Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_gk38 _database_code_CSD 175273 data_global _audit_creation_method Xtal3.6 _audit_creation_date 01-11-29 _audit_update_record ? _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Koutsantonis, George' 'Griffith, Christopher S.' 'Skelton, Brian W.' 'White, Allan H.' _publ_contact_author_name 'Dr George Koutsantonis' _publ_contact_author_address ; Department of Chemistry University of Western Australia 35 Stirling Highway Crawley Western Australia 6009 Australia ; _publ_contact_author_email GAK@CHEM.UWA.EDU.AU _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_phone (+61)_08-9380_3481 _publ_section_title ; Reactions of Metalloalkynes. New C2 Bonding Mode in a Trimetallic Complex ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C23 H15 B1 F4 O6 Ru3' _chemical_formula_moiety ? _chemical_formula_weight 777.38 _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 14.292(3) _cell_length_b 10.397(3) _cell_length_c 9.281(3) _cell_angle_alpha 93.04(3) _cell_angle_beta 103.04(2) _cell_angle_gamma 107.29(2) _cell_volume 1272.1(7) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 2.029 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 18.9 _cell_measurement_theta_max 25.9 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.824 _exptl_crystal_description prism _exptl_crystal_size_max .75 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .18 _exptl_crystal_size_rad ? _exptl_crystal_colour dark _diffrn_measurement_device_type ; CAD4 diffractometer ; _diffrn_measurement_method '2\q-\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; Xtal absorb ; _exptl_absorpt_correction_T_min .58 _exptl_absorpt_correction_T_max .75 _diffrn_reflns_number 9772 _reflns_number_total 6140 _reflns_Friedel_coverage ? _reflns_number_gt 5065 _reflns_threshold_expression 'I > 3.00 sig(I )' _diffrn_reflns_theta_max 28.03 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .048 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 5 _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .06 _refine_ls_wR_factor_ref .071 _refine_ls_goodness_of_fit_ref 1.901 _refine_ls_number_reflns 5065 _refine_ls_number_parameters 335 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .049 _refine_diff_density_min -1.281 _refine_diff_density_max 1.185 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Enraf Nonius Software' _computing_cell_refinement 'Enraf Nonius Software' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 46 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 30 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' B ? 