504 .5142(2) -.1040(3) .1023(2) .032(2) Uani ? ? 1.00000 ? ? C505 .4961(2) -.0042(3) .1180(2) .031(2) Uani ? ? 1.00000 ? ? C501' .3222(3) -.0492(3) .2129(2) .045(3) Uani ? ? 1.00000 ? ? C502' .2935(3) -.1289(4) .1690(2) .045(3) Uani ? ? 1.00000 ? ? C503' .3441(3) -.2101(3) .1802(2) .046(3) Uani ? ? 1.00000 ? ? C504' .4023(3) -.1828(3) .2313(2) .043(3) Uani ? ? 1.00000 ? ? C505' .3890(3) -.0829(3) .2518(2) .042(3) Uani ? ? 1.00000 ? ? C6 .2977(2) .1155(2) -.01900(19) .022(2) Uani ? ? 1.00000 ? ? C7 .2690(2) .0722(2) -.0697(2) .025(2) Uani ? ? 1.00000 ? ? C701 .2400(2) .0166(3) -.13155(19) .026(2) Uani ? ? 1.00000 ? ? C702 .1619(2) .0094(3) -.1606(2) .035(2) Uani ? ? 1.00000 ? ? C703 .1616(3) -.0549(3) -.2214(2) .036(2) Uani ? ? 1.00000 ? ? C704 .2381(3) -.0875(3) -.2306(2) .036(2) Uani ? ? 1.00000 ? ? C705 .2873(2) -.0452(3) -.1749(2) .032(2) Uani ? ? 1.00000 ? ? C701' .1959(5) -.1683(6) -.0264(4) .0306(18) Uiso ? ? .50000 ? ? C702' .1181(6) -.1781(7) -.0638(5) .047(2) Uiso ? ? .50000 ? ? C703' .1379(5) -.2572(6) -.1254(4) .040(2) Uiso ? ? .50000 ? ? C704' .2214(5) -.2814(6) -.1284(4) .0303(18) Uiso ? ? .50000 ? ? C705' .2588(5) -.2311(6) -.0649(4) .0308(18) Uiso ? ? .50000 ? ? C701" .2281(5) -.2048(6) -.0392(4) .039(2) Uiso ? ? .50000 ? ? C702" .1494(6) -.1916(7) -.0493(5) .050(2) Uiso ? ? .50000 ? ? C703" .1180(6) -.2309(7) -.1079(5) .051(2) Uiso ? ? .50000 ? ? C704" .1769(6) -.2757(7) -.1306(5) .056(3) Uiso ? ? .50000 ? ? C705" .2423(8) -.2607(10) -.0965(7) .086(4) Uiso ? ? .50000 ? ? H0 .23286 .42206 .19252 .03909 Uiso ? ? 1.00000 ? ? H112 .19384 .24817 -.11196 .03600 Uiso ? ? 1.00000 ? ? H113 .11377 .24408 -.21884 .05100 Uiso ? ? 1.00000 ? ? H114 -.02132 .26033 -.21316 .05600 Uiso ? ? 1.00000 ? ? H115 -.07855 .27586 -.10155 .05500 Uiso ? ? 1.00000 ? ? H116 -.00085 .28007 .00575 .04200 Uiso ? ? 1.00000 ? ? H122 .18368 .22522 .16888 .03700 Uiso ? ? 1.00000 ? ? H123 .15053 .08879 .24179 .04500 Uiso ? ? 1.00000 ? ? H124 .08196 -.04731 .19242 .04700 Uiso ? ? 1.00000 ? ? H125 .04722 -.04949 .06871 .04800 Uiso ? ? 1.00000 ? ? H126 .07968 .08609 -.00521 .03900 Uiso ? ? 1.00000 ? ? H5 .41295 .16025 .12226 .03000 Uiso ? ? 1.00000 ? ? H502 .35884 -.06498 .00144 .03300 Uiso ? ? 1.00000 ? ? H503 .45563 -.20593 .02977 .03800 Uiso ? ? 1.00000 ? ? H504 .55788 -.14229 .12282 .04000 Uiso ? ? 1.00000 ? ? H505 .52541 .03853 .15201 .03900 Uiso ? ? 1.00000 ? ? H501' .29837 .01687 .21598 .05400 Uiso ? ? 1.00000 ? ? H502' .24756 -.12712 .13640 .05500 Uiso ? ? 1.00000 ? ? H503' .33826 -.27426 .15674 .05500 Uiso ? ? 1.00000 ? ? H504' .44477 -.22441 .24912 .05200 Uiso ? ? 1.00000 ? ? H505' .42036 -.04408 .28599 .05200 Uiso ? ? 1.00000 ? ? H702 .11592 .04144 -.14140 .04300 Uiso ? ? 1.00000 ? ? H703 .11585 -.07251 -.25184 .04400 Uiso ? ? 1.00000 ? ? H704 .25398 -.12999 -.26877 .04500 Uiso ? ? 1.00000 ? ? H705 .34267 -.05688 -.16781 .04000 Uiso ? ? 