Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _audit_creation_method Xtal3.6 _audit_creation_date 00-11-07 _audit_update_record ? #============================================================================== # ; ? ; _journal_coden_Cambridge 182 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Prof M I Bruce' _publ_contact_author_address ; Prof M I Bruce Department of Chemistry University of Adelaide Adelaide 5005 AUSTRALIA ; _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal 'Chemical Communications' _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name 'Bruce, M. I.' 'Skelton, Brian W.' 'White, Allan H.' 'Zaitseva, Natasha N.' _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram 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. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_br632 _database_code_CSD 153644 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C37.5 H25 Cl O9 P2 Ru3' _chemical_formula_moiety ? _chemical_formula_weight 1020.22 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 25.256(2) _cell_length_b 11.7380(10) _cell_length_c 27.138(2) _cell_angle_alpha 90.00000 _cell_angle_beta 99.6030(10) _cell_angle_gamma 90.00000 _cell_volume 7932.5(11) _cell_formula_units_Z 8 _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 5788 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 26.4 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.327 _exptl_crystal_description block _exptl_crystal_size_max .25 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .14 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _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 .754 _exptl_absorpt_correction_T_max .928 _diffrn_reflns_number 47035 _reflns_number_total 10119 _reflns_Friedel_coverage ? _reflns_number_gt 7147 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.31 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .035 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _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 .035 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_number_reflns 7147 _refine_ls_number_parameters 583 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .042 _refine_diff_density_min -.365 _refine_diff_density_max .799 _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' _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 ? 0 300 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 200 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 8 .132019 .158997 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 72 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 16 .090027 .094971 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 24 -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 .307881(10) .77253(2) .399069(10) .03851(14) Uani ? ? 1.00000 ? ? Ru2 .398762(10) .64559(2) .400983(10) .04043(14) Uani ? ? 1.00000 ? ? Ru3 .398576(11) .78390(2) .483171(10) .04223(15) Uani ? ? 1.00000 ? ? C11 .26205(14) .6829(3) .43538(15) .0543(18) Uani ? ? 1.00000 ? ? O11 .23686(11) .6309(3) .45776(11) .0807(18) Uani ? ? 1.00000 ? ? C12 .27620(15) .7042(3) .33758(15) .0544(18) Uani ? ? 1.00000 ? ? O12 .25496(12) .6591(3) .30266(11) .0790(18) Uani ? ? 1.00000 ? ? C13 .26598(13) .9083(3) .38964(14) .0550(18) Uani ? ? 1.00000 ? ? O13 .24063(12) .9881(3) .38207(13) .094(2) Uani ? ? 1.00000 ? ? C21 .36328(17) .5329(3) .43362(17) .069(2) Uani ? ? 1.00000 ? ? O21 .34341(15) .4628(3) .45274(14) .106(2) Uani ? ? 1.00000 ? ? C22 .46782(16) .5803(3) .42282(16) .062(2) Uani ? ? 1.00000 ? ? O22 .50714(12) .5370(3) .43823(13) .099(2) Uani ? ? 1.00000 ? ? C23 .39180(15) .5802(3) .33628(15) .0543(18) Uani ? ? 1.00000 ? ? O23 .38904(14) .5368(2) .29818(11) .083(2) Uani ? ? 1.00000 ? ? C31 .36389(15) .6953(3) .52992(14) .0571(18) Uani ? ? 1.00000 ? ? O31 .34238(12) .6424(3) .55544(11) .0840(18) Uani ? ? 1.00000 ? ? C32 .40052(15) .9310(4) .51192(13) .058(2) Uani ? ? 1.00000 ? ? O32 .40231(14) 1.0225(3) .52649(11) .091(2) Uani ? ? 1.00000 ? ? C33 .46847(17) .7424(4) .51423(15) .065(2) Uani ? ? 1.00000 ? ? O33 .51093(13) .7210(3) .53285(14) .106(2) Uani ? ? 1.00000 ? ? C1 .38014(11) .8234(2) .37654(11) .0343(15) Uani ? ? 1.00000 ? ? C2 .42325(12) .8259(3) .41575(11) .0363(15) Uani ? ? 1.00000 ? ? C3 .47762(12) .8789(3) .41214(12) .0363(16) Uani ? ? 1.00000 ? ? P1 .38761(3) .89392(7) .31948(3) .0332(4) Uani ? ? 1.00000 ? ? C111 .33695(12) .8568(3) .26714(11) .0381(15) Uani ? ? 1.00000 ? ? C112 .34573(14) .7664(3) .23629(13) .0470(18) Uani ? ? 1.00000 ? ? C113 .30600(18) .7326(4) .19790(17) .068(3) Uani ? ? 1.00000 ? ? C114 .25848(19) .7890(4) .18928(18) .076(3) Uani ? ? 1.00000 ? ? C115 .24928(16) .8793(4) .21881(17) .069(2) Uani ? ? 1.00000 ? ? C116 .28826(13) .9138(3) .25806(14) .0511(18) Uani ? ? 1.00000 ? ? C121 .37835(12) 1.0443(3) .33263(12) .0391(16) Uani ? ? 1.00000 ? ? C122 .38463(16) 1.1242(3) .29586(16) .056(2) Uani ? ? 1.00000 ? ? C123 .3879(2) 1.2384(3) .3072(2) .071(2) Uani ? ? 1.00000 ? ? C124 .38566(18) 1.2752(3) .3545(2) .068(2) Uani ? ? 1.00000 ? ? C125 .37834(16) 1.1994(3) .39089(17) .059(2) Uani ? ? 1.00000 ? ? C126 .37449(13) 1.0841(3) .37995(14) .0458(18) Uani ? ? 1.00000 ? ? C0 .44981(12) .8692(3) .30478(12) .0385(16) Uani ? ? 1.00000 ? ? P2 .50245(3) .86418(7) .35284(3) .0367(4) Uani ? ? 1.00000 ? ? C211 .54095(12) .7335(3) .35478(12) .0409(17) Uani ? ? 1.00000 ? ? C212 .58393(15) .7116(3) .39284(16) .055(2) Uani ? ? 1.00000 ? ? C213 .61219(16) .6106(4) .39293(18) .066(2) Uani ? ? 1.00000 ? ? C214 .59834(17) .5320(4) .35557(19) .071(3) Uani ? ? 1.00000 ? ? C215 .55552(19) .5527(4) .31827(17) .066(3) Uani ? ? 1.00000 ? ? C216 .52656(15) .6529(3) .31825(15) .0495(18) Uani ? ? 1.00000 ? ? C221 .55001(12) .9796(3) .35042(11) .0410(17) Uani ? ? 1.00000 ? ? C222 .60344(14) .9628(3) .34726(14) .0514(18) Uani ? ? 1.00000 ? ? C223 .63723(16) 1.0551(4) .34523(16) .066(2) Uani ? ? 1.00000 ? ? C224 .61797(18) 1.1637(4) .34685(16) .070(3) Uani ? ? 1.00000 ? ? C225 .5654(2) 1.1817(4) .35010(18) .074(2) Uani ? ? 1.00000 ? ? C226 .53132(17) 1.0903(3) .35149(16) .061(2) Uani ? ? 1.00000 ? ? Cl1 .2704(7) 1.1685(11) .4928(7) .387(15) Uani ? ? 0.50000 ? ? Cl2 .2129(5) 1.3116(10) .4613(8) .394(15) Uani ? ? 0.50000 ? ? C01 .2435(9) 1.255(2) .4483(5) .153(14) Uani ? ? 0.50000 ? ? H .3359(14) .841(3) .4562(13) .068(11) Uiso ? ? 1.00000 ? ? H3a .5039(12) .845(3) .4365(11) .037(8) Uiso ? ? 1.00000 ? ? H3b .4745(11) .955(3) .4155(10) .032(8) Uiso ? ? 1.00000 ? ? H112 .3785(15) .727(3) .2403(13) .055(11) Uiso ? ? 