# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1494 data_br534 # 2. EXPERIMENTAL DATA #--------------------- _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _chemical_formula_sum 'C29 H18 Au1 O9 P1 Ru3' _chemical_formula_moiety ? _chemical_formula_weight 1041.59 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 13.821(4) _cell_length_b 11.566(2) _cell_length_c 10.433(2) _cell_angle_alpha 74.740(10) _cell_angle_beta 87.68(2) _cell_angle_gamma 89.81(2) _cell_volume 1607.6(6) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 2.150 _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 13.6 _cell_measurement_theta_max 18.6 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 6.03 _exptl_crystal_description ? _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _diffrn_measurement_device_type 'Enraf Nonius CAD diffractometer' _diffrn_measurement_method '2theta/omega scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details 'XTAL absorb' _exptl_absorpt_correction_T_min 0.29 _exptl_absorpt_correction_T_max 0.48 _diffrn_reflns_number 5646 _reflns_number_total 5646 _reflns_Friedel_coverage ? _reflns_number_gt ? _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 -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _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 0.059 _refine_ls_wR_factor_ref 0.057 _refine_ls_goodness_of_fit_ref 1.724 _refine_ls_number_reflns 3256 _refine_ls_number_parameters 396 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref #<< use NfA code _refine_ls_shift/su_max .082 _refine_diff_density_min -1.43 _refine_diff_density_max 1.95 _refine_ls_extinction_method ? _refine_ls_extinction_coef 0 _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 58 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 18 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 32 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 2 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 6 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 2 -2.688 8.798 '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 Au .21792(5) .74037(6) .26947(7) .0542(5) Uani ? ? 1.00000 ? ? Ru1 .15878(12) .97394(13) .18022(17) .0726(14) Uani ? ? 1.00000 ? ? Ru2 .35929(14) .95642(16) .2357(2) .104(2) Uani ? ? 1.00000 ? ? Ru3 .21985(11) .87728(15) .44762(15) .0670(14) Uani ? ? 1.00000 ? ? C11 .1457(18) 1.1106(19) .045(2) .12(2) Uani ? ? 1.00000 ? ? O11 .1396(16) 1.1976(14) -.0432(16) .17(2) Uani ? ? 1.00000 ? ? C12 .1446(18) .877(2) .058(2) .12(3) Uani ? ? 1.00000 ? ? O12 .1328(13) .8372(13) -.0280(16) .141(18) Uani ? ? 1.00000 ? ? C13 .0254(15) .960(2) .238(3) .13(3) Uani ? ? 1.00000 ? ? O13 -.0542(11) .9612(16) .2659(19) .16(2) Uani ? ? 1.00000 ? ? C21 .446(3) 1.041(4) .245(5) .149(18) Uiso ? ? .592(8) ? ? O21 .511(3) 1.103(3) .277(4) .216(16) Uiso ? ? .592(8) ? ? C21' .460(4) 1.073(5) .156(5) .094(17) Uiso ? ? .408(8) ? ? O21' .523(3) 1.132(4) .123(4) .136(15) Uiso ? ? .408(8) ? ? C22 .4230(12) .8156(18) .206(2) .09(2) Uani ? ? 1.00000 ? ? O22 .4678(9) .7359(13) .1911(15) .106(15) Uani ? ? 1.00000 ? ? C23 .357(3) 1.029(3) .043(4) .113(13) Uiso ? ? .592(8) ? ? O23 .357(2) 1.070(3) -.073(3) .145(11) Uiso ? ? .592(8) ? ? C23' .459(5) .906(6) .419(7) .16(3) Uiso ? ? .408(8) ? ? O23' .492(4) .887(4) .516(5) .18(2) Uiso ? ? .408(8) ? ? C31 .2495(16) .922(2) .604(2) .11(2) Uani ? ? 1.00000 ? ? O31 .2703(13) .9515(17) .6961(16) .16(2) Uani ? ? 1.00000 ? ? C32 .2650(15) .7185(18) .5195(17) .09(2) Uani ? ? 1.00000 ? ? O32 .3015(13) .6284(14) .5706(14) .136(17) Uani ? ? 1.00000 ? ? C33 .0890(14) .845(2) .509(2) .10(2) Uani ? ? 1.00000 ? ? O33 .0118(10) .8221(15) .5442(16) .131(17) Uani ? ? 1.00000 ? ? P1 .2187(3) .5494(4) .2408(5) .056(4) Uani ? ? 1.00000 ? ? C111 .2916(12) .5298(14) .0990(16) .058(14) Uani ? ? 1.00000 ? ? C112 .3104(12) .6285(15) -.0061(16) .064(15) Uani ? ? 1.00000 ? ? C113 .3644(14) .6144(18) -.1182(18) .086(19) Uani ? ? 1.00000 ? ? C114 .3938(14) .504(2) -.125(2) .10(2) Uani ? ? 1.00000 ? ? C115 .3749(15) .4064(19) -.021(2) .10(2) Uani ? ? 1.00000 ? ? C116 .3246(14) .4210(17) .089(2) .086(19) Uani ? ? 1.00000 ? ? C121 .0971(11) .5011(15) .2172(16) .059(14) Uani ? ? 1.00000 ? ? C122 .0179(15) .5496(19) .268(2) .10(2) Uani ? ? 1.00000 ? ? C123 -.0756(14) .516(2) .260(2) .11(2) Uani ? ? 1.00000 ? ? C124 -.0916(13) .430(2) .199(2) .10(2) Uani ? ? 1.00000 ? ? C125 -.0196(15) .377(2) .149(2) .11(2) Uani ? ? 1.00000 ? ? C126 .0783(14) .4110(17) .1540(18) .080(18) Uani ? ? 1.00000 ? ? C131 .2624(11) .4381(13) .3798(16) .054(13) Uani ? ? 1.00000 ? ? C132 .2020(14) .3529(16) .4655(17) .077(17) Uani ? ? 1.00000 ? ? C133 .2433(16) .2754(18) .573(2) .10(2) Uani ? ? 1.00000 ? ? C134 .3381(17) .2755(19) .597(2) .12(2) Uani ? ? 1.00000 ? ? C135 .3984(17) .356(2) .514(2) .13(3) Uani ? ? 1.00000 ? ? C136 .3618(13) .4363(17) .405(2) .089(19) Uani ? ? 1.00000 ? ? C1 .260(3) 1.093(3) .246(3) .10(4) Uani ? ? .592(8) ? ? C1' .286(3) 1.060(4) .346(4) .07(4) Uani ? ? .408(8) ? ? C2 .1939(14) 1.0583(18) .335(2) .09(2) Uani ? ? 1.00000 ? ? H112 .28714 .70947 -.00379 .07900 Uiso ? ? 1.00000 ? ? H113 .38006 .68629 -.19253 .10600 Uiso ? ? 1.00000 ? ? H114 .42974 .49511 -.20521 .11800 Uiso ? ? 1.00000 ? ? H115 .39546 .32501 -.02462 .12900 Uiso ? ? 1.00000 ? ? H116 .31132 .35082 .16416 .11000 Uiso ? ? 1.00000 ? ? H122 .02975 .61362 .31244 .11800 Uiso ? ? 1.00000 ? ? H123 -.13116 .55560 .29593 .13200 Uiso ? ? 1.00000 ? ? H124 -.15745 .40405 .18971 .11200 Uiso ? ? 1.00000 ? ? H125 -.03490 .31071 .11035 .13100 Uiso ? ? 1.00000 ? ? H126 .13231 .37226 .11342 .09700 Uiso ? ? 1.00000 ? ? H132 .13162 .34670 .44991 .09400 Uiso ? ? 1.00000 ? ? H133 .20040 .21819 .63748 .12400 Uiso ? ? 1.00000 ? ? H134 .36302 .21663 .67412 .12800 Uiso ? ? 1.00000 ? ? H135 .47054 .35680 .52941 .14400 Uiso ? ? 1.00000 ? ? H136 .40514 .49471 .34436 .10200 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 Au .0607(5) .0485(4) .0573(4) .0047(3) -.0070(3) -.0198(3) Ru1 .0803(12) .0491(10) .0933(13) .0079(8) -.0329(10) -.0233(9) Ru2 .0795(14) .0729(13) .167(2) -.0263(11) .0499(14) -.0532(14) Ru3 .0595(10) .0860(12) .0682(10) .0053(9) -.0040(8) -.0428(10) C11 .16(2) .075(16) .12(2) .013(16) -.003(18) -.033(15) O11 .28(3) .100(13) .117(14) .033(15) -.036(15) -.016(11) C12 .16(2) .101(18) .14(2) .060(16) -.100(18) -.074(16) O12 .198(18) .092(12) .156(15) .043(11) -.113(14) -.058(11) C13 .058(15) .13(2) .20(3) .017(14) -.064(17) -.05(2) O13 .068(11) .174(18) .23(2) .007(11) -.054(12) -.012(16) C22 .030(11) .112(18) .126(18) -.004(11) .003(11) -.047(15) O22 .071(10) .123(13) .143(13) .025(9) -.010(9) -.069(11) C31 .12(2) .13(2) .107(18) .050(16) -.017(15) -.080(17) O31 .20(2) .20(2) .137(15) .058(15) -.070(14) -.122(15) C32 .120(19) .111(18) .053(12) -.015(14) .002(12) -.042(12) O32 .21(2) .116(13) .089(11) .047(13) -.042(12) -.035(10) C33 .057(14) .12(2) .107(17) -.007(13) .017(12) -.025(15) O33 .079(12) .149(15) .161(15) -.000(10) .034(11) -.037(13) P1 .055(3) .052(3) .062(3) .006(2) -.012(3) -.016(2) C111 .060(12) .053(11) .074(12) .005(9) -.020(10) -.035(10) C112 .067(13) .064(12) .067(12) .008(10) -.024(10) -.024(10) C113 .084(15) .099(17) .076(14) -.010(13) .011(12) -.029(13) C114 .059(14) .16(2) .084(15) .005(14) .003(12) -.061(16) C115 .090(17) .106(18) .13(2) .009(14) .024(15) -.063(16) C116 .085(15) .067(13) .112(17) -.008(11) .015(13) -.040(13) C121 .043(11) .067(12) .074(12) .009(9) -.002(9) -.031(10) C122 .095(17) .101(17) .116(18) -.001(14) -.023(14) -.056(15) C123 .052(14) .13(2) .16(2) .000(13) .017(14) -.061(18) C124 .041(12) .14(2) .099(16) -.007(13) -.000(12) -.017(15) C125 .072(15) .14(2) .13(2) -.057(15) -.008(14) -.057(17) C126 .079(15) .097(16) .075(13) -.006(12) .011(11) -.041(12) C131 .053(11) .044(10) .075(12) .009(8) -.014(9) -.031(9) C132 .090(15) .073(14) .066(13) -.013(11) -.015(11) -.013(11) C133 .12(2) .087(16) .085(15) -.026(14) -.019(14) -.010(13) C134 .14(2) .083(16) .111(18) -.003(15) -.067(17) .013(14) C135 .11(2) .093(18) .15(2) .022(15) -.068(18) .012(16) C136 .057(13) .080(15) .110(17) -.015(11) .001(12) .009(13) C1 .11(3) .10(3) .10(3) -.05(2) .02(2) -.05(2) C1' .09(4) .06(3) .07(3) -.02(3) .04(3) -.05(3) C2 .082(15) .090(16) .138(19) .014(12) -.040(14) -.075(15) # 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 if value to be published Au Ru1 . . 2.7488(16) ? Au Ru2 . . 3.114(2) ? Au Ru3 . . 2.742(2) ? Au C12 . . 2.59(2) ? Au P1 . . 2.305(5) ? Ru1 Ru2 . . 2.850(3) ? Ru1 Ru3 . . 2.879(2) ? Ru1 C11 . . 1.84(2) ? Ru1 C12 . . 1.92(3) ? Ru1 C13 . . 1.91(2) ? Ru1 C1 . . 2.22(4) ? Ru1 C2 . . 2.16(2) ? Ru2 Ru3 . . 2.836(3) ? Ru2 C21 . . 1.57(5) ? Ru2 C21' . . 1.94(5) ? Ru2 C22 . . 1.94(2) ? Ru2 C23 . . 1.96(4) ? Ru2 C23' . . 2.35(7) ? Ru2 C1 . . 2.11(4) ? Ru2 C1' . . 2.10(5) ? Ru3 C31 . . 1.89(2) ? Ru3 C32 . . 1.91(2) ? Ru3 C33 . . 1.900(19) ? Ru3 C1' . . 2.28(4) ? Ru3 C2 . . 2.152(18) ? C11 O11 . . 1.18(2) ? C12 O12 . . 1.13(3) ? C13 O13 . . 1.13(3) ? C21 O21 . . 1.26(7) ? C21 C21' . . .92(6) ? C21 O21' . . 1.75(6) ? O21 C21' . . 1.58(7) ? O21 O21' . . 1.56(6) ? C21' O21' . . 1.09(6) ? C22 O22 . . 1.15(3) ? C23 O23 . . 1.17(5) ? C23' O23' . . 1.11(9) ? C31 O31 . . 1.15(3) ? C32 O32 . . 1.16(2) ? C33 O33 . . 1.12(2) ? P1 C111 . . 1.820(18) ? P1 C121 . . 1.820(17) ? P1 C131 . . 1.792(15) ? C111 C112 . . 1.38(2) ? C111 C116 . . 1.37(3) ? C112 C113 . . 1.41(3) ? C112 H112 . . .995(18) ? C113 C114 . . 1.35(3) ? C113 H113 . . .994(17) ? C114 C115 . . 1.37(3) ? C114 H114 . . .98(2) ? C115 C116 . . 1.36(3) ? C115 H115 . . .99(2) ? C116 H116 . . .981(17) ? C121 C122 . . 1.38(3) ? C121 C126 . . 1.40(3) ? C122 C123 . . 1.36(3) ? C122 H122 . . .99(2) ? C123 C124 . . 1.33(4) ? C123 H123 . . 1.01(2) ? C124 C125 . . 1.33(3) ? C124 H124 . . .98(2) ? C125 C126 . . 1.42(3) ? C125 H125 . . .98(3) ? C126 H126 . . 1.00(2) ? C131 C132 . . 1.40(2) ? C131 C136 . . 1.41(2) ? C132 C133 . . 1.38(3) ? C132 H132 . . 1.00(2) ? C133 C134 . . 1.34(3) ? C133 H133 . . .99(2) ? C134 C135 . . 1.35(3) ? C134 H134 . . .98(2) ? C135 C136 . . 1.38(3) ? C135 H135 . . 1.02(2) ? C136 H136 . . .982(18) ? C1 C1' . . 1.09(5) ? C1 C2 . . 1.26(4) ? C1' C2 . . 1.28(5) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES if value to be published Ru1 Au Ru2 . . . 57.76(5) ? Ru1 Au Ru3 . . . 63.25(5) ? Ru1 Au C12 . . . 42.1(6) ? Ru1 Au P1 . . . 147.64(12) ? Ru2 Au Ru3 . . . 57.50(6) ? Ru2 Au C12 . . . 83.0(5) ? Ru2 Au P1 . . . 139.05(12) ? Ru3 Au C12 . . . 105.2(6) ? Ru3 Au P1 . . . 146.28(12) ? C12 Au P1 . . . 106.1(6) ? Au Ru1 Ru2 . . . 67.57(5) ? Au Ru1 Ru3 . . . 58.25(5) ? Au Ru1 C11 . . . 150.5(8) ? Au Ru1 C12 . . . 64.5(6) ? Au Ru1 C13 . . . 101.2(7) ? Au Ru1 C1 . . . 109.4(9) ? Au Ru1 C2 . . . 105.4(5) ? Ru2 Ru1 Ru3 . . . 59.34(6) ? Ru2 Ru1 C11 . . . 106.3(8) ? Ru2 Ru1 C12 . . . 103.9(7) ? Ru2 Ru1 C13 . . . 150.8(8) ? Ru2 Ru1 C1 . . . 47.3(9) ? Ru2 Ru1 C2 . . . 67.6(5) ? Ru3 Ru1 C11 . . . 