1.00000 ? ? H701' .20894 -.13003 .01553 .08400 Uiso ? ? .50000 ? ? H702' .07140 -.14861 -.05350 .10100 Uiso ? ? .50000 ? ? H703' .09787 -.28415 -.15514 .07500 Uiso ? ? .50000 ? ? H704' .24251 -.32092 -.16461 .08900 Uiso ? ? .50000 ? ? H705' .31367 -.23827 -.05318 .08500 Uiso ? ? .50000 ? ? H701" .26668 -.18554 -.00440 .08400 Uiso ? ? .50000 ? ? H702" .12402 -.15280 -.01287 .10100 Uiso ? ? .50000 ? ? H703" .06444 -.22455 -.12659 .05900 Uiso ? ? .50000 ? ? H704" .16838 -.31809 -.17220 .06200 Uiso ? ? .50000 ? ? H705" .29024 -.28911 -.11356 .08900 Uiso ? ? .50000 ? ? 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 Ru1 .0236(2) .02124(13) .02041(14) .00151(13) .00062(12) .00020(11) Ru2 .0236(2) .02000(13) .01820(13) -.00198(13) .00069(12) .00058(11) Ru3 .0249(2) .02105(13) .01889(14) -.00015(13) -.00212(12) -.00217(11) Fe5 .0283(4) .0254(3) .0250(3) .0027(2) .0020(2) .0035(2) Fe7 .0367(4) .0243(3) .0253(3) -.0049(3) .0016(2) .0004(2) O0 .0292(17) .0264(13) .0194(12) .0014(11) -.0007(11) -.0049(9) C11 .029(3) .0280(18) .0237(19) .0016(17) .0007(16) .0020(14) O11 .049(2) .0248(13) .0422(17) -.0005(13) -.0006(14) .0021(12) C12 .023(3) .0263(18) .031(2) .0018(16) .0027(17) .0031(15) O12 .041(2) .0400(16) .0352(16) .0044(14) -.0062(14) .0082(12) C13 .032(3) .035(2) .025(2) .0026(18) -.0053(17) -.0004(16) O13 .033(2) .062(2) .0336(16) -.0023(15) .0073(13) .0034(14) C21 .028(3) .0294(19) .025(2) -.0017(17) .0024(17) .0021(15) O21 .049(2) .0306(15) .0370(16) -.0156(13) .0008(14) .0001(12) C22 .033(3) .032(2) .025(2) -.0032(18) -.0020(17) .0037(15) O22 .035(2) .061(2) .0397(18) .0101(16) .0101(14) -.0018(14) C23 .031(3) .0260(18) .025(2) -.0043(17) .0033(17) -.0010(14) O23 .049(2) .0434(17) .0267(15) -.0078(15) -.0080(14) .0096(12) C31 .026(3) .0299(19) .024(2) .0034(17) -.0010(16) -.0018(15) O31 .042(2) .0317(15) .0382(16) -.0070(13) .0002(14) -.0079(12) C32 .038(3) .0281(19) .0229(19) -.0011(18) -.0062(17) -.0045(14) O32 .030(2) .0549(19) .0397(17) -.0003(15) .0042(13) -.0095(14) C33 .036(3) .031(2) .030(2) -.0006(18) -.0072(18) -.0058(16) O33 .083(3) .0448(18) .0362(18) -.0056(17) -.0118(17) .0158(14) C1 .027(2) .0213(16) .0184(17) .0001(15) .0014(15) .0010(13) C111 .028(3) .0210(16) .0242(19) -.0036(16) -.0049(16) .0024(13) C112 .036(3) .0239(18) .024(2) -.0055(17) -.0030(17) .0007(14) C113 .065(3) .035(2) .025(2) -.005(2) -.009(2) .0013(17) C114 .050(3) .036(2) .047(3) -.006(2) -.024(2) .006(2) C115 .031(3) .035(2) .063(3) -.001(2) -.017(2) .002(2) C116 .029(3) .033(2) .037(2) -.0029(18) -.0046(18) .0040(17) C121 .019(2) .0263(17) .0250(19) .0018(16) .0026(16) .0020(14) C122 .041(3) .0274(19) .024(2) -.0049(18) .0004(18) .0019(15) C123 .051(3) .035(2) .026(2) .003(2) .0056(19) .0105(17) C124 .044(3) .028(2) .043(3) -.005(2) .012(2) .0113(17) C125 .039(3) .032(2) .047(3) -.010(2) .000(2) .0042(18) C126 .033(3) .035(2) .031(2) -.0074(19) .0007(18) .0039(17) C2 .026(2) .0199(15) .0153(16) -.0016(15) .0029(14) .0006(12) C3 .026(2) .0203(16) .0186(17) .0001(15) .0006(15) .0010(13) C4 .022(2) .0201(15) .0200(17) -.0039(15) .0029(15) -.0014(13) C5 .026(3) .0237(17) .0232(18) -.0017(16) .0010(16) -.0006(13) C501 .023(3) .0256(18) .026(2) -.0002(16) .0035(16) .0036(14) C502 .032(3) .0255(18) .0234(19) .0035(17) .0021(16) .0019(14) C503 .039(3) .0257(18) .033(2) .0078(18) .0108(18) .0003(16) C504 .021(3) .035(2) .041(2) .0082(18) .0034(18) .0048(17) C505 .026(3) .029(2) .039(2) -.0003(18) .0006(19) .0044(16) C501' .051(3) .048(3) .037(2) .009(2) .018(2) .006(2) C502' .033(3) .064(3) .038(3) -.006(2) .008(2) .012(2) C503' .057(3) .038(2) .043(3) -.013(2) .014(2) .005(2) C504' .047(3) .049(3) .035(2) .008(2) .005(2) .019(2) C505' .050(3) .054(3) .023(2) -.004(2) .004(2) .0026(19) C6 .019(2) .0206(16) .0265(19) .0031(15) .0037(15) .0002(13) C7 .022(3) .0215(17) .032(2) .0017(16) -.0003(16) .0003(14) C701 .029(3) .0219(17) .026(2) -.0034(16) -.0022(17) .0010(14) C702 .034(3) .026(2) .043(2) .0023(18) -.011(2) -.0049(16) C703 .047(3) .027(2) .032(2) -.006(2) -.014(2) -.0012(16) C704 .048(3) .038(2) .023(2) -.010(2) .0085(18) -.0064(17) C705 .036(3) .036(2) .025(2) -.0061(19) .0075(18) -.0055(16) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ru1 Ru2 . . 2.8191(6) ? Ru1 Ru3 . . 3.4851(7) ? Ru1 O0 . . 2.098(2) ? Ru1 C11 . . 1.909(4) ? Ru1 C12 . . 1.886(4) ? Ru1 C13 . . 1.954(4) ? Ru1 C1 . . 2.434(3) ? Ru1 C2 . . 2.228(3) ? Ru2 Ru3 . . 2.7806(6) ? Ru2 C21 . . 1.917(4) ? Ru2 C22 . . 1.914(4) ? Ru2 C23 . . 1.930(4) ? Ru2 C2 . . 2.109(3) ? Ru2 C3 . . 2.279(3) ? Ru3 O0 . . 2.121(3) ? Ru3 C31 . . 1.963(4) ? Ru3 C32 . . 1.871(4) ? Ru3 C33 . . 1.932(4) ? Ru3 C3 . . 2.082(3) ? Fe5 C501 . . 2.049(4) ? Fe5 C502 . . 2.053(4) ? Fe5 C503 . . 2.058(4) ? Fe5 C504 . . 2.046(4) ? Fe5 C505 . . 2.025(4) ? Fe5 C501' . . 2.042(5) ? Fe5 C502' . . 2.043(5) ? Fe5 C503' . . 2.026(5) ? Fe5 C504' . . 2.042(4) ? Fe5 C505' . . 2.053(4) ? Fe7 C701 . . 2.054(3) ? Fe7 C702 . . 2.037(4) ? Fe7 C703 . . 2.026(4) ? Fe7 C704 . . 2.024(4) ? Fe7 C705 . . 2.024(4) ? Fe7 C701' . . 2.039(8) ? Fe7 C702' . . 2.059(10) ? Fe7 C703' . . 2.049(9) ? Fe7 C704' . . 2.075(7) ? Fe7 C705' . . 2.073(8) ? Fe7 C701" . . 2.037(8) ? Fe7 C702" . . 1.996(10) ? Fe7 C703" . . 2.047(10) ? Fe7 C704" . . 2.019(10) ? Fe7 C705" . . 2.003(13) ? O0 H0 . . .722 ? C11 O11 . . 1.134(4) ? C12 O12 . . 1.141(4) ? C13 O13 . . 1.129(5) ? C21 O21 . . 1.137(4) ? C22 O22 . . 1.132(5) ? C23 O23 . . 1.143(4) ? C31 O31 . . 1.133(4) ? C32 O32 . . 1.138(5) ? C33 O33 . . 1.134(5) ? C1 C111 . . 1.503(5) ? C1 C121 . . 1.512(5) ? C1 C2 . . 1.395(5) ? C111 C112 . . 1.388(5) ? C111 C116 . . 1.395(6) ? C112 C113 . . 1.392(5) ? C112 H112 . . .965 ? C113 C114 . . 1.368(7) ? C113 H113 . . .970 ? C114 C115 . . 1.358(6) ? C114 H114 . . .972 ? C115 C116 . . 1.386(6) ? C115 H115 . . .967 ? C116 H116 . . .977 ? C121 C122 . . 1.390(5) ? C121 C126 . . 1.395(5) ? C122 C123 . . 1.399(5) ? C122 H122 . . .968 ? C123 C124 . . 1.372(6) ? C123 H123 . . .968 ? C124 C125 . . 1.372(6) ? C124 H124 . . .971 ? C125 C126 . . 1.391(6) ? C125 H125 . . .971 ? C126 H126 . . .972 ? C2 C3 . . 1.397(5) ? C3 C4 . . 1.500(5) ? C4 C5 . . 