1.00000 ? ? H113 .3137(15) .673(4) .1810(15) .072(13) Uiso ? ? 1.00000 ? ? H114 .2299(16) .776(3) .1647(15) .069(12) Uiso ? ? 1.00000 ? ? H115 .2152(17) .924(3) .2118(15) .084(13) Uiso ? ? 1.00000 ? ? H116 .2824(12) .977(3) .2760(12) .044(9) Uiso ? ? 1.00000 ? ? H122 .3853(13) 1.100(3) .2673(13) .048(11) Uiso ? ? 1.00000 ? ? H123 .3922(17) 1.285(4) .2840(16) .080(15) Uiso ? ? 1.00000 ? ? H124 .3866(12) 1.348(3) .3633(12) .044(9) Uiso ? ? 1.00000 ? ? H125 .3745(15) 1.220(3) .4246(15) .068(12) Uiso ? ? 1.00000 ? ? H126 .3711(12) 1.032(3) .4063(12) .050(10) Uiso ? ? 1.00000 ? ? H0a .4570(11) .891(2) .2742(11) .030(7) Uiso ? ? 1.00000 ? ? H212 .5941(17) .756(3) .4172(16) .070(14) Uiso ? ? 1.00000 ? ? H213 .6388(15) .601(3) .4176(15) .070(13) Uiso ? ? 1.00000 ? ? H214 .6212(17) .464(4) .3498(16) .100(15) Uiso ? ? 1.00000 ? ? H215 .5484(15) .503(4) .2932(14) .082(15) Uiso ? ? 1.00000 ? ? H216 .5022(12) .665(3) .2946(11) .033(9) Uiso ? ? 1.00000 ? ? H222 .6162(13) .894(3) .3468(12) .045(10) Uiso ? ? 1.00000 ? ? H223 .6733(16) 1.038(3) .3480(14) .078(13) Uiso ? ? 1.00000 ? ? H224 .6406(16) 1.225(3) .3444(15) .073(12) Uiso ? ? 1.00000 ? ? H225 .5519(16) 1.256(3) .3498(15) .071(13) Uiso ? ? 1.00000 ? ? H226 .4978(15) 1.100(3) .3514(14) .069(13) Uiso ? ? 1.00000 ? ? H01a .24649 1.16306 .46827 .22155 Uiso ? ? 0.50000 ? ? H01b .26989 1.24823 .47728 .07843 Uiso ? ? 0.50000 ? ? 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 .03403(13) .03772(15) .04555(16) -.00348(11) .01179(11) .00046(11) Ru2 .04318(15) .02919(13) .05156(17) .00009(11) .01562(12) .00447(11) Ru3 .04343(15) .04741(17) .03676(15) -.00160(12) .00932(11) .00549(12) C11 .046(2) .055(2) .064(2) -.0053(17) .0151(17) .0014(18) O11 .0743(19) .082(2) .095(2) -.0165(16) .0406(17) .0193(17) C12 .051(2) .056(2) .059(2) -.0169(17) .0174(18) .0005(18) O12 .083(2) .086(2) .0676(19) -.0445(17) .0111(16) -.0166(16) C13 .0403(19) .060(2) .067(2) .0006(17) .0158(17) .003(2) O13 .074(2) .071(2) .142(3) .0334(17) .032(2) .029(2) C21 .078(3) .042(2) .098(3) -.002(2) .046(3) .004(2) O21 .132(3) .0524(18) .155(3) -.0085(19) .086(3) .026(2) C22 .062(2) .044(2) .084(3) .0045(18) .025(2) .021(2) O22 .0639(19) .096(2) .142(3) .0334(18) .029(2) .057(2) C23 .069(2) .036(2) .061(2) -.0011(17) .020(2) .0033(17) O23 .132(3) .0517(17) .067(2) -.0006(17) .0257(18) -.0101(15) C31 .057(2) .064(2) .051(2) .0027(19) .0112(18) .0134(18) O31 .088(2) .092(2) .080(2) -.0027(18) .0369(17) .0388(18) C32 .064(2) .065(3) .043(2) -.009(2) .0038(17) -.0032(19) O32 .120(3) .069(2) .079(2) -.007(2) .0000(19) -.0216(17) C33 .056(2) .084(3) .054(2) -.003(2) .006(2) .015(2) O33 .067(2) .130(3) .109(3) .007(2) -.021(2) .030(2) C1 .0371(16) .0262(15) .0409(17) -.0027(12) .0099(13) -.0008(12) C2 .0388(16) .0330(16) .0389(17) .0010(13) .0119(13) .0040(13) C3 .0357(16) .0337(18) .0392(18) -.0027(13) .0053(13) -.0020(14) P1 .0319(4) .0310(4) .0364(4) -.0015(3) .0048(3) .0014(3) C111 .0360(16) .0402(17) .0375(17) -.0072(13) .0045(13) .0025(14) C112 .0407(19) .051(2) .050(2) -.0062(16) .0096(15) -.0045(16) C113 .062(3) .079(3) .064(3) -.018(2) .011(2) -.030(2) C114 .057(3) .100(4) .064(3) -.019(3) -.011(2) -.015(3) C115 .042(2) .080(3) .078(3) -.001(2) -.013(2) .005(2) C116 .0413(19) .047(2) .062(2) .0014(16) .0001(16) -.0002(18) C121 .0366(16) .0317(16) .0476(19) .0001(13) .0030(13) .0019(14) C122 .070(3) .043(2) .056(3) .0001(18) .012(2) .0071(19) C123 .087(3) .040(2) .085(3) -.003(2) .011(3) .018(2) C124 .078(3) .032(2) .089(3) -.003(2) .001(2) -.006(2) C125 .065(2) .044(2) .066(3) .0033(18) .006(2) -.010(2) C126 .048(2) .0357(18) .053(2) .0024(15) .0068(16) -.0018(16) C0 .0336(16) .047(2) .0362(17) .0006(13) .0100(13) .0041(14) P2 .0315(4) .0383(4) .0404(4) -.0020(3) .0067(3) .0017(3) C211 .0333(16) .0398(18) .052(2) .0003(13) .0145(14) .0044(15) C212 .044(2) .055(2) .064(3) .0035(17) .0019(18) .002(2) C213 .049(2) .067(3) .079(3) .008(2) .003(2) .014(2) C214 .067(3) .052(3) .099(4) .019(2) .025(3) .008(2) C215 .079(3) .054(3) .068(3) .012(2) .019(2) -.007(2) C216 .047(2) .051(2) .051(2) .0047(17) .0092(18) .0005(18) C221 .0403(17) .047(2) .0361(17) -.0068(14) .0079(13) .0017(14) C222 .048(2) .052(2) .057(2) -.0066(18) .0171(17) -.0077(18) C223 .046(2) .082(3) .075(3) -.023(2) .024(2) -.014(2) C224 .070(3) .068(3) .075(3) -.035(2) .021(2) -.007(2) C225 .078(3) .046(2) .097(3) -.013(2) .012(3) .006(2) C226 .050(2) .050(2) .084(3) -.0052(19) .012(2) .009(2) Cl1 .380(18) .284(12) .49(2) -.025(14) .053(16) -.027(16) Cl2 .194(8) .228(9) .66(3) -.020(7) -.221(13) -.053(13) C01 .179(19) .23(2) .063(7) -.121(17) .060(10) -.048(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 Ru1 Ru2 . . 2.7297(4) ? Ru1 Ru3 . . 2.9546(4) ? Ru1 C11 . . 1.949(4) ? Ru1 C12 . . 1.903(4) ? Ru1 C13 . . 1.907(3) ? Ru1 C1 . . 2.106(3) ? Ru1 H . . 1.78(3) ? Ru2 Ru3 . . 2.7593(4) ? Ru2 C21 . . 1.898(4) ? Ru2 C22 . . 1.907(4) ? Ru2 C23 . . 1.897(4) ? Ru2 C1 . . 2.217(2) ? Ru2 C2 . . 2.223(3) ? Ru3 C31 . . 1.957(4) ? Ru3 C32 . . 1.892(5) ? Ru3 C33 . . 1.889(4) ? Ru3 C1 . . 2.891(3) ? Ru3 C2 . . 2.088(3) ? Ru3 H . . 1.76(3) ? C11 O11 . . 1.129(5) ? C12 O12 . . 1.139(5) ? C13 O13 . . 1.134(5) ? C21 O21 . . 1.134(6) ? C22 O22 . . 1.132(5) ? C23 O23 . . 1.144(5) ? C31 O31 . . 1.134(5) ? C32 O32 . . 1.143(6) ? C33 O33 . . 1.135(5) ? C1 C2 . . 1.390(4) ? C1 P1 . . 1.793(3) ? C2 C3 . . 1.525(5) ? C3 P2 . . 1.830(4) ? C3 H3a . . .94(3) ? C3 H3b . . .90(4) ? P1 C111 . . 1.799(3) ? P1 C121 . . 1.824(4) ? P1 C0 . . 1.709(3) ? C111 C112 . . 1.392(5) ? C111 C116 . . 1.385(5) ? C112 C113 . . 1.379(5) ? C112 H112 . . .94(4) ? C113 C114 . . 1.356(7) ? C113 H113 . . .88(5) ? C114 C115 . . 1.372(7) ? C114 H114 . . .91(4) ? C115 C116 . . 1.385(5) ? C115 H115 . . 1.00(4) ? C116 H116 . . .91(3) ? C121 C122 . . 1.398(5) ? C121 C126 . . 1.385(5) ? C122 C123 . . 1.375(5) ? C122 H122 . . .83(4) ? C123 C124 . . 1.364(8) ? C123 H123 . . .85(5) ? C124 C125 . . 1.365(6) ? C124 H124 . . .89(4) ? C125 C126 . . 1.386(5) ? C125 H125 . . .97(4) ? C126 H126 . . .96(3) ? C0 P2 . . 1.701(3) ? C0 H0a . . .92(3) ? P2 C211 . . 1.812(3) ? P2 C221 . . 1.819(3) ? C211 C212 . . 1.392(5) ? C211 C216 . . 1.375(5) ? C212 C213 . . 1.384(6) ? C212 H212 . . .85(4) ? C213 C214 . . 1.372(7) ? C213 H213 . . .87(4) ? C214 C215 . . 1.374(6) ? C214 H214 . . 1.01(5) ? C215 C216 . . 1.385(6) ? C215 H215 . . .89(4) ? C216 H216 . . .82(3) ? C221 C222 . . 1.381(5) ? C221 C226 . . 1.384(5) ? C222 C223 . . 1.386(6) ? C222 H222 . . .87(4) ? C223 C224 . . 