145.3(8) ? Ru3 Ru1 C12 . . . 122.5(6) ? Ru3 Ru1 C13 . . . 91.7(8) ? Ru3 Ru1 C1 . . . 66.5(8) ? Ru3 Ru1 C2 . . . 48.0(5) ? C11 Ru1 C12 . . . 90.7(10) ? C11 Ru1 C13 . . . 96.1(10) ? C11 Ru1 C1 . . . 80.7(11) ? C11 Ru1 C2 . . . 97.9(9) ? C12 Ru1 C13 . . . 94.1(11) ? C12 Ru1 C1 . . . 144.0(12) ? C12 Ru1 C2 . . . 169.3(8) ? C13 Ru1 C1 . . . 121.5(13) ? C13 Ru1 C2 . . . 91.3(10) ? C1 Ru1 C2 . . . 33.4(10) ? Au Ru2 Ru1 . . . 54.67(5) ? Au Ru2 Ru3 . . . 54.63(5) ? Au Ru2 C21 . . . 165.2(16) ? Au Ru2 C21' . . . 158.9(17) ? Au Ru2 C22 . . . 67.3(5) ? Au Ru2 C23 . . . 101.2(12) ? Au Ru2 C23' . . . 106.0(17) ? Au Ru2 C1 . . . 100.3(10) ? Au Ru2 C1' . . . 102.1(11) ? Ru1 Ru2 Ru3 . . . 60.84(6) ? Ru1 Ru2 C21 . . . 138.7(17) ? Ru1 Ru2 C21' . . . 126.8(14) ? Ru1 Ru2 C22 . . . 114.9(6) ? Ru1 Ru2 C23 . . . 75.3(11) ? Ru1 Ru2 C23' . . . 139.7(17) ? Ru1 Ru2 C1 . . . 50.4(10) ? Ru1 Ru2 C1' . . . 69.0(12) ? Ru3 Ru2 C21 . . . 121.7(18) ? Ru3 Ru2 C21' . . . 146.5(17) ? Ru3 Ru2 C22 . . . 107.6(5) ? Ru3 Ru2 C23 . . . 136.2(11) ? Ru3 Ru2 C23' . . . 79.0(17) ? Ru3 Ru2 C1 . . . 68.5(9) ? Ru3 Ru2 C1' . . . 52.4(10) ? C21 Ru2 C21' . . . 28(2) ? C21 Ru2 C22 . . . 103.6(19) ? C21 Ru2 C23 . . . 90(2) ? C21 Ru2 C23' . . . 60(2) ? C21 Ru2 C1 . . . 90(2) ? C21 Ru2 C1' . . . 82(2) ? C21' Ru2 C22 . . . 97.7(17) ? C21' Ru2 C23 . . . 63(2) ? C21' Ru2 C23' . . . 85(2) ? C21' Ru2 C1 . . . 91.9(18) ? C21' Ru2 C1' . . . 97(2) ? C22 Ru2 C23 . . . 90.8(13) ? C22 Ru2 C23' . . . 79(2) ? C22 Ru2 C1 . . . 165.2(12) ? C22 Ru2 C1' . . . 156.4(11) ? C23 Ru2 C23' . . . 145(2) ? C23 Ru2 C1 . . . 83.5(15) ? C23 Ru2 C1' . . . 112.3(16) ? C23' Ru2 C1 . . . 113(2) ? C23' Ru2 C1' . . . 84(2) ? C1 Ru2 C1' . . . 30.0(14) ? Au Ru3 Ru1 . . . 58.50(5) ? Au Ru3 Ru2 . . . 67.87(6) ? Au Ru3 C31 . . . 158.2(7) ? Au Ru3 C32 . . . 67.1(6) ? Au Ru3 C33 . . . 95.5(8) ? Au Ru3 C1' . . . 109.4(12) ? Au Ru3 C2 . . . 105.9(6) ? Ru1 Ru3 Ru2 . . . 59.82(6) ? Ru1 Ru3 C31 . . . 142.4(7) ? Ru1 Ru3 C32 . . . 125.6(6) ? Ru1 Ru3 C33 . . . 90.5(6) ? Ru1 Ru3 C1' . . . 66.5(11) ? Ru1 Ru3 C2 . . . 48.3(6) ? Ru2 Ru3 C31 . . . 113.7(7) ? Ru2 Ru3 C32 . . . 99.5(6) ? Ru2 Ru3 C33 . . . 150.2(6) ? Ru2 Ru3 C1' . . . 47.0(11) ? Ru2 Ru3 C2 . . . 68.0(6) ? C31 Ru3 C32 . . . 91.6(9) ? C31 Ru3 C33 . . . 91.1(10) ? C31 Ru3 C1' . . . 82.7(13) ? C31 Ru3 C2 . . . 94.1(9) ? C32 Ru3 C33 . . . 95.9(9) ? C32 Ru3 C1' . . . 137.1(13) ? C32 Ru3 C2 . . . 167.5(8) ? C33 Ru3 C1' . . . 126.6(13) ? C33 Ru3 C2 . . . 95.1(8) ? C1' Ru3 C2 . . . 33.6(12) ? Ru1 C11 O11 . . . 178(2) ? Au C12 Ru1 . . . 73.4(8) ? Au C12 O12 . . . 118.1(16) ? Ru1 C12 O12 . . . 168.3(17) ? Ru1 C13 O13 . . . 174(2) ? Ru2 C21 O21 . . . 169(4) ? Ru2 C21 C21' . . . 99(5) ? Ru2 C21 O21' . . . 132(3) ? O21 C21 C21' . . . 92(5) ? O21 C21 O21' . . . 60(3) ? C21' C21 O21' . . . 32(4) ? C21 O21 C21' . . . 35(3) ? C21 O21 O21' . . . 76(3) ? C21' O21 O21' . . . 41(3) ? Ru2 C21' C21 . . . 53(4) ? Ru2 C21' O21 . . . 106(3) ? Ru2 C21' O21' . . . 173(4) ? C21 C21' O21 . . . 53(4) ? C21 C21' O21' . . . 121(7) ? O21 C21' O21' . . . 68(4) ? C21 O21' O21 . . . 44(2) ? C21 O21' C21' . . . 27(3) ? O21 O21' C21' . . . 71(4) ? Ru2 C22 O22 . . . 174.1(17) ? Ru2 C23 O23 . . . 178(4) ? Ru2 C23' O23' . . . 168(6) ? Ru3 C31 O31 . . . 177.4(19) ? Ru3 C32 O32 . . . 171(2) ? Ru3 C33 O33 . . . 177(2) ? Au P1 C111 . . . 115.6(5) ? Au P1 C121 . . . 111.1(6) ? Au P1 C131 . . . 113.8(6) ? C111 P1 C121 . . . 105.4(8) ? C111 P1 C131 . . . 104.4(7) ? C121 P1 C131 . . . 105.7(7) ? P1 C111 C112 . . . 118.4(13) ? P1 C111 C116 . . . 123.2(12) ? C112 C111 C116 . . . 118.3(17) ? C111 C112 C113 . . . 119.2(17) ? C111 C112 H112 . . . 121.2(17) ? C113 C112 H112 . . . 119.6(15) ? C112 C113 C114 . . . 120.5(16) ? C112 C113 H113 . . . 119(2) ? C114 C113 H113 . . . 120(2) ? C113 C114 C115 . . . 120(2) ? C113 C114 H114 . . . 120.0(19) ? C115 C114 H114 . . . 120(2) ? C114 C115 C116 . . . 119(2) ? C114 C115 H115 . . . 121(2) ? C116 C115 H115 . . . 119.9(18) ? C111 C116 C115 . . . 122.7(17) ? C111 C116 H116 . . . 118(2) ? C115 C116 H116 . . . 119(2) ? P1 C121 C122 . . . 120.1(16) ? P1 C121 C126 . . . 123.3(13) ? C122 C121 C126 . . . 116.5(17) ? C121 C122 C123 . . . 124(2) ? C121 C122 H122 . . . 118(2) ? C123 C122 H122 . . . 118(2) ? C122 C123 C124 . . . 118(2) ? C122 C123 H123 . . . 121(3) ? C124 C123 H123 . . . 121(2) ? C123 C124 C125 . . . 122(2) ? C123 C124 H124 . . . 121(2) ? C125 C124 H124 . . . 118(2) ? C124 C125 C126 . . . 122(2) ? C124 C125 H125 . . . 119(2) ? C126 C125 H125 . . . 119(2) ? C121 C126 C125 . . . 117.5(18) ? C121 C126 H126 . . . 121.1(18) ? C125 C126 H126 . . . 121(2) ? P1 C131 C132 . . . 122.8(13) ? P1 C131 C136 . . . 119.1(11) ? C132 C131 C136 . . . 118.1(14) ? C131 C132 C133 . . . 117.4(17) ? C131 C132 H132 . . . 121.9(15) ? C133 C132 H132 . . . 120.6(17) ? C132 C133 C134 . . . 123.9(18) ? C132 C133 H133 . . . 118(2) ? C134 C133 H133 . . . 118.0(19) ? C133 C134 C135 . . . 120(2) ? C133 C134 H134 . . . 120(2) ? C135 C134 H134 . . . 121(2) ? C134 C135 C136 . . . 119(2) ? C134 C135 H135 . . . 121(2) ? C136 C135 H135 . . . 119(2) ? C131 C136 C135 . . . 121.3(17) ? C131 C136 H136 . . . 118.7(17) ? C135 C136 H136 . . . 120.0(19) ? Ru1 C1 Ru2 . . . 82.3(14) ? Ru1 C1 C1' . . . 116(3) ? Ru1 C1 C2 . . . 71(2) ? Ru2 C1 C1' . . . 74(3) ? Ru2 C1 C2 . . . 113(2) ? C1' C1 C2 . . . 66(3) ? Ru2 C1' Ru3 . . . 80.6(15) ? Ru2 C1' C1 . . . 76(3) ? Ru2 C1' C2 . . . 112(3) ? Ru3 C1' C1 . . . 110(4) ? Ru3 C1' C2 . . . 67.8(19) ? C1 C1' C2 . . . 63(3) ? Ru1 C2 Ru3 . . . 83.7(8) ? Ru1 C2 C1 . . . 76(2) ? Ru1 C2 C1' . . . 110(2) ? Ru3 C2 C1 . . . 111(2) ? Ru3 C2 C1' . . . 78.6(19) ? C1 C2 C1' . . . 51(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 if 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 if value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Additional items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Additional 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 Au O12 3.275(16) . . ? Au C13 3.64(2) . . ? Au C22 2.965(17) . . ? Au O22 3.521(13) . . ? Au C32 2.661(18) . . ? Au O32 3.320(15) . . ? Au C33 3.48(2) . . ? Au C111 3.500(18) . . ? Au C112 3.637(19) . . ? Au C121 3.413(18) . . ? Au C122 3.55(2) . . ? Au C131 3.442(15) . . ? Au H112 3.0796(9) . . ? Au H122 2.9494(10) . . ? Ru1 O11 3.011(15) . . ? Ru1 O12 3.038(18) . . ? Ru1 O13 3.034(15) . . ? Ru1 C23 3.02(4) . . ? Ru1 O23 3.69(3) . . ? Ru1 C33 3.46(2) . . ? Ru1 C1' 2.87(5) . . ? Ru2 O21 2.81(4) . . ? Ru2 O21' 3.03(4) . . ? Ru2 O22 3.085(15) . . ? Ru2 O23 3.14(3) . . ? Ru2 O23' 3.43(5) . . ? Ru2 C32 3.669(17) . . ? Ru2 C2 2.85(2) . . ? Ru3 C13 3.50(2) . . ? Ru3 C23' 3.32(7) . . ? Ru3 O31 3.04(2) . . ? Ru3 O32 3.059(15) . . ? Ru3 O33 3.022(14) . . ? Ru3 C1 2.85(3) . . ? C11 C12 2.67(3) . . ? C11 C13 2.79(3) . . ? C11 C1 2.64(4) . . ? C12 C13 2.81(4) . . ? O12 H112 2.574(17) . . ? O12 H125 2.525(17) . '2 565' ? C13 C33 2.96(3) . . ? C13 C2 2.92(3) . . ? C21 C22 2.77(6) . . ? C21 C23 2.52(6) . . ? C21 C23' 2.07(7) . . ? C21 O23' 2.98(8) . '2 676' ? C21 C1 2.64(6) . . ? C21 C1' 2.44(6) . . ? O21 C23' 2.45(7) . . ? O21 O23' 2.19(7) . '2 676' ? C21' C22 2.93(6) . . ? C21' C23 2.04(7) . . ? C21' O23 2.84(6) . . ? C21' C23' 2.90(8) . . ? C21' C1 2.92(6) . . ? O21' C23 2.84(6) . . ? C22 C23 2.78(4) . . ? C22 C23' 2.75(8) . . ? C23 C1 2.72(6) . . ? C23' O23' 2.75(9) . '2 676' ? C23' C1' 2.98(8) . . ? O23' O23' 2.55(7) . '2 676' ? C31 C32 2.72(3) . . ? C31 C33 2.71(3) . . ? C31 C1' 2.77(4) . . ? C31 C2 2.97(3) . . ? C32 C33 2.83(3) . . ? C33 C2 2.99(3) . . ? P1 C112 2.754(17) . . ? P1 C116 2.81(2) . . ? P1 C122 2.78(2) . . ? P1 C126 2.84(2) . . ? P1 C132 2.805(16) . . ? P1 C136 2.77(2) . . ? P1 H112 2.857(4) . . ? P1 H122 2.837(5) . . ? P1 H136 2.839(5) . . ? C111 C113 2.40(2) . . ? C111 C114 2.76(3) . . ? C111 C115 2.39(3) . . ? C111 C121 2.90(2) . . ? C111 C131 2.85(2) . . ? C111 H112 2.074(14) . . ? C111 H116 2.023(15) . . ? C112 C114 2.40(3) . . ? C112 C115 2.76(3) . . ? C112 C116 2.35(2) . . ? C112 H113 2.080(16) . . ? C113 C115 2.36(3) . . ? C113 C116 2.71(2) . . ? C113 H112 2.09(2) . . ? C113 H114 2.03(2) . . ? C114 C116 2.35(3) . . ? C114 H113 2.05(2) . . ? C114 H115 2.07(2) . . ? C115 H114 2.05(2) . . ? C115 H116 2.03(2) . . ? C116 H115 2.05(2) . . ? C121 C123 2.42(2) . . ? C121 C124 2.77(2) . . ? C121 C125 2.41(3) . . ? C121 C131 2.88(2) . . ? C121 H122 2.036(18) . . ? C121 H126 2.105(19) . . ? C121 H132 2.668(15) . . ? C122 C124 2.31(3) . . ? C122 C125 2.67(4) . . ? C122 C126 2.36(3) . . ? C122 H123 2.07(2) . . ? C123 C125 2.32(4) . . ? C123 C126 2.77(3) . . ? C123 H122 2.03(2) . . ? C123 H124 2.01(2) . . ? C124 C126 2.40(3) . . ? C124 H123 2.04(2) . . ? C124 H125 1.99(2) . . ? C125 H124 1.98(2) . . ? C125 H126 2.12(2) . . ? C126 H125 2.08(2) . . ? C131 C133 2.37(2) . . ? C131 C134 2.78(2) . . ? C131 C135 2.43(3) . . ? C131 H132 2.102(15) . . ? C131 H136 2.068(15) . . ? C132 C134 2.40(3) . . ? C132 C135 2.79(3) . . ? C132 C136 2.41(3) . . ? C132 H133 2.043(16) . . ? C133 C135 2.33(3) . . ? C133 C136 2.70(3) . . ? C133 H132 2.07(2) . . ? C133 H134 2.02(2) . . ? C134 C136 2.36(3) . . ? C134 H133 2.01(2) . . ? C134 H135 2.07(2) . . ? C135 H134 2.03(2) . . ? C135 H136 2.06(2) . . ? C136 H135 2.074(19) . . ? H112 H113 2.3811(4) . . ? H113 H114 2.3484(4) . . ? H114 H115 2.3722(3) . . ? H115 H116 2.3329(4) . . ? H122 H123 2.3511(6) . . ? H123 H124 2.3435(3) . . ? H124 H125 2.2505(4) . . ? H132 H133 2.3564(3) . . ? H133 H134 2.2943(6) . . ? H134 H135 2.3795(3) . . ? H135 H136 2.3663(3) . . ? _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 C29_H18_Au_O9_P_Ru3 _chemical_formula_structural [HAu(PPH3)Ru3C2H2(CO)9] _exptl_crystal_F_000 1960 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 7 6 7 9 0 0 0 10 0 0 0 7 -7 -6 -7 -9 0 0 0 -10 0 0 0 -7 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min -13 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _reflns_number_observed 5646 _reflns_d_resolution_high ? _reflns_d_resolution_low ? _diffrn_reflns_av_sigmaI/netI .073 _diffrn_reflns_theta_min 1.8 _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 atomblock _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.059 _refine_ls_wR_factor_all 0.057 _refine_ls_goodness_of_fit_all 1.472 _refine_ls_shift/su_mean .00766 data_br535l # 2. EXPERIMENTAL DATA #--------------------- _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _chemical_formula_sum 'C29 H18 Au1 O9 P1 Ru3' _chemical_formula_moiety ? _chemical_formula_weight 1041.6 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 12.9880(10) _cell_length_b 15.539(2) _cell_length_c 16.129(2) _cell_angle_alpha 90.00000 _cell_angle_beta 105.509(2) _cell_angle_gamma 90.00000 _cell_volume 3136.6(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.205 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5468 _cell_measurement_theta_min 0 _cell_measurement_theta_max 30 _cell_measurement_temperature 153 _exptl_absorpt_coefficient_mu 6.03 _exptl_crystal_description prism _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Bruker SADABS' _exptl_absorpt_correction_T_min 0.389 _exptl_absorpt_correction_T_max 0.625 _diffrn_reflns_number 7930 _reflns_number_total 7930 _reflns_Friedel_coverage 0 _reflns_number_gt 6284 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.4 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _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 .035 _refine_ls_wR_factor_ref .037 _refine_ls_goodness_of_fit_ref 1.216 _refine_ls_number_reflns 6284 _refine_ls_number_parameters 456 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refined _refine_ls_shift/su_max .099 _refine_diff_density_min -1.3 _refine_diff_density_max 2.06 _refine_ls_extinction_method none _refine_ls_extinction_coef .00000 _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack 0 # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Bruker SMART software' _computing_cell_refinement 'Bruker SMART software' _computing_data_reduction 'Bruker SAINT software' _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 ? 0 116 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 36 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 68 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 4 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 12 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 4 -2.688 8.798 '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 Au .973889(16) .740159(13) .722264(13) .02486(10) Uani ? ? 1.00000 ? ? Ru1 1.07339(3) .64554(3) .62443(3) .02352(19) Uani ? ? 1.00000 ? ? Ru2 1.28069(3) .69212(3) .75191(3) .0245(2) Uani ? ? 1.00000 ? ? Ru3 1.14243(3) .81928(3) .67460(3) .0266(2) Uani ? ? 1.00000 ? ? C11 1.1109(5) .5560(4) .5570(4) .039(3) Uani ? ? 1.00000 ? ? O11 1.1326(4) .5043(3) .5147(3) .065(3) Uani ? ? 1.00000 ? ? C12 .9983(4) .5670(3) .6837(3) .030(3) Uani ? ? 1.00000 ? ? O12 .9568(4) .5155(3) .7128(3) .046(2) Uani ? ? 1.00000 ? ? C13 .9472(5) .6800(4) .5395(4) .035(3) Uani ? ? 1.00000 ? ? O13 .8709(3) .6998(3) .4898(3) .049(2) Uani ? ? 1.00000 ? ? C21 1.3808(4) .6032(4) .7555(4) .034(3) Uani ? ? 1.00000 ? ? O21 1.4431(4) .5509(3) .7550(3) .056(3) Uani ? ? 1.00000 ? ? C22 1.2387(5) .6659(3) .8574(3) .032(3) Uani ? ? 1.00000 ? ? O22 1.2086(4) .6498(3) .9155(3) .046(2) Uani ? ? 1.00000 ? ? C23 1.3859(5) .7746(4) .8026(3) .035(3) Uani ? ? 1.00000 ? ? O23 1.4515(3) .8230(3) .8332(3) .046(2) Uani ? ? 1.00000 ? ? C31 1.2374(5) .9102(4) .6731(4) .037(3) Uani ? ? 1.00000 ? ? O31 1.2966(4) .9650(3) .6714(3) .052(2) Uani ? ? 1.00000 ? ? C32 1.1331(4) .8528(4) .7881(4) .034(3) Uani ? ? 1.00000 ? ? O32 1.1368(4) .8762(3) .8555(3) .048(2) Uani ? ? 1.00000 ? ? C33 1.0244(5) .8774(4) .5960(4) .040(3) Uani ? ? 1.00000 ? ? O33 .9558(4) .9117(3) .5483(3) .060(3) Uani ? ? 1.00000 ? ? P1 .83358(11) .76204(8) .78131(8) .0236(6) Uani ? ? 1.00000 ? ? C111 .8023(4) .6725(3) .8419(3) .027(2) Uani ? ? 1.00000 ? ? C112 .8784(6) .6076(4) .8714(4) .038(3) Uani ? ? 1.00000 ? ? C113 .8540(6) .5383(4) .9176(4) .045(3) Uani ? ? 1.00000 ? ? C114 .7573(6) .5325(4) .9358(4) .048(4) Uani ? ? 1.00000 ? ? C115 .6795(6) .5950(4) .9066(4) .046(3) Uani ? ? 1.00000 ? ? C116 .7021(5) .6641(4) .8587(4) .042(3) Uani ? ? 1.00000 ? ? C121 .7089(4) .7823(3) .6984(3) .026(2) Uani ? ? 1.00000 ? ? C122 .6931(5) .7396(4) .6198(4) .033(3) Uani ? ? 1.00000 ? ? C123 .5980(5) .7523(4) .5563(4) .037(3) Uani ? ? 1.00000 ? ? C124 .5206(5) .8049(4) .5718(4) .035(3) Uani ? ? 1.00000 ? ? C125 .5362(5) .8478(4) .6491(4) .035(3) Uani ? ? 1.00000 ? ? C126 .6318(4) .8371(3) .7125(4) .031(3) Uani ? ? 1.00000 ? ? C131 .8475(4) .8558(4) .8503(3) .029(3) Uani ? ? 1.00000 ? ? C132 .8395(5) .8516(4) .9342(3) .033(3) Uani ? ? 1.00000 ? ? C133 .8502(5) .9256(4) .9853(4) .038(3) Uani ? ? 1.00000 ? ? C134 .8683(5) 1.0045(4) .9501(4) .046(3) Uani ? ? 1.00000 ? ? C135 .8753(5) 1.0090(4) .8671(5) .046(3) Uani ? ? 1.00000 ? ? C136 .8664(5) .9342(4) .8176(4) .039(3) Uani ? ? 1.00000 ? ? C1 1.2660(5) .7427(4) .6308(4) .033(3) Uani ? ? 1.00000 ? ? C2 1.1678(5) .7296(4) .5750(4) .034(3) Uani ? ? 1.00000 ? ? H112 .944(4) .610(4) .858(3) .031(16) Uiso ? ? 1.00000 ? ? H113 .915(6) .493(5) .945(4) .07(2) Uiso ? ? 1.00000 ? ? H114 .749(6) .479(5) .980(4) .08(3) Uiso ? ? 1.00000 ? ? H115 .605(6) .595(4) .927(4) .06(2) Uiso ? ? 1.00000 ? ? H116 .659(8) .710(6) .856(6) .12(4) Uiso ? ? 1.00000 ? ? H122 .754(5) .703(4) .606(4) .042(17) Uiso ? ? 1.00000 ? ? H123 .599(6) .733(4) .500(5) .06(2) Uiso ? ? 1.00000 ? ? H124 .468(5) .814(3) .527(4) .031(15) Uiso ? ? 1.00000 ? ? H125 .479(5) .887(4) .656(4) .048(18) Uiso ? ? 1.00000 ? ? H126 .641(4) .868(3) .766(3) .027(14) Uiso ? ? 1.00000 ? ? H132 .832(5) .796(4) .970(4) .048(18) Uiso ? ? 1.00000 ? ? H133 .847(4) .919(3) 1.042(3) .031(15) Uiso ? ? 1.00000 ? ? H134 .882(5) 1.055(4) .991(4) .06(2) Uiso ? ? 1.00000 ? ? H135 .900(5) 1.059(4) .835(4) .045(18) Uiso ? ? 1.00000 ? ? H136 .871(4) .947(3) .764(3) .014(12) Uiso ? ? 1.00000 ? ? H1 1.310(4) .764(3) .614(3) .019(15) Uiso ? ? 1.00000 ? ? H2 1.159(4) .744(3) .521(3) .007(11) 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 Au .02477(11) .02507(11) .02523(11) .00161(8) .00755(8) -.00160(8) Ru1 .0241(2) .0212(2) .0247(2) -.00127(16) .00556(17) -.00390(16) Ru2 .0249(2) .0216(2) .0255(2) -.00202(16) .00395(17) -.00262(16) Ru3 .0277(2) .0190(2) .0336(2) -.00050(16) .00898(19) -.00076(16) C11 .028(3) .038(3) .051(4) -.004(2) .010(3) -.013(3) O11 .049(3) .060(3) .095(4) -.015(2) .032(3) -.051(3) C12 .032(3) .024(3) .032(3) -.001(2) .004(2) -.003(2) O12 .056(3) .030(2) .059(3) -.006(2) .025(2) .001(2) C13 .042(3) .033(3) .032(3) .004(3) .010(3) -.002(2) O13 .041(3) .069(3) .031(2) .014(2) .001(2) .003(2) C21 .027(3) .034(3) .040(3) -.002(2) .005(3) -.007(2) O21 .042(3) .042(3) .079(3) .011(2) .010(2) -.007(2) C22 .037(3) .026(3) .028(3) -.005(2) .002(2) -.003(2) O22 .060(3) .040(3) .038(2) -.003(2) .016(2) .0023(19) C23 .040(3) .039(3) .025(3) -.009(3) .010(3) -.002(2) O23 .048(3) .055(3) .034(2) -.024(2) .010(2) -.010(2) C31 .037(3) .027(3) .049(4) .001(2) .016(3) -.003(3) O31 .051(3) .025(2) .083(3) -.011(2) .026(3) -.008(2) C32 .032(3) .032(3) .036(3) -.002(2) .005(3) -.002(2) O32 .048(3) .048(3) .046(3) .003(2) .008(2) -.014(2) C33 .053(4) .029(3) .047(4) .001(3) .028(3) .003(3) O33 .052(3) .051(3) .072(3) .021(2) .007(3) .023(3) P1 .0245(7) .0227(7) .0234(6) .0004(5) .0063(5) -.0008(5) C111 .026(3) .027(3) .027(3) -.001(2) .005(2) -.001(2) C112 .050(4) .030(3) .033(3) .007(3) .011(3) .000(2) C113 .067(5) .032(3) .036(3) .006(3) .013(3) .001(3) C114 .075(5) .034(3) .032(3) -.009(3) .008(3) .007(3) C115 .050(4) .045(4) .044(4) -.010(3) .015(3) .010(3) C116 .042(4) .037(4) .047(4) -.000(3) .011(3) .008(3) C121 .033(3) .021(2) .022(2) -.002(2) .006(2) .002(2) C122 .036(3) .033(3) .030(3) -.004(2) .009(2) -.003(2) C123 .038(3) .043(3) .026(3) -.010(3) .004(2) -.002(2) C124 .028(3) .038(3) .030(3) -.006(2) -.007(3) .007(2) C125 .027(3) .035(3) .041(3) .005(2) .002(3) .005(3) C126 .028(3) .027(3) .033(3) .002(2) .001(2) -.004(2) C131 .021(3) .033(3) .031(3) -.001(2) .002(2) -.004(2) C132 .036(3) .034(3) .025(3) .006(2) .002(2) -.004(2) C133 .041(3) .044(4) .026(3) .009(3) .004(3) -.009(2) C134 .041(4) .042(4) .051(4) -.000(3) .006(3) -.022(3) C135 .048(4) .032(3) .062(4) -.011(3) .022(3) -.009(3) C136 .048(4) .031(3) .040(3) -.006(3) .016(3) -.004(3) C1 .041(3) .028(3) .029(3) -.006(3) .008(3) -.001(2) C2 .043(3) .031(3) .032(3) .000(3) .016(3) -.002(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES if value to be published Au Ru1 . . 2.7226(5) ? Au Ru3 . . 2.7919(5) ? Au P1 . . 2.2960(15) ? Ru1 Ru2 . . 3.0066(6) ? Ru1 Ru3 . . 2.8913(7) ? Ru1 C11 . . 1.908(7) ? Ru1 C12 . . 1.963(6) ? Ru1 C13 . . 1.910(5) ? Ru1 C2 . . 2.090(7) ? Ru2 Ru3 . . 2.7361(6) ? Ru2 C21 . . 1.888(6) ? Ru2 C22 . . 1.963(6) ? Ru2 C23 . . 1.892(6) ? Ru2 C1 . . 2.066(6) ? Ru3 C31 . . 1.880(6) ? Ru3 C32 . . 1.938(6) ? Ru3 C33 . . 1.932(6) ? Ru3 C1 . . 2.258(7) ? Ru3 C2 . . 2.217(6) ? C11 O11 . . 1.137(9) ? C12 O12 . . 1.134(8) ? C13 O13 . . 1.137(7) ? C21 O21 . . 1.147(8) ? C22 O22 . . 1.136(8) ? C23 O23 . . 1.144(7) ? C31 O31 . . 1.152(8) ? C32 O32 . . 1.136(8) ? C33 O33 . . 1.142(7) ? P1 C111 . . 1.808(6) ? P1 C121 . . 1.831(5) ? P1 C131 . . 1.813(6) ? C111 C112 . . 1.403(8) ? C111 C116 . . 1.405(9) ? C112 C113 . . 1.394(9) ? C112 H112 . . .93(6) ? C113 C114 . . 1.367(12) ? C113 H113 . . 1.06(7) ? C114 C115 . . 1.390(10) ? C114 H114 . . 1.11(8) ? C115 C116 . . 1.399(10) ? C115 H115 . . 1.10(8) ? C116 H116 . . .89(10) ? C121 C122 . . 1.397(8) ? C121 C126 . . 1.379(8) ? C122 C123 . . 1.391(8) ? C122 H122 . . 1.05(7) ? C123 C124 . . 1.369(9) ? C123 H123 . . .95(8) ? C124 C125 . . 1.381(8) ? C124 H124 . . .86(5) ? C125 C126 . . 1.391(7) ? C125 H125 . . 1.00(7) ? C126 H126 . . .97(5) ? C131 C132 . . 1.386(8) ? C131 C136 . . 1.374(8) ? C132 C133 . . 1.400(8) ? C132 H132 . . 1.05(7) ? C133 C134 . . 1.397(10) ? C133 H133 . . .93(6) ? C134 C135 . . 1.368(11) ? C134 H134 . . 1.01(7) ? C135 C136 . . 1.397(9) ? C135 H135 . . 1.03(7) ? C136 H136 . . .91(5) ? C1 C2 . . 1.366(8) ? C1 H1 . . .78(6) ? C2 H2 . . .88(5) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES if value to be published Ru1 Au Ru3 . . . 63.229(15) ? Ru1 Au P1 . . . 150.78(3) ? Ru3 Au P1 . . . 144.76(3) ? Au Ru1 Ru2 . . . 87.174(16) ? Au Ru1 Ru3 . . . 59.555(14) ? Au Ru1 C11 . . . 163.2(2) ? Au Ru1 C12 . . . 71.27(17) ? Au Ru1 C13 . . . 79.3(2) ? Au Ru1 C2 . . . 107.53(17) ? Ru2 Ru1 Ru3 . . . 55.237(12) ? Ru2 Ru1 C11 . . . 104.31(16) ? Ru2 Ru1 C12 . . . 106.70(14) ? Ru2 Ru1 C13 . . . 149.61(17) ? Ru2 Ru1 C2 . . . 66.50(15) ? Ru3 Ru1 C11 . . . 137.2(2) ? Ru3 Ru1 C12 . . . 126.99(16) ? Ru3 Ru1 C13 . . . 94.66(17) ? Ru3 Ru1 C2 . . . 49.72(17) ? C11 Ru1 C12 . . . 93.4(3) ? C11 Ru1 C13 . . . 95.5(2) ? C11 Ru1 C2 . . . 88.5(3) ? C12 Ru1 C13 . . . 94.6(2) ? C12 Ru1 C2 . . . 173.2(2) ? C13 Ru1 C2 . . . 91.7(2) ? Ru1 Ru2 Ru3 . . . 60.241(15) ? Ru1 Ru2 C21 . . . 109.17(16) ? Ru1 Ru2 C22 . . . 97.88(16) ? Ru1 Ru2 C23 . . . 150.43(17) ? Ru1 Ru2 C1 . . . 66.77(17) ? Ru3 Ru2 C21 . . . 154.88(18) ? Ru3 Ru2 C22 . . . 104.12(16) ? Ru3 Ru2 C23 . . . 91.03(17) ? Ru3 Ru2 C1 . . . 53.92(18) ? C21 Ru2 C22 . . . 99.8(2) ? C21 Ru2 C23 . . . 94.1(2) ? C21 Ru2 C1 . . . 101.3(3) ? C22 Ru2 C23 . . . 95.8(2) ? C22 Ru2 C1 . . . 157.1(2) ? C23 Ru2 C1 . . . 91.4(2) ? Au Ru3 Ru1 . . . 57.217(13) ? Au Ru3 Ru2 . . . 91.367(18) ? Au Ru3 C31 . . . 154.2(2) ? Au Ru3 C32 . . . 66.82(17) ? Au Ru3 C33 . . . 81.0(2) ? Au Ru3 C1 . . . 121.94(16) ? Au Ru3 C2 . . . 101.67(17) ? Ru1 Ru3 Ru2 . . . 64.522(15) ? Ru1 Ru3 C31 . . . 148.6(2) ? Ru1 Ru3 C32 . . . 114.98(17) ? Ru1 Ru3 C33 . . . 96.92(17) ? Ru1 Ru3 C1 . . . 67.25(15) ? Ru1 Ru3 C2 . . . 46.01(17) ? Ru2 Ru3 C31 . . . 101.28(17) ? Ru2 Ru3 C32 . . . 