1.348(5) ? C4 C6 . . 1.446(5) ? C5 C501 . . 1.445(5) ? C5 H5 . . .961 ? C501 C502 . . 1.425(5) ? C501 C505 . . 1.434(5) ? C502 C503 . . 1.423(5) ? C502 H502 . . .967 ? C503 C504 . . 1.414(6) ? C503 H503 . . .971 ? C504 C505 . . 1.408(5) ? C504 H504 . . .971 ? C505 H505 . . .976 ? C501' C502' . . 1.419(6) ? C501' C505' . . 1.402(6) ? C501' H501' . . .978 ? C502' C503' . . 1.402(6) ? C502' H502' . . .972 ? C503' C504' . . 1.396(6) ? C503' H503' . . .968 ? C504' C505' . . 1.412(6) ? C504' H504' . . .964 ? C505' H505' . . .967 ? C6 C7 . . 1.195(5) ? C7 C701 . . 1.440(5) ? C701 C702 . . 1.425(6) ? C701 C705 . . 1.427(5) ? C702 C703 . . 1.419(5) ? C702 H702 . . .975 ? C703 C704 . . 1.394(6) ? C703 H703 . . .976 ? C704 C705 . . 1.424(6) ? C704 H704 . . .957 ? C705 H705 . . .963 ? C701' C702' . . 1.483(12) ? C701' C705' . . 1.560(11) ? C701' H701' . . .950 ? C702' C703' . . 1.604(12) ? C702' H702' . . .918 ? C703' C704' . . 1.467(12) ? C703' H703' . . .934 ? C704' C705' . . 1.481(11) ? C704' H704' . . .939 ? C705' H705' . . .959 ? C701" C702" . . 1.362(13) ? C701" C705" . . 1.329(15) ? C701" H701" . . .941 ? C702" C703" . . 1.303(13) ? C702" C704" . . 1.954(14) ? C702" H702" . . .969 ? C703" C704" . . 1.259(14) ? C703" H703" . . .971 ? C704" C705" . . 1.281(16) ? C704" H704" . . .964 ? C705" H705" . . .968 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Ru2 Ru1 Ru3 . . . 51.017(14) ? Ru2 Ru1 O0 . . . 85.54(7) ? Ru2 Ru1 C11 . . . 85.35(12) ? Ru2 Ru1 C12 . . . 92.92(12) ? Ru2 Ru1 C13 . . . 169.75(11) ? Ru2 Ru1 C1 . . . 78.52(9) ? Ru2 Ru1 C2 . . . 47.65(9) ? Ru3 Ru1 O0 . . . 34.53(7) ? Ru3 Ru1 C11 . . . 86.61(12) ? Ru3 Ru1 C12 . . . 143.71(12) ? Ru3 Ru1 C13 . . . 121.93(11) ? Ru3 Ru1 C1 . . . 88.16(9) ? Ru3 Ru1 C2 . . . 58.08(9) ? O0 Ru1 C11 . . . 89.62(13) ? O0 Ru1 C12 . . . 175.77(13) ? O0 Ru1 C13 . . . 87.68(13) ? O0 Ru1 C1 . . . 95.40(10) ? O0 Ru1 C2 . . . 78.80(10) ? C11 Ru1 C12 . . . 86.33(15) ? C11 Ru1 C13 . . . 102.32(16) ? C11 Ru1 C1 . . . 162.65(14) ? C11 Ru1 C2 . . . 131.92(15) ? C12 Ru1 C13 . . . 94.35(16) ? C12 Ru1 C1 . . . 88.15(13) ? C12 Ru1 C2 . . . 103.06(14) ? C13 Ru1 C1 . . . 94.49(14) ? C13 Ru1 C2 . . . 123.31(14) ? C1 Ru1 C2 . . . 34.45(13) ? Ru1 Ru2 Ru3 . . . 76.976(15) ? Ru1 Ru2 C21 . . . 99.13(12) ? Ru1 Ru2 C22 . . . 168.04(11) ? Ru1 Ru2 C23 . . . 91.55(12) ? Ru1 Ru2 C2 . . . 51.33(9) ? Ru1 Ru2 C3 . . . 76.27(9) ? Ru3 Ru2 C21 . . . 82.12(11) ? Ru3 Ru2 C22 . . . 101.03(11) ? Ru3 Ru2 C23 . . . 168.33(12) ? Ru3 Ru2 C2 . . . 73.76(9) ? Ru3 Ru2 C3 . . . 47.31(8) ? C21 Ru2 C22 . . . 92.21(16) ? C21 Ru2 C23 . . . 97.81(15) ? C21 Ru2 C2 . . . 145.03(14) ? C21 Ru2 C3 . . . 129.26(14) ? C22 Ru2 C23 . . . 90.64(16) ? C22 Ru2 C2 . . . 116.72(15) ? C22 Ru2 C3 . . . 93.63(14) ? C23 Ru2 C2 . . . 100.87(14) ? C23 Ru2 C3 . . . 132.42(14) ? C2 Ru2 C3 . . . 36.87(13) ? Ru1 Ru3 Ru2 . . . 52.007(10) ? Ru1 Ru3 O0 . . . 34.10(6) ? Ru1 Ru3 C31 . . . 103.89(11) ? Ru1 Ru3 C32 . . . 141.79(11) ? Ru1 Ru3 C33 . . . 117.03(12) ? Ru1 Ru3 C3 . . . 