1.368(7) ? C223 H223 . . .92(4) ? C224 C225 . . 1.362(7) ? C224 H224 . . .93(4) ? C225 C226 . . 1.380(6) ? C225 H225 . . .94(4) ? C226 H226 . . .85(4) ? Cl1 C01 . . 1.64(2) ? Cl1 H01a . . .823(17) ? Cl1 H01b . . 1.025(14) ? Cl1 Cl2 . '7 576' 1.27(3) ? Cl1 C01 . '7 576' 1.92(3) ? Cl2 C01 . . 1.12(3) ? C01 H01a . . 1.20(2) ? C01 H01b . . .946(16) ? 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 . . . 57.920(9) ? Ru2 Ru1 C11 . . . 105.32(10) ? Ru2 Ru1 C12 . . . 90.91(11) ? Ru2 Ru1 C13 . . . 154.82(11) ? Ru2 Ru1 C1 . . . 52.67(7) ? Ru2 Ru1 H . . . 91.1(11) ? Ru3 Ru1 C11 . . . 94.77(10) ? Ru3 Ru1 C12 . . . 148.72(11) ? Ru3 Ru1 C13 . . . 114.04(10) ? Ru3 Ru1 C1 . . . 67.27(8) ? Ru3 Ru1 H . . . 33.3(11) ? C11 Ru1 C12 . . . 91.00(16) ? C11 Ru1 C13 . . . 98.97(15) ? C11 Ru1 C1 . . . 156.43(12) ? C11 Ru1 H . . . 89.2(12) ? C12 Ru1 C13 . . . 95.27(15) ? C12 Ru1 C1 . . . 97.06(14) ? C12 Ru1 H . . . 177.9(11) ? C13 Ru1 C1 . . . 102.27(13) ? C13 Ru1 H . . . 82.6(11) ? C1 Ru1 H . . . 83.5(12) ? Ru1 Ru2 Ru3 . . . 65.129(9) ? Ru1 Ru2 C21 . . . 85.89(12) ? Ru1 Ru2 C22 . . . 161.43(13) ? Ru1 Ru2 C23 . . . 104.80(11) ? Ru1 Ru2 C1 . . . 49.05(8) ? Ru1 Ru2 C2 . . . 72.03(8) ? Ru3 Ru2 C21 . . . 88.18(13) ? Ru3 Ru2 C22 . . . 96.32(12) ? Ru3 Ru2 C23 . . . 166.81(11) ? Ru3 Ru2 C1 . . . 70.06(8) ? Ru3 Ru2 C2 . . . 48.08(8) ? C21 Ru2 C22 . . . 93.06(17) ? C21 Ru2 C23 . . . 99.90(17) ? C21 Ru2 C1 . . . 134.65(15) ? C21 Ru2 C2 . . . 135.92(15) ? C22 Ru2 C23 . . . 93.66(17) ? C22 Ru2 C1 . . . 127.51(13) ? C22 Ru2 C2 . . . 96.55(13) ? C23 Ru2 C1 . . . 96.99(13) ? C23 Ru2 C2 . . . 122.15(14) ? C1 Ru2 C2 . . . 36.49(10) ? Ru1 Ru3 Ru2 . . . 56.952(9) ? Ru1 Ru3 C31 . . . 95.95(10) ? Ru1 Ru3 C32 . . . 108.86(11) ? Ru1 Ru3 C33 . . . 151.58(13) ? Ru1 Ru3 C1 . . . 42.21(6) ? Ru1 Ru3 C2 . . . 68.90(8) ? Ru1 Ru3 H . . . 33.8(11) ? Ru2 Ru3 C31 . . . 105.82(10) ? Ru2 Ru3 C32 . . . 150.09(12) ? Ru2 Ru3 C33 . . . 94.67(13) ? Ru2 Ru3 C1 . . . 46.12(5) ? Ru2 Ru3 C2 . . . 52.38(9) ? Ru2 Ru3 H . . . 90.6(12) ? C31 Ru3 C32 . . . 101.61(16) ? C31 Ru3 C33 . . . 93.43(17) ? C31 Ru3 C1 . . . 136.01(11) ? C31 Ru3 C2 . . . 157.66(14) ? C31 Ru3 H . . . 90.2(12) ? C32 Ru3 C33 . . . 95.35(18) ? C32 Ru3 C1 . . . 104.78(12) ? C32 Ru3 C2 . . . 98.91(15) ? C32 Ru3 H . . . 77.5(11) ? C33 Ru3 C1 . . . 118.07(14) ? C33 Ru3 C2 . . . 93.36(16) ? C33 Ru3 H . . . 172.5(11) ? C1 Ru3 C2 . . . 26.71(10) ? C1 Ru3 H . . . 62.6(12) ? C2 Ru3 H . . . 85.7(12) ? Ru1 C11 O11 . . . 177.7(3) ? Ru1 C12 O12 . . . 175.1(4) ? Ru1 C13 O13 . . . 177.3(3) ? Ru2 C21 O21 . . . 177.5(4) ? Ru2 C22 O22 . . . 174.9(4) ? Ru2 C23 O23 . . . 176.9(3) ? Ru3 C31 O31 . . . 177.3(3) ? Ru3 C32 O32 . . . 175.7(3) ? Ru3 C33 O33 . . . 177.8(4) ? Ru1 C1 Ru2 . . . 78.29(9) ? Ru1 C1 Ru3 . . . 70.52(9) ? Ru1 C1 C2 . . . 112.9(2) ? Ru1 C1 P1 . . . 127.07(14) ? Ru2 C1 Ru3 . . . 63.81(7) ? Ru2 C1 C2 . . . 71.99(18) ? Ru2 C1 P1 . . . 130.19(15) ? Ru3 C1 C2 . . . 42.46(16) ? Ru3 C1 P1 . . . 156.33(13) ? C2 C1 P1 . . . 118.0(2) ? Ru2 C2 Ru3 . . . 79.54(12) ? Ru2 C2 C1 . . . 71.52(17) ? Ru2 C2 C3 . . . 127.1(2) ? Ru3 C2 C1 . . . 110.8(2) ? Ru3 C2 C3 . . . 123.8(2) ? C1 C2 C3 . . . 123.9(3) ? C2 C3 P2 . . . 117.5(2) ? C2 C3 H3a . . . 109(2) ? C2 C3 H3b . . . 107.6(18) ? P2 C3 H3a . . . 106(2) ? P2 C3 H3b . . . 103.3(19) ? H3a C3 H3b . . . 114(3) ? C1 P1 C111 . . . 113.98(14) ? C1 P1 C121 . . . 104.03(14) ? C1 P1 C0 . . . 110.88(15) ? C111 P1 C121 . . . 106.94(15) ? C111 P1 C0 . . . 109.57(15) ? C121 P1 C0 . . . 111.28(16) ? P1 C111 C112 . . . 119.7(2) ? P1 C111 C116 . . . 121.1(3) ? C112 C111 C116 . . . 119.1(3) ? C111 C112 C113 . . . 120.3(3) ? C111 C112 H112 . . . 122(2) ? C113 C112 H112 . . . 118(2) ? C112 C113 C114 . . . 120.1(4) ? C112 C113 H113 . . . 115(2) ? C114 C113 H113 . . . 125(2) ? C113 C114 C115 . . . 120.5(4) ? C113 C114 H114 . . . 128(3) ? C115 C114 H114 . . . 112(2) ? C114 C115 C116 . . . 120.5(4) ? C114 C115 H115 . . . 121(2) ? C116 C115 H115 . . . 118(2) ? C111 C116 C115 . . . 119.4(3) ? C111 C116 H116 . . . 121.0(18) ? C115 C116 H116 . . . 119.4(18) ? P1 C121 C122 . . . 118.4(3) ? P1 C121 C126 . . . 122.6(3) ? C122 C121 C126 . . . 118.0(3) ? C121 C122 C123 . . . 120.3(4) ? C121 C122 H122 . . . 117(2) ? C123 C122 H122 . . . 122(2) ? C122 C123 C124 . . . 120.6(4) ? C122 C123 H123 . . . 118(3) ? C124 C123 H123 . . . 121(3) ? C123 C124 C125 . . . 120.4(4) ? C123 C124 H124 . . . 124(2) ? C125 C124 H124 . . . 116(2) ? C124 C125 C126 . . . 119.7(4) ? C124 C125 H125 . . . 125(2) ? C126 C125 H125 . . . 116(2) ? C121 C126 C125 . . . 121.0(4) ? C121 C126 H126 . . . 120(2) ? C125 C126 H126 . . . 118(2) ? P1 C0 P2 . . . 117.3(2) ? P1 C0 H0a . . . 119.6(17) ? P2 C0 H0a . . . 117.2(17) ? C3 P2 C0 . . . 109.41(15) ? C3 P2 C211 . . . 108.38(15) ? C3 P2 C221 . . . 106.66(15) ? C0 P2 C211 . . . 113.49(16) ? C0 P2 C221 . . . 112.51(15) ? C211 P2 C221 . . . 106.09(15) ? P2 C211 C212 . . . 121.7(3) ? P2 C211 C216 . . . 119.0(2) ? C212 C211 C216 . . . 119.2(3) ? C211 C212 C213 . . . 119.9(4) ? C211 C212 H212 . . . 124(3) ? C213 C212 H212 . . . 116(3) ? C212 C213 C214 . . . 120.5(4) ? C212 C213 H213 . . . 116(2) ? C214 C213 H213 . . . 123(2) ? C213 C214 C215 . . . 119.8(4) ? C213 C214 H214 . . . 124(2) ? C215 C214 H214 . . . 115(2) ? C214 C215 C216 . . . 120.1(4) ? C214 C215 H215 . . . 119(3) ? C216 C215 H215 . . . 121(3) ? C211 C216 C215 . . . 120.5(3) ? C211 C216 H216 . . . 121(2) ? C215 C216 H216 . . . 118(2) ? P2 C221 C222 . . . 123.6(3) ? P2 C221 C226 . . . 118.0(3) ? C222 C221 C226 . . . 118.4(3) ? C221 C222 C223 . . . 120.4(3) ? C221 C222 H222 . . . 120(2) ? C223 C222 H222 . . . 120(2) ? C222 C223 C224 . . . 120.2(4) ? C222 C223 H223 . . . 116(2) ? C224 C223 H223 . . . 123(2) ? C223 C224 C225 . . . 120.2(4) ? C223 C224 H224 . . . 120(2) ? C225 C224 H224 . . . 120(2) ? C224 C225 C226 . . . 120.0(4) ? C224 C225 H225 . . . 120(3) ? C226 C225 H225 . . . 120(3) ? C221 C226 C225 . . . 120.8(4) ? C221 C226 H226 . . . 118(2) ? C225 C226 H226 . . . 121(2) ? C01 Cl1 H01a . . . 45.0(11) ? C01 Cl1 H01b . . . 32.4(9) ? C01 Cl1 Cl2 . . '7 576' 129.8(13) ? C01 Cl1 C01 . . '7 576' 102.3(12) ? H01a Cl1 H01b . . . 77.4(13) ? H01a Cl1 Cl2 . . '7 576' 153(2) ? H01a Cl1 C01 . . '7 576' 119.9(17) ? H01b Cl1 Cl2 . . '7 576' 102.4(13) ? H01b Cl1 C01 . . '7 576' 85.6(12) ? Cl2 Cl1 C01 '7 576' . '7 576' 34.1(10) ? C01 Cl2 Cl1 . . '7 576' 106.5(15) ? Cl1 C01 Cl2 . . . 111.0(16) ? Cl1 C01 H01a . . . 28.9(7) ? Cl1 C01 H01b . . . 35.5(10) ? Cl1 C01 Cl1 . . '7 576' 77.7(9) ? Cl2 C01 H01a . . . 