0 2 0 .000977 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 8 .013977 .01001 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 12 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 6 -1.42 .835999 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 .91546(3) .72622(4) .63068(4) .04423(15) Uani ? ? 1.00000 ? ? Ru2 .75153(4) .58378(4) .91465(5) .0541(2) Uani ? ? 1.00000 ? ? Ru3 .62539(3) .85242(4) .71555(5) .0539(2) Uani ? ? 1.00000 ? ? C11 .9944(5) .8810(6) .7642(7) .062(2) Uani ? ? 1.00000 ? ? O11 1.0449(5) .9754(5) .8463(6) .092(2) Uani ? ? 1.00000 ? ? C12 .9735(4) .6197(6) .7529(6) .056(2) Uani ? ? 1.00000 ? ? O12 1.0090(4) .5503(5) .8204(5) .084(2) Uani ? ? 1.00000 ? ? C101 .9661(6) .6762(7) .4298(6) .067(3) Uani ? ? 1.00000 ? ? C102 .8671(7) .5863(7) .4147(7) .074(3) Uani ? ? 1.00000 ? ? C103 .8012(5) .6644(7) .4068(6) .071(3) Uani ? ? 1.00000 ? ? C104 .8568(6) .8007(7) .4173(6) .069(3) Uani ? ? 1.00000 ? ? C105 .9598(5) .8057(7) .4306(6) .067(3) Uani ? ? 1.00000 ? ? C21 .8844(5) .6780(6) 1.0255(6) .057(2) Uani ? ? 1.00000 ? ? O21 .9670(4) .7312(5) 1.0860(5) .076(2) Uani ? ? 1.00000 ? ? C22 .7012(6) .6857(8) 1.0303(7) .079(3) Uani ? ? 1.00000 ? ? O22 .6665(6) .7423(9) 1.1022(6) .132(5) Uani ? ? 1.00000 ? ? C201 .7298(10) .4036(8) .7534(12) .101(5) Uani ? ? 1.00000 ? ? C202 .6398(8) .4143(9) .7451(11) .103(5) Uani ? ? 1.00000 ? ? C203 .6174(8) .3976(10) .8773(17) .122(6) Uani ? ? 1.00000 ? ? C204 .6967(12) .3790(10) .9801(11) .119(6) Uani ? ? 1.00000 ? ? C205 .7709(8) .3790(8) .904(2) .142(7) Uani ? ? 1.00000 ? ? C31 .6040(5) .7966(7) .5127(9) .072(3) Uani ? ? 1.00000 ? ? O31 .5939(5) .7677(7) .3895(6) .105(3) Uani ? ? 1.00000 ? ? C32 .5183(5) .7006(8) .7305(10) .082(3) Uani ? ? 1.00000 ? ? O32 .4543(5) .6092(7) .7395(10) .130(4) Uani ? ? 1.00000 ? ? C301 .5709(7) 1.0225(10) .7758(13) .102(5) Uani ? ? 1.00000 ? ? C302 .6329(9) .9975(9) .9090(10) .107(5) Uani ? ? 1.00000 ? ? C303 .7290(8) 1.0242(9) .8896(13) .109(5) Uani ? ? 1.00000 ? ? C304 .7277(7) 1.0660(8) .7460(12) .095(4) Uani ? ? 1.00000 ? ? C305 .6318(7) 1.0664(7) .6838(10) .087(4) Uani ? ? 1.00000 ? ? C1 .8009(4) .7174(5) .7351(5) .0467(18) Uani ? ? 1.00000 ? ? C2 .7275(4) .7481(5) .7521(6) .050(2) Uani ? ? 1.00000 ? ? B .7501(7) 1.1705(10) .3469(13) .088(4) Uani ? ? 1.00000 ? ? F11 .8021(6) 1.2313(9) .2517(9) .179(5) Uani ? ? 1.00000 ? ? F12 .6591(6) 1.1080(16) .2915(15) .302(11) Uani ? ? 1.00000 ? ? F13 .7736(12) 1.2595(9) .4613(12) .251(8) Uani ? ? 1.00000 ? ? F14 .7869(9) 1.0738(9) .3973(14) .217(7) Uani ? ? 1.00000 ? ? H101 1.02732 .65151 .43664 .08500 Uiso ? ? 1.00000 ? ? H102 .84918 .48919 .40796 .09600 Uiso ? ? 1.00000 ? ? H103 .72861 .62919 .39738 .09000 Uiso ? ? 1.00000 ? ? H104 .83220 .87787 .41776 .08800 Uiso ? ? 1.00000 ? ? H105 1.01503 .88868 .43908 .08800 Uiso ? ? 1.00000 ? ? H201 .76560 .41029 .67483 .12000 Uiso ? ? 