87.88(16) ? Ru2 Ru3 C33 . . . 160.97(17) ? Ru2 Ru3 C1 . . . 47.69(15) ? Ru2 Ru3 C2 . . . 70.73(14) ? C31 Ru3 C32 . . . 91.0(3) ? C31 Ru3 C33 . . . 92.8(3) ? C31 Ru3 C1 . . . 82.4(3) ? C31 Ru3 C2 . . . 103.7(3) ? C32 Ru3 C33 . . . 104.8(3) ? C32 Ru3 C1 . . . 131.8(2) ? C32 Ru3 C2 . . . 155.9(2) ? C33 Ru3 C1 . . . 123.1(3) ? C33 Ru3 C2 . . . 93.6(2) ? C1 Ru3 C2 . . . 35.5(2) ? Ru1 C11 O11 . . . 177.9(6) ? Ru1 C12 O12 . . . 173.3(5) ? Ru1 C13 O13 . . . 178.8(6) ? Ru2 C21 O21 . . . 177.1(6) ? Ru2 C22 O22 . . . 176.0(5) ? Ru2 C23 O23 . . . 178.3(6) ? Ru3 C31 O31 . . . 178.8(6) ? Ru3 C32 O32 . . . 173.4(5) ? Ru3 C33 O33 . . . 178.7(7) ? Au P1 C111 . . . 115.35(19) ? Au P1 C121 . . . 111.6(2) ? Au P1 C131 . . . 114.4(2) ? C111 P1 C121 . . . 104.2(2) ? C111 P1 C131 . . . 106.7(3) ? C121 P1 C131 . . . 103.5(2) ? P1 C111 C112 . . . 119.8(5) ? P1 C111 C116 . . . 122.0(4) ? C112 C111 C116 . . . 118.2(5) ? C111 C112 C113 . . . 119.8(7) ? C111 C112 H112 . . . 120(3) ? C113 C112 H112 . . . 120(3) ? C112 C113 C114 . . . 121.2(6) ? C112 C113 H113 . . . 119(4) ? C114 C113 H113 . . . 119(5) ? C113 C114 C115 . . . 120.6(6) ? C113 C114 H114 . . . 116(4) ? C115 C114 H114 . . . 123(4) ? C114 C115 C116 . . . 118.8(7) ? C114 C115 H115 . . . 121(4) ? C116 C115 H115 . . . 120(4) ? C111 C116 C115 . . . 121.3(6) ? C111 C116 H116 . . . 121(7) ? C115 C116 H116 . . . 115(7) ? P1 C121 C122 . . . 117.9(4) ? P1 C121 C126 . . . 121.7(4) ? C122 C121 C126 . . . 120.4(5) ? C121 C122 C123 . . . 119.1(6) ? C121 C122 H122 . . . 121(3) ? C123 C122 H122 . . . 120(3) ? C122 C123 C124 . . . 120.1(6) ? C122 C123 H123 . . . 115(4) ? C124 C123 H123 . . . 124(4) ? C123 C124 C125 . . . 121.1(5) ? C123 C124 H124 . . . 114(4) ? C125 C124 H124 . . . 125(4) ? C124 C125 C126 . . . 119.5(6) ? C124 C125 H125 . . . 118(3) ? C126 C125 H125 . . . 123(3) ? C121 C126 C125 . . . 119.8(5) ? C121 C126 H126 . . . 122(3) ? C125 C126 H126 . . . 118(3) ? P1 C131 C132 . . . 122.6(4) ? P1 C131 C136 . . . 118.4(5) ? C132 C131 C136 . . . 119.0(5) ? C131 C132 C133 . . . 120.9(5) ? C131 C132 H132 . . . 128(4) ? C133 C132 H132 . . . 111(4) ? C132 C133 C134 . . . 118.9(6) ? C132 C133 H133 . . . 118(3) ? C134 C133 H133 . . . 123(3) ? C133 C134 C135 . . . 120.3(6) ? C133 C134 H134 . . . 116(4) ? C135 C134 H134 . . . 123(4) ? C134 C135 C136 . . . 120.0(6) ? C134 C135 H135 . . . 130(3) ? C136 C135 H135 . . . 109(4) ? C131 C136 C135 . . . 120.9(6) ? C131 C136 H136 . . . 128(3) ? C135 C136 H136 . . . 111(3) ? Ru2 C1 Ru3 . . . 78.4(2) ? Ru2 C1 C2 . . . 113.7(5) ? Ru2 C1 H1 . . . 128(4) ? Ru3 C1 C2 . . . 70.6(4) ? Ru3 C1 H1 . . . 122(4) ? C2 C1 H1 . . . 119(4) ? Ru1 C2 Ru3 . . . 84.3(3) ? Ru1 C2 C1 . . . 112.4(4) ? Ru1 C2 H2 . . . 128(3) ? Ru3 C2 C1 . . . 73.9(4) ? Ru3 C2 H2 . . . 124(3) ? C1 C2 H2 . . . 117(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 if 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 if value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Additional items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Additional 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 Au Ru2 3.9554(6) . . ? Au C12 2.799(5) . . ? Au O12 3.498(4) . . ? Au C13 3.022(6) . . ? Au O13 3.682(4) . . ? Au C32 2.700(5) . . ? Au O32 3.337(4) . . ? Au C33 3.137(7) . . ? Au C111 3.478(6) . . ? Au C112 3.628(7) . . ? Au C121 3.423(6) . . ? Au C122 3.579(6) . . ? Au C131 3.465(6) . . ? Au H112 3.08(6) . . ? Au H122 3.02(5) . . ? Ru1 O11 3.044(6) . . ? Ru1 O12 3.091(5) . . ? Ru1 O13 3.047(4) . . ? Ru1 C33 3.666(6) . . ? Ru1 C1 2.900(7) . . ? Ru1 H2 2.72(5) . . ? Ru2 O21 3.034(5) . . ? Ru2 O22 3.098(5) . . ? Ru2 O23 3.036(4) . . ? Ru2 C31 3.610(6) . . ? Ru2 C32 3.294(6) . . ? Ru2 C2 2.898(6) . . ? Ru2 H1 2.61(6) . . ? Ru3 C13 3.593(5) . . ? Ru3 C23 3.354(5) . . ? Ru3 O31 3.031(5) . . ? Ru3 O32 3.068(5) . . ? Ru3 O33 3.074(4) . . ? Ru3 H1 2.75(6) . . ? Ru3 H2 2.80(5) . . ? C11 C12 2.818(9) . . ? C11 C13 2.827(9) . . ? C11 C2 2.792(8) . . ? C12 C13 2.847(8) . . ? O12 H126 2.69(5) . '2 646' ? C13 C2 2.873(9) . . ? C21 C22 2.946(9) . . ? C21 C23 2.766(8) . . ? C22 C23 2.861(9) . . ? O22 H114 2.59(8) . '3 767' ? C23 C1 2.836(7) . . ? C31 C32 2.723(9) . . ? C31 C33 2.760(8) . . ? C31 C1 2.741(8) . . ? P1 C112 2.785(6) . . ? P1 C116 2.816(8) . . ? P1 C122 2.775(5) . . ? P1 C126 2.812(5) . . ? P1 C132 2.814(6) . . ? P1 C136 2.747(6) . . ? P1 H112 2.87(5) . . ? P1 H122 2.89(6) . . ? C111 C113 2.419(8) . . ? C111 C114 2.800(9) . . ? C111 C115 2.444(10) . . ? C111 C121 2.871(7) . . ? C111 C131 2.905(8) . . ? C111 H112 2.04(6) . . ? C111 H116 2.01(11) . . ? C112 C114 2.406(11) . . ? C112 C115 2.797(11) . . ? C112 C116 2.409(10) . . ? C112 H113 2.13(7) . . ? C113 C115 2.395(11) . . ? C113 C116 2.760(9) . . ? C113 H112 2.03(6) . . ? C113 H114 2.10(8) . . ? C114 C116 2.401(9) . . ? C114 H113 2.10(8) . . ? C114 H115 2.17(7) . . ? C115 H114 2.21(7) . . ? C115 H116 1.95(10) . . ? C116 H115 2.16(8) . . ? C121 C123 2.404(7) . . ? C121 C124 2.757(7) . . ? C121 C125 2.396(8) . . ? C121 C131 2.861(7) . . ? C121 H122 2.13(6) . . ? C121 H126 2.06(6) . . ? C122 C124 2.391(8) . . ? C122 C125 2.778(9) . . ? C122 C126 2.409(9) . . ? C122 H123 1.99(7) . . ? C123 C125 2.394(9) . . ? C123 C126 2.772(8) . . ? C123 H122 2.12(6) . . ? C123 H124 1.89(6) . . ? C124 C126 2.395(7) . . ? C124 H123 2.06(8) . . ? C124 H125 2.04(7) . . ? C125 H124 2.00(5) . . ? C125 H126 2.03(5) . . ? C126 H125 2.10(6) . . ? C131 C133 2.424(8) . . ? C131 C134 2.787(9) . . ? C131 C135 2.411(8) . . ? C131 H126 2.67(5) . . ? C131 H132 2.20(7) . . ? C131 H136 2.06(5) . . ? C132 C134 2.408(9) . . ? C132 C135 2.764(9) . . ? C132 C136 2.378(9) . . ? C132 H133 2.01(6) . . ? C133 C135 2.398(10) . . ? C133 C136 2.770(9) . . ? C133 H132 2.03(7) . . ? C133 H134 2.06(7) . . ? C134 C136 2.394(10) . . ? C134 H133 2.06(6) . . ? C134 H135 2.18(7) . . ? C135 H134 2.10(7) . . ? C135 H136 1.91(5) . . ? C136 H135 1.99(6) . . ? C1 H2 1.94(4) . . ? C2 H1 1.86(6) . . ? H112 H113 2.39(10) . . ? H113 H114 2.37(12) . . ? H115 H116 2.33(13) . . ? H122 H123 2.32(8) . . ? H123 H124 2.25(10) . . ? H124 H125 2.34(8) . . ? H125 H126 2.39(7) . . ? H132 H133 2.22(9) . . ? H133 H134 2.36(9) . . ? H135 H136 2.07(8) . . ? H1 H2 2.14(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 C29_H18_Au_O9_P_Ru3 _chemical_formula_structural HAu(PPh3)Ru3C2H2(CO)9 _exptl_crystal_F_000 1960 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 17 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min -21 _reflns_limit_l_max 20 _reflns_number_observed ? _reflns_d_resolution_high .724 _reflns_d_resolution_low 11.315 _diffrn_reflns_av_sigmaI/netI .058 _diffrn_reflns_theta_min 1.8 _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 .052 _refine_ls_wR_factor_all .04 _refine_ls_goodness_of_fit_all 1.137 _refine_ls_shift/su_mean .003 data_br546l # 2. EXPERIMENTAL DATA #--------------------- _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _chemical_formula_sum 'C47 H32 Au2 O9 P2 Ru3' _chemical_formula_moiety ? _chemical_formula_weight 1499.85 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 18.203(4) _cell_length_b 12.731(2) _cell_length_c 21.825(4) _cell_angle_alpha 90.00000 _cell_angle_beta 110.494(3) _cell_angle_gamma 90.00000 _cell_volume 4737.7(15) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.103 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 0 _cell_measurement_theta_max 30 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 7.227 _exptl_crystal_description bar _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _diffrn_measurement_device_type 'CCD area detector diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Bruker SADABS' _exptl_absorpt_correction_T_min 0.346 _exptl_absorpt_correction_T_max 0.746 _diffrn_reflns_number 11919 _reflns_number_total 11919 _reflns_Friedel_coverage 0 _reflns_number_gt 8950 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 28.9 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents 0.097 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _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 .048 _refine_ls_wR_factor_ref .053 _refine_ls_goodness_of_fit_ref 1.791 _refine_ls_number_reflns 8950 _refine_ls_number_parameters 569 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max .047 _refine_diff_density_min -3.608 _refine_diff_density_max 2.595 _refine_ls_extinction_method none _refine_ls_extinction_coef .00000 _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack 0 # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Bruker SMART software' _computing_cell_refinement 'Bruker SMART software' _computing_data_reduction 'Bruker SAINT software' _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 ? 0 188 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 128 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 36 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 8 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 12 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au1 .280259(18) -.10003(2) .536063(15) .01676(14) Uani ? ? 1.00000 ? ? Au2 .221936(18) .01453(2) .394978(15) .01766(14) Uani ? ? 1.00000 ? ? Ru1 .21173(3) -.19261(5) .41807(3) .0139(3) Uani ? ? 1.00000 ? ? Ru2 .34569(4) -.10910(5) .38672(3) .0143(3) Uani ? ? 1.00000 ? ? Ru3 .37383(4) -.23539(5) .49542(3) .0150(3) Uani ? ? 1.00000 ? ? C11 .1328(4) -.1165(6) .4433(4) .019(3) Uani ? ? 1.00000 ? ? O11 .0790(3) -.0823(5) .4514(3) .029(3) Uani ? ? 1.00000 ? ? C12 .1489(5) -.1939(6) .3270(4) .024(4) Uani ? ? 1.00000 ? ? O12 .1114(4) -.1938(5) .2734(3) .040(3) Uani ? ? 1.00000 ? ? C13 .1814(5) -.3246(6) .4423(4) .027(4) Uani ? ? 1.00000 ? ? O13 .1619(4) -.4033(5) .4550(4) .047(4) Uani ? ? 1.00000 ? ? C21 .3840(5) .0079(6) .4429(4) .021(4) Uani ? ? 1.00000 ? ? O21 .4131(3) .0754(4) .4773(3) .027(3) Uani ? ? 1.00000 ? ? C22 .3010(5) -.0447(7) .3016(5) .030(4) Uani ? ? 1.00000 ? ? O22 .2780(5) -.0111(6) .2493(3) .058(5) Uani ? ? 1.00000 ? ? C23 .4458(5) -.1321(7) .3828(4) .026(4) Uani ? ? 1.00000 ? ? O23 .5057(3) -.1446(5) .3778(3) .037(3) Uani ? ? 1.00000 ? ? C31 .4385(4) -.1471(6) .5672(4) .018(3) Uani ? ? 1.00000 ? ? O31 .4849(3) -.0991(5) .6072(3) .031(3) Uani ? ? 1.00000 ? ? C32 .3553(5) -.3406(7) .5492(4) .029(4) Uani ? ? 1.00000 ? ? O32 .3435(5) -.4067(5) .5802(4) .056(4) Uani ? ? 1.00000 ? ? C33 .4573(5) -.3054(7) .4815(4) .028(4) Uani ? ? 1.00000 ? ? O33 .5059(4) -.3499(6) .4699(3) .050(4) Uani ? ? 1.00000 ? ? C1 .3044(4) -.2626(5) .4019(4) .017(3) Uani ? ? 1.00000 ? ? C2 .3191(5) -.2758(6) .3442(4) .023(4) Uani ? ? 1.00000 ? ? P1 .28735(11) -.00369(16) .62745(9) .0163(8) Uani ? ? 1.00000 ? ? C111 .2835(4) .1376(6) .6185(4) .019(3) Uani ? ? 1.00000 ? ? C112 .2489(5) .2018(7) .6527(4) .030(4) Uani ? ? 1.00000 ? ? C113 .2434(6) .3071(8) .6415(5) .042(5) Uani ? ? 1.00000 ? ? C114 .2754(6) .3536(7) .6004(5) .041(5) Uani ? ? 1.00000 ? ? C115 .3128(5) .2919(7) .5675(5) .037(5) Uani ? ? 1.00000 ? ? C116 .3146(5) .1851(7) .5753(4) .026(4) Uani ? ? 1.00000 ? ? C121 .2098(5) -.0328(6) .6599(4) .018(3) Uani ? ? 1.00000 ? ? C122 .1357(5) -.0490(6) .6168(4) .025(4) Uani ? ? 1.00000 ? ? C123 .0748(5) -.0695(7) .6401(5) .033(4) Uani ? ? 1.00000 ? ? C124 .0888(6) -.0733(7) .7060(5) .035(5) Uani ? ? 1.00000 ? ? C125 .1637(6) -.0552(6) .7496(4) .029(4) Uani ? ? 1.00000 ? ? C126 .2246(5) -.0349(6) .7269(4) .021(4) Uani ? ? 1.00000 ? ? C131 .3780(5) -.0301(7) .6952(4) .024(4) Uani ? ? 1.00000 ? ? C132 .4269(5) .0486(9) .7311(4) .039(5) Uani ? ? 1.00000 ? ? C133 .4963(6) .0257(12) .7808(5) .066(7) Uani ? ? 1.00000 ? ? C134 .5140(6) -.0810(12) .7960(5) .071(8) Uani ? ? 1.00000 ? ? C135 .4660(6) -.1585(10) .7625(5) .053(6) Uani ? ? 1.00000 ? ? C136 .3968(6) -.1352(8) .7108(5) .044(5) Uani ? ? 1.00000 ? ? P2 .17456(12) .18032(15) .36489(10) .0171(9) Uani ? ? 1.00000 ? ? C211 .1190(4) .1860(6) .2774(4) .017(3) Uani ? ? 1.00000 ? ? C212 .1088(5) .2775(6) .2429(4) .023(4) Uani ? ? 1.00000 ? ? C213 .0602(5) .2821(7) .1774(4) .031(4) Uani ? ? 1.00000 ? ? C214 .0240(5) .1931(8) .1465(4) .033(5) Uani ? ? 1.00000 ? ? C215 .0359(5) .0999(7) .1806(4) .032(4) Uani ? ? 1.00000 ? ? C216 .0833(5) .0950(7) .2457(4) .027(4) Uani ? ? 1.00000 ? ? C221 .2483(4) .2802(6) .3758(4) .017(3) Uani ? ? 1.00000 ? ? C222 .2445(5) .3780(6) .4024(4) .026(4) Uani ? ? 1.00000 ? ? C223 .3052(6) .4505(6) .4081(4) .033(4) Uani ? ? 1.00000 ? ? C224 .3654(5) .4266(7) .3873(5) .035(4) Uani ? ? 1.00000 ? ? C225 .3698(5) .3305(7) .3608(5) .038(5) Uani ? ? 1.00000 ? ? C226 .3113(5) .2553(6) .3558(4) .029(4) Uani ? ? 1.00000 ? ? C231 .1068(4) .2300(6) .4033(4) .018(3) Uani ? ? 1.00000 ? ? C232 .0448(5) .2944(6) .3720(4) .029(4) Uani ? ? 1.00000 ? ? C233 -.0073(6) .3264(8) .4029(5) .043(5) Uani ? ? 1.00000 ? ? C234 .0044(6) .2936(8) .4649(5) .042(5) Uani ? ? 1.00000 ? ? C235 .0669(6) .2289(8) .4974(4) .042(5) Uani ? ? 1.00000 ? ? C236 .1184(5) .1960(7) .4671(4) .028(4) Uani ? ? 1.00000 ? ? H112 .22616 .17064 .68209 .09100 Uiso ? ? 1.00000 ? ? H113 .21725 .35244 .66369 .11600 Uiso ? ? 1.00000 ? ? H114 .27461 .42752 .59500 .10000 Uiso ? ? 1.00000 ? ? H115 .33341 .32456 .53681 .07600 Uiso ? ? 1.00000 ? ? H116 .33975 .14298 .55105 .07100 Uiso ? ? 1.00000 ? ? H122 .12420 -.04663 .57058 .06500 Uiso ? ? 1.00000 ? ? H123 .02324 -.08303 .60946 .09300 Uiso ? ? 1.00000 ? ? H124 .04603 -.08604 .72153 .11500 Uiso ? ? 1.00000 ? ? H125 .17380 -.05553 .79534 .08000 Uiso ? ? 1.00000 ? ? H126 .27558 -.02241 .75718 .06200 Uiso ? ? 1.00000 ? ? H132 .41262 .12124 .72110 .11300 Uiso ? ? 1.00000 ? ? H133 .53020 .07947 .80430 .17100 Uiso ? ? 1.00000 ? ? H134 .56149 -.09627 .83088 .18000 Uiso ? ? 1.00000 ? ? H135 .48122 -.22887 .77385 .22000 Uiso ? ? 1.00000 ? ? H136 .36290 -.19095 .68731 .12000 Uiso ? ? 1.00000 ? ? H212 .13424 .34005 .26401 .08500 Uiso ? ? 1.00000 ? ? H213 .05082 .34890 .15467 .09100 Uiso ? ? 1.00000 ? ? H214 -.00980 .19590 .10208 .09200 Uiso ? ? 1.00000 ? ? H215 .01228 .03653 .15738 .11700 Uiso ? ? 1.00000 ? ? H216 .09239 .03027 .26923 .08800 Uiso ? ? 1.00000 ? ? H222 .20123 .39607 .41513 .08400 Uiso ? ? 1.00000 ? ? H223 .30262 .51873 .42637 .10200 Uiso ? ? 1.00000 ? ? H224 .40457 .47693 .39039 .11200 Uiso ? ? 1.00000 ? ? H225 .41227 .31327 .34671 .10500 Uiso ? ? 1.00000 ? ? H226 .31399 .18727 .33790 .08100 Uiso ? ? 1.00000 ? ? H232 .03587 .31827 .32826 .09200 Uiso ? ? 1.00000 ? ? H233 -.04920 .37135 .38104 .14000 Uiso ? ? 1.00000 ? ? H234 -.02992 .31370 .48721 .13200 Uiso ? ? 1.00000 ? ? H235 .07548 .20311 .54068 .12500 Uiso ? ? 1.00000 ? ? H236 .15962 .14969 .48914 .07700 Uiso ? ? 1.00000 ? ? H2a .27653 -.28797 .30348 .02900 Uiso ? ? 1.00000 ? ? H2b .36177 -.32145 .34373 .02900 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 Au1 .01514(16) .01420(15) .01717(15) -.00037(12) .00093(11) -.00241(11) Au2 .01533(16) .00883(14) .02334(16) .00106(12) -.00010(12) .00163(12) Ru1 .0099(3) .0089(3) .0173(3) -.0023(2) -.0024(2) -.0001(2) Ru2 .0120(3) .0107(3) .0167(3) -.0018(2) .0007(2) -.0006(2) Ru3 .0114(3) .0108(3) .0171(3) .0006(2) -.0018(2) .0003(2) C11 .013(4) .014(4) .022(4) -.004(3) -.005(3) -.001(3) O11 .017(3) .034(4) .031(3) .006(3) .001(3) -.002(3) C12 .024(5) .013(4) .031(5) -.005(3) .004(4) -.001(3) O12 .039(4) .040(4) .022(3) .002(3) -.012(3) -.008(3) C13 .019(4) .020(4) .037(5) -.002(4) .004(4) .001(4) O13 .033(4) .026(4) .081(6) -.008(3) .019(4) .018(4) C21 .016(4) .017(4) .033(5) -.004(3) .013(4) -.001(3) O21 .027(3) .025(3) .027(3) -.009(3) .007(3) -.011(3) C22 .027(5) .024(5) .038(5) .002(4) .008(4) .003(4) O22 .073(6) .069(6) .031(4) .023(4) .018(4) .023(4) C23 .016(4) .023(4) .031(5) -.004(4) -.000(4) -.008(4) O23 .019(3) .043(4) .046(4) -.005(3) .009(3) -.016(3) C31 .013(4) .021(4) .019(4) -.001(3) .003(3) .000(3) O31 .023(3) .038(4) .030(3) -.013(3) .006(3) -.009(3) C32 .029(5) .022(5) .025(5) .000(4) -.004(4) .012(4) O32 .057(5) .039(4) .055(5) -.011(4) -.005(4) .028(4) C33 .023(5) .031(5) .022(4) .008(4) -.001(3) -.002(4) O33 .034(4) .063(5) .047(4) .022(4) .005(3) -.004(4) C1 .017(4) .007(3) .022(4) .000(3) -.001(3) .000(3) C2 .023(4) .015(4) .027(4) -.002(3) .005(4) -.005(3) P1 .0114(10) .0179(10) .0145(9) .0026(8) -.0019(8) .0010(8) C111 .012(4) .014(4) .020(4) -.003(3) -.007(3) .003(3) C112 .029(5) .021(5) .039(5) -.003(4) .011(4) -.008(4) C113 .034(6) .029(5) .062(7) -.008(5) .017(5) -.010(5) C114 .028(5) .023(5) .059(7) -.006(4) -.001(5) .006(5) C115 .025(5) .032(5) .043(6) -.012(4) -.002(4) .015(4) C116 .017(4) .033(5) .018(4) -.004(4) -.005(3) .002(4) C121 .020(4) .012(4) .020(4) .003(3) .003(3) .003(3) C122 .015(4) .024(5) .028(5) -.002(3) -.003(3) .003(4) C123 .015(4) .033(5) .041(6) -.006(4) -.003(4) -.005(4) C124 .026(5) .029(5) .052(6) -.002(4) .017(5) .006(4) C125 .039(6) .017(4) .032(5) -.001(4) .014(4) .008(4) C126 .015(4) .015(4) .028(4) .001(3) .004(3) -.001(3) C131 .011(4) .039(5) .019(4) .006(4) .002(3) .008(4) C132 .013(4) .066(7) .029(5) -.006(5) -.006(4) .004(5) C133 .024(6) .125(12) .032(6) -.007(7) -.010(5) .010(7) C134 .026(6) .136(13) .037(6) .026(7) -.006(5) .039(7) C135 .045(7) .076(8) .041(6) .036(6) .017(5) .038(6) C136 .044(6) .053(7) .036(6) .022(5) .017(5) .021(5) P2 .0160(10) .0104(9) .0211(10) .0004(8) .0019(8) .0017(8) C211 .016(4) .011(4) .023(4) .003(3) .005(3) -.002(3) C212 .022(4) .023(4) .024(4) -.002(4) .006(3) .002(3) C213 .030(5) .032(5) .024(5) .001(4) .002(4) .009(4) C214 .025(5) .050(6) .021(4) .003(4) .006(4) -.004(4) C215 .024(5) .035(5) .031(5) -.014(4) .002(4) -.011(4) C216 .021(4) .025(5) .030(5) -.006(4) .003(4) -.004(4) C221 .013(4) .013(4) .019(4) .000(3) -.002(3) .006(3) C222 .029(5) .019(4) .018(4) -.005(4) -.005(3) .005(3) C223 .042(6) .012(4) .028(5) -.005(4) -.009(4) -.003(3) C224 .022(5) .024(5) .040(5) -.010(4) -.011(4) .006(4) C225 .023(5) .029(5) .053(6) -.006(4) .002(4) .013(4) C226 .024(5) .019(4) .037(5) -.001(4) .003(4) .000(4) C231 .013(4) .015(4) .023(4) -.002(3) .003(3) -.002(3) C232 .033(5) .021(4) .034(5) .011(4) .014(4) .009(4) C233 .044(6) .040(6) .046(6) .016(5) .017(5) .014(5) C234 .039(6) .056(7) .036(6) .014(5) .017(5) .002(5) C235 .042(6) .059(7) .022(5) .004(5) .007(4) .002(5) C236 .024(5) .034(5) .019(4) -.000(4) -.003(3) .000(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 if value to be published Au1 Au2 . . 3.2321(6) ? Au1 Ru1 . . 2.7069(7) ? Au1 Ru3 . . 2.7778(8) ? Au1 P1 . . 2.306(2) ? Au2 Ru1 . . 2.7034(8) ? Au2 Ru2 . . 2.8051(8) ? Au2 P2 . . 2.288(2) ? Ru1 Ru2 . . 2.9517(11) ? Ru1 Ru3 . . 2.8923(9) ? Ru1 C11 . . 1.965(9) ? Ru1 C12 . . 1.915(8) ? Ru1 C13 . . 1.901(9) ? Ru1 C1 . . 2.045(9) ? Ru2 Ru3 . . 2.7613(9) ? Ru2 C21 . . 1.899(8) ? Ru2 C22 . . 1.931(9) ? Ru2 C23 . . 1.877(9) ? Ru2 C1 . . 2.160(7) ? Ru2 C2 . . 2.299(8) ? Ru3 C31 . . 1.952(7) ? Ru3 C32 . . 1.887(9) ? Ru3 C33 . . 1.876(10) ? Ru3 C1 . . 2.019(7) ? C11 O11 . . 1.141(11) ? C12 O12 . . 1.130(9) ? C13 O13 . . 1.129(11) ? C21 O21 . . 1.143(9) ? C22 O22 . . 1.150(11) ? C23 O23 . . 1.144(12) ? C31 O31 . . 1.154(9) ? C32 O32 . . 1.146(12) ? C33 O33 . . 1.149(13) ? C1 C2 . . 1.386(13) ? C2 H2a . . .966(7) ? C2 H2b . . .973(9) ? P1 C111 . . 1.808(8) ? P1 C121 . . 1.825(10) ? P1 C131 . . 1.820(7) ? C111 C112 . . 1.397(13) ? C111 C116 . . 1.396(13) ? C112 C113 . . 1.360(13) ? C112 H112 . . .962(11) ? C113 C114 . . 1.363(17) ? C113 H113 . . .978(12) ? C114 C115 . . 1.393(16) ? C114 H114 . . .949(9) ? C115 C116 . . 1.369(13) ? C115 H115 . . .969(11) ? C116 H116 . . .973(10) ? C121 C122 . . 1.365(10) ? C121 C126 . . 1.391(12) ? C122 C123 . . 1.396(15) ? C122 H122 . . .956(9) ? C123 C124 . . 1.372(15) ? C123 H123 . . .958(8) ? C124 C125 . . 1.382(12) ? C124 H124 . . .964(12) ? C125 C126 . . 1.388(15) ? C125 H125 . . .949(9) ? C126 H126 . . .945(7) ? C131 C132 . . 1.386(12) ? C131 C136 . . 1.394(14) ? C132 C133 . . 1.379(12) ? C132 H132 . . .964(11) ? C133 C134 . . 1.41(2) ? C133 H133 . . .943(13) ? C134 C135 . . 1.350(17) ? C134 H134 . . .950(10) ? C135 C136 . . 1.397(13) ? C135 H135 . . .945(12) ? C136 H136 . . .963(10) ? P2 C211 . . 1.823(7) ? P2 C221 . . 1.803(8) ? P2 C231 . . 1.830(9) ? C211 C212 . . 1.364(11) ? C211 C216 . . 1.389(11) ? C212 C213 . . 1.393(11) ? C212 H212 . . .955(8) ? C213 C214 . . 1.365(13) ? C213 H213 . . .969(9) ? C214 C215 . . 1.377(13) ? C214 H214 . . .950(8) ? C215 C216 . . 1.383(11) ? C215 H215 . . .969(9) ? C216 H216 . . .954(8) ? C221 C222 . . 1.386(11) ? C221 C226 . . 1.399(14) ? C222 C223 . . 1.412(13) ? C222 H222 . . .950(10) ? C223 C224 . . 1.359(16) ? C223 H223 . . .963(8) ? C224 C225 . . 1.368(13) ? C224 H224 . . .944(9) ? C225 C226 . . 1.407(13) ? C225 H225 . . .952(11) ? C226 H226 . . .959(9) ? C231 C232 . . 1.368(11) ? C231 C236 . . 1.401(12) ? C232 C233 . . 1.403(17) ? C232 H232 . . .960(9) ? C233 C234 . . 1.361(15) ? C233 H233 . . .939(10) ? C234 C235 . . 1.383(14) ? C234 H234 . . .951(12) ? C235 C236 . . 1.389(16) ? C235 H235 . . .960(10) ? C236 H236 . . .943(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 if value to be published Au2 Au1 Ru1 . . . 53.267(18) ? Au2 Au1 Ru3 . . . 90.534(19) ? Au2 Au1 P1 . . . 118.96(5) ? Ru1 Au1 Ru3 . . . 63.64(2) ? Ru1 Au1 P1 . . . 157.21(5) ? Ru3 Au1 P1 . . . 138.70(5) ? Au1 Au2 Ru1 . . . 53.366(15) ? Au1 Au2 Ru2 . . . 78.738(17) ? Au1 Au2 P2 . . . 130.91(6) ? Ru1 Au2 Ru2 . . . 64.77(2) ? Ru1 Au2 P2 . . . 155.49(6) ? Ru2 Au2 P2 . . . 136.87(7) ? Au1 Ru1 Au2 . . . 73.367(19) ? Au1 Ru1 Ru2 . . . 85.46(2) ? Au1 Ru1 Ru3 . . . 59.37(2) ? Au1 Ru1 C11 . . . 70.0(2) ? Au1 Ru1 C12 . . . 154.2(2) ? Au1 Ru1 C13 . . . 101.7(3) ? Au1 Ru1 C1 . . . 102.76(19) ? Au2 Ru1 Ru2 . . . 59.28(2) ? Au2 Ru1 Ru3 . . . 99.78(2) ? Au2 Ru1 C11 . . . 71.1(2) ? Au2 Ru1 C12 . . . 82.5(2) ? Au2 Ru1 C13 . . . 163.7(3) ? Au2 Ru1 C1 . . . 106.1(2) ? Ru2 Ru1 Ru3 . . . 56.38(2) ? Ru2 Ru1 C11 . . . 129.2(2) ? Ru2 Ru1 C12 . . . 90.2(3) ? Ru2 Ru1 C13 . . . 136.6(3) ? Ru2 Ru1 C1 . . . 47.0(2) ? Ru3 Ru1 C11 . . . 128.8(2) ? Ru3 Ru1 C12 . . . 136.1(3) ? Ru3 Ru1 C13 . . . 90.5(2) ? Ru3 Ru1 C1 . . . 44.3(2) ? C11 Ru1 C12 . . . 93.8(3) ? C11 Ru1 C13 . . . 92.6(4) ? C11 Ru1 C1 . . . 172.6(3) ? C12 Ru1 C13 . . . 98.9(3) ? C12 Ru1 C1 . . . 92.6(3) ? C13 Ru1 C1 . . . 90.0(4) ? Au2 Ru2 Ru1 . . . 55.95(2) ? Au2 Ru2 Ru3 . . . 100.55(3) ? Au2 Ru2 C21 . . . 68.9(3) ? Au2 Ru2 C22 . . . 75.3(3) ? Au2 Ru2 C23 . . . 154.8(3) ? Au2 Ru2 C1 . . . 99.6(2) ? Au2 Ru2 C2 . . . 118.9(2) ? Ru1 Ru2 Ru3 . . . 60.72(2) ? Ru1 Ru2 C21 . . . 106.2(3) ? Ru1 Ru2 C22 . . . 105.8(3) ? Ru1 Ru2 C23 . . . 148.0(3) ? Ru1 Ru2 C1 . . . 43.8(2) ? Ru1 Ru2 C2 . . . 71.7(2) ? Ru3 Ru2 C21 . . . 89.2(3) ? Ru3 Ru2 C22 . . . 164.4(3) ? Ru3 Ru2 C23 . . . 93.3(3) ? Ru3 Ru2 C1 . . . 46.49(18) ? Ru3 Ru2 C2 . . . 76.0(2) ? C21 Ru2 C22 . . . 102.9(3) ? C21 Ru2 C23 . . . 90.5(4) ? C21 Ru2 C1 . . . 132.8(3) ? C21 Ru2 C2 . . . 164.2(3) ? C22 Ru2 C23 . . . 96.4(4) ? C22 Ru2 C1 . . . 118.6(3) ? C22 Ru2 C2 . . . 92.6(3) ? C23 Ru2 C1 . . . 105.1(3) ? C23 Ru2 C2 . . . 84.7(3) ? C1 Ru2 C2 . . . 36.0(3) ? Au1 Ru3 Ru1 . . . 56.99(2) ? Au1 Ru3 Ru2 . . . 87.88(2) ? Au1 Ru3 C31 . . . 69.6(2) ? Au1 Ru3 C32 . . . 88.8(3) ? Au1 Ru3 C33 . . . 165.6(2) ? Au1 Ru3 C1 . . . 101.1(2) ? Ru1 Ru3 Ru2 . . . 62.90(2) ? Ru1 Ru3 C31 . . . 124.4(2) ? Ru1 Ru3 C32 . . . 97.4(3) ? Ru1 Ru3 C33 . . . 135.5(2) ? Ru1 Ru3 C1 . . . 45.0(2) ? Ru2 Ru3 C31 . . . 103.4(2) ? Ru2 Ru3 C32 . . . 158.1(2) ? Ru2 Ru3 C33 . . . 93.1(3) ? Ru2 Ru3 C1 . . . 50.9(2) ? C31 Ru3 C32 . . . 95.7(3) ? C31 Ru3 C33 . . . 96.2(3) ? C31 Ru3 C1 . . . 153.9(3) ? C32 Ru3 C33 . . . 95.4(4) ? C32 Ru3 C1 . . . 108.8(3) ? C33 Ru3 C1 . . . 90.6(3) ? Ru1 C11 O11 . . . 169.6(6) ? Ru1 C12 O12 . . . 179.3(8) ? Ru1 C13 O13 . . . 178.2(7) ? Ru2 C21 O21 . . . 174.4(8) ? Ru2 C22 O22 . . . 174.9(9) ? Ru2 C23 O23 . . . 177.1(8) ? Ru3 C31 O31 . . . 170.9(8) ? Ru3 C32 O32 . . . 177.8(8) ? Ru3 C33 O33 . . . 176.6(7) ? Ru1 C1 Ru2 . . . 89.1(3) ? Ru1 C1 Ru3 . . . 90.7(3) ? Ru1 C1 C2 . . . 130.1(5) ? Ru2 C1 Ru3 . . . 82.6(2) ? Ru2 C1 C2 . . . 77.5(5) ? Ru3 C1 C2 . . . 133.4(6) ? Ru2 C2 C1 . . . 66.5(4) ? Ru2 C2 H2a . . . 120.5(6) ? Ru2 C2 H2b . . . 120.0(6) ? C1 C2 H2a . . . 120.5(9) ? C1 C2 H2b . . . 119.4(7) ? H2a C2 H2b . . . 106.3(8) ? Au1 P1 C111 . . . 116.6(3) ? Au1 P1 C121 . . . 114.3(2) ? Au1 P1 C131 . . . 111.4(3) ? C111 P1 C121 . . . 103.8(4) ? C111 P1 C131 . . . 105.1(4) ? C121 P1 C131 . . . 104.5(4) ? P1 C111 C112 . . . 122.1(7) ? P1 C111 C116 . . . 119.6(7) ? C112 C111 C116 . . . 118.3(8) ? C111 C112 C113 . . . 119.9(10) ? C111 C112 H112 . . . 119.7(8) ? C113 C112 H112 . . . 120.3(10) ? C112 C113 C114 . . . 121.6(11) ? C112 C113 H113 . . . 120.7(12) ? C114 C113 H113 . . . 117.6(9) ? C113 C114 C115 . . . 119.6(9) ? C113 C114 H114 . . . 121.5(11) ? C115 C114 H114 . . . 118.9(11) ? C114 C115 C116 . . . 119.4(10) ? C114 C115 H115 . . . 119.5(9) ? C116 C115 H115 . . . 120.9(10) ? C111 C116 C115 . . . 121.1(9) ? C111 C116 H116 . . . 120.5(8) ? C115 C116 H116 . . . 118.4(10) ? P1 C121 C122 . . . 118.4(7) ? P1 C121 C126 . . . 121.4(6) ? C122 C121 C126 . . . 120.2(9) ? C121 C122 C123 . . . 119.8(8) ? C121 C122 H122 . . . 121.4(10) ? C123 C122 H122 . . . 118.8(7) ? C122 C123 C124 . . . 120.6(8) ? C122 C123 H123 . . . 119.2(10) ? C124 C123 H123 . . . 120.1(11) ? C123 C124 C125 . . . 119.5(10) ? C123 C124 H124 . . . 119.8(8) ? C125 C124 H124 . . . 120.6(10) ? C124 C125 C126 . . . 120.3(9) ? C124 C125 H125 . . . 120.3(11) ? C126 C125 H125 . . . 119.4(8) ? C121 C126 C125 . . . 119.6(7) ? C121 C126 H126 . . . 120.9(9) ? C125 C126 H126 . . . 119.5(9) ? P1 C131 C132 . . . 123.1(7) ? P1 C131 C136 . . . 116.9(6) ? C132 C131 C136 . . . 120.1(7) ? C131 C132 C133 . . . 121.5(10) ? C131 C132 H132 . . . 119.8(8) ? C133 C132 H132 . . . 118.7(10) ? C132 C133 C134 . . . 117.4(11) ? C132 C133 H133 . . . 121.3(14) ? C134 C133 H133 . . . 121.3(10) ? C133 C134 C135 . . . 121.7(9) ? C133 C134 H134 . . . 117.0(12) ? C135 C134 H134 . . . 121.3(14) ? C134 C135 C136 . . . 120.8(11) ? C134 C135 H135 . . . 118.4(10) ? C136 C135 H135 . . . 120.7(10) ? C131 C136 C135 . . . 118.5(9) ? C131 C136 H136 . . . 121.3(9) ? C135 C136 H136 . . . 120.2(10) ? Au2 P2 C211 . . . 110.7(2) ? Au2 P2 C221 . . . 115.1(2) ? Au2 P2 C231 . . . 115.7(3) ? C211 P2 C221 . . . 103.0(4) ? C211 P2 C231 . . . 104.5(4) ? C221 P2 C231 . . . 106.6(4) ? P2 C211 C212 . . . 122.1(5) ? P2 C211 C216 . . . 118.6(6) ? C212 C211 C216 . . . 119.2(7) ? C211 C212 C213 . . . 121.1(7) ? C211 C212 H212 . . . 119.7(7) ? C213 C212 H212 . . . 119.1(8) ? C212 C213 C214 . . . 119.7(8) ? C212 C213 H213 . . . 119.8(8) ? C214 C213 H213 . . . 120.5(8) ? C213 C214 C215 . . . 119.5(7) ? C213 C214 H214 . . . 120.1(9) ? C215 C214 H214 . . . 120.4(9) ? C214 C215 C216 . . . 121.2(8) ? C214 C215 H215 . . . 118.6(8) ? C216 C215 H215 . . . 120.2(9) ? C211 C216 C215 . . . 119.3(8) ? C211 C216 H216 . . . 119.3(7) ? C215 C216 H216 . . . 121.4(8) ? P2 C221 C222 . . . 123.0(7) ? P2 C221 C226 . . . 116.9(6) ? C222 C221 C226 . . . 120.0(8) ? C221 C222 C223 . . . 118.2(9) ? C221 C222 H222 . . . 120.5(8) ? C223 C222 H222 . . . 121.3(8) ? C222 C223 C224 . . . 121.4(8) ? C222 C223 H223 . . . 118.5(10) ? C224 C223 H223 . . . 120.1(9) ? C223 C224 C225 . . . 121.1(9) ? C223 C224 H224 . . . 120.1(9) ? C225 C224 H224 . . . 118.8(11) ? C224 C225 C226 . . . 119.1(10) ? C224 C225 H225 . . . 121.1(9) ? C226 C225 H225 . . . 119.8(9) ? C221 C226 C225 . . . 120.2(8) ? C221 C226 H226 . . . 119.7(9) ? C225 C226 H226 . . . 120.1(10) ? P2 C231 C232 . . . 123.3(7) ? P2 C231 C236 . . . 117.2(6) ? C232 C231 C236 . . . 119.5(9) ? C231 C232 C233 . . . 120.8(9) ? C231 C232 H232 . . . 120.7(10) ? C233 C232 H232 . . . 118.5(8) ? C232 C233 C234 . . . 119.5(9) ? C232 C233 H233 . . . 119.9(11) ? C234 C233 H233 . . . 120.5(12) ? C233 C234 C235 . . . 120.4(11) ? C233 C234 H234 . . . 121.7(10) ? C235 C234 H234 . . . 117.9(10) ? C234 C235 C236 . . . 120.5(9) ? C234 C235 H235 . . . 121.9(12) ? C236 C235 H235 . . . 117.5(9) ? C231 C236 C235 . . . 119.2(8) ? C231 C236 H236 . . . 121.2(10) ? C235 C236 H236 . . . 119.6(9) ? 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 if 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 if value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Additional items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Additional 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 Au1 Ru2 3.8437(10) . . ? Au1 C11 2.747(7) . . ? Au1 O11 3.485(5) . . ? Au1 C31 2.784(8) . . ? Au1 O31 3.499(6) . . ? Au1 C32 3.325(9) . . ? Au1 C121 3.480(9) . . ? Au1 C131 3.419(7) . . ? Au2 C11 2.779(9) . . ? Au2 O11 3.472(7) . . ? Au2 C12 3.103(8) . . ? Au2 C21 2.765(8) . . ? Au2 O21 3.400(6) . . ? Au2 C22 2.975(11) . . ? Au2 C211 3.391(7) . . ? Au2 C221 3.462(7) . . ? Au2 C231 3.495(8) . . ? Au2 H216 2.9328(5) . . ? Au2 H236 3.1786(5) . . ? Ru1 O11 3.094(7) . . ? Ru1 O12 3.045(5) . . ? Ru1 O13 3.030(7) . . ? Ru1 C2 3.122(10) . . ? Ru2 O21 3.039(5) . . ? Ru2 O22 3.079(7) . . ? Ru2 O23 3.020(7) . . ? Ru2 C33 3.422(8) . . ? Ru2 H2a 2.9102(6) . . ? Ru2 H2b 2.9097(7) . . ? Ru3 C13 3.474(8) . . ? Ru3 C21 3.331(8) . . ? Ru3 C23 3.426(10) . . ? Ru3 O31 3.097(5) . . ? Ru3 O32 3.033(8) . . ? Ru3 O33 3.024(8) . . ? Ru3 C2 3.138(8) . . ? C11 C12 2.832(13) . . ? C11 C13 2.796(11) . . ? O11 H122 2.479(6) . . ? C12 C13 2.900(12) . . ? C12 C1 2.865(10) . . ? C13 C1 2.793(13) . . ? C21 C22 2.996(12) . . ? C21 C23 2.682(13) . . ? O21 H116 2.573(7) . . ? C22 C23 2.839(11) . . ? C23 C2 2.831(11) . . ? O23 H116 2.696(5) . '3 656' ? O23 H135 2.690(7) . '4 544' ? C31 C32 2.846(12) . . ? C31 C33 2.850(12) . . ? C31 P1 3.895(9) . . ? O31 P1 3.965(7) . . ? C32 C33 2.784(15) . . ? O32 H114 2.533(8) . '1 545' ? C33 C1 2.771(10) . . ? C1 H2a 2.052(8) . . ? C1 H2b 2.047(9) . . ? P1 C112 2.812(9) . . ? P1 C116 2.777(9) . . ? P1 C122 2.750(9) . . ? P1 C126 2.812(10) . . ? P1 C132 2.826(8) . . ? P1 C136 2.747(10) . . ? P1 H112 2.919(2) . . ? P1 H116 2.879(2) . . ? P1 H122 2.842(2) . . ? P1 H126 2.923(2) . . ? P1 H132 2.9400(18) . . ? P1 H136 2.833(2) . . ? P1 H236 3.6628(18) . . ? C111 C113 2.387(13) . . ? C111 C114 2.774(12) . . ? C111 C115 2.408(13) . . ? C111 C121 2.858(12) . . ? C111 C131 2.881(11) . . ? C111 H112 2.051(9) . . ? C111 H116 2.068(9) . . ? C111 H132 2.626(6) . . ? C112 C114 2.378(14) . . ? C112 C115 2.765(15) . . ? C112 C116 2.397(15) . . ? C112 H113 2.041(9) . . ? C113 C115 2.381(17) . . ? C113 C116 2.738(15) . . ? C113 H112 2.024(11) . . ? C113 H114 2.026(11) . . ? C114 C116 2.384(13) . . ? C114 H113 2.012(12) . . ? C114 H115 2.051(12) . . ? C115 H114 2.029(10) . . ? C115 H116 2.022(9) . . ? C116 H115 2.044(9) . . ? C121 C123 2.388(12) . . ? C121 C124 2.773(15) . . ? C121 C125 2.402(14) . . ? C121 C131 2.883(11) . . ? C121 H112 2.632(7) . . ? C121 H122 2.034(7) . . ? C121 H126 2.044(7) . . ? C122 C124 2.405(16) . . ? C122 C125 2.764(13) . . ? C122 C126 2.388(10) . . ? C122 H123 2.043(9) . . ? C123 C125 2.379(12) . . ? C123 C126 2.757(10) . . ? C123 H122 2.037(11) . . ? C123 H124 2.032(11) . . ? C124 C126 2.402(13) . . ? C124 H123 2.030(9) . . ? C124 H125 2.033(9) . . ? C125 H124 2.049(10) . . ? C125 H126 2.028(10) . . ? C126 H125 2.031(10) . . ? C131 C133 2.413(12) . . ? C131 C134 2.753(12) . . ? C131 C135 2.398(13) . . ? C131 H126 2.661(10) . . ? C131 H132 2.044(9) . . ? C131 H136 2.066(9) . . ? C132 C134 2.382(16) . . ? C132 C135 2.755(16) . . ? C132 C136 2.408(15) . . ? C132 H133 2.035(8) . . ? C133 C135 2.410(19) . . ? C133 C136 2.806(16) . . ? C133 H132 2.027(12) . . ? C133 H134 2.026(13) . . ? C134 C136 2.388(13) . . ? C134 H133 2.063(15) . . ? C134 H135 1.983(14) . . ? C135 H134 2.014(10) . . ? C135 H136 2.057(9) . . ? C136 H135 2.048(10) . . ? P2 C212 2.797(8) . . ? P2 C216 2.771(8) . . ? P2 C222 2.810(8) . . ? P2 C226 2.737(10) . . ? P2 C232 2.822(10) . . ? P2 C236 2.766(10) . . ? P2 H212 2.897(2) . . ? P2 H216 2.8388(19) . . ? P2 H222 2.934(2) . . ? P2 H226 2.801(2) . . ? P2 H232 2.947(2) . . ? P2 H236 2.845(2) . . ? C211 C213 2.401(11) . . ? C211 C214 2.775(10) . . ? C211 C215 2.392(11) . . ? C211 C221 2.837(9) . . ? C211 C231 2.887(12) . . ? C211 H212 2.016(7) . . ? C211 H216 2.034(7) . . ? C212 C214 2.385(11) . . ? C212 C215 2.732(12) . . ? C212 C216 2.375(12) . . ? C212 H213 2.055(8) . . ? C212 H232 2.690(10) . . ? C213 C215 2.368(13) . . ? C213 C216 2.763(12) . . ? C213 H212 2.036(8) . . ? C213 H214 2.017(8) . . ? C214 C216 2.403(12) . . ? C214 H213 2.036(10) . . ? C214 H215 2.027(10) . . ? C215 H214 2.031(9) . . ? C215 H216 2.048(9) . . ? C216 H124 2.692(10) . '3 556' ? C216 H215 2.049(8) . . ? C221 C223 2.401(11) . . ? C221 C224 2.776(12) . . ? C221 C225 2.432(14) . . ? C221 C231 2.913(12) . . ? C221 H222 2.040(8) . . ? C221 H226 2.051(9) . . ? C222 C224 2.416(14) . . ? C222 C225 2.800(15) . . ? C222 C226 2.412(14) . . ? C222 H223 2.053(8) . . ? C223 C225 2.374(15) . . ? C223 C226 2.754(12) . . ? C223 H222 2.071(11) . . ? C223 H224 2.006(11) . . ? C224 C226 2.392(12) . . ? C224 H223 2.022(11) . . ? C224 H225 2.031(10) . . ? C225 H224 2.002(9) . . ? C225 H226 2.062(9) . . ? C226 H225 2.054(10) . . ? C231 C233 2.409(14) . . ? C231 C234 2.775(15) . . ? C231 C235 2.406(14) . . ? C231 H222 2.680(8) . . ? C231 H232 2.033(7) . . ? C231 H236 2.054(7) . . ? C232 C234 2.388(16) . . ? C232 C235 2.753(14) . . ? C232 C236 2.392(11) . . ? C232 H233 2.041(10) . . ? C233 C235 2.381(13) . . ? C233 C236 2.777(13) . . ? C233 H232 2.044(13) . . ? C233 H234 2.028(12) . . ? C234 C236 2.406(15) . . ? C234 H233 2.008(9) . . ? C234 H235 2.058(9) . . ? C235 H234 2.012(11) . . ? C235 H236 2.027(11) . . ? C236 H235 2.020(10) . . ? H112 H113 2.3450(4) . . ? H113 H114 2.3124(3) . . ? H114 H115 2.3299(2) . . ? H115 H116 2.3300(4) . . ? H122 H123 2.3247(3) . . ? H123 H124 2.3336(4) . . ? H124 H125 2.3520(4) . . ? H125 H126 2.3204(4) . . ? H132 H133 2.3323(3) . . ? H133 H134 2.3314(3) . . ? H134 H135 2.2936(2) . . ? H135 H136 2.3645(3) . . ? H212 H213 2.3400(4) . . ? H213 H214 2.3329(3) . . ? H214 H215 2.3227(3) . . ? H215 H216 2.3663(4) . . ? H222 H223 2.3639(3) . . ? H223 H224 2.3161(3) . . ? H224 H225 2.3159(3) . . ? H225 H226 2.3600(3) . . ? H232 H233 2.3304(3) . . ? H233 H234 2.3370(4) . . ? H234 H235 2.3361(3) . . ? H235 H236 2.2978(3) . . ? H2a H2b 1.5513(2) . . ? _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 C47_H32_Au2_O9_P2_Ru3 _chemical_formula_structural (PPh3PAu)2Ru3(CO)9(CCH2) _exptl_crystal_F_000 2824 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 24 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min -29 _reflns_limit_l_max 27 _reflns_number_observed ? _reflns_d_resolution_high .735 _reflns_d_resolution_low 10.784 _diffrn_reflns_av_sigmaI/netI .073 _diffrn_reflns_theta_min 1.88 _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 atomblock _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .086 _refine_ls_wR_factor_all .056 _refine_ls_goodness_of_fit_all 1.646 _refine_ls_shift/su_mean .003 data_br553 _audit_creation_date 97-01-16 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical C29_H19_O9_P_Ru3 #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural [HRu3(CHCHCOH)(CO)6(PPh3)] #ActaC _chemical_formula_sum C29_H19_O9_P_Ru3 #ActaC _chemical_formula_weight 845.65 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection 'Enraf Nonius software' #ActaC _computing_cell_refinement 'Enraf Nonius software' #ActaC _computing_data_reduction xtal_DIFDAT_ABSORB_SORTRF_ADDREF #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 14.567(4) #ActaC _cell_length_b 12.553(4) #ActaC _cell_length_c 9.122(5) #ActaC _cell_angle_alpha 89.16(3) #ActaC _cell_angle_beta 81.42(3) #ActaC _cell_angle_gamma 65.88(3) #ActaC _cell_volume 1503.4(11) #ActaC _cell_formula_units_Z ? #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 8 #ActaC _cell_measurement_theta_min 18.7 #ActaC _cell_measurement_theta_max 23.1 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting triclinic #ActaC _symmetry_space_group_name_H-M p_-1 #ActaC _symmetry_space_group_name_Hall -p_1 #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,-y,-z _exptl_crystal_description ? #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour ? #ActaC _exptl_crystal_size_max 0.25 #ActaC _exptl_crystal_size_mid 0.12 #ActaC _exptl_crystal_size_min 0.08 #ActaC _exptl_crystal_density_diffrn 1.868 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 824 #ActaC _exptl_absorpt_process_details 'XTAL ABSORB' _exptl_absorpt_coefficient_mu 1.59 #ActaC _exptl_absorpt_correction_type gaussian #ActaC _exptl_absorpt_correction_T_min 0.83 #ActaC _exptl_absorpt_correction_T_max 0.89 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type xray_tube #ActaC _diffrn_radiation_source 'rotating anode' #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector 'single counter' #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method 'theta/omega scans' #ActaC _diffrn_standards_number 8 #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time 3600 #ActaC _diffrn_standards_decay_% 0 #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC 11 7 5 -11 -7 -5 -6 6 5 6 -6 -5 8 -7 5 -8 7 -5 8 7 -5 -8 -7 5 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 5274 #ActaC _diffrn_reflns_av_R_equivalents 0 #ActaC _diffrn_reflns_av_sigmaI/netI 0 #ActaC _diffrn_reflns_limit_h_min -17 #ActaC _diffrn_reflns_limit_h_max 17 #ActaC _diffrn_reflns_limit_k_min -14 #ActaC _diffrn_reflns_limit_k_max 14 #ActaC _diffrn_reflns_limit_l_min -10 #ActaC _diffrn_reflns_limit_l_max 0 #ActaC _diffrn_reflns_theta_min 1.55 #ActaC _diffrn_reflns_theta_max 24.98 #ActaC _diffrn_reflns_reduction_process equatorial_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 58 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 P ? 0 2 .09 .095 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 18 .008 .006 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 38 0 0 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 #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Ru1 .70781(2) .79650(3) .10673(3) .0285(3) Uani ? ? Ru2 .88586(2) .83348(3) .04728(4) .0362(3) Uani ? ? Ru3 .86162(3) .72853(3) .31244(4) .0404(3) Uani ? ? C11 .6098(3) .9073(4) .2567(5) .041(4) Uani ? ? O11 .5524(3) .9794(3) .3397(4) .068(3) Uani ? ? C12 .6467(3) .9038(4) -.0314(5) .039(4) Uani ? ? O12 .6100(3) .9748(3) -.1096(4) .062(3) Uani ? ? C21 .7905(4) .9684(4) .1636(6) .056(5) Uani ? ? O21 .7404(3) 1.0551(3) .2270(4) .080(4) Uani ? ? C22 1.0042(4) .8559(4) .0670(6) .060(5) Uani ? ? O22 1.0739(3) .8723(4) .0797(6) .098(5) Uani ? ? C23 .8823(4) .8935(4) -.1456(6) .054(5) Uani ? ? O23 .8837(4) .9246(4) -.2632(4) .091(5) Uani ? ? C31 .7623(4) .8359(5) .4701(6) .054(5) Uani ? ? O31 .7068(3) .8967(4) .5637(4) .088(5) Uani ? ? C32 .9712(4) .7468(4) .3835(6) .064(5) Uani ? ? O32 1.0375(3) .7565(4) .4224(5) .102(5) Uani ? ? C33 .8810(4) .5906(5) .4143(6) .056(5) Uani ? ? O33 .8961(3) .5048(3) .4690(5) .087(5) Uani ? ? C1 .9586(3) .6519(4) .1200(5) .044(4) Uani ? ? C2 .9325(3) .6433(4) -.0199(5) .042(4) Uani ? ? C3 .8313(3) .6983(3) -.0476(5) .037(4) Uani ? ? O3 .8278(3) .6814(3) -.1953(4) .054(4) Uani ? ? P1 .62208(8) .67751(9) .08348(11) .0321(9) Uani ? ? C111 .6722(3) .5336(3) .1636(4) .033(3) Uani ? ? C112 .7753(3) .4761(4) .1667(5) .045(4) Uani ? ? C113 .8158(4) .3675(4) .2239(6) .055(5) Uani ? ? C114 .7522(4) .3152(5) .2796(6) .057(5) Uani ? ? C115 .6500(4) .3709(5) .2771(6) .056(5) Uani ? ? C116 .6102(4) .4787(4) .2182(5) .047(5) Uani ? ? C121 .6251(3) .6418(4) -.1112(4) .038(4) Uani ? ? C122 .6742(4) .5289(4) -.1730(5) .052(5) Uani ? ? C123 .6778(5) .5089(6) -.3243(6) .067(6) Uani ? ? C124 .6338(5) .5977(6) -.4106(6) .073(7) Uani ? ? C125 .5856(5) .7084(6) -.3514(6) .065(6) Uani ? ? C126 .5796(4) .7321(5) -.2013(5) .052(5) Uani ? ? C131 .4870(3) .7345(4) .1600(5) .039(4) Uani ? ? C132 .4133(4) .7319(5) .0826(7) .057(5) Uani ? ? C133 .3130(4) .7724(5) .1476(8) .073(6) Uani ? ? C134 .2845(4) .8125(5) .2921(9) .072(6) Uani ? ? C135 .3563(4) .8148(5) .3720(7) .066(6) Uani ? ? C136 .4567(4) .7762(4) .3064(5) .048(4) Uani ? ? H112 .820(3) .504(3) .127(4) .028(10) Uiso ? ? H113 .885(3) .327(4) .230(4) .048(13) Uiso ? ? H114 .776(3) .247(4) .311(4) .037(12) Uiso ? ? H115 .608(3) .344(4) .314(5) .046(13) Uiso ? ? H116 .551(3) .512(4) .227(5) .045(14) Uiso ? ? H122 .707(3) .463(4) -.113(4) .045(12) Uiso ? ? H123 .714(3) .432(4) -.359(5) .052(14) Uiso ? ? H124 .644(4) .581(5) -.500(6) .09(2) Uiso ? ? H125 .554(4) .770(5) -.391(6) .07(2) Uiso ? ? H126 .544(3) .804(4) -.165(5) .056(15) Uiso ? ? H132 .426(3) .718(4) -.007(5) .047(15) Uiso ? ? H133 .269(3) .767(3) .087(5) .045(12) Uiso ? ? H134 .213(4) .841(4) .339(6) .079(17) Uiso ? ? H135 .335(3) .844(4) .462(5) .045(14) Uiso ? ? H136 .506(3) .783(3) .348(4) .040(12) Uiso ? ? H1 1.035(3) .614(3) .114(4) .042(11) Uiso ? ? H2 .982(3) .602(4) -.100(5) .050(13) Uiso ? ? H3 .778(4) .703(5) -.206(6) .05(2) Uiso ? ? H .765(3) .699(4) .248(5) .064(14) Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Ru1 .02736(17) .02946(18) .02992(18) -.01191(14) -.00771(13) .00080(13) Ru2 .03189(19) .03079(19) .0494(2) -.01610(15) -.00761(15) .00277(15) Ru3 .0403(2) .0407(2) .0474(2) -.01927(17) -.02094(17) .00934(16) C11 .038(2) .046(3) .039(3) -.014(2) -.011(2) .001(2) O11 .058(2) .070(2) .056(2) -.007(2) .0013(18) -.0229(19) C12 .040(2) .038(2) .042(3) -.018(2) -.008(2) .003(2) O12 .072(2) .055(2) .059(2) -.0214(18) -.0302(19) .0213(18) C21 .061(3) .046(3) .065(3) -.029(3) -.004(3) -.002(3) O21 .089(3) .042(2) .097(3) -.024(2) .013(2) -.024(2) C22 .047(3) .048(3) .092(4) -.023(3) -.020(3) .013(3) O22 .058(3) .094(3) .169(5) -.051(2) -.037(3) .021(3) C23 .057(3) .048(3) .061(3) -.026(2) -.012(3) .008(2) O23 .128(4) .087(3) .064(3) -.052(3) -.016(3) .021(2) C31 .066(3) .064(3) .046(3) -.036(3) -.024(3) .008(3) O31 .094(3) .097(3) .060(3) -.029(3) -.004(2) -.022(2) C32 .066(4) .060(3) .078(4) -.031(3) -.035(3) .012(3) O32 .090(3) .120(4) .138(4) -.068(3) -.074(3) .027(3) C33 .051(3) .061(3) .061(3) -.024(3) -.027(3) .014(3) O33 .096(3) .069(3) .114(3) -.041(2) -.060(3) .054(3) C1 .025(2) .034(2) .073(3) -.011(2) -.008(2) .007(2) C2 .036(2) .029(2) .058(3) -.014(2) .001(2) -.004(2) C3 .039(2) .031(2) .044(3) -.018(2) -.005(2) -.0020(18) O3 .053(3) .066(2) .043(2) -.028(2) .0015(18) -.0123(16) P1 .0328(6) .0373(6) .0307(6) -.0176(5) -.0093(4) .0020(4) C111 .037(2) .034(2) .030(2) -.0160(19) -.0074(18) -.0001(17) C112 .040(3) .037(3) .057(3) -.018(2) -.001(2) .003(2) C113 .043(3) .039(3) .078(4) -.012(2) -.012(3) .008(2) C114 .063(4) .039(3) .071(4) -.022(3) -.014(3) .014(3) C115 .062(4) .056(3) .066(3) -.040(3) -.018(3) .022(3) C116 .042(3) .056(3) .053(3) -.026(3) -.015(2) .009(2) C121 .042(2) .054(3) .032(2) -.031(2) -.0100(19) .002(2) C122 .065(3) .053(3) .041(3) -.028(3) -.012(2) -.001(2) C123 .091(4) .066(4) .045(3) -.031(3) -.012(3) -.015(3) C124 .108(5) .099(5) .032(3) -.061(4) -.013(3) -.005(3) C125 .086(4) .082(4) .047(3) -.049(4) -.034(3) .014(3) C126 .068(3) .059(3) .043(3) -.035(3) -.024(3) .004(3) C131 .029(2) .045(2) .044(3) -.017(2) -.0061(19) .007(2) C132 .047(3) .072(4) .059(4) -.028(3) -.018(3) .003(3) C133 .038(3) .088(4) .102(5) -.028(3) -.028(3) .015(4) C134 .033(3) .060(4) .114(6) -.013(3) -.004(3) .017(4) C135 .065(4) .057(3) .063(4) -.023(3) .019(3) .002(3) C136 .047(3) .055(3) .046(3) -.024(2) -.007(2) .003(2) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls:_Fsqd_sigma_weight______full_matrix _refine_ls_structure_factor_coef Fsqd #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment refined #ActaC _refine_ls_extinction_method Zachariasen #ActaC _refine_ls_extinction_coef 113(66) #ActaC _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 5274 #ActaC _refine_ls_number_parameters 456 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .039 #ActaC _refine_ls_R_factor_obs .039 #ActaC _refine_ls_wR_factor_all .063 #ActaC _refine_ls_wR_factor_obs .063 #ActaC _refine_ls_goodness_of_fit_all 1.229 #ActaC _refine_ls_goodness_of_fit_obs 1.229 #ActaC _refine_ls_shift/esd_max .071 #ActaC _refine_ls_shift/esd_mean .002 #ActaC _refine_diff_density_min -.5 #ActaC _refine_diff_density_max .555 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Ru1 Ru2 2.7917(9) . . ? Ru1 Ru3 2.9857(10) . . ? Ru1 C11 1.922(4) . . ? Ru1 C12 1.871(4) . . ? Ru1 C3 2.054(4) . . ? Ru1 P1 2.3342(15) . . ? Ru1 H 1.81(4) . . ? Ru2 Ru3 2.7826(13) . . ? Ru2 C21 1.901(4) . . ? Ru2 C22 1.891(6) . . ? Ru2 C23 1.903(5) . . ? Ru2 C1 2.224(4) . . ? Ru2 C2 2.265(4) . . ? Ru2 C3 2.368(5) . . ? Ru3 C31 1.955(4) . . ? Ru3 C32 1.906(7) . . ? Ru3 C33 1.890(6) . . ? Ru3 C1 2.050(4) . . ? Ru3 H 1.77(5) . . ? C11 O11 1.141(5) . . ? C12 O12 1.137(5) . . ? C21 O21 1.138(6) . . ? C22 O22 1.137(8) . . ? C23 O23 1.136(7) . . ? C31 O31 1.128(6) . . ? C32 O32 1.128(9) . . ? C33 O33 1.132(7) . . ? C1 C2 1.402(7) . . ? C1 H1 1.01(4) . . ? C2 C3 1.410(6) . . ? C2 H2 .93(4) . . ? C3 O3 1.379(6) . . ? O3 H3 .68(5) . . ? P1 C111 1.837(4) . . ? P1 C121 1.828(4) . . ? P1 C131 1.824(4) . . ? C111 C112 1.380(6) . . ? C111 C116 1.379(8) . . ? C112 C113 1.376(7) . . ? C112 H112 .88(4) . . ? C113 C114 1.375(9) . . ? C113 H113 .94(4) . . ? C114 C115 1.366(8) . . ? C114 H114 .84(4) . . ? C115 C116 1.373(7) . . ? C115 H115 .83(5) . . ? C116 H116 .78(4) . . ? C121 C122 1.382(6) . . ? C121 C126 1.387(7) . . ? C122 C123 1.396(7) . . ? C122 H122 .98(4) . . ? C123 C124 1.347(9) . . ? C123 H123 .92(4) . . ? C124 C125 1.351(9) . . ? C124 H124 .82(6) . . ? C125 C126 1.388(8) . . ? C125 H125 .83(5) . . ? C126 H126 .88(4) . . ? C131 C132 1.381(8) . . ? C131 C136 1.381(6) . . ? C132 C133 1.373(8) . . ? C132 H132 .81(4) . . ? C133 C134 1.359(11) . . ? C133 H133 .93(5) . . ? C134 C135 1.371(11) . . ? C134 H134 .98(5) . . ? C135 C136 1.379(8) . . ? C135 H135 .87(4) . . ? C136 H136 .89(5) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC Ru1 O11 3.061(3) . . ? Ru1 O12 3.006(3) . . ? Ru1 C21 2.953(7) . . ? Ru1 C1 3.371(4) . . ? Ru1 C2 3.089(4) . . ? Ru1 O3 3.058(4) . . ? Ru1 C121 3.453(5) . . ? Ru1 H3 2.97(5) . . ? Ru2 C12 3.413(5) . . ? Ru2 O21 3.033(3) . . ? Ru2 O22 3.027(5) . . ? Ru2 O23 3.039(4) . . ? Ru2 C32 3.474(6) . . ? Ru2 O3 3.355(5) . . ? Ru2 H1 2.85(3) . . ? Ru2 H2 2.91(4) . . ? Ru3 C21 3.120(5) . . ? Ru3 O31 3.083(4) . . ? Ru3 O32 3.034(6) . . ? Ru3 O33 3.020(4) . . ? Ru3 C2 3.108(5) . . ? Ru3 C3 3.425(5) . . ? Ru3 H1 2.73(3) . . ? C11 C12 2.601(6) . . ? C11 H136 2.63(5) . . ? C11 H 2.66(4) . . ? C12 C3 2.852(5) . . ? C21 C22 2.844(7) . . ? C21 C23 2.924(7) . . ? C22 C23 2.731(8) . . ? C22 C1 2.914(8) . . ? O22 H133 2.61(4) . 1_655 ? C23 C3 2.929(8) . . ? C31 C32 2.768(8) . . ? C31 C33 2.857(7) . . ? C31 H 2.66(5) . . ? C32 C33 2.762(9) . . ? C32 C1 2.761(8) . . ? C33 C1 2.970(7) . . ? C33 H 2.42(4) . . ? C1 C3 2.460(7) . . ? C1 H2 2.05(4) . . ? C2 O3 2.286(7) . . ? C2 H1 1.98(4) . . ? C3 H2 2.01(4) . . ? C3 H3 1.72(6) . . ? O3 H2 2.34(4) . . ? P1 C112 2.790(4) . . ? P1 C116 2.823(6) . . ? P1 C122 2.823(5) . . ? P1 C126 2.772(5) . . ? P1 C132 2.833(6) . . ? P1 C136 2.765(5) . . ? P1 H136 2.74(4) . . ? C111 C113 2.402(6) . . ? C111 C114 2.768(6) . . ? C111 C115 2.392(8) . . ? C111 C121 2.872(6) . . ? C111 C131 2.847(5) . . ? C111 H112 2.00(4) . . ? C111 H116 1.90(5) . . ? C111 H122 2.59(4) . . ? C112 C114 2.376(8) . . ? C112 C115 2.733(9) . . ? C112 C116 2.368(8) . . ? C112 H113 2.05(4) . . ? C113 C115 2.373(9) . . ? C113 C116 2.747(7) . . ? C113 H112 1.93(4) . . ? C113 H114 1.94(5) . . ? C114 C116 2.376(7) . . ? C114 H113 1.98(5) . . ? C114 H115 1.95(5) . . ? C115 H114 1.93(4) . . ? C115 H116 1.88(4) . . ? C116 H115 1.89(5) . . ? C121 C123 2.399(7) . . ? C121 C124 2.768(7) . . ? C121 C125 2.400(7) . . ? C121 C131 2.865(5) . . ? C121 H122 2.07(4) . . ? C121 H126 1.99(4) . . ? C121 H132 2.67(4) . . ? C121 H3 2.67(6) . . ? C122 C124 2.387(8) . . ? C122 C125 2.745(8) . . ? C122 C126 2.385(7) . . ? C122 H123 1.97(4) . . ? C123 C125 2.339(9) . . ? C123 C126 2.738(8) . . ? C123 H122 2.06(4) . . ? C123 H124 1.86(6) . . ? C124 C126 2.381(8) . . ? C124 H123 2.02(4) . . ? C124 H125 1.99(5) . . ? C125 H124 1.93(5) . . ? C125 H126 1.96(5) . . ? C126 H125 1.84(5) . . ? C126 H132 2.70(5) . . ? C131 C133 2.400(8) . . ? C131 C134 2.779(7) . . ? C131 C135 2.402(7) . . ? C131 H116 2.65(4) . . ? C131 H132 1.92(5) . . ? C131 H136 1.92(4) . . ? C132 C134 2.372(8) . . ? C132 C135 2.731(9) . . ? C132 C136 2.363(9) . . ? C132 H133 1.96(5) . . ? C133 C135 2.358(11) . . ? C133 C136 2.734(10) . . ? C133 H132 1.89(4) . . ? C133 H134 2.04(5) . . ? C134 C136 2.383(9) . . ? C134 H133 2.03(5) . . ? C134 H135 1.92(5) . . ? C135 H134 2.04(6) . . ? C135 H136 2.03(5) . . ? C136 H135 1.99(4) . . ? H112 H113 2.28(5) . . ? H113 H114 2.23(7) . . ? H114 H115 2.24(6) . . ? H115 H116 2.11(6) . . ? H122 H123 2.27(6) . . ? H123 H124 2.23(7) . . ? H124 H125 2.34(7) . . ? H125 H126 2.08(7) . . ? H132 H133 2.16(6) . . ? H133 H134 2.38(6) . . ? H134 H135 2.25(8) . . ? H135 H136 2.36(6) . . ? H1 H2 2.24(6) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC Ru2 Ru1 Ru3 57.47(3) . . . ? Ru2 Ru1 C11 111.33(17) . . . ? Ru2 Ru1 C12 91.96(16) . . . ? Ru2 Ru1 C3 56.05(15) . . . ? Ru2 Ru1 P1 149.38(3) . . . ? Ru2 Ru1 H 87.5(16) . . . ? Ru3 Ru1 C11 89.67(14) . . . ? Ru3 Ru1 C12 145.15(17) . . . ? Ru3 Ru1 C3 83.43(13) . . . ? Ru3 Ru1 P1 118.38(3) . . . ? Ru3 Ru1 H 33.0(17) . . . ? C11 Ru1 C12 86.55(17) . . . ? C11 Ru1 C3 167.4(2) . . . ? C11 Ru1 P1 98.56(17) . . . ? C11 Ru1 H 90.8(11) . . . ? C12 Ru1 C3 93.07(16) . . . ? C12 Ru1 P1 96.43(17) . . . ? C12 Ru1 H 176.9(14) . . . ? C3 Ru1 P1 94.03(15) . . . ? C3 Ru1 H 89.2(11) . . . ? P1 Ru1 H 85.6(17) . . . ? Ru1 Ru2 Ru3 64.771(18) . . . ? Ru1 Ru2 C21 75.3(2) . . . ? Ru1 Ru2 C22 163.45(17) . . . ? Ru1 Ru2 C23 103.74(18) . . . ? Ru1 Ru2 C1 83.62(13) . . . ? Ru1 Ru2 C2 74.47(12) . . . ? Ru1 Ru2 C3 46.02(9) . . . ? Ru3 Ru2 C21 81.19(16) . . . ? Ru3 Ru2 C22 99.80(17) . . . ? Ru3 Ru2 C23 167.8(2) . . . ? Ru3 Ru2 C1 46.71(12) . . . ? Ru3 Ru2 C2 75.23(13) . . . ? Ru3 Ru2 C3 82.94(11) . . . ? C21 Ru2 C22 97.2(2) . . . ? C21 Ru2 C23 100.5(2) . . . ? C21 Ru2 C1 127.8(2) . . . ? C21 Ru2 C2 147.5(2) . . . ? C21 Ru2 C3 120.3(2) . . . ? C22 Ru2 C23 92.0(3) . . . ? C22 Ru2 C1 89.8(2) . . . ? C22 Ru2 C2 108.57(18) . . . ? C22 Ru2 C3 142.28(16) . . . ? C23 Ru2 C1 131.08(18) . . . ? C23 Ru2 C2 98.2(2) . . . ? C23 Ru2 C3 85.8(2) . . . ? C1 Ru2 C2 36.39(19) . . . ? C1 Ru2 C3 64.68(17) . . . ? C2 Ru2 C3 35.34(15) . . . ? Ru1 Ru3 Ru2 57.76(3) . . . ? Ru1 Ru3 C31 91.39(17) . . . ? Ru1 Ru3 C32 149.66(17) . . . ? Ru1 Ru3 C33 116.31(19) . . . ? Ru1 Ru3 C1 81.75(14) . . . ? Ru1 Ru3 H 33.9(14) . . . ? Ru2 Ru3 C31 114.09(16) . . . ? Ru2 Ru3 C32 93.74(17) . . . ? Ru2 Ru3 C33 148.84(15) . . . ? Ru2 Ru3 C1 52.17(12) . . . ? Ru2 Ru3 H 88.6(14) . . . ? C31 Ru3 C32 91.6(2) . . . ? C31 Ru3 C33 96.0(2) . . . ? C31 Ru3 C1 166.2(2) . . . ? C31 Ru3 H 91.1(12) . . . ? C32 Ru3 C33 93.4(2) . . . ? C32 Ru3 C1 88.5(2) . . . ? C32 Ru3 H 175.4(13) . . . ? C33 Ru3 C1 97.79(19) . . . ? C33 Ru3 H 82.6(14) . . . ? C1 Ru3 H 89.8(12) . . . ? Ru1 C11 O11 175.0(4) . . . ? Ru1 C12 O12 175.3(5) . . . ? Ru2 C21 O21 172.3(6) . . . ? Ru2 C22 O22 178.3(4) . . . ? Ru2 C23 O23 176.8(4) . . . ? Ru3 C31 O31 178.1(5) . . . ? Ru3 C32 O32 178.4(5) . . . ? Ru3 C33 O33 176.4(4) . . . ? Ru2 C1 Ru3 81.13(13) . . . ? Ru2 C1 C2 73.4(3) . . . ? Ru2 C1 H1 119(3) . . . ? Ru3 C1 C2 127.4(3) . . . ? Ru3 C1 H1 123(2) . . . ? C2 C1 H1 110(2) . . . ? Ru2 C2 C1 70.2(3) . . . ? Ru2 C2 C3 76.3(2) . . . ? Ru2 C2 H2 126(3) . . . ? C1 C2 C3 122.0(4) . . . ? C1 C2 H2 122(3) . . . ? C3 C2 H2 116(3) . . . ? Ru1 C3 Ru2 77.93(14) . . . ? Ru1 C3 C2 125.1(3) . . . ? Ru1 C3 O3 124.7(3) . . . ? Ru2 C3 C2 68.3(3) . . . ? Ru2 C3 O3 125.0(3) . . . ? C2 C3 O3 110.1(3) . . . ? C3 O3 H3 109(4) . . . ? Ru1 P1 C111 116.90(17) . . . ? Ru1 P1 C121 111.52(18) . . . ? Ru1 P1 C131 117.91(17) . . . ? C111 P1 C121 103.2(2) . . . ? C111 P1 C131 102.1(2) . . . ? C121 P1 C131 103.3(2) . . . ? P1 C111 C112 119.6(4) . . . ? P1 C111 C116 122.1(3) . . . ? C112 C111 C116 118.2(4) . . . ? C111 C112 C113 121.3(5) . . . ? C111 C112 H112 123(2) . . . ? C113 C112 H112 116(2) . . . ? C112 C113 C114 119.4(5) . . . ? C112 C113 H113 124(3) . . . ? C114 C113 H113 117(3) . . . ? C113 C114 C115 120.0(5) . . . ? C113 C114 H114 120(3) . . . ? C115 C114 H114 120(3) . . . ? C114 C115 C116 120.4(6) . . . ? C114 C115 H115 123(3) . . . ? C116 C115 H115 116(3) . . . ? C111 C116 C115 120.7(5) . . . ? C111 C116 H116 120(4) . . . ? C115 C116 H116 118(4) . . . ? P1 C121 C122 122.5(3) . . . ? P1 C121 C126 118.5(3) . . . ? C122 C121 C126 118.9(4) . . . ? C121 C122 C123 119.4(5) . . . ? C121 C122 H122 121(2) . . . ? C123 C122 H122 119(2) . . . ? C122 C123 C124 121.0(6) . . . ? C122 C123 H123 115(3) . . . ? C124 C123 H123 124(3) . . . ? C123 C124 C125 120.2(6) . . . ? C123 C124 H124 116(4) . . . ? C125 C124 H124 123(4) . . . ? C124 C125 C126 120.7(6) . . . ? C124 C125 H125 130(4) . . . ? C126 C125 H125 110(4) . . . ? C121 C126 C125 119.8(5) . . . ? C121 C126 H126 122(3) . . . ? C125 C126 H126 118(3) . . . ? P1 C131 C132 123.7(3) . . . ? P1 C131 C136 118.6(4) . . . ? C132 C131 C136 117.6(4) . . . ? C131 C132 C133 121.2(6) . . . ? C131 C132 H132 120(4) . . . ? C133 C132 H132 118(3) . . . ? C132 C133 C134 120.5(7) . . . ? C132 C133 H133 115(2) . . . ? C134 C133 H133 124(2) . . . ? C133 C134 C135 119.5(5) . . . ? C133 C134 H134 121(3) . . . ? C135 C134 H134 120(3) . . . ? C134 C135 C136 120.2(6) . . . ? C134 C135 H135 117(3) . . . ? C136 C135 H135 123(3) . . . ? C131 C136 C135 121.0(5) . . . ? C131 C136 H136 114(2) . . . ? C135 C136 H136 125(2) . . . ? Ru1 H Ru3 113(3) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min -14 _reflns_limit_k_max 14 _reflns_limit_l_min -10 _reflns_limit_l_max 0 _reflns_number_total 5274 #ActaC _reflns_number_observed 5274 #ActaC _reflns_observed_criterion ? _reflns_d_resolution_high .841 _reflns_d_resolution_low 13.096 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 2.4999 _publ_requested_journal ? #ActaC _publ_requested_coeditor_name ? #ActaC _publ_contact_author #ActaC ; ? name ? institute ? department ? address ? city ? country ; _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_contact_author_phone ? #ActaC _publ_contact_author_fax ? #ActaC _publ_contact_author_email ? #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title #ActaC ; ? ; _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; ? ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #============================================================================== # (IUCr Office 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 ?