112.6(18) ? Cl2 C01 H01b . . . 102.4(17) ? Cl2 C01 Cl1 . . '7 576' 39.4(12) ? H01a C01 H01b . . . 64.4(11) ? H01a C01 Cl1 . . '7 576' 92.9(10) ? H01b C01 Cl1 . . '7 576' 63.1(11) ? Ru1 H Ru3 . . . 113(2) ? Cl1 H01a C01 . . . 106.1(13) ? Cl1 H01b C01 . . . 112.2(17) ? 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 #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ru1 O11 3.078(3) . . ? Ru1 O12 3.039(3) . . ? Ru1 O13 3.040(3) . . ? Ru1 C21 3.211(4) . . ? Ru1 O21 3.963(4) . . ? Ru1 C23 3.701(4) . . ? Ru1 C31 3.709(4) . . ? Ru1 C32 3.990(4) . . ? Ru1 C2 2.941(3) . . ? Ru1 P1 3.4930(9) . . ? Ru1 C111 3.900(3) . . ? Ru1 C126 4.095(4) . . ? Ru1 H126 3.43(3) . . ? Ru2 C11 3.750(4) . . ? Ru2 C12 3.352(4) . . ? Ru2 O12 4.135(3) . . ? Ru2 O21 3.031(4) . . ? Ru2 O22 3.036(3) . . ? Ru2 O23 3.041(3) . . ? Ru2 C31 3.793(4) . . ? Ru2 C33 3.469(4) . . ? Ru2 C3 3.370(3) . . ? Ru2 P1 3.6415(9) . . ? Ru2 C0 4.061(3) . . ? Ru2 P2 4.0360(9) . . ? Ru2 H 3.29(4) . . ? Ru2 H3a 3.55(3) . . ? Ru2 H124 3.64(3) . '1 545' ? Ru3 C11 3.672(3) . . ? Ru3 O11 4.135(3) . '7 566' ? Ru3 C21 3.299(4) . . ? Ru3 O21 4.055(4) . . ? Ru3 C22 3.522(4) . . ? Ru3 O31 3.090(3) . . ? Ru3 O32 3.033(3) . . ? Ru3 O33 3.023(3) . . ? Ru3 C3 3.198(3) . . ? Ru3 H3a 3.21(3) . . ? Ru3 H3b 3.50(3) . . ? Ru3 H126 3.58(3) . . ? C11 C12 2.748(6) . . ? C11 C13 2.931(5) . . ? C11 H 2.62(3) . . ? O11 Cl1 3.777(14) . '7 566' ? O11 Cl2 3.800(12) . '1 545' ? C12 C13 2.815(5) . . ? C13 H 2.44(3) . . ? O13 Cl1 3.650(17) . . ? C21 C22 2.761(6) . . ? C21 C23 2.905(6) . . ? O21 Cl1 3.773(19) . '7 566' ? O21 Cl2 3.785(14) . '1 545' ? C22 C23 2.774(5) . . ? O22 O33 3.180(5) . '3 666' ? O23 H112 2.72(4) . . ? C31 C32 2.983(6) . . ? C31 C33 2.800(6) . . ? C31 H 2.64(3) . . ? C32 C33 2.795(6) . . ? C32 H 2.29(3) . . ? O32 Cl1 3.722(17) . . ? O32 Cl2 3.562(14) . '7 576' ? C33 C2 2.896(5) . . ? C1 C3 2.574(4) . . ? C1 C121 2.851(4) . . ? C1 C0 2.885(5) . . ? C1 H 2.60(4) . . ? C1 H126 2.60(4) . . ? C2 P1 2.737(3) . . ? C2 P2 2.874(3) . . ? C2 H 2.63(4) . . ? C2 H3a 2.03(3) . . ? C2 H3b 1.99(3) . . ? C3 C0 2.883(4) . . ? C3 C211 2.954(5) . . ? C3 C221 2.927(5) . . ? P1 C112 2.768(3) . . ? P1 C116 2.781(3) . . ? P1 C122 2.776(4) . . ? P1 C126 2.823(4) . . ? P1 P2 2.9117(11) . . ? P1 H122 2.80(4) . . ? P1 H0a 2.30(3) . . ? C111 C113 2.404(5) . . ? C111 C114 2.762(5) . . ? C111 C115 2.392(5) . . ? C111 C121 2.911(5) . . ? C111 C0 2.867(4) . . ? C111 H112 2.05(4) . . ? C111 H116 2.01(3) . . ? C112 C114 2.370(6) . . ? C112 C115 2.744(5) . . ? C112 C116 2.395(5) . . ? C112 H113 1.92(4) . . ? C113 C115 2.369(7) . . ? C113 C116 2.763(6) . . ? C113 H112 1.99(3) . . ? C113 H114 2.05(4) . . ? C114 C116 2.393(6) . . ? C114 H113 1.99(4) . . ? C114 H115 2.07(4) . . ? C115 H114 1.90(4) . . ? C115 H116 2.00(3) . . ? C116 H115 2.05(4) . . ? C121 C123 2.404(5) . . ? C121 C124 2.774(5) . . ? C121 C125 2.411(5) . . ? C121 C0 2.917(5) . . ? C121 H122 1.92(4) . . ? C121 H126 2.04(3) . . ? C122 C124 2.379(6) . . ? C122 C125 2.755(6) . . ? C122 C126 2.385(6) . . ? C122 H123 1.93(5) . . ? C123 C125 2.368(7) . . ? C123 C126 2.742(6) . . ? C123 H122 1.95(4) . . ? C123 H124 2.00(3) . . ? C124 C126 2.378(5) . . ? C124 H123 1.95(4) . . ? C124 H125 2.07(4) . . ? C125 H124 1.92(4) . . ? C125 H126 2.02(4) . . ? C126 H125 2.00(4) . . ? C0 C211 2.938(4) . . ? C0 C221 2.928(4) . . ? P2 C212 2.806(4) . . ? P2 C216 2.756(4) . . ? P2 C222 2.828(4) . . ? P2 C226 2.754(4) . . ? P2 H3a 2.28(3) . . ? P2 H3b 2.22(3) . . ? P2 H0a 2.27(3) . . ? P2 H226 2.77(4) . . ? C211 C213 2.402(5) . . ? C211 C214 2.772(6) . . ? C211 C215 2.396(6) . . ? C211 C221 2.902(5) . . ? C211 H212 2.00(4) . . ? C211 H216 1.93(3) . . ? C212 C214 2.392(6) . . ? C212 C215 2.758(6) . . ? C212 C216 2.386(5) . . ? C212 Cl2 3.663(14) . '5 545' ? C212 H213 1.94(4) . . ? C212 H222 2.67(4) . . ? C213 C215 2.377(6) . . ? C213 C216 2.751(5) . . ? C213 Cl2 3.729(14) . '5 545' ? C213 H212 1.91(4) . . ? C213 H214 2.11(5) . . ? C214 C216 2.390(6) . . ? C214 H213 1.99(4) . . ? C214 H215 1.96(4) . . ? C215 H214 2.02(4) . . ? C215 H216 1.92(3) . . ? C216 H215 2.00(5) . . ? C221 C223 2.400(5) . . ? C221 C224 2.771(6) . . ? C221 C225 2.404(6) . . ? C221 H222 1.97(3) . . ? C221 H226 1.94(4) . . ? C222 C224 2.387(6) . . ? C222 C225 2.749(6) . . ? C222 C226 2.375(5) . . ? C222 H223 1.97(4) . . ? C223 C225 2.366(7) . . ? C223 C226 2.740(6) . . ? C223 H222 1.97(4) . . ? C223 H224 2.00(4) . . ? C224 C226 2.375(6) . . ? C224 H223 2.03(4) . . ? C224 H225 2.00(4) . . ? C225 H224 2.00(4) . . ? C225 H226 1.96(4) . . ? C226 H225 2.02(4) . . ? Cl1 Cl1 2.24(2) . '7 576' ? Cl1 Cl2 2.29(2) . . ? Cl1 H125 3.51(5) . . ? Cl1 H01a 2.315(15) . '7 576' ? Cl1 H01b 1.710(18) . '7 576' ? Cl2 Cl2 2.95(2) . '7 576' ? Cl2 C01 2.63(2) . '7 576' ? Cl2 H212 3.11(4) . '5 455' ? Cl2 H213 3.21(4) . '5 455' ? Cl2 H01a 2.03(2) . '7 576' ? Cl2 H01a 1.934(12) . . ? Cl2 H01b 1.614(12) . . ? Cl2 H01b 1.79(2) . '7 576' ? C01 C01 2.77(2) . '7 576' ? C01 H01a 2.434(16) . '7 576' ? C01 H01b 2.103(15) . '7 576' ? H3a H3b 1.55(5) . . ? H112 H113 2.19(5) . . ? H114 H115 2.22(5) . . ? H115 H116 2.31(5) . . ? H122 H123 2.22(6) . . ? H123 H124 2.30(6) . . ? H124 H125 2.30(5) . . ? H125 H126 2.26(5) . . ? H212 H213 2.14(5) . . ? H214 H215 2.24(5) . . ? H215 H216 2.23(6) . . ? H222 H223 2.22(5) . . ? H223 H224 2.34(5) . . ? H224 H225 2.30(6) . . ? H225 H226 2.29(5) . . ? H01a H01b 1.16632(8) . . ? H01a H01b 1.90862(10) . '7 576' ? H01b H01b 1.71614(9) . '7 576' ? _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 4008 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 34 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min -36 _reflns_limit_l_max 36 _reflns_number_observed ? _reflns_d_resolution_high .726 _reflns_d_resolution_low 13.379 _diffrn_reflns_av_sigmaI/netI .078 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _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 .059 _refine_ls_wR_factor_all .04 _refine_ls_goodness_of_fit_all 1.032 _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 data_br660 _database_code_CSD 153645 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C37.5 H26 B1 Cl1 F4 O9 P2 Ru3' _chemical_formula_moiety ? _chemical_formula_weight 1108.03 _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 11.3115(6) _cell_length_b 11.4716(7) _cell_length_c 17.8808(10) _cell_angle_alpha 74.8530(10) _cell_angle_beta 88.5280(10) _cell_angle_gamma 63.3200(10) _cell_volume 1989.8(2) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6688 