1.00000 ? ? H202 .59765 .43086 .65777 .13000 Uiso ? ? 1.00000 ? ? H203 .55419 .39882 .89884 .15400 Uiso ? ? 1.00000 ? ? H204 .70537 .36678 1.08367 .15400 Uiso ? ? 1.00000 ? ? H205 .83751 .36674 .93500 .16500 Uiso ? ? 1.00000 ? ? H301 .49862 1.00899 .75836 .12800 Uiso ? ? 1.00000 ? ? H302 .61076 .96591 .99684 .12900 Uiso ? ? 1.00000 ? ? H303 .78598 1.01806 .96464 .13200 Uiso ? ? 1.00000 ? ? H304 .78563 1.08805 .70323 .12600 Uiso ? ? 1.00000 ? ? H305 .60878 1.09240 .58576 .12200 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru1 .0554(2) .0496(2) .0328(2) .02208(17) .01354(16) .00753(15) Ru2 .0671(3) .0591(3) .0387(2) .0200(2) .0172(2) .01344(18) Ru3 .0499(2) .0590(3) .0551(3) .02260(19) .01113(19) .0043(2) C11 .073(4) .060(3) .052(3) .019(3) .019(3) .009(3) O11 .115(4) .065(3) .070(3) .006(3) .003(3) -.005(2) C12 .068(3) .065(3) .045(3) .035(3) .018(2) .008(2) O12 .115(4) .100(3) .068(3) .072(3) .028(3) .031(3) C101 .090(4) .091(4) .039(3) .048(4) .025(3) .009(3) C102 .122(6) .063(3) .038(3) .033(4) .016(3) .001(3) C103 .080(4) .091(5) .036(3) .023(3) .008(3) .008(3) C104 .102(5) .079(4) .036(3) .046(4) .010(3) .017(3) C105 .084(4) .084(4) .039(3) .024(3) .029(3) .020(3) C21 .082(4) .057(3) .039(3) .028(3) .017(3) .016(2) O21 .082(3) .085(3) .049(2) .019(2) .008(2) -.003(2) C22 .099(5) .112(5) .046(3) .054(4) .029(3) .028(3) O22 .176(7) .225(8) .055(3) .138(6) .048(4) .023(4) C201 .142(8) .054(4) .100(7) .002(5) .059(6) -.014(4) C202 .108(7) .082(5) .085(6) -.004(5) .003(5) .013(4) C203 .088(6) .093(6) .175(12) -.004(5) .056(7) .015(7) C204 .164(11) .086(6) .081(6) .001(6) .023(7) .037(5) C205 .095(6) .048(4) .237(15) .019(4) -.037(8) -.010(6) C31 .061(3) .074(4) .073(4) .021(3) .003(3) .007(3) O31 .107(4) .143(5) .053(3) .041(4) -.003(3) -.009(3) C32 .056(3) .085(4) .107(6) .021(3) .023(4) .016(4) O32 .086(4) .114(5) .192(8) .012(4) .057(5) .050(5) C301 .089(5) .104(6) .125(8) .058(5) .020(5) -.011(6) C302 .166(9) .101(6) .076(5) .064(6) .052(6) -.007(4) C303 .103(6) .080(5) .121(8) .050(5) -.034(6) -.044(5) C304 .089(5) .062(4) .122(8) .011(4) .023(5) -.008(4) C305 .111(6) .064(4) .088(5) .044(4) .007(5) .005(4) C1 .056(3) .053(2) .033(2) .021(2) .010(2) .007(2) C2 .055(3) .053(3) .043(3) .017(2) .014(2) .009(2) B .072(5) .086(5) .105(7) .015(4) .033(5) .012(5) F11 .123(5) .247(9) .171(7) .040(6) .051(5) .112(7) F12 .088(5) .42(2) .304(14) -.026(8) .033(7) -.064(13) F13 .413(18) .134(6) .216(9) .014(9) .203(11) -.013(6) F14 .249(10) .150(6) .320(12) .114(7) .118(9) .131(7) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 C11 . . 1.865(5) ? Ru1 C12 . . 1.859(6) ? Ru1 C101 . . 2.236(7) ? Ru1 C102 . . 2.254(6) ? Ru1 C103 . . 2.258(5) ? Ru1 C104 . . 2.241(6) ? Ru1 C105 . . 2.217(6) ? Ru1 C1 . . 2.065(6) ? Ru2 C21 . . 1.879(6) ? Ru2 C22 . . 1.864(9) ? Ru2 C201 . . 2.234(10) ? Ru2 C202 . . 2.243(8) ? Ru2 C203 . . 2.228(9) ? Ru2 C204 . . 2.208(10) ? Ru2 C205 . . 2.227(10) ? Ru2 C1 . . 2.323(5) ? Ru2 C2 . . 2.388(6) ? Ru3 C31 . . 1.869(8) ? Ru3 C32 . . 1.881(7) ? Ru3 C301 . . 2.226(12) ? Ru3 C302 . . 2.245(10) ? Ru3 C303 . . 2.244(9) ? Ru3 C304 . . 2.228(7) ? Ru3 C305 . . 2.237(8) ? Ru3 C2 . . 2.044(6) ? C11 O11 . . 1.147(7) ? C12 O12 . . 1.137(8) ? C101 C102 . . 1.416(11) ? C101 C105 . . 1.376(11) ? C101 H101 . . .972 ? C102 C103 . . 1.408(13) ? C102 H102 . . .960 ? C103 C104 . . 1.389(9) ? C103 H103 . . .974 ? C104 C105 . . 1.434(12) ? C104 H104 . . .967 ? C105 H105 . . .966 ? C21 O21 . . 1.138(7) ? C22 O22 . . 1.148(13) ? C201 C202 . . 1.309(19) ? C201 C205 . . 1.46(2) ? C201 H201 . . .975 ? C202 C203 . . 1.34(2) ? C202 H202 . . .952 ? C203 C204 . . 1.376(19) ? C203 H203 . . .972 ? C204 C205 . . 1.40(2) ? C204 H204 . . .961 ? C205 H205 . . .979 ? C31 O31 . . 1.132(10) ? C32 O32 . . 1.128(10) ? C301 C302 . . 1.434(15) ? C301 C305 . . 1.355(16) ? C301 H301 . . .974 ? C302 C303 . . 1.373(18) ? C302 H302 . . .978 ? C303 C304 . . 1.421(16) ? C303 H303 . . .965 ? C304 C305 . . 1.363(14) ? C304 H304 . . .970 ? C305 H305 . . .976 ? C1 C2 . . 1.223(9) ? B F11 . . 1.345(15) ? B F12 . . 1.240(12) ? B F13 . . 1.283(15) ? B F14 . . 1.326(16) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 Ru1 C12 . . . 90.2(3) ? C11 Ru1 C101 . . . 119.2(3) ? C11 Ru1 C102 . . . 155.2(3) ? C11 Ru1 C103 . . . 140.5(3) ? C11 Ru1 C104 . . . 106.1(3) ? C11 Ru1 C105 . . . 96.1(3) ? C11 Ru1 C1 . . . 87.7(3) ? C12 Ru1 C101 . . . 96.7(3) ? C12 Ru1 C102 . . . 98.0(3) ? C12 Ru1 C103 . . . 129.2(2) ? C12 Ru1 C104 . . . 157.3(3) ? C12 Ru1 C105 . . . 126.7(3) ? C12 Ru1 C1 . . . 95.6(2) ? C101 Ru1 C102 . . . 36.8(3) ? C101 Ru1 C103 . . . 61.1(3) ? C101 Ru1 C104 . . . 61.7(3) ? C101 Ru1 C105 . . . 36.0(3) ? C101 Ru1 C1 . . . 150.2(2) ? C102 Ru1 C103 . . . 36.4(3) ? C102 Ru1 C104 . . . 60.8(3) ? C102 Ru1 C105 . . . 60.4(2) ? C102 Ru1 C1 . . . 114.5(3) ? C103 Ru1 C104 . . . 36.0(2) ? C103 Ru1 C105 . . . 60.6(2) ? C103 Ru1 C1 . . . 90.3(2) ? C104 Ru1 C105 . . . 37.5(3) ? C104 Ru1 C1 . . . 100.7(3) ? C105 Ru1 C1 . . . 137.4(3) ? C21 Ru2 C22 . . . 90.3(3) ? C21 Ru2 C201 . . . 117.3(4) ? C21 Ru2 C202 . . . 151.3(4) ? C21 Ru2 C203 . . . 147.4(4) ? C21 Ru2 C204 . . . 111.4(4) ? C21 Ru2 C205 . . . 96.1(3) ? C21 Ru2 C1 . . . 82.7(2) ? C21 Ru2 C2 . . . 98.8(2) ? C22 Ru2 C201 . . . 151.2(4) ? C22 Ru2 C202 . . . 118.0(4) ? C22 Ru2 C203 . . . 94.4(4) ? C22 Ru2 C204 . . . 102.3(5) ? C22 Ru2 C205 . . . 137.5(5) ? C22 Ru2 C1 . . . 105.8(3) ? C22 Ru2 C2 . . . 80.5(3) ? C201 Ru2 C202 . . . 34.0(5) ? C201 Ru2 C203 . . . 58.1(5) ? C201 Ru2 C204 . . . 61.4(4) ? C201 Ru2 C205 . . . 38.1(5) ? C201 Ru2 C1 . . . 87.1(3) ? C201 Ru2 C2 . . . 102.0(3) ? C202 Ru2 C203 . . . 35.0(5) ? C202 Ru2 C204 . . . 60.4(4) ? C202 Ru2 C205 . . . 60.3(4) ? C202 Ru2 C1 . . . 93.4(3) ? C202 Ru2 C2 . . . 91.3(3) ? C203 Ru2 C204 . . . 36.1(5) ? C203 Ru2 C205 . . . 59.7(4) ? C203 Ru2 C1 . . . 126.5(4) ? C203 Ru2 C2 . . . 113.9(4) ? C204 Ru2 C205 . . . 36.8(6) ? C204 Ru2 C1 . . . 148.6(3) ? C204 Ru2 C2 . . . 149.6(3) ? C205 Ru2 C1 . . . 116.7(5) ? C205 Ru2 C2 . . . 139.0(5) ? C1 Ru2 C2 . . . 30.1(2) ? C31 Ru3 C32 . . . 91.3(3) ? C31 Ru3 C301 . . . 117.4(4) ? C31 Ru3 C302 . . . 153.6(4) ? C31 Ru3 C303 . . . 138.6(4) ? C31 Ru3 C304 . . . 103.1(4) ? C31 Ru3 C305 . . . 94.3(3) ? C31 Ru3 C2 . . . 86.3(3) ? C32 Ru3 C301 . . . 101.5(4) ? C32 Ru3 C302 . . . 101.0(4) ? C32 Ru3 C303 . . . 130.2(4) ? C32 Ru3 C304 . . . 160.4(4) ? C32 Ru3 C305 . . . 131.4(4) ? C32 Ru3 C2 . . . 92.6(3) ? C301 Ru3 C302 . . . 37.4(4) ? C301 Ru3 C303 . . . 60.8(4) ? C301 Ru3 C304 . . . 60.2(4) ? C301 Ru3 C305 . . . 35.3(4) ? C301 Ru3 C2 . . . 151.7(3) ? C302 Ru3 C303 . . . 35.6(4) ? C302 Ru3 C304 . . . 60.6(4) ? C302 Ru3 C305 . . . 60.1(3) ? C302 Ru3 C2 . . . 116.0(3) ? C303 Ru3 C304 . . . 37.1(4) ? C303 Ru3 C305 . . . 60.0(3) ? C303 Ru3 C2 . . . 91.4(3) ? C304 Ru3 C305 . . . 35.5(3) ? C304 Ru3 C2 . . . 101.4(3) ? C305 Ru3 C2 . . . 135.9(3) ? Ru1 C11 O11 . . . 178.4(7) ? Ru1 C12 O12 . . . 176.0(5) ? Ru1 C101 C102 . . . 72.3(4) ? Ru1 C101 C105 . . . 71.3(4) ? Ru1 C101 H101 . . . 122.6 ? C102 C101 C105 . . . 107.4(8) ? C102 C101 H101 . . . 126.7 ? C105 C101 H101 . . . 126.0 ? Ru1 C102 C101 . . . 70.9(4) ? Ru1 C102 C103 . . . 72.0(4) ? Ru1 C102 H102 . . . 124.2 ? C101 C102 C103 . . . 107.9(6) ? C101 C102 H102 . . . 125.0 ? C103 C102 H102 . . . 127.0 ? Ru1 C103 C102 . . . 71.6(3) ? Ru1 C103 C104 . . . 71.3(3) ? Ru1 C103 H103 . . . 122.3 ? C102 C103 C104 . . . 109.0(7) ? C102 C103 H103 . . . 125.8 ? C104 C103 H103 . . . 125.3 ? Ru1 C104 C103 . . . 72.7(4) ? Ru1 C104 C105 . . . 70.3(4) ? Ru1 C104 H104 . . . 121.0 ? C103 C104 C105 . . . 106.3(7) ? C103 C104 H104 . . . 127.6 ? C105 C104 H104 . . . 126.1 ? Ru1 C105 C101 . . . 72.8(4) ? Ru1 C105 C104 . . . 72.2(4) ? Ru1 C105 H105 . . . 121.3 ? C101 C105 C104 . . . 109.5(6) ? C101 C105 H105 . . . 126.6 ? C104 C105 H105 . . . 123.9 ? Ru2 C21 O21 . . . 175.6(6) ? Ru2 C22 O22 . . . 176.4(7) ? Ru2 C201 C202 . . . 73.4(6) ? Ru2 C201 C205 . . . 70.7(6) ? Ru2 C201 H201 . . . 121.8 ? C202 C201 C205 . . . 108.4(12) ? C202 C201 H201 . . . 127.8 ? C205 C201 H201 . . . 123.8 ? Ru2 C202 C201 . . . 72.6(5) ? Ru2 C202 C203 . . . 71.9(5) ? Ru2 C202 H202 . . . 122.1 ? C201 C202 C203 . . . 109.4(10) ? C201 C202 H202 . . . 124.3 ? C203 C202 H202 . . . 126.3 ? Ru2 C203 C202 . . . 73.1(6) ? Ru2 C203 C204 . . . 71.1(6) ? Ru2 C203 H203 . . . 122.5 ? C202 C203 C204 . . . 110.8(12) ? C202 C203 H203 . . . 125.2 ? C204 C203 H203 . . . 124.0 ? Ru2 C204 C203 . . . 72.7(6) ? Ru2 C204 C205 . . . 72.3(6) ? Ru2 C204 H204 . . . 120.3 ? C203 C204 C205 . . . 106.1(11) ? C203 C204 H204 . . . 131.5 ? C205 C204 H204 . . . 122.5 ? Ru2 C205 C201 . . . 71.2(6) ? Ru2 C205 C204 . . . 70.9(6) ? Ru2 C205 H205 . . . 122.0 ? C201 C205 C204 . . . 105.2(11) ? C201 C205 H205 . . . 122.4 ? C204 C205 H205 . . . 132.4 ? Ru3 C31 O31 . . . 177.2(6) ? Ru3 C32 O32 . . . 179.7(8) ? Ru3 C301 C302 . . . 72.0(6) ? Ru3 C301 C305 . . . 72.8(6) ? Ru3 C301 H301 . . . 120.4 ? C302 C301 C305 . . . 107.0(9) ? C302 C301 H301 . . . 124.6 ? C305 C301 H301 . . . 128.3 ? Ru3 C302 C301 . . . 70.6(6) ? Ru3 C302 C303 . . . 72.1(6) ? Ru3 C302 H302 . . . 121.9 ? C301 C302 C303 . . . 107.4(10) ? C301 C302 H302 . . . 126.4 ? C303 C302 H302 . . . 126.2 ? Ru3 C303 C302 . . . 72.2(5) ? Ru3 C303 C304 . . . 70.9(5) ? Ru3 C303 H303 . . . 124.4 ? C302 C303 C304 . . . 107.8(9) ? C302 C303 H303 . . . 124.0 ? C304 C303 H303 . . . 128.2 ? Ru3 C304 C303 . . . 72.1(5) ? Ru3 C304 C305 . . . 72.6(4) ? Ru3 C304 H304 . . . 120.1 ? C303 C304 C305 . . . 107.2(10) ? C303 C304 H304 . . . 124.5 ? C305 C304 H304 . . . 128.3 ? Ru3 C305 C301 . . . 71.9(6) ? Ru3 C305 C304 . . . 71.9(5) ? Ru3 C305 H305 . . . 122.0 ? C301 C305 C304 . . . 110.6(9) ? C301 C305 H305 . . . 123.9 ? C304 C305 H305 . . . 125.5 ? Ru1 C1 Ru2 . . . 129.5(3) ? Ru1 C1 C2 . . . 152.5(5) ? Ru2 C1 C2 . . . 77.9(4) ? Ru2 C2 Ru3 . . . 132.7(3) ? Ru2 C2 C1 . . . 72.1(4) ? Ru3 C2 C1 . . . 155.2(5) ? F11 B F12 . . . 115.6(11) ? F11 B F13 . . . 106.0(9) ? F11 B F14 . . . 108.7(11) ? F12 B F13 . . . 118.1(14) ? F12 B F14 . . . 103.0(11) ? F13 B F14 . . . 104.6(11) ? 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 ? ? ? ? ? ? ? ? ? ? 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 ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 748 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 7 5 4 -7 -5 -5 13 0 0 -13 0 0 0 9 0 0 -9 0 0 0 11 0 0 -11 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min -18 _reflns_limit_h_max 17 _reflns_limit_k_min -13 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _reflns_number_observed 5065 _reflns_d_resolution_high .756 _reflns_d_resolution_low 13.167 _diffrn_reflns_av_sigmaI/netI 0 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_reduction_process equatorial_monochr_Lp _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .075 _refine_ls_wR_factor_all .071 _refine_ls_goodness_of_fit_all 1.818 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end