63.88(10) ? Ru2 Ru3 O0 . . . 86.10(6) ? Ru2 Ru3 C31 . . . 106.56(10) ? Ru2 Ru3 C32 . . . 89.85(11) ? Ru2 Ru3 C33 . . . 154.22(11) ? Ru2 Ru3 C3 . . . 53.59(9) ? O0 Ru3 C31 . . . 96.35(13) ? O0 Ru3 C32 . . . 174.89(13) ? O0 Ru3 C33 . . . 86.03(14) ? O0 Ru3 C3 . . . 81.78(12) ? C31 Ru3 C32 . . . 87.79(16) ? C31 Ru3 C33 . . . 98.69(15) ? C31 Ru3 C3 . . . 160.08(14) ? C32 Ru3 C33 . . . 96.33(17) ? C32 Ru3 C3 . . . 93.31(15) ? C33 Ru3 C3 . . . 100.95(14) ? C501 Fe5 C502 . . . 40.65(14) ? C501 Fe5 C503 . . . 68.28(14) ? C501 Fe5 C504 . . . 68.61(15) ? C501 Fe5 C505 . . . 41.22(15) ? C501 Fe5 C501' . . . 108.94(16) ? C501 Fe5 C502' . . . 121.98(17) ? C501 Fe5 C503' . . . 156.37(17) ? C501 Fe5 C504' . . . 162.41(16) ? C501 Fe5 C505' . . . 125.97(16) ? C502 Fe5 C503 . . . 40.50(15) ? C502 Fe5 C504 . . . 68.23(16) ? C502 Fe5 C505 . . . 68.58(15) ? C502 Fe5 C501' . . . 125.89(17) ? C502 Fe5 C502' . . . 108.08(17) ? C502 Fe5 C503' . . . 120.72(16) ? C502 Fe5 C504' . . . 155.42(16) ? C502 Fe5 C505' . . . 162.63(16) ? C503 Fe5 C504 . . . 40.31(16) ? C503 Fe5 C505 . . . 68.03(15) ? C503 Fe5 C501' . . . 162.04(17) ? C503 Fe5 C502' . . . 124.51(17) ? C503 Fe5 C503' . . . 106.96(16) ? C503 Fe5 C504' . . . 120.49(16) ? C503 Fe5 C505' . . . 155.88(17) ? C504 Fe5 C505 . . . 40.45(15) ? C504 Fe5 C501' . . . 156.85(17) ? C504 Fe5 C502' . . . 160.44(17) ? C504 Fe5 C503' . . . 123.68(17) ? C504 Fe5 C504' . . . 107.36(17) ? C504 Fe5 C505' . . . 121.50(17) ? C505 Fe5 C501' . . . 122.41(17) ? C505 Fe5 C502' . . . 157.93(17) ? C505 Fe5 C503' . . . 160.51(18) ? C505 Fe5 C504' . . . 124.74(17) ? C505 Fe5 C505' . . . 108.57(17) ? C501' Fe5 C502' . . . 40.67(18) ? C501' Fe5 C503' . . . 68.05(18) ? C501' Fe5 C504' . . . 67.62(18) ? C501' Fe5 C505' . . . 40.03(18) ? C502' Fe5 C503' . . . 40.30(19) ? C502' Fe5 C504' . . . 67.52(18) ? C502' Fe5 C505' . . . 67.72(18) ? C503' Fe5 C504' . . . 40.14(18) ? C503' Fe5 C505' . . . 67.82(18) ? C504' Fe5 C505' . . . 40.34(17) ? C701 Fe7 C702 . . . 40.77(16) ? C701 Fe7 C703 . . . 68.86(15) ? C701 Fe7 C704 . . . 68.83(15) ? C701 Fe7 C705 . . . 40.94(15) ? C701 Fe7 C701' . . . 105.6(2) ? C701 Fe7 C702' . . . 122.0(3) ? C701 Fe7 C703' . . . 165.4(3) ? C701 Fe7 C704' . . . 152.3(2) ? C701 Fe7 C705' . . . 119.0(2) ? C701 Fe7 C701" . . . 114.3(3) ? C701 Fe7 C702" . . . 123.2(3) ? C701 Fe7 C703" . . . 149.1(3) ? C701 Fe7 C704" . . . 173.8(3) ? C701 Fe7 C705" . . . 137.0(4) ? C702 Fe7 C703 . . . 40.88(16) ? C702 Fe7 C704 . . . 68.28(17) ? C702 Fe7 C705 . . . 68.68(17) ? C702 Fe7 C701' . . . 117.2(2) ? C702 Fe7 C702' . . . 102.5(3) ? C702 Fe7 C703' . . . 127.2(3) ? C702 Fe7 C704' . . . 163.2(2) ? C702 Fe7 C705' . . . 154.7(2) ? C702 Fe7 C701" . . . 137.3(3) ? C702 Fe7 C702" . . . 115.2(3) ? C702 Fe7 C703" . . . 115.7(3) ? C702 Fe7 C704" . . . 145.3(3) ? C702 Fe7 C705" . . . 175.6(4) ? C703 Fe7 C704 . . . 40.28(18) ? C703 Fe7 C705 . . . 68.81(17) ? C703 Fe7 C701' . . . 152.2(3) ? C703 Fe7 C702' . . . 115.9(3) ? C703 Fe7 C703' . . . 107.1(3) ? C703 Fe7 C704' . . . 