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 1.344 _exptl_crystal_description plate _exptl_crystal_size_max .2 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .06 _exptl_crystal_size_rad ? _exptl_crystal_colour pale-yellow _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 .792 _exptl_absorpt_correction_T_max .948 _diffrn_reflns_number 22008 _reflns_number_total 9720 _reflns_Friedel_coverage 0 _reflns_number_gt 8639 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.2 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .020 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _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 .027 _refine_ls_wR_factor_ref .034 _refine_ls_goodness_of_fit_ref 1.281 _refine_ls_number_reflns 8639 _refine_ls_number_parameters 640 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .031 _refine_diff_density_min -.803 _refine_diff_density_max 1.186 _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 75 .002 .002 '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' Cl ? 0 2 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 18 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 4 .09 .095 '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' B ? 0 2 0 .001 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 8 .014 .01 '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 .091625(16) .533480(17) .812672(10) .01820(15) Uani ? ? 1.00000 ? ? Ru2 .314704(17) .309935(17) .798867(9) .01845(15) Uani ? ? 1.00000 ? ? Ru3 .319640(17) .381907(18) .933461(9) .01918(16) Uani ? ? 1.00000 ? ? C11 -.0246(2) .4729(2) .87350(14) .026(2) Uani ? ? 1.00000 ? ? O11 -.09055(19) .4365(2) .91102(11) .039(2) Uani ? ? 1.00000 ? ? C12 .0074(2) .5388(2) .71942(13) .025(2) Uani ? ? 1.00000 ? ? O12 -.04658(17) .5377(2) .66712(10) .0339(17) Uani ? ? 1.00000 ? ? C13 -.0077(2) .7239(2) .80385(13) .025(2) Uani ? ? 1.00000 ? ? O13 -.06591(18) .83793(17) .79621(11) .0359(17) Uani ? ? 1.00000 ? ? C21 .2413(2) .2026(2) .86144(14) .028(2) Uani ? ? 1.00000 ? ? O21 .1966(2) .1365(2) .89659(11) .0374(19) Uani ? ? 1.00000 ? ? C22 .4948(2) .1705(2) .80549(14) .028(2) Uani ? ? 1.00000 ? ? O22 .60062(19) .0863(2) .81319(12) .0435(19) Uani ? ? 1.00000 ? ? C23 .2582(2) .3044(2) .69998(14) .027(2) Uani ? ? 1.00000 ? ? O23 .2196(2) .29921(19) .64344(10) .0394(18) Uani ? ? 1.00000 ? ? C31 .2296(3) .2989(3) 1.00800(13) .029(2) Uani ? ? 1.00000 ? ? O31 .1744(2) .2527(2) 1.04924(11) .046(2) Uani ? ? 1.00000 ? ? C32 .3362(2) .4990(3) .98614(13) .026(2) Uani ? ? 1.00000 ? ? O32 .34958(18) .5701(2) 1.01520(11) .0374(19) Uani ? ? 1.00000 ? ? C33 .4895(3) .2320(3) .97171(14) .031(2) Uani ? ? 1.00000 ? ? O33 .5915(2) .1418(2) .99529(13) .054(2) Uani ? ? 1.00000 ? ? C1 .2697(2) .5238(2) .76898(11) .0169(17) Uani ? ? 1.00000 ? ? C2 .3792(2) .4500(2) .82710(12) .0183(17) Uani ? ? 1.00000 ? ? C3 .5155(2) .4480(3) .82131(13) .022(2) Uani ? ? 1.00000 ? ? P1 .28356(5) .62816(5) .68125(3) .0164(4) Uani ? ? 1.00000 ? ? C111 .1591(2) .6813(2) .60285(12) .0207(18) Uani ? ? 1.00000 ? ? C112 .1752(2) .5993(3) .55387(13) .027(2) Uani ? ? 1.00000 ? ? C113 .0687(3) .6368(3) .49939(15) .035(3) Uani ? ? 1.00000 ? ? C114 -.0487(3) .7535(3) .49354(15) .038(3) Uani ? ? 1.00000 ? ? C115 -.0629(3) .8369(3) .54021(15) .033(2) Uani ? ? 1.00000 ? ? C116 .0408(2) .8004(2) .59594(14) .025(2) Uani ? ? 1.00000 ? ? C121 .2815(2) .7732(2) .70322(12) .0191(17) Uani ? ? 1.00000 ? ? C122 .3063(2) .8668(2) .64586(13) .0231(19) Uani ? ? 1.00000 ? ? C123 .3256(2) .9664(2) .66663(15) .028(2) Uani ? ? 1.00000 ? ? C124 .3184(2) .9725(2) .74282(16) .030(2) Uani ? ? 1.00000 ? ? C125 .2898(2) .8839(2) .79906(15) .027(2) Uani ? ? 1.00000 ? ? C126 .2710(2) .7831(2) .77975(13) .0208(18) Uani ? ? 1.00000 ? ? C0 .4461(2) .5366(2) .65031(12) .0199(18) Uani ? ? 1.00000 ? ? P2 .57529(5) .48788(6) .72673(3) .0184(5) Uani ? ? 1.00000 ? ? C221 .6159(2) .6257(2) .71757(13) .0213(18) Uani ? ? 1.00000 ? ? C222 .6338(2) .6665(2) .78126(14) .026(2) Uani ? ? 1.00000 ? ? C223 .6655(3) .7735(3) .77013(16) .033(2) Uani ? ? 1.00000 ? ? C224 .6763(2) .8411(3) .69655(16) .032(2) Uani ? ? 1.00000 ? ? C225 .6602(2) .8003(3) .63310(15) .031(2) Uani ? ? 1.00000 ? ? C226 .6318(2) .6913(3) .64319(14) .027(2) Uani ? ? 1.00000 ? ? C211 .7215(2) .3426(2) .71641(13) .0231(19) Uani ? ? 1.00000 ? ? C212 .8282(3) .2825(3) .7740(2) .055(3) Uani ? ? 1.00000 ? ? C213 .9433(3) .1723(4) .7669(3) .065(4) Uani ? ? 1.00000 ? ? C214 .9523(3) .1198(3) .70497(18) .039(3) Uani ? ? 1.00000 ? ? C215 .8479(3) .1774(3) .64946(18) .041(3) Uani ? ? 1.00000 ? ? C216 .7317(3) .2904(3) .65412(16) .035(2) Uani ? ? 1.00000 ? ? B .5165(3) .2103(3) .55841(18) .038(3) Uani ? ? 1.00000 ? ? F1 .4707(2) .34888(17) .52093(10) .0506(18) Uani ? ? 1.00000 ? ? F2 .5245(2) .1934(2) .63778(9) .055(2) Uani ? ? 1.00000 ? ? F3 .4323(2) .1668(2) .53628(10) .059(2) Uani ? ? 1.00000 ? ? F4 .6425(2) .1405(2) .53692(12) .070(2) Uani ? ? 1.00000 ? ? Cl1 .07844(19) .8612(2) .96875(13) .0626(19) Uani ? ? .50000 ? ? Cl2 -.1048(2) 1.1319(2) .97723(17) .079(3) Uani ? ? .50000 ? ? C01 -.0842(7) .9904(7) .9472(5) .055(7) Uani ? ? .50000 ? ? H .159(3) .527(3) .8990(16) .040(8) Uiso ? ? 1.00000 ? ? H3a .519(3) .504(3) .8445(16) .033(7) Uiso ? ? 1.00000 ? ? H3b .582(3) .363(3) .8502(15) .028(7) Uiso ? ? 1.00000 ? ? H112 .253(2) .525(3) .5551(13) .016(6) Uiso ? ? 1.00000 ? ? H113 .081(3) .585(3) .4657(16) .031(7) Uiso ? ? 1.00000 ? ? H114 -.122(3) .774(3) .4595(16) .033(7) Uiso ? ? 1.00000 ? ? H115 -.143(3) .919(3) .5340(15) .033(7) Uiso ? ? 1.00000 ? ? H116 .035(2) .850(3) .6318(14) .024(6) Uiso ? ? 1.00000 ? ? H122 .304(2) .859(3) .5907(15) .026(7) Uiso ? ? 1.00000 ? ? H123 .350(3) 1.020(3) .6309(16) .033(7) Uiso ? ? 1.00000 ? ? H124 .326(3) 1.035(3) .7522(16) .034(8) Uiso ? ? 1.00000 ? ? H125 .288(3) .892(3) .8493(16) .030(7) Uiso ? ? 1.00000 ? ? H126 .255(2) .724(2) .8174(13) .009(5) Uiso ? ? 1.00000 ? ? H0a .448(3) .463(3) .6454(15) .027(7) Uiso ? ? 1.00000 ? ? H0b .458(2) .585(3) .6029(15) .024(6) Uiso ? ? 1.00000 ? ? H212 .821(4) .315(4) .816(2) .070(12) Uiso ? ? 1.00000 ? ? H213 .990(3) .133(4) .808(2) .053(10) Uiso ? ? 1.00000 ? ? H214 1.027(3) .041(3) .7041(18) .047(9) Uiso ? ? 1.00000 ? ? H215 .853(3) .148(3) .6093(18) .045(9) Uiso ? ? 1.00000 ? ? H216 .663(3) .333(3) .6172(17) .035(8) Uiso ? ? 1.00000 ? ? H222 .623(2) .627(3) .8281(15) .023(6) Uiso ? ? 1.00000 ? ? H223 .668(3) .807(3) .8110(16) .034(7) Uiso ? ? 1.00000 ? ? H224 .698(3) .908(3) .6893(17) .045(9) Uiso ? ? 