# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2066 ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_global _audit_creation_method Xtal3.6 _audit_creation_date 99-09-30 _audit_update_record ? #============================================================================== # (Publishing Staff Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _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 'Skelton, B. W.' _publ_contact_author_address ; Department of Chemistry University of Western Australia Nedlands Western Australia 6907 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; ? #<< paper title text ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; 'White, Allan H.' . ; Crystallography Centre, University of Western Australia, Nedlands, WA 6907 Australia. ; _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_br491 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C26 H6 O17 Ru5 W1' _chemical_formula_moiety ? _chemical_formula_weight 1279.52 _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 8.550(3) _cell_length_b 24.014(10) _cell_length_c 16.669(6) _cell_angle_alpha 90.00000 _cell_angle_beta 90.34(3) _cell_angle_gamma 90.00000 _cell_volume 3422(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.481 _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 16.5 _cell_measurement_theta_max 16.8 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 5.57 _exptl_crystal_description plate _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_size_rad ? _exptl_crystal_colour black _diffrn_measurement_device_type ; CAD4 ; _diffrn_measurement_method '2\Q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_T_max 0.64 _diffrn_reflns_number 6008 _reflns_number_total 6008 _reflns_Friedel_coverage ? _reflns_number_gt 3957 _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 ? _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt .034 _refine_ls_wR_factor_ref .034 _refine_ls_goodness_of_fit_ref 1.332 _refine_ls_number_reflns 3957 _refine_ls_number_parameters 447 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed #<< use NfA code _refine_ls_shift/su_max .086 _refine_diff_density_min -.680 _refine_diff_density_max 0.748 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 2512(44) _refine_ls_abs_structure_details none _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 ? 0 104 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 68 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 20 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 20 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' W ? 0 4 -1.421 6.872 '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 .22655(10) .07582(3) .39229(5) .0504(5) Uani ? ? 1.00000 ? ? Ru2 .10493(9) .15929(3) .29029(5) .0412(5) Uani ? ? 1.00000 ? ? Ru3 .03950(9) .16237(3) .45373(5) .0401(5) Uani ? ? 1.00000 ? ? W4 .25236(5) .39838(2) .39084(3) .0459(3) Uani ? ? 1.00000 ? ? Ru5 .40532(9) .30936(3) .48486(4) .0374(4) Uani ? ? 1.00000 ? ? Ru6 .45834(9) .30833(3) .32706(4) .0411(5) Uani ? ? 1.00000 ? ? C11 .0765(16) .0153(5) .3811(8) .081(9) Uani ? ? 1.00000 ? ? O11 -.0144(11) -.0172(4) .3699(7) .113(8) Uani ? ? 1.00000 ? ? C12 .3134(15) .0482(5) .4919(8) .072(9) Uani ? ? 1.00000 ? ? O12 .3702(12) .0355(4) .5486(5) .099(7) Uani ? ? 1.00000 ? ? C13 .3862(15) .0446(5) .3248(8) .069(8) Uani ? ? 1.00000 ? ? O13 .4804(12) .0280(4) .2879(6) .106(8) Uani ? ? 1.00000 ? ? C21 -.0172(14) .1038(5) .2369(7) .065(8) Uani ? ? 1.00000 ? ? O21 -.0991(12) .0728(4) .2053(6) .111(8) Uani ? ? 1.00000 ? ? C22 .2734(14) .1526(5) .2153(6) .062(8) Uani ? ? 1.00000 ? ? O22 .3734(10) .1476(4) .1732(5) .101(7) Uani ? ? 1.00000 ? ? C23 .0150(13) .2271(5) .2440(7) .058(8) Uani ? ? 1.00000 ? ? O23 -.0317(12) .2674(4) .2231(6) .095(7) Uani ? ? 1.00000 ? ? C31 -.1227(15) .1113(5) .4840(7) .069(8) Uani ? ? 1.00000 ? ? O31 -.2238(11) .0823(4) .4969(6) .109(8) Uani ? ? 1.00000 ? ? C32 .1385(14) .1576(5) .5568(7) .063(8) Uani ? ? 1.00000 ? ? O32 .1998(11) .1561(4) .6166(5) .097(7) Uani ? ? 1.00000 ? ? C33 -.0665(12) .2319(4) .4732(6) .050(7) Uani ? ? 1.00000 ? ? O33 -.1214(9) .2739(3) .4822(5) .076(6) Uani ? ? 1.00000 ? ? C41 .4588(17) .4342(5) .3860(8) .085(10) Uani ? ? 1.00000 ? ? O41 .5763(11) .4588(4) .3818(6) .101(7) Uani ? ? 1.00000 ? ? C42 .2305(16) .4063(5) .2733(8) .077(9) Uani ? ? 1.00000 ? ? O42 .2123(13) .4121(4) .2055(5) .113(8) Uani ? ? 1.00000 ? ? C51 .5539(13) .3623(5) .5237(6) .057(7) Uani ? ? 1.00000 ? ? O51 .6449(10) .3931(4) .5459(5) .092(6) Uani ? ? 1.00000 ? ? C52 .2711(12) .3074(4) .5762(6) .051(7) Uani ? ? 1.00000 ? ? O52 .1926(10) .3064(4) .6313(5) .092(7) Uani ? ? 1.00000 ? ? C53 .5172(13) .2437(5) .5146(6) .053(7) Uani ? ? 1.00000 ? ? O53 .5712(10) .2024(3) .5302(5) .077(6) Uani ? ? 1.00000 ? ? C61 .6460(16) .3491(5) .3088(7) .078(9) Uani ? ? 1.00000 ? ? O61 .7605(11) .3717(5) .2961(6) .121(8) Uani ? ? 1.00000 ? ? C62 .3884(12) .3000(4) .2165(6) .050(7) Uani ? ? 1.00000 ? ? O62 .3492(10) .2920(4) .1536(4) .086(6) Uani ? ? 1.00000 ? ? C63 .5699(12) .2398(5) .3293(6) .057(7) Uani ? ? 1.00000 ? ? O63 .6320(10) .1986(4) .3322(6) .094(7) Uani ? ? 1.00000 ? ? C1 .2668(10) .1555(4) .3937(5) .036(5) Uani ? ? 1.00000 ? ? C2 .2213(9) .2071(4) .3870(5) .034(5) Uani ? ? 1.00000 ? ? C3 .2720(9) .2634(4) .3943(5) .035(5) Uani ? ? 1.00000 ? ? C4 .2328(10) .3165(4) .3863(5) .035(5) Uani ? ? 1.00000 ? ? C401 .129(3) .4267(8) .5083(9) .110(14) Uani ? ? 1.00000 ? ? C402 .2039(17) .4717(7) .4786(11) .093(12) Uani ? ? 1.00000 ? ? C403 .1368(17) .4851(5) .4049(9) .082(10) Uani ? ? 1.00000 ? ? C404 .0220(16) .4482(7) .3886(8) .080(10) Uani ? ? 1.00000 ? ? C405 .0123(18) .4108(6) .4517(13) .104(13) Uani ? ? 1.00000 ? ? H -.06343 .16153 .35985 .09500 Uiso ? ? 1.00000 ? ? H401 .15287 .40980 .55934 .13500 Uiso ? ? 1.00000 ? ? H402 .29296 .49190 .50430 .11300 Uiso ? ? 1.00000 ? ? H403 .17245 .51578 .36915 .10300 Uiso ? ? 1.00000 ? ? H404 -.04449 .44808 .34057 .10000 Uiso ? ? 1.00000 ? ? H405 -.05905 .37965 .45659 .12700 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 .0550(6) .0326(5) .0637(6) .0048(4) .0077(5) .0006(4) Ru2 .0457(5) .0399(5) .0380(5) -.0060(4) .0003(4) -.0047(4) Ru3 .0419(5) .0372(5) .0412(5) .0004(4) .0074(4) .0046(4) W4 .0539(3) .0326(2) .0512(3) -.0036(2) -.0085(2) -.0021(2) Ru5 .0369(4) .0444(5) .0310(4) -.0015(4) -.0024(3) -.0041(4) Ru6 .0399(5) .0508(5) .0325(4) -.0106(4) .0017(3) -.0036(4) C11 .093(10) .031(7) .118(12) .001(7) -.002(9) .000(7) O11 .105(8) .063(7) .169(10) -.026(6) -.003(7) .000(7) C12 .085(9) .054(8) .078(9) .015(7) .024(8) .011(7) O12 .123(8) .104(8) .070(6) .035(6) -.005(6) .023(6) C13 .076(9) .050(7) .080(9) .009(7) .003(7) -.016(7) O13 .101(8) .103(8) .113(8) .030(6) .027(6) -.024(6) C21 .076(8) .064(8) .056(7) -.013(7) .015(6) -.009(6) O21 .128(9) .093(7) .112(8) -.044(6) -.028(7) -.038(6) C22 .060(8) .083(9) .043(7) -.016(7) .003(6) -.018(6) O22 .080(7) .146(9) .075(6) -.019(6) .027(5) -.029(6) C23 .065(8) .054(8) .057(7) -.012(6) .000(6) -.005(6) O23 .127(8) .056(6) .103(7) .016(6) -.026(6) .013(5) C31 .081(9) .057(8) .070(8) .006(7) .035(7) .022(6) O31 .103(7) .070(6) .154(9) -.023(6) .057(7) .025(6) C32 .068(8) .063(8) .057(8) .009(6) .006(6) .002(7) O32 .116(8) .131(9) .045(5) .034(6) -.012(5) -.003(5) C33 .054(7) .043(7) .053(7) .002(5) .014(5) .005(5) O33 .061(5) .051(5) .116(7) .013(4) .017(5) -.003(5) C41 .109(11) .045(8) .102(11) -.006(8) -.032(9) .005(7) O41 .092(7) .073(6) .137(9) -.037(6) -.002(6) -.002(6) C42 .118(11) .039(7) .073(9) .007(7) -.015(8) .003(7) O42 .177(11) .107(8) .053(6) .026(7) -.020(6) .013(6) C51 .067(8) .069(8) .036(6) -.017(6) -.010(5) -.005(6) O51 .096(7) .091(7) .089(6) -.052(6) -.034(5) .001(5) C52 .053(7) .059(7) .040(6) .015(6) -.002(5) -.005(5) O52 .077(6) .133(8) .066(6) .016(6) .032(5) -.004(6) C53 .056(7) .069(8) .034(6) -.003(6) -.004(5) .006(6) O53 .084(6) .068(6) .079(6) .024(5) -.011(5) .015(5) C61 .091(10) .087(10) .056(8) -.028(8) -.001(7) -.017(7) O61 .082(7) .150(10) .131(9) -.077(7) .049(6) -.051(7) C62 .057(7) .057(7) .037(6) -.018(6) .012(5) -.005(5) O62 .099(7) .130(8) .030(4) -.030(6) -.006(4) -.006(5) C63 .040(6) .085(9) .046(6) .011(6) .015(5) -.003(6) O63 .072(6) .102(8) .107(8) .030(6) .016(5) -.004(6) C1 .035(5) .042(6) .032(5) .000(5) -.004(4) -.002(5) C2 .023(5) .049(6) .029(5) -.004(4) .003(4) -.001(4) C3 .026(5) .052(6) .028(5) -.000(5) -.002(4) -.006(5) C4 .029(5) .047(6) .028(5) -.002(4) -.001(4) -.007(4) C401 .162(18) .092(13) .076(10) .088(13) .010(11) -.003(10) C402 .089(11) .075(11) .114(13) .026(9) -.019(10) -.042(10) C403 .090(10) .043(8) .112(12) .010(7) .011(9) -.006(8) C404 .070(9) .081(10) .088(10) .009(8) -.002(8) -.015(9) C405 .091(11) .041(8) .181(18) -.004(8) .065(12) -.026(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 . . 2.8229(13) ? Ru1 Ru3 . . 2.8188(13) ? Ru1 C11 . . 1.947(13) ? Ru1 C12 . . 1.932(13) ? Ru1 C13 . . 1.926(13) ? Ru1 C1 . . 1.944(9) ? Ru2 Ru3 . . 2.7855(15) ? Ru2 C21 . . 1.910(12) ? Ru2 C22 . . 1.919(11) ? Ru2 C23 . . 1.957(12) ? Ru2 C1 . . 2.205(8) ? Ru2 C2 . . 2.210(9) ? Ru2 H . . 1.8545(9) ? Ru3 C31 . . 1.922(12) ? Ru3 C32 . . 1.914(12) ? Ru3 C33 . . 1.929(11) ? Ru3 C1 . . 2.197(9) ? Ru3 C2 . . 2.197(8) ? Ru3 H . . 1.7909(10) ? W4 Ru5 . . 2.9516(11) ? W4 Ru6 . . 2.9884(12) ? W4 C41 . . 1.966(14) ? W4 C42 . . 1.976(13) ? W4 C4 . . 1.975(9) ? W4 C401 . . 2.329(17) ? W4 C402 . . 2.328(17) ? W4 C403 . . 2.318(13) ? W4 C404 . . 2.304(14) ? W4 C405 . . 2.314(17) ? Ru5 Ru6 . . 2.6719(13) ? Ru5 C51 . . 1.907(11) ? Ru5 C52 . . 1.912(10) ? Ru5 C53 . . 1.909(12) ? Ru5 C3 . . 2.186(9) ? Ru5 C4 . . 2.208(8) ? Ru6 C61 . . 1.906(13) ? Ru6 C62 . . 1.944(10) ? Ru6 C63 . . 1.903(12) ? Ru6 C3 . . 2.232(9) ? Ru6 C4 . . 2.181(8) ? C11 O11 . . 1.116(16) ? C12 O12 . . 1.104(16) ? C13 O13 . . 1.092(16) ? C21 O21 . . 1.147(15) ? C22 O22 . . 1.116(14) ? C23 O23 . . 1.102(15) ? C31 O31 . . 1.131(15) ? C32 O32 . . 1.124(14) ? C33 O33 . . 1.123(13) ? C41 O41 . . 1.167(17) ? C42 O42 . . 1.148(15) ? C51 O51 . . 1.135(14) ? C52 O52 . . 1.141(13) ? C53 O53 . . 1.123(14) ? C61 O61 . . 1.139(16) ? C62 O62 . . 1.116(12) ? C63 O63 . . 1.124(16) ? C1 C2 . . 1.302(13) ? C2 C3 . . 1.426(14) ? C3 C4 . . 1.324(13) ? C401 C402 . . 1.35(2) ? C401 C405 . . 1.42(3) ? C401 H401 . . .962(16) ? C402 C403 . . 1.39(2) ? C402 H402 . . .997(15) ? C403 C404 . . 1.35(2) ? C403 H403 . . .995(14) ? C404 C405 . . 1.39(2) ? C404 H404 . . .979(13) ? C405 H405 . . .968(14) ? 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 . . . 59.17(4) ? Ru2 Ru1 C11 . . . 103.4(4) ? Ru2 Ru1 C12 . . . 154.1(4) ? Ru2 Ru1 C13 . . . 100.6(4) ? Ru2 Ru1 C1 . . . 51.1(2) ? Ru3 Ru1 C11 . . . 102.2(4) ? Ru3 Ru1 C12 . . . 99.0(4) ? Ru3 Ru1 C13 . . . 154.8(4) ? Ru3 Ru1 C1 . . . 51.0(3) ? C11 Ru1 C12 . . . 94.3(5) ? C11 Ru1 C13 . . . 97.0(5) ? C11 Ru1 C1 . . . 148.5(5) ? C12 Ru1 C13 . . . 95.6(5) ? C12 Ru1 C1 . . . 105.1(4) ? C13 Ru1 C1 . . . 105.3(4) ? Ru1 Ru2 Ru3 . . . 60.34(3) ? Ru1 Ru2 C21 . . . 89.1(3) ? Ru1 Ru2 C22 . . . 93.3(3) ? Ru1 Ru2 C23 . . . 166.1(3) ? Ru1 Ru2 C1 . . . 43.4(2) ? Ru1 Ru2 C2 . . . 76.5(2) ? Ru1 Ru2 H . . . 85.90(4) ? Ru3 Ru2 C21 . . . 111.2(3) ? Ru3 Ru2 C22 . . . 142.7(3) ? Ru3 Ru2 C23 . . . 106.4(3) ? Ru3 Ru2 C1 . . . 50.6(2) ? Ru3 Ru2 C2 . . . 50.6(2) ? Ru3 Ru2 H . . . 39.34(3) ? C21 Ru2 C22 . . . 92.7(5) ? C21 Ru2 C23 . . . 100.6(5) ? C21 Ru2 C1 . . . 132.4(4) ? C21 Ru2 C2 . . . 160.9(4) ? C21 Ru2 H . . . 83.6(3) ? C22 Ru2 C23 . . . 96.2(5) ? C22 Ru2 C1 . . . 92.0(4) ? C22 Ru2 C2 . . . 100.5(4) ? C22 Ru2 H . . . 176.2(3) ? C23 Ru2 C1 . . . 125.8(4) ? C23 Ru2 C2 . . . 91.7(4) ? C23 Ru2 H . . . 85.3(3) ? C1 Ru2 C2 . . . 34.3(3) ? C1 Ru2 H . . . 89.9(2) ? C2 Ru2 H . . . 82.9(2) ? Ru1 Ru3 Ru2 . . . 60.49(3) ? Ru1 Ru3 C31 . . . 92.1(4) ? Ru1 Ru3 C32 . . . 91.9(3) ? Ru1 Ru3 C33 . . . 165.4(3) ? Ru1 Ru3 C1 . . . 43.4(2) ? Ru1 Ru3 C2 . . . 76.8(2) ? Ru1 Ru3 H . . . 87.20(4) ? Ru2 Ru3 C31 . . . 112.9(3) ? Ru2 Ru3 C32 . . . 141.8(3) ? Ru2 Ru3 C33 . . . 106.5(3) ? Ru2 Ru3 C1 . . . 50.9(2) ? Ru2 Ru3 C2 . . . 51.0(2) ? Ru2 Ru3 H . . . 41.02(3) ? C31 Ru3 C32 . . . 92.4(5) ? C31 Ru3 C33 . . . 99.7(5) ? C31 Ru3 C1 . . . 135.5(4) ? C31 Ru3 C2 . . . 163.5(4) ? C31 Ru3 H . . . 82.6(3) ? C32 Ru3 C33 . . . 96.1(5) ? C32 Ru3 C1 . . . 91.0(4) ? C32 Ru3 C2 . . . 100.0(4) ? C32 Ru3 H . . . 174.9(3) ? C33 Ru3 C1 . . . 124.0(4) ? C33 Ru3 C2 . . . 89.8(4) ? C33 Ru3 H . . . 85.9(3) ? C1 Ru3 C2 . . . 34.5(3) ? C1 Ru3 H . . . 91.8(2) ? C2 Ru3 H . . . 84.7(2) ? Ru5 W4 Ru6 . . . 53.46(3) ? Ru5 W4 C41 . . . 86.8(4) ? Ru5 W4 C42 . . . 129.4(3) ? Ru5 W4 C4 . . . 48.4(2) ? Ru5 W4 C401 . . . 88.0(5) ? Ru5 W4 C402 . . . 107.1(4) ? Ru5 W4 C403 . . . 141.7(4) ? Ru5 W4 C404 . . . 139.5(4) ? Ru5 W4 C405 . . . 104.6(4) ? Ru6 W4 C41 . . . 76.8(4) ? Ru6 W4 C42 . . . 76.7(4) ? Ru6 W4 C4 . . . 46.8(2) ? Ru6 W4 C401 . . . 141.3(5) ? Ru6 W4 C402 . . . 151.4(4) ? Ru6 W4 C403 . . . 159.8(4) ? Ru6 W4 C404 . . . 151.1(4) ? Ru6 W4 C405 . . . 140.8(3) ? C41 W4 C42 . . . 89.8(6) ? C41 W4 C4 . . . 120.7(4) ? C41 W4 C401 . . . 108.5(6) ? C41 W4 C402 . . . 81.8(5) ? C41 W4 C403 . . . 89.7(5) ? C41 W4 C404 . . . 122.7(5) ? C41 W4 C405 . . . 139.5(5) ? C42 W4 C4 . . . 92.9(4) ? C42 W4 C401 . . . 139.9(6) ? C42 W4 C402 . . . 122.3(5) ? C42 W4 C403 . . . 88.6(5) ? C42 W4 C404 . . . 81.8(5) ? C42 W4 C405 . . . 110.1(7) ? C4 W4 C401 . . . 106.5(5) ? C4 W4 C402 . . . 139.6(5) ? C4 W4 C403 . . . 149.6(4) ? C4 W4 C404 . . . 116.3(4) ? C4 W4 C405 . . . 94.0(4) ? C401 W4 C402 . . . 33.7(6) ? C401 W4 C403 . . . 57.2(6) ? C401 W4 C404 . . . 58.2(6) ? C401 W4 C405 . . . 35.7(7) ? C402 W4 C403 . . . 34.8(6) ? C402 W4 C404 . . . 57.5(5) ? C402 W4 C405 . . . 57.7(5) ? C403 W4 C404 . . . 34.0(5) ? C403 W4 C405 . . . 57.4(5) ? C404 W4 C405 . . . 35.0(6) ? W4 Ru5 Ru6 . . . 63.97(3) ? W4 Ru5 C51 . . . 89.4(3) ? W4 Ru5 C52 . . . 100.0(3) ? W4 Ru5 C53 . . . 163.0(3) ? W4 Ru5 C3 . . . 76.8(3) ? W4 Ru5 C4 . . . 42.0(2) ? Ru6 Ru5 C51 . . . 102.9(3) ? Ru6 Ru5 C52 . . . 152.8(3) ? Ru6 Ru5 C53 . . . 99.2(3) ? Ru6 Ru5 C3 . . . 53.6(2) ? Ru6 Ru5 C4 . . . 52.0(2) ? C51 Ru5 C52 . . . 98.5(4) ? C51 Ru5 C53 . . . 97.5(5) ? C51 Ru5 C3 . . . 156.1(4) ? C51 Ru5 C4 . . . 129.9(4) ? C52 Ru5 C53 . . . 94.3(4) ? C52 Ru5 C3 . . . 103.0(4) ? C52 Ru5 C4 . . . 101.1(4) ? C53 Ru5 C3 . . . 91.2(4) ? C53 Ru5 C4 . . . 126.1(4) ? C3 Ru5 C4 . . . 35.1(3) ? W4 Ru6 Ru5 . . . 62.57(3) ? W4 Ru6 C61 . . . 100.6(4) ? W4 Ru6 C62 . . . 103.5(3) ? W4 Ru6 C63 . . . 156.3(3) ? W4 Ru6 C3 . . . 75.4(2) ? W4 Ru6 C4 . . . 41.4(2) ? Ru5 Ru6 C61 . . . 107.5(3) ? Ru5 Ru6 C62 . . . 151.7(3) ? Ru5 Ru6 C63 . . . 94.4(3) ? Ru5 Ru6 C3 . . . 52.0(2) ? Ru5 Ru6 C4 . . . 53.0(2) ? C61 Ru6 C62 . . . 99.0(5) ? C61 Ru6 C63 . . . 91.5(5) ? C61 Ru6 C3 . . . 158.9(4) ? C61 Ru6 C4 . . . 140.7(5) ? C62 Ru6 C63 . . . 94.6(4) ? C62 Ru6 C3 . . . 102.1(4) ? C62 Ru6 C4 . . . 99.8(4) ? C63 Ru6 C3 . . . 86.1(4) ? C63 Ru6 C4 . . . 120.9(4) ? C3 Ru6 C4 . . . 34.9(3) ? Ru1 C11 O11 . . . 174.6(12) ? Ru1 C12 O12 . . . 174.9(11) ? Ru1 C13 O13 . . . 177.6(11) ? Ru2 C21 O21 . . . 175.4(11) ? Ru2 C22 O22 . . . 177.9(10) ? Ru2 C23 O23 . . . 174.5(10) ? Ru3 C31 O31 . . . 175.0(11) ? Ru3 C32 O32 . . . 177.8(10) ? Ru3 C33 O33 . . . 176.0(9) ? W4 C41 O41 . . . 175.4(11) ? W4 C42 O42 . . . 177.2(12) ? Ru5 C51 O51 . . . 178.5(10) ? Ru5 C52 O52 . . . 179.1(9) ? Ru5 C53 O53 . . . 173.7(10) ? Ru6 C61 O61 . . . 177.1(11) ? Ru6 C62 O62 . . . 176.1(9) ? Ru6 C63 O63 . . . 177.7(10) ? Ru1 C1 Ru2 . . . 85.5(3) ? Ru1 C1 Ru3 . . . 85.6(3) ? Ru1 C1 C2 . . . 151.9(7) ? Ru2 C1 Ru3 . . . 78.5(3) ? Ru2 C1 C2 . . . 73.0(5) ? Ru3 C1 C2 . . . 72.8(5) ? Ru2 C2 Ru3 . . . 78.4(3) ? Ru2 C2 C1 . . . 72.7(5) ? Ru2 C2 C3 . . . 133.6(6) ? Ru3 C2 C1 . . . 72.8(5) ? Ru3 C2 C3 . . . 129.5(6) ? C1 C2 C3 . . . 143.6(8) ? Ru5 C3 Ru6 . . . 74.4(3) ? Ru5 C3 C2 . . . 134.0(6) ? Ru5 C3 C4 . . . 73.4(5) ? Ru6 C3 C2 . . . 129.3(6) ? Ru6 C3 C4 . . . 70.5(5) ? C2 C3 C4 . . . 145.9(8) ? W4 C4 Ru5 . . . 89.6(3) ? W4 C4 Ru6 . . . 91.8(3) ? W4 C4 C3 . . . 158.9(7) ? Ru5 C4 Ru6 . . . 75.0(3) ? Ru5 C4 C3 . . . 71.5(5) ? Ru6 C4 C3 . . . 74.6(5) ? W4 C401 C402 . . . 73.1(10) ? W4 C401 C405 . . . 71.6(10) ? W4 C401 H401 . . . 121.8(15) ? C402 C401 C405 . . . 107.7(14) ? C402 C401 H401 . . . 124.4(19) ? C405 C401 H401 . . . 128(2) ? W4 C402 C401 . . . 73.2(10) ? W4 C402 C403 . . . 72.2(9) ? W4 C402 H402 . . . 120.0(11) ? C401 C402 C403 . . . 108.4(14) ? C401 C402 H402 . . . 126.3(17) ? C403 C402 H402 . . . 125.3(15) ? W4 C403 C402 . . . 73.0(8) ? W4 C403 C404 . . . 72.5(8) ? W4 C403 H403 . . . 118.2(11) ? C402 C403 C404 . . . 108.7(13) ? C402 C403 H403 . . . 125.0(14) ? C404 C403 H403 . . . 126.2(15) ? W4 C404 C403 . . . 73.6(8) ? W4 C404 C405 . . . 72.9(9) ? W4 C404 H404 . . . 120.3(11) ? C403 C404 C405 . . . 108.7(13) ? C403 C404 H404 . . . 125.7(15) ? C405 C404 H404 . . . 125.6(15) ? W4 C405 C401 . . . 72.7(10) ? W4 C405 C404 . . . 72.1(9) ? W4 C405 H405 . . . 119.9(12) ? C401 C405 C404 . . . 106.5(13) ? C401 C405 H405 . . . 126(2) ? C404 C405 H405 . . . 127.2(19) ? Ru2 H Ru3 . . . 99.64(4) ? 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 3.061(10) . . ? Ru1 O12 3.033(9) . . ? Ru1 O13 3.018(10) . . ? Ru1 C21 3.383(11) . . ? Ru1 C31 3.468(12) . . ? Ru1 C32 3.459(12) . . ? Ru1 C2 3.153(10) . . ? Ru1 H 3.2650(12) . . ? Ru2 O21 3.055(10) . . ? Ru2 O22 3.035(9) . . ? Ru2 O23 3.056(9) . . ? Ru2 C3 3.356(9) . . ? Ru3 O31 3.050(9) . . ? Ru3 O32 3.037(8) . . ? Ru3 O33 3.050(8) . . ? Ru3 C3 3.293(9) . . ? W4 O41 3.130(9) . . ? W4 O42 3.123(8) . . ? W4 C51 3.498(11) . . ? W4 C3 3.246(10) . . ? W4 H401 2.9523(11) . . ? W4 H402 2.9552(10) . . ? W4 H403 2.9228(12) . . ? W4 H404 2.9229(9) . . ? W4 H405 2.9202(10) . . ? Ru5 C41 3.452(13) . . ? Ru5 O51 3.042(9) . . ? Ru5 O52 3.053(8) . . ? Ru5 O53 3.027(8) . . ? Ru5 C63 3.397(11) . . ? Ru5 C2 3.338(9) . . ? Ru5 H401 3.4713(11) . . ? Ru6 C41 3.178(12) . . ? Ru6 C42 3.180(12) . . ? Ru6 O61 3.044(10) . . ? Ru6 O62 3.059(7) . . ? Ru6 O63 3.026(10) . . ? Ru6 C2 3.323(9) . . ? C11 C12 2.845(19) . . ? C11 C13 2.901(19) . . ? C12 C13 2.859(18) . . ? O13 H403 2.933(10) . '2 545' ? O13 H404 2.929(10) . '2 545' ? C21 C22 2.772(17) . . ? C21 C23 2.976(17) . . ? C21 H 2.508(11) . . ? C22 C23 2.886(16) . . ? C22 C1 2.975(13) . . ? C23 C2 2.995(14) . . ? C23 H 2.583(11) . . ? C31 C32 2.769(17) . . ? C31 C33 2.943(16) . . ? C31 H 2.451(12) . . ? C32 C33 2.859(15) . . ? C32 C1 2.938(14) . . ? C33 C2 2.919(13) . . ? C33 H 2.536(10) . . ? O33 H405 2.630(8) . . ? C41 C42 2.78(2) . . ? C41 C51 2.981(17) . . ? C41 C61 2.901(18) . . ? C41 C402 2.83(2) . . ? C41 H402 2.802(14) . . ? O41 C61 2.963(16) . . ? O41 O61 2.987(14) . . ? O41 H402 2.496(10) . '3 666' ? C42 C4 2.863(15) . . ? C42 C404 2.815(19) . . ? C42 H404 2.797(13) . . ? C51 C52 2.894(15) . . ? C51 C53 2.869(17) . . ? O51 H402 2.934(9) . '3 666' ? O51 H405 2.961(9) . '1 655' ? C52 C53 2.802(15) . . ? C52 H401 2.672(11) . . ? O52 H401 2.778(9) . . ? C53 C3 2.932(13) . . ? C61 C62 2.927(16) . . ? C61 C63 2.728(18) . . ? O61 H404 2.585(10) . '1 655' ? C62 C63 2.827(15) . . ? C63 C3 2.831(13) . . ? O63 H 2.788(9) . '1 655' ? C1 C3 2.592(13) . . ? C1 H 2.879(9) . . ? C2 C4 2.630(13) . . ? C2 H 2.704(8) . . ? C401 C403 2.22(2) . . ? C401 C404 2.25(2) . . ? C401 H402 2.10(2) . . ? C401 H405 2.14(2) . . ? C402 C404 2.23(2) . . ? C402 C405 2.24(2) . . ? C402 H401 2.054(17) . . ? C402 H403 2.125(17) . . ? C403 C405 2.22(2) . . ? C403 H402 2.129(15) . . ? C403 H404 2.079(14) . . ? C404 H403 2.098(15) . . ? C404 H405 2.117(15) . . ? C405 H401 2.15(2) . . ? C405 H404 2.11(2) . . ? H401 H402 2.4852(7) . . ? H401 H405 2.5892(6) . . ? H402 H403 2.5373(7) . . ? H403 H404 2.5100(7) . . ? H404 H405 2.5414(7) . . ? _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 2368 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 11 8 -4 -11 -8 4 11 -8 -4 11 8 4 12 -7 -4 12 7 -4 -12 7 4 -12 -7 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min -19 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 28 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _reflns_number_observed 3957 _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 'single counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type F _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .060 _refine_ls_wR_factor_all .039 _refine_ls_goodness_of_fit_all 1.220 _refine_ls_shift/su_mean .0096 #========================================================================== # 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_br516 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C44 H28 O10 P2 Ru3 W1' _chemical_formula_moiety ? _chemical_formula_weight 1265.71 _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 16.066(13) _cell_length_b 15.250(11) _cell_length_c 18.27(2) _cell_angle_alpha 90.00000 _cell_angle_beta 95.15(8) _cell_angle_gamma 90.00000 _cell_volume 4458(7) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.886 _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 15.3 _cell_measurement_theta_max 15.7 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 3.696 _exptl_crystal_description block _exptl_crystal_size_max 1.17 _exptl_crystal_size_mid 0.82 _exptl_crystal_size_min 0.40 _exptl_crystal_size_rad ? _exptl_crystal_colour black _diffrn_measurement_device_type CAD4 _diffrn_measurement_method '2\Q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min 0.14 _exptl_absorpt_correction_T_max 0.35 _diffrn_reflns_number 10241 _reflns_number_total 10241 _reflns_Friedel_coverage 0 _reflns_number_gt 7507 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 29.97 _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 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .046 _refine_ls_wR_factor_ref .049 _refine_ls_goodness_of_fit_ref 2.048 _refine_ls_number_reflns 7507 _refine_ls_number_parameters 546 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment mixed _refine_ls_shift/su_max .02 _refine_diff_density_min -2.288 _refine_diff_density_max 1.983 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 1180(186) _refine_ls_abs_structure_details none _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 DIFDAT SORTRF ADDREF ABSORB' _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 ? 0 176 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 112 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 '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' W ? 0 4 -1.421 6.872 '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 .15365(4) .73726(3) .43824(3) .0383(3) Uani ? ? 1.00000 ? ? Ru2 .09982(4) .84117(4) .55096(3) .0512(4) Uani ? ? 1.00000 ? ? Ru3 .25152(4) .75009(4) .57105(3) .0428(3) Uani ? ? 1.00000 ? ? W4 .06908(2) .58988(2) .83648(2) .04848(18) Uani ? ? 1.00000 ? ? C11 .2013(5) .8184(5) .3751(4) .055(5) Uani ? ? 1.00000 ? ? O11 .2323(4) .8683(4) .3391(3) .078(4) Uani ? ? 1.00000 ? ? C12 .0557(5) .7202(5) .3751(4) .055(5) Uani ? ? 1.00000 ? ? O12 -.0054(4) .7082(5) .3398(4) .088(5) Uani ? ? 1.00000 ? ? C21 .1124(7) .9365(6) .4854(6) .089(7) Uani ? ? 1.00000 ? ? O21 .1202(6) .9940(5) .4495(5) .153(8) Uani ? ? 