124.0(2) ? C703 Fe7 C705' . . . 162.3(2) ? C703 Fe7 C701" . . . 172.7(3) ? C703 Fe7 C702" . . . 133.3(3) ? C703 Fe7 C703" . . . 106.7(3) ? C703 Fe7 C704" . . . 115.0(3) ? C703 Fe7 C705" . . . 143.5(4) ? C704 Fe7 C705 . . . 41.20(16) ? C704 Fe7 C701' . . . 165.1(3) ? C704 Fe7 C702' . . . 152.3(3) ? C704 Fe7 C703' . . . 117.8(3) ? C704 Fe7 C704' . . . 104.3(2) ? C704 Fe7 C705' . . . 124.9(3) ? C704 Fe7 C701" . . . 146.5(3) ? C704 Fe7 C702" . . . 166.0(3) ? C704 Fe7 C703" . . . 128.4(3) ? C704 Fe7 C704" . . . 110.6(3) ? C704 Fe7 C705" . . . 115.2(4) ? C705 Fe7 C701' . . . 125.8(2) ? C705 Fe7 C702' . . . 161.4(3) ? C705 Fe7 C703' . . . 152.2(3) ? C705 Fe7 C704' . . . 116.3(3) ? C705 Fe7 C705' . . . 105.9(3) ? C705 Fe7 C701" . . . 118.0(3) ? C705 Fe7 C702" . . . 152.5(3) ? C705 Fe7 C703" . . . 168.0(3) ? C705 Fe7 C704" . . . 134.7(3) ? C705 Fe7 C705" . . . 112.0(4) ? C701' Fe7 C702' . . . 42.4(3) ? C701' Fe7 C703' . . . 71.0(3) ? C701' Fe7 C704' . . . 74.0(3) ? C701' Fe7 C705' . . . 44.6(3) ? C702' Fe7 C703' . . . 46.0(3) ? C702' Fe7 C704' . . . 77.0(3) ? C702' Fe7 C705' . . . 74.8(3) ? C703' Fe7 C704' . . . 41.7(3) ? C703' Fe7 C705' . . . 69.2(3) ? C704' Fe7 C705' . . . 41.8(3) ? C701" Fe7 C702" . . . 39.5(4) ? C701" Fe7 C703" . . . 67.1(4) ? C701" Fe7 C704" . . . 62.5(4) ? C701" Fe7 C705" . . . 38.4(4) ? C702" Fe7 C703" . . . 37.6(4) ? C702" Fe7 C704" . . . 58.3(4) ? C702" Fe7 C705" . . . 62.1(5) ? C703" Fe7 C704" . . . 36.1(4) ? C703" Fe7 C705" . . . 64.6(5) ? C704" Fe7 C705" . . . 37.1(5) ? Ru1 O0 Ru3 . . . 111.37(11) ? Ru1 O0 H0 . . . 109.7 ? Ru3 O0 H0 . . . 111.0 ? Ru1 C11 O11 . . . 177.5(4) ? Ru1 C12 O12 . . . 174.2(3) ? Ru1 C13 O13 . . . 175.8(3) ? Ru2 C21 O21 . . . 178.1(3) ? Ru2 C22 O22 . . . 178.3(3) ? Ru2 C23 O23 . . . 175.9(3) ? Ru3 C31 O31 . . . 174.9(3) ? Ru3 C32 O32 . . . 179.6(3) ? Ru3 C33 O33 . . . 176.8(3) ? Ru1 C1 C111 . . . 106.2(2) ? Ru1 C1 C121 . . . 119.9(2) ? Ru1 C1 C2 . . . 64.67(18) ? C111 C1 C121 . . . 114.3(3) ? C111 C1 C2 . . . 123.0(3) ? C121 C1 C2 . . . 118.2(3) ? C1 C111 C112 . . . 120.7(3) ? C1 C111 C116 . . . 121.3(3) ? C112 C111 C116 . . . 117.8(3) ? C111 C112 C113 . . . 120.6(4) ? C111 C112 H112 . . . 118.8 ? C113 C112 H112 . . . 120.6 ? C112 C113 C114 . . . 120.3(4) ? C112 C113 H113 . . . 119.7 ? C114 C113 H113 . . . 119.9 ? C113 C114 C115 . . . 120.0(4) ? C113 C114 H114 . . . 119.2 ? C115 C114 H114 . . . 120.8 ? C114 C115 C116 . . . 120.6(4) ? C114 C115 H115 . . . 119.5 ? C116 C115 H115 . . . 119.9 ? C111 C116 C115 . . . 120.7(4) ? C111 C116 H116 . . . 119.8 ? C115 C116 H116 . . . 119.5 ? C1 C121 C122 . . . 122.0(3) ? C1 C121 C126 . . . 120.0(3) ? C122 C121 C126 . . . 117.9(3) ? C121 C122 C123 . . . 120.4(3) ? C121 C122 H122 . . . 119.9 ? C123 C122 H122 . . . 119.7 ? C122 C123 C124 . . . 120.7(4) ? C122 C123 H123 . . . 119.6 ? C124 C123 H123 . . . 119.7 ? C123 C124 C125 . . . 119.7(4) ? C123 C124 H124 . . . 120.0 ? C125 C124 H124 . . . 120.3 ? C124 C125 C126 . . . 120.2(4) ? C124 C125 H125 . . . 