1.00000 ? ? H225 .666(3) .842(3) .5828(17) .037(8) Uiso ? ? 1.00000 ? ? H226 .624(3) .665(3) .6019(16) .036(8) Uiso ? ? 1.00000 ? ? H01a -.102(6) 1.029(7) .891(4) .048(19) Uiso ? ? .50000 ? ? H01b -.144(6) .958(6) .982(3) .033(14) 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 .01608(9) .01785(9) .02134(9) -.00839(7) .00131(6) -.00533(7) Ru2 .02074(9) .01458(9) .01995(9) -.00760(7) -.00077(6) -.00536(6) Ru3 .02096(9) .02081(10) .01660(8) -.01055(7) .00071(6) -.00458(7) C11 .0244(11) .0241(12) .0300(12) -.0110(10) .0022(9) -.0072(9) O11 .0355(10) .0426(12) .0445(11) -.0249(9) .0122(8) -.0081(9) C12 .0195(11) .0230(12) .0306(12) -.0101(9) .0015(9) -.0053(9) O12 .0298(9) .0393(11) .0342(9) -.0165(8) -.0063(7) -.0109(8) C13 .0230(11) .0275(12) .0272(11) -.0141(10) .0054(9) -.0086(9) O13 .0349(10) .0206(9) .0496(11) -.0105(8) .0086(8) -.0101(8) C21 .0322(13) .0238(12) .0286(12) -.0126(10) -.0005(9) -.0097(10) O21 .0498(12) .0340(10) .0388(10) -.0287(9) .0089(9) -.0093(8) C22 .0311(13) .0240(12) .0272(11) -.0107(11) .0000(9) -.0088(9) O22 .0332(10) .0332(11) .0483(11) .0006(9) .0003(9) -.0157(9) C23 .0331(13) .0166(11) .0292(12) -.0089(10) -.0028(10) -.0061(9) O23 .0559(12) .0293(10) .0316(9) -.0161(9) -.0100(8) -.0115(8) C31 .0351(13) .0340(14) .0217(11) -.0186(11) .0021(9) -.0077(10) O31 .0602(14) .0609(14) .0332(10) -.0447(12) .0138(9) -.0095(10) C32 .0210(11) .0335(13) .0236(11) -.0119(10) .0023(8) -.0093(10) O32 .0358(10) .0448(11) .0407(10) -.0195(9) .0014(8) -.0242(9) C33 .0327(13) .0340(14) .0228(11) -.0146(12) -.0023(9) -.0020(10) O33 .0383(12) .0437(13) .0497(12) .0017(10) -.0110(10) -.0009(10) C1 .0180(10) .0148(10) .0186(9) -.0076(8) .0019(7) -.0057(8) C2 .0206(10) .0176(10) .0196(10) -.0100(8) .0014(8) -.0075(8) C3 .0199(11) .0283(12) .0192(10) -.0126(10) -.0008(8) -.0047(9) P1 .0158(2) .0158(3) .0173(2) -.0067(2) .00014(19) -.0051(2) C111 .0188(10) .0233(11) .0189(10) -.0103(9) -.0028(8) -.0025(8) C112 .0285(12) .0289(13) .0232(11) -.0131(11) -.0009(9) -.0075(10) C113 .0430(15) .0421(16) .0265(12) -.0225(13) -.0056(11) -.0116(11) C114 .0355(14) .0468(17) .0303(13) -.0206(13) -.0130(11) -.0016(12) C115 .0235(12) .0326(14) .0349(13) -.0090(11) -.0074(10) -.0017(11) C116 .0223(11) .0244(12) .0277(11) -.0103(9) -.0019(9) -.0052(9) C121 .0154(9) .0166(10) .0244(10) -.0055(8) .0009(8) -.0075(8) C122 .0209(11) .0180(11) .0270(11) -.0068(9) .0019(8) -.0049(9) C123 .0245(12) .0155(11) .0412(14) -.0082(9) .0020(10) -.0032(10) C124 .0289(13) .0172(12) .0460(15) -.0094(10) -.0033(10) -.0117(11) C125 .0271(12) .0219(12) .0328(12) -.0080(10) -.0014(9) -.0126(10) C126 .0193(10) .0178(11) .0250(11) -.0074(9) .0014(8) -.0073(9) C0 .0191(10) .0216(11) .0194(10) -.0085(9) .0015(8) -.0081(9) P2 .0155(2) .0188(3) .0205(3) -.0072(2) .0008(2) -.0059(2) C221 .0151(10) .0183(11) .0291(11) -.0065(8) .0002(8) -.0064(9) C222 .0279(12) .0258(12) .0252(11) -.0133(10) -.0014(9) -.0045(9) C223 .0328(13) .0299(13) .0385(14) -.0162(11) -.0042(11) -.0112(11) C224 .0243(12) .0239(13) .0489(15) -.0135(10) -.0040(10) -.0069(11) C225 .0272(12) .0317(14) .0339(13) -.0171(11) .0009(10) -.0003(11) C226 .0242(11) .0311(13) .0279(12) -.0155(10) .0030(9) -.0074(10) C211 .0175(10) .0190(11) .0313(11) -.0069(9) .0010(8) -.0073(9) C212 .0329(15) .051(2) .071(2) .0039(14) -.0196(14) -.0394(18) C213 .0289(16) .057(2) .090(3) .0105(15) -.0272(17) -.042(2) C214 .0237(13) .0247(14) .0592(18) -.0022(11) .0014(12) -.0150(13) C215 .0318(14) .0396(16) .0443(16) -.0040(12) .0047(12) -.0235(13) C216 .0257(13) .0337(14) .0352(14) -.0033(11) -.0004(10) -.0134(11) B .0484(19) .0367(17) .0300(14) -.0179(15) .0072(13) -.0122(13) F1 .0710(12) .0363(10) .0448(10) -.0261(9) -.0027(9) -.0082(8) F2 .0650(12) .0720(13) .0249(8) -.0307(10) .0081(8) -.0116(8) F3 .0976(16) .0648(13) .0386(9) -.0594(12) .0076(10) -.0104(9) F4 .0574(12) .0799(15) .0575(12) -.0091(11) .0174(10) -.0383(11) Cl1 .0534(10) .0494(10) .0736(12) -.0151(8) .0117(9) -.0153(9) Cl2 .0890(16) .0516(11) .117(2) -.0402(11) .0426(14) -.0445(13) C01 .053(4) .036(3) .076(5) -.019(3) .019(4) -.016(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 . . 2.7372(2) ? Ru1 Ru3 . . 2.9388(2) ? Ru1 C11 . . 1.935(3) ? Ru1 C12 . . 1.915(3) ? Ru1 C13 . . 1.919(2) ? Ru1 C1 . . 2.108(2) ? Ru1 H . . 1.71(3) ? Ru2 Ru3 . . 2.7502(3) ? Ru2 C21 . . 1.899(3) ? Ru2 C22 . . 1.926(2) ? Ru2 C23 . . 1.922(3) ? Ru2 C1 . . 2.185(2) ? Ru2 C2 . . 2.206(3) ? Ru3 C31 . . 1.964(3) ? Ru3 C32 . . 1.903(3) ? Ru3 C33 . . 1.898(2) ? Ru3 C2 . . 2.077(2) ? Ru3 H . . 1.80(2) ? C11 O11 . . 1.135(4) ? C12 O12 . . 1.136(4) ? C13 O13 . . 1.141(3) ? C21 O21 . . 1.142(4) ? C22 O22 . . 1.134(3) ? C23 O23 . . 1.137(4) ? C31 O31 . . 1.133(4) ? C32 O32 . . 1.138(4) ? C33 O33 . . 1.142(3) ? C1 C2 . . 1.413(3) ? C1 P1 . . 1.758(2) ? C2 C3 . . 1.532(4) ? C3 P2 . . 1.828(2) ? C3 H3a . . .87(4) ? C3 H3b . . .94(2) ? P1 C111 . . 1.789(2) ? P1 C121 . . 1.797(3) ? P1 C0 . . 1.819(2) ? C111 C112 . . 1.398(4) ? C111 C116 . . 1.397(3) ? C112 C113 . . 1.401(4) ? C112 H112 . . .90(2) ? C113 C114 . . 1.380(4) ? C113 H113 . . .92(3) ? C114 C115 . . 1.382(5) ? C114 H114 . . .94(3) ? C115 C116 . . 1.395(4) ? C115 H115 . . .95(2) ? C116 H116 . . .95(3) ? C121 C122 . . 1.401(3) ? C121 C126 . . 1.400(3) ? C122 C123 . . 1.393(4) ? C122 H122 . . 1.01(3) ? C123 C124 . . 1.381(4) ? C123 H123 . . .89(3) ? C124 C125 . . 1.376(4) ? C124 H124 . . .82(4) ? C125 C126 . . 1.392(4) ? C125 H125 . . .92(3) ? C126 H126 . . .90(2) ? C0 P2 . . 1.813(2) ? C0 H0a . . .86(4) ? C0 H0b . . .92(3) ? P2 C221 . . 1.802(3) ? P2 C211 . . 1.794(2) ? C221 C222 . . 1.390(4) ? C221 C226 . . 1.398(3) ? C222 C223 . . 1.392(5) ? C222 H222 . . .87(3) ? C223 C224 . . 1.375(4) ? C223 H223 . . .92(3) ? C224 C225 . . 1.381(5) ? C224 H224 . . .89(4) ? C225 C226 . . 1.392(5) ? C225 H225 . . .92(3) ? C226 H226 . . .89(3) ? C211 C212 . . 1.392(4) ? C211 C216 . . 1.376(4) ? C212 C213 . . 1.380(4) ? C212 H212 . . .92(4) ? C213 C214 . . 1.374(6) ? C213 H213 . . .81(3) ? C214 C215 . . 1.355(4) ? C214 H214 . . .92(3) ? C215 C216 . . 1.391(4) ? C215 H215 . . .86(4) ? C216 H216 . . .89(3) ? B F1 . . 1.402(4) ? B F2 . . 1.381(4) ? B F3 . . 1.365(6) ? B F4 . . 1.388(4) ? Cl1 C01 . . 1.737(6) ? Cl1 Cl2 . '2 577' 1.050(4) ? Cl2 C01 . . 1.757(10) ? C01 H01a . . .97(6) ? C01 H01b . . 1.03(7) ? 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 . . . 57.832(8) ? Ru2 Ru1 C11 . . . 108.51(7) ? Ru2 Ru1 C12 . . . 89.69(6) ? Ru2 Ru1 C13 . . . 152.68(8) ? Ru2 Ru1 C1 . . . 51.63(6) ? Ru2 Ru1 H . . . 91.9(8) ? Ru3 Ru1 C11 . . . 95.03(7) ? Ru3 Ru1 C12 . . . 147.02(6) ? Ru3 Ru1 C13 . . . 115.16(8) ? Ru3 Ru1 C1 . . . 67.69(5) ? Ru3 Ru1 H . . . 34.2(8) ? C11 Ru1 C12 . . . 89.88(11) ? C11 Ru1 C13 . . . 98.17(11) ? C11 Ru1 C1 . . . 158.29(7) ? C11 Ru1 H . . . 86.5(12) ? C12 Ru1 C13 . . . 96.25(10) ? C12 Ru1 C1 . . . 97.86(10) ? C12 Ru1 H . . . 176.4(11) ? C13 Ru1 C1 . . . 101.08(10) ? C13 Ru1 H . . . 83.8(9) ? C1 Ru1 H . . . 85.7(11) ? Ru1 Ru2 Ru3 . . . 64.763(8) ? Ru1 Ru2 C21 . . . 87.30(7) ? Ru1 Ru2 C22 . . . 164.25(10) ? Ru1 Ru2 C23 . . . 97.98(6) ? Ru1 Ru2 C1 . . . 49.17(6) ? Ru1 Ru2 C2 . . . 72.29(5) ? Ru3 Ru2 C21 . . . 82.20(9) ? Ru3 Ru2 C22 . . . 101.56(8) ? Ru3 Ru2 C23 . . . 162.71(6) ? Ru3 Ru2 C1 . . . 70.76(6) ? Ru3 Ru2 C2 . . . 48.01(6) ? C21 Ru2 C22 . . . 98.93(11) ? C21 Ru2 C23 . . . 96.65(13) ? C21 Ru2 C1 . . . 135.20(9) ? C21 Ru2 C2 . . . 130.20(11) ? C22 Ru2 C23 . . . 95.66(11) ? C22 Ru2 C1 . . . 120.66(11) ? C22 Ru2 C2 . . . 92.86(11) ? C23 Ru2 C1 . . . 99.17(9) ? C23 Ru2 C2 . . . 130.20(10) ? C1 Ru2 C2 . . . 37.54(7) ? Ru1 Ru3 Ru2 . . . 57.405(7) ? Ru1 Ru3 C31 . . . 94.86(7) ? Ru1 Ru3 C32 . . . 110.88(6) ? Ru1 Ru3 C33 . . . 149.42(9) ? Ru1 Ru3 C2 . . . 69.55(6) ? Ru1 Ru3 H . . . 32.2(11) ? Ru2 Ru3 C31 . . . 107.12(9) ? Ru2 Ru3 C32 . . . 150.38(7) ? Ru2 Ru3 C33 . . . 92.08(9) ? Ru2 Ru3 C2 . . . 52.14(8) ? Ru2 Ru3 H . . . 89.5(10) ? C31 Ru3 C32 . . . 100.69(12) ? C31 Ru3 C33 . . . 92.53(11) ? C31 Ru3 C2 . . . 158.40(12) ? C31 Ru3 H . . . 87.6(10) ? C32 Ru3 C33 . . . 96.75(12) ? C32 Ru3 C2 . . . 98.91(11) ? C32 Ru3 H . . . 81.5(12) ? C33 Ru3 C2 . . . 94.12(9) ? C33 Ru3 H . . . 178.3(12) ? C2 Ru3 H . . . 86.3(9) ? Ru1 C11 O11 . . . 178.1(2) ? Ru1 C12 O12 . . . 175.5(2) ? Ru1 C13 O13 . . . 177.8(2) ? Ru2 C21 O21 . . . 177.3(3) ? Ru2 C22 O22 . . . 176.7(2) ? Ru2 C23 O23 . . . 176.2(3) ? Ru3 C31 O31 . . . 177.8(2) ? Ru3 C32 O32 . . . 176.9(2) ? Ru3 C33 O33 . . . 179.5(2) ? Ru1 C1 Ru2 . . . 79.20(9) ? Ru1 C1 C2 . . . 112.12(15) ? Ru1 C1 P1 . . . 126.39(9) ? Ru2 C1 C2 . . . 72.05(13) ? Ru2 C1 P1 . . . 129.43(12) ? C2 C1 P1 . . . 119.35(19) ? Ru2 C2 Ru3 . . . 79.85(9) ? Ru2 C2 C1 . . . 70.42(16) ? Ru2 C2 C3 . . . 128.68(16) ? Ru3 C2 C1 . . . 110.64(16) ? Ru3 C2 C3 . . . 121.54(14) ? C1 C2 C3 . . . 126.1(2) ? C2 C3 P2 . . . 121.07(16) ? C2 C3 H3a . . . 110(2) ? C2 C3 H3b . . . 110(2) ? P2 C3 H3a . . . 105(2) ? P2 C3 H3b . . . 106.5(17) ? H3a C3 H3b . . . 104(3) ? C1 P1 C111 . . . 115.57(12) ? C1 P1 C121 . . . 106.91(11) ? C1 P1 C0 . . . 108.10(9) ? C111 P1 C121 . . . 110.40(10) ? C111 P1 C0 . . . 108.55(11) ? C121 P1 C0 . . . 106.96(13) ? P1 C111 C112 . . . 120.57(15) ? P1 C111 C116 . . . 118.5(2) ? C112 C111 C116 . . . 120.7(2) ? C111 C112 C113 . . . 118.6(2) ? C111 C112 H112 . . . 122(2) ? C113 C112 H112 . . . 119(2) ? C112 C113 C114 . . . 120.5(3) ? C112 C113 H113 . . . 118.4(15) ? C114 C113 H113 . . . 121.0(15) ? C113 C114 C115 . . . 120.9(3) ? C113 C114 H114 . . . 120.0(18) ? C115 C114 H114 . . . 119.1(18) ? C114 C115 C116 . . . 119.7(2) ? C114 C115 H115 . . . 120(2) ? C116 C115 H115 . . . 120(2) ? C111 C116 C115 . . . 119.6(3) ? C111 C116 H116 . . . 116.4(13) ? C115 C116 H116 . . . 123.9(13) ? P1 C121 C122 . . . 119.56(19) ? P1 C121 C126 . . . 119.61(18) ? C122 C121 C126 . . . 120.4(3) ? C121 C122 C123 . . . 119.1(2) ? C121 C122 H122 . . . 116.5(19) ? C123 C122 H122 . . . 124.3(19) ? C122 C123 C124 . . . 119.7(3) ? C122 C123 H123 . . . 119(2) ? C124 C123 H123 . . . 121(2) ? C123 C124 C125 . . . 121.6(3) ? C123 C124 H124 . . . 117(2) ? C125 C124 H124 . . . 121(2) ? C124 C125 C126 . . . 119.7(3) ? C124 C125 H125 . . . 117(2) ? C126 C125 H125 . . . 123(2) ? C121 C126 C125 . . . 119.4(2) ? C121 C126 H126 . . . 121.4(18) ? C125 C126 H126 . . . 119.1(18) ? P1 C0 P2 . . . 109.79(13) ? P1 C0 H0a . . . 105.2(18) ? P1 C0 H0b . . . 112.2(14) ? P2 C0 H0a . . . 107.4(16) ? P2 C0 H0b . . . 113(2) ? H0a C0 H0b . . . 109(3) ? C3 P2 C0 . . . 108.97(12) ? C3 P2 C221 . . . 110.31(13) ? C3 P2 C211 . . . 110.38(10) ? C0 P2 C221 . . . 109.39(11) ? C0 P2 C211 . . . 109.21(12) ? C221 P2 C211 . . . 108.57(12) ? P2 C221 C222 . . . 122.61(19) ? P2 C221 C226 . . . 117.8(2) ? C222 C221 C226 . . . 119.6(3) ? C221 C222 C223 . . . 119.7(2) ? C221 C222 H222 . . . 121(2) ? C223 C222 H222 . . . 120(2) ? C222 C223 C224 . . . 120.6(3) ? C222 C223 H223 . . . 120(2) ? C224 C223 H223 . . . 119(2) ? C223 C224 C225 . . . 120.1(3) ? C223 C224 H224 . . . 121(2) ? C225 C224 H224 . . . 119(2) ? C224 C225 C226 . . . 120.2(3) ? C224 C225 H225 . . . 123(3) ? C226 C225 H225 . . . 116(3) ? C221 C226 C225 . . . 119.8(3) ? C221 C226 H226 . . . 121(2) ? C225 C226 H226 . . . 119(2) ? P2 C211 C212 . . . 117.8(2) ? P2 C211 C216 . . . 122.60(17) ? C212 C211 C216 . . . 119.6(2) ? C211 C212 C213 . . . 119.3(4) ? C211 C212 H212 . . . 120(2) ? C213 C212 H212 . . . 121(2) ? C212 C213 C214 . . . 120.8(3) ? C212 C213 H213 . . . 111(3) ? C214 C213 H213 . . . 126(3) ? C213 C214 C215 . . . 119.9(3) ? C213 C214 H214 . . . 119(2) ? C215 C214 H214 . . . 121(2) ? C214 C215 C216 . . . 120.6(3) ? C214 C215 H215 . . . 121.3(18) ? C216 C215 H215 . . . 118.0(18) ? C211 C216 C215 . . . 119.8(3) ? C211 C216 H216 . . . 118(2) ? C215 C216 H216 . . . 123(2) ? F1 B F2 . . . 107.9(3) ? F1 B F3 . . . 110.0(2) ? F1 B F4 . . . 107.7(3) ? F2 B F3 . . . 111.4(3) ? F2 B F4 . . . 109.6(2) ? F3 B F4 . . . 110.2(3) ? C01 Cl1 Cl2 . . '2 577' 101.2(4) ? C01 Cl2 Cl1 . . '2 577' 130.7(3) ? Cl1 C01 Cl2 . . . 112.2(5) ? Cl1 C01 H01a . . . 108(4) ? Cl1 C01 H01b . . . 108(3) ? Cl2 C01 H01a . . . 101(5) ? Cl2 C01 H01b . . . 101(4) ? H01a C01 H01b . . . 125(6) ? Ru1 H Ru3 . . . 113.6(17) ? 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 #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ru1 O11 3.071(2) . . ? Ru1 O12 3.049(2) . . ? Ru1 O13 3.0596(18) . . ? Ru1 C21 3.257(2) . . ? Ru1 C23 3.556(3) . . ? Ru1 C31 3.671(2) . . ? Ru1 C2 2.947(2) . . ? Ru1 P1 3.4549(6) . . ? Ru1 H126 3.45(3) . . ? Ru2 C11 3.821(2) . . ? Ru2 C12 3.332(2) . . ? Ru2 O21 3.041(2) . . ? Ru2 O22 3.0585(17) . . ? Ru2 O23 3.057(2) . . ? Ru2 C31 3.822(2) . . ? Ru2 C33 3.398(3) . . ? Ru2 C3 3.382(3) . . ? Ru2 P1 3.5699(6) . . ? Ru2 F2 3.8119(18) . . ? Ru2 H 3.28(3) . . ? Ru2 H3b 3.52(4) . . ? Ru2 H124 3.42(4) . '1 545' ? Ru2 H0a 3.54(3) . . ? Ru3 C11 3.658(3) . . ? Ru3 C21 3.123(3) . . ? Ru3 O21 3.851(3) . . ? Ru3 C22 3.660(3) . . ? Ru3 O31 3.097(3) . . ? Ru3 O32 3.040(3) . . ? Ru3 O33 3.0402(18) . . ? Ru3 C1 2.8943(19) . . ? Ru3 C3 3.161(3) . . ? Ru3 H3a 3.33(3) . . ? Ru3 H3b 3.23(3) . . ? C11 C12 2.720(3) . . ? C11 C13 2.913(4) . . ? C11 H 2.50(4) . . ? O11 Cl1 3.473(3) . '2 567' ? O11 Cl2 3.459(4) . '1 545' ? C12 C13 2.855(4) . . ? C12 C23 2.998(3) . . ? C13 H 2.43(2) . . ? O13 Cl1 3.652(3) . . ? C21 C22 2.907(4) . . ? C21 C23 2.854(3) . . ? O21 Cl1 3.872(4) . '1 545' ? O21 Cl1 3.880(3) . '2 567' ? O21 Cl2 3.843(4) . '2 567' ? O21 Cl2 3.685(4) . '1 545' ? O21 H01b 2.35(6) . '2 567' ? C22 C23 2.852(3) . . ? C22 C2 3.000(4) . . ? C22 F2 2.965(3) . . ? O22 F2 3.043(3) . . ? C23 F2 3.010(3) . . ? O23 B 3.479(4) . . ? O23 F2 3.109(3) . . ? O23 F3 3.126(3) . . ? O23 H114 2.66(4) . '2 566' ? C31 C32 2.978(5) . . ? C31 C33 2.791(4) . . ? C31 H 2.61(3) . . ? O31 Cl1 3.690(4) . '2 567' ? C32 C33 2.842(4) . . ? C32 Cl1 3.789(3) . . ? C32 H 2.42(3) . . ? O32 Cl1 3.276(2) . . ? O32 Cl2 3.330(3) . '2 577' ? O32 H3a 2.67(3) . '2 667' ? C33 C2 2.912(3) . . ? O33 Cl1 3.787(4) . '2 667' ? O33 Cl2 3.395(4) . '1 645' ? C1 C3 2.626(3) . . ? C1 C121 2.857(3) . . ? C1 C0 2.896(3) . . ? C1 H 2.61(3) . . ? C1 H126 2.59(3) . . ? C2 P1 2.7426(18) . . ? C2 P2 2.929(2) . . ? C2 H 2.66(3) . . ? C2 H3a 2.00(4) . . ? C2 H3b 2.05(3) . . ? C3 C0 2.963(3) . . ? C3 C221 2.979(4) . . ? C3 C211 2.974(3) . . ? P1 C112 2.775(3) . . ? P1 C116 2.746(2) . . ? P1 C122 2.771(3) . . ? P1 C126 2.771(3) . . ? P1 P2 2.9708(8) . . ? P1 H116 2.77(2) . . ? P1 H0a 2.21(3) . . ? P1 H0b 2.33(3) . . ? C111 C113 2.407(4) . . ? C111 C114 2.770(4) . . ? C111 C115 2.413(3) . . ? C111 C121 2.945(4) . . ? C111 C0 2.929(3) . . ? C111 H112 2.03(3) . . ? C111 H116 2.00(3) . . ? C112 C114 2.414(3) . . ? C112 C115 2.800(3) . . ? C112 C116 2.429(4) . . ? C112 F1 3.454(3) . . ? C112 H113 2.00(3) . . ? C113 C115 2.402(4) . . ? C113 C116 2.782(5) . . ? C113 H112 2.01(2) . . ? C113 H114 2.02(2) . . ? C114 C116 2.401(5) . . ? C114 H113 2.01(3) . . ? C114 H115 2.03(3) . . ? C115 F4 3.566(3) . '1 465' ? C115 H114 2.02(4) . . ? C115 H116 2.08(3) . . ? C116 H115 2.04(3) . . ? C121 C123 2.409(4) . . ? C121 C124 2.761(4) . . ? C121 C125 2.411(4) . . ? C121 C0 2.906(3) . . ? C121 H122 2.06(3) . . ? C121 H126 2.02(2) . . ? C122 C124 2.399(4) . . ? C122 C125 2.793(4) . . ? C122 C126 2.430(3) . . ? C122 F4 3.320(3) . '2 666' ? C122 H123 1.98(4) . . ? C123 C125 2.406(4) . . ? C123 C126 2.788(4) . . ? C123 F3 3.424(4) . '1 565' ? C123 H122 2.14(3) . . ? C123 H124 1.89(4) . . ? C124 C126 2.393(4) . . ? C124 H123 2.00(3) . . ? C124 H125 1.98(3) . . ? C125 Cl1 3.842(3) . . ? C125 H124 1.93(4) . . ? C125 H126 1.99(3) . . ? C126 H125 2.05(4) . . ? C0 C221 2.950(4) . . ? C0 C211 2.940(3) . . ? C0 F1 3.478(4) . . ? C0 F1 3.293(3) . '2 666' ? P2 C222 2.808(3) . . ? P2 C226 2.748(3) . . ? P2 C212 2.735(3) . . ? P2 C216 2.787(3) . . ? P2 H3a 2.21(3) . . ? P2 H3b 2.28(3) . . ? P2 H0a 2.23(3) . . ? P2 H0b 2.33(2) . . ? P2 H212 2.80(3) . . ? C221 C223 2.406(5) . . ? C221 C224 2.782(4) . . ? C221 C225 2.414(4) . . ? C221 C211 2.920(4) . . ? C221 H222 1.98(3) . . ? C221 H226 2.01(3) . . ? C222 C224 2.404(4) . . ? C222 C225 2.776(4) . . ? C222 C226 2.410(4) . . ? C222 H223 2.01(4) . . ? C223 C225 2.387(4) . . ? C223 C226 2.770(5) . . ? C223 H222 1.98(3) . . ? C223 H224 1.98(3) . . ? C224 C226 2.404(5) . . ? C224 F2 3.467(3) . '1 565' ? C224 H223 1.99(3) . . ? C224 H225 2.04(3) . . ? C225 F3 3.101(4) . '2 666' ? C225 H224 1.97(4) . . ? C225 H226 1.98(4) . . ? C226 B 3.683(4) . '2 666' ? C226 F1 3.395(4) . '2 666' ? C226 F3 3.131(3) . '2 666' ? C226 H225 1.98(3) . . ? C211 C213 2.392(3) . . ? C211 C214 2.765(3) . . ? C211 C215 2.394(4) . . ? C211 H212 2.01(4) . . ? C211 H216 1.96(3) . . ? C212 C214 2.395(5) . . ? C212 C215 2.755(6) . . ? C212 C216 2.392(5) . . ? C212 Cl2 3.529(4) . '1 645' ? C212 H213 1.83(3) . . ? C213 C215 2.362(6) . . ? C213 C216 2.747(5) . . ? C213 Cl2 3.723(5) . '1 645' ? C213 H212 2.01(4) . . ? C213 H214 1.99(4) . . ? C213 H01a 2.59(7) . '1 645' ? C214 C216 2.385(3) . . ? C214 H213 1.96(4) . . ? C214 H215 1.95(4) . . ? C215 F2 3.588(4) . . ? C215 F4 3.346(5) . . ? C215 H214 1.99(3) . . ? C215 H216 2.01(2) . . ? C216 B 3.569(6) . . ? C216 F1 3.547(4) . . ? C216 F2 3.059(5) . . ? C216 F4 3.452(5) . . ? C216 H215 1.95(3) . . ? B H122 3.35(3) . '2 666' ? B H0a 3.42(3) . . ? B H0b 3.31(3) . '2 666' ? B H216 2.97(4) . . ? B H224 3.37(3) . '1 545' ? B H226 2.97(3) . '2 666' ? F1 F1 3.702(3) . '2 666' ? F1 F2 2.250(2) . . ? F1 F3 2.266(4) . . ? F1 F4 2.252(3) . . ? F1 H112 2.57(2) . . ? F1 H0a 2.82(3) . . ? F1 H0b 3.35(3) . . ? F1 H0b 2.39(3) . '2 666' ? F1 H216 2.72(4) . . ? F1 H226 2.54(3) . '2 666' ? F2 F3 2.269(3) . . ? F2 F4 2.263(3) . . ? F2 H0a 2.86(3) . . ? F2 H216 2.66(4) . . ? F2 H224 2.86(3) . '1 545' ? F3 F3 3.987(3) . '2 656' ? F3 F4 2.258(4) . . ? F3 H114 3.26(3) . '2 566' ? F3 H123 2.53(3) . '1 545' ? F3 H225 2.48(3) . '2 666' ? F3 H225 3.35(3) . '1 545' ? F3 H226 2.59(3) . '2 666' ? F4 H115 2.63(3) . '1 645' ? F4 H122 2.35(3) . '2 666' ? F4 H0b 3.21(2) . '2 666' ? F4 H215 2.78(4) . . ? F4 H216 3.02(4) . . ? F4 H224 3.12(3) . '1 545' ? F4 H225 3.19(4) . '1 545' ? Cl1 Cl1 3.349(3) . '2 577' ? Cl1 Cl2 2.901(3) . . ? Cl1 C01 2.569(10) . '2 577' ? Cl1 H125 3.23(3) . . ? Cl1 H126 3.60(2) . . ? Cl1 H213 3.41(3) . '1 465' ? Cl1 H01a 3.15(8) . '2 577' ? Cl1 H01a 2.24(5) . . ? Cl1 H01b 2.28(6) . . ? Cl1 H01b 2.82(8) . '2 577' ? Cl2 Cl2 2.796(3) . '2 577' ? Cl2 C01 2.197(7) . '2 577' ? Cl2 H212 2.96(3) . '1 465' ? Cl2 H213 3.18(4) . '1 465' ? Cl2 H01a 2.93(6) . '2 577' ? Cl2 H01a 2.16(8) . . ? Cl2 H01b 2.57(6) . '2 577' ? Cl2 H01b 2.20(8) . . ? C01 C01 2.831(14) . '2 577' ? H3a H3b 1.42(4) . . ? H3a H222 2.17(5) . . ? H112 H113 2.28(4) . . ? H113 H114 2.33(3) . . ? H114 H115 2.32(5) . . ? H122 H123 2.40(5) . . ? H123 H124 2.22(4) . . ? H124 H125 2.23(4) . . ? H125 H126 2.33(5) . . ? H0a H0b 1.45(4) . . ? H0a H216 2.34(4) . . ? H212 H213 2.15(5) . . ? H213 H214 2.31(5) . . ? H213 H01a 2.20(9) . '1 645' ? H214 H215 2.28(4) . . ? H215 H216 2.27(4) . . ? H222 H223 2.28(5) . . ? H223 H224 2.28(4) . . ? H224 H225 2.32(5) . . ? H225 H226 2.23(5) . . ? H01a H01b 1.77(9) . . ? _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 1086 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 -23 _reflns_limit_l_max 24 _reflns_number_observed ? _reflns_d_resolution_high .728 _reflns_d_resolution_low 17.103 _diffrn_reflns_av_sigmaI/netI .024 _diffrn_reflns_theta_min 1.19 _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 .032 _refine_ls_wR_factor_all .07 _refine_ls_goodness_of_fit_all 2.476 _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