1.00000 ? ? C22 .0829(6) .9016(6) .6395(6) .083(7) Uani ? ? 1.00000 ? ? O22 .0734(5) .9356(6) .6939(5) .136(7) Uani ? ? 1.00000 ? ? C23 -.0153(6) .8304(5) .5133(5) .064(5) Uani ? ? 1.00000 ? ? O23 -.0818(4) .8233(5) .4891(4) .092(5) Uani ? ? 1.00000 ? ? C31 .3267(5) .8076(5) .5158(4) .059(5) Uani ? ? 1.00000 ? ? O31 .3747(4) .8447(4) .4837(3) .089(5) Uani ? ? 1.00000 ? ? C32 .2998(5) .7606(6) .6692(5) .069(6) Uani ? ? 1.00000 ? ? O32 .3298(5) .7672(5) .7287(3) .106(5) Uani ? ? 1.00000 ? ? C41 .1167(7) .6148(7) .9370(5) .088(7) Uani ? ? 1.00000 ? ? O41 .1441(6) .6313(6) .9963(4) .147(7) Uani ? ? 1.00000 ? ? C42 .0394(6) .7126(7) .8488(4) .071(6) Uani ? ? 1.00000 ? ? O42 .0175(5) .7842(5) .8580(4) .111(6) Uani ? ? 1.00000 ? ? C43 .1905(7) .5778(8) .8298(6) .098(8) Uani ? ? 1.00000 ? ? O43 .2633(5) .5705(7) .8246(5) .151(8) Uani ? ? 1.00000 ? ? C1 .1260(4) .6991(4) .5368(3) .039(4) Uani ? ? 1.00000 ? ? C2 .1239(4) .7100(5) .6084(4) .046(4) Uani ? ? 1.00000 ? ? C3 .1049(4) .6776(5) .6761(4) .047(4) Uani ? ? 1.00000 ? ? C4 .0908(5) .6505(5) .7345(4) .049(4) Uani ? ? 1.00000 ? ? P1 .22908(11) .62307(11) .39613(9) .0368(9) Uani ? ? 1.00000 ? ? C111 .1821(4) .5140(4) .3959(4) .041(4) Uani ? ? 1.00000 ? ? C112 .2137(5) .4471(5) .3549(5) .055(5) Uani ? ? 1.00000 ? ? C113 .1791(6) .3646(5) .3536(5) .070(6) Uani ? ? 1.00000 ? ? C114 .1114(6) .3490(5) .3924(5) .068(6) Uani ? ? 1.00000 ? ? C115 .0792(6) .4139(6) .4330(5) .068(6) Uani ? ? 1.00000 ? ? C116 .1139(5) .4973(5) .4348(4) .057(5) Uani ? ? 1.00000 ? ? C121 .2572(4) .6306(4) .3022(3) .040(4) Uani ? ? 1.00000 ? ? C122 .3372(5) .6189(6) .2807(4) .064(5) Uani ? ? 1.00000 ? ? C123 .3496(6) .6205(7) .2069(5) .079(6) Uani ? ? 1.00000 ? ? C124 .2871(6) .6318(5) .1547(4) .062(5) Uani ? ? 1.00000 ? ? C125 .2080(6) .6436(5) .1734(4) .060(5) Uani ? ? 1.00000 ? ? C126 .1943(5) .6435(5) .2482(4) .052(4) Uani ? ? 1.00000 ? ? C0 .3303(4) .6086(4) .4497(3) .041(4) Uani ? ? 1.00000 ? ? P2 .31992(12) .61953(13) .54864(9) .0431(10) Uani ? ? 1.00000 ? ? C211 .2796(4) .5136(5) .5735(4) .046(4) Uani ? ? 1.00000 ? ? C212 .3122(6) .4364(6) .5480(5) .073(6) Uani ? ? 1.00000 ? ? C213 .2826(7) .3562(6) .5656(6) .089(7) Uani ? ? 1.00000 ? ? C214 .2173(8) .3517(6) .6106(6) .090(7) Uani ? ? 1.00000 ? ? C215 .1842(8) .4246(7) .6345(7) .112(9) Uani ? ? 1.00000 ? ? C216 .2156(6) .5063(6) .6183(5) .081(6) Uani ? ? 1.00000 ? ? C221 .4261(5) .6188(5) .5921(4) .050(4) Uani ? ? 1.00000 ? ? C222 .4921(5) .6597(6) .5615(4) .067(5) Uani ? ? 1.00000 ? ? C223 .5689(5) .6677(7) .6006(5) .077(6) Uani ? ? 1.00000 ? ? C224 .5801(6) .6390(7) .6722(5) .076(6) Uani ? ? 1.00000 ? ? C225 .5165(7) .5975(7) .7024(5) .091(7) Uani ? ? 1.00000 ? ? C226 .4403(6) .5865(7) .6629(5) .079(6) Uani ? ? 1.00000 ? ? C401 .0339(6) .4487(6) .7961(6) .080(7) Uani ? ? 1.00000 ? ? C402 .0232(7) .4534(6) .8709(6) .086(7) Uani ? ? 1.00000 ? ? C403 -.0389(7) .5128(7) .8807(6) .084(7) Uani ? ? 1.00000 ? ? C404 -.0673(6) .5442(6) .8109(7) .084(7) Uani ? ? 1.00000 ? ? C405 -.0236(7) .5050(6) .7603(4) .074(6) Uani ? ? 1.00000 ? ? H .202(4) .856(4) .590(4) .07(2) Uiso ? ? 1.00000 ? ? H112 .26092 .45948 .32657 .06700 Uiso ? ? 1.00000 ? ? H113 .20267 .31773 .32552 .08500 Uiso ? ? 1.00000 ? ? H114 .08489 .29129 .39045 .08500 Uiso ? ? 1.00000 ? ? H115 .03141 .40142 .46006 .08400 Uiso ? ? 1.00000 ? ? H116 .09082 .54377 .46360 .07300 Uiso ? ? 1.00000 ? ? H122 .38469 .60977 .31727 .07900 Uiso ? ? 1.00000 ? ? H123 .40599 .61194 .19190 .09500 Uiso ? ? 1.00000 ? ? H124 .29880 .63237 .10348 .07700 Uiso ? ? 1.00000 ? ? H125 .16206 .65230 .13501 .07600 Uiso ? ? 1.00000 ? ? H126 .13763 .65334 .26197 .06700 Uiso ? ? 1.00000 ? ? H0a .36973 .65093 .43430 .05300 Uiso ? ? 1.00000 ? ? H0b .35270 .55109 .43944 .05300 Uiso ? ? 1.00000 ? ? H212 .35734 .44118 .51642 .09100 Uiso ? ? 1.00000 ? ? H213 .30718 .30252 .54734 .10900 Uiso ? ? 1.00000 ? ? H214 .19503 .29614 .62481 .11200 Uiso ? ? 1.00000 ? ? H215 .13468 .42202 .66084 .13200 Uiso ? ? 1.00000 ? ? H216 .19287 .55888 .63867 .10100 Uiso ? ? 1.00000 ? ? H222 .48421 .68306 .51066 .08500 Uiso ? ? 1.00000 ? ? H223 .61547 .69549 .57677 .09200 Uiso ? ? 1.00000 ? ? H224 .63383 .64932 .70079 .09100 Uiso ? ? 1.00000 ? ? H225 .52557 .57594 .75313 .11200 Uiso ? ? 1.00000 ? ? H226 .39478 .55578 .68500 .09300 Uiso ? ? 1.00000 ? ? H401 .07367 .41283 .77268 .09900 Uiso ? ? 1.00000 ? ? H402 .05457 .42094 .90949 .10800 Uiso ? ? 1.00000 ? ? H403 -.06161 .53022 .92561 .10600 Uiso ? ? 1.00000 ? ? H404 -.11199 .58721 .79834 .10300 Uiso ? ? 1.00000 ? ? H405 -.03099 .51575 .70708 .08900 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 .0376(3) .0460(3) .0324(3) -.0005(3) .0088(2) .0003(2) Ru2 .0553(4) .0469(3) .0549(4) -.0024(3) .0247(3) -.0060(3) Ru3 .0397(3) .0552(3) .0346(3) -.0137(3) .0090(3) -.0063(2) W4 .0478(2) .0694(2) .02872(14) .00547(16) .00587(12) .00169(13) C11 .062(5) .061(5) .042(4) .006(4) .007(4) -.001(4) O11 .097(5) .075(4) .065(4) -.017(4) .024(4) .022(3) C12 .046(5) .071(5) .050(5) .004(4) .013(4) -.004(4) O12 .053(4) .129(6) .078(5) .003(4) -.011(3) -.008(4) C21 .100(8) .056(5) .120(9) .019(5) .059(7) .015(5) O21 .214(10) .070(5) .195(9) .036(5) .126(8) .053(5) C22 .078(7) .094(7) .085(7) -.023(5) .046(6) -.037(5) O22 .120(7) .168(8) .126(7) -.018(6) .049(6) -.087(6) C23 .069(6) .058(5) .069(6) .013(5) .028(5) .004(4) O23 .060(4) .099(5) .116(6) .009(4) .007(4) -.000(4) C31 .051(5) .067(5) .059(5) -.012(4) .007(4) -.004(4) O31 .082(5) .107(5) .081(5) -.046(4) .025(4) .006(4) C32 .061(6) .092(6) .056(5) -.029(5) .016(5) -.016(5) O32 .113(6) .158(7) .046(4) -.029(5) -.008(4) -.022(4) C41 .094(8) .114(8) .054(6) -.014(6) -.001(5) .006(5) O41 .195(10) .197(9) .042(4) -.038(7) -.035(5) .011(5) C42 .080(7) .087(7) .043(5) -.007(5) -.002(4) .005(4) O42 .122(7) .091(5) .124(7) .015(5) .027(5) -.010(5) C43 .064(7) .138(10) .087(8) .007(7) -.018(6) .021(7) O43 .046(5) .227(10) .181(9) .039(6) .019(5) .025(7) C1 .029(4) .048(4) .040(4) -.006(3) .001(3) -.005(3) C2 .045(4) .055(4) .040(4) -.012(3) .011(3) -.006(3) C3 .035(4) .070(5) .038(4) -.010(4) .009(3) -.005(3) C4 .047(5) .066(5) .033(4) .001(4) .005(3) -.004(3) P1 .0322(10) .0471(9) .0315(9) -.0032(8) .0054(7) -.0008(7) C111 .032(4) .050(4) .041(4) -.005(3) -.000(3) .004(3) C112 .041(5) .051(4) .075(6) .000(4) .012(4) -.003(4) C113 .073(6) .046(4) .092(7) .001(4) .012(5) -.003(4) C114 .070(6) .064(5) .071(6) -.015(5) .007(5) .004(4) C115 .069(6) .071(6) .068(6) -.022(5) .024(5) .003(4) C116 .053(5) .067(5) .052(5) -.015(4) .016(4) -.002(4) C121 .043(4) .045(4) .033(3) -.002(3) .003(3) -.001(3) C122 .044(5) .103(6) .045(4) .014(4) .014(4) .009(4) C123 .068(6) .123(8) .050(5) .020(6) .032(5) .005(5) C124 .085(7) .068(5) .038(4) .003(5) .022(5) -.002(4) C125 .073(6) .071(5) .035(4) -.008(4) .005(4) -.003(4) C126 .045(5) .075(5) .039(4) -.004(4) .011(4) .002(4) C0 .036(4) .055(4) .032(3) -.003(3) .001(3) .000(3) P2 .0348(11) .0608(11) .0336(9) -.0059(9) .0030(8) .0033(8) C211 .042(4) .055(4) .038(4) -.007(3) -.001(3) .005(3) C212 .068(6) .070(6) .087(7) .016(5) .038(5) .011(5) C213 .113(9) .069(6) .089(7) .018(6) .028(7) .016(5) C214 .133(10) .060(6) .081(7) -.016(6) .027(7) .017(5) C215 .145(11) .072(7) .134(10) -.009(7) .101(9) .005(6) C216 .110(8) .061(5) .082(6) -.004(5) .058(6) -.003(5) C221 .039(4) .067(5) .041(4) -.004(4) -.004(3) -.003(3) C222 .043(5) .103(7) .056(5) -.014(5) .008(4) .006(5) C223 .037(5) .119(8) .076(6) -.014(5) .010(5) -.010(6) C224 .050(6) .103(7) .071(6) .013(5) -.015(5) -.013(5) C225 .070(7) .134(9) .066(6) -.010(6) -.011(5) .019(6) C226 .056(6) .122(8) .057(5) -.017(5) -.009(4) .024(5) C401 .072(7) .081(6) .091(8) .005(5) .032(6) -.031(6) C402 .107(9) .069(6) .078(7) .012(6) -.005(6) .021(5) C403 .087(8) .092(7) .079(7) -.035(6) .047(6) -.017(6) C404 .055(6) .082(7) .115(9) .004(5) .001(6) -.006(6) C405 .090(8) .087(7) .043(5) -.025(6) .001(5) -.003(4) # 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 . . 2.796(2) ? Ru1 Ru3 . . 2.777(3) ? Ru1 C11 . . 1.901(8) ? Ru1 C12 . . 1.880(8) ? Ru1 C1 . . 1.980(7) ? Ru1 P1 . . 2.294(2) ? Ru2 Ru3 . . 2.800(2) ? Ru2 C21 . . 1.904(10) ? Ru2 C22 . . 1.908(10) ? Ru2 C23 . . 1.925(9) ? Ru2 C1 . . 2.223(7) ? Ru2 C2 . . 2.274(7) ? Ru2 H . . 1.74(7) ? Ru3 C31 . . 1.862(8) ? Ru3 C32 . . 1.898(9) ? Ru3 C1 . . 2.200(6) ? Ru3 C2 . . 2.302(7) ? Ru3 P2 . . 2.329(2) ? Ru3 H . . 1.86(7) ? W4 C41 . . 1.959(10) ? W4 C42 . . 1.947(10) ? W4 C43 . . 1.979(11) ? W4 C4 . . 2.134(7) ? W4 C401 . . 2.327(10) ? W4 C402 . . 2.313(10) ? W4 C403 . . 2.300(11) ? W4 C404 . . 2.312(9) ? W4 C405 . . 2.335(9) ? C11 O11 . . 1.148(10) ? C12 O12 . . 1.139(10) ? C21 O21 . . 1.113(13) ? C22 O22 . . 1.138(13) ? C23 O23 . . 1.124(11) ? C31 O31 . . 1.156(10) ? C32 O32 . . 1.151(10) ? C41 O41 . . 1.164(12) ? C42 O42 . . 1.168(12) ? C43 O43 . . 1.178(13) ? C1 C2 . . 1.318(9) ? C2 C3 . . 1.391(10) ? C3 C4 . . 1.190(10) ? P1 C111 . . 1.828(7) ? P1 C121 . . 1.817(7) ? P1 C0 . . 1.833(7) ? C111 C112 . . 1.391(10) ? C111 C116 . . 1.382(10) ? C112 C113 . . 1.371(11) ? C112 H112 . . .974(8) ? C113 C114 . . 1.373(13) ? C113 H113 . . .977(9) ? C114 C115 . . 1.361(12) ? C114 H114 . . .978(8) ? C115 C116 . . 1.387(11) ? C115 H115 . . .972(9) ? C116 H116 . . .976(8) ? C121 C122 . . 1.391(11) ? C121 C126 . . 1.364(9) ? C122 C123 . . 1.378(12) ? C122 H122 . . .980(7) ? C123 C124 . . 1.333(12) ? C123 H123 . . .979(10) ? C124 C125 . . 1.354(13) ? C124 H124 . . .971(8) ? C125 C126 . . 1.401(10) ? C125 H125 . . .983(8) ? C126 H126 . . .975(8) ? C0 P2 . . 1.836(7) ? C0 H0a . . .964(7) ? C0 H0b . . .974(6) ? P2 C211 . . 1.810(7) ? P2 C221 . . 1.814(7) ? C211 C212 . . 1.386(11) ? C211 C216 . . 1.379(13) ? C212 C213 . . 1.362(13) ? C212 H212 . . .969(9) ? C213 C214 . . 1.391(16) ? C213 H213 . . .979(10) ? C214 C215 . . 1.321(15) ? C214 H214 . . .966(10) ? C215 C216 . . 1.391(14) ? C215 H215 . . .965(13) ? C216 H216 . . .966(9) ? C221 C222 . . 1.393(11) ? C221 C226 . . 1.383(11) ? C222 C223 . . 1.371(11) ? C222 H222 . . .994(8) ? C223 C224 . . 1.378(14) ? C223 H223 . . .994(9) ? C224 C225 . . 1.358(15) ? C224 H224 . . .977(9) ? C225 C226 . . 1.380(13) ? C225 H225 . . .979(10) ? C226 H226 . . .985(9) ? C401 C402 . . 1.390(15) ? C401 C405 . . 1.379(13) ? C401 H401 . . .967(10) ? C402 C403 . . 1.371(15) ? C402 H402 . . .969(10) ? C403 C404 . . 1.400(15) ? C403 H403 . . .963(10) ? C404 C405 . . 1.356(15) ? C404 H404 . . .984(9) ? C405 H405 . . .984(8) ? 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 . . . 60.33(6) ? Ru2 Ru1 C11 . . . 104.3(2) ? Ru2 Ru1 C12 . . . 103.4(3) ? Ru2 Ru1 C1 . . . 52.1(2) ? Ru2 Ru1 P1 . . . 152.24(5) ? Ru3 Ru1 C11 . . . 104.9(2) ? Ru3 Ru1 C12 . . . 157.1(3) ? Ru3 Ru1 C1 . . . 51.86(19) ? Ru3 Ru1 P1 . . . 94.10(7) ? C11 Ru1 C12 . . . 94.5(3) ? C11 Ru1 C1 . . . 151.5(3) ? C11 Ru1 P1 . . . 92.1(2) ? C12 Ru1 C1 . . . 105.8(3) ? C12 Ru1 P1 . . . 97.3(3) ? C1 Ru1 P1 . . . 104.6(2) ? Ru1 Ru2 Ru3 . . . 59.49(5) ? Ru1 Ru2 C21 . . . 85.0(3) ? Ru1 Ru2 C22 . . . 167.9(3) ? Ru1 Ru2 C23 . . . 92.3(3) ? Ru1 Ru2 C1 . . . 44.68(17) ? Ru1 Ru2 C2 . . . 77.85(19) ? Ru1 Ru2 H . . . 92(2) ? Ru3 Ru2 C21 . . . 108.7(3) ? Ru3 Ru2 C22 . . . 108.4(3) ? Ru3 Ru2 C23 . . . 143.4(2) ? Ru3 Ru2 C1 . . . 50.36(16) ? Ru3 Ru2 C2 . . . 52.73(18) ? Ru3 Ru2 H . . . 41(2) ? C21 Ru2 C22 . . . 101.4(4) ? C21 Ru2 C23 . . . 89.6(4) ? C21 Ru2 C1 . . . 129.7(4) ? C21 Ru2 C2 . . . 159.6(4) ? C21 Ru2 H . . . 91(2) ? C22 Ru2 C23 . . . 98.1(4) ? C22 Ru2 C1 . . . 127.7(3) ? C22 Ru2 C2 . . . 93.7(3) ? C22 Ru2 H . . . 77(2) ? C23 Ru2 C1 . . . 93.5(3) ? C23 Ru2 C2 . . . 101.9(3) ? C23 Ru2 H . . . 175(2) ? C1 Ru2 C2 . . . 34.1(2) ? C1 Ru2 H . . . 90(2) ? C2 Ru2 H . . . 79(2) ? Ru1 Ru3 Ru2 . . . 60.18(4) ? Ru1 Ru3 C31 . . . 84.6(2) ? Ru1 Ru3 C32 . . . 169.7(3) ? Ru1 Ru3 C1 . . . 45.06(17) ? Ru1 Ru3 C2 . . . 77.82(18) ? Ru1 Ru3 P2 . . . 91.47(6) ? Ru1 Ru3 H . . . 90(2) ? Ru2 Ru3 C31 . . . 107.2(2) ? Ru2 Ru3 C32 . . . 111.0(3) ? Ru2 Ru3 C1 . . . 51.09(17) ? Ru2 Ru3 C2 . . . 51.82(17) ? Ru2 Ru3 P2 . . . 145.12(5) ? Ru2 Ru3 H . . . 37(2) ? C31 Ru3 C32 . . . 103.9(4) ? C31 Ru3 C1 . . . 129.5(3) ? C31 Ru3 C2 . . . 157.6(3) ? C31 Ru3 P2 . . . 88.1(3) ? C31 Ru3 H . . . 90(2) ? C32 Ru3 C1 . . . 125.9(3) ? C32 Ru3 C2 . . . 92.5(3) ? C32 Ru3 P2 . . . 94.6(3) ? C32 Ru3 H . . . 84(2) ? C1 Ru3 C2 . . . 33.9(2) ? C1 Ru3 P2 . . . 94.87(18) ? C1 Ru3 H . . . 88(2) ? C2 Ru3 P2 . . . 105.80(18) ? C2 Ru3 H . . . 76(2) ? P2 Ru3 H . . . 178(2) ? C41 W4 C42 . . . 77.4(4) ? C41 W4 C43 . . . 76.8(4) ? C41 W4 C4 . . . 130.7(4) ? C41 W4 C401 . . . 122.6(4) ? C41 W4 C402 . . . 91.7(4) ? C41 W4 C403 . . . 90.7(4) ? C41 W4 C404 . . . 122.0(4) ? C41 W4 C405 . . . 147.1(4) ? C42 W4 C43 . . . 110.5(4) ? C42 W4 C4 . . . 75.4(3) ? C42 W4 C401 . . . 150.4(4) ? C42 W4 C402 . . . 138.1(4) ? C42 W4 C403 . . . 104.4(4) ? C42 W4 C404 . . . 94.3(4) ? C42 W4 C405 . . . 117.0(4) ? C43 W4 C4 . . . 75.5(4) ? C43 W4 C401 . . . 96.1(4) ? C43 W4 C402 . . . 105.9(4) ? C43 W4 C403 . . . 138.9(4) ? C43 W4 C404 . . . 152.3(4) ? C43 W4 C405 . . . 119.4(4) ? C4 W4 C401 . . . 100.2(3) ? C4 W4 C402 . . . 134.8(3) ? C4 W4 C403 . . . 135.6(3) ? C4 W4 C404 . . . 100.4(4) ? C4 W4 C405 . . . 82.2(3) ? C401 W4 C402 . . . 34.9(4) ? C401 W4 C403 . . . 58.1(4) ? C401 W4 C404 . . . 57.2(3) ? C401 W4 C405 . . . 34.4(3) ? C402 W4 C403 . . . 34.6(4) ? C402 W4 C404 . . . 57.4(4) ? C402 W4 C405 . . . 57.3(3) ? C403 W4 C404 . . . 35.3(4) ? C403 W4 C405 . . . 57.8(3) ? C404 W4 C405 . . . 33.9(4) ? Ru1 C11 O11 . . . 177.4(6) ? Ru1 C12 O12 . . . 176.6(7) ? Ru2 C21 O21 . . . 177.7(9) ? Ru2 C22 O22 . . . 178.1(9) ? Ru2 C23 O23 . . . 177.5(8) ? Ru3 C31 O31 . . . 177.9(7) ? Ru3 C32 O32 . . . 179.6(8) ? W4 C41 O41 . . . 179.0(9) ? W4 C42 O42 . . . 176.3(8) ? W4 C43 O43 . . . 178.7(10) ? Ru1 C1 Ru2 . . . 83.2(2) ? Ru1 C1 Ru3 . . . 83.1(2) ? Ru1 C1 C2 . . . 153.1(5) ? Ru2 C1 Ru3 . . . 78.6(2) ? Ru2 C1 C2 . . . 75.1(4) ? Ru3 C1 C2 . . . 77.3(4) ? Ru2 C2 Ru3 . . . 75.4(2) ? Ru2 C2 C1 . . . 70.8(4) ? Ru2 C2 C3 . . . 132.8(5) ? Ru3 C2 C1 . . . 68.8(4) ? Ru3 C2 C3 . . . 129.0(5) ? C1 C2 C3 . . . 149.7(7) ? C2 C3 C4 . . . 178.3(7) ? W4 C4 C3 . . . 174.7(6) ? Ru1 P1 C111 . . . 117.4(2) ? Ru1 P1 C121 . . . 116.8(2) ? Ru1 P1 C0 . . . 112.4(2) ? C111 P1 C121 . . . 101.2(3) ? C111 P1 C0 . . . 103.8(3) ? C121 P1 C0 . . . 103.3(3) ? P1 C111 C112 . . . 119.9(5) ? P1 C111 C116 . . . 120.9(5) ? C112 C111 C116 . . . 119.1(6) ? C111 C112 C113 . . . 121.0(7) ? C111 C112 H112 . . . 118.8(7) ? C113 C112 H112 . . . 120.2(8) ? C112 C113 C114 . . . 119.3(8) ? C112 C113 H113 . . . 120.3(9) ? C114 C113 H113 . . . 120.4(8) ? C113 C114 C115 . . . 120.7(8) ? C113 C114 H114 . . . 120.0(8) ? C115 C114 H114 . . . 119.3(9) ? C114 C115 C116 . . . 120.6(8) ? C114 C115 H115 . . . 119.4(8) ? C116 C115 H115 . . . 120.0(8) ? C111 C116 C115 . . . 119.3(7) ? C111 C116 H116 . . . 120.0(7) ? C115 C116 H116 . . . 120.7(8) ? P1 C121 C122 . . . 125.0(5) ? P1 C121 C126 . . . 117.6(6) ? C122 C121 C126 . . . 117.2(6) ? C121 C122 C123 . . . 119.6(7) ? C121 C122 H122 . . . 120.5(7) ? C123 C122 H122 . . . 119.9(8) ? C122 C123 C124 . . . 122.3(9) ? C122 C123 H123 . . . 119.3(8) ? C124 C123 H123 . . . 118.4(9) ? C123 C124 C125 . . . 119.9(8) ? C123 C124 H124 . . . 119.3(9) ? C125 C124 H124 . . . 120.8(8) ? C124 C125 C126 . . . 118.9(7) ? C124 C125 H125 . . . 119.8(7) ? C126 C125 H125 . . . 121.3(8) ? C121 C126 C125 . . . 122.1(7) ? C121 C126 H126 . . . 118.8(7) ? C125 C126 H126 . . . 119.2(7) ? P1 C0 P2 . . . 111.2(4) ? P1 C0 H0a . . . 109.7(5) ? P1 C0 H0b . . . 109.3(5) ? P2 C0 H0a . . . 110.3(5) ? P2 C0 H0b . . . 109.8(5) ? H0a C0 H0b . . . 106.3(6) ? Ru3 P2 C0 . . . 109.6(2) ? Ru3 P2 C211 . . . 122.2(2) ? Ru3 P2 C221 . . . 111.6(3) ? C0 P2 C211 . . . 103.4(3) ? C0 P2 C221 . . . 105.5(3) ? C211 P2 C221 . . . 103.2(3) ? P2 C211 C212 . . . 121.3(6) ? P2 C211 C216 . . . 121.6(6) ? C212 C211 C216 . . . 117.1(7) ? C211 C212 C213 . . . 122.4(9) ? C211 C212 H212 . . . 117.5(8) ? C213 C212 H212 . . . 120.1(9) ? C212 C213 C214 . . . 118.6(9) ? C212 C213 H213 . . . 120.8(11) ? C214 C213 H213 . . . 120.6(9) ? C213 C214 C215 . . . 120.3(10) ? C213 C214 H214 . . . 121.3(10) ? C215 C214 H214 . . . 118.4(12) ? C214 C215 C216 . . . 121.3(11) ? C214 C215 H215 . . . 120.6(11) ? C216 C215 H215 . . . 118.0(10) ? C211 C216 C215 . . . 120.2(9) ? C211 C216 H216 . . . 119.3(8) ? C215 C216 H216 . . . 120.5(10) ? P2 C221 C222 . . . 123.0(6) ? P2 C221 C226 . . . 118.8(6) ? C222 C221 C226 . . . 117.7(7) ? C221 C222 C223 . . . 121.0(8) ? C221 C222 H222 . . . 119.6(7) ? C223 C222 H222 . . . 119.4(8) ? C222 C223 C224 . . . 120.2(8) ? C222 C223 H223 . . . 119.1(9) ? C224 C223 H223 . . . 120.8(8) ? C223 C224 C225 . . . 119.6(8) ? C223 C224 H224 . . . 119.3(9) ? C225 C224 H224 . . . 121.1(10) ? C224 C225 C226 . . . 120.6(9) ? C224 C225 H225 . . . 119.3(10) ? C226 C225 H225 . . . 120.0(10) ? C221 C226 C225 . . . 120.8(8) ? C221 C226 H226 . . . 119.1(8) ? C225 C226 H226 . . . 120.1(9) ? W4 C401 C402 . . . 72.0(6) ? W4 C401 C405 . . . 73.1(6) ? W4 C401 H401 . . . 121.0(7) ? C402 C401 C405 . . . 107.1(9) ? C402 C401 H401 . . . 127.6(10) ? C405 C401 H401 . . . 125.3(10) ? W4 C402 C401 . . . 73.2(6) ? W4 C402 C403 . . . 72.2(6) ? W4 C402 H402 . . . 120.0(8) ? C401 C402 C403 . . . 108.9(9) ? C401 C402 H402 . . . 125.9(10) ? C403 C402 H402 . . . 125.2(10) ? W4 C403 C402 . . . 73.2(6) ? W4 C403 C404 . . . 72.8(6) ? W4 C403 H403 . . . 121.0(8) ? C402 C403 C404 . . . 106.6(9) ? C402 C403 H403 . . . 129.2(10) ? C404 C403 H403 . . . 124.1(10) ? W4 C404 C403 . . . 71.9(6) ? W4 C404 C405 . . . 74.0(6) ? W4 C404 H404 . . . 120.0(7) ? C403 C404 C405 . . . 108.8(9) ? C403 C404 H404 . . . 127.9(12) ? C405 C404 H404 . . . 123.3(11) ? W4 C405 C401 . . . 72.5(5) ? W4 C405 C404 . . . 72.1(5) ? W4 C405 H405 . . . 120.7(7) ? C401 C405 C404 . . . 108.6(8) ? C401 C405 H405 . . . 126.5(10) ? C404 C405 H405 . . . 124.9(10) ? Ru2 H Ru3 . . . 102(3) ? 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 3.048(6) . . ? Ru1 O12 3.018(6) . . ? Ru1 C21 3.243(10) . . ? Ru1 O21 3.960(8) . . ? Ru1 C23 3.457(10) . . ? Ru1 O23 4.186(8) . . ? Ru1 C31 3.193(8) . . ? Ru1 O31 3.929(7) . . ? Ru1 C2 3.211(8) . . ? Ru1 C111 3.531(7) . . ? Ru1 C121 3.510(7) . . ? Ru1 C0 3.440(7) . . ? Ru1 P2 3.670(3) . . ? Ru1 H 3.35(7) . . ? Ru1 H116 3.166(2) . . ? Ru2 O21 4.334(9) . '3 576' ? Ru2 O21 3.016(8) . . ? Ru2 O22 3.045(9) . . ? Ru2 O23 3.048(7) . . ? Ru2 C3 3.377(7) . . ? Ru3 O31 3.017(7) . . ? Ru3 O32 3.049(7) . . ? Ru3 C3 3.356(7) . . ? Ru3 P1 3.726(4) . . ? Ru3 C0 3.415(7) . . ? Ru3 C211 3.632(7) . . ? Ru3 C221 3.438(8) . . ? Ru3 H216 3.336(2) . . ? W4 O41 3.122(8) . . ? W4 O42 3.114(8) . . ? W4 O43 3.157(8) . . ? W4 C3 3.320(8) . . ? W4 H401 2.944(2) . . ? W4 H402 2.9201(18) . . ? W4 H403 2.9158(19) . . ? W4 H404 2.930(2) . . ? W4 H405 2.961(2) . . ? C11 C12 2.777(11) . . ? C11 O21 3.322(11) . . ? C11 O31 3.293(10) . . ? C11 P1 3.032(8) . . ? O11 C21 3.587(13) . . ? O11 O21 3.409(11) . . ? O11 C31 3.568(10) . . ? O11 O31 3.354(9) . . ? O11 P1 3.886(6) . . ? O11 C404 3.562(12) . '4 564' ? O11 H112 3.340(7) . 2 ? O11 H113 3.362(7) . 2 ? O11 H224 2.870(6) . '4 464' ? O11 H404 2.758(7) . '4 564' ? C12 O23 3.535(11) . . ? C12 P1 3.146(8) . . ? O12 O23 3.551(10) . . ? O12 O32 3.216(9) . '4 464' ? O12 C215 3.578(14) . '3 566' ? O12 C401 3.451(12) . '3 566' ? O12 H126 2.928(7) . . ? O12 H214 3.175(7) . '3 566' ? O12 H215 2.874(7) . '3 566' ? O12 H401 2.904(7) . '3 566' ? C21 C22 2.948(15) . . ? C21 C23 2.698(14) . . ? C21 O23 3.574(13) . . ? C21 H 2.59(7) . . ? O21 O22 4.024(12) . '3 576' ? O21 C23 3.575(13) . . ? O21 C23 3.265(12) . '3 576' ? O21 O23 3.092(10) . '3 576' ? O21 O23 4.273(12) . . ? O21 O41 4.366(14) . '2 556' ? O21 C123 3.515(13) . 2 ? O21 C124 3.283(12) . 2 ? O21 H123 3.141(9) . 2 ? O21 H124 2.704(8) . 