119.9 ? C126 C125 H125 . . . 119.9 ? C121 C126 C125 . . . 121.1(4) ? C121 C126 H126 . . . 119.3 ? C125 C126 H126 . . . 119.6 ? Ru1 C2 Ru2 . . . 81.02(11) ? Ru1 C2 C1 . . . 80.9(2) ? Ru1 C2 C3 . . . 120.7(2) ? Ru2 C2 C1 . . . 143.8(3) ? Ru2 C2 C3 . . . 78.2(2) ? C1 C2 C3 . . . 137.8(3) ? Ru2 C3 Ru3 . . . 79.10(11) ? Ru2 C3 C2 . . . 64.94(18) ? Ru2 C3 C4 . . . 127.2(2) ? Ru3 C3 C2 . . . 116.7(2) ? Ru3 C3 C4 . . . 126.5(2) ? C2 C3 C4 . . . 116.7(3) ? C3 C4 C5 . . . 120.8(3) ? C3 C4 C6 . . . 118.0(3) ? C5 C4 C6 . . . 121.2(3) ? C4 C5 C501 . . . 130.5(3) ? C4 C5 H5 . . . 114.9 ? C501 C5 H5 . . . 114.6 ? Fe5 C501 C5 . . . 122.8(3) ? Fe5 C501 C502 . . . 69.8(2) ? Fe5 C501 C505 . . . 68.5(2) ? C5 C501 C502 . . . 131.2(3) ? C5 C501 C505 . . . 121.7(3) ? C502 C501 C505 . . . 107.0(3) ? Fe5 C502 C501 . . . 69.5(2) ? Fe5 C502 C503 . . . 69.9(2) ? Fe5 C502 H502 . . . 125.5 ? C501 C502 C503 . . . 108.1(3) ? C501 C502 H502 . . . 125.8 ? C503 C502 H502 . . . 126.1 ? Fe5 C503 C502 . . . 69.6(2) ? Fe5 C503 C504 . . . 69.4(2) ? Fe5 C503 H503 . . . 127.1 ? C502 C503 C504 . . . 108.3(3) ? C502 C503 H503 . . . 125.3 ? C504 C503 H503 . . . 126.5 ? Fe5 C504 C503 . . . 70.3(2) ? Fe5 C504 C505 . . . 69.0(2) ? Fe5 C504 H504 . . . 126.5 ? C503 C504 C505 . . . 108.1(3) ? C503 C504 H504 . . . 125.5 ? C505 C504 H504 . . . 126.4 ? Fe5 C505 C501 . . . 70.3(2) ? Fe5 C505 C504 . . . 70.6(2) ? Fe5 C505 H505 . . . 125.2 ? C501 C505 C504 . . . 108.6(3) ? C501 C505 H505 . . . 125.9 ? C504 C505 H505 . . . 125.5 ? Fe5 C501' C502' . . . 69.7(3) ? Fe5 C501' C505' . . . 70.4(3) ? Fe5 C501' H501' . . . 126.5 ? C502' C501' C505' . . . 108.0(4) ? C502' C501' H501' . . . 125.4 ? C505' C501' H501' . . . 126.5 ? Fe5 C502' C501' . . . 69.6(3) ? Fe5 C502' C503' . . . 69.2(3) ? Fe5 C502' H502' . . . 125.7 ? C501' C502' C503' . . . 107.6(4) ? C501' C502' H502' . . . 126.3 ? C503' C502' H502' . . . 126.2 ? Fe5 C503' C502' . . . 70.5(3) ? Fe5 C503' C504' . . . 70.5(3) ? Fe5 C503' H503' . . . 125.7 ? C502' C503' C504' . . . 108.4(4) ? C502' C503' H503' . . . 124.9 ? C504' C503' H503' . . . 126.7 ? Fe5 C504' C503' . . . 69.3(2) ? Fe5 C504' C505' . . . 70.3(2) ? Fe5 C504' H504' . . . 125.4 ? C503' C504' C505' . . . 108.3(4) ? C503' C504' H504' . . . 126.0 ? C505' C504' H504' . . . 125.8 ? Fe5 C505' C501' . . . 69.5(2) ? Fe5 C505' C504' . . . 69.4(2) ? Fe5 C505' H505' . . . 126.0 ? C501' C505' C504' . . . 107.7(4) ? C501' C505' H505' . . . 125.7 ? C504' C505' H505' . . . 126.6 ? C4 C6 C7 . . . 178.1(4) ? C6 C7 C701 . . . 175.7(4) ? Fe7 C701 C7 . . . 126.5(3) ? Fe7 C701 C702 . . . 69.0(2) ? Fe7 C701 C705 . . . 68.4(2) ? C7 C701 C702 . . . 128.7(3) ? C7 C701 C705 . . . 124.4(4) ? C702 C701 C705 . . . 106.9(3) ? Fe7 C702 C701 . . . 70.3(2) ? Fe7 C702 C703 . . . 69.1(2) ? Fe7 C702 H702 . . . 125.1 ? C701 C702 C703 . . . 108.4(4) ? C701 C702 H702 . . . 126.1 ? C703 C702 H702 . . . 125.5 ? Fe7 C703 C702 . . . 70.0(2) ? Fe7 C703 C704 . . . 69.8(2) ? Fe7 C703 H703 . . . 126.5 ? C702 C703 C704 . . . 108.2(4) ? C702 C703 H703 . . . 125.7 ? C704 C703 H703 . . . 126.1 ? Fe7 C704 C703 . . . 69.9(2) ? Fe7 C704 C705 . . . 69.4(2) ? Fe7 C704 H704 . . . 127.6 ? C703 C704 C705 . . . 108.6(3) ? C703 C704 H704 . . . 124.8 ? C705 C704 H704 . . . 126.6 ? Fe7 C705 C701 . . . 70.6(2) ? Fe7 C705 C704 . . . 69.4(2) ? Fe7 C705 H705 . . . 125.1 ? C701 C705 C704 . . . 107.9(4) ? C701 C705 H705 . . . 126.3 ? C704 C705 H705 . . . 125.8 ? Fe7 C701' C702' . . . 69.5(5) ? Fe7 C701' C705' . . . 68.9(4) ? Fe7 C701' H701' . . . 128.8 ? C702' C701' C705' . . . 111.1(6) ? C702' C701' H701' . . . 127.4 ? C705' C701' H701' . . . 121.5 ? Fe7 C702' C701' . . . 68.0(5) ? Fe7 C702' C703' . . . 66.7(5) ? Fe7 C702' H702' . . . 128.4 ? C701' C702' C703' . . . 100.5(7) ? C701' C702' H702' . . . 129.5 ? C703' C702' H702' . . . 129.9 ? Fe7 C703' C702' . . . 67.4(5) ? Fe7 C703' C704' . . . 70.1(5) ? Fe7 C703' H703' . . . 132.1 ? C702' C703' C704' . . . 113.9(7) ? C702' C703' H703' . . . 120.4 ? C704' C703' H703' . . . 125.7 ? Fe7 C704' C703' . . . 68.2(4) ? Fe7 C704' C705' . . . 69.0(4) ? Fe7 C704' H704' . . . 126.8 ? C703' C704' C705' . . . 105.1(7) ? C703' C704' H704' . . . 123.6 ? C705' C704' H704' . . . 131.2 ? Fe7 C705' C701' . . . 66.6(4) ? Fe7 C705' C704' . . . 69.2(4) ? Fe7 C705' H705' . . . 129.3 ? C701' C705' C704' . . . 109.0(6) ? C701' C705' H705' . . . 129.4 ? C704' C705' H705' . . . 121.6 ? Fe7 C701" C702" . . . 68.6(5) ? Fe7 C701" C705" . . . 69.4(6) ? Fe7 C701" H701" . . . 124.6 ? C702" C701" C705" . . . 100.0(9) ? C702" C701" H701" . . . 136.1 ? C705" C701" H701" . . . 123.9 ? Fe7 C702" C701" . . . 71.9(5) ? Fe7 C702" C703" . . . 73.3(6) ? Fe7 C702" C704" . . . 61.5(4) ? C701" C702" C703" . . . 115.8(9) ? C701" C702" H702" . . . 116.1 ? C703" C702" H702" . . . 128.1 ? Fe7 C703" C702" . . . 69.1(6) ? Fe7 C703" C704" . . . 70.8(6) ? Fe7 C703" H703" . . . 121.5 ? C702" C703" C704" . . . 99.4(9) ? C702" C703" H703" . . . 128.0 ? C704" C703" H703" . . . 132.6 ? Fe7 C704" C703" . . . 73.2(6) ? Fe7 C704" C705" . . . 70.8(7) ? Fe7 C704" H704" . . . 126.1 ? C703" C704" C705" . . . 116.9(10) ? C703" C704" H704" . . . 116.9 ? C705" C704" H704" . . . 126.2 ? Fe7 C705" C701" . . . 72.2(7) ? Fe7 C705" C704" . . . 72.1(7) ? Fe7 C705" H705" . . . 121.7 ? C701" C705" C704" . . . 107.5(11) ? C701" C705" H705" . . . 131.8 ? C704" C705" H705" . . . 120.7 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2328 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 29 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min -31 _reflns_limit_l_max 31 _reflns_number_observed ? _reflns_d_resolution_high .583 _reflns_d_resolution_low 10.84 _diffrn_reflns_av_sigmaI/netI .223 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 153 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type atomblock _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .1 _refine_ls_wR_factor_all .041 _refine_ls_goodness_of_fit_all .973 _refine_ls_shift/su_mean .003 #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end