Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Yasuhiro Arikawa' _publ_contact_author_address ; Department of Applied Chemistry Faculty of Engineering Nagasaki University Nagasaki 852-8521 Japan ; _publ_contact_author_email arikawa@net.nagasaki-u.ac.jp _publ_contact_author_fax +81-95-819-2684 _publ_contact_author_phone +81-95-819-2673 _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_section_title ; Regioselective Nucleophilic Addition of Triphenylphosphine to the Nitrosylruthenium Alkynyl Complexes Having a Hydrotris(pyrazol-1-yl)borate: Formation of Phosphonio-Alkenyl, -Alkynyl, and -Allenyl Species ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; loop_ _publ_author_name 'Yasuhiro Arikawa' 'Takanori Inoue' 'Yoshimasa Nishimura' 'Masayoshi Onishi' #------------------------------------------------------------------------------ data_0416 _database_code_depnum_ccdc_archive 'CCDC 252270' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C35 H31 B2 Cl F4 N7 O P Ru ' _chemical_formula_moiety 'C35 H31 B Cl N7 O P Ru, B F4 ' _chemical_formula_weight 830.79 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _cell_length_a 19.641(2) _cell_length_b 10.1468(7) _cell_length_c 20.1828(4) _cell_angle_alpha 90 _cell_angle_beta 112.3862(5) _cell_angle_gamma 90 _cell_volume 3719.1(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.596 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.779 _exptl_absorpt_correction_T_max 0.942 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Quantum CCD/Rigaku AFC7' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32298 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9782 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9782 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8360 _reflns_number_gt 5847 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0714 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 8359 _refine_ls_number_parameters 469 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.02000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0014 _refine_diff_density_max 0.49 _refine_diff_density_min -0.47 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru Ru -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.48255(1) 0.16948(2) 0.124804(9) 0.03632(5) Uani 1.00 d . . . Cl Cl 0.37313(4) 0.28920(7) 0.10693(4) 0.0589(2) Uani 1.00 d . . . P P 0.45087(3) -0.00802(6) 0.32764(3) 0.0407(2) Uani 1.00 d . . . F(1) F 0.61555(9) -0.1936(2) 0.2948(1) 0.0849(6) Uani 1.00 d . . . F(2) F 0.7251(1) -0.0963(2) 0.3535(2) 0.138(1) Uani 1.00 d . . . F(3) F 0.6951(2) -0.2915(3) 0.3899(2) 0.168(1) Uani 1.00 d . . . F(4) F 0.7183(1) -0.2783(2) 0.2902(2) 0.151(1) Uani 1.00 d . . . O O 0.4146(1) -0.0491(2) 0.0334(1) 0.0768(7) Uani 1.00 d . . . N(1) N 0.4388(1) 0.0362(2) 0.0726(1) 0.0450(6) Uani 1.00 d . . . N(2) N 0.5854(1) 