#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/24/2012444.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2012444 loop_ _publ_author_name 'Bruno, Giuseppe' 'Nicol\'o, Francesco' 'Tresoldi, Giuseppe' 'Lanza, Santo' _publ_section_title ; trans-Diacetonitrilebis(di-2-pyridyl sulfide-N,N')ruthenium(II) bis(tetrafluoroborate) monohydrate ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m56 _journal_page_last m58 _journal_paper_doi 10.1107/S0108270101018091 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Ru(C2H3N)2(C10 H8 N2 S)2].2(BF4).H2O' _chemical_formula_moiety 'C24 H22 N6 Ru S2 2+, 2(B F4 1-), H2 O' _chemical_formula_sum 'C24 H24 B2 F8 N6 O Ru S2' _chemical_formula_weight 751.30 _chemical_name_systematic ; trans-bis(acetonitrile)-bis(di-2-pyridylsulfide-N,N')-ruthenium(ii) bis(tetrafluoroborate) monohydrate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 77.016(7) _cell_angle_beta 75.004(6) _cell_angle_gamma 68.225(6) _cell_formula_units_Z 2 _cell_length_a 10.0709(7) _cell_length_b 12.6595(8) _cell_length_c 13.5470(10) _cell_measurement_reflns_used 37 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 16.02 _cell_measurement_theta_min 8.17 _cell_volume 1533.3(2) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Bruker,1999)' _computing_data_reduction XSCANS _computing_molecular_graphics 'XPW (SHELXTL; Siemens, 1996)' _computing_publication_material 'PARST97 (Nardelli, 1995) and SHELXL97' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS90 (Sheldrick, 1990)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full .983 _diffrn_measured_fraction_theta_max .983 _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0299 _diffrn_reflns_av_sigmaI/netI .0219 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 7496 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 1.57 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 197 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .727 _exptl_absorpt_correction_T_max .8259 _exptl_absorpt_correction_T_min .6889 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; by seven indexed faces (XPREPW in SHELXTL; Siemens, 1996) ; _exptl_crystal_colour pale_yellow _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prysmatic _exptl_crystal_F_000 752 _exptl_crystal_size_max .36 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .25 _refine_diff_density_max .525 _refine_diff_density_min -.392 _refine_ls_extinction_coef .0028(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 440 _refine_ls_number_reflns 5922 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all .0443 _refine_ls_R_factor_gt .0316 _refine_ls_shift/su_max .051 _refine_ls_shift/su_mean .004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.9658P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .0772 _refine_ls_wR_factor_ref .0852 _reflns_number_gt 4761 _reflns_number_total 5922 _reflns_threshold_expression >2\s(I) _cod_data_source_file na1542.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'none' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_sg_symbol_H-M P-1 _cod_database_code 2012444 _cod_database_fobs_code 2012444 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Ru1 .5000 .5000 .0000 .03497(10) Uani d S 1 . . Ru N1 .5978(3) .3215(2) .02163(17) .0426(5) Uani d . 1 . . N C1 .5364(4) .2561(3) -.0051(2) .0516(7) Uani d . 1 . . C H1 .4501 .2926 -.0299 .062 Uiso calc R 1 . . H C2 .5949(5) .1389(3) .0026(3) .0697(10) Uani d . 1 . . C H2 .5488 .0969 -.0158 .084 Uiso calc R 1 . . H C3 .7239(6) .0842(3) .0382(3) .0857(13) Uani d . 1 . . C H3 .7676 .0049 .0421 .103 Uiso calc R 1 . . H C4 .7862(5) .1480(3) .0676(3) .0745(11) Uani d . 1 . . C H4 .8726 .1124 .0923 .089 Uiso calc R 1 . . H C5 .7203(3) .2664(3) .0604(2) .0519(7) Uani d . 1 . . C S1 .80545(9) .34311(8) .10157(7) .0585(2) Uani d . 1 . . S C6 .6585(3) .4328(3) .1807(2) .0484(7) Uani d . 1 . . C C7 .6782(4) .4332(3) .2783(3) .0649(9) Uani d . 1 . . C H7 .7629 .3841 .3011 .078 Uiso calc R 1 . . H C8 .5719(5) .5065(4) .3405(3) .0741(11) Uani d . 1 . . C H8 .5844 .5096 .4054 .089 Uiso calc R 1 . . H C9 .4464(4) .5756(3) .3060(2) .0643(9) Uani d . 1 . . C H9 .3721 .6254 .3475 .077 Uiso calc R 1 . . H C10 .4319(4) .5702(3) .2092(2) .0504(7) Uani d . 1 . . C H10 .3456 .6162 .1872 .060 Uiso calc R 1 . . H N2 .5367(3) .5013(2) .14480(17) .0421(5) Uani d . 1 . . N N3 .6882(3) .5266(2) -.07705(17) .0415(5) Uani d . 1 . . N C11 .7904(3) .5444(3) -.1224(2) .0483(7) Uani d . 1 . . C C12 .9247(4) .5660(4) -.1778(3) .0775(11) Uani d . 1 . . C H12A 1.0048 .4950 -.1768 .116 Uiso calc R 1 . . H H12B .9415 .6186 -.1452 .116 Uiso calc R 1 . . H H12C .9162 .5987 -.2480 .116 Uiso calc R 1 . . H Ru2 .5000 .0000 .5000 .03769(10) Uani d S 1 . . Ru N4 .3750(2) .17193(19) .51251(19) .0443(5) Uani d . 1 . . N C13 .3093(3) .2031(3) .6071(3) .0534(7) Uani d . 1 . . C H13 .3202 .1464 .6644 .064 Uiso calc R 1 . . H C14 .2278(4) .3138(3) .6228(3) .0679(9) Uani d . 1 . . C H14 .1876 .3315 .6895 .081 Uiso calc R 1 . . H C15 .2058(4) .3979(3) .5401(4) .0739(11) Uani d . 1 . . C H15 .1504 .4735 .5493 .089 Uiso calc R 1 . . H C16 .2673(4) .3687(3) .4426(3) .0638(9) Uani d . 1 . . C H16 .2525 .4243 .3849 .077 Uiso calc R 1 . . H C17 .3515(3) .2558(3) .4313(2) .0494(7) Uani d . 1 . . C S2 .43334(10) .22457(7) .30422(6) .0581(2) Uani d . 1 . . S C18 .3829(3) .1060(3) .3008(2) .0467(7) Uani d . 1 . . C C19 .3218(3) .1116(3) .2182(2) .0565(8) Uani d . 1 . . C H19 .3059 .1769 .1688 .068 Uiso calc R 1 . . H C20 .2852(4) .0209(3) .2099(3) .0624(9) Uani d . 1 . . C H20 .2468 .0227 .1538 .075 Uiso calc R 1 . . H C21 .3057(3) -.0731(3) .2857(3) .0591(8) Uani d . 1 . . C H21 .2797 -.1353 .2825 .071 Uiso calc R 1 . . H C22 .3655(3) -.0734(3) .3665(2) .0496(7) Uani d . 1 . . C H22 .3774 -.1365 .4182 .060 Uiso calc R 1 . . H N5 .4077(2) .0133(2) .37408(17) .0432(5) Uani d . 1 . . N N6 .6772(3) .0372(2) .41339(18) .0444(5) Uani d . 1 . . N C23 .7854(3) .0495(3) .3741(2) .0500(7) Uani d . 1 . . C C24 .9247(4) .0654(4) .3237(3) .0745(11) Uani d . 1 . . C H24A .9084 .1344 .2746 .112 Uiso calc R 1 . . H H24B .9858 .0009 .2887 .112 Uiso calc R 1 . . H H24C .9715 .0715 .3745 .112 Uiso calc R 1 . . H B1 .0766(5) .7393(4) .5048(3) .0661(11) Uani d . 1 . . B F1 -.0135(5) .8416(3) .4887(4) .197(2) Uani d . 1 . . F F2 .0894(4) .6796(3) .4248(2) .1297(11) Uani d . 1 . . F F3 .2127(3) .7381(3) .5038(2) .1249(11) Uani d . 1 . . F F4 .0336(3) .6803(3) .5939(2) .1212(10) Uani d . 1 . . F B2 .1943(6) .2454(4) .9234(4) .0747(12) Uani d . 1 . . B F5 .3217(14) .1845(13) .8897(15) .202(7) Uani d P .55(2) A 1 F F6 .2077(16) .3463(8) .8939(13) .179(6) Uani d P .55(2) A 1 F F7 .1507(17) .2074(14) 1.0198(9) .205(8) Uani d P .55(2) A 1 F F8 .1033(18) .2267(18) .8888(11) .166(5) Uani d P .55(2) A 1 F F5A .3007(18) .1719(10) .8596(9) .120(5) Uani d P .45(2) A 2 F F7A .208(3) .1899(12) 1.0168(12) .165(8) Uani d P .45(2) A 2 F F6A .1953(13) .3471(12) .9400(18) .174(8) Uani d P .45(2) A 2 F F8A .0579(13) .2803(10) .8852(8) .088(3) Uani d P .45(2) A 2 F O .9078(5) .2009(5) .7862(3) .163(2) Uani d . 1 . . O H0A .9179 .2317 .7215 .080 Uiso d . 1 . . H H0B .9564 .2240 .8135 .080 Uiso d . 1 . . H 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 .03699(17) .04050(18) .03119(16) -.01942(13) -.00549(12) -.00249(12) N1 .0471(13) .0449(13) .0358(12) -.0205(11) -.0031(10) -.0028(10) C1 .0625(19) .0530(18) .0444(16) -.0317(15) .0029(14) -.0107(13) C2 .093(3) .056(2) .063(2) -.038(2) .007(2) -.0178(17) C3 .118(4) .046(2) .078(3) -.012(2) -.013(3) -.0128(19) C4 .087(3) .054(2) .066(2) .0001(19) -.022(2) -.0096(17) C5 .0556(18) .0513(17) .0416(16) -.0131(14) -.0074(13) -.0031(13) S1 .0474(4) .0689(5) .0579(5) -.0153(4) -.0194(4) -.0030(4) C6 .0551(18) .0586(18) .0404(15) -.0302(15) -.0152(13) .0020(13) C7 .074(2) .086(3) .0491(19) -.041(2) -.0248(17) .0007(18) C8 .095(3) .109(3) .0407(18) -.057(3) -.0163(19) -.0110(19) C9 .082(2) .082(2) .0418(17) -.045(2) .0027(17) -.0197(16) C10 .0575(18) .0567(18) .0418(16) -.0283(15) -.0029(13) -.0081(13) N2 .0474(13) .0508(13) .0354(12) -.0269(11) -.0068(10) -.0035(10) N3 .0429(13) .0481(13) .0373(12) -.0215(11) -.0076(10) -.0028(10) C11 .0430(16) .0508(17) .0498(17) -.0196(14) -.0076(14) .0009(13) C12 .0457(19) .087(3) .089(3) -.0318(19) .0035(18) .006(2) Ru2 .03723(17) .03944(18) .03546(17) -.01596(13) -.01024(13) .00574(12) N4 .0431(13) .0423(13) .0479(14) -.0170(10) -.0128(11) .0020(10) C13 .0521(18) .0529(18) .0535(18) -.0164(14) -.0110(14) -.0056(14) C14 .066(2) .063(2) .076(2) -.0145(17) -.0143(19) -.0222(19) C15 .075(2) .0477(19) .103(3) -.0145(17) -.028(2) -.017(2) C16 .072(2) .0428(17) .084(3) -.0246(16) -.034(2) .0086(17) C17 .0482(16) .0452(16) .0589(18) -.0223(13) -.0204(14) .0079(13) S2 .0660(5) .0575(5) .0493(4) -.0301(4) -.0166(4) .0184(4) C18 .0401(15) .0548(17) .0377(14) -.0133(13) -.0072(12) .0035(12) C19 .0505(18) .070(2) .0380(16) -.0109(16) -.0113(13) -.0001(14) C20 .0544(19) .083(2) .0460(18) -.0114(18) -.0148(15) -.0162(17) C21 .0520(18) .070(2) .062(2) -.0203(16) -.0140(16) -.0189(17) C22 .0474(16) .0520(17) .0515(17) -.0197(14) -.0126(13) -.0026(13) N5 .0401(12) .0495(13) .0389(12) -.0172(10) -.0104(10) .0027(10) N6 .0411(13) .0467(13) .0430(13) -.0170(11) -.0085(11) .0032(10) C23 .0447(17) .0520(17) .0493(17) -.0175(14) -.0123(14) .0067(13) C24 .0491(19) .092(3) .075(2) -.0329(19) -.0046(17) .012(2) B1 .075(3) .065(3) .062(3) -.030(2) -.026(2) .012(2) F1 .228(5) .083(2) .251(5) .019(2) -.137(4) .016(3) F2 .139(3) .183(3) .094(2) -.073(2) -.0276(19) -.034(2) F3 .114(2) .187(3) .103(2) -.093(2) -.0193(18) -.006(2) F4 .132(2) .152(3) .0819(18) -.080(2) -.0105(17) .0233(18) B2 .089(3) .075(3) .068(3) -.026(3) -.036(3) -.004(2) F5 .097(6) .235(12) .312(18) -.032(6) -.003(8) -.195(13) F6 .266(13) .079(6) .229(12) -.088(7) -.133(9) .062(7) F7 .196(10) .192(11) .074(6) .074(8) -.008(6) .020(5) F8 .153(10) .199(14) .198(9) -.073(9) -.117(8) -.005(9) F5A .164(11) .093(6) .084(6) -.034(5) .002(5) -.021(5) F7A .31(2) .106(7) .115(10) -.059(11) -.158(13) .033(6) F6A .104(7) .126(9) .35(2) -.005(6) -.104(9) -.132(13) F8A .081(5) .115(7) .079(5) -.027(4) -.035(4) -.020(4) O .172(4) .290(6) .095(3) -.152(4) -.033(3) -.020(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 .8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N3 Ru1 N3 . 2_665 180.0000(10) ? N3 Ru1 N1 . 2_665 86.79(9) ? N3 Ru1 N1 . . 93.21(9) yes N1 Ru1 N1 2_665 . 180.00(13) ? N3 Ru1 N2 . 2_665 86.25(9) ? N1 Ru1 N2 . 2_665 91.71(9) ? N3 Ru1 N2 . . 93.75(9) yes N1 Ru1 N2 . . 88.29(9) yes N2 Ru1 N2 2_665 . 180.0 ? C5 N1 C1 . . 117.2(3) ? C5 N1 Ru1 . . 124.0(2) ? C1 N1 Ru1 . . 118.8(2) ? N1 C1 C2 . . 123.2(3) ? N1 C1 H1 . . 118.4 ? C2 C1 H1 . . 118.4 ? C1 C2 C3 . . 118.7(4) ? C1 C2 H2 . . 120.6 ? C3 C2 H2 . . 120.6 ? C4 C3 C2 . . 119.1(4) ? C4 C3 H3 . . 120.5 ? C2 C3 H3 . . 120.5 ? C3 C4 C5 . . 119.7(4) ? C3 C4 H4 . . 120.1 ? C5 C4 H4 . . 120.1 ? N1 C5 C4 . . 121.9(3) ? N1 C5 S1 . . 120.8(2) yes C4 C5 S1 . . 117.3(3) ? C5 S1 C6 . . 102.30(10) yes N2 C6 C7 . . 122.5(3) ? N2 C6 S1 . . 120.7(2) yes C7 C6 S1 . . 116.6(3) ? C8 C7 C6 . . 119.2(3) ? C8 C7 H7 . . 120.4 ? C6 C7 H7 . . 120.4 ? C7 C8 C9 . . 119.0(3) ? C7 C8 H8 . . 120.5 ? C9 C8 H8 . . 120.5 ? C8 C9 C10 . . 119.1(3) ? C8 C9 H9 . . 120.4 ? C10 C9 H9 . . 120.4 ? N2 C10 C9 . . 123.2(3) ? N2 C10 H10 . . 118.4 ? C9 C10 H10 . . 118.4 ? C10 N2 C6 . . 116.8(2) ? C10 N2 Ru1 . . 119.4(2) ? C6 N2 Ru1 . . 123.8(2) ? C11 N3 Ru1 . . 177.5(2) yes N3 C11 C12 . . 178.0(3) yes C11 C12 H12A . . 109.5 ? C11 C12 H12B . . 109.5 ? H12A C12 H12B . . 109.5 ? C11 C12 H12C . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? N6 Ru2 N6 2_656 . 180.0 ? N6 Ru2 N4 2_656 . 85.99(9) ? N6 Ru2 N4 . . 94.01(9) yes N6 Ru2 N4 . 2_656 85.99(9) ? N4 Ru2 N4 . 2_656 180.00(14) ? N6 Ru2 N5 . 2_656 85.12(9) ? N6 Ru2 N5 . . 94.88(9) yes N4 Ru2 N5 . . 88.61(9) yes N4 Ru2 N5 2_656 . 91.39(9) ? N5 Ru2 N5 2_656 . 180.0000(10) ? C17 N4 C13 . . 116.5(3) ? C17 N4 Ru2 . . 124.2(2) ? C13 N4 Ru2 . . 119.30(19) ? N4 C13 C14 . . 123.3(3) ? N4 C13 H13 . . 118.3 ? C14 C13 H13 . . 118.3 ? C15 C14 C13 . . 119.6(4) ? C15 C14 H14 . . 120.2 ? C13 C14 H14 . . 120.2 ? C14 C15 C16 . . 118.7(3) ? C14 C15 H15 . . 120.7 ? C16 C15 H15 . . 120.7 ? C15 C16 C17 . . 119.4(3) ? C15 C16 H16 . . 120.3 ? C17 C16 H16 . . 120.3 ? N4 C17 C16 . . 122.6(3) ? N4 C17 S2 . . 120.1(2) yes C16 C17 S2 . . 117.3(3) ? C18 S2 C17 . . 102.40(10) yes N5 C18 C19 . . 122.2(3) ? N5 C18 S2 . . 120.7(2) yes C19 C18 S2 . . 117.1(2) ? C20 C19 C18 . . 119.6(3) ? C20 C19 H19 . . 120.2 ? C18 C19 H19 . . 120.2 ? C19 C20 C21 . . 119.1(3) ? C19 C20 H20 . . 120.5 ? C21 C20 H20 . . 120.5 ? C20 C21 C22 . . 118.7(3) ? C20 C21 H21 . . 120.7 ? C22 C21 H21 . . 120.7 ? N5 C22 C21 . . 123.2(3) ? N5 C22 H22 . . 118.4 ? C21 C22 H22 . . 118.4 ? C18 N5 C22 . . 117.2(3) ? C18 N5 Ru2 . . 123.7(2) ? C22 N5 Ru2 . . 119.00(19) ? C23 N6 Ru2 . . 171.5(2) yes N6 C23 C24 . . 179.9(4) yes C23 C24 H24A . . 109.5 ? C23 C24 H24B . . 109.5 ? H24A C24 H24B . . 109.5 ? C23 C24 H24C . . 109.5 ? H24A C24 H24C . . 109.5 ? H24B C24 H24C . . 109.5 ? F1 B1 F4 . . 112.9(5) ? F1 B1 F3 . . 112.6(4) ? F4 B1 F3 . . 107.7(3) ? F1 B1 F2 . . 108.5(4) ? F4 B1 F2 . . 107.9(4) ? F3 B1 F2 . . 107.0(4) ? F8 B2 F5 . . 111.4(9) ? F8 B2 F6 . . 116.5(9) ? F5 B2 F6 . . 99.6(11) ? F8 B2 F7 . . 96.0(12) ? F5 B2 F7 . . 110.9(10) ? F6 B2 F7 . . 122.9(12) ? F7A B2 F6A . . 96.8(11) ? F7A B2 F5A . . 103.5(10) ? F6A B2 F5A . . 126.3(12) ? F7A B2 F8A . . 122.5(12) ? F6A B2 F8A . . 102.3(7) ? F5A B2 F8A . . 107.2(8) ? H0A O H0B . . 106.3 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 N3 . 2.022(2) yes Ru1 N1 . 2.088(2) yes Ru1 N2 . 2.092(2) yes N1 C5 . 1.348(4) ? N1 C1 . 1.353(4) ? C1 C2 . 1.369(5) ? C1 H1 . .9300 ? C2 C3 . 1.380(6) ? C2 H2 . .9300 ? C3 C4 . 1.361(6) ? C3 H3 . .9300 ? C4 C5 . 1.387(5) ? C4 H4 . .9300 ? C5 S1 . 1.761(3) yes S1 C6 . 1.763(3) yes C6 N2 . 1.351(4) ? C6 C7 . 1.389(4) ? C7 C8 . 1.365(5) ? C7 H7 . .9300 ? C8 C9 . 1.373(5) ? C8 H8 . .9300 ? C9 C10 . 1.375(4) ? C9 H9 . .9300 ? C10 N2 . 1.348(4) ? C10 H10 . .9300 ? N3 C11 . 1.127(4) yes C11 C12 . 1.457(4) yes C12 H12A . .9600 ? C12 H12B . .9600 ? C12 H12C . .9600 ? Ru2 N6 . 2.018(2) yes Ru2 N4 . 2.091(2) yes Ru2 N5 . 2.093(2) yes N4 C17 . 1.348(4) ? N4 C13 . 1.353(4) ? C13 C14 . 1.369(4) ? C13 H13 . .9300 ? C14 C15 . 1.363(5) ? C14 H14 . .9300 ? C15 C16 . 1.374(5) ? C15 H15 . .9300 ? C16 C17 . 1.385(5) ? C16 H16 . .9300 ? C17 S2 . 1.768(3) yes S2 C18 . 1.767(3) yes C18 N5 . 1.346(3) ? C18 C19 . 1.387(4) ? C19 C20 . 1.364(5) ? C19 H19 . .9300 ? C20 C21 . 1.376(5) ? C20 H20 . .9300 ? C21 C22 . 1.378(4) ? C21 H21 . .9300 ? C22 N5 . 1.347(4) ? C22 H22 . .9300 ? N6 C23 . 1.133(4) yes C23 C24 . 1.458(4) yes C24 H24A . .9600 ? C24 H24B . .9600 ? C24 H24C . .9600 ? B1 F1 . 1.285(5) ? B1 F4 . 1.329(5) ? B1 F3 . 1.362(5) ? B1 F2 . 1.410(5) ? B2 F8 . 1.245(13) ? B2 F5 . 1.253(14) ? B2 F6 . 1.296(10) ? B2 F7 . 1.307(14) ? B2 F7A . 1.317(13) ? B2 F6A . 1.360(12) ? B2 F5A . 1.380(14) ? B2 F8A . 1.472(13) ? O H0A . .872 ? O H0B . .843 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _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 C19 H19 F7A 1_554 .93 2.45 3.050(10) 122 ? C20 H20 F7A 1_554 .93 2.46 3.050(10) 121 ? C12 H12C F4 1_654 .96 2.38 3.205(5) 144 yes C12 H12A F6 1_654 .96 2.45 3.340(10) 154 ? O H0A F2 2_666 .87 2.05 2.917(5) 171 yes O H0B F8 1_655 .84 2.02 2.830(10) 162 yes O H0B F8A 1_655 .84 1.96 2.810(10) 176 yes 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 _geom_torsion_publ_flag N3 Ru1 N1 C5 . 50.6(2) ? N3 Ru1 N1 C5 2_665 -129.4(2) ? N2 Ru1 N1 C5 2_665 137.0(2) ? N2 Ru1 N1 C5 . -43.0(2) ? N3 Ru1 N1 C1 . -128.9(2) ? N3 Ru1 N1 C1 2_665 51.1(2) ? N2 Ru1 N1 C1 2_665 -42.6(2) ? N2 Ru1 N1 C1 . 137.4(2) ? C5 N1 C1 C2 . -2.1(4) ? Ru1 N1 C1 C2 . 177.6(2) ? N1 C1 C2 C3 . -.7(5) ? C1 C2 C3 C4 . 2.0(6) ? C2 C3 C4 C5 . -.6(6) ? C1 N1 C5 C4 . 3.6(4) ? Ru1 N1 C5 C4 . -176.0(3) ? C1 N1 C5 S1 . -177.9(2) ? Ru1 N1 C5 S1 . 2.5(3) ? C3 C4 C5 N1 . -2.3(6) ? C3 C4 C5 S1 . 179.1(3) ? N1 C5 S1 C6 . 49.1(3) yes C4 C5 S1 C6 . -132.2(3) ? C5 S1 C6 N2 . -53.4(3) yes C5 S1 C6 C7 . 129.7(3) ? N2 C6 C7 C8 . -1.0(5) ? S1 C6 C7 C8 . 175.8(3) ? C6 C7 C8 C9 . 1.9(6) ? C7 C8 C9 C10 . -.8(5) ? C8 C9 C10 N2 . -1.2(5) ? C9 C10 N2 C6 . 2.1(4) ? C9 C10 N2 Ru1 . 179.4(2) ? C7 C6 N2 C10 . -1.0(4) ? S1 C6 N2 C10 . -177.7(2) ? C7 C6 N2 Ru1 . -178.2(2) ? S1 C6 N2 Ru1 . 5.2(3) ? N3 Ru1 N2 C10 . 128.5(2) ? N3 Ru1 N2 C10 2_665 -51.5(2) ? N1 Ru1 N2 C10 2_665 41.6(2) ? N1 Ru1 N2 C10 . -138.4(2) ? N3 Ru1 N2 C6 . -54.5(2) ? N3 Ru1 N2 C6 2_665 125.5(2) ? N1 Ru1 N2 C6 2_665 -141.4(2) ? N1 Ru1 N2 C6 . 38.6(2) ? N6 Ru2 N4 C17 2_656 -125.6(2) ? N6 Ru2 N4 C17 . 54.4(2) ? N5 Ru2 N4 C17 2_656 139.6(2) ? N5 Ru2 N4 C17 . -40.4(2) ? N6 Ru2 N4 C13 2_656 52.8(2) ? N6 Ru2 N4 C13 . -127.2(2) ? N5 Ru2 N4 C13 2_656 -42.0(2) ? N5 Ru2 N4 C13 . 138.0(2) ? C17 N4 C13 C14 . -2.7(5) ? Ru2 N4 C13 C14 . 178.8(3) ? N4 C13 C14 C15 . 2.3(5) ? C13 C14 C15 C16 . -.3(6) ? C14 C15 C16 C17 . -1.1(5) ? C13 N4 C17 C16 . 1.2(4) ? Ru2 N4 C17 C16 . 179.6(2) ? C13 N4 C17 S2 . 179.5(2) ? Ru2 N4 C17 S2 . -2.0(3) ? C15 C16 C17 N4 . .7(5) ? C15 C16 C17 S2 . -177.7(3) ? N4 C17 S2 C18 . 51.9(3) yes C16 C17 S2 C18 . -129.7(3) ? C17 S2 C18 N5 . -52.0(3) yes C17 S2 C18 C19 . 129.9(2) ? N5 C18 C19 C20 . -.1(5) ? S2 C18 C19 C20 . 177.9(2) ? C18 C19 C20 C21 . 2.0(5) ? C19 C20 C21 C22 . -1.3(5) ? C20 C21 C22 N5 . -1.3(5) ? C19 C18 N5 C22 . -2.4(4) ? S2 C18 N5 C22 . 179.7(2) ? C19 C18 N5 Ru2 . 179.8(2) ? S2 C18 N5 Ru2 . 1.9(3) ? C21 C22 N5 C18 . 3.1(4) ? C21 C22 N5 Ru2 . -179.0(2) ? N6 Ru2 N5 C18 2_656 126.5(2) ? N6 Ru2 N5 C18 . -53.5(2) ? N4 Ru2 N5 C18 . 40.4(2) ? N4 Ru2 N5 C18 2_656 -139.6(2) ? N6 Ru2 N5 C22 2_656 -51.3(2) ? N6 Ru2 N5 C22 . 128.7(2) ? N4 Ru2 N5 C22 . -137.4(2) ? N4 Ru2 N5 C22 2_656 42.6(2) ?