2 ? C22 C23 2.893(13) . . ? C22 O43 3.588(13) . '2 556' ? C22 H 2.28(7) . . ? O22 O42 3.948(12) . . ? O22 O43 3.375(12) . '2 556' ? O22 C225 3.503(14) . '2 556' ? O22 C226 3.506(13) . '2 556' ? O22 H 3.15(7) . . ? O22 H123 2.784(9) . '4 465' ? O22 H225 2.885(9) . '2 556' ? O22 H226 2.883(9) . '2 556' ? O23 O43 4.065(12) . '4 464' ? O23 C114 3.466(11) . '3 566' ? O23 H114 2.813(8) . '3 566' ? O23 H124 3.039(8) . '4 465' ? O23 H214 3.201(7) . '3 566' ? C31 C32 2.961(12) . . ? C31 P2 2.934(8) . . ? C31 H 2.64(7) . . ? O31 O41 4.331(12) . '4 564' ? O31 O42 3.920(11) . '4 564' ? O31 P2 3.762(7) . . ? O31 C222 3.619(11) . . ? O31 C402 3.429(12) . '2 556' ? O31 C403 3.265(12) . '4 564' ? O31 H0a 3.086(7) . . ? O31 H222 3.043(7) . . ? O31 H402 2.463(6) . '2 556' ? O31 H403 2.453(7) . '4 564' ? C32 P2 3.120(9) . . ? C32 H 2.51(7) . . ? O32 O43 3.681(13) . . ? O32 P2 3.977(8) . . ? O32 C214 3.356(13) . '2 556' ? O32 C215 3.486(13) . '2 556' ? O32 C226 3.543(12) . . ? O32 C401 3.584(12) . '2 556' ? O32 H214 2.775(7) . '2 556' ? O32 H215 3.127(7) . '2 556' ? O32 H401 2.713(8) . '2 556' ? C41 C42 2.443(13) . . ? C41 O42 3.295(13) . . ? C41 C43 2.445(15) . . ? C41 O43 3.328(14) . . ? O41 C42 3.289(12) . . ? O41 O42 3.881(12) . . ? O41 C43 3.299(14) . . ? O41 O43 3.929(13) . . ? O41 C124 3.528(12) . '1 556' ? O41 C125 3.312(11) . '1 556' ? O41 C403 3.661(14) . '3 567' ? O41 H124 3.022(9) . '1 556' ? O41 H125 2.544(8) . '1 556' ? O41 H213 2.862(10) . '2 556' ? O41 H223 3.079(9) . '4 465' ? O41 H403 3.191(9) . '3 567' ? C42 C4 2.499(11) . . ? O42 C4 3.334(11) . . ? O42 C122 3.442(11) . '4 465' ? O42 C213 3.556(13) . '2 556' ? O42 H122 2.727(8) . '4 465' ? O42 H0a 3.026(8) . '4 465' ? O42 H213 3.181(8) . '2 556' ? O42 H222 2.930(9) . '4 465' ? C43 C4 2.520(12) . . ? O43 C4 3.324(11) . . ? C1 C3 2.615(10) . . ? C2 C4 2.580(10) . . ? C2 H 2.59(7) . . ? C2 H216 2.597(7) . . ? C3 H216 2.433(7) . . ? C4 C405 2.942(12) . . ? P1 C112 2.795(8) . . ? P1 C116 2.801(8) . . ? P1 C122 2.852(9) . . ? P1 C126 2.730(8) . . ? P1 P2 3.028(4) . . ? P1 H112 2.867(2) . . ? P1 H116 2.900(2) . . ? P1 H126 2.781(3) . . ? P1 H0a 2.342(2) . . ? P1 H0b 2.343(2) . . ? C111 C113 2.403(10) . . ? C111 C114 2.758(11) . . ? C111 C115 2.390(11) . . ? C111 C121 2.815(9) . . ? C111 C0 2.880(9) . . ? C111 H112 2.047(7) . . ? C111 H116 2.052(7) . . ? C112 C114 2.367(12) . . ? C112 C115 2.738(12) . . ? C112 C116 2.390(11) . . ? C112 H113 2.046(7) . . ? C113 C115 2.377(13) . . ? C113 C116 2.769(12) . . ? C113 H112 2.043(9) . . ? C113 H114 2.046(9) . . ? C114 C116 2.388(11) . . ? C114 H113 2.049(9) . . ? C114 H115 2.024(9) . . ? C115 H114 2.028(9) . . ? C115 H116 2.063(9) . . ? C116 H115 2.053(8) . . ? C121 C123 2.393(12) . . ? C121 C124 2.779(11) . . ? C121 C125 2.419(10) . . ? C121 C0 2.862(9) . . ? C121 H112 2.649(7) . . ? C121 H122 2.068(7) . . ? C121 H126 2.022(7) . . ? C122 C124 2.375(11) . . ? C122 C125 2.745(11) . . ? C122 C126 2.352(11) . . ? C122 H123 2.044(8) . . ? C123 C125 2.327(13) . . ? C123 C126 2.696(12) . . ? C123 H122 2.051(9) . . ? C123 H124 1.998(9) . . ? C124 C126 2.372(12) . . ? C124 H123 1.994(9) . . ? C124 H125 2.031(10) . . ? C125 H124 2.031(8) . . ? C125 H126 2.060(8) . . ? C126 H125 2.088(7) . . ? C0 C211 2.862(10) . . ? C0 C221 2.905(10) . . ? C0 H122 2.647(7) . . ? P2 C212 2.794(9) . . ? P2 C216 2.791(10) . . ? P2 C222 2.825(9) . . ? P2 C226 2.760(9) . . ? P2 H0a 2.352(3) . . ? P2 H0b 2.352(3) . . ? P2 H212 2.857(3) . . ? P2 H216 2.887(3) . . ? P2 H222 2.952(3) . . ? P2 H226 2.838(3) . . ? C211 C213 2.408(11) . . ? C211 C214 2.772(12) . . ? C211 C215 2.401(14) . . ? C211 C221 2.840(10) . . ? C211 H212 2.025(7) . . ? C211 H216 2.034(7) . . ? C212 C214 2.368(14) . . ? C212 C215 2.711(16) . . ? C212 C216 2.358(14) . . ? C212 H213 2.045(9) . . ? C213 C215 2.352(16) . . ? C213 C216 2.745(13) . . ? C213 H212 2.030(10) . . ? C213 H214 2.065(11) . . ? C214 C216 2.364(12) . . ? C214 H213 2.069(11) . . ? C214 H215 1.993(11) . . ? C215 H214 1.973(10) . . ? C215 H216 2.056(10) . . ? C216 H215 2.032(10) . . ? C221 C223 2.406(11) . . ? C221 C224 2.781(11) . . ? C221 C225 2.403(12) . . ? C221 H222 2.073(8) . . ? C221 H226 2.051(8) . . ? C222 C224 2.383(12) . . ? C222 C225 2.739(13) . . ? C222 C226 2.377(13) . . ? C222 H223 2.047(8) . . ? C223 C225 2.365(14) . . ? C223 C226 2.743(13) . . ? C223 H222 2.051(9) . . ? C223 H224 2.043(9) . . ? C224 C226 2.380(13) . . ? C224 H223 2.071(10) . . ? C224 H225 2.027(10) . . ? C225 H224 2.042(11) . . ? C225 H226 2.059(11) . . ? C226 H225 2.053(8) . . ? C401 C403 2.246(15) . . ? C401 C404 2.221(14) . . ? C401 H402 2.109(11) . . ? C401 H405 2.118(10) . . ? C402 C404 2.221(14) . . ? C402 C405 2.227(13) . . ? C402 H401 2.123(11) . . ? C402 H403 2.116(11) . . ? C403 C405 2.240(13) . . ? C403 H402 2.085(10) . . ? C403 H404 2.149(10) . . ? C404 H403 2.098(13) . . ? C404 H405 2.082(13) . . ? C405 H401 2.092(10) . . ? C405 H404 2.067(10) . . ? H112 H113 2.3550(15) . . ? H113 H114 2.3565(16) . . ? H114 H115 2.3178(13) . . ? H115 H116 2.3700(15) . . ? H122 H123 2.346(3) . . ? H122 H0a 2.262(3) . . ? H123 H124 2.2744(16) . . ? H124 H125 2.3404(17) . . ? H125 H126 2.387(3) . . ? H0a H0b 1.5513(11) . . ? H0a H222 2.2602(15) . . ? H0b H212 2.1849(15) . . ? H212 H213 2.3498(14) . . ? H213 H214 2.3910(17) . . ? H214 H215 2.2744(13) . . ? H215 H216 2.3371(14) . . ? H215 H401 2.348(2) . . ? H222 H223 2.3419(16) . . ? H223 H224 2.366(3) . . ? H224 H225 2.3431(13) . . ? H225 H226 2.3642(16) . . ? _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 2432 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 7 9 -5 -7 -9 5 -7 9 -5 7 -9 7 6 -9 -7 6 9 -7 -6 9 7 -6 -9 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min -25 _reflns_limit_l_max 25 _reflns_number_observed ? _reflns_d_resolution_high .711 _reflns_d_resolution_low 12.589 _diffrn_reflns_av_sigmaI/netI 0 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_reduction_process 'perpendicular monochr Lp' _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single 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 .064 _refine_ls_wR_factor_all .052 _refine_ls_goodness_of_fit_all 1.856 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end data_br525 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C21 H6 O12 Ru3 W1' _chemical_formula_moiety ? _chemical_formula_weight 937.34 _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 12.894(9) _cell_length_b 11.513(10) _cell_length_c 10.121(3) _cell_angle_alpha 101.31(5) _cell_angle_beta 108.93(4) _cell_angle_gamma 104.19(6) _cell_volume 1314.1(17) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 2.369 _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 21.5 _cell_measurement_theta_max 25.3 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 6.111 _exptl_crystal_description prism _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_size_rad ? _exptl_crystal_colour 'dark red' _diffrn_measurement_device_type ; CAD4 ; _diffrn_measurement_method '2\Q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min 0.21 _exptl_absorpt_correction_T_max 0.37 _diffrn_reflns_number 6010 _reflns_number_total 6010 _reflns_Friedel_coverage ? _reflns_number_gt 5047 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt 0.056 _refine_ls_wR_factor_ref 0.076 _refine_ls_goodness_of_fit_ref 2.13 _refine_ls_number_reflns 5047 _refine_ls_number_parameters 335 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref #<< use NfA code _refine_ls_shift/su_max .028 _refine_diff_density_min -1.25 _refine_diff_density_max 1.45 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 1180(186) _refine_ls_abs_structure_details none _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 42 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 24 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 12 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' W ? 0 2 -1.421 6.872 '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 .41245(8) 1.17666(9) .98972(11) .0479(4) Uani ? ? 1.00000 ? ? Ru2 .19031(8) 1.00636(9) .80501(11) .0466(4) Uani ? ? 1.00000 ? ? Ru3 .34088(9) 1.11725(9) .68534(11) .0472(4) Uani ? ? 1.00000 ? ? W4 .20530(4) .53978(4) .36858(5) .0420(2) Uani ? ? 1.00000 ? ? C11 .5737(12) 1.2556(13) 1.0436(15) .061(6) Uani ? ? 1.00000 ? ? O11 .6689(10) 1.3001(13) 1.0721(13) .097(6) Uani ? ? 1.00000 ? ? C12 .3838(13) 1.3324(15) 1.0421(17) .074(7) Uani ? ? 1.00000 ? ? O12 .3619(12) 1.4193(12) 1.0645(17) .118(8) Uani ? ? 1.00000 ? ? C13 .4212(12) 1.1397(15) 1.1684(16) .067(6) Uani ? ? 1.00000 ? ? O13 .4228(10) 1.1133(12) 1.2702(12) .088(6) Uani ? ? 1.00000 ? ? C21 .0561(12) .8915(14) .6409(16) .067(6) Uani ? ? 1.00000 ? ? O21 -.0216(11) .8260(14) .5422(16) .125(7) Uani ? ? 1.00000 ? ? C22 .1780(12) .9142(16) .9346(19) .077(7) Uani ? ? 1.00000 ? ? O22 .1700(13) .8571(14) 1.0193(15) .114(8) Uani ? ? 1.00000 ? ? C23 .1230(13) 1.1180(14) .8739(18) .074(7) Uani ? ? 1.00000 ? ? O23 .0817(13) 1.1851(15) .923(2) .142(9) Uani ? ? 1.00000 ? ? C31 .2562(12) 1.0462(14) .4773(15) .062(6) Uani ? ? 1.00000 ? ? O31 .2004(11) .9940(12) .3587(10) .099(6) Uani ? ? 1.00000 ? ? C32 .4883(13) 1.1356(14) .6752(18) .069(7) Uani ? ? 1.00000 ? ? O32 .5765(11) 1.1474(14) .6717(17) .108(8) Uani ? ? 1.00000 ? ? C33 .3585(14) 1.2893(14) .7072(15) .065(6) Uani ? ? 1.00000 ? ? O33 .3687(11) 1.3939(11) .7225(14) .095(6) Uani ? ? 1.00000 ? ? C41 .2349(12) .3753(13) .3526(14) .059(6) Uani ? ? 1.00000 ? ? O41 .2495(11) .2818(10) .3439(14) .099(6) Uani ? ? 1.00000 ? ? C42 .3808(12) .5951(12) .4462(17) .063(6) Uani ? ? 1.00000 ? ? O42 .4759(9) .6255(11) .4784(14) .088(6) Uani ? ? 1.00000 ? ? C43 .1596(12) .4873(16) .523(2) .074(7) Uani ? ? 1.00000 ? ? O43 .1337(11) .4646(13) .6150(14) .102(7) Uani ? ? 1.00000 ? ? C1 .3719(9) 1.0148(12) .8499(12) .045(4) Uani ? ? 1.00000 ? ? C2 .3100(10) .9279(11) .7225(12) .043(4) Uani ? ? 1.00000 ? ? C3 .2862(10) .8102(12) .6263(12) .044(4) Uani ? ? 1.00000 ? ? C4 .2623(10) .7101(11) .5378(12) .043(4) Uani ? ? 1.00000 ? ? C401 .1480(14) .6563(16) .2196(16) .075(7) Uani ? ? 1.00000 ? ? C402 .0565(13) .6047(16) .2504(15) .067(7) Uani ? ? 1.00000 ? ? C403 .0183(15) .482(2) .195(2) .092(9) Uani ? ? 1.00000 ? ? C404 .088(3) .448(2) .127(2) .129(12) Uani ? ? 1.00000 ? ? C405 .173(2) .565(4) .135(2) .138(16) Uani ? ? 1.00000 ? ? H401 .19528 .74719 .25661 .08200 Uiso ? ? 1.00000 ? ? H402 .02312 .65379 .30411 .08600 Uiso ? ? 1.00000 ? ? H403 -.04844 .42655 .19970 .09200 Uiso ? ? 1.00000 ? ? H404 .08914 .36583 .08311 .12900 Uiso ? ? 1.00000 ? ? H405 .22661 .58057 .09069 .22000 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 .0462(5) .0419(5) .0458(5) .0144(4) .0115(4) .0034(4) Ru2 .0420(5) .0377(5) .0537(6) .0135(4) .0170(4) .0029(4) Ru3 .0486(6) .0424(5) .0487(6) .0160(4) .0152(4) .0154(4) W4 .0426(3) .0381(3) .0401(3) .0140(2) .0128(2) .00577(19) C11 .053(8) .055(8) .057(8) .013(6) .010(6) .006(6) O11 .061(7) .112(10) .095(9) .001(7) .024(6) .025(7) C12 .063(9) .058(9) .076(10) .018(7) .010(8) -.002(8) O12 .120(11) .064(8) .164(13) .050(8) .049(10) .008(8) C13 .055(8) .074(10) .061(9) .020(7) .021(7) .002(8) O13 .094(8) .110(10) .054(6) .021(7) .029(6) .028(6) C21 .052(8) .062(9) .069(9) .016(7) .010(7) .012(7) O21 .075(8) .112(11) .112(10) .004(8) -.009(8) -.012(9) C22 .052(8) .075(11) .086(11) .017(7) .028(8) -.009(9) O22 .132(12) .123(12) .105(10) .026(9) .064(9) .063(9) C23 .060(9) .059(9) .087(11) .021(7) .023(8) -.000(8) O23 .111(11) .129(13) .185(16) .063(10) .069(11) -.006(12) C31 .068(9) .065(9) .053(8) .023(7) .022(7) .022(7) O31 .126(10) .101(9) .028(5) .018(7) .002(6) .008(5) C32 .066(9) .056(8) .092(11) .018(7) .035(8) .033(8) O32 .080(8) .124(11) .159(13) .038(8) .073(9) .077(10) C33 .089(10) .056(9) .050(7) .030(8) .019(7) .021(6) O33 .113(9) .055(7) .121(10) .036(7) .039(8) .034(7) C41 .065(8) .056(8) .047(7) .022(7) .007(6) .016(6) O41 .117(10) .048(6) .119(10) .035(6) .025(8) .021(6) C42 .053(8) .045(7) .095(11) .023(6) .033(8) .012(7) O42 .053(6) .095(9) .114(9) .031(6) .023(6) .029(7) C43 .050(8) .084(11) .092(11) .017(7) .036(8) .026(9) O43 .111(10) .119(11) .093(9) .024(8) .067(8) .037(8) C1 .039(6) .060(7) .040(6) .026(5) .010(5) .019(5) C2 .045(6) .050(7) .038(6) .019(5) .019(5) .012(5) C3 .046(6) .054(7) .036(5) .025(5) .013(5) .015(5) C4 .046(6) .049(7) .036(6) .020(5) .013(5) .015(5) C401 .077(10) .074(10) .047(8) .004(8) .003(7) .027(7) C402 .068(9) .085(11) .054(8) .041(9) .022(7) .021(8) C403 .067(10) .096(14) .070(11) .004(10) -.006(9) .018(10) C404 .20(3) .077(13) .058(11) .091(16) -.026(14) -.026(10) C405 .128(18) .31(4) .042(9) .15(2) .041(11) .085(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 . . 2.8068(19) ? Ru1 Ru3 . . 2.7981(18) ? Ru1 C11 . . 1.894(14) ? Ru1 C12 . . 1.927(18) ? Ru1 C13 . . 1.912(18) ? Ru1 C1 . . 1.939(12) ? Ru2 Ru3 . . 2.790(2) ? Ru2 C21 . . 1.911(11) ? Ru2 C22 . . 1.86(2) ? Ru2 C23 . . 1.865(19) ? Ru2 C1 . . 2.209(13) ? Ru2 C2 . . 2.262(14) ? Ru3 C31 . . 1.921(13) ? Ru3 C32 . . 1.899(19) ? Ru3 C33 . . 1.897(17) ? Ru3 C1 . . 2.213(14) ? Ru3 C2 . . 2.246(13) ? W4 C41 . . 2.009(17) ? W4 C42 . . 2.022(14) ? W4 C43 . . 1.99(2) ? W4 C4 . . 2.116(11) ? W4 C401 . . 2.275(18) ? W4 C402 . . 2.288(18) ? W4 C403 . . 2.314(16) ? W4 C404 . . 2.276(17) ? W4 C405 . . 2.35(2) ? C11 O11 . . 1.122(19) ? C12 O12 . . 1.11(2) ? C13 O13 . . 1.13(2) ? C21 O21 . . 1.120(16) ? C22 O22 . . 1.19(3) ? C23 O23 . . 1.16(3) ? C31 O31 . . 1.125(14) ? C32 O32 . . 1.12(2) ? C33 O33 . . 1.15(2) ? C41 O41 . . 1.13(2) ? C42 O42 . . 1.104(18) ? C43 O43 . . 1.14(3) ? C1 C2 . . 1.317(13) ? C2 C3 . . 1.401(17) ? C3 C4 . . 1.212(16) ? C401 C402 . . 1.35(3) ? C401 C405 . . 1.40(4) ? C401 H401 . . .996(15) ? C402 C403 . . 1.32(3) ? C402 H402 . . .98(2) ? C403 C404 . . 1.37(4) ? C403 H403 . . .96(2) ? C404 C405 . . 1.48(4) ? C404 H404 . . .97(3) ? C405 H405 . . .94(3) ? 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 . . . 59.70(5) ? Ru2 Ru1 C11 . . . 154.7(5) ? Ru2 Ru1 C12 . . . 103.2(4) ? Ru2 Ru1 C13 . . . 98.9(4) ? Ru2 Ru1 C1 . . . 51.6(4) ? Ru3 Ru1 C11 . . . 98.7(5) ? Ru3 Ru1 C12 . . . 103.2(5) ? Ru3 Ru1 C13 . . . 154.3(4) ? Ru3 Ru1 C1 . . . 51.9(4) ? C11 Ru1 C12 . . . 94.1(7) ? C11 Ru1 C13 . . . 97.8(6) ? C11 Ru1 C1 . . . 105.6(6) ? C12 Ru1 C13 . . . 95.1(8) ? C12 Ru1 C1 . . . 149.8(5) ? C13 Ru1 C1 . . . 104.5(6) ? Ru1 Ru2 Ru3 . . . 59.99(5) ? Ru1 Ru2 C21 . . . 164.8(6) ? Ru1 Ru2 C22 . . . 95.5(4) ? Ru1 Ru2 C23 . . . 90.1(4) ? Ru1 Ru2 C1 . . . 43.5(3) ? Ru1 Ru2 C2 . . . 76.6(2) ? Ru3 Ru2 C21 . . . 105.2(6) ? Ru3 Ru2 C22 . . . 143.3(5) ? Ru3 Ru2 C23 . . . 111.2(6) ? Ru3 Ru2 C1 . . . 50.9(4) ? Ru3 Ru2 C2 . . . 51.5(3) ? C21 Ru2 C22 . . . 95.7(7) ? C21 Ru2 C23 . . . 99.2(7) ? C21 Ru2 C1 . . . 125.8(6) ? C21 Ru2 C2 . . . 91.6(6) ? C22 Ru2 C23 . . . 94.4(9) ? C22 Ru2 C1 . . . 92.4(6) ? C22 Ru2 C2 . . . 99.0(7) ? C23 Ru2 C1 . . . 133.5(5) ? C23 Ru2 C2 . . . 161.9(6) ? C1 Ru2 C2 . . . 34.2(4) ? Ru1 Ru3 Ru2 . . . 60.30(5) ? Ru1 Ru3 C31 . . . 164.8(5) ? Ru1 Ru3 C32 . . . 98.3(5) ? Ru1 Ru3 C33 . . . 87.4(4) ? Ru1 Ru3 C1 . . . 43.6(3) ? Ru1 Ru3 C2 . . . 77.0(3) ? Ru2 Ru3 C31 . . . 104.5(5) ? Ru2 Ru3 C32 . . . 143.8(6) ? Ru2 Ru3 C33 . . . 112.8(6) ? Ru2 Ru3 C1 . . . 50.8(3) ? Ru2 Ru3 C2 . . . 52.0(4) ? C31 Ru3 C32 . . . 94.1(7) ? C31 Ru3 C33 . . . 100.6(6) ? C31 Ru3 C1 . . . 127.2(6) ? C31 Ru3 C2 . . . 92.9(6) ? C32 Ru3 C33 . . . 93.3(7) ? C32 Ru3 C1 . . . 93.2(7) ? C32 Ru3 C2 . . . 97.1(6) ? C33 Ru3 C1 . . . 131.0(5) ? C33 Ru3 C2 . . . 162.4(6) ? C1 Ru3 C2 . . . 34.4(4) ? C41 W4 C42 . . . 77.8(6) ? C41 W4 C43 . . . 78.7(7) ? C41 W4 C4 . . . 135.4(5) ? C41 W4 C401 . . . 138.4(6) ? C41 W4 C402 . . . 135.7(5) ? C41 W4 C403 . . . 102.5(7) ? C41 W4 C404 . . . 83.7(8) ? C41 W4 C405 . . . 103.9(11) ? C42 W4 C43 . . . 106.8(7) ? C42 W4 C4 . . . 75.2(6) ? C42 W4 C401 . . . 107.1(6) ? C42 W4 C402 . . . 139.5(6) ? C42 W4 C403 . . . 156.5(8) ? C42 W4 C404 . . . 123.6(10) ? C42 W4 C405 . . . 97.4(8) ? C43 W4 C4 . . . 76.1(6) ? C43 W4 C401 . . . 134.2(7) ? C43 W4 C402 . . . 102.6(7) ? C43 W4 C403 . . . 96.2(7) ? C43 W4 C404 . . . 121.0(8) ? C43 W4 C405 . . . 155.6(7) ? C4 W4 C401 . . . 83.8(5) ? C4 W4 C402 . . . 85.8(5) ? C4 W4 C403 . . . 116.1(7) ? C4 W4 C404 . . . 140.8(8) ? C4 W4 C405 . . . 114.2(10) ? C401 W4 C402 . . . 34.3(7) ? C401 W4 C403 . . . 56.9(7) ? C401 W4 C404 . . . 58.7(7) ? C401 W4 C405 . . . 35.1(11) ? C402 W4 C403 . . . 33.2(7) ? C402 W4 C404 . . . 57.2(9) ? C402 W4 C405 . . . 58.3(9) ? C403 W4 C404 . . . 34.8(11) ? C403 W4 C405 . . . 59.4(8) ? C404 W4 C405 . . . 37.4(10) ? Ru1 C11 O11 . . . 178.0(14) ? Ru1 C12 O12 . . . 175.8(13) ? Ru1 C13 O13 . . . 177.1(11) ? Ru2 C21 O21 . . . 178.0(17) ? Ru2 C22 O22 . . . 178.7(16) ? Ru2 C23 O23 . . . 176.3(18) ? Ru3 C31 O31 . . . 172.6(15) ? Ru3 C32 O32 . . . 178.8(15) ? Ru3 C33 O33 . . . 178.8(16) ? W4 C41 O41 . . . 178.6(15) ? W4 C42 O42 . . . 174.8(16) ? W4 C43 O43 . . . 175.9(16) ? Ru1 C1 Ru2 . . . 84.9(5) ? Ru1 C1 Ru3 . . . 84.5(5) ? Ru1 C1 C2 . . . 153.2(11) ? Ru2 C1 Ru3 . . . 78.2(4) ? Ru2 C1 C2 . . . 75.1(8) ? Ru3 C1 C2 . . . 74.2(8) ? Ru2 C2 Ru3 . . . 76.5(4) ? Ru2 C2 C1 . . . 70.7(8) ? Ru2 C2 C3 . . . 129.5(8) ? Ru3 C2 C1 . . . 71.4(8) ? Ru3 C2 C3 . . . 129.7(10) ? C1 C2 C3 . . . 150.1(13) ? C2 C3 C4 . . . 176.8(13) ? W4 C4 C3 . . . 173.8(11) ? W4 C401 C402 . . . 73.4(11) ? W4 C401 C405 . . . 75.4(15) ? W4 C401 H401 . . . 115.5(10) ? C402 C401 C405 . . . 111.1(18) ? C402 C401 H401 . . . 125.2(19) ? C405 C401 H401 . . . 124(2) ? W4 C402 C401 . . . 72.3(11) ? W4 C402 C403 . . . 74.5(12) ? W4 C402 H402 . . . 121.5(11) ? C401 C402 C403 . . . 110.6(18) ? C401 C402 H402 . . . 123.4(17) ? C403 C402 H402 . . . 126.0(18) ? W4 C403 C402 . . . 72.3(9) ? W4 C403 C404 . . . 71.1(11) ? W4 C403 H403 . . . 123.7(16) ? C402 C403 C404 . . . 108.7(18) ? C402 C403 H403 . . . 124(2) ? C404 C403 H403 . . . 127(2) ? W4 C404 C403 . . . 74.1(10) ? W4 C404 C405 . . . 74.1(10) ? W4 C404 H404 . . . 116.0(19) ? C403 C404 C405 . . . 108(2) ? C403 C404 H404 . . . 131(3) ? C405 C404 H404 . . . 121(3) ? W4 C405 C401 . . . 69.5(11) ? W4 C405 C404 . . . 68.6(13) ? W4 C405 H405 . . . 129(2) ? C401 C405 C404 . . . 101(2) ? C401 C405 H405 . . . 125(4) ? C404 C405 H405 . . . 133(3) ? 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 3.016(12) . . ? Ru1 O12 3.030(16) . . ? Ru1 O13 3.037(13) . . ? Ru1 C23 3.373(16) . . ? Ru1 C33 3.309(16) . . ? Ru1 C2 3.170(11) . . ? Ru2 O21 3.031(11) . . ? Ru2 O22 3.055(18) . . ? Ru2 O23 3.03(2) . . ? Ru2 C3 3.334(14) . . ? Ru3 O31 3.039(8) . . ? Ru3 O32 3.023(16) . . ? Ru3 O33 3.049(13) . . ? Ru3 C3 3.320(13) . . ? W4 O41 3.137(14) . . ? W4 O42 3.123(11) . . ? W4 O43 3.126(16) . . ? W4 C3 3.323(11) . . ? W4 H401 2.850(2) . . ? W4 H402 2.9189(17) . . ? W4 H403 2.955(2) . . ? W4 H404 2.8379(11) . . ? W4 H405 3.0270(10) . . ? C11 C12 2.80(3) . . ? C11 C13 2.87(2) . . ? C12 C13 2.83(3) . . ? C21 C22 2.80(2) . . ? C21 C23 2.88(2) . . ? C22 C23 2.74(3) . . ? C22 C1 2.95(2) . . ? O23 H404 2.332(18) . '1 566' ? C31 C32 2.797(19) . . ? C31 C33 2.937(18) . . ? C32 C33 2.76(3) . . ? C32 C1 3.00(2) . . ? O32 H401 2.679(13) . '2 676' ? C41 C42 2.531(18) . . ? C41 C43 2.54(3) . . ? C41 C404 2.87(3) . . ? C42 C4 2.53(2) . . ? C43 C4 2.53(2) . . ? O43 H402 2.603(16) . '2 566' ? C1 C3 2.626(15) . . ? C2 C4 2.612(16) . . ? C4 C401 2.936(18) . . ? C401 C403 2.19(3) . . ? C401 C404 2.23(3) . . ? C401 H402 2.05(2) . . ? C401 H405 2.08(2) . . ? C402 C404 2.19(3) . . ? C402 C405 2.26(4) . . ? C402 H401 2.084(17) . . ? C402 H403 2.019(16) . . ? C403 C405 2.31(4) . . ? C403 H402 2.05(2) . . ? C403 H404 2.14(2) . . ? C404 H403 2.09(3) . . ? C404 H405 2.23(3) . . ? C405 H401 2.12(4) . . ? C405 H404 2.15(4) . . ? _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_000 868 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 6 5 -5 -6 -5 13 0 0 -13 0 0 0 11 0 0 -11 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 -14 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _reflns_number_observed 6010 _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min 1 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type F _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .062 _refine_ls_wR_factor_all .077 _refine_ls_goodness_of_fit_all 2.10 _refine_ls_shift/su_mean .0028 #========================================================================== # 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_br550 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C26 H6 Fe O17 Ru4 W1' _chemical_formula_moiety ? _chemical_formula_weight 1234.31 _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 8.502(2) _cell_length_b 23.997(3) _cell_length_c 16.551(3) _cell_angle_alpha 90.00000 _cell_angle_beta 90.778(2) _cell_angle_gamma 90.00000 _cell_volume 3376.5(11) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.426 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6361 _cell_measurement_theta_min 1 _cell_measurement_theta_max 29.5 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 5.63 _exptl_crystal_description plate _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _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 0.627 _exptl_absorpt_correction_T_max 0.862 _diffrn_reflns_number 35896 _reflns_number_total 8561 _reflns_Friedel_coverage ? _reflns_number_gt 6935 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.01 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .025 _refine_ls_wR_factor_ref .031 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_number_reflns 6935 _refine_ls_number_parameters 469 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max .043 _refine_diff_density_min -.705 _refine_diff_density_max 1.23 _refine_ls_extinction_method none _refine_ls_extinction_coef .00000 _refine_ls_abs_structure_details none _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 ? 0 104 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 68 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 20 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 16 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' W ? 0 4 -1.421 6.872 'Int Tables Vol IV Tables 2.2B and 2.3.1' Fe ? 0 4 .301 .845 '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 .77219(4) .075600(10) .60892(2) .0490(2) Uani ? ? .740(3) ? ? Fe1 .77219(4) .075600(10) .60892(2) .0490(2) Uani ? ? .260(3) ? ? Ru2 .89676(4) .158790(10) .71145(2) .04149(16) Uani ? ? 1.00000 ? ? Ru3 .96102(3) .161370(10) .54678(2) .04034(15) Uani ? ? 1.00000 ? ? W4 .74494(2) .397930(10) .608830(10) .04696(10) Uani ? ? 1.00000 ? ? Ru5 .59873(4) .30815(2) .51694(2) .0385(2) Uani ? ? .407(3) ? ? Fe5 .59873(4) .30815(2) .51694(2) .0385(2) Uani ? ? .593(3) ? ? Ru6 .54012(4) .307100(10) .67184(2) .04112(18) Uani ? ? .872(3) ? ? Fe6 .54012(4) .307100(10) .67184(2) .04112(18) Uani ? ? .128(3) ? ? C11 .9214(6) .0178(2) .6223(3) .077(3) Uani ? ? 1.00000 ? ? O11 1.0148(5) -.01543(17) .6311(3) .124(4) Uani ? ? 1.00000 ? ? C12 .6849(6) .04984(18) .5108(3) .070(3) Uani ? ? 1.00000 ? ? O12 .6286(5) .03642(16) .4521(2) .100(3) Uani ? ? 1.00000 ? ? C13 .6182(6) .04516(18) .6748(3) .071(3) Uani ? ? 1.00000 ? ? O13 .5185(5) .02959(17) .7146(3) .107(3) Uani ? ? 1.00000 ? ? C21 1.0244(6) .10447(17) .7669(3) .067(3) Uani ? ? 1.00000 ? ? O21 1.1062(5) .07421(16) .7987(3) .105(3) Uani ? ? 1.00000 ? ? C22 .7287(6) .15187(19) .7866(3) .063(3) Uani ? ? 1.00000 ? ? O22 .6280(5) .14698(18) .8299(2) .099(3) Uani ? ? 1.00000 ? ? C23 .9851(5) .22658(17) .7560(3) .056(2) Uani ? ? 1.00000 ? ? O23 1.0331(5) .26742(15) .7795(2) .092(3) Uani ? ? 1.00000 ? ? C31 1.1258(6) .11009(18) .5177(3) .065(3) Uani ? ? 1.00000 ? ? O31 1.2254(5) .08158(15) .5022(3) .106(3) Uani ? ? 1.00000 ? ? C32 .8632(5) .15717(18) .4427(3) .058(2) Uani ? ? 1.00000 ? ? O32 .8005(5) .15484(18) .3817(2) .092(3) Uani ? ? 1.00000 ? ? C33 1.0690(5) .23121(16) .5280(2) .049(2) Uani ? ? 1.00000 ? ? O33 1.1207(4) .27355(13) .5187(2) .075(2) Uani ? ? 1.00000 ? ? C41 .5355(6) .43328(18) .6226(3) .074(3) Uani ? ? 1.00000 ? ? O41 .4211(5) .45921(16) .6271(3) .106(3) Uani ? ? 1.00000 ? ? C42 .7775(7) .40418(18) .7279(3) .077(3) Uani ? ? 1.00000 ? ? O42 .8033(7) .40959(16) .7952(3) .118(3) Uani ? ? 1.00000 ? ? C51 .4546(6) .35957(18) .4836(3) .062(3) Uani ? ? 1.00000 ? ? O51 .3632(5) .39140(15) .4610(2) .093(3) Uani ? ? 1.00000 ? ? C52 .7293(5) .30731(18) .4295(3) .055(2) Uani ? ? 1.00000 ? ? O52 .8080(4) .30459(17) .3741(2) .090(3) Uani ? ? 1.00000 ? ? C53 .4900(5) .24484(19) .4892(2) .055(2) Uani ? ? 1.00000 ? ? O53 .4301(4) .20386(15) .4720(2) .081(2) Uani ? ? 1.00000 ? ? C61 .3485(6) .3460(2) .6875(3) .075(3) Uani ? ? 1.00000 ? ? O61 .2306(5) .36686(18) .6965(3) .113(3) Uani ? ? 1.00000 ? ? C62 .6088(5) .30053(18) .7823(3) .056(2) Uani ? ? 1.00000 ? ? O62 .6492(5) .29361(17) .84642(19) .091(3) Uani ? ? 1.00000 ? ? C63 .4331(5) .23887(19) .6708(3) .056(2) Uani ? ? 1.00000 ? ? O63 .3731(4) .19666(15) .6709(2) .089(3) Uani ? ? 1.00000 ? ? C1 .7340(4) .15352(15) .6076(2) .042(2) Uani ? ? 1.00000 ? ? C2 .7757(4) .20676(13) .61313(18) .0355(17) Uani ? ? 1.00000 ? ? C3 .7266(4) .26277(13) .60641(18) .0347(17) Uani ? ? 1.00000 ? ? C4 .7673(4) .31539(14) .61241(19) .0382(17) Uani ? ? 1.00000 ? ? C401 .8577(10) .4289(3) .4884(4) .098(5) Uani ? ? 1.00000 ? ? C402 .7818(8) .4735(3) .5228(4) .092(4) Uani ? ? 1.00000 ? ? C403 .8557(7) .48546(19) .5958(4) .080(4) Uani ? ? 1.00000 ? ? C404 .9762(6) .4476(2) .6084(4) .078(3) Uani ? ? 1.00000 ? ? C405 .9772(8) .4114(2) .5415(5) .094(5) Uani ? ? 1.00000 ? ? c0 .89092 .44906 .55167 .04369 Uiso ? ? 1.00000 ? ? H0 1.052(4) .1592(15) .646(2) .059(11) Uiso ? ? 1.00000 ? ? H401 .830(5) .4112(17) .448(3) .050(12) Uiso ? ? 1.00000 ? ? H402 .694(9) .494(3) .489(5) .18(3) Uiso ? ? 1.00000 ? ? H403 .823(6) .510(2) .638(3) .078(15) Uiso ? ? 1.00000 ? ? H404 1.050(7) .451(2) .656(3) .11(2) Uiso ? ? 1.00000 ? ? H405 1.050(6) .388(2) .541(3) .074(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 .0530(3) .03252(19) .0616(3) -.00308(14) .00355(17) -.00078(14) Fe1 .0530(3) .03252(19) .0616(3) -.00308(14) .00355(17) -.00078(14) Ru2 .04593(17) .03892(15) .03958(15) .00452(12) -.00107(12) .00462(11) Ru3 .04154(16) .03763(14) .04198(16) .00014(11) .00582(12) -.00347(11) W4 .05444(11) .03322(8) .05293(10) .00276(6) -.00948(7) .00238(6) Ru5 .0385(2) .0434(2) .0335(2) .00214(15) -.00208(15) .00443(14) Fe5 .0385(2) .0434(2) .0335(2) .00214(15) -.00208(15) .00443(14) Ru6 .03963(19) .04918(19) .03461(17) .00975(13) .00244(12) .00259(12) Fe6 .03963(19) .04918(19) .03461(17) .00975(13) .00244(12) .00259(12) C11 .075(3) .054(3) .104(4) -.000(2) .001(3) -.007(2) O11 .101(3) .086(3) .186(5) .036(3) -.009(3) -.014(3) C12 .069(3) .050(2) .093(4) -.009(2) .009(3) -.005(2) O12 .111(3) .098(3) .089(3) -.028(2) -.016(2) -.020(2) C13 .082(3) .050(2) .082(3) -.004(2) .006(3) .009(2) O13 .108(3) .094(3) .121(3) -.017(2) .037(3) .027(2) C21 .077(3) .056(3) .066(3) .013(2) -.011(2) .010(2) O21 .125(4) .087(3) .102(3) .044(2) -.028(2) .025(2) C22 .070(3) .070(3) .050(2) .012(2) .002(2) .014(2) O22 .083(3) .136(3) .079(2) .021(2) .037(2) .028(2) C23 .063(3) .053(2) .053(2) .001(2) -.009(2) -.0007(18) O23 .115(3) .073(2) .087(3) -.020(2) -.017(2) -.0160(19) C31 .064(3) .054(2) .079(3) .004(2) .018(2) -.012(2) O31 .089(3) .078(2) .151(4) .030(2) .036(3) -.020(2) C32 .063(3) .067(3) .045(2) -.015(2) .007(2) -.0031(19) O32 .099(3) .126(3) .052(2) -.023(2) -.005(2) -.006(2) C33 .042(2) .050(2) .054(2) .0032(16) .0077(17) -.0035(17) O33 .065(2) .0537(18) .107(3) -.0142(15) .0135(18) -.0009(17) C41 .085(3) .046(2) .090(3) .016(2) -.008(3) -.006(2) O41 .094(3) .073(2) .152(4) .041(2) -.002(3) -.004(2) C42 .110(4) .053(3) .068(3) -.006(3) -.020(3) -.004(2) O42 .189(5) .097(3) .068(3) -.034(3) -.027(3) -.011(2) C51 .072(3) .060(3) .053(2) .004(2) -.001(2) .000(2) O51 .096(3) .090(3) .091(3) .042(2) -.022(2) .005(2) C52 .049(2) .067(3) .050(2) -.0066(19) .000(2) .0047(19) O52 .075(2) .129(3) .066(2) -.016(2) .024(2) -.004(2) C53 .051(2) .064(3) .048(2) .006(2) .0003(18) .0060(19) O53 .077(2) .079(2) .087(2) -.0208(18) -.0061(19) -.0127(18) C61 .071(3) .081(3) .073(3) .028(3) .011(3) .021(2) O61 .076(3) .130(3) .134(4) .056(3) .028(2) .045(3) C62 .054(2) .069(3) .044(2) .013(2) .0063(18) -.0017(18) O62 .096(3) .135(3) .0420(18) .022(2) -.0058(18) .0087(19) C63 .045(2) .070(3) .051(2) .001(2) .0045(18) .0070(19) O63 .072(2) .086(3) .108(3) -.028(2) .007(2) .009(2) C1 .0367(19) .048(2) .043(2) -.0004(14) .0027(15) .0007(15) C2 .0372(18) .0366(16) .0328(16) .0001(13) .0018(14) .0012(12) C3 .0332(18) .0393(17) .0316(16) .0022(13) .0015(13) -.0003(12) C4 .0351(18) .0437(18) .0356(17) .0043(14) -.0021(14) .0008(13) C401 .142(7) .087(4) .064(4) -.061(5) .005(4) .008(3) C402 .095(4) .070(4) .110(5) -.016(3) -.020(4) .043(3) C403 .097(4) .041(2) .103(4) -.009(2) -.013(3) .005(3) C404 .069(3) .063(3) .102(4) -.010(2) -.018(3) .014(3) C405 .081(4) .049(3) .155(7) .002(3) .045(4) .024(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 W1 Ru2 . . 2.9066(5) ? W1 Fe2 . . 2.9066(5) ? W1 Ru3 . . 2.9867(5) ? W1 Fe3 . . 2.9867(5) ? W1 C1 . . 1.991(3) ? W1 C11 . . 1.988(5) ? W1 C12 . . 1.992(5) ? W1 C01 . . 2.303(7) ? W1 C02 . . 2.299(5) ? W1 C03 . . 2.313(5) ? W1 C04 . . 2.329(6) ? W1 C05 . . 2.344(7) ? Ru2 Ru3 . . 2.6185(6) ? Ru2 Fe3 . . 2.6185(6) ? Ru2 C1 . . 2.126(3) ? Ru2 C2 . . 2.126(3) ? Ru2 C21 . . 1.819(5) ? Ru2 C22 . . 1.836(4) ? Ru2 C23 . . 1.833(4) ? Fe2 Ru3 . . 2.6185(6) ? Fe2 Fe3 . . 2.6185(6) ? Fe2 C1 . . 2.126(3) ? Fe2 C2 . . 2.126(3) ? Fe2 C21 . . 1.819(5) ? Fe2 C22 . . 1.836(4) ? Fe2 C23 . . 1.833(4) ? Ru3 C1 . . 2.188(3) ? Ru3 C2 . . 2.206(3) ? Ru3 C31 . . 1.898(5) ? Ru3 C32 . . 1.918(4) ? Ru3 C33 . . 1.873(4) ? Fe3 C1 . . 2.188(3) ? Fe3 C2 . . 2.206(3) ? Fe3 C31 . . 1.898(5) ? Fe3 C32 . . 1.918(4) ? Fe3 C33 . . 1.873(4) ? Ru4 Ru5 . . 2.7877(6) ? Ru4 Ru6 . . 2.8135(5) ? Ru4 Fe6 . . 2.8135(5) ? Ru4 C3 . . 2.219(3) ? Ru4 C4 . . 2.197(3) ? Ru4 C41 . . 1.931(5) ? Ru4 C42 . . 1.906(4) ? Ru4 C43 . . 1.938(4) ? Ru4 H0 . . 1.81(4) ? Ru5 Ru6 . . 2.8173(5) ? Ru5 Fe6 . . 2.8173(5) ? Ru5 C3 . . 2.234(3) ? Ru5 C4 . . 2.196(3) ? Ru5 C51 . . 1.921(5) ? Ru5 C52 . . 1.914(5) ? Ru5 C53 . . 1.934(4) ? Ru5 H0 . . 1.72(4) ? Ru6 C4 . . 1.898(4) ? Ru6 C61 . . 1.891(5) ? Ru6 C62 . . 1.881(5) ? Ru6 C63 . . 1.865(5) ? Fe6 C4 . . 1.898(4) ? Fe6 C61 . . 1.891(5) ? Fe6 C62 . . 1.881(5) ? Fe6 C63 . . 1.865(5) ? C1 C2 . . 1.312(5) ? C2 C3 . . 1.411(4) ? C3 C4 . . 1.329(5) ? C11 O11 . . 1.158(6) ? C12 O12 . . 1.140(7) ? C21 O21 . . 1.149(6) ? C22 O22 . . 1.145(6) ? C23 O23 . . 1.142(6) ? C31 O31 . . 1.133(7) ? C32 O32 . . 1.124(5) ? C33 O33 . . 1.134(6) ? C41 O41 . . 1.121(6) ? C42 O42 . . 1.136(5) ? C43 O43 . . 1.119(5) ? C51 O51 . . 1.131(6) ? C52 O52 . . 1.129(6) ? C53 O53 . . 1.129(6) ? C61 O61 . . 1.133(7) ? C62 O62 . . 1.124(7) ? C63 O63 . . 1.143(7) ? C01 C02 . . 1.408(9) ? C01 C05 . . 1.399(10) ? C01 H01 . . .83(5) ? C02 C03 . . 1.382(8) ? C02 H02 . . 1.01(6) ? C03 C04 . . 1.385(9) ? C03 H03 . . .96(5) ? C04 C05 . . 1.376(10) ? C04 H04 . . 1.06(8) ? C05 H05 . . .82(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 W1 Fe2 . . . .00000 ? Ru2 W1 Ru3 . . . 52.739(14) ? Ru2 W1 Fe3 . . . 52.739(14) ? Ru2 W1 C1 . . . 47.01(9) ? Ru2 W1 C11 . . . 89.94(14) ? Ru2 W1 C12 . . . 128.78(14) ? Ru2 W1 C01 . . . 102.37(17) ? Ru2 W1 C02 . . . 137.94(15) ? Ru2 W1 C03 . . . 142.76(16) ? Ru2 W1 C04 . . . 108.48(16) ? Ru2 W1 C05 . . . 88.12(18) ? Fe2 W1 Ru3 . . . 52.739(14) ? Fe2 W1 Fe3 . . . 52.739(14) ? Fe2 W1 C1 . . . 47.01(9) ? Fe2 W1 C11 . . . 89.94(14) ? Fe2 W1 C12 . . . 128.78(14) ? Fe2 W1 C01 . . . 102.37(17) ? Fe2 W1 C02 . . . 137.94(15) ? Fe2 W1 C03 . . . 142.76(16) ? Fe2 W1 C04 . . . 108.48(16) ? Fe2 W1 C05 . . . 88.12(18) ? Ru3 W1 Fe3 . . . .00000 ? Ru3 W1 C1 . . . 47.10(9) ? Ru3 W1 C11 . . . 75.17(13) ? Ru3 W1 C12 . . . 77.50(15) ? Ru3 W1 C01 . . . 141.16(14) ? Ru3 W1 C02 . . . 151.90(15) ? Ru3 W1 C03 . . . 159.26(15) ? Ru3 W1 C04 . . . 149.93(16) ? Ru3 W1 C05 . . . 140.84(18) ? Fe3 W1 C1 . . . 47.10(9) ? Fe3 W1 C11 . . . 75.17(13) ? Fe3 W1 C12 . . . 77.50(15) ? Fe3 W1 C01 . . . 141.16(14) ? Fe3 W1 C02 . . . 151.90(15) ? Fe3 W1 C03 . . . 159.26(15) ? Fe3 W1 C04 . . . 149.93(16) ? Fe3 W1 C05 . . . 140.84(18) ? C1 W1 C11 . . . 120.43(16) ? C1 W1 C12 . . . 91.93(15) ? C1 W1 C01 . . . 94.11(17) ? C1 W1 C02 . . . 115.78(16) ? C1 W1 C03 . . . 150.17(17) ? C1 W1 C04 . . . 141.17(19) ? C1 W1 C05 . . . 107.5(2) ? C11 W1 C12 . . . 88.1(2) ? C11 W1 C01 . . . 140.4(2) ? C11 W1 C02 . . . 123.09(18) ? C11 W1 C03 . . . 89.4(2) ? C11 W1 C04 . . . 82.3(2) ? C11 W1 C05 . . . 109.8(2) ? C12 W1 C01 . . . 111.1(3) ? C12 W1 C02 . . . 81.7(2) ? C12 W1 C03 . . . 88.4(2) ? C12 W1 C04 . . . 121.9(2) ? C12 W1 C05 . . . 139.8(2) ? C01 W1 C02 . . . 35.6(2) ? C01 W1 C03 . . . 58.3(2) ? C01 W1 C04 . . . 58.1(2) ? C01 W1 C05 . . . 35.0(3) ? C02 W1 C03 . . . 34.9(2) ? C02 W1 C04 . . . 58.2(2) ? C02 W1 C05 . . . 58.2(2) ? C03 W1 C04 . . . 34.7(2) ? C03 W1 C05 . . . 57.4(2) ? C04 W1 C05 . . . 34.2(2) ? W1 Ru2 Ru3 . . . 65.201(13) ? W1 Ru2 Fe3 . . . 65.201(13) ? W1 Ru2 C1 . . . 43.23(9) ? W1 Ru2 C2 . . . 78.70(9) ? W1 Ru2 C21 . . . 86.41(14) ? W1 Ru2 C22 . . . 99.31(13) ? W1 Ru2 C23 . . . 162.88(13) ? Ru3 Ru2 Fe3 . . . .00(12) ? Ru3 Ru2 C1 . . . 53.73(9) ? Ru3 Ru2 C2 . . . 54.21(8) ? Ru3 Ru2 C21 . . . 99.60(14) ? Ru3 Ru2 C22 . . . 153.75(13) ? Ru3 Ru2 C23 . . . 97.76(13) ? Fe3 Ru2 C1 . . . 53.73(9) ? Fe3 Ru2 C2 . . . 54.21(8) ? Fe3 Ru2 C21 . . . 99.60(14) ? Fe3 Ru2 C22 . . . 153.75(13) ? Fe3 Ru2 C23 . . . 97.76(13) ? C1 Ru2 C2 . . . 35.96(13) ? C1 Ru2 C21 . . . 127.91(16) ? C1 Ru2 C22 . . . 100.27(16) ? C1 Ru2 C23 . . . 125.88(16) ? C2 Ru2 C21 . . . 153.47(16) ? C2 Ru2 C22 . . . 103.57(16) ? C2 Ru2 C23 . . . 90.06(16) ? C21 Ru2 C22 . . . 100.4(2) ? C21 Ru2 C23 . . . 98.7(2) ? C22 Ru2 C23 . . . 95.84(18) ? W1 Fe2 Ru3 . . . 65.201(13) ? W1 Fe2 Fe3 . . . 65.201(13) ? W1 Fe2 C1 . . . 43.23(9) ? W1 Fe2 C2 . . . 78.70(9) ? W1 Fe2 C21 . . . 86.41(14) ? W1 Fe2 C22 . . . 99.31(13) ? W1 Fe2 C23 . . . 162.88(13) ? Ru3 Fe2 Fe3 . . . .00(12) ? Ru3 Fe2 C1 . . . 53.73(9) ? Ru3 Fe2 C2 . . . 54.21(8) ? Ru3 Fe2 C21 . . . 99.60(14) ? Ru3 Fe2 C22 . . . 153.75(13) ? Ru3 Fe2 C23 . . . 97.76(13) ? Fe3 Fe2 C1 . . . 53.73(9) ? Fe3 Fe2 C2 . . . 54.21(8) ? Fe3 Fe2 C21 . . . 99.60(14) ? Fe3 Fe2 C22 . . . 153.75(13) ? Fe3 Fe2 C23 . . . 97.76(13) ? C1 Fe2 C2 . . . 35.96(13) ? C1 Fe2 C21 . . . 127.91(16) ? C1 Fe2 C22 . . . 100.27(16) ? C1 Fe2 C23 . . . 125.88(16) ? C2 Fe2 C21 . . . 153.47(16) ? C2 Fe2 C22 . . . 103.57(16) ? C2 Fe2 C23 . . . 90.06(16) ? C21 Fe2 C22 . . . 100.4(2) ? C21 Fe2 C23 . . . 98.7(2) ? C22 Fe2 C23 . . . 95.84(18) ? W1 Ru3 Ru2 . . . 62.060(12) ? W1 Ru3 Fe2 . . . 62.060(12) ? W1 Ru3 C1 . . . 41.79(9) ? W1 Ru3 C2 . . . 75.76(8) ? W1 Ru3 C31 . . . 101.21(15) ? W1 Ru3 C32 . . . 102.78(13) ? W1 Ru3 C33 . . . 156.95(13) ? Ru2 Ru3 Fe2 . . . .00000 ? Ru2 Ru3 C1 . . . 51.55(8) ? Ru2 Ru3 C2 . . . 51.42(8) ? Ru2 Ru3 C31 . . . 107.71(15) ? Ru2 Ru3 C32 . . . 150.98(13) ? Ru2 Ru3 C33 . . . 95.64(13) ? Fe2 Ru3 C1 . . . 51.55(8) ? Fe2 Ru3 C2 . . . 51.42(8) ? Fe2 Ru3 C31 . . . 107.71(15) ? Fe2 Ru3 C32 . . . 150.98(13) ? Fe2 Ru3 C33 . . . 95.64(13) ? C1 Ru3 C2 . . . 34.75(12) ? C1 Ru3 C31 . . . 141.36(18) ? C1 Ru3 C32 . . . 100.17(15) ? C1 Ru3 C33 . . . 120.47(16) ? C2 Ru3 C31 . . . 158.16(17) ? C2 Ru3 C32 . . . 102.51(15) ? C2 Ru3 C33 . . . 85.78(15) ? C31 Ru3 C32 . . . 99.3(2) ? C31 Ru3 C33 . . . 90.8(2) ? C32 Ru3 C33 . . . 94.51(18) ? W1 Fe3 Ru2 . . . 62.060(12) ? W1 Fe3 Fe2 . . . 62.060(12) ? W1 Fe3 C1 . . . 41.79(9) ? W1 Fe3 C2 . . . 75.76(8) ? W1 Fe3 C31 . . . 101.21(15) ? W1 Fe3 C32 . . . 102.78(13) ? W1 Fe3 C33 . . . 156.95(13) ? Ru2 Fe3 Fe2 . . . .00000 ? Ru2 Fe3 C1 . . . 51.55(8) ? Ru2 Fe3 C2 . . . 51.42(8) ? Ru2 Fe3 C31 . . . 107.71(15) ? Ru2 Fe3 C32 . . . 150.98(13) ? Ru2 Fe3 C33 . . . 95.64(13) ? Fe2 Fe3 C1 . . . 51.55(8) ? Fe2 Fe3 C2 . . . 51.42(8) ? Fe2 Fe3 C31 . . . 107.71(15) ? Fe2 Fe3 C32 . . . 150.98(13) ? Fe2 Fe3 C33 . . . 95.64(13) ? C1 Fe3 C2 . . . 34.75(12) ? C1 Fe3 C31 . . . 141.36(18) ? C1 Fe3 C32 . . . 100.17(15) ? C1 Fe3 C33 . . . 120.47(16) ? C2 Fe3 C31 . . . 158.16(17) ? C2 Fe3 C32 . . . 102.51(15) ? C2 Fe3 C33 . . . 85.78(15) ? C31 Fe3 C32 . . . 99.3(2) ? C31 Fe3 C33 . . . 90.8(2) ? C32 Fe3 C33 . . . 94.51(18) ? Ru5 Ru4 Ru6 . . . 60.392(12) ? Ru5 Ru4 Fe6 . . . 60.392(12) ? Ru5 Ru4 C3 . . . 51.47(8) ? Ru5 Ru4 C4 . . . 50.59(9) ? Ru5 Ru4 C41 . . . 112.48(15) ? Ru5 Ru4 C42 . . . 142.55(14) ? Ru5 Ru4 C43 . . . 106.00(12) ? Ru5 Ru4 H0 . . . 36.7(12) ? Ru6 Ru4 Fe6 . . . .00000 ? Ru6 Ru4 C3 . . . 76.44(8) ? Ru6 Ru4 C4 . . . 42.32(9) ? Ru6 Ru4 C41 . . . 92.56(14) ? Ru6 Ru4 C42 . . . 92.73(13) ? Ru6 Ru4 C43 . . . 164.82(12) ? Ru6 Ru4 H0 . . . 83.5(12) ? Fe6 Ru4 C3 . . . 76.44(8) ? Fe6 Ru4 C4 . . . 42.32(9) ? Fe6 Ru4 C41 . . . 92.56(14) ? Fe6 Ru4 C42 . . . 92.73(13) ? Fe6 Ru4 C43 . . . 164.82(12) ? Fe6 Ru4 H0 . . . 83.5(12) ? C3 Ru4 C4 . . . 35.02(12) ? C3 Ru4 C41 . . . 163.56(16) ? C3 Ru4 C42 . . . 99.75(16) ? C3 Ru4 C43 . . . 89.77(14) ? C3 Ru4 H0 . . . 82.2(12) ? C4 Ru4 C41 . . . 134.81(16) ? C4 Ru4 C42 . . . 91.96(16) ? C4 Ru4 C43 . . . 124.65(15) ? C4 Ru4 H0 . . . 87.2(12) ? C41 Ru4 C42 . . . 92.9(2) ? C41 Ru4 C43 . . . 99.45(18) ? C41 Ru4 H0 . . . 84.5(12) ? C42 Ru4 C43 . . . 95.89(18) ? C42 Ru4 H0 . . . 175.3(12) ? C43 Ru4 H0 . . . 88.4(12) ? Ru4 Ru5 Ru6 . . . 60.257(14) ? Ru4 Ru5 Fe6 . . . 60.257(14) ? Ru4 Ru5 C3 . . . 51.00(8) ? Ru4 Ru5 C4 . . . 50.63(9) ? Ru4 Ru5 C51 . . . 111.39(14) ? Ru4 Ru5 C52 . . . 142.66(14) ? Ru4 Ru5 C53 . . . 105.91(13) ? Ru4 Ru5 H0 . . . 38.9(12) ? Ru6 Ru5 Fe6 . . . .00000 ? Ru6 Ru5 C3 . . . 76.14(8) ? Ru6 Ru5 C4 . . . 42.26(9) ? Ru6 Ru5 C51 . . . 90.69(13) ? Ru6 Ru5 C52 . . . 92.98(14) ? Ru6 Ru5 C53 . . . 165.17(12) ? Ru6 Ru5 H0 . . . 84.9(12) ? Fe6 Ru5 C3 . . . 76.14(8) ? Fe6 Ru5 C4 . . . 42.26(9) ? Fe6 Ru5 C51 . . . 90.69(13) ? Fe6 Ru5 C52 . . . 92.98(14) ? Fe6 Ru5 C53 . . . 165.17(12) ? Fe6 Ru5 H0 . . . 84.9(12) ? C3 Ru5 C4 . . . 34.90(12) ? C3 Ru5 C51 . . . 161.69(16) ? C3 Ru5 C52 . . . 100.21(16) ? C3 Ru5 C53 . . . 90.98(15) ? C3 Ru5 H0 . . . 83.6(12) ? C4 Ru5 C51 . . . 132.89(16) ? C4 Ru5 C52 . . . 92.03(16) ? C4 Ru5 C53 . . . 125.76(16) ? C4 Ru5 H0 . . . 89.4(12) ? C51 Ru5 C52 . . . 93.0(2) ? C51 Ru5 C53 . . . 100.06(19) ? C51 Ru5 H0 . . . 82.5(12) ? C52 Ru5 C53 . . . 96.58(19) ? C52 Ru5 H0 . . . 175.0(12) ? C53 Ru5 H0 . . . 86.5(12) ? Ru4 Ru6 Ru5 . . . 59.350(15) ? Ru4 Ru6 C4 . . . 51.21(10) ? Ru4 Ru6 C61 . . . 101.21(16) ? Ru4 Ru6 C62 . . . 98.34(15) ? Ru4 Ru6 C63 . . . 155.39(14) ? Ru5 Ru6 C4 . . . 51.09(10) ? Ru5 Ru6 C61 . . . 101.72(16) ? Ru5 Ru6 C62 . . . 153.34(14) ? Ru5 Ru6 C63 . . . 100.74(15) ? C4 Ru6 C61 . . . 147.00(18) ? C4 Ru6 C62 . . . 104.38(17) ? C4 Ru6 C63 . . . 105.74(18) ? C61 Ru6 C62 . . . 96.7(2) ? C61 Ru6 C63 . . . 96.9(2) ? C62 Ru6 C63 . . . 96.0(2) ? Ru4 Fe6 Ru5 . . . 59.350(15) ? Ru4 Fe6 C4 . . . 51.21(10) ? Ru4 Fe6 C61 . . . 101.21(16) ? Ru4 Fe6 C62 . . . 98.34(15) ? Ru4 Fe6 C63 . . . 155.39(14) ? Ru5 Fe6 C4 . . . 51.09(10) ? Ru5 Fe6 C61 . . . 101.72(16) ? Ru5 Fe6 C62 . . . 153.34(14) ? Ru5 Fe6 C63 . . . 100.74(15) ? C4 Fe6 C61 . . . 147.00(18) ? C4 Fe6 C62 . . . 104.38(17) ? C4 Fe6 C63 . . . 105.74(18) ? C61 Fe6 C62 . . . 96.7(2) ? C61 Fe6 C63 . . . 96.9(2) ? C62 Fe6 C63 . . . 96.0(2) ? W1 C1 Ru2 . . . 89.77(13) ? W1 C1 Fe2 . . . 89.77(13) ? W1 C1 Ru3 . . . 91.11(13) ? W1 C1 Fe3 . . . 91.11(13) ? W1 C1 C2 . . . 158.4(3) ? Ru2 C1 Fe2 . . . .00000 ? Ru2 C1 Ru3 . . . 74.72(11) ? Ru2 C1 Fe3 . . . 74.72(11) ? Ru2 C1 C2 . . . 72.0(2) ? Fe2 C1 Ru3 . . . 74.72(11) ? Fe2 C1 Fe3 . . . 74.72(11) ? Fe2 C1 C2 . . . 72.0(2) ? Ru3 C1 Fe3 . . . .00(7) ? Ru3 C1 C2 . . . 73.3(2) ? Fe3 C1 C2 . . . 73.3(2) ? Ru2 C2 Fe2 . . . .00(12) ? Ru2 C2 Ru3 . . . 74.37(10) ? Ru2 C2 Fe3 . . . 74.37(10) ? Ru2 C2 C1 . . . 72.0(2) ? Ru2 C2 C3 . . . 133.7(2) ? Fe2 C2 Ru3 . . . 74.37(10) ? Fe2 C2 Fe3 . . . 74.37(10) ? Fe2 C2 C1 . . . 72.0(2) ? Fe2 C2 C3 . . . 133.7(2) ? Ru3 C2 Fe3 . . . .00(12) ? Ru3 C2 C1 . . . 71.9(2) ? Ru3 C2 C3 . . . 129.4(2) ? Fe3 C2 C1 . . . 71.9(2) ? Fe3 C2 C3 . . . 129.4(2) ? C1 C2 C3 . . . 146.4(3) ? Ru4 C3 Ru5 . . . 77.53(10) ? Ru4 C3 C2 . . . 129.8(2) ? Ru4 C3 C4 . . . 71.6(2) ? Ru5 C3 C2 . . . 132.9(2) ? Ru5 C3 C4 . . . 71.0(2) ? C2 C3 C4 . . . 146.3(3) ? Ru4 C4 Ru5 . . . 78.78(11) ? Ru4 C4 Ru6 . . . 86.47(13) ? Ru4 C4 Fe6 . . . 86.47(13) ? Ru4 C4 C3 . . . 73.4(2) ? Ru5 C4 Ru6 . . . 86.65(13) ? Ru5 C4 Fe6 . . . 86.65(13) ? Ru5 C4 C3 . . . 74.1(2) ? Ru6 C4 Fe6 . . . .00(10) ? Ru6 C4 C3 . . . 154.3(3) ? Fe6 C4 C3 . . . 154.3(3) ? W1 C11 O11 . . . 172.3(4) ? W1 C12 O12 . . . 176.2(5) ? Ru2 C21 Fe2 . . . .00000 ? Ru2 C21 O21 . . . 178.5(4) ? Fe2 C21 O21 . . . 178.5(4) ? Ru2 C22 Fe2 . . . .00000 ? Ru2 C22 O22 . . . 177.0(4) ? Fe2 C22 O22 . . . 177.0(4) ? Ru2 C23 Fe2 . . . .00000 ? Ru2 C23 O23 . . . 176.2(4) ? Fe2 C23 O23 . . . 176.2(4) ? Ru3 C31 Fe3 . . . .00000 ? Ru3 C31 O31 . . . 176.8(5) ? Fe3 C31 O31 . . . 176.8(5) ? Ru3 C32 Fe3 . . . .00000 ? Ru3 C32 O32 . . . 176.2(4) ? Fe3 C32 O32 . . . 176.2(4) ? Ru3 C33 Fe3 . . . .00(7) ? Ru3 C33 O33 . . . 177.6(4) ? Fe3 C33 O33 . . . 177.6(4) ? Ru4 C41 O41 . . . 177.4(4) ? Ru4 C42 O42 . . . 177.9(4) ? Ru4 C43 O43 . . . 174.6(4) ? Ru5 C51 O51 . . . 176.4(4) ? Ru5 C52 O52 . . . 178.5(4) ? Ru5 C53 O53 . . . 177.0(4) ? Ru6 C61 Fe6 . . . .00000 ? Ru6 C61 O61 . . . 177.5(5) ? Fe6 C61 O61 . . . 177.5(5) ? Ru6 C62 Fe6 . . . .00(7) ? Ru6 C62 O62 . . . 177.0(4) ? Fe6 C62 O62 . . . 177.0(4) ? Ru6 C63 Fe6 . . . .00000 ? Ru6 C63 O63 . . . 175.6(4) ? Fe6 C63 O63 . . . 175.6(4) ? W1 C01 C02 . . . 72.0(4) ? W1 C01 C05 . . . 74.1(4) ? W1 C01 H01 . . . 124(3) ? C02 C01 C05 . . . 107.2(5) ? C02 C01 H01 . . . 115(3) ? C05 C01 H01 . . . 137(3) ? W1 C02 C01 . . . 72.3(4) ? W1 C02 C03 . . . 73.1(3) ? W1 C02 H02 . . . 125(3) ? C01 C02 C03 . . . 107.5(5) ? C01 C02 H02 . . . 132(3) ? C03 C02 H02 . . . 121(3) ? W1 C03 C02 . . . 72.0(3) ? W1 C03 C04 . . . 73.2(3) ? W1 C03 H03 . . . 112(3) ? C02 C03 C04 . . . 108.7(5) ? C02 C03 H03 . . . 121(3) ? C04 C03 H03 . . . 129(3) ? W1 C04 C03 . . . 72.0(3) ? W1 C04 C05 . . . 73.5(4) ? W1 C04 H04 . . . 127(4) ? C03 C04 C05 . . . 108.2(6) ? C03 C04 H04 . . . 132(4) ? C05 C04 H04 . . . 119(4) ? W1 C05 C01 . . . 70.9(4) ? W1 C05 C04 . . . 72.3(4) ? W1 C05 H05 . . . 114(3) ? C01 C05 C04 . . . 108.3(6) ? C01 C05 H05 . . . 123(3) ? C04 C05 H05 . . . 128(3) ? Ru4 H0 Ru5 . . . 104(2) ? 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 W1 C2 3.247(3) . . ? W1 O11 3.139(4) . . ? W1 O12 3.130(4) . . ? W1 C21 3.331(5) . . ? W1 H01 2.85(5) . . ? W1 H02 2.99(6) . . ? W1 H03 2.82(5) . . ? W1 H04 3.08(8) . . ? W1 H05 2.78(4) . . ? Ru2 C3 3.264(3) . . ? Ru2 O21 2.968(4) . . ? Ru2 O22 2.980(4) . . ? Ru2 O23 2.974(4) . . ? Ru2 C33 3.366(4) . . ? Fe2 C3 3.264(3) . . ? Fe2 O21 2.968(4) . . ? Fe2 O22 2.980(4) . . ? Fe2 O23 2.974(4) . . ? Fe2 C33 3.366(4) . . ? Ru3 C3 3.287(3) . . ? Ru3 C11 3.136(4) . . ? Ru3 C12 3.211(5) . . ? Ru3 C21 3.429(4) . . ? Ru3 C23 3.393(4) . . ? Ru3 O31 3.030(4) . . ? Ru3 O32 3.040(3) . . ? Ru3 O33 3.007(4) . . ? Fe3 C3 3.287(3) . . ? Fe3 C11 3.136(4) . . ? Fe3 C12 3.211(5) . . ? Fe3 C21 3.429(4) . . ? Fe3 C23 3.393(4) . . ? Fe3 O31 3.030(4) . . ? Fe3 O32 3.040(3) . . ? Fe3 O33 3.007(4) . . ? Ru4 C2 3.305(3) . . ? Ru4 O41 3.051(4) . . ? Ru4 O42 3.042(4) . . ? Ru4 O43 3.053(3) . . ? Ru5 C2 3.358(3) . . ? Ru5 O51 3.051(4) . . ? Ru5 O52 3.044(4) . . ? Ru5 O53 3.062(4) . . ? Ru6 C3 3.148(3) . . ? Ru6 C41 3.483(5) . . ? Ru6 C42 3.473(4) . . ? Ru6 C51 3.429(5) . . ? Ru6 C52 3.488(4) . . ? Ru6 O61 3.023(4) . . ? Ru6 O62 3.004(4) . . ? Ru6 O63 3.006(4) . . ? Ru6 H0 3.17(4) . . ? Fe6 C3 3.148(3) . . ? Fe6 C41 3.483(5) . . ? Fe6 C42 3.473(4) . . ? Fe6 C51 3.429(5) . . ? Fe6 C52 3.488(4) . . ? Fe6 O61 3.023(4) . . ? Fe6 O62 3.004(4) . . ? Fe6 O63 3.006(4) . . ? Fe6 H0 3.17(4) . . ? C1 C3 2.608(5) . . ? C1 C12 2.863(6) . . ? C2 C4 2.623(5) . . ? C2 C23 2.809(5) . . ? C2 C33 2.787(5) . . ? C3 C43 2.940(5) . . ? C3 C53 2.979(5) . . ? C3 H0 2.66(4) . . ? C4 C42 2.958(5) . . ? C4 C52 2.964(6) . . ? C4 C62 2.986(6) . . ? C4 C63 3.000(6) . . ? C11 C12 2.767(8) . . ? C11 C21 2.975(7) . . ? C11 C31 2.849(7) . . ? C11 C04 2.853(9) . . ? O11 C31 2.963(6) . . ? O11 O31 2.984(6) . . ? O11 H04 2.41(8) . '3 666' ? C12 C02 2.818(8) . . ? C21 C22 2.809(6) . . ? C21 C23 2.771(6) . . ? C22 C23 2.724(6) . . ? C22 H05 2.66(4) . . ? C31 C32 2.907(7) . . ? C31 C33 2.684(7) . . ? O31 H02 2.62(6) . '1 655' ? C32 C33 2.784(6) . . ? C41 C42 2.780(6) . . ? C41 C43 2.952(6) . . ? C41 H0 2.51(4) . . ? C42 C43 2.854(6) . . ? C43 H0 2.61(4) . . ? C51 C52 2.783(7) . . ? C51 C53 2.955(6) . . ? C51 H0 2.41(4) . . ? C52 C53 2.873(6) . . ? C53 H0 2.51(4) . . ? C61 C62 2.818(7) . . ? C61 C63 2.810(7) . . ? C62 C63 2.784(8) . . ? C01 C03 2.250(8) . . ? C01 C04 2.250(9) . . ? C01 H02 2.21(6) . . ? C01 H05 1.97(4) . . ? C02 C04 2.249(9) . . ? C02 C05 2.259(9) . . ? C02 H01 1.91(5) . . ? C02 H03 2.05(5) . . ? C03 C05 2.237(9) . . ? C03 H02 2.09(6) . . ? C03 H04 2.24(8) . . ? C04 H03 2.13(5) . . ? C04 H05 1.98(4) . . ? C05 H01 2.08(5) . . ? C05 H04 2.10(8) . . ? _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 2296 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 11 _reflns_limit_k_min 0 _reflns_limit_k_max 32 _reflns_limit_l_min -22 _reflns_limit_l_max 22 _reflns_number_observed ? _reflns_d_resolution_high .733 _reflns_d_resolution_low 13.587 _diffrn_reflns_av_sigmaI/netI .044 _diffrn_reflns_theta_min 1.49 _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 .037 _refine_ls_wR_factor_all .034 _refine_ls_goodness_of_fit_all .983 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end data_br550l # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C26 H6 Fe1 O17 Ru4 W1' _chemical_formula_moiety ? _chemical_formula_weight 1234.31 _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 8.499(2) _cell_length_b 23.949(11) _cell_length_c 16.537(8) _cell_angle_alpha 90.00000 _cell_angle_beta 90.76(3) _cell_angle_gamma 90.00000 _cell_volume 3366(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.434 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 14.5 _cell_measurement_theta_max 17.5 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 5.646 _exptl_crystal_description block _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.15 _exptl_crystal_size_rad ? _exptl_crystal_colour 'dark-red' _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\Q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; XTAL absorb ; _exptl_absorpt_correction_T_min 0.19 _exptl_absorpt_correction_T_max 0.44 _diffrn_reflns_number 12119 _reflns_number_total 4233 _reflns_Friedel_coverage ? _reflns_number_gt 1949 _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 .0822 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number 10 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F #<< use NfA code _refine_ls_R_factor_gt .043 _refine_ls_wR_factor_ref .047 _refine_ls_goodness_of_fit_ref 1.611 _refine_ls_number_reflns 4227 _refine_ls_number_parameters 446 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref #<< use NfA code _refine_ls_shift/su_max .076 _refine_diff_density_min -1.823 _refine_diff_density_max 2.341 _refine_ls_extinction_method none _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 ? 0 104 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 68 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 24 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 16 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' W ? 0 4 -1.421 6.872 'Int Tables Vol IV Tables 2.2B and 2.3.1' Fe ? 0 4 .301 .845 '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 .77220(10) .07560(3) .60862(6) .0486(7) Uani ? ? .694(8) ? ? Fe1 .77220(10) .07560(3) .60862(6) .0486(7) Uani ? ? .306(8) ? ? Ru2 .89660(10) .15859(3) .71106(5) .0414(5) Uani ? ? 1.00000 ? ? Ru3 .96090(10) .16125(3) .54651(5) .0409(5) Uani ? ? 1.00000 ? ? W4 .74518(6) .397860(10) .60891(3) .0466(3) Uani ? ? 1.00000 ? ? Ru5 .59830(10) .30818(4) .51671(6) .0388(6) Uani ? ? .478(8) ? ? Fe5 .59830(10) .30818(4) .51671(6) .0388(6) Uani ? ? .522(8) ? ? Ru6 .54040(10) .30698(3) .67186(5) .0413(5) Uani ? ? .860(8) ? ? Fe6 .54040(10) .30698(3) .67186(5) .0413(5) Uani ? ? .140(8) ? ? C11 .925(2) .0172(5) .6211(9) .085(9) Uani ? ? 1.00000 ? ? O11 1.0170(10) -.0157(4) .6323(8) .123(8) Uani ? ? 1.00000 ? ? C12 .687(2) .0494(4) .5111(9) .068(8) Uani ? ? 1.00000 ? ? O12 .6270(10) .0368(4) .4521(7) .098(8) Uani ? ? 1.00000 ? ? C13 .617(2) .0456(4) .6758(9) .072(8) Uani ? ? 1.00000 ? ? O13 .5190(10) .0292(4) .7136(7) .108(9) Uani ? ? 1.00000 ? ? C21 1.022(2) .1043(4) .7662(7) .065(8) Uani ? ? 1.00000 ? ? O21 1.1070(10) .0747(4) .7990(7) .112(9) Uani ? ? 1.00000 ? ? C22 .727(2) .1519(4) .7882(7) .060(7) Uani ? ? 1.00000 ? ? O22 .6290(10) .1466(4) .8292(6) .097(8) Uani ? ? 1.00000 ? ? C23 .9860(10) .2265(4) .7558(7) .055(7) Uani ? ? 1.00000 ? ? O23 1.0350(10) .2676(3) .7775(6) .090(7) Uani ? ? 1.00000 ? ? C31 1.130(2) .1098(4) .5188(8) .061(8) Uani ? ? 1.00000 ? ? O31 1.2280(10) .0815(3) .5017(7) .114(8) Uani ? ? 1.00000 ? ? C32 .862(2) .1572(4) .4415(8) .062(8) Uani ? ? 1.00000 ? ? O32 .8000(10) .1545(4) .3828(6) .094(7) Uani ? ? 1.00000 ? ? C33 1.0690(10) .2310(4) .5284(7) .051(7) Uani ? ? 1.00000 ? ? O33 1.1230(10) .2735(3) .5189(5) .069(6) Uani ? ? 1.00000 ? ? C41 .534(2) .4316(4) .6215(7) .065(8) Uani ? ? 1.00000 ? ? O41 .4210(10) .4591(3) .6260(7) .102(8) Uani ? ? 1.00000 ? ? C42 .773(2) .4044(4) .7294(9) .075(9) Uani ? ? 1.00000 ? ? O42 .805(2) .4099(4) .7958(7) .122(8) Uani ? ? 1.00000 ? ? C51 .454(2) .3596(5) .4808(7) .062(8) Uani ? ? 1.00000 ? ? O51 .3660(10) .3920(3) .4597(6) .086(7) Uani ? ? 1.00000 ? ? C52 .7320(10) .3070(4) .4291(7) .055(7) Uani ? ? 1.00000 ? ? O52 .8070(10) .3045(4) .3724(6) .093(7) Uani ? ? 1.00000 ? ? C53 .4900(10) .2441(5) .4875(7) .053(7) Uani ? ? 1.00000 ? ? O53 .4280(10) .2040(3) .4717(6) .082(7) Uani ? ? 1.00000 ? ? C61 .351(2) .3455(5) .6872(8) .075(9) Uani ? ? 1.00000 ? ? O61 .2310(10) .3667(4) .6958(7) .114(8) Uani ? ? 1.00000 ? ? C62 .6100(10) .3000(4) .7819(7) .054(7) Uani ? ? 1.00000 ? ? O62 .6490(10) .2926(4) .8472(6) .089(7) Uani ? ? 1.00000 ? ? C63 .4330(10) .2376(5) .6676(7) .056(7) Uani ? ? 1.00000 ? ? O63 .3750(10) .1960(3) .6694(5) .080(7) Uani ? ? 1.00000 ? ? C1 .7310(10) .1537(3) .6063(6) .044(6) Uani ? ? 1.00000 ? ? C2 .7760(10) .2069(3) .6134(5) .035(5) Uani ? ? 1.00000 ? ? C3 .7250(10) .2624(3) .6056(6) .038(5) Uani ? ? 1.00000 ? ? C4 .7650(10) .3161(3) .6118(6) .041(6) Uani ? ? 1.00000 ? ? C401 .854(2) .4287(6) .4901(9) .094(13) Uani ? ? 1.00000 ? ? C402 .781(2) .4729(6) .5210(10) .101(13) Uani ? ? 1.00000 ? ? C403 .858(2) .4860(4) .5960(10) .092(12) Uani ? ? 1.00000 ? ? C404 .978(2) .4463(6) .6080(10) .083(9) Uani ? ? 1.00000 ? ? C405 .984(2) .4114(5) .5440(10) .097(12) Uani ? ? 1.00000 ? ? H401 .82480 .41170 .44030 .11400 Uiso ? ? 1.00000 ? ? H402 .69410 .49290 .49780 .12300 Uiso ? ? 1.00000 ? ? H403 .83110 .51580 .63190 .11500 Uiso ? ? 1.00000 ? ? H404 1.04710 .44520 .65350 .10800 Uiso ? ? 1.00000 ? ? H405 1.05490 .38170 .53400 .11400 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 .0539(7) .0310(5) .0610(8) -.0030(4) .0075(6) -.0005(4) Fe1 .0539(7) .0310(5) .0610(8) -.0030(4) .0075(6) .0005(4) Ru2 .0467(5) .0364(4) .0412(5) .0045(3) .0020(4) .0043(3) Ru3 .0434(5) .0356(4) .0439(6) -.0003(3) .0089(4) -.0034(3) W4 .0554(3) .0309(2) .0532(3) .0026(2) -.0061(2) .0026(2) Ru5 .0400(6) .0417(6) .0348(7) .0022(4) .0010(5) .0042(4) Fe5 .0400(6) .0417(6) .0348(7) .0022(4) .0010(5) .0042(4) Ru6 .0416(5) .0472(5) .0353(6) .0099(4) .0054(4) .0031(3) Fe6 .0416(5) .0472(5) .0353(6) .0099(4) .0054(4) .0031(3) C11 .100(10) .056(7) .100(10) .004(8) -.010(10) .010(7) O11 .079(8) .090(7) .200(10) .035(6) -.004(9) .007(7) C12 .066(8) .049(6) .090(10) .010(6) .002(8) .000(6) O12 .106(9) .089(6) .100(9) .024(6) -.002(7) .020(6) C13 .072(9) .053(6) .090(10) .009(6) .014(8) .008(6) O13 .107(9) .098(7) .120(10) .014(6) .052(8) .033(6) C21 .090(10) .056(6) .049(8) .008(6) .003(7) .008(5) O21 .120(10) .084(6) .130(10) .046(6) -.020(8) .032(6) C22 .066(8) .069(7) .045(7) .015(6) .009(7) .010(5) O22 .072(7) .127(8) .092(8) .010(6) .032(7) .032(6) C23 .059(7) .058(6) .047(7) .005(5) .000(6) .005(5) O23 .109(8) .059(5) .100(9) .016(5) -.022(7) .014(5) C31 .065(8) .050(6) .069(9) .002(6) .014(7) .010(5) O31 .088(8) .074(6) .180(10) .037(6) .033(8) .020(6) C32 .058(8) .058(6) .070(10) .011(6) -.010(7) .011(6) O32 .096(8) .119(7) .067(7) .024(6) -.002(6) .010(6) C33 .035(6) .055(6) .063(8) .004(5) .007(6) .004(5) O33 .065(6) .053(4) .091(7) .013(4) .022(5) .001(4) C41 .076(9) .058(6) .060(9) .016(7) .000(7) .001(5) O41 .089(8) .068(5) .150(10) .034(5) .002(7) -.009(5) C42 .090(10) .044(6) .090(10) .009(6) -.032(9) .016(6) O42 .190(10) .100(7) .076(8) -.036(8) -.031(9) .019(6) C51 .063(8) .068(7) .056(8) -.001(6) .011(7) .010(6) O51 .077(6) .087(6) .092(8) .033(5) -.021(6) .002(5) C52 .054(7) .066(6) .046(8) -.011(6) -.001(6) .005(5) O52 .081(7) .127(7) .073(8) -.017(6) .031(6) .001(6) C53 .050(7) .067(6) .041(7) .010(6) .013(6) .000(5) O53 .088(7) .068(5) .090(8) -.029(5) -.008(6) .013(5) C61 .080(10) .085(8) .060(10) .014(8) .022(8) .020(6) O61 .085(7) .139(8) .120(10) .065(7) .026(7) .036(7) C62 .055(7) .070(6) .038(7) .011(5) .005(6) .004(5) O62 .089(7) .125(7) .052(6) .028(6) -.013(6) .008(5) C63 .037(6) .077(7) .054(8) .002(6) .004(6) .007(6) O63 .079(7) .089(6) .072(7) -.030(5) .015(5) .005(5) C1 .045(6) .037(4) .050(7) .005(4) .006(5) .009(4) C2 .031(5) .042(4) .031(6) .004(4) .012(4) .001(4) C3 .039(6) .040(4) .036(6) .000(4) .014(5) .001(4) C4 .044(6) .045(5) .035(6) .004(4) .021(5) .000(4) C401 .13(2) .083(9) .070(10) -.060(10) -.010(10) .017(8) C402 .15(2) .073(9) .080(10) -.030(10) -.040(10) .044(8) C403 .100(10) .037(6) .14(2) .001(7) -.010(10) .008(7) C404 .070(9) .080(8) .100(10) .022(8) -.015(9) .005(8) C405 .110(10) .042(6) .14(2) .010(7) .050(10) .017(7) # 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 . . 2.8090(14) ? Ru1 Ru3 . . 2.8068(13) ? Ru1 C11 . . 1.918(15) ? Ru1 C12 . . 1.868(15) ? Ru1 C13 . . 1.879(15) ? Ru1 C1 . . 1.903(7) ? Fe1 Ru2 . . 2.8090(14) ? Fe1 Ru3 . . 2.8068(13) ? Fe1 C11 . . 1.918(15) ? Fe1 C12 . . 1.868(15) ? Fe1 C13 . . 1.879(15) ? Fe1 C1 . . 1.903(7) ? Ru2 Ru3 . . 2.7833(17) ? Ru2 C21 . . 1.906(13) ? Ru2 C22 . . 1.944(15) ? Ru2 C23 . . 1.938(10) ? Ru2 C1 . . 2.221(9) ? Ru2 C2 . . 2.226(8) ? Ru3 C31 . . 1.952(14) ? Ru3 C32 . . 1.922(14) ? Ru3 C33 . . 1.932(9) ? Ru3 C1 . . 2.209(9) ? Ru3 C2 . . 2.221(8) ? W4 Ru5 . . 2.9061(13) ? W4 Fe5 . . 2.9061(13) ? W4 Ru6 . . 2.9829(12) ? W4 Fe6 . . 2.9829(12) ? W4 C41 . . 1.982(16) ? W4 C42 . . 2.010(15) ? W4 C4 . . 1.966(7) ? W4 C401 . . 2.304(15) ? W4 C402 . . 2.334(15) ? W4 C403 . . 2.329(11) ? W4 C404 . . 2.294(16) ? W4 C405 . . 2.331(17) ? Ru5 Ru6 . . 2.6190(18) ? Ru5 Fe6 . . 2.6190(18) ? Ru5 C51 . . 1.831(14) ? Ru5 C52 . . 1.853(11) ? Ru5 C53 . . 1.850(11) ? Ru5 C3 . . 2.117(9) ? Ru5 C4 . . 2.111(9) ? Fe5 Ru6 . . 2.6190(18) ? Fe5 Fe6 . . 2.6190(18) ? Fe5 C51 . . 1.831(14) ? Fe5 C52 . . 1.853(11) ? Fe5 C53 . . 1.850(11) ? Fe5 C3 . . 2.117(9) ? Fe5 C4 . . 2.111(9) ? Ru6 C61 . . 1.875(16) ? Ru6 C62 . . 1.913(11) ? Ru6 C63 . . 1.897(11) ? Ru6 C3 . . 2.202(9) ? Ru6 C4 . . 2.174(9) ? Fe6 C61 . . 1.875(16) ? Fe6 C62 . . 1.913(11) ? Fe6 C63 . . 1.897(11) ? Fe6 C3 . . 2.202(9) ? Fe6 C4 . . 2.174(9) ? C11 O11 . . 1.124(17) ? C12 O12 . . 1.136(18) ? C13 O13 . . 1.119(18) ? C21 O21 . . 1.144(16) ? C22 O22 . . 1.088(18) ? C23 O23 . . 1.126(12) ? C31 O31 . . 1.113(17) ? C32 O32 . . 1.100(17) ? C33 O33 . . 1.128(12) ? C41 O41 . . 1.168(17) ? C42 O42 . . 1.14(2) ? C51 O51 . . 1.130(16) ? C52 O52 . . 1.142(14) ? C53 O53 . . 1.125(14) ? C61 O61 . . 1.150(18) ? C62 O62 . . 1.139(15) ? C63 O63 . . 1.112(14) ? C1 C2 . . 1.335(10) ? C2 C3 . . 1.403(10) ? C3 C4 . . 1.334(10) ? C401 C402 . . 1.33(2) ? C401 C405 . . 1.47(2) ? C401 H401 . . .949(15) ? C402 C403 . . 1.43(2) ? C402 H402 . . .956(16) ? C403 C404 . . 1.41(2) ? C403 H403 . . .958(13) ? C404 C405 . . 1.35(2) ? C404 H404 . . .949(17) ? C405 H405 . . .948(14) ? 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 . . . 59.42(4) ? Ru2 Ru1 C11 . . . 101.7(4) ? Ru2 Ru1 C12 . . . 153.8(3) ? Ru2 Ru1 C13 . . . 100.1(4) ? Ru2 Ru1 C1 . . . 52.0(3) ? Ru3 Ru1 C11 . . . 100.5(5) ? Ru3 Ru1 C12 . . . 98.4(4) ? Ru3 Ru1 C13 . . . 154.8(3) ? Ru3 Ru1 C1 . . . 51.7(3) ? C11 Ru1 C12 . . . 95.9(6) ? C11 Ru1 C13 . . . 97.9(6) ? C11 Ru1 C1 . . . 147.5(5) ? C12 Ru1 C13 . . . 96.6(7) ? C12 Ru1 C1 . . . 104.1(4) ? C13 Ru1 C1 . . . 104.9(4) ? Ru2 Fe1 Ru3 . . . 59.42(4) ? Ru2 Fe1 C11 . . . 101.7(4) ? Ru2 Fe1 C12 . . . 153.8(3) ? Ru2 Fe1 C13 . . . 100.1(4) ? Ru2 Fe1 C1 . . . 52.0(3) ? Ru3 Fe1 C11 . . . 100.5(5) ? Ru3 Fe1 C12 . . . 98.4(4) ? Ru3 Fe1 C13 . . . 154.8(3) ? Ru3 Fe1 C1 . . . 51.7(3) ? C11 Fe1 C12 . . . 95.9(6) ? C11 Fe1 C13 . . . 97.9(6) ? C11 Fe1 C1 . . . 147.5(5) ? C12 Fe1 C13 . . . 96.6(7) ? C12 Fe1 C1 . . . 104.1(4) ? C13 Fe1 C1 . . . 104.9(4) ? Ru1 Ru2 Fe1 . . . .00(12) ? Ru1 Ru2 Ru3 . . . 60.25(4) ? Ru1 Ru2 C21 . . . 90.5(3) ? Ru1 Ru2 C22 . . . 93.5(3) ? Ru1 Ru2 C23 . . . 165.2(3) ? Ru1 Ru2 C1 . . . 42.49(19) ? Ru1 Ru2 C2 . . . 76.4(2) ? Fe1 Ru2 Ru3 . . . 60.25(4) ? Fe1 Ru2 C21 . . . 90.5(3) ? Fe1 Ru2 C22 . . . 93.5(3) ? Fe1 Ru2 C23 . . . 165.2(3) ? Fe1 Ru2 C1 . . . 42.49(19) ? Fe1 Ru2 C2 . . . 76.4(2) ? Ru3 Ru2 C21 . . . 111.6(4) ? Ru3 Ru2 C22 . . . 143.2(4) ? Ru3 Ru2 C23 . . . 105.8(3) ? Ru3 Ru2 C1 . . . 50.9(2) ? Ru3 Ru2 C2 . . . 51.2(2) ? C21 Ru2 C22 . . . 92.6(6) ? C21 Ru2 C23 . . . 100.1(5) ? C21 Ru2 C1 . . . 133.0(4) ? C21 Ru2 C2 . . . 162.0(4) ? C22 Ru2 C23 . . . 96.3(4) ? C22 Ru2 C1 . . . 92.3(5) ? C22 Ru2 C2 . . . 100.4(5) ? C23 Ru2 C1 . . . 125.7(4) ? C23 Ru2 C2 . . . 90.9(4) ? C1 Ru2 C2 . . . 34.9(3) ? Ru1 Ru3 Fe1 . . . .00(7) ? Ru1 Ru3 Ru2 . . . 60.33(3) ? Ru1 Ru3 C31 . . . 92.9(4) ? Ru1 Ru3 C32 . . . 92.8(4) ? Ru1 Ru3 C33 . . . 164.6(3) ? Ru1 Ru3 C1 . . . 42.55(19) ? Ru1 Ru3 C2 . . . 76.5(2) ? Fe1 Ru3 Ru2 . . . 60.33(3) ? Fe1 Ru3 C31 . . . 92.9(4) ? Fe1 Ru3 C32 . . . 92.8(4) ? Fe1 Ru3 C33 . . . 164.6(3) ? Fe1 Ru3 C1 . . . 42.55(19) ? Fe1 Ru3 C2 . . . 76.5(2) ? Ru2 Ru3 C31 . . . 111.7(4) ? Ru2 Ru3 C32 . . . 142.5(5) ? Ru2 Ru3 C33 . . . 105.7(3) ? Ru2 Ru3 C1 . . . 51.3(3) ? Ru2 Ru3 C2 . . . 51.3(2) ? C31 Ru3 C32 . . . 94.0(6) ? C31 Ru3 C33 . . . 99.0(5) ? C31 Ru3 C1 . . . 135.4(4) ? C31 Ru3 C2 . . . 162.8(4) ? C32 Ru3 C33 . . . 96.1(5) ? C32 Ru3 C1 . . . 91.2(6) ? C32 Ru3 C2 . . . 99.8(5) ? C33 Ru3 C1 . . . 124.4(3) ? C33 Ru3 C2 . . . 89.6(3) ? C1 Ru3 C2 . . . 35.1(3) ? Ru5 W4 Fe5 . . . .00000 ? Ru5 W4 Ru6 . . . 52.79(4) ? Ru5 W4 Fe6 . . . 52.79(4) ? Ru5 W4 C41 . . . 88.5(3) ? Ru5 W4 C42 . . . 128.5(3) ? Ru5 W4 C4 . . . 46.6(3) ? Ru5 W4 C401 . . . 87.9(4) ? Ru5 W4 C402 . . . 107.5(4) ? Ru5 W4 C403 . . . 142.8(4) ? Ru5 W4 C404 . . . 137.3(4) ? Ru5 W4 C405 . . . 103.4(4) ? Fe5 W4 Ru6 . . . 52.79(4) ? Fe5 W4 Fe6 . . . 52.79(4) ? Fe5 W4 C41 . . . 88.5(3) ? Fe5 W4 C42 . . . 128.5(3) ? Fe5 W4 C4 . . . 46.6(3) ? Fe5 W4 C401 . . . 87.9(4) ? Fe5 W4 C402 . . . 107.5(4) ? Fe5 W4 C403 . . . 142.8(4) ? Fe5 W4 C404 . . . 137.3(4) ? Fe5 W4 C405 . . . 103.4(4) ? Ru6 W4 Fe6 . . . .00000 ? Ru6 W4 C41 . . . 74.2(3) ? Ru6 W4 C42 . . . 76.8(4) ? Ru6 W4 C4 . . . 46.8(3) ? Ru6 W4 C401 . . . 140.7(4) ? Ru6 W4 C402 . . . 149.4(4) ? Ru6 W4 C403 . . . 159.4(4) ? Ru6 W4 C404 . . . 151.5(4) ? Ru6 W4 C405 . . . 141.1(3) ? Fe6 W4 C41 . . . 74.2(3) ? Fe6 W4 C42 . . . 76.8(4) ? Fe6 W4 C4 . . . 46.8(3) ? Fe6 W4 C401 . . . 140.7(4) ? Fe6 W4 C402 . . . 149.4(4) ? Fe6 W4 C403 . . . 159.4(4) ? Fe6 W4 C404 . . . 151.5(4) ? Fe6 W4 C405 . . . 141.1(3) ? C41 W4 C42 . . . 87.6(6) ? C41 W4 C4 . . . 118.8(4) ? C41 W4 C401 . . . 109.5(5) ? C41 W4 C402 . . . 83.0(5) ? C41 W4 C403 . . . 90.8(5) ? C41 W4 C404 . . . 125.2(5) ? C41 W4 C405 . . . 141.9(5) ? C42 W4 C4 . . . 92.6(4) ? C42 W4 C401 . . . 141.0(6) ? C42 W4 C402 . . . 122.9(5) ? C42 W4 C403 . . . 88.7(5) ? C42 W4 C404 . . . 82.9(6) ? C42 W4 C405 . . . 110.7(6) ? C4 W4 C401 . . . 107.7(5) ? C4 W4 C402 . . . 140.4(5) ? C4 W4 C403 . . . 150.4(5) ? C4 W4 C404 . . . 115.5(5) ? C4 W4 C405 . . . 94.3(4) ? C401 W4 C402 . . . 33.4(5) ? C401 W4 C403 . . . 57.4(5) ? C401 W4 C404 . . . 58.4(6) ? C401 W4 C405 . . . 37.0(6) ? C402 W4 C403 . . . 35.7(6) ? C402 W4 C404 . . . 59.1(6) ? C402 W4 C405 . . . 59.0(5) ? C403 W4 C404 . . . 35.4(5) ? C403 W4 C405 . . . 58.0(5) ? C404 W4 C405 . . . 33.9(5) ? W4 Ru5 Ru6 . . . 65.11(3) ? W4 Ru5 Fe6 . . . 65.11(3) ? W4 Ru5 C51 . . . 87.4(4) ? W4 Ru5 C52 . . . 99.1(3) ? W4 Ru5 C53 . . . 163.5(4) ? W4 Ru5 C3 . . . 78.9(2) ? W4 Ru5 C4 . . . 42.6(2) ? Ru6 Ru5 Fe6 . . . .00000 ? Ru6 Ru5 C51 . . . 101.0(4) ? Ru6 Ru5 C52 . . . 153.0(3) ? Ru6 Ru5 C53 . . . 98.5(4) ? Ru6 Ru5 C3 . . . 54.2(3) ? Ru6 Ru5 C4 . . . 53.4(3) ? Fe6 Ru5 C51 . . . 101.0(4) ? Fe6 Ru5 C52 . . . 153.0(3) ? Fe6 Ru5 C53 . . . 98.5(4) ? Fe6 Ru5 C3 . . . 54.2(3) ? Fe6 Ru5 C4 . . . 53.4(3) ? C51 Ru5 C52 . . . 99.9(5) ? C51 Ru5 C53 . . . 98.3(5) ? C51 Ru5 C3 . . . 154.9(5) ? C51 Ru5 C4 . . . 128.4(4) ? C52 Ru5 C53 . . . 95.2(4) ? C52 Ru5 C3 . . . 102.9(4) ? C52 Ru5 C4 . . . 99.9(4) ? C53 Ru5 C3 . . . 89.9(4) ? C53 Ru5 C4 . . . 126.6(4) ? C3 Ru5 C4 . . . 36.8(3) ? W4 Fe5 Ru6 . . . 65.11(3) ? W4 Fe5 Fe6 . . . 65.11(3) ? W4 Fe5 C51 . . . 87.4(4) ? W4 Fe5 C52 . . . 99.1(3) ? W4 Fe5 C53 . . . 163.5(4) ? W4 Fe5 C3 . . . 78.9(2) ? W4 Fe5 C4 . . . 42.6(2) ? Ru6 Fe5 Fe6 . . . .00000 ? Ru6 Fe5 C51 . . . 101.0(4) ? Ru6 Fe5 C52 . . . 153.0(3) ? Ru6 Fe5 C53 . . . 98.5(4) ? Ru6 Fe5 C3 . . . 54.2(3) ? Ru6 Fe5 C4 . . . 53.4(3) ? Fe6 Fe5 C51 . . . 101.0(4) ? Fe6 Fe5 C52 . . . 153.0(3) ? Fe6 Fe5 C53 . . . 98.5(4) ? Fe6 Fe5 C3 . . . 54.2(3) ? Fe6 Fe5 C4 . . . 53.4(3) ? C51 Fe5 C52 . . . 99.9(5) ? C51 Fe5 C53 . . . 98.3(5) ? C51 Fe5 C3 . . . 154.9(5) ? C51 Fe5 C4 . . . 128.4(4) ? C52 Fe5 C53 . . . 95.2(4) ? C52 Fe5 C3 . . . 102.9(4) ? C52 Fe5 C4 . . . 99.9(4) ? C53 Fe5 C3 . . . 89.9(4) ? C53 Fe5 C4 . . . 126.6(4) ? C3 Fe5 C4 . . . 36.8(3) ? W4 Ru6 Ru5 . . . 62.10(3) ? W4 Ru6 Fe5 . . . 62.10(3) ? W4 Ru6 C61 . . . 101.2(4) ? W4 Ru6 C62 . . . 102.8(3) ? W4 Ru6 C63 . . . 155.4(3) ? W4 Ru6 C3 . . . 75.9(2) ? W4 Ru6 C4 . . . 41.2(2) ? Ru5 Ru6 Fe5 . . . .00(7) ? Ru5 Ru6 C61 . . . 107.4(4) ? Ru5 Ru6 C62 . . . 150.8(3) ? Ru5 Ru6 C63 . . . 94.0(3) ? Ru5 Ru6 C3 . . . 51.2(2) ? Ru5 Ru6 C4 . . . 51.2(3) ? Fe5 Ru6 C61 . . . 107.4(4) ? Fe5 Ru6 C62 . . . 150.8(3) ? Fe5 Ru6 C63 . . . 94.0(3) ? Fe5 Ru6 C3 . . . 51.2(2) ? Fe5 Ru6 C4 . . . 51.2(3) ? C61 Ru6 C62 . . . 99.8(5) ? C61 Ru6 C63 . . . 91.3(5) ? C61 Ru6 C3 . . . 157.6(5) ? C61 Ru6 C4 . . . 140.6(4) ? C62 Ru6 C63 . . . 95.8(4) ? C62 Ru6 C3 . . . 102.6(4) ? C62 Ru6 C4 . . . 100.4(4) ? C63 Ru6 C3 . . . 84.4(4) ? C63 Ru6 C4 . . . 119.7(4) ? C3 Ru6 C4 . . . 35.5(3) ? W4 Fe6 Ru5 . . . 62.10(3) ? W4 Fe6 Fe5 . . . 62.10(3) ? W4 Fe6 C61 . . . 101.2(4) ? W4 Fe6 C62 . . . 102.8(3) ? W4 Fe6 C63 . . . 155.4(3) ? W4 Fe6 C3 . . . 75.9(2) ? W4 Fe6 C4 . . . 41.2(2) ? Ru5 Fe6 Fe5 . . . .00(7) ? Ru5 Fe6 C61 . . . 107.4(4) ? Ru5 Fe6 C62 . . . 150.8(3) ? Ru5 Fe6 C63 . . . 94.0(3) ? Ru5 Fe6 C3 . . . 51.2(2) ? Ru5 Fe6 C4 . . . 51.2(3) ? Fe5 Fe6 C61 . . . 107.4(4) ? Fe5 Fe6 C62 . . . 150.8(3) ? Fe5 Fe6 C63 . . . 94.0(3) ? Fe5 Fe6 C3 . . . 51.2(2) ? Fe5 Fe6 C4 . . . 51.2(3) ? C61 Fe6 C62 . . . 99.8(5) ? C61 Fe6 C63 . . . 91.3(5) ? C61 Fe6 C3 . . . 157.6(5) ? C61 Fe6 C4 . . . 140.6(4) ? C62 Fe6 C63 . . . 95.8(4) ? C62 Fe6 C3 . . . 102.6(4) ? C62 Fe6 C4 . . . 100.4(4) ? C63 Fe6 C3 . . . 84.4(4) ? C63 Fe6 C4 . . . 119.7(4) ? C3 Fe6 C4 . . . 35.5(3) ? Ru1 C11 Fe1 . . . .00000 ? Ru1 C11 O11 . . . 176.2(13) ? Fe1 C11 O11 . . . 176.2(13) ? Ru1 C12 Fe1 . . . .00(10) ? Ru1 C12 O12 . . . 174.6(12) ? Fe1 C12 O12 . . . 174.6(12) ? Ru1 C13 Fe1 . . . .00000 ? Ru1 C13 O13 . . . 176.5(13) ? Fe1 C13 O13 . . . 176.5(13) ? Ru2 C21 O21 . . . 174.5(12) ? Ru2 C22 O22 . . . 177.0(11) ? Ru2 C23 O23 . . . 175.7(10) ? Ru3 C31 O31 . . . 178.2(11) ? Ru3 C32 O32 . . . 177.3(14) ? Ru3 C33 O33 . . . 175.4(8) ? W4 C41 O41 . . . 169.6(10) ? W4 C42 O42 . . . 172.5(15) ? Ru5 C51 Fe5 . . . .00(12) ? Ru5 C51 O51 . . . 178.7(11) ? Fe5 C51 O51 . . . 178.7(11) ? Ru5 C52 Fe5 . . . .00(12) ? Ru5 C52 O52 . . . 175.6(9) ? Fe5 C52 O52 . . . 175.6(9) ? Ru5 C53 Fe5 . . . .00(7) ? Ru5 C53 O53 . . . 177.3(10) ? Fe5 C53 O53 . . . 177.3(10) ? Ru6 C61 Fe6 . . . .00000 ? Ru6 C61 O61 . . . 176.6(12) ? Fe6 C61 O61 . . . 176.6(12) ? Ru6 C62 Fe6 . . . .00(7) ? Ru6 C62 O62 . . . 176.0(9) ? Fe6 C62 O62 . . . 176.0(9) ? Ru6 C63 Fe6 . . . .00(10) ? Ru6 C63 O63 . . . 175.6(10) ? Fe6 C63 O63 . . . 175.6(10) ? Ru1 C1 Fe1 . . . .00(12) ? Ru1 C1 Ru2 . . . 85.5(3) ? Ru1 C1 Ru3 . . . 85.7(3) ? Ru1 C1 C2 . . . 152.1(7) ? Fe1 C1 Ru2 . . . 85.5(3) ? Fe1 C1 Ru3 . . . 85.7(3) ? Fe1 C1 C2 . . . 152.1(7) ? Ru2 C1 Ru3 . . . 77.9(3) ? Ru2 C1 C2 . . . 72.7(5) ? Ru3 C1 C2 . . . 73.0(5) ? Ru2 C2 Ru3 . . . 77.5(3) ? Ru2 C2 C1 . . . 72.3(5) ? Ru2 C2 C3 . . . 134.2(6) ? Ru3 C2 C1 . . . 72.0(5) ? Ru3 C2 C3 . . . 129.8(6) ? C1 C2 C3 . . . 143.9(8) ? Ru5 C3 Fe5 . . . .00(12) ? Ru5 C3 Ru6 . . . 74.6(3) ? Ru5 C3 Fe6 . . . 74.6(3) ? Ru5 C3 C2 . . . 135.1(7) ? Ru5 C3 C4 . . . 71.4(5) ? Fe5 C3 Ru6 . . . 74.6(3) ? Fe5 C3 Fe6 . . . 74.6(3) ? Fe5 C3 C2 . . . 135.1(7) ? Fe5 C3 C4 . . . 71.4(5) ? Ru6 C3 Fe6 . . . .00(7) ? Ru6 C3 C2 . . . 129.4(7) ? Ru6 C3 C4 . . . 71.1(5) ? Fe6 C3 C2 . . . 129.4(7) ? Fe6 C3 C4 . . . 71.1(5) ? C2 C3 C4 . . . 145.9(9) ? W4 C4 Ru5 . . . 90.9(3) ? W4 C4 Fe5 . . . 90.9(3) ? W4 C4 Ru6 . . . 92.0(3) ? W4 C4 Fe6 . . . 92.0(3) ? W4 C4 C3 . . . 159.5(7) ? Ru5 C4 Fe5 . . . .00(7) ? Ru5 C4 Ru6 . . . 75.3(3) ? Ru5 C4 Fe6 . . . 75.3(3) ? Ru5 C4 C3 . . . 71.8(6) ? Fe5 C4 Ru6 . . . 75.3(3) ? Fe5 C4 Fe6 . . . 75.3(3) ? Fe5 C4 C3 . . . 71.8(6) ? Ru6 C4 Fe6 . . . .00000 ? Ru6 C4 C3 . . . 73.4(5) ? Fe6 C4 C3 . . . 73.4(5) ? W4 C401 C402 . . . 74.5(10) ? W4 C401 C405 . . . 72.5(9) ? W4 C401 H401 . . . 120.0(12) ? C402 C401 C405 . . . 110.0(14) ? C402 C401 H401 . . . 123.8(16) ? C405 C401 H401 . . . 126.2(15) ? W4 C402 C401 . . . 72.1(9) ? W4 C402 C403 . . . 72.0(8) ? W4 C402 H402 . . . 121.9(13) ? C401 C402 C403 . . . 107.3(14) ? C401 C402 H402 . . . 127.2(16) ? C403 C402 H402 . . . 125.5(15) ? W4 C403 C402 . . . 72.3(8) ? W4 C403 C404 . . . 70.9(8) ? W4 C403 H403 . . . 121.1(12) ? C402 C403 C404 . . . 107.3(12) ? C402 C403 H403 . . . 126.2(15) ? C404 C403 H403 . . . 126.5(16) ? W4 C404 C403 . . . 73.7(9) ? W4 C404 C405 . . . 74.6(10) ? W4 C404 H404 . . . 120.4(12) ? C403 C404 C405 . . . 110.0(15) ? C403 C404 H404 . . . 124.8(15) ? C405 C404 H404 . . . 125.1(16) ? W4 C405 C401 . . . 70.5(9) ? W4 C405 C404 . . . 71.5(10) ? W4 C405 H405 . . . 122.4(11) ? C401 C405 C404 . . . 105.4(13) ? C401 C405 H405 . . . 125.4(15) ? C404 C405 H405 . . . 129.2(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 3.040(9) . . ? Ru1 O12 3.000(11) . . ? Ru1 O13 2.996(10) . . ? Ru1 C21 3.409(14) . . ? Ru1 C31 3.499(16) . . ? Ru1 C32 3.478(13) . . ? Ru1 C2 3.146(7) . . ? Fe1 O11 3.040(9) . . ? Fe1 O12 3.000(11) . . ? Fe1 O13 2.996(10) . . ? Fe1 C21 3.409(14) . . ? Fe1 C31 3.499(16) . . ? Fe1 C32 3.478(13) . . ? Fe1 C2 3.146(7) . . ? Ru2 O21 3.046(10) . . ? Ru2 O22 3.031(9) . . ? Ru2 O23 3.061(8) . . ? Ru2 C3 3.359(8) . . ? Ru3 O31 3.065(8) . . ? Ru3 O32 3.021(10) . . ? Ru3 O33 3.058(8) . . ? Ru3 C3 3.301(8) . . ? W4 O41 3.137(8) . . ? W4 O42 3.139(12) . . ? W4 C51 3.363(15) . . ? W4 C3 3.249(7) . . ? W4 H401 2.8970(14) . . ? W4 H402 2.9537(10) . . ? W4 H403 2.9408(13) . . ? W4 H404 2.8919(7) . . ? W4 H405 2.9496(8) . . ? Ru5 C41 3.473(11) . . ? Ru5 O51 2.961(8) . . ? Ru5 O52 2.994(10) . . ? Ru5 O53 2.974(8) . . ? Ru5 C63 3.339(11) . . ? Ru5 C2 3.264(8) . . ? Fe5 C41 3.473(11) . . ? Fe5 O51 2.961(8) . . ? Fe5 O52 2.994(10) . . ? Fe5 O53 2.974(8) . . ? Fe5 C63 3.339(11) . . ? Fe5 C2 3.264(8) . . ? Ru6 C41 3.099(10) . . ? Ru6 C42 3.195(13) . . ? Ru6 C51 3.471(12) . . ? Ru6 C53 3.422(12) . . ? Ru6 O61 3.024(9) . . ? Ru6 O62 3.051(10) . . ? Ru6 O63 3.007(8) . . ? Ru6 C2 3.277(8) . . ? Fe6 C41 3.099(10) . . ? Fe6 C42 3.195(13) . . ? Fe6 C51 3.471(12) . . ? Fe6 C53 3.422(12) . . ? Fe6 O61 3.024(9) . . ? Fe6 O62 3.051(10) . . ? Fe6 O63 3.007(8) . . ? Fe6 C2 3.277(8) . . ? C11 C12 2.81(2) . . ? C11 C13 2.86(2) . . ? C12 C13 2.80(2) . . ? C12 C1 2.974(14) . . ? C13 C1 2.999(14) . . ? C21 C22 2.78(2) . . ? C21 C23 2.947(14) . . ? C22 C23 2.891(17) . . ? C23 C2 2.973(13) . . ? C31 C32 2.83(2) . . ? C31 C33 2.953(14) . . ? C32 C33 2.867(17) . . ? C32 C1 2.959(17) . . ? C33 C2 2.933(13) . . ? O33 H405 2.668(7) . . ? C41 C42 2.76(2) . . ? C41 C51 2.968(16) . . ? C41 C61 2.810(19) . . ? C41 C402 2.87(2) . . ? O41 C61 2.966(15) . . ? O41 O61 2.981(13) . . ? O41 H402 2.533(10) . '3 666' ? C42 C62 2.993(15) . . ? C42 C4 2.873(15) . . ? C42 C404 2.86(2) . . ? C51 C52 2.820(18) . . ? C51 C53 2.785(17) . . ? C52 C53 2.736(14) . . ? C52 H401 2.634(10) . . ? C53 C3 2.809(14) . . ? C61 C62 2.897(18) . . ? C61 C63 2.697(17) . . ? O61 H404 2.537(9) . '1 455' ? C62 C63 2.827(15) . . ? C63 C3 2.762(13) . . ? C1 C3 2.604(10) . . ? C2 C4 2.617(10) . . ? C401 C403 2.22(2) . . ? C401 C404 2.24(2) . . ? C401 H402 2.057(16) . . ? C401 H405 2.163(16) . . ? C402 C404 2.28(2) . . ? C402 C405 2.30(2) . . ? C402 H401 2.020(15) . . ? C402 H403 2.140(16) . . ? C403 C405 2.26(2) . . ? C403 H402 2.132(17) . . ? C403 H404 2.098(16) . . ? C404 H403 2.121(15) . . ? C404 H405 2.083(15) . . ? C405 H401 2.170(17) . . ? C405 H404 2.048(16) . . ? _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 ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 11 8 -4 -11 -8 4 -11 8 -4 11 -8 6 0 0 -6 0 0 0 22 0 0 -22 0 0 0 14 0 0 -14 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 29 _reflns_limit_l_min -19 _reflns_limit_l_max 19 _reflns_number_observed ? _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI .067 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'single counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type F _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .062 _refine_ls_wR_factor_all .052 _refine_ls_goodness_of_fit_all 1.473 _refine_ls_shift/su_mean .0065 #========================================================================== # 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_br551 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C26 H6 Co2 O17 Ru3 W1' _chemical_formula_moiety ? _chemical_formula_weight 1195.24 _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 21.830(11) _cell_length_b 9.293(4) _cell_length_c 8.991(5) _cell_angle_alpha 111.73(4) _cell_angle_beta 98.27(4) _cell_angle_gamma 97.96(4) _cell_volume 1639.9(16) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 2.421 _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 10.9 _cell_measurement_theta_max 14.3 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 5.902 _exptl_crystal_description fragment _exptl_crystal_size_max .55 _exptl_crystal_size_mid .33 _exptl_crystal_size_min .12 _exptl_crystal_size_rad ? _exptl_crystal_colour black _diffrn_measurement_device_type ; ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .16 _exptl_absorpt_correction_T_max .49 _diffrn_reflns_number 5744 _reflns_number_total ? _reflns_Friedel_coverage ? _reflns_number_gt ? _reflns_threshold_expression 'F > .00 sig(F )' _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 10 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef ? #<< use NfA code _refine_ls_R_factor_gt ? _refine_ls_wR_factor_ref ? _refine_ls_goodness_of_fit_ref ? _refine_ls_number_reflns ? _refine_ls_number_parameters ? _refine_ls_weighting_scheme ? _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? #<< use NfA code _refine_ls_shift/su_max ? _refine_diff_density_min ? _refine_diff_density_max ? _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 _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 52 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 34 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 12 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 6 -1.42 .835999 'Int Tables Vol IV Tables 2.2B and 2.3.1' W ? 0 2 -1.421 6.872 'Int Tables Vol IV Tables 2.2B and 2.3.1' Co ? 0 4 .299011 .973022 '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 .63314(4) .46490(9) .35744(11) .0565(4) Uani ? ? 1.00000 ? ? Co2 .64321(4) .16174(9) .16603(11) .0520(4) Uani ? ? .141(6) ? ? Ru2 .64321(4) .16174(9) .16603(11) .0520(4) Uani ? ? .859(6) ? ? Co3 .61431(6) .21606(14) .44598(18) .0589(7) Uani ? ? .859(6) ? ? Ru3 .61431(6) .21606(14) .44598(18) .0589(7) Uani ? ? .141(6) ? ? W4 .86884(2) .39707(3) .74522(4) .03622(17) Uani ? ? 1.00000 ? ? Co5 .86788(5) .08580(11) .62900(14) .0387(5) Uani ? ? 1.00000 ? ? Ru6 .85534(3) .19451(7) .39201(8) .0399(3) Uani ? ? 1.00000 ? ? C11 .5556(6) .4982(13) .2577(19) .089(7) Uani ? ? 1.00000 ? ? O11 .5094(5) .5128(12) .1952(16) .139(7) Uani ? ? 1.00000 ? ? C12 .6386(5) .6330(14) .5613(18) .075(6) Uani ? ? 1.00000 ? ? O12 .6453(5) .7298(12) .6895(13) .109(6) Uani ? ? 1.00000 ? ? C13 .6826(6) .5824(12) .2704(15) .075(6) Uani ? ? 1.00000 ? ? O13 .7164(5) .6526(10) .2234(13) .112(6) Uani ? ? 1.00000 ? ? C21 .5697(6) .1601(13) .0294(15) .073(6) Uani ? ? 1.00000 ? ? O21 .5250(4) .1539(10) -.0572(13) .108(5) Uani ? ? 1.00000 ? ? C22 .6965(6) .1968(13) .0306(15) .074(6) Uani ? ? 1.00000 ? ? O22 .7286(5) .2202(12) -.0500(12) .111(6) Uani ? ? 1.00000 ? ? C23 .6366(6) -.0619(13) .0856(14) .076(6) Uani ? ? 1.00000 ? ? O23 .6327(5) -.1959(10) .0448(12) .122(6) Uani ? ? 1.00000 ? ? C31 .5377(6) .2324(17) .3806(17) .092(8) Uani ? ? 1.00000 ? ? O31 .4859(5) .2323(15) .3384(17) .154(8) Uani ? ? 1.00000 ? ? C32 .6255(6) .3202(15) .6666(18) .084(7) Uani ? ? 1.00000 ? ? O32 .6296(5) .3860(13) .8049(14) .123(6) Uani ? ? 1.00000 ? ? C33 .6010(6) .0163(15) .4264(18) .093(8) Uani ? ? 1.00000 ? ? O33 .5902(6) -.1138(11) .4089(16) .154(8) Uani ? ? 1.00000 ? ? C41 .9598(5) .3982(10) .7569(12) .056(5) Uani ? ? 1.00000 ? ? O41 1.0138(3) .4073(8) .7638(11) .086(4) Uani ? ? 1.00000 ? ? C42 .8789(5) .3113(9) .9159(11) .049(4) Uani ? ? 1.00000 ? ? O42 .8852(4) .2799(8) 1.0277(9) .078(4) Uani ? ? 1.00000 ? ? C51 .9391(5) .0629(10) .7331(13) .057(5) Uani ? ? 1.00000 ? ? O51 .9827(4) .0491(9) .8109(11) .096(5) Uani ? ? 1.00000 ? ? C52 .8078(5) -.0476(10) .6554(13) .058(5) Uani ? ? 1.00000 ? ? O52 .7685(4) -.1335(9) .6620(12) .101(5) Uani ? ? 1.00000 ? ? C53 .8758(5) -.0346(11) .4268(13) .061(5) Uani ? ? 1.00000 ? ? O53 .8874(5) -.1479(9) .3365(10) .101(5) Uani ? ? 1.00000 ? ? C61 .9421(5) .2544(12) .3881(14) .066(5) Uani ? ? 1.00000 ? ? O61 .9928(4) .2907(10) .3840(12) .103(5) Uani ? ? 1.00000 ? ? C62 .8289(6) .0442(11) .1658(13) .068(6) Uani ? ? 1.00000 ? ? O62 .8118(5) -.0433(9) .0376(10) .110(5) Uani ? ? 1.00000 ? ? C63 .8370(5) .3721(10) .3510(11) .050(4) Uani ? ? 1.00000 ? ? O63 .8276(4) .4754(7) .3184(9) .072(4) Uani ? ? 1.00000 ? ? C1 .6917(4) .3399(9) .4034(11) .046(4) Uani ? ? 1.00000 ? ? C2 .7100(4) .2106(9) .3968(11) .043(4) Uani ? ? 1.00000 ? ? C3 .7579(4) .1317(9) .4452(11) .040(4) Uani ? ? 1.00000 ? ? C4 .8056(4) .2025(8) .5855(10) .035(3) Uani ? ? 1.00000 ? ? C401 .8712(6) .6439(10) .7321(17) .071(6) Uani ? ? 1.00000 ? ? C402 .8084(5) .5732(10) .7143(14) .067(5) Uani ? ? 1.00000 ? ? C403 .8029(7) .5565(13) .863(2) .092(8) Uani ? ? 1.00000 ? ? C404 .8641(14) .623(2) .963(2) .145(15) Uani ? ? 1.00000 ? ? C405 .9007(7) .6710(13) .887(2) .116(8) Uani ? ? 1.00000 ? ? H2 .747(4) .031(9) .410(11) .05(2) Uiso ? ? 1.00000 ? ? H401 .88972 .66895 .65082 .08300 Uiso ? ? 1.00000 ? ? H402 .77456 .54146 .61707 .08000 Uiso ? ? 1.00000 ? ? H403 .76450 .50935 .88648 .11500 Uiso ? ? 1.00000 ? ? H404 .87387 .62783 1.07218 .18500 Uiso ? ? 1.00000 ? ? H405 .94505 .72044 .93296 .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 .0487(5) .0537(4) .0761(6) .0155(3) .0063(4) .0369(4) Co2 .0519(5) .0519(5) .0523(6) .0046(3) -.0029(4) .0281(4) Ru2 .0519(5) .0519(5) .0523(6) .0046(3) -.0029(4) .0281(4) Co3 .0486(8) .0695(8) .0776(10) .0158(6) .0189(7) .0472(7) Ru3 .0486(8) .0695(8) .0776(10) .0158(6) .0189(7) .0472(7) W4 .0447(2) .03079(17) .0328(2) .00824(13) .00914(16) .01170(14) Co5 .0459(7) .0343(5) .0388(7) .0105(5) .0070(6) .0179(5) Ru6 .0526(4) .0414(3) .0335(4) .0158(3) .0170(3) .0187(3) C11 .060(8) .079(7) .133(13) .022(6) -.002(8) .052(8) O11 .082(7) .126(7) .198(13) .034(5) -.034(7) .069(8) C12 .055(7) .083(8) .105(11) .023(6) .030(7) .049(8) O12 .088(7) .123(7) .097(8) .015(6) .027(6) .021(6) C13 .097(9) .064(6) .081(9) .020(6) .009(7) .049(6) O13 .120(8) .108(6) .149(10) .020(6) .035(7) .096(7) C21 .067(7) .085(7) .075(9) .010(6) .002(7) .047(7) O21 .084(6) .111(7) .120(9) .001(5) -.029(6) .062(6) C22 .078(8) .087(7) .056(8) .009(6) .002(7) .034(6) O22 .106(8) .173(9) .090(7) .030(7) .043(6) .083(7) C23 .090(9) .073(7) .051(8) .015(6) -.007(6) .018(6) O23 .183(11) .069(5) .094(7) .026(6) -.007(7) .023(5) C31 .066(8) .154(12) .098(11) .042(8) .037(8) .082(10) O31 .061(6) .239(13) .231(15) .053(7) .044(8) .159(12) C32 .083(9) .105(9) .084(10) .035(7) .025(8) .053(8) O32 .135(9) .151(9) .086(8) .037(7) .037(8) .043(7) C33 .090(10) .093(9) .124(13) .022(7) .037(9) .068(9) O33 .201(12) .089(7) .193(13) .008(7) .060(11) .079(8) C41 .058(6) .046(5) .061(7) .010(4) .004(5) .023(5) O41 .051(5) .079(5) .110(7) .005(4) -.003(5) .027(5) C42 .069(6) .044(4) .034(6) .009(4) .013(5) .016(4) O42 .120(7) .073(4) .041(5) .017(4) .015(5) .026(4) C51 .060(6) .044(5) .067(7) .019(4) .003(6) .022(5) O51 .082(6) .092(5) .100(7) .028(4) -.027(5) .036(5) C52 .069(7) .044(5) .070(7) .013(5) .005(6) .035(5) O52 .090(6) .087(5) .149(9) -.006(4) .018(6) .085(6) C53 .071(7) .055(5) .052(7) .025(5) .003(6) .016(5) O53 .187(10) .076(5) .061(5) .076(6) .043(6) .025(4) C61 .066(7) .075(6) .080(8) .031(6) .040(7) .044(6) O61 .074(6) .115(6) .145(9) .024(5) .058(6) .066(6) C62 .122(10) .055(5) .036(7) .035(6) .016(7) .021(5) O62 .218(11) .073(5) .032(5) .047(6) .013(6) .011(4) C63 .069(6) .053(5) .042(6) .020(4) .023(5) .027(4) O63 .107(6) .066(4) .067(5) .031(4) .033(5) .044(4) C1 .044(5) .046(4) .047(6) .001(4) .001(4) .024(4) C2 .040(5) .045(4) .038(5) .000(3) -.002(4) .017(4) C3 .044(5) .033(4) .048(6) .008(3) .013(4) .023(4) C4 .040(5) .035(4) .033(5) .007(3) .009(4) .019(3) C401 .077(8) .035(5) .116(11) .018(5) .041(8) .035(6) C402 .066(7) .035(4) .077(9) .024(4) -.009(6) .001(5) C403 .122(12) .049(6) .127(15) .030(7) .086(11) .032(8) C404 .32(3) .072(10) .064(11) .112(16) .079(16) .017(8) C405 .104(11) .040(6) .121(15) .018(6) -.065(11) -.029(7) # 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 Co2 . . 2.7636(15) ? Ru1 Ru2 . . 2.7636(15) ? Ru1 Co3 . . 2.710(2) ? Ru1 Ru3 . . 2.710(2) ? Ru1 C11 . . 1.919(13) ? Ru1 C12 . . 1.892(12) ? Ru1 C13 . . 1.876(14) ? Ru1 C1 . . 1.942(10) ? Co2 Co3 . . 2.568(2) ? Co2 Ru3 . . 2.568(2) ? Co2 C21 . . 1.870(13) ? Co2 C22 . . 1.881(14) ? Co2 C23 . . 1.907(12) ? Co2 C1 . . 2.160(7) ? Co2 C2 . . 2.210(9) ? Ru2 Co3 . . 2.568(2) ? Ru2 Ru3 . . 2.568(2) ? Ru2 C21 . . 1.870(13) ? Ru2 C22 . . 1.881(14) ? Ru2 C23 . . 1.907(12) ? Ru2 C1 . . 2.160(7) ? Ru2 C2 . . 2.210(9) ? Co3 C31 . . 1.738(14) ? Co3 C32 . . 1.818(15) ? Co3 C33 . . 1.776(15) ? Co3 C1 . . 2.073(10) ? Co3 C2 . . 2.200(9) ? Ru3 C31 . . 1.738(14) ? Ru3 C32 . . 1.818(15) ? Ru3 C33 . . 1.776(15) ? Ru3 C1 . . 2.073(10) ? Ru3 C2 . . 2.200(9) ? W4 Co5 . . 2.6830(15) ? W4 Ru6 . . 2.9776(16) ? W4 C41 . . 1.972(11) ? W4 C42 . . 1.974(11) ? W4 C4 . . 2.013(6) ? W4 C401 . . 2.333(12) ? W4 C402 . . 2.307(11) ? W4 C403 . . 2.294(16) ? W4 C404 . . 2.307(17) ? W4 C405 . . 2.332(10) ? Co5 Ru6 . . 2.672(2) ? Co5 C42 . . 2.604(8) ? Co5 C51 . . 1.778(11) ? Co5 C52 . . 1.781(11) ? Co5 C53 . . 1.795(10) ? Co5 C4 . . 1.936(9) ? Ru6 C53 . . 2.355(11) ? Ru6 C61 . . 1.907(12) ? Ru6 C62 . . 1.938(10) ? Ru6 C63 . . 1.901(11) ? Ru6 C3 . . 2.292(9) ? Ru6 C4 . . 2.163(9) ? C11 O11 . . 1.132(18) ? C12 O12 . . 1.143(16) ? C13 O13 . . 1.144(18) ? C21 O21 . . 1.137(16) ? C22 O22 . . 1.132(18) ? C23 O23 . . 1.148(15) ? C31 O31 . . 1.140(17) ? C32 O32 . . 1.149(18) ? C33 O33 . . 1.145(18) ? C41 O41 . . 1.161(13) ? C42 O42 . . 1.142(14) ? C51 O51 . . 1.148(14) ? C52 O52 . . 1.113(14) ? C53 O53 . . 1.154(12) ? C61 O61 . . 1.123(15) ? C62 O62 . . 1.108(12) ? C63 O63 . . 1.138(13) ? C1 C2 . . 1.301(13) ? C2 C3 . . 1.462(13) ? C3 C4 . . 1.388(10) ? C3 H2 . . .86(8) ? C401 C402 . . 1.394(16) ? C401 C405 . . 1.36(2) ? C401 H401 . . .969(16) ? C402 C403 . . 1.42(3) ? C402 H402 . . .980(11) ? C403 C404 . . 1.41(3) ? C403 H403 . . .976(18) ? C404 C405 . . 1.26(3) ? C404 H404 . . .957(18) ? C405 H405 . . .970(14) ? 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 Co2 Ru1 Ru2 . . . .00(10) ? Co2 Ru1 Co3 . . . 55.94(5) ? Co2 Ru1 Ru3 . . . 55.94(5) ? Co2 Ru1 C11 . . . 106.4(3) ? Co2 Ru1 C12 . . . 152.8(5) ? Co2 Ru1 C13 . . . 100.4(3) ? Co2 Ru1 C1 . . . 51.1(2) ? Ru2 Ru1 Co3 . . . 55.94(5) ? Ru2 Ru1 Ru3 . . . 55.94(5) ? Ru2 Ru1 C11 . . . 106.4(3) ? Ru2 Ru1 C12 . . . 152.8(5) ? Ru2 Ru1 C13 . . . 100.4(3) ? Ru2 Ru1 C1 . . . 51.1(2) ? Co3 Ru1 Ru3 . . . .00(7) ? Co3 Ru1 C11 . . . 112.3(4) ? Co3 Ru1 C12 . . . 99.8(5) ? Co3 Ru1 C13 . . . 148.8(4) ? Co3 Ru1 C1 . . . 49.6(3) ? Ru3 Ru1 C11 . . . 112.3(4) ? Ru3 Ru1 C12 . . . 99.8(5) ? Ru3 Ru1 C13 . . . 148.8(4) ? Ru3 Ru1 C1 . . . 49.6(3) ? C11 Ru1 C12 . . . 93.6(5) ? C11 Ru1 C13 . . . 92.8(6) ? C11 Ru1 C1 . . . 155.5(4) ? C12 Ru1 C13 . . . 96.7(6) ? C12 Ru1 C1 . . . 105.1(5) ? C13 Ru1 C1 . . . 100.4(5) ? Ru1 Co2 Co3 . . . 60.97(6) ? Ru1 Co2 Ru3 . . . 60.97(6) ? Ru1 Co2 C21 . . . 84.8(3) ? Ru1 Co2 C22 . . . 102.7(3) ? Ru1 Co2 C23 . . . 161.0(4) ? Ru1 Co2 C1 . . . 44.4(3) ? Ru1 Co2 C2 . . . 78.4(2) ? Co3 Co2 Ru3 . . . .00(7) ? Co3 Co2 C21 . . . 105.3(4) ? Co3 Co2 C22 . . . 152.8(3) ? Co3 Co2 C23 . . . 100.5(4) ? Co3 Co2 C1 . . . 51.1(3) ? Co3 Co2 C2 . . . 54.2(2) ? Ru3 Co2 C21 . . . 105.3(4) ? Ru3 Co2 C22 . . . 152.8(3) ? Ru3 Co2 C23 . . . 100.5(4) ? Ru3 Co2 C1 . . . 51.1(3) ? Ru3 Co2 C2 . . . 54.2(2) ? C21 Co2 C22 . . . 93.8(6) ? C21 Co2 C23 . . . 97.3(5) ? C21 Co2 C1 . . . 128.8(4) ? C21 Co2 C2 . . . 158.2(5) ? C22 Co2 C23 . . . 96.1(5) ? C22 Co2 C1 . . . 101.7(4) ? C22 Co2 C2 . . . 103.3(4) ? C23 Co2 C1 . . . 128.4(5) ? C23 Co2 C2 . . . 94.3(4) ? C1 Co2 C2 . . . 34.6(3) ? Ru1 Ru2 Co3 . . . 60.97(6) ? Ru1 Ru2 Ru3 . . . 60.97(6) ? Ru1 Ru2 C21 . . . 84.8(3) ? Ru1 Ru2 C22 . . . 102.7(3) ? Ru1 Ru2 C23 . . . 161.0(4) ? Ru1 Ru2 C1 . . . 44.4(3) ? Ru1 Ru2 C2 . . . 78.4(2) ? Co3 Ru2 Ru3 . . . .00(7) ? Co3 Ru2 C21 . . . 105.3(4) ? Co3 Ru2 C22 . . . 152.8(3) ? Co3 Ru2 C23 . . . 100.5(4) ? Co3 Ru2 C1 . . . 51.1(3) ? Co3 Ru2 C2 . . . 54.2(2) ? Ru3 Ru2 C21 . . . 105.3(4) ? Ru3 Ru2 C22 . . . 152.8(3) ? Ru3 Ru2 C23 . . . 100.5(4) ? Ru3 Ru2 C1 . . . 51.1(3) ? Ru3 Ru2 C2 . . . 54.2(2) ? C21 Ru2 C22 . . . 93.8(6) ? C21 Ru2 C23 . . . 97.3(5) ? C21 Ru2 C1 . . . 128.8(4) ? C21 Ru2 C2 . . . 158.2(5) ? C22 Ru2 C23 . . . 96.1(5) ? C22 Ru2 C1 . . . 101.7(4) ? C22 Ru2 C2 . . . 103.3(4) ? C23 Ru2 C1 . . . 128.4(5) ? C23 Ru2 C2 . . . 94.3(4) ? C1 Ru2 C2 . . . 34.6(3) ? Ru1 Co3 Co2 . . . 63.09(6) ? Ru1 Co3 Ru2 . . . 63.09(6) ? Ru1 Co3 C31 . . . 77.1(6) ? Ru1 Co3 C32 . . . 100.2(5) ? Ru1 Co3 C33 . . . 158.9(5) ? Ru1 Co3 C1 . . . 45.5(3) ? Ru1 Co3 C2 . . . 79.8(3) ? Co2 Co3 Ru2 . . . .00000 ? Co2 Co3 C31 . . . 93.9(5) ? Co2 Co3 C32 . . . 154.5(5) ? Co2 Co3 C33 . . . 96.5(5) ? Co2 Co3 C1 . . . 54.2(2) ? Co2 Co3 C2 . . . 54.6(2) ? Ru2 Co3 C31 . . . 93.9(5) ? Ru2 Co3 C32 . . . 154.5(5) ? Ru2 Co3 C33 . . . 96.5(5) ? Ru2 Co3 C1 . . . 54.2(2) ? Ru2 Co3 C2 . . . 54.6(2) ? C31 Co3 C32 . . . 101.2(6) ? C31 Co3 C33 . . . 100.7(7) ? C31 Co3 C1 . . . 121.3(6) ? C31 Co3 C2 . . . 147.2(6) ? C32 Co3 C33 . . . 100.7(7) ? C32 Co3 C1 . . . 100.3(5) ? C32 Co3 C2 . . . 105.6(5) ? C33 Co3 C1 . . . 127.5(5) ? C33 Co3 C2 . . . 92.6(5) ? C1 Co3 C2 . . . 35.3(3) ? Ru1 Ru3 Co2 . . . 63.09(6) ? Ru1 Ru3 Ru2 . . . 63.09(6) ? Ru1 Ru3 C31 . . . 77.1(6) ? Ru1 Ru3 C32 . . . 100.2(5) ? Ru1 Ru3 C33 . . . 158.9(5) ? Ru1 Ru3 C1 . . . 45.5(3) ? Ru1 Ru3 C2 . . . 79.8(3) ? Co2 Ru3 Ru2 . . . .00000 ? Co2 Ru3 C31 . . . 93.9(5) ? Co2 Ru3 C32 . . . 154.5(5) ? Co2 Ru3 C33 . . . 96.5(5) ? Co2 Ru3 C1 . . . 54.2(2) ? Co2 Ru3 C2 . . . 54.6(2) ? Ru2 Ru3 C31 . . . 93.9(5) ? Ru2 Ru3 C32 . . . 154.5(5) ? Ru2 Ru3 C33 . . . 96.5(5) ? Ru2 Ru3 C1 . . . 54.2(2) ? Ru2 Ru3 C2 . . . 54.6(2) ? C31 Ru3 C32 . . . 101.2(6) ? C31 Ru3 C33 . . . 100.7(7) ? C31 Ru3 C1 . . . 121.3(6) ? C31 Ru3 C2 . . . 147.2(6) ? C32 Ru3 C33 . . . 100.7(7) ? C32 Ru3 C1 . . . 100.3(5) ? C32 Ru3 C2 . . . 105.6(5) ? C33 Ru3 C1 . . . 127.5(5) ? C33 Ru3 C2 . . . 92.6(5) ? C1 Ru3 C2 . . . 35.3(3) ? Co5 W4 Ru6 . . . 56.04(6) ? Co5 W4 C41 . . . 78.8(2) ? Co5 W4 C42 . . . 66.0(2) ? Co5 W4 C4 . . . 46.0(2) ? Co5 W4 C401 . . . 155.9(4) ? Co5 W4 C402 . . . 140.9(2) ? Co5 W4 C403 . . . 136.2(4) ? Co5 W4 C404 . . . 148.0(5) ? Co5 W4 C405 . . . 162.5(4) ? Ru6 W4 C41 . . . 84.4(3) ? Ru6 W4 C42 . . . 122.0(2) ? Ru6 W4 C4 . . . 46.6(3) ? Ru6 W4 C401 . . . 100.1(3) ? Ru6 W4 C402 . . . 98.1(3) ? Ru6 W4 C403 . . . 127.7(4) ? Ru6 W4 C404 . . . 154.7(5) ? Ru6 W4 C405 . . . 130.4(5) ? C41 W4 C42 . . . 84.2(5) ? C41 W4 C4 . . . 118.7(3) ? C41 W4 C401 . . . 97.2(4) ? C41 W4 C402 . . . 132.0(4) ? C41 W4 C403 . . . 140.3(4) ? C41 W4 C404 . . . 105.3(8) ? C41 W4 C405 . . . 85.5(5) ? C42 W4 C4 . . . 93.0(3) ? C42 W4 C401 . . . 137.7(4) ? C42 W4 C402 . . . 130.0(4) ? C42 W4 C403 . . . 94.0(6) ? C42 W4 C404 . . . 82.7(6) ? C42 W4 C405 . . . 105.0(6) ? C4 W4 C401 . . . 121.7(4) ? C4 W4 C402 . . . 95.0(3) ? C4 W4 C403 . . . 101.0(4) ? C4 W4 C404 . . . 135.2(8) ? C4 W4 C405 . . . 151.5(5) ? C401 W4 C402 . . . 35.0(4) ? C401 W4 C403 . . . 58.8(6) ? C401 W4 C404 . . . 56.0(6) ? C401 W4 C405 . . . 33.9(6) ? C402 W4 C403 . . . 36.1(6) ? C402 W4 C404 . . . 57.9(7) ? C402 W4 C405 . . . 56.6(5) ? C403 W4 C404 . . . 35.7(8) ? C403 W4 C405 . . . 56.6(5) ? C404 W4 C405 . . . 31.6(8) ? W4 Co5 Ru6 . . . 67.57(6) ? W4 Co5 C42 . . . 43.8(2) ? W4 Co5 C51 . . . 106.9(2) ? W4 Co5 C52 . . . 120.4(3) ? W4 Co5 C53 . . . 126.1(4) ? W4 Co5 C4 . . . 48.42(18) ? Ru6 Co5 C42 . . . 111.4(2) ? Ru6 Co5 C51 . . . 127.1(4) ? Ru6 Co5 C52 . . . 124.9(4) ? Ru6 Co5 C53 . . . 59.9(4) ? Ru6 Co5 C4 . . . 53.1(3) ? C42 Co5 C51 . . . 80.5(4) ? C42 Co5 C52 . . . 95.0(4) ? C42 Co5 C53 . . . 165.5(4) ? C42 Co5 C4 . . . 77.6(3) ? C51 Co5 C52 . . . 103.8(5) ? C51 Co5 C53 . . . 95.8(5) ? C51 Co5 C4 . . . 155.1(3) ? C52 Co5 C53 . . . 99.5(5) ? C52 Co5 C4 . . . 89.9(4) ? C53 Co5 C4 . . . 102.5(4) ? W4 Ru6 Co5 . . . 56.40(4) ? W4 Ru6 C53 . . . 96.9(3) ? W4 Ru6 C61 . . . 95.2(3) ? W4 Ru6 C62 . . . 167.8(4) ? W4 Ru6 C63 . . . 86.2(3) ? W4 Ru6 C3 . . . 75.8(2) ? W4 Ru6 C4 . . . 42.53(16) ? Co5 Ru6 C53 . . . 41.2(3) ? Co5 Ru6 C61 . . . 100.2(4) ? Co5 Ru6 C62 . . . 119.0(4) ? Co5 Ru6 C63 . . . 141.7(3) ? Co5 Ru6 C3 . . . 70.7(3) ? Co5 Ru6 C4 . . . 45.7(2) ? C53 Ru6 C61 . . . 90.0(5) ? C53 Ru6 C62 . . . 81.0(4) ? C53 Ru6 C63 . . . 176.7(3) ? C53 Ru6 C3 . . . 86.1(4) ? C53 Ru6 C4 . . . 80.1(4) ? C61 Ru6 C62 . . . 96.8(5) ? C61 Ru6 C63 . . . 90.5(5) ? C61 Ru6 C3 . . . 169.7(4) ? C61 Ru6 C4 . . . 133.6(4) ? C62 Ru6 C63 . . . 95.7(5) ? C62 Ru6 C3 . . . 92.1(4) ? C62 Ru6 C4 . . . 125.5(4) ? C63 Ru6 C3 . . . 93.8(4) ? C63 Ru6 C4 . . . 101.8(4) ? C3 Ru6 C4 . . . 36.2(3) ? Ru1 C11 O11 . . . 177.7(10) ? Ru1 C12 O12 . . . 174.7(13) ? Ru1 C13 O13 . . . 175.2(12) ? Co2 C21 Ru2 . . . .00000 ? Co2 C21 O21 . . . 177.6(10) ? Ru2 C21 O21 . . . 177.6(10) ? Co2 C22 Ru2 . . . .00000 ? Co2 C22 O22 . . . 179.0(11) ? Ru2 C22 O22 . . . 179.0(11) ? Co2 C23 Ru2 . . . .00(7) ? Co2 C23 O23 . . . 176.7(12) ? Ru2 C23 O23 . . . 176.7(12) ? Co3 C31 Ru3 . . . .00(15) ? Co3 C31 O31 . . . 174.8(16) ? Ru3 C31 O31 . . . 174.8(16) ? Co3 C32 Ru3 . . . .00(7) ? Co3 C32 O32 . . . 176.7(13) ? Ru3 C32 O32 . . . 176.7(13) ? Co3 C33 Ru3 . . . .00(7) ? Co3 C33 O33 . . . 177.2(13) ? Ru3 C33 O33 . . . 177.2(13) ? W4 C41 O41 . . . 176.1(9) ? W4 C42 Co5 . . . 70.2(3) ? W4 C42 O42 . . . 171.8(7) ? Co5 C42 O42 . . . 118.0(6) ? Co5 C51 O51 . . . 174.3(11) ? Co5 C52 O52 . . . 175.6(10) ? Co5 C53 Ru6 . . . 78.9(4) ? Co5 C53 O53 . . . 150.5(11) ? Ru6 C53 O53 . . . 130.4(10) ? Ru6 C61 O61 . . . 178.8(13) ? Ru6 C62 O62 . . . 177.6(12) ? Ru6 C63 O63 . . . 175.9(9) ? Ru1 C1 Co2 . . . 84.5(3) ? Ru1 C1 Ru2 . . . 84.5(3) ? Ru1 C1 Co3 . . . 84.8(3) ? Ru1 C1 Ru3 . . . 84.8(3) ? Ru1 C1 C2 . . . 155.8(6) ? Co2 C1 Ru2 . . . .00000 ? Co2 C1 Co3 . . . 74.7(2) ? Co2 C1 Ru3 . . . 74.7(2) ? Co2 C1 C2 . . . 74.8(5) ? Ru2 C1 Co3 . . . 74.7(2) ? Ru2 C1 Ru3 . . . 74.7(2) ? Ru2 C1 C2 . . . 74.8(5) ? Co3 C1 Ru3 . . . .00(12) ? Co3 C1 C2 . . . 77.7(6) ? Ru3 C1 C2 . . . 77.7(6) ? Co2 C2 Ru2 . . . .00(12) ? Co2 C2 Co3 . . . 71.2(3) ? Co2 C2 Ru3 . . . 71.2(3) ? Co2 C2 C1 . . . 70.6(5) ? Co2 C2 C3 . . . 134.4(5) ? Ru2 C2 Co3 . . . 71.2(3) ? Ru2 C2 Ru3 . . . 71.2(3) ? Ru2 C2 C1 . . . 70.6(5) ? Ru2 C2 C3 . . . 134.4(5) ? Co3 C2 Ru3 . . . .00(12) ? Co3 C2 C1 . . . 67.0(6) ? Co3 C2 C3 . . . 130.1(7) ? Ru3 C2 C1 . . . 67.0(6) ? Ru3 C2 C3 . . . 130.1(7) ? C1 C2 C3 . . . 150.1(7) ? Ru6 C3 C2 . . . 115.3(7) ? Ru6 C3 C4 . . . 66.9(5) ? Ru6 C3 H2 . . . 109(6) ? C2 C3 C4 . . . 124.4(7) ? C2 C3 H2 . . . 115(6) ? C4 C3 H2 . . . 115(6) ? W4 C4 Co5 . . . 85.6(3) ? W4 C4 Ru6 . . . 90.9(3) ? W4 C4 C3 . . . 148.9(7) ? Co5 C4 Ru6 . . . 81.2(3) ? Co5 C4 C3 . . . 119.8(5) ? Ru6 C4 C3 . . . 77.0(6) ? W4 C401 C402 . . . 71.5(6) ? W4 C401 C405 . . . 73.0(8) ? W4 C401 H401 . . . 120.7(8) ? C402 C401 C405 . . . 106.0(14) ? C402 C401 H401 . . . 126.8(13) ? C405 C401 H401 . . . 127.2(13) ? W4 C402 C401 . . . 73.6(7) ? W4 C402 C403 . . . 71.5(8) ? W4 C402 H402 . . . 120.7(6) ? C401 C402 C403 . . . 107.3(11) ? C401 C402 H402 . . . 126.1(14) ? C403 C402 H402 . . . 126.6(12) ? W4 C403 C402 . . . 72.5(8) ? W4 C403 C404 . . . 72.7(11) ? W4 C403 H403 . . . 119.2(9) ? C402 C403 C404 . . . 103.9(15) ? C402 C403 H403 . . . 126.0(15) ? C404 C403 H403 . . . 130(2) ? W4 C404 C403 . . . 71.6(8) ? W4 C404 C405 . . . 75.3(11) ? W4 C404 H404 . . . 119.7(16) ? C403 C404 C405 . . . 110.2(17) ? C403 C404 H404 . . . 122(3) ? C405 C404 H404 . . . 128(3) ? W4 C405 C401 . . . 73.1(6) ? W4 C405 C404 . . . 73.1(8) ? W4 C405 H405 . . . 120.8(10) ? C401 C405 C404 . . . 112.5(15) ? C401 C405 H405 . . . 124(2) ? C404 C405 H405 . . . 124(2) ? 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 ? ? ? ? ? ? _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 1116 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 11 8 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min ? _reflns_limit_h_max ? _reflns_limit_k_min ? _reflns_limit_k_max ? _reflns_limit_l_min ? _reflns_limit_l_max ? _reflns_number_observed ? _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 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type ? _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_wR_factor_all ? _refine_ls_goodness_of_fit_all ? _refine_ls_shift/su_mean ? #========================================================================== # 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_br552 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C26 H6 Fe2 O17 Ru3 W1' _chemical_formula_moiety ? _chemical_formula_weight 1189.12 _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 8.442(2) _cell_length_b 23.940(5) _cell_length_c 16.422(3) _cell_angle_alpha 90.00000 _cell_angle_beta 90.941(5) _cell_angle_gamma 90.00000 _cell_volume 3318.5(12) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.38 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6865 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 5.71 _exptl_crystal_description rod _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid .09 _exptl_crystal_size_min .065 _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 0.587 _exptl_absorpt_correction_T_max 0.831 _diffrn_reflns_number 36381 _reflns_number_total 8324 _reflns_Friedel_coverage ? _reflns_number_gt 5403 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.19 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .039 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .039 _refine_ls_wR_factor_ref .042 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_number_reflns 5403 _refine_ls_number_parameters 469 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .02 _refine_diff_density_min -.739 _refine_diff_density_max 1.563 _refine_ls_extinction_method none _refine_ls_extinction_coef .00000 _refine_ls_abs_structure_details none _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 ? 0 104 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 68 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 24 0 0 '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' W ? 0 4 -1.421 6.872 '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' 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 .77164(9) .07580(3) .60820(5) .0465(5) Uani ? ? .554(6) ? ? Fe1 .77164(9) .07580(3) .60820(5) .0465(5) Uani ? ? .446(6) ? ? Ru2 .89818(7) .15853(2) .71087(3) .0403(3) Uani ? ? 1.00000 ? ? Ru3 .96108(7) .16101(2) .54480(3) .0392(3) Uani ? ? 1.00000 ? ? W4 .74267(4) .397398(12) .609177(19) .04562(18) Uani ? ? 1.00000 ? ? Ru5 .60165(11) .30781(4) .51799(5) .0381(6) Uani ? ? .083(6) ? ? Fe5 .60165(11) .30781(4) .51799(5) .0381(6) Uani ? ? .917(6) ? ? Ru6 .54307(9) .30564(3) .66958(4) .0399(5) Uani ? ? .364(6) ? ? Fe6 .54307(9) .30564(3) .66958(4) .0399(5) Uani ? ? .636(6) ? ? C1 .7355(8) .1522(3) .6065(4) .040(4) Uani ? ? 1.00000 ? ? C2 .7747(8) .2057(3) .6117(3) .034(4) Uani ? ? 1.00000 ? ? C3 .7254(8) .2625(3) .6057(4) .037(4) Uani ? ? 1.00000 ? ? C4 .7635(7) .3154(3) .6122(3) .033(4) Uani ? ? 1.00000 ? ? C11 .9201(12) .0195(4) .6215(6) .075(7) Uani ? ? 1.00000 ? ? O11 1.0158(10) -.0135(3) .6315(5) .117(7) Uani ? ? 1.00000 ? ? C12 .6862(11) .0494(4) .5111(6) .065(6) Uani ? ? 1.00000 ? ? O12 .6281(9) .0368(3) .4512(4) .095(5) Uani ? ? 1.00000 ? ? C13 .6203(13) .0459(4) .6739(6) .074(7) Uani ? ? 1.00000 ? ? O13 .5194(10) .0298(3) .7141(5) .108(6) Uani ? ? 1.00000 ? ? C21 1.0308(12) .1052(4) .7666(5) .063(6) Uani ? ? 1.00000 ? ? O21 1.1119(9) .0746(3) .7994(4) .102(6) Uani ? ? 1.00000 ? ? C22 .7298(11) .1516(3) .7876(5) .060(5) Uani ? ? 1.00000 ? ? O22 .6296(8) .1460(3) .8313(4) .094(5) Uani ? ? 1.00000 ? ? C23 .9863(10) .2268(4) .7555(5) .056(5) Uani ? ? 1.00000 ? ? O23 1.0353(9) .2675(3) .7794(4) .089(5) Uani ? ? 1.00000 ? ? C31 1.1282(11) .1104(3) .5161(5) .062(6) Uani ? ? 1.00000 ? ? O31 1.2297(9) .0818(3) .5000(5) .103(6) Uani ? ? 1.00000 ? ? C32 .8629(10) .1567(3) .4389(5) .057(5) Uani ? ? 1.00000 ? ? O32 .8003(8) .1541(3) .3784(4) .088(5) Uani ? ? 1.00000 ? ? C33 1.0696(10) .2315(3) .5244(4) .050(5) Uani ? ? 1.00000 ? ? O33 1.1228(7) .2738(3) .5160(4) .070(4) Uani ? ? 1.00000 ? ? C41 .5321(12) .4329(4) .6262(5) .070(6) Uani ? ? 1.00000 ? ? O41 .4213(9) .4597(3) .6333(5) .103(6) Uani ? ? 1.00000 ? ? C42 .7821(13) .4030(4) .7294(6) .077(7) Uani ? ? 1.00000 ? ? O42 .8112(12) .4075(3) .7972(4) .122(7) Uani ? ? 1.00000 ? ? C51 .4611(10) .3591(4) .4864(5) .055(5) Uani ? ? 1.00000 ? ? O51 .3696(8) .3913(3) .4635(4) .084(5) Uani ? ? 1.00000 ? ? C52 .7317(9) .3060(3) .4316(5) .051(5) Uani ? ? 1.00000 ? ? O52 .8109(8) .3038(3) .3760(4) .084(5) Uani ? ? 1.00000 ? ? C53 .4941(9) .2459(4) .4892(4) .049(5) Uani ? ? 1.00000 ? ? O53 .4322(8) .2063(3) .4699(4) .079(5) Uani ? ? 1.00000 ? ? C61 .3553(12) .3427(4) .6802(5) .071(6) Uani ? ? 1.00000 ? ? O61 .2350(9) .3627(3) .6863(5) .112(6) Uani ? ? 1.00000 ? ? C62 .6080(10) .3002(3) .7776(5) .055(5) Uani ? ? 1.00000 ? ? O62 .6477(8) .2945(3) .8436(3) .088(5) Uani ? ? 1.00000 ? ? C63 .4393(11) .2394(4) .6687(5) .059(5) Uani ? ? 1.00000 ? ? O63 .3792(8) .1972(3) .6705(4) .082(5) Uani ? ? 1.00000 ? ? C401 .8498(16) .4293(5) .4859(7) .086(8) Uani ? ? 1.00000 ? ? C402 .7758(14) .4737(5) .5222(8) .085(8) Uani ? ? 1.00000 ? ? C403 .8563(14) .4853(4) .5956(8) .081(7) Uani ? ? 1.00000 ? ? C404 .9746(13) .4466(5) .6070(8) .077(8) Uani ? ? 1.00000 ? ? C405 .9772(14) .4122(5) .5385(8) .081(8) Uani ? ? 1.00000 ? ? H0 1.074(9) .158(3) .645(4) .07(2) Uiso ? ? 1.00000 ? ? H401 .815(6) .405(2) .442(3) .009(13) Uiso ? ? 1.00000 ? ? H402 .668(14) .501(5) .518(7) .14(4) Uiso ? ? 1.00000 ? ? H403 .815(8) .511(3) .628(4) .05(2) Uiso ? ? 1.00000 ? ? H404 1.030(13) .445(5) .650(6) .11(4) Uiso ? ? 1.00000 ? ? H405 1.032(11) .384(4) .537(5) .08(3) 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 .0524(6) .0313(4) .0558(5) -.0026(3) .0018(4) -.0010(3) Fe1 .0524(6) .0313(4) .0558(5) -.0026(3) .0018(4) -.0010(3) Ru2 .0457(4) .0382(3) .0369(3) .0042(3) -.0024(2) .0036(2) Ru3 .0404(3) .0374(3) .0398(3) .0007(3) .0042(2) -.0030(2) W4 .0529(2) .03251(16) .0511(2) .00246(15) -.00998(14) .00246(14) Ru5 .0391(6) .0422(6) .0330(6) .0021(4) -.0036(4) .0041(4) Fe5 .0391(6) .0422(6) .0330(6) .0021(4) -.0036(4) .0041(4) Ru6 .0397(5) .0467(6) .0333(5) .0098(4) .0020(3) .0019(3) Fe6 .0397(5) .0467(6) .0333(5) .0098(4) .0020(3) .0019(3) C1 .039(4) .045(4) .035(4) -.009(3) -.004(3) .003(3) C2 .038(4) .036(4) .028(3) -.001(3) -.003(3) -.001(3) C3 .040(4) .040(4) .030(3) .001(3) .006(3) .001(3) C4 .023(3) .047(4) .030(3) -.001(3) .001(3) .002(3) C11 .071(7) .060(6) .095(7) .008(5) -.006(6) -.013(5) O11 .099(6) .077(6) .173(8) .029(5) -.001(6) -.011(5) C12 .068(6) .048(5) .080(7) -.009(4) .005(5) -.005(5) O12 .111(6) .091(6) .084(5) -.024(4) -.012(4) -.019(4) C13 .092(8) .050(5) .080(7) -.001(5) -.010(6) .009(5) O13 .121(7) .096(6) .108(6) -.025(5) .039(5) .021(4) C21 .088(7) .048(5) .054(5) .006(5) -.005(5) .001(4) O21 .122(7) .081(5) .100(5) .035(5) -.036(5) .022(4) C22 .070(6) .063(6) .047(5) .009(5) .004(4) .013(4) O22 .090(5) .118(6) .075(5) .019(4) .038(4) .024(4) C23 .061(6) .062(6) .045(5) .004(4) -.005(4) -.003(4) O23 .114(6) .068(5) .083(5) -.014(4) -.023(4) -.017(4) C31 .063(6) .052(5) .072(6) .008(4) .019(5) .000(4) O31 .088(5) .073(5) .149(7) .028(4) .036(5) -.015(4) C32 .067(6) .060(5) .044(5) -.008(4) .016(4) -.001(4) O32 .093(5) .126(6) .044(4) -.020(4) -.013(3) .003(4) C33 .056(5) .050(5) .044(4) .002(4) .003(4) -.002(4) O33 .061(4) .053(4) .097(5) -.013(3) .014(3) -.002(3) C41 .081(7) .049(5) .079(6) .012(5) .001(5) -.006(4) O41 .084(5) .076(5) .149(7) .038(4) -.000(5) -.014(4) C42 .119(9) .044(5) .069(6) -.013(5) -.007(6) -.002(4) O42 .210(10) .099(6) .057(4) -.034(6) -.035(5) -.009(4) C51 .064(6) .056(5) .046(4) .007(4) .001(4) .003(4) O51 .083(5) .093(5) .076(4) .037(4) -.025(4) .000(4) C52 .052(5) .058(5) .042(4) -.006(4) -.006(4) .003(4) O52 .078(5) .119(6) .057(4) -.013(4) .028(3) -.006(4) C53 .044(5) .063(5) .040(4) -.003(4) -.005(3) -.001(4) O53 .078(5) .084(5) .074(4) -.023(4) -.014(3) -.011(3) C61 .066(6) .078(7) .069(6) .022(5) .001(5) .017(5) O61 .085(5) .113(6) .139(7) .049(5) .017(5) .040(5) C62 .049(5) .062(5) .053(5) .008(4) .007(4) -.002(4) O62 .092(5) .132(6) .040(3) .015(4) -.006(3) .008(4) C63 .062(6) .066(6) .049(5) .001(5) .007(4) .004(4) O63 .066(4) .089(5) .092(5) -.018(4) .005(4) .007(4) C401 .116(10) .071(8) .070(7) -.048(7) -.002(6) .012(6) C402 .082(8) .061(7) .111(9) -.011(6) -.016(7) .033(6) C403 .091(8) .031(5) .122(9) .000(5) -.008(7) -.000(5) C404 .070(7) .063(7) .097(9) -.014(5) -.004(6) .013(6) C405 .068(7) .052(7) .124(10) .003(5) .031(7) .015(7) # 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 . . 2.8013(10) ? Ru1 Ru3 . . 2.8032(10) ? Ru1 C1 . . 1.855(7) ? Ru1 C11 . . 1.851(10) ? Ru1 C12 . . 1.850(10) ? Ru1 C13 . . 1.831(10) ? Fe1 Ru2 . . 2.8013(10) ? Fe1 Ru3 . . 2.8032(10) ? Fe1 C1 . . 1.855(7) ? Fe1 C11 . . 1.851(10) ? Fe1 C12 . . 1.850(10) ? Fe1 C13 . . 1.831(10) ? Ru2 Ru3 . . 2.7876(9) ? Ru2 C1 . . 2.184(6) ? Ru2 C2 . . 2.227(6) ? Ru2 C21 . . 1.921(9) ? Ru2 C22 . . 1.922(9) ? Ru2 C23 . . 1.934(9) ? Ru2 H0 . . 1.85(7) ? Ru3 C1 . . 2.182(7) ? Ru3 C2 . . 2.211(6) ? Ru3 C31 . . 1.925(9) ? Ru3 C32 . . 1.917(8) ? Ru3 C33 . . 1.951(8) ? Ru3 H0 . . 1.89(7) ? W4 Ru5 . . 2.8637(10) ? W4 Fe5 . . 2.8637(10) ? W4 Ru6 . . 2.9501(9) ? W4 Fe6 . . 2.9501(9) ? W4 C4 . . 1.972(7) ? W4 C41 . . 1.994(10) ? W4 C42 . . 2.001(10) ? W4 C401 . . 2.358(11) ? W4 C402 . . 2.339(12) ? W4 C403 . . 2.324(10) ? W4 C404 . . 2.285(11) ? W4 C405 . . 2.338(12) ? Ru5 Ru6 . . 2.5465(12) ? Ru5 Fe6 . . 2.5465(12) ? Ru5 C3 . . 2.072(6) ? Ru5 C4 . . 2.056(6) ? Ru5 C51 . . 1.780(9) ? Ru5 C52 . . 1.808(8) ? Ru5 C53 . . 1.797(8) ? Fe5 Ru6 . . 2.5465(12) ? Fe5 Fe6 . . 2.5465(12) ? Fe5 C3 . . 2.072(6) ? Fe5 C4 . . 2.056(6) ? Fe5 C51 . . 1.780(9) ? Fe5 C52 . . 1.808(8) ? Fe5 C53 . . 1.797(8) ? Ru6 C3 . . 2.143(7) ? Ru6 C4 . . 2.112(6) ? Ru6 C61 . . 1.827(10) ? Ru6 C62 . . 1.853(8) ? Ru6 C63 . . 1.812(9) ? Fe6 C3 . . 2.143(7) ? Fe6 C4 . . 2.112(6) ? Fe6 C61 . . 1.827(10) ? Fe6 C62 . . 1.853(8) ? Fe6 C63 . . 1.812(9) ? C1 C2 . . 1.325(10) ? C2 C3 . . 1.425(9) ? C3 C4 . . 1.310(10) ? C11 O11 . . 1.139(13) ? C12 O12 . . 1.133(12) ? C13 O13 . . 1.153(13) ? C21 O21 . . 1.132(12) ? C22 O22 . . 1.126(11) ? C23 O23 . . 1.128(11) ? C31 O31 . . 1.131(11) ? C32 O32 . . 1.120(10) ? C33 O33 . . 1.118(10) ? C41 O41 . . 1.141(12) ? C42 O42 . . 1.141(12) ? C51 O51 . . 1.150(11) ? C52 O52 . . 1.142(10) ? C53 O53 . . 1.125(11) ? C61 O61 . . 1.130(13) ? C62 O62 . . 1.138(10) ? C63 O63 . . 1.132(12) ? C401 C402 . . 1.375(17) ? C401 C405 . . 1.428(17) ? C401 H401 . . .96(5) ? C402 C403 . . 1.402(17) ? C402 H402 . . 1.12(12) ? C403 C404 . . 1.373(15) ? C403 H403 . . .89(7) ? C404 C405 . . 1.394(18) ? C404 H404 . . .84(10) ? C405 H405 . . .82(9) ? 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 . . . 59.65(2) ? Ru2 Ru1 C1 . . . 51.1(2) ? Ru2 Ru1 C11 . . . 101.1(3) ? Ru2 Ru1 C12 . . . 154.1(3) ? Ru2 Ru1 C13 . . . 100.6(3) ? Ru3 Ru1 C1 . . . 51.0(2) ? Ru3 Ru1 C11 . . . 100.6(3) ? Ru3 Ru1 C12 . . . 98.3(3) ? Ru3 Ru1 C13 . . . 155.7(3) ? C1 Ru1 C11 . . . 146.2(4) ? C1 Ru1 C12 . . . 105.2(3) ? C1 Ru1 C13 . . . 106.2(4) ? C11 Ru1 C12 . . . 96.1(4) ? C11 Ru1 C13 . . . 97.1(4) ? C12 Ru1 C13 . . . 96.2(4) ? Ru2 Fe1 Ru3 . . . 59.65(2) ? Ru2 Fe1 C1 . . . 51.1(2) ? Ru2 Fe1 C11 . . . 101.1(3) ? Ru2 Fe1 C12 . . . 154.1(3) ? Ru2 Fe1 C13 . . . 100.6(3) ? Ru3 Fe1 C1 . . . 51.0(2) ? Ru3 Fe1 C11 . . . 100.6(3) ? Ru3 Fe1 C12 . . . 98.3(3) ? Ru3 Fe1 C13 . . . 155.7(3) ? C1 Fe1 C11 . . . 146.2(4) ? C1 Fe1 C12 . . . 105.2(3) ? C1 Fe1 C13 . . . 106.2(4) ? C11 Fe1 C12 . . . 96.1(4) ? C11 Fe1 C13 . . . 97.1(4) ? C12 Fe1 C13 . . . 96.2(4) ? Ru1 Ru2 Fe1 . . . .00(10) ? Ru1 Ru2 Ru3 . . . 60.21(2) ? Ru1 Ru2 C1 . . . 41.42(18) ? Ru1 Ru2 C2 . . . 75.49(16) ? Ru1 Ru2 C21 . . . 91.7(3) ? Ru1 Ru2 C22 . . . 93.1(2) ? Ru1 Ru2 C23 . . . 164.9(2) ? Ru1 Ru2 H0 . . . 87(2) ? Fe1 Ru2 Ru3 . . . 60.21(2) ? Fe1 Ru2 C1 . . . 41.42(18) ? Fe1 Ru2 C2 . . . 75.49(16) ? Fe1 Ru2 C21 . . . 91.7(3) ? Fe1 Ru2 C22 . . . 93.1(2) ? Fe1 Ru2 C23 . . . 164.9(2) ? Fe1 Ru2 H0 . . . 87(2) ? Ru3 Ru2 C1 . . . 50.28(17) ? Ru3 Ru2 C2 . . . 50.83(16) ? Ru3 Ru2 C21 . . . 111.2(3) ? Ru3 Ru2 C22 . . . 142.9(3) ? Ru3 Ru2 C23 . . . 105.9(2) ? Ru3 Ru2 H0 . . . 42(2) ? C1 Ru2 C2 . . . 35.0(2) ? C1 Ru2 C21 . . . 133.0(3) ? C1 Ru2 C22 . . . 92.6(3) ? C1 Ru2 C23 . . . 126.1(3) ? C1 Ru2 H0 . . . 92(2) ? C2 Ru2 C21 . . . 161.5(3) ? C2 Ru2 C22 . . . 100.4(3) ? C2 Ru2 C23 . . . 91.2(3) ? C2 Ru2 H0 . . . 87(2) ? C21 Ru2 C22 . . . 93.5(4) ? C21 Ru2 C23 . . . 99.4(4) ? C21 Ru2 H0 . . . 79(2) ? C22 Ru2 C23 . . . 96.3(3) ? C22 Ru2 H0 . . . 172(2) ? C23 Ru2 H0 . . . 85(2) ? Ru1 Ru3 Fe1 . . . .00000 ? Ru1 Ru3 Ru2 . . . 60.14(2) ? Ru1 Ru3 C1 . . . 41.39(18) ? Ru1 Ru3 C2 . . . 75.68(17) ? Ru1 Ru3 C31 . . . 93.3(3) ? Ru1 Ru3 C32 . . . 93.2(3) ? Ru1 Ru3 C33 . . . 164.8(2) ? Ru1 Ru3 H0 . . . 86(2) ? Fe1 Ru3 Ru2 . . . 60.14(2) ? Fe1 Ru3 C1 . . . 41.39(18) ? Fe1 Ru3 C2 . . . 75.68(17) ? Fe1 Ru3 C31 . . . 93.3(3) ? Fe1 Ru3 C32 . . . 93.2(3) ? Fe1 Ru3 C33 . . . 164.8(2) ? Fe1 Ru3 H0 . . . 86(2) ? Ru2 Ru3 C1 . . . 50.35(17) ? Ru2 Ru3 C2 . . . 51.34(15) ? Ru2 Ru3 C31 . . . 112.2(3) ? Ru2 Ru3 C32 . . . 143.1(3) ? Ru2 Ru3 C33 . . . 106.5(2) ? Ru2 Ru3 H0 . . . 41(2) ? C1 Ru3 C2 . . . 35.1(2) ? C1 Ru3 C31 . . . 134.6(3) ? C1 Ru3 C32 . . . 92.8(3) ? C1 Ru3 C33 . . . 125.4(3) ? C1 Ru3 H0 . . . 91(2) ? C2 Ru3 C31 . . . 163.2(3) ? C2 Ru3 C32 . . . 100.2(3) ? C2 Ru3 C33 . . . 90.4(3) ? C2 Ru3 H0 . . . 86(2) ? C31 Ru3 C32 . . . 92.9(4) ? C31 Ru3 C33 . . . 98.9(4) ? C31 Ru3 H0 . . . 80(2) ? C32 Ru3 C33 . . . 95.1(3) ? C32 Ru3 H0 . . . 173(2) ? C33 Ru3 H0 . . . 87(2) ? Ru5 W4 Fe5 . . . .00(10) ? Ru5 W4 Ru6 . . . 51.93(3) ? Ru5 W4 Fe6 . . . 51.93(3) ? Ru5 W4 C4 . . . 45.87(17) ? Ru5 W4 C41 . . . 91.7(3) ? Ru5 W4 C42 . . . 128.8(3) ? Ru5 W4 C401 . . . 87.4(3) ? Ru5 W4 C402 . . . 108.6(3) ? Ru5 W4 C403 . . . 142.8(3) ? Ru5 W4 C404 . . . 136.6(3) ? Ru5 W4 C405 . . . 101.7(3) ? Fe5 W4 Ru6 . . . 51.93(3) ? Fe5 W4 Fe6 . . . 51.93(3) ? Fe5 W4 C4 . . . 45.87(17) ? Fe5 W4 C41 . . . 91.7(3) ? Fe5 W4 C42 . . . 128.8(3) ? Fe5 W4 C401 . . . 87.4(3) ? Fe5 W4 C402 . . . 108.6(3) ? Fe5 W4 C403 . . . 142.8(3) ? Fe5 W4 C404 . . . 136.6(3) ? Fe5 W4 C405 . . . 101.7(3) ? Ru6 W4 Fe6 . . . .00000 ? Ru6 W4 C4 . . . 45.67(17) ? Ru6 W4 C41 . . . 75.8(3) ? Ru6 W4 C42 . . . 78.7(3) ? Ru6 W4 C401 . . . 139.4(3) ? Ru6 W4 C402 . . . 149.5(3) ? Ru6 W4 C403 . . . 160.9(3) ? Ru6 W4 C404 . . . 152.0(3) ? Ru6 W4 C405 . . . 140.6(3) ? Fe6 W4 C4 . . . 45.67(17) ? Fe6 W4 C41 . . . 75.8(3) ? Fe6 W4 C42 . . . 78.7(3) ? Fe6 W4 C401 . . . 139.4(3) ? Fe6 W4 C402 . . . 149.5(3) ? Fe6 W4 C403 . . . 160.9(3) ? Fe6 W4 C404 . . . 152.0(3) ? Fe6 W4 C405 . . . 140.6(3) ? C4 W4 C41 . . . 120.0(3) ? C4 W4 C42 . . . 91.6(3) ? C4 W4 C401 . . . 108.0(3) ? C4 W4 C402 . . . 141.4(3) ? C4 W4 C403 . . . 150.1(3) ? C4 W4 C404 . . . 115.9(3) ? C4 W4 C405 . . . 95.0(3) ? C41 W4 C42 . . . 88.1(4) ? C41 W4 C401 . . . 109.8(4) ? C41 W4 C402 . . . 82.4(4) ? C41 W4 C403 . . . 89.9(4) ? C41 W4 C404 . . . 123.3(4) ? C41 W4 C405 . . . 140.3(4) ? C42 W4 C401 . . . 139.9(4) ? C42 W4 C402 . . . 122.0(4) ? C42 W4 C403 . . . 88.4(4) ? C42 W4 C404 . . . 81.5(4) ? C42 W4 C405 . . . 110.5(4) ? C401 W4 C402 . . . 34.0(4) ? C401 W4 C403 . . . 57.3(4) ? C401 W4 C404 . . . 58.6(4) ? C401 W4 C405 . . . 35.4(4) ? C402 W4 C403 . . . 35.0(4) ? C402 W4 C404 . . . 58.5(4) ? C402 W4 C405 . . . 57.8(4) ? C403 W4 C404 . . . 34.7(4) ? C403 W4 C405 . . . 57.4(4) ? C404 W4 C405 . . . 35.1(4) ? W4 Ru5 Ru6 . . . 65.78(3) ? W4 Ru5 Fe6 . . . 65.78(3) ? W4 Ru5 C3 . . . 80.10(19) ? W4 Ru5 C4 . . . 43.5(2) ? W4 Ru5 C51 . . . 84.5(3) ? W4 Ru5 C52 . . . 100.1(2) ? W4 Ru5 C53 . . . 163.6(2) ? Ru6 Ru5 Fe6 . . . .00(10) ? Ru6 Ru5 C3 . . . 54.11(18) ? Ru6 Ru5 C4 . . . 53.36(17) ? Ru6 Ru5 C51 . . . 99.2(3) ? Ru6 Ru5 C52 . . . 153.7(2) ? Ru6 Ru5 C53 . . . 97.8(2) ? Fe6 Ru5 C3 . . . 54.11(18) ? Fe6 Ru5 C4 . . . 53.36(17) ? Fe6 Ru5 C51 . . . 99.2(3) ? Fe6 Ru5 C52 . . . 153.7(2) ? Fe6 Ru5 C53 . . . 97.8(2) ? C3 Ru5 C4 . . . 37.0(3) ? C3 Ru5 C51 . . . 152.9(3) ? C3 Ru5 C52 . . . 103.1(3) ? C3 Ru5 C53 . . . 89.9(3) ? C4 Ru5 C51 . . . 126.2(3) ? C4 Ru5 C52 . . . 100.8(3) ? C4 Ru5 C53 . . . 126.7(3) ? C51 Ru5 C52 . . . 101.4(4) ? C51 Ru5 C53 . . . 99.3(4) ? C52 Ru5 C53 . . . 94.8(3) ? W4 Fe5 Ru6 . . . 65.78(3) ? W4 Fe5 Fe6 . . . 65.78(3) ? W4 Fe5 C3 . . . 80.10(19) ? W4 Fe5 C4 . . . 43.5(2) ? W4 Fe5 C51 . . . 84.5(3) ? W4 Fe5 C52 . . . 100.1(2) ? W4 Fe5 C53 . . . 163.6(2) ? Ru6 Fe5 Fe6 . . . .00(10) ? Ru6 Fe5 C3 . . . 54.11(18) ? Ru6 Fe5 C4 . . . 53.36(17) ? Ru6 Fe5 C51 . . . 99.2(3) ? Ru6 Fe5 C52 . . . 153.7(2) ? Ru6 Fe5 C53 . . . 97.8(2) ? Fe6 Fe5 C3 . . . 54.11(18) ? Fe6 Fe5 C4 . . . 53.36(17) ? Fe6 Fe5 C51 . . . 99.2(3) ? Fe6 Fe5 C52 . . . 153.7(2) ? Fe6 Fe5 C53 . . . 97.8(2) ? C3 Fe5 C4 . . . 37.0(3) ? C3 Fe5 C51 . . . 152.9(3) ? C3 Fe5 C52 . . . 103.1(3) ? C3 Fe5 C53 . . . 89.9(3) ? C4 Fe5 C51 . . . 126.2(3) ? C4 Fe5 C52 . . . 100.8(3) ? C4 Fe5 C53 . . . 126.7(3) ? C51 Fe5 C52 . . . 101.4(4) ? C51 Fe5 C53 . . . 99.3(4) ? C52 Fe5 C53 . . . 94.8(3) ? W4 Ru6 Ru5 . . . 62.29(3) ? W4 Ru6 Fe5 . . . 62.29(3) ? W4 Ru6 C3 . . . 77.01(18) ? W4 Ru6 C4 . . . 41.91(19) ? W4 Ru6 C61 . . . 99.9(3) ? W4 Ru6 C62 . . . 102.3(3) ? W4 Ru6 C63 . . . 158.1(3) ? Ru5 Ru6 Fe5 . . . .00(7) ? Ru5 Ru6 C3 . . . 51.56(16) ? Ru5 Ru6 C4 . . . 51.33(16) ? Ru5 Ru6 C61 . . . 105.4(3) ? Ru5 Ru6 C62 . . . 151.4(3) ? Ru5 Ru6 C63 . . . 96.4(3) ? Fe5 Ru6 C3 . . . 51.56(16) ? Fe5 Ru6 C4 . . . 51.33(16) ? Fe5 Ru6 C61 . . . 105.4(3) ? Fe5 Ru6 C62 . . . 151.4(3) ? Fe5 Ru6 C63 . . . 96.4(3) ? C3 Ru6 C4 . . . 35.8(3) ? C3 Ru6 C61 . . . 155.8(3) ? C3 Ru6 C62 . . . 103.4(3) ? C3 Ru6 C63 . . . 85.8(3) ? C4 Ru6 C61 . . . 139.5(4) ? C4 Ru6 C62 . . . 100.7(3) ? C4 Ru6 C63 . . . 121.5(3) ? C61 Ru6 C62 . . . 100.8(4) ? C61 Ru6 C63 . . . 90.3(4) ? C62 Ru6 C63 . . . 94.7(4) ? W4 Fe6 Ru5 . . . 62.29(3) ? W4 Fe6 Fe5 . . . 62.29(3) ? W4 Fe6 C3 . . . 77.01(18) ? W4 Fe6 C4 . . . 41.91(19) ? W4 Fe6 C61 . . . 99.9(3) ? W4 Fe6 C62 . . . 102.3(3) ? W4 Fe6 C63 . . . 158.1(3) ? Ru5 Fe6 Fe5 . . . .00(7) ? Ru5 Fe6 C3 . . . 51.56(16) ? Ru5 Fe6 C4 . . . 51.33(16) ? Ru5 Fe6 C61 . . . 105.4(3) ? Ru5 Fe6 C62 . . . 151.4(3) ? Ru5 Fe6 C63 . . . 96.4(3) ? Fe5 Fe6 C3 . . . 51.56(16) ? Fe5 Fe6 C4 . . . 51.33(16) ? Fe5 Fe6 C61 . . . 105.4(3) ? Fe5 Fe6 C62 . . . 151.4(3) ? Fe5 Fe6 C63 . . . 96.4(3) ? C3 Fe6 C4 . . . 35.8(3) ? C3 Fe6 C61 . . . 155.8(3) ? C3 Fe6 C62 . . . 103.4(3) ? C3 Fe6 C63 . . . 85.8(3) ? C4 Fe6 C61 . . . 139.5(4) ? C4 Fe6 C62 . . . 100.7(3) ? C4 Fe6 C63 . . . 121.5(3) ? C61 Fe6 C62 . . . 100.8(4) ? C61 Fe6 C63 . . . 90.3(4) ? C62 Fe6 C63 . . . 94.7(4) ? Ru1 C1 Fe1 . . . .00(7) ? Ru1 C1 Ru2 . . . 87.4(3) ? Ru1 C1 Ru3 . . . 87.6(3) ? Ru1 C1 C2 . . . 155.7(6) ? Fe1 C1 Ru2 . . . 87.4(3) ? Fe1 C1 Ru3 . . . 87.6(3) ? Fe1 C1 C2 . . . 155.7(6) ? Ru2 C1 Ru3 . . . 79.4(2) ? Ru2 C1 C2 . . . 74.3(4) ? Ru3 C1 C2 . . . 73.6(4) ? Ru2 C2 Ru3 . . . 77.8(2) ? Ru2 C2 C1 . . . 70.8(4) ? Ru2 C2 C3 . . . 131.9(4) ? Ru3 C2 C1 . . . 71.2(4) ? Ru3 C2 C3 . . . 129.5(4) ? C1 C2 C3 . . . 147.7(6) ? Ru5 C3 Fe5 . . . .00(12) ? Ru5 C3 Ru6 . . . 74.3(2) ? Ru5 C3 Fe6 . . . 74.3(2) ? Ru5 C3 C2 . . . 133.7(4) ? Ru5 C3 C4 . . . 70.8(4) ? Fe5 C3 Ru6 . . . 74.3(2) ? Fe5 C3 Fe6 . . . 74.3(2) ? Fe5 C3 C2 . . . 133.7(4) ? Fe5 C3 C4 . . . 70.8(4) ? Ru6 C3 Fe6 . . . .00000 ? Ru6 C3 C2 . . . 129.6(5) ? Ru6 C3 C4 . . . 70.8(4) ? Fe6 C3 C2 . . . 129.6(5) ? Fe6 C3 C4 . . . 70.8(4) ? C2 C3 C4 . . . 147.7(6) ? W4 C4 Ru5 . . . 90.6(3) ? W4 C4 Fe5 . . . 90.6(3) ? W4 C4 Ru6 . . . 92.4(3) ? W4 C4 Fe6 . . . 92.4(3) ? W4 C4 C3 . . . 159.8(5) ? Ru5 C4 Fe5 . . . .00(10) ? Ru5 C4 Ru6 . . . 75.3(2) ? Ru5 C4 Fe6 . . . 75.3(2) ? Ru5 C4 C3 . . . 72.2(4) ? Fe5 C4 Ru6 . . . 75.3(2) ? Fe5 C4 Fe6 . . . 75.3(2) ? Fe5 C4 C3 . . . 72.2(4) ? Ru6 C4 Fe6 . . . .00000 ? Ru6 C4 C3 . . . 73.3(4) ? Fe6 C4 C3 . . . 73.3(4) ? Ru1 C11 Fe1 . . . .00(12) ? Ru1 C11 O11 . . . 176.9(9) ? Fe1 C11 O11 . . . 176.9(9) ? Ru1 C12 Fe1 . . . .00(7) ? Ru1 C12 O12 . . . 175.1(8) ? Fe1 C12 O12 . . . 175.1(8) ? Ru1 C13 Fe1 . . . .00(10) ? Ru1 C13 O13 . . . 175.8(9) ? Fe1 C13 O13 . . . 175.8(9) ? Ru2 C21 O21 . . . 178.3(8) ? Ru2 C22 O22 . . . 177.9(8) ? Ru2 C23 O23 . . . 177.7(7) ? Ru3 C31 O31 . . . 177.9(8) ? Ru3 C32 O32 . . . 177.5(8) ? Ru3 C33 O33 . . . 174.6(7) ? W4 C41 O41 . . . 170.9(8) ? W4 C42 O42 . . . 176.7(10) ? Ru5 C51 Fe5 . . . .00(11) ? Ru5 C51 O51 . . . 177.7(7) ? Fe5 C51 O51 . . . 177.7(7) ? Ru5 C52 Fe5 . . . .00(12) ? Ru5 C52 O52 . . . 178.0(7) ? Fe5 C52 O52 . . . 178.0(7) ? Ru5 C53 Fe5 . . . .00(7) ? Ru5 C53 O53 . . . 177.2(7) ? Fe5 C53 O53 . . . 177.2(7) ? Ru6 C61 Fe6 . . . .00(7) ? Ru6 C61 O61 . . . 176.1(9) ? Fe6 C61 O61 . . . 176.1(9) ? Ru6 C62 Fe6 . . . .00000 ? Ru6 C62 O62 . . . 177.1(8) ? Fe6 C62 O62 . . . 177.1(8) ? Ru6 C63 Fe6 . . . .00000 ? Ru6 C63 O63 . . . 177.1(8) ? Fe6 C63 O63 . . . 177.1(8) ? W4 C401 C402 . . . 72.2(7) ? W4 C401 C405 . . . 71.5(7) ? W4 C401 H401 . . . 109(3) ? C402 C401 C405 . . . 107.6(10) ? C402 C401 H401 . . . 131(3) ? C405 C401 H401 . . . 120(3) ? W4 C402 C401 . . . 73.7(7) ? W4 C402 C403 . . . 71.9(6) ? W4 C402 H402 . . . 112(6) ? C401 C402 C403 . . . 108.0(10) ? C401 C402 H402 . . . 143(6) ? C403 C402 H402 . . . 109(6) ? W4 C403 C402 . . . 73.1(6) ? W4 C403 C404 . . . 71.1(6) ? W4 C403 H403 . . . 114(5) ? C402 C403 C404 . . . 109.0(10) ? C402 C403 H403 . . . 118(5) ? C404 C403 H403 . . . 133(5) ? W4 C404 C403 . . . 74.2(6) ? W4 C404 C405 . . . 74.5(7) ? W4 C404 H404 . . . 115(7) ? C403 C404 C405 . . . 108.0(11) ? C403 C404 H404 . . . 122(7) ? C405 C404 H404 . . . 130(7) ? W4 C405 C401 . . . 73.1(7) ? W4 C405 C404 . . . 70.4(7) ? W4 C405 H405 . . . 112(7) ? C401 C405 C404 . . . 107.3(10) ? C401 C405 H405 . . . 129(6) ? C404 C405 H405 . . . 122(6) ? Ru2 H0 Ru3 . . . 97(3) ? 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 C2 3.111(7) . . ? Ru1 O11 2.990(8) . . ? Ru1 O12 2.981(7) . . ? Ru1 O13 2.982(8) . . ? Ru1 C21 3.444(9) . . ? Ru1 C22 3.482(8) . . ? Ru1 C31 3.491(9) . . ? Ru1 C32 3.484(8) . . ? Fe1 C2 3.111(7) . . ? Fe1 O11 2.990(8) . . ? Fe1 O12 2.981(7) . . ? Fe1 O13 2.982(8) . . ? Fe1 C21 3.444(9) . . ? Fe1 C22 3.482(8) . . ? Fe1 C31 3.491(9) . . ? Fe1 C32 3.484(8) . . ? Ru2 C3 3.350(7) . . ? Ru2 O21 3.053(7) . . ? Ru2 O22 3.048(7) . . ? Ru2 O23 3.062(7) . . ? Ru3 C3 3.305(7) . . ? Ru3 O31 3.055(7) . . ? Ru3 O32 3.036(6) . . ? Ru3 O33 3.066(6) . . ? W4 C3 3.233(7) . . ? W4 O41 3.127(7) . . ? W4 O42 3.141(7) . . ? W4 C51 3.225(8) . . ? W4 H401 2.83(5) . . ? W4 H402 2.95(11) . . ? W4 H403 2.81(7) . . ? W4 H404 2.75(11) . . ? W4 H405 2.75(9) . . ? Ru5 C2 3.225(6) . . ? Ru5 O51 2.929(7) . . ? Ru5 O52 2.950(6) . . ? Ru5 O53 2.921(7) . . ? Ru5 C63 3.286(9) . . ? Fe5 C2 3.225(6) . . ? Fe5 O51 2.929(7) . . ? Fe5 O52 2.950(6) . . ? Fe5 O53 2.921(7) . . ? Fe5 C63 3.286(9) . . ? Ru6 C2 3.242(6) . . ? Ru6 C41 3.130(9) . . ? Ru6 C42 3.226(10) . . ? Ru6 C51 3.332(8) . . ? Ru6 C53 3.309(7) . . ? Ru6 O61 2.955(8) . . ? Ru6 O62 2.989(6) . . ? Ru6 O63 2.943(7) . . ? Fe6 C2 3.242(6) . . ? Fe6 C41 3.130(9) . . ? Fe6 C42 3.226(10) . . ? Fe6 C51 3.332(8) . . ? Fe6 C53 3.309(7) . . ? Fe6 O61 2.955(8) . . ? Fe6 O62 2.989(6) . . ? Fe6 O63 2.943(7) . . ? C1 C3 2.641(10) . . ? C1 C12 2.943(11) . . ? C1 C13 2.947(12) . . ? C1 C22 2.975(10) . . ? C1 C32 2.973(10) . . ? C2 C4 2.626(9) . . ? C2 C23 2.980(10) . . ? C2 C33 2.958(10) . . ? C3 C53 2.740(10) . . ? C3 C63 2.701(11) . . ? C4 C42 2.849(11) . . ? C4 C52 2.982(9) . . ? C11 C12 2.753(14) . . ? C11 C13 2.760(15) . . ? C12 C13 2.741(14) . . ? C21 C22 2.800(13) . . ? C21 C23 2.941(12) . . ? C21 H0 2.40(7) . . ? O21 O41 2.980(10) . '2 646' ? C22 C23 2.872(12) . . ? C23 H0 2.56(7) . . ? C31 C32 2.785(12) . . ? C31 C33 2.945(12) . . ? C31 H0 2.46(7) . . ? C32 C33 2.854(11) . . ? C33 H0 2.65(7) . . ? C41 C42 2.779(14) . . ? C41 C51 2.951(12) . . ? C41 C61 2.778(13) . . ? C41 C402 2.868(15) . . ? C41 H402 2.67(11) . . ? O41 C61 2.960(12) . . ? O41 O61 2.944(11) . . ? C42 C62 2.980(12) . . ? C42 C404 2.806(16) . . ? C42 H404 2.68(11) . . ? C51 C52 2.777(12) . . ? C51 C53 2.725(12) . . ? O51 H402 2.62(12) . '3 666' ? C52 C53 2.654(11) . . ? C52 H401 2.48(5) . . ? O52 H401 2.66(5) . . ? C53 C63 2.997(11) . . ? C61 C62 2.834(12) . . ? C61 C63 2.580(14) . . ? O61 H404 2.69(11) . '1 455' ? C62 C63 2.694(12) . . ? C401 C403 2.246(16) . . ? C401 C404 2.274(17) . . ? C401 H402 2.37(12) . . ? C401 H405 2.05(9) . . ? C402 C404 2.259(17) . . ? C402 C405 2.262(16) . . ? C402 H401 2.13(5) . . ? C402 H403 1.98(7) . . ? C403 C405 2.239(16) . . ? C403 H402 2.05(11) . . ? C403 H404 1.95(11) . . ? C404 H403 2.08(7) . . ? C404 H405 1.96(9) . . ? C405 H401 2.08(5) . . ? C405 H404 2.04(10) . . ? H402 H403 2.18(13) . . ? H404 H405 2.38(14) . . ? _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 2224 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 11 _reflns_limit_k_min 0 _reflns_limit_k_max 31 _reflns_limit_l_min -21 _reflns_limit_l_max 21 _reflns_number_observed ? _reflns_d_resolution_high .729 _reflns_d_resolution_low 13.504 _diffrn_reflns_av_sigmaI/netI .11 _diffrn_reflns_theta_min 1.5 _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 .075 _refine_ls_wR_factor_all .047 _refine_ls_goodness_of_fit_all 1.044 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #--end data_br604 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C26 H6 Fe2 O17 Ru3 W1' _chemical_formula_moiety ? _chemical_formula_weight 1189.07 _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 8.4640(10) _cell_length_b 23.850(3) _cell_length_c 16.454(2) _cell_angle_alpha 90.00000 _cell_angle_beta 90.798(2) _cell_angle_gamma 90.00000 _cell_volume 3321.2(7) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.378 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5592 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 5.70 _exptl_crystal_description plate _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.04 _exptl_crystal_size_rad ? _exptl_crystal_colour ? #<< use NfA code _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 .578 _exptl_absorpt_correction_T_max .914 _diffrn_reflns_number 38658 _reflns_number_total 8349 _reflns_Friedel_coverage ? _reflns_number_gt 6229 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.14 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .039 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .036 _refine_ls_wR_factor_ref .04 _refine_ls_goodness_of_fit_ref 1.249 _refine_ls_number_reflns 6229 _refine_ls_number_parameters 469 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .023 _refine_diff_density_min -.976 _refine_diff_density_max 1.813 _refine_ls_extinction_method ? _refine_ls_extinction_coef .00000 _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 ? 0 104 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 24 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 68 .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' W ? 0 4 -1.421 6.872 '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 .77152(8) .07584(3) .60715(4) .0469(4) Uani ? ? .257(5) ? ? Fe1 .77152(8) .07584(3) .60715(4) .0469(4) Uani ? ? .743(5) ? ? Ru2 .89820(5) .157208(18) .70989(2) .0405(2) Uani ? ? 1.00000 ? ? Ru3 .96170(5) .159920(18) .54439(2) .0392(2) Uani ? ? 1.00000 ? ? W4 .74295(3) .397009(9) .609214(14) .04563(13) Uani ? ? 1.00000 ? ? Ru5 .60138(7) .30724(3) .51680(4) .0373(4) Uani ? ? .183(4) ? ? Fe5 .60138(7) .30724(3) .51680(4) .0373(4) Uani ? ? .817(4) ? ? Ru6 .54223(6) .30501(2) .66974(3) .0397(3) Uani ? ? .478(4) ? ? Fe6 .54223(6) .30501(2) .66974(3) .0397(3) Uani ? ? .522(4) ? ? C1 .7351(5) .1511(2) .6056(3) .041(3) Uani ? ? 1.00000 ? ? C2 .7754(5) .2050(2) .6112(3) .035(2) Uani ? ? 1.00000 ? ? C3 .7268(5) .2614(2) .6054(3) .035(2) Uani ? ? 1.00000 ? ? C4 .7639(5) .3142(2) .6121(3) .036(3) Uani ? ? 1.00000 ? ? C11 .9215(8) .0210(3) .6208(5) .076(5) Uani ? ? 1.00000 ? ? O11 1.0159(7) -.0120(3) .6284(4) .115(5) Uani ? ? 1.00000 ? ? C12 .6872(8) .0508(3) .5114(5) .066(4) Uani ? ? 1.00000 ? ? O12 .6292(7) .0376(2) .4519(3) .093(4) Uani ? ? 1.00000 ? ? C13 .6220(8) .0465(3) .6720(4) .070(4) Uani ? ? 1.00000 ? ? O13 .5240(7) .0299(3) .7127(4) .105(4) Uani ? ? 1.00000 ? ? C21 1.0290(8) .1038(3) .7659(4) .064(4) Uani ? ? 1.00000 ? ? O21 1.1125(7) .0736(2) .7989(3) .103(4) Uani ? ? 1.00000 ? ? C22 .7301(8) .1506(3) .7858(4) .060(4) Uani ? ? 1.00000 ? ? O22 .6296(6) .1454(3) .8297(3) .095(4) Uani ? ? 1.00000 ? ? C23 .9876(7) .2252(3) .7548(4) .056(4) Uani ? ? 1.00000 ? ? O23 1.0341(7) .2663(2) .7776(3) .087(4) Uani ? ? 1.00000 ? ? C31 1.1289(7) .1096(3) .5142(4) .060(4) Uani ? ? 1.00000 ? ? O31 1.2319(6) .0814(2) .4982(4) .099(4) Uani ? ? 1.00000 ? ? C32 .8639(7) .1560(3) .4394(4) .057(4) Uani ? ? 1.00000 ? ? O32 .8009(6) .1542(3) .3784(3) .092(4) Uani ? ? 1.00000 ? ? C33 1.0695(6) .2302(3) .5254(3) .050(3) Uani ? ? 1.00000 ? ? O33 1.1237(5) .2726(2) .5166(3) .071(3) Uani ? ? 1.00000 ? ? C41 .5332(8) .4329(3) .6248(5) .072(4) Uani ? ? 1.00000 ? ? O41 .4168(6) .4588(2) .6292(4) .103(4) Uani ? ? 1.00000 ? ? C42 .7750(10) .4031(3) .7293(5) .078(5) Uani ? ? 1.00000 ? ? O42 .8063(9) .4083(2) .7955(4) .122(5) Uani ? ? 1.00000 ? ? C51 .4585(7) .3593(3) .4845(3) .058(4) Uani ? ? 1.00000 ? ? O51 .3680(6) .3909(2) .4621(3) .089(4) Uani ? ? 1.00000 ? ? C52 .7309(6) .3057(3) .4307(3) .052(3) Uani ? ? 1.00000 ? ? O52 .8110(5) .3035(2) .3746(3) .084(3) Uani ? ? 1.00000 ? ? C53 .4938(7) .2450(3) .4878(3) .050(3) Uani ? ? 1.00000 ? ? O53 .4332(6) .2045(2) .4697(3) .080(3) Uani ? ? 1.00000 ? ? C61 .3543(9) .3430(3) .6808(4) .072(4) Uani ? ? 1.00000 ? ? O61 .2333(6) .3627(3) .6879(4) .110(4) Uani ? ? 1.00000 ? ? C62 .6076(7) .2991(3) .7774(4) .056(4) Uani ? ? 1.00000 ? ? O62 .6466(6) .2918(2) .8434(3) .084(4) Uani ? ? 1.00000 ? ? C63 .4386(7) .2378(3) .6685(4) .055(4) Uani ? ? 1.00000 ? ? O63 .3782(5) .1954(2) .6691(3) .085(4) Uani ? ? 1.00000 ? ? C401 .8556(12) .4288(4) .4871(5) .090(6) Uani ? ? 1.00000 ? ? C402 .7804(10) .4738(4) .5241(6) .087(6) Uani ? ? 1.00000 ? ? C403 .8556(9) .4856(3) .5976(6) .078(5) Uani ? ? 1.00000 ? ? C404 .9746(8) .4472(3) .6087(5) .073(5) Uani ? ? 1.00000 ? ? C405 .9767(10) .4109(3) .5395(7) .088(6) Uani ? ? 1.00000 ? ? H0 1.060(6) .155(2) .637(3) .049(14) Uiso ? ? 1.00000 ? ? H401 .814(5) .4080(18) .444(3) .014(10) Uiso ? ? 1.00000 ? ? H402 .693(10) .497(4) .498(5) .13(3) Uiso ? ? 1.00000 ? ? H403 .811(9) .514(3) .637(5) .11(3) Uiso ? ? 1.00000 ? ? H404 1.046(6) .446(2) .651(3) .047(15) Uiso ? ? 1.00000 ? ? H405 1.055(9) .384(3) .554(5) .11(3) 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 .0515(4) .0307(4) .0588(5) -.0026(3) .0056(3) -.0008(3) Fe1 .0515(4) .0307(4) .0588(5) -.0026(3) .0056(3) -.0008(3) Ru2 .0461(2) .0366(2) .0388(2) .00451(18) .00030(17) .00434(18) Ru3 .0408(2) .0359(2) .0411(2) .00037(17) .00744(17) -.00288(18) W4 .05379(14) .03111(12) .05175(14) .00283(10) -.00771(10) .00208(10) Ru5 .0376(4) .0402(4) .0339(4) .0018(3) -.0007(2) .0038(3) Fe5 .0376(4) .0402(4) .0339(4) .0018(3) -.0007(2) .0038(3) Ru6 .0397(3) .0453(4) .0344(3) .0091(2) .0037(2) .0023(2) Fe6 .0397(3) .0453(4) .0344(3) .0091(2) .0037(2) .0023(2) C1 .035(2) .045(3) .042(3) -.001(2) .004(2) -.001(2) C2 .040(2) .036(3) .030(2) -.001(2) .0035(19) -.000(2) C3 .036(2) .038(3) .030(2) .000(2) .0022(19) .000(2) C4 .032(2) .047(3) .031(2) .003(2) .0004(18) .001(2) C11 .070(4) .053(4) .106(6) -.003(4) .001(4) -.013(4) O11 .095(4) .078(4) .171(6) .030(3) -.005(4) -.010(4) C12 .067(4) .046(4) .084(5) -.011(3) .010(4) -.005(3) O12 .104(4) .087(4) .089(4) -.025(3) -.011(3) -.022(3) C13 .071(4) .058(4) .080(5) -.003(3) -.004(4) .006(4) O13 .106(4) .099(5) .110(5) -.026(3) .035(3) .021(3) C21 .078(4) .048(4) .066(4) .007(3) -.010(3) .007(3) O21 .127(5) .080(4) .101(4) .037(4) -.039(4) .019(3) C22 .069(4) .061(4) .052(3) .011(3) .008(3) .012(3) O22 .079(3) .128(5) .078(3) .018(3) .035(3) .032(3) C23 .065(4) .051(4) .051(3) .002(3) -.003(3) -.001(3) O23 .114(4) .064(3) .083(4) -.019(3) -.012(3) -.017(3) C31 .057(4) .047(4) .075(4) .002(3) .013(3) -.007(3) O31 .086(4) .070(4) .142(5) .028(3) .035(3) -.015(3) C32 .064(4) .065(4) .044(3) -.013(3) .010(3) -.000(3) O32 .093(4) .130(5) .052(3) -.027(3) -.009(3) -.004(3) C33 .044(3) .053(4) .052(3) -.000(3) .006(2) -.005(3) O33 .065(3) .052(3) .097(4) -.015(2) .013(2) -.000(2) C41 .080(5) .041(4) .095(5) .015(3) -.003(4) -.004(3) O41 .090(4) .072(4) .147(5) .034(3) .003(4) -.010(3) C42 .117(6) .044(4) .072(5) -.008(4) -.021(4) -.004(3) O42 .201(7) .097(5) .066(4) -.038(4) -.030(4) -.008(3) C51 .069(4) .060(4) .045(3) .003(3) .002(3) -.000(3) O51 .094(4) .088(4) .085(4) .044(3) -.023(3) .005(3) C52 .045(3) .064(4) .048(3) -.004(3) -.001(3) .003(3) O52 .072(3) .116(5) .064(3) -.014(3) .026(2) -.005(3) C53 .048(3) .056(4) .045(3) .002(3) -.001(2) .002(3) O53 .075(3) .078(4) .086(3) -.020(3) -.003(3) -.013(3) C61 .081(5) .065(5) .071(4) .023(4) .002(4) .024(4) O61 .074(3) .118(5) .140(5) .049(3) .016(3) .040(4) C62 .055(3) .067(4) .046(3) .014(3) .008(3) -.002(3) O62 .084(3) .125(5) .043(3) .013(3) -.000(2) .006(3) C63 .045(3) .069(4) .053(3) .003(3) .010(3) -.001(3) O63 .067(3) .086(4) .103(4) -.018(3) .016(3) .008(3) C401 .124(7) .075(6) .070(5) -.048(6) .005(5) .012(4) C402 .089(6) .065(5) .106(7) -.008(4) -.012(5) .047(5) C403 .082(5) .041(4) .110(7) -.007(4) -.005(5) .004(4) C404 .065(4) .062(5) .091(5) -.015(4) -.014(4) .006(4) C405 .073(5) .052(5) .141(9) .003(4) .041(5) .029(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 . . 2.7789(8) ? Ru1 Ru3 . . 2.7794(8) ? Ru1 C1 . . 1.821(5) ? Ru1 C11 . . 1.834(7) ? Ru1 C12 . . 1.821(7) ? Ru1 C13 . . 1.807(7) ? Fe1 Ru2 . . 2.7789(8) ? Fe1 Ru3 . . 2.7794(8) ? Fe1 C1 . . 1.821(5) ? Fe1 C11 . . 1.834(7) ? Fe1 C12 . . 1.821(7) ? Fe1 C13 . . 1.807(7) ? Ru2 Ru3 . . 2.7837(7) ? Ru2 C1 . . 2.192(5) ? Ru2 C2 . . 2.229(5) ? Ru2 C21 . . 1.914(7) ? Ru2 C22 . . 1.913(6) ? Ru2 C23 . . 1.932(6) ? Ru2 H0 . . 1.83(5) ? Ru3 C1 . . 2.188(5) ? Ru3 C2 . . 2.213(5) ? Ru3 C31 . . 1.927(6) ? Ru3 C32 . . 1.907(6) ? Ru3 C33 . . 1.937(6) ? Ru3 H0 . . 1.74(5) ? W4 Ru5 . . 2.8777(7) ? W4 Fe5 . . 2.8777(7) ? W4 Ru6 . . 2.9563(6) ? W4 Fe6 . . 2.9563(6) ? W4 C4 . . 1.985(5) ? W4 C41 . . 1.991(7) ? W4 C42 . . 1.996(8) ? W4 C401 . . 2.361(9) ? W4 C402 . . 2.329(9) ? W4 C403 . . 2.327(7) ? W4 C404 . . 2.297(7) ? W4 C405 . . 2.324(9) ? Ru5 Ru6 . . 2.5731(8) ? Ru5 Fe6 . . 2.5731(8) ? Ru5 C3 . . 2.099(4) ? Ru5 C4 . . 2.078(4) ? Ru5 C51 . . 1.808(6) ? Ru5 C52 . . 1.804(6) ? Ru5 C53 . . 1.802(6) ? Fe5 Ru6 . . 2.5731(8) ? Fe5 Fe6 . . 2.5731(8) ? Fe5 C3 . . 2.099(4) ? Fe5 C4 . . 2.078(4) ? Fe5 C51 . . 1.808(6) ? Fe5 C52 . . 1.804(6) ? Fe5 C53 . . 1.802(6) ? Ru6 C3 . . 2.165(5) ? Ru6 C4 . . 2.125(4) ? Ru6 C61 . . 1.842(7) ? Ru6 C62 . . 1.854(6) ? Ru6 C63 . . 1.828(7) ? Fe6 C3 . . 2.165(5) ? Fe6 C4 . . 2.125(4) ? Fe6 C61 . . 1.842(7) ? Fe6 C62 . . 1.854(6) ? Fe6 C63 . . 1.828(7) ? C1 C2 . . 1.333(7) ? C2 C3 . . 1.410(7) ? C3 C4 . . 1.301(7) ? C11 O11 . . 1.127(9) ? C12 O12 . . 1.134(9) ? C13 O13 . . 1.144(9) ? C21 O21 . . 1.142(9) ? C22 O22 . . 1.130(8) ? C23 O23 . . 1.119(8) ? C31 O31 . . 1.135(8) ? C32 O32 . . 1.132(8) ? C33 O33 . . 1.120(8) ? C41 O41 . . 1.166(9) ? C42 O42 . . 1.124(10) ? C51 O51 . . 1.133(8) ? C52 O52 . . 1.153(7) ? C53 O53 . . 1.132(8) ? C61 O61 . . 1.134(9) ? C62 O62 . . 1.143(7) ? C63 O63 . . 1.133(9) ? C401 C402 . . 1.392(13) ? C401 C405 . . 1.396(13) ? C401 H401 . . .93(4) ? C402 C403 . . 1.387(13) ? C402 H402 . . 1.02(9) ? C403 C404 . . 1.371(11) ? C403 H403 . . 1.01(8) ? C404 C405 . . 1.431(13) ? C404 H404 . . .92(5) ? C405 H405 . . .95(8) ? 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 . . . 60.11(2) ? Ru2 Ru1 C1 . . . 51.99(15) ? Ru2 Ru1 C11 . . . 99.4(2) ? Ru2 Ru1 C12 . . . 154.0(2) ? Ru2 Ru1 C13 . . . 100.3(2) ? Ru3 Ru1 C1 . . . 51.86(15) ? Ru3 Ru1 C11 . . . 99.0(2) ? Ru3 Ru1 C12 . . . 97.9(2) ? Ru3 Ru1 C13 . . . 155.8(2) ? C1 Ru1 C11 . . . 145.2(3) ? C1 Ru1 C12 . . . 104.3(3) ? C1 Ru1 C13 . . . 105.7(3) ? C11 Ru1 C12 . . . 97.7(3) ? C11 Ru1 C13 . . . 98.1(3) ? C12 Ru1 C13 . . . 96.6(3) ? Ru2 Fe1 Ru3 . . . 60.11(2) ? Ru2 Fe1 C1 . . . 51.99(15) ? Ru2 Fe1 C11 . . . 99.4(2) ? Ru2 Fe1 C12 . . . 154.0(2) ? Ru2 Fe1 C13 . . . 100.3(2) ? Ru3 Fe1 C1 . . . 51.86(15) ? Ru3 Fe1 C11 . . . 99.0(2) ? Ru3 Fe1 C12 . . . 97.9(2) ? Ru3 Fe1 C13 . . . 155.8(2) ? C1 Fe1 C11 . . . 145.2(3) ? C1 Fe1 C12 . . . 104.3(3) ? C1 Fe1 C13 . . . 105.7(3) ? C11 Fe1 C12 . . . 97.7(3) ? C11 Fe1 C13 . . . 98.1(3) ? C12 Fe1 C13 . . . 96.6(3) ? Ru1 Ru2 Fe1 . . . .00000 ? Ru1 Ru2 Ru3 . . . 59.95(2) ? Ru1 Ru2 C1 . . . 40.87(14) ? Ru1 Ru2 C2 . . . 75.02(12) ? Ru1 Ru2 C21 . . . 92.5(2) ? Ru1 Ru2 C22 . . . 93.19(19) ? Ru1 Ru2 C23 . . . 164.70(18) ? Ru1 Ru2 H0 . . . 82.4(15) ? Fe1 Ru2 Ru3 . . . 59.95(2) ? Fe1 Ru2 C1 . . . 40.87(14) ? Fe1 Ru2 C2 . . . 75.02(12) ? Fe1 Ru2 C21 . . . 92.5(2) ? Fe1 Ru2 C22 . . . 93.19(19) ? Fe1 Ru2 C23 . . . 164.70(18) ? Fe1 Ru2 H0 . . . 82.4(15) ? Ru3 Ru2 C1 . . . 50.48(12) ? Ru3 Ru2 C2 . . . 50.92(12) ? Ru3 Ru2 C21 . . . 111.6(2) ? Ru3 Ru2 C22 . . . 142.78(19) ? Ru3 Ru2 C23 . . . 105.96(18) ? Ru3 Ru2 H0 . . . 37.5(15) ? C1 Ru2 C2 . . . 35.08(19) ? C1 Ru2 C21 . . . 133.3(2) ? C1 Ru2 C22 . . . 92.3(2) ? C1 Ru2 C23 . . . 126.5(2) ? C1 Ru2 H0 . . . 87.5(15) ? C2 Ru2 C21 . . . 162.0(2) ? C2 Ru2 C22 . . . 100.1(2) ? C2 Ru2 C23 . . . 91.5(2) ? C2 Ru2 H0 . . . 83.5(15) ? C21 Ru2 C22 . . . 93.5(3) ? C21 Ru2 C23 . . . 98.8(3) ? C21 Ru2 H0 . . . 81.9(15) ? C22 Ru2 C23 . . . 96.3(3) ? C22 Ru2 H0 . . . 173.5(16) ? C23 Ru2 H0 . . . 89.0(16) ? Ru1 Ru3 Fe1 . . . .00(10) ? Ru1 Ru3 Ru2 . . . 59.937(18) ? Ru1 Ru3 C1 . . . 40.86(14) ? Ru1 Ru3 C2 . . . 75.25(13) ? Ru1 Ru3 C31 . . . 94.44(19) ? Ru1 Ru3 C32 . . . 93.17(19) ? Ru1 Ru3 C33 . . . 164.00(17) ? Ru1 Ru3 H0 . . . 84.0(16) ? Fe1 Ru3 Ru2 . . . 59.937(18) ? Fe1 Ru3 C1 . . . 40.86(14) ? Fe1 Ru3 C2 . . . 75.25(13) ? Fe1 Ru3 C31 . . . 94.44(19) ? Fe1 Ru3 C32 . . . 93.17(19) ? Fe1 Ru3 C33 . . . 164.00(17) ? Fe1 Ru3 H0 . . . 84.0(16) ? Ru2 Ru3 C1 . . . 50.61(12) ? Ru2 Ru3 C2 . . . 51.46(12) ? Ru2 Ru3 C31 . . . 113.0(2) ? Ru2 Ru3 C32 . . . 142.90(18) ? Ru2 Ru3 C33 . . . 105.99(17) ? Ru2 Ru3 H0 . . . 39.9(16) ? C1 Ru3 C2 . . . 35.25(19) ? C1 Ru3 C31 . . . 135.2(2) ? C1 Ru3 C32 . . . 92.3(2) ? C1 Ru3 C33 . . . 125.1(2) ? C1 Ru3 H0 . . . 90.0(16) ? C2 Ru3 C31 . . . 164.1(2) ? C2 Ru3 C32 . . . 99.8(2) ? C2 Ru3 C33 . . . 90.0(2) ? C2 Ru3 H0 . . . 86.2(16) ? C31 Ru3 C32 . . . 92.7(3) ? C31 Ru3 C33 . . . 98.6(3) ? C31 Ru3 H0 . . . 80.7(16) ? C32 Ru3 C33 . . . 95.5(3) ? C32 Ru3 H0 . . . 172.6(17) ? C33 Ru3 H0 . . . 88.9(17) ? Ru5 W4 Fe5 . . . .00(10) ? Ru5 W4 Ru6 . . . 52.321(17) ? Ru5 W4 Fe6 . . . 52.321(17) ? Ru5 W4 C4 . . . 46.23(13) ? Ru5 W4 C41 . . . 91.3(2) ? Ru5 W4 C42 . . . 128.8(2) ? Ru5 W4 C401 . . . 87.7(2) ? Ru5 W4 C402 . . . 109.1(2) ? Ru5 W4 C403 . . . 143.2(2) ? Ru5 W4 C404 . . . 137.3(2) ? Ru5 W4 C405 . . . 101.3(2) ? Fe5 W4 Ru6 . . . 52.321(17) ? Fe5 W4 Fe6 . . . 52.321(17) ? Fe5 W4 C4 . . . 46.23(13) ? Fe5 W4 C41 . . . 91.3(2) ? Fe5 W4 C42 . . . 128.8(2) ? Fe5 W4 C401 . . . 87.7(2) ? Fe5 W4 C402 . . . 109.1(2) ? Fe5 W4 C403 . . . 143.2(2) ? Fe5 W4 C404 . . . 137.3(2) ? Fe5 W4 C405 . . . 101.3(2) ? Ru6 W4 Fe6 . . . .00(10) ? Ru6 W4 C4 . . . 45.91(13) ? Ru6 W4 C41 . . . 76.0(2) ? Ru6 W4 C42 . . . 78.0(2) ? Ru6 W4 C401 . . . 140.0(2) ? Ru6 W4 C402 . . . 150.4(2) ? Ru6 W4 C403 . . . 160.0(2) ? Ru6 W4 C404 . . . 151.9(2) ? Ru6 W4 C405 . . . 140.3(2) ? Fe6 W4 C4 . . . 45.91(13) ? Fe6 W4 C41 . . . 76.0(2) ? Fe6 W4 C42 . . . 78.0(2) ? Fe6 W4 C401 . . . 140.0(2) ? Fe6 W4 C402 . . . 150.4(2) ? Fe6 W4 C403 . . . 160.0(2) ? Fe6 W4 C404 . . . 151.9(2) ? Fe6 W4 C405 . . . 140.3(2) ? C4 W4 C41 . . . 120.3(2) ? C4 W4 C42 . . . 92.2(2) ? C4 W4 C401 . . . 107.7(3) ? C4 W4 C402 . . . 141.7(3) ? C4 W4 C403 . . . 150.4(2) ? C4 W4 C404 . . . 116.3(2) ? C4 W4 C405 . . . 94.5(2) ? C41 W4 C42 . . . 87.1(3) ? C41 W4 C401 . . . 110.1(3) ? C41 W4 C402 . . . 82.4(3) ? C41 W4 C403 . . . 89.3(3) ? C41 W4 C404 . . . 122.6(3) ? C41 W4 C405 . . . 140.3(3) ? C42 W4 C401 . . . 140.2(3) ? C42 W4 C402 . . . 121.3(3) ? C42 W4 C403 . . . 88.0(3) ? C42 W4 C404 . . . 82.0(3) ? C42 W4 C405 . . . 111.9(4) ? C401 W4 C402 . . . 34.5(3) ? C401 W4 C403 . . . 57.8(3) ? C401 W4 C404 . . . 58.3(3) ? C401 W4 C405 . . . 34.7(3) ? C402 W4 C403 . . . 34.7(3) ? C402 W4 C404 . . . 57.6(3) ? C402 W4 C405 . . . 57.8(3) ? C403 W4 C404 . . . 34.5(3) ? C403 W4 C405 . . . 58.5(3) ? C404 W4 C405 . . . 36.1(3) ? W4 Ru5 Ru6 . . . 65.41(2) ? W4 Ru5 Fe6 . . . 65.41(2) ? W4 Ru5 C3 . . . 79.49(13) ? W4 Ru5 C4 . . . 43.60(15) ? W4 Ru5 C51 . . . 85.2(2) ? W4 Ru5 C52 . . . 100.2(2) ? W4 Ru5 C53 . . . 163.30(18) ? Ru6 Ru5 Fe6 . . . .00000 ? Ru6 Ru5 C3 . . . 54.08(12) ? Ru6 Ru5 C4 . . . 53.07(12) ? Ru6 Ru5 C51 . . . 99.37(19) ? Ru6 Ru5 C52 . . . 153.69(18) ? Ru6 Ru5 C53 . . . 97.90(18) ? Fe6 Ru5 C3 . . . 54.08(12) ? Fe6 Ru5 C4 . . . 53.07(12) ? Fe6 Ru5 C51 . . . 99.37(19) ? Fe6 Ru5 C52 . . . 153.69(18) ? Fe6 Ru5 C53 . . . 97.90(18) ? C3 Ru5 C4 . . . 36.3(2) ? C3 Ru5 C51 . . . 153.1(2) ? C3 Ru5 C52 . . . 103.2(2) ? C3 Ru5 C53 . . . 90.2(2) ? C4 Ru5 C51 . . . 126.9(2) ? C4 Ru5 C52 . . . 101.0(2) ? C4 Ru5 C53 . . . 126.3(2) ? C51 Ru5 C52 . . . 101.2(3) ? C51 Ru5 C53 . . . 98.9(3) ? C52 Ru5 C53 . . . 94.9(3) ? W4 Fe5 Ru6 . . . 65.41(2) ? W4 Fe5 Fe6 . . . 65.41(2) ? W4 Fe5 C3 . . . 79.49(13) ? W4 Fe5 C4 . . . 43.60(15) ? W4 Fe5 C51 . . . 85.2(2) ? W4 Fe5 C52 . . . 100.2(2) ? W4 Fe5 C53 . . . 163.30(18) ? Ru6 Fe5 Fe6 . . . .00000 ? Ru6 Fe5 C3 . . . 54.08(12) ? Ru6 Fe5 C4 . . . 53.07(12) ? Ru6 Fe5 C51 . . . 99.37(19) ? Ru6 Fe5 C52 . . . 153.69(18) ? Ru6 Fe5 C53 . . . 97.90(18) ? Fe6 Fe5 C3 . . . 54.08(12) ? Fe6 Fe5 C4 . . . 53.07(12) ? Fe6 Fe5 C51 . . . 99.37(19) ? Fe6 Fe5 C52 . . . 153.69(18) ? Fe6 Fe5 C53 . . . 97.90(18) ? C3 Fe5 C4 . . . 36.3(2) ? C3 Fe5 C51 . . . 153.1(2) ? C3 Fe5 C52 . . . 103.2(2) ? C3 Fe5 C53 . . . 90.2(2) ? C4 Fe5 C51 . . . 126.9(2) ? C4 Fe5 C52 . . . 101.0(2) ? C4 Fe5 C53 . . . 126.3(2) ? C51 Fe5 C52 . . . 101.2(3) ? C51 Fe5 C53 . . . 98.9(3) ? C52 Fe5 C53 . . . 94.9(3) ? W4 Ru6 Ru5 . . . 62.267(18) ? W4 Ru6 Fe5 . . . 62.267(18) ? W4 Ru6 C3 . . . 76.69(13) ? W4 Ru6 C4 . . . 42.14(14) ? W4 Ru6 C61 . . . 99.8(2) ? W4 Ru6 C62 . . . 102.3(2) ? W4 Ru6 C63 . . . 157.73(19) ? Ru5 Ru6 Fe5 . . . .00000 ? Ru5 Ru6 C3 . . . 51.71(12) ? Ru5 Ru6 C4 . . . 51.43(12) ? Ru5 Ru6 C61 . . . 105.5(2) ? Ru5 Ru6 C62 . . . 151.25(18) ? Ru5 Ru6 C63 . . . 96.16(19) ? Fe5 Ru6 C3 . . . 51.71(12) ? Fe5 Ru6 C4 . . . 51.43(12) ? Fe5 Ru6 C61 . . . 105.5(2) ? Fe5 Ru6 C62 . . . 151.25(18) ? Fe5 Ru6 C63 . . . 96.16(19) ? C3 Ru6 C4 . . . 35.3(2) ? C3 Ru6 C61 . . . 156.2(2) ? C3 Ru6 C62 . . . 102.9(2) ? C3 Ru6 C63 . . . 85.6(2) ? C4 Ru6 C61 . . . 139.7(3) ? C4 Ru6 C62 . . . 100.4(2) ? C4 Ru6 C63 . . . 120.8(2) ? C61 Ru6 C62 . . . 100.9(3) ? C61 Ru6 C63 . . . 91.0(3) ? C62 Ru6 C63 . . . 94.6(3) ? W4 Fe6 Ru5 . . . 62.267(18) ? W4 Fe6 Fe5 . . . 62.267(18) ? W4 Fe6 C3 . . . 76.69(13) ? W4 Fe6 C4 . . . 42.14(14) ? W4 Fe6 C61 . . . 99.8(2) ? W4 Fe6 C62 . . . 102.3(2) ? W4 Fe6 C63 . . . 157.73(19) ? Ru5 Fe6 Fe5 . . . .00000 ? Ru5 Fe6 C3 . . . 51.71(12) ? Ru5 Fe6 C4 . . . 51.43(12) ? Ru5 Fe6 C61 . . . 105.5(2) ? Ru5 Fe6 C62 . . . 151.25(18) ? Ru5 Fe6 C63 . . . 96.16(19) ? Fe5 Fe6 C3 . . . 51.71(12) ? Fe5 Fe6 C4 . . . 51.43(12) ? Fe5 Fe6 C61 . . . 105.5(2) ? Fe5 Fe6 C62 . . . 151.25(18) ? Fe5 Fe6 C63 . . . 96.16(19) ? C3 Fe6 C4 . . . 35.3(2) ? C3 Fe6 C61 . . . 156.2(2) ? C3 Fe6 C62 . . . 102.9(2) ? C3 Fe6 C63 . . . 85.6(2) ? C4 Fe6 C61 . . . 139.7(3) ? C4 Fe6 C62 . . . 100.4(2) ? C4 Fe6 C63 . . . 120.8(2) ? C61 Fe6 C62 . . . 100.9(3) ? C61 Fe6 C63 . . . 91.0(3) ? C62 Fe6 C63 . . . 94.6(3) ? Ru1 C1 Fe1 . . . .00000 ? Ru1 C1 Ru2 . . . 87.1(2) ? Ru1 C1 Ru3 . . . 87.3(2) ? Ru1 C1 C2 . . . 155.0(4) ? Fe1 C1 Ru2 . . . 87.1(2) ? Fe1 C1 Ru3 . . . 87.3(2) ? Fe1 C1 C2 . . . 155.0(4) ? Ru2 C1 Ru3 . . . 78.91(15) ? Ru2 C1 C2 . . . 74.0(3) ? Ru3 C1 C2 . . . 73.4(3) ? Ru2 C2 Ru3 . . . 77.62(15) ? Ru2 C2 C1 . . . 71.0(3) ? Ru2 C2 C3 . . . 132.0(3) ? Ru3 C2 C1 . . . 71.4(3) ? Ru3 C2 C3 . . . 129.7(3) ? C1 C2 C3 . . . 147.3(4) ? Ru5 C3 Fe5 . . . .00000 ? Ru5 C3 Ru6 . . . 74.21(15) ? Ru5 C3 Fe6 . . . 74.21(15) ? Ru5 C3 C2 . . . 133.5(3) ? Ru5 C3 C4 . . . 71.0(3) ? Fe5 C3 Ru6 . . . 74.21(15) ? Fe5 C3 Fe6 . . . 74.21(15) ? Fe5 C3 C2 . . . 133.5(3) ? Fe5 C3 C4 . . . 71.0(3) ? Ru6 C3 Fe6 . . . .00(12) ? Ru6 C3 C2 . . . 129.6(3) ? Ru6 C3 C4 . . . 70.6(3) ? Fe6 C3 C2 . . . 129.6(3) ? Fe6 C3 C4 . . . 70.6(3) ? C2 C3 C4 . . . 148.0(4) ? W4 C4 Ru5 . . . 90.2(2) ? W4 C4 Fe5 . . . 90.2(2) ? W4 C4 Ru6 . . . 91.9(2) ? W4 C4 Fe6 . . . 91.9(2) ? W4 C4 C3 . . . 160.0(4) ? Ru5 C4 Fe5 . . . .00(7) ? Ru5 C4 Ru6 . . . 75.50(14) ? Ru5 C4 Fe6 . . . 75.50(14) ? Ru5 C4 C3 . . . 72.7(3) ? Fe5 C4 Ru6 . . . 75.50(14) ? Fe5 C4 Fe6 . . . 75.50(14) ? Fe5 C4 C3 . . . 72.7(3) ? Ru6 C4 Fe6 . . . .00000 ? Ru6 C4 C3 . . . 74.1(3) ? Fe6 C4 C3 . . . 74.1(3) ? Ru1 C11 Fe1 . . . .00(11) ? Ru1 C11 O11 . . . 178.5(7) ? Fe1 C11 O11 . . . 178.5(7) ? Ru1 C12 Fe1 . . . .00000 ? Ru1 C12 O12 . . . 176.2(6) ? Fe1 C12 O12 . . . 176.2(6) ? Ru1 C13 Fe1 . . . .00(10) ? Ru1 C13 O13 . . . 177.2(6) ? Fe1 C13 O13 . . . 177.2(6) ? Ru2 C21 O21 . . . 177.0(6) ? Ru2 C22 O22 . . . 178.2(6) ? Ru2 C23 O23 . . . 175.9(6) ? Ru3 C31 O31 . . . 177.0(6) ? Ru3 C32 O32 . . . 177.6(6) ? Ru3 C33 O33 . . . 175.5(5) ? W4 C41 O41 . . . 172.6(6) ? W4 C42 O42 . . . 173.8(8) ? Ru5 C51 Fe5 . . . .00(10) ? Ru5 C51 O51 . . . 177.7(6) ? Fe5 C51 O51 . . . 177.7(6) ? Ru5 C52 Fe5 . . . .00000 ? Ru5 C52 O52 . . . 178.0(5) ? Fe5 C52 O52 . . . 178.0(5) ? Ru5 C53 Fe5 . . . .00(7) ? Ru5 C53 O53 . . . 176.6(5) ? Fe5 C53 O53 . . . 176.6(5) ? Ru6 C61 Fe6 . . . .00000 ? Ru6 C61 O61 . . . 175.0(7) ? Fe6 C61 O61 . . . 175.0(7) ? Ru6 C62 Fe6 . . . .00(7) ? Ru6 C62 O62 . . . 175.6(6) ? Fe6 C62 O62 . . . 175.6(6) ? Ru6 C63 Fe6 . . . .00(7) ? Ru6 C63 O63 . . . 177.9(5) ? Fe6 C63 O63 . . . 177.9(5) ? W4 C401 C402 . . . 71.5(5) ? W4 C401 C405 . . . 71.2(5) ? W4 C401 H401 . . . 109(3) ? C402 C401 C405 . . . 107.6(8) ? C402 C401 H401 . . . 125(3) ? C405 C401 H401 . . . 125(3) ? W4 C402 C401 . . . 74.0(5) ? W4 C402 C403 . . . 72.6(5) ? W4 C402 H402 . . . 126(5) ? C401 C402 C403 . . . 109.3(8) ? C401 C402 H402 . . . 125(5) ? C403 C402 H402 . . . 125(5) ? W4 C403 C402 . . . 72.7(5) ? W4 C403 C404 . . . 71.5(4) ? W4 C403 H403 . . . 113(5) ? C402 C403 C404 . . . 107.9(7) ? C402 C403 H403 . . . 122(5) ? C404 C403 H403 . . . 130(5) ? W4 C404 C403 . . . 74.0(4) ? W4 C404 C405 . . . 73.0(5) ? W4 C404 H404 . . . 123(3) ? C403 C404 C405 . . . 108.4(7) ? C403 C404 H404 . . . 126(3) ? C405 C404 H404 . . . 125(3) ? W4 C405 C401 . . . 74.1(5) ? W4 C405 C404 . . . 70.9(5) ? W4 C405 H405 . . . 112(5) ? C401 C405 C404 . . . 106.8(7) ? C401 C405 H405 . . . 150(5) ? C404 C405 H405 . . . 103(5) ? Ru2 H0 Ru3 . . . 103(2) ? 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 C2 3.081(5) . . ? Ru1 O11 2.961(6) . . ? Ru1 O12 2.953(6) . . ? Ru1 O13 2.951(6) . . ? Ru1 C21 3.443(7) . . ? Ru1 C22 3.460(6) . . ? Ru1 C31 3.502(6) . . ? Ru1 C32 3.456(6) . . ? Ru1 H0 3.12(5) . . ? Fe1 C2 3.081(5) . . ? Fe1 O11 2.961(6) . . ? Fe1 O12 2.953(6) . . ? Fe1 O13 2.951(6) . . ? Fe1 C21 3.443(7) . . ? Fe1 C22 3.460(6) . . ? Fe1 C31 3.502(6) . . ? Fe1 C32 3.456(6) . . ? Fe1 H0 3.12(5) . . ? Ru2 Ru6 4.6780(8) . . ? Ru2 C3 3.341(5) . . ? Ru2 C11 3.570(8) . . ? Ru2 C13 3.575(7) . . ? Ru2 O21 3.055(6) . . ? Ru2 O22 3.043(5) . . ? Ru2 O23 3.050(5) . . ? Ru2 C33 3.804(6) . . ? Ru3 Ru5 4.6704(8) . . ? Ru3 C3 3.297(5) . . ? Ru3 C11 3.561(7) . . ? Ru3 C12 3.525(7) . . ? Ru3 C23 3.800(6) . . ? Ru3 O31 3.061(5) . . ? Ru3 O32 3.038(5) . . ? Ru3 O33 3.055(5) . . ? Ru3 O62 3.854(5) . '4 554' ? W4 C3 3.238(5) . . ? W4 O41 3.150(5) . . ? W4 O42 3.116(6) . . ? W4 C51 3.267(6) . . ? W4 O51 3.967(5) . . ? W4 C52 3.657(6) . . ? W4 C61 3.739(7) . . ? W4 C62 3.810(6) . . ? W4 H401 2.80(4) . . ? W4 H402 3.04(9) . . ? W4 H403 2.88(8) . . ? W4 H404 2.90(5) . . ? W4 H405 2.82(8) . . ? Ru5 C2 3.235(5) . . ? Ru5 C41 3.537(7) . . ? Ru5 O51 2.941(5) . . ? Ru5 O52 2.957(5) . . ? Ru5 O53 2.933(5) . . ? Ru5 C61 3.542(7) . . ? Ru5 C63 3.312(6) . . ? Ru5 C401 3.647(10) . . ? Ru5 H401 3.24(4) . . ? Fe5 C2 3.235(5) . . ? Fe5 C41 3.537(7) . . ? Fe5 O51 2.941(5) . . ? Fe5 O52 2.957(5) . . ? Fe5 O53 2.933(5) . . ? Fe5 C61 3.542(7) . . ? Fe5 C63 3.312(6) . . ? Fe5 H401 3.24(4) . . ? Ru6 C2 3.251(5) . . ? Ru6 C41 3.140(7) . . ? Ru6 O41 3.874(6) . . ? Ru6 C42 3.204(7) . . ? Ru6 C51 3.377(6) . . ? Ru6 C53 3.338(6) . . ? Ru6 O61 2.973(6) . . ? Ru6 O62 2.995(4) . . ? Ru6 O63 2.960(5) . . ? Fe6 C2 3.251(5) . . ? Fe6 C41 3.140(7) . . ? Fe6 C42 3.204(7) . . ? Fe6 C51 3.377(6) . . ? Fe6 C53 3.338(6) . . ? Fe6 O61 2.973(6) . . ? Fe6 O62 2.995(4) . . ? Fe6 O63 2.960(5) . . ? C1 C3 2.632(7) . . ? C1 C12 2.875(9) . . ? C1 C13 2.891(9) . . ? C1 C22 2.967(8) . . ? C1 C32 2.959(8) . . ? C2 C4 2.606(7) . . ? C2 C23 2.988(7) . . ? C2 C33 2.940(7) . . ? C3 C53 2.772(7) . . ? C3 C63 2.724(7) . . ? C4 C42 2.867(9) . . ? C11 C12 2.752(10) . . ? C11 C13 2.750(10) . . ? C12 C13 2.709(11) . . ? C21 C22 2.788(9) . . ? C21 C23 2.921(9) . . ? C21 H0 2.46(5) . . ? O21 O41 2.994(8) . '2 646' ? C22 C23 2.865(9) . . ? C23 H0 2.64(5) . . ? C31 C32 2.774(9) . . ? C31 C33 2.928(9) . . ? C31 H0 2.38(5) . . ? C32 C33 2.845(8) . . ? C33 H0 2.58(5) . . ? C41 C42 2.747(11) . . ? C41 C51 2.961(9) . . ? C41 C61 2.790(10) . . ? C41 C402 2.858(12) . . ? O41 C61 2.941(9) . . ? O41 O61 2.940(8) . . ? O41 H402 2.51(9) . '3 666' ? C42 C62 2.970(10) . . ? C42 C404 2.826(11) . . ? C51 C52 2.791(8) . . ? C51 C53 2.744(9) . . ? C52 C53 2.657(8) . . ? C52 H401 2.55(4) . . ? C61 C62 2.850(9) . . ? C61 C63 2.618(10) . . ? O61 H404 2.61(5) . '1 455' ? C62 C63 2.707(9) . . ? C401 C403 2.267(12) . . ? C401 C404 2.269(12) . . ? C401 H402 2.15(9) . . ? C401 H405 2.27(8) . . ? C402 C404 2.230(12) . . ? C402 C405 2.250(12) . . ? C402 H401 2.07(4) . . ? C402 H403 2.10(8) . . ? C403 C405 2.273(12) . . ? C403 H402 2.14(9) . . ? C403 H404 2.05(5) . . ? C404 H403 2.16(8) . . ? C404 H405 1.89(8) . . ? C405 H401 2.08(4) . . ? C405 H404 2.10(5) . . ? H404 H405 2.18(10) . . ? _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 2224 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 11 _reflns_limit_k_min 0 _reflns_limit_k_max 31 _reflns_limit_l_min -22 _reflns_limit_l_max 22 _reflns_number_observed ? _reflns_d_resolution_high .73 _reflns_d_resolution_low 13.506 _diffrn_reflns_av_sigmaI/netI .064 _diffrn_reflns_theta_min 1.5 _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 .057 _refine_ls_wR_factor_all .043 _refine_ls_goodness_of_fit_all 1.153 _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 #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end