0.0885(2) 0.1449(1) 0.0444(6) Uani 1.00 d . . . N(3) N 0.6372(1) 0.1600(2) 0.1312(1) 0.0517(6) Uani 1.00 d . . . N(4) N 0.5416(1) 0.3293(2) 0.18223(10) 0.0437(5) Uani 1.00 d . . . N(5) N 0.6037(1) 0.3702(2) 0.1733(1) 0.0507(6) Uani 1.00 d . . . N(6) N 0.4939(1) 0.2698(2) 0.0353(1) 0.0479(6) Uani 1.00 d . . . N(7) N 0.5603(1) 0.3226(2) 0.0432(1) 0.0533(6) Uani 1.00 d . . . C(1) C 0.6123(2) -0.0328(2) 0.1634(1) 0.0577(8) Uani 1.00 d . . . C(2) C 0.6812(2) -0.0409(3) 0.1604(2) 0.074(1) Uani 1.00 d . . . C(3) C 0.6950(1) 0.0806(3) 0.1402(2) 0.0680(10) Uani 1.00 d . . . C(4) C 0.5343(2) 0.4053(2) 0.2334(1) 0.0545(8) Uani 1.00 d . . . C(5) C 0.5917(2) 0.4940(3) 0.2579(2) 0.0660(9) Uani 1.00 d . . . C(6) C 0.6339(2) 0.4691(3) 0.2190(2) 0.0660(9) Uani 1.00 d . . . C(7) C 0.4484(2) 0.2910(2) -0.0323(1) 0.0575(8) Uani 1.00 d . . . C(8) C 0.4852(2) 0.3565(3) -0.0689(2) 0.073(1) Uani 1.00 d . . . C(9) C 0.5548(2) 0.3754(3) -0.0198(2) 0.071(1) Uani 1.00 d . . . C(10) C 0.4822(1) 0.1011(2) 0.2202(1) 0.0390(6) Uani 1.00 d . . . C(11) C 0.4455(1) 0.0036(2) 0.2366(1) 0.0389(6) Uani 1.00 d . . . C(12) C 0.3930(1) -0.0900(2) 0.1853(1) 0.0448(7) Uani 1.00 d . . . C(13) C 0.4128(2) -0.2213(3) 0.1827(1) 0.0563(8) Uani 1.00 d . . . C(14) C 0.3632(2) -0.3072(3) 0.1349(2) 0.076(1) Uani 1.00 d . . . C(15) C 0.2951(2) -0.2629(4) 0.0889(2) 0.087(1) Uani 1.00 d . . . C(16) C 0.2755(2) -0.1337(4) 0.0918(2) 0.082(1) Uani 1.00 d . . . C(17) C 0.3235(1) -0.0479(3) 0.1401(2) 0.0604(8) Uani 1.00 d . . . C(18) C 0.4529(1) -0.1778(2) 0.3547(1) 0.0450(6) Uani 1.00 d . . . C(19) C 0.5185(2) -0.2411(3) 0.3926(2) 0.0675(10) Uani 1.00 d . . . C(20) C 0.5187(2) -0.3759(3) 0.4040(2) 0.092(1) Uani 1.00 d . . . C(21) C 0.4539(2) -0.4459(3) 0.3786(2) 0.085(1) Uani 1.00 d . . . C(22) C 0.3891(2) -0.3841(3) 0.3422(2) 0.070(1) Uani 1.00 d . . . C(23) C 0.3880(1) -0.2500(2) 0.3290(1) 0.0531(8) Uani 1.00 d . . . C(24) C 0.3710(1) 0.0703(2) 0.3323(1) 0.0456(7) Uani 1.00 d . . . C(25) C 0.3428(2) 0.0319(3) 0.3828(2) 0.0697(10) Uani 1.00 d . . . C(26) C 0.2871(2) 0.1041(4) 0.3911(2) 0.097(1) Uani 1.00 d . . . C(27) C 0.2619(2) 0.2154(4) 0.3517(2) 0.093(1) Uani 1.00 d . . . C(28) C 0.2897(2) 0.2557(3) 0.3024(2) 0.0728(10) Uani 1.00 d . . . C(29) C 0.3440(1) 0.1831(2) 0.2917(1) 0.0538(7) Uani 1.00 d . . . C(30) C 0.5290(1) 0.0809(2) 0.3882(1) 0.0492(7) Uani 1.00 d . . . C(31) C 0.5189(2) 0.1795(3) 0.4314(1) 0.0625(8) Uani 1.00 d . . . C(32) C 0.5786(2) 0.2484(3) 0.4767(2) 0.087(1) Uani 1.00 d . . . C(33) C 0.6477(2) 0.2184(4) 0.4816(2) 0.092(1) Uani 1.00 d . . . C(34) C 0.6593(2) 0.1196(4) 0.4400(2) 0.083(1) Uani 1.00 d . . . C(35) C 0.5992(2) 0.0520(3) 0.3917(2) 0.0634(9) Uani 1.00 d . . . B(1) B 0.6248(2) 0.3082(3) 0.1145(2) 0.0575(10) Uani 1.00 d . . . B(2) B 0.6899(2) -0.2143(5) 0.3329(3) 0.094(2) Uani 1.00 d . . . H(1) H 0.6756 0.3471 0.1132 0.0688 Uiso 1.00 calc . . . H(2) H 0.5873 -0.1041 0.1769 0.0693 Uiso 1.00 calc . . . H(3) H 0.7131 -0.1175 0.1706 0.0882 Uiso 1.00 calc . . . H(4) H 0.7394 0.1061 0.1333 0.0816 Uiso 1.00 calc . . . H(5) H 0.4946 0.3988 0.2507 0.0654 Uiso 1.00 calc . . . H(6) H 0.6002 0.5601 0.2949 0.0791 Uiso 1.00 calc . . . H(7) H 0.6786 0.5157 0.2237 0.0793 Uiso 1.00 calc . . . H(8) H 0.3971 0.2644 -0.0528 0.0690 Uiso 1.00 calc . . . H(9) H 0.4657 0.3834 -0.1188 0.0880 Uiso 1.00 calc . . . H(10) H 0.5942 0.4197 -0.0288 0.0848 Uiso 1.00 calc . . . H(11) H 0.5152 0.1489 0.2616 0.0468 Uiso 1.00 calc . . . H(12) H 0.4610 -0.2524 0.2142 0.0675 Uiso 1.00 calc . . . H(13) H 0.3764 -0.3991 0.1337 0.0909 Uiso 1.00 calc . . . H(14) H 0.2612 -0.3228 0.0547 0.1039 Uiso 1.00 calc . . . H(15) H 0.2276 -0.1027 0.0596 0.0987 Uiso 1.00 calc . . . H(16) H 0.3087 0.0425 0.1426 0.0725 Uiso 1.00 calc . . . H(17) H 0.5642 -0.1916 0.4111 0.0810 Uiso 1.00 calc . . . H(18) H 0.5647 -0.4210 0.4301 0.1101 Uiso 1.00 calc . . . H(19) H 0.4545 -0.5402 0.3867 0.1026 Uiso 1.00 calc . . . H(20) H 0.3435 -0.4338 0.3253 0.0838 Uiso 1.00 calc . . . H(21) H 0.3418 -0.2064 0.3017 0.0637 Uiso 1.00 calc . . . H(22) H 0.3622 -0.0456 0.4121 0.0836 Uiso 1.00 calc . . . H(23) H 0.2660 0.0757 0.4251 0.1168 Uiso 1.00 calc . . . H(24) H 0.2236 0.2669 0.3586 0.1119 Uiso 1.00 calc . . . H(25) H 0.2711 0.3354 0.2749 0.0874 Uiso 1.00 calc . . . H(26) H 0.3632 0.2105 0.2562 0.0645 Uiso 1.00 calc . . . H(27) H 0.4699 0.1995 0.4296 0.0751 Uiso 1.00 calc . . . H(28) H 0.5713 0.3192 0.5056 0.1044 Uiso 1.00 calc . . . H(29) H 0.6894 0.2669 0.5145 0.1100 Uiso 1.00 calc . . . H(30) H 0.7089 0.0974 0.4445 0.0998 Uiso 1.00 calc . . . H(31) H 0.6065 -0.0149 0.3606 0.0761 Uiso 1.00 calc . . . 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 Ru 0.0401(1) 0.03819(9) 0.03308(9) -0.00074(8) 0.01670(7) -0.00207(8) Cl 0.0504(4) 0.0644(4) 0.0639(4) 0.0150(3) 0.0242(3) 0.0049(3) P 0.0463(3) 0.0412(3) 0.0386(3) 0.0008(3) 0.0207(3) 0.0046(2) F(1) 0.058(1) 0.087(1) 0.100(1) 0.0019(9) 0.0197(10) 0.005(1) F(2) 0.083(2) 0.110(2) 0.224(3) -0.035(1) 0.061(2) -0.067(2) F(3) 0.106(2) 0.190(3) 0.146(2) -0.007(2) -0.023(2) 0.053(2) F(4) 0.084(2) 0.106(2) 0.280(4) -0.020(1) 0.089(2) -0.067(2) O 0.103(2) 0.073(1) 0.055(1) -0.028(1) 0.030(1) -0.027(1) N(1) 0.050(1) 0.050(1) 0.036(1) -0.0046(9) 0.0176(9) -0.0038(9) N(2) 0.043(1) 0.049(1) 0.043(1) 0.0003(9) 0.0177(9) -0.0062(9) N(3) 0.041(1) 0.064(1) 0.054(1) -0.005(1) 0.0225(10) -0.014(1) N(4) 0.053(1) 0.0421(10) 0.040(1) -0.0042(9) 0.0226(9) -0.0063(9) N(5) 0.054(1) 0.050(1) 0.053(1) -0.0128(9) 0.024(1) -0.0109(9) N(6) 0.062(1) 0.049(1) 0.037(1) -0.0004(10) 0.023(1) 0.0006(9) N(7) 0.072(1) 0.052(1) 0.050(1) -0.011(1) 0.040(1) -0.0049(10) C(1) 0.060(2) 0.050(1) 0.060(2) 0.009(1) 0.018(1) -0.008(1) C(2) 0.057(2) 0.075(2) 0.084(2) 0.020(2) 0.022(2) -0.019(2) C(3) 0.043(2) 0.092(2) 0.071(2) 0.003(1) 0.024(1) -0.031(2) C(4) 0.073(2) 0.049(1) 0.047(1) 0.001(1) 0.029(1) -0.010(1) C(5) 0.083(2) 0.058(2) 0.055(2) -0.009(1) 0.025(2) -0.021(1) C(6) 0.068(2) 0.058(2) 0.069(2) -0.020(1) 0.022(2) -0.019(1) C(7) 0.078(2) 0.056(1) 0.039(1) 0.012(1) 0.022(1) -0.001(1) C(8) 0.125(3) 0.062(2) 0.046(2) 0.015(2) 0.047(2) 0.009(1) C(9) 0.119(3) 0.053(1) 0.070(2) -0.007(2) 0.069(2) -0.003(1) C(10) 0.041(1) 0.044(1) 0.033(1) 0.0040(10) 0.016(1) 0.0009(9) C(11) 0.038(1) 0.045(1) 0.037(1) 0.0020(9) 0.0175(10) 0.0005(9) C(12) 0.048(1) 0.052(1) 0.042(1) -0.007(1) 0.026(1) -0.002(1) C(13) 0.072(2) 0.054(1) 0.057(2) -0.004(1) 0.039(2) -0.008(1) C(14) 0.113(3) 0.061(2) 0.080(2) -0.029(2) 0.067(2) -0.026(2) C(15) 0.086(3) 0.108(3) 0.078(2) -0.054(2) 0.046(2) -0.037(2) C(16) 0.054(2) 0.108(3) 0.080(2) -0.027(2) 0.020(2) -0.019(2) C(17) 0.046(2) 0.070(2) 0.065(2) -0.010(1) 0.021(1) -0.007(1) C(18) 0.048(1) 0.040(1) 0.052(1) 0.003(1) 0.024(1) 0.009(1) C(19) 0.058(2) 0.067(2) 0.083(2) 0.009(1) 0.033(2) 0.027(2) C(20) 0.085(3) 0.073(2) 0.129(3) 0.033(2) 0.054(2) 0.047(2) C(21) 0.111(3) 0.047(2) 0.121(3) 0.012(2) 0.069(3) 0.018(2) C(22) 0.091(2) 0.050(1) 0.082(2) -0.011(2) 0.047(2) -0.002(1) C(23) 0.061(2) 0.050(1) 0.055(2) -0.001(1) 0.029(1) 0.001(1) C(24) 0.052(1) 0.046(1) 0.045(1) 0.002(1) 0.025(1) -0.001(1) C(25) 0.091(2) 0.067(2) 0.077(2) 0.012(2) 0.061(2) 0.011(1) C(26) 0.120(3) 0.101(3) 0.114(3) 0.023(2) 0.092(3) 0.008(2) C(27) 0.097(3) 0.103(3) 0.101(3) 0.033(2) 0.062(2) -0.009(2) C(28) 0.080(2) 0.067(2) 0.069(2) 0.026(2) 0.025(2) 0.000(2) C(29) 0.060(2) 0.054(1) 0.047(1) 0.009(1) 0.021(1) 0.002(1) C(30) 0.057(2) 0.053(1) 0.037(1) -0.006(1) 0.017(1) 0.008(1) C(31) 0.082(2) 0.063(2) 0.039(1) -0.009(1) 0.018(1) -0.001(1) C(32) 0.116(3) 0.083(2) 0.047(2) -0.025(2) 0.015(2) -0.007(2) C(33) 0.098(3) 0.105(3) 0.049(2) -0.043(2) 0.002(2) 0.011(2) C(34) 0.060(2) 0.111(3) 0.067(2) -0.023(2) 0.012(2) 0.029(2) C(35) 0.057(2) 0.076(2) 0.055(2) -0.007(1) 0.019(1) 0.014(1) B(1) 0.057(2) 0.063(2) 0.065(2) -0.015(1) 0.037(2) -0.012(1) B(2) 0.060(3) 0.082(3) 0.130(4) -0.003(2) 0.026(3) -0.010(3) #------------------------------------------------------------------------------ _computing_data_collection D*TREK _computing_cell_refinement D*TREK _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru Cl 2.3737(7) . . yes Ru N(1) 1.729(2) . . yes Ru N(2) 2.072(2) . . yes Ru N(4) 2.072(2) . . yes Ru N(6) 2.158(2) . . yes Ru C(10) 2.048(2) . . yes P C(11) 1.804(2) . . yes P C(18) 1.804(2) . . yes P C(24) 1.792(2) . . yes P C(30) 1.799(3) . . yes F(1) B(2) 1.383(5) . . yes F(2) B(2) 1.366(5) . . yes F(3) B(2) 1.362(6) . . yes F(4) B(2) 1.359(5) . . yes O N(1) 1.146(2) . . yes N(2) N(3) 1.362(3) . . yes N(2) C(1) 1.336(3) . . yes N(3) C(3) 1.347(3) . . yes N(3) B(1) 1.540(4) . . yes N(4) N(5) 1.364(3) . . yes N(4) C(4) 1.340(3) . . yes N(5) C(6) 1.340(3) . . yes N(5) B(1) 1.531(3) . . yes N(6) N(7) 1.362(3) . . yes N(6) C(7) 1.333(3) . . yes N(7) C(9) 1.346(3) . . yes N(7) B(1) 1.519(4) . . yes C(1) C(2) 1.381(4) . . yes C(2) C(3) 1.357(4) . . yes C(4) C(5) 1.378(4) . . yes C(5) C(6) 1.365(4) . . yes C(7) C(8) 1.385(4) . . yes C(8) C(9) 1.362(4) . . yes C(10) C(11) 1.339(3) . . yes C(11) C(12) 1.491(3) . . yes C(12) C(13) 1.394(3) . . yes C(12) C(17) 1.389(4) . . yes C(13) C(14) 1.388(4) . . yes C(14) C(15) 1.380(5) . . yes C(15) C(16) 1.373(5) . . yes C(16) C(17) 1.378(4) . . yes C(18) C(19) 1.380(4) . . yes C(18) C(23) 1.388(3) . . yes C(19) C(20) 1.387(4) . . yes C(20) C(21) 1.375(5) . . yes C(21) C(22) 1.357(4) . . yes C(22) C(23) 1.385(4) . . yes C(24) C(25) 1.389(3) . . yes C(24) C(29) 1.389(3) . . yes C(25) C(26) 1.379(4) . . yes C(26) C(27) 1.362(5) . . yes C(27) C(28) 1.366(5) . . yes C(28) C(29) 1.379(4) . . yes C(30) C(31) 1.391(4) . . yes C(30) C(35) 1.385(4) . . yes C(31) C(32) 1.372(4) . . yes C(32) C(33) 1.358(5) . . yes C(33) C(34) 1.380(5) . . yes C(34) C(35) 1.392(4) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl Ru N(1) 95.53(7) . . . yes Cl Ru N(2) 172.37(5) . . . yes Cl Ru N(4) 88.06(5) . . . yes Cl Ru N(6) 90.43(6) . . . yes Cl Ru C(10) 89.39(6) . . . yes N(1) Ru N(2) 91.76(8) . . . yes N(1) Ru N(4) 174.63(8) . . . yes N(1) Ru N(6) 92.57(8) . . . yes N(1) Ru C(10) 97.40(9) . . . yes N(2) Ru N(4) 84.51(7) . . . yes N(2) Ru N(6) 87.00(8) . . . yes N(2) Ru C(10) 91.90(8) . . . yes N(4) Ru N(6) 83.39(7) . . . yes N(4) Ru C(10) 86.60(8) . . . yes N(6) Ru C(10) 169.99(8) . . . yes C(11) P C(18) 110.9(1) . . . yes C(11) P C(24) 108.2(1) . . . yes C(11) P C(30) 111.3(1) . . . yes C(18) P C(24) 109.1(1) . . . yes C(18) P C(30) 111.0(1) . . . yes C(24) P C(30) 106.2(1) . . . yes Ru N(1) O 172.0(2) . . . yes Ru N(2) N(3) 119.8(1) . . . yes Ru N(2) C(1) 132.3(2) . . . yes N(3) N(2) C(1) 107.5(2) . . . yes N(2) N(3) C(3) 108.1(2) . . . yes N(2) N(3) B(1) 119.7(2) . . . yes C(3) N(3) B(1) 132.0(2) . . . yes Ru N(4) N(5) 120.1(1) . . . yes Ru N(4) C(4) 132.9(2) . . . yes N(5) N(4) C(4) 106.9(2) . . . yes N(4) N(5) C(6) 108.6(2) . . . yes N(4) N(5) B(1) 119.8(2) . . . yes C(6) N(5) B(1) 131.5(2) . . . yes Ru N(6) N(7) 119.1(1) . . . yes Ru N(6) C(7) 133.6(2) . . . yes N(7) N(6) C(7) 107.2(2) . . . yes N(6) N(7) C(9) 108.5(2) . . . yes N(6) N(7) B(1) 119.3(2) . . . yes C(9) N(7) B(1) 132.2(2) . . . yes N(2) C(1) C(2) 109.4(2) . . . yes C(1) C(2) C(3) 105.7(2) . . . yes N(3) C(3) C(2) 109.2(2) . . . yes N(4) C(4) C(5) 109.8(2) . . . yes C(4) C(5) C(6) 105.4(2) . . . yes N(5) C(6) C(5) 109.2(2) . . . yes N(6) C(7) C(8) 109.9(3) . . . yes C(7) C(8) C(9) 105.3(2) . . . yes N(7) C(9) C(8) 109.1(3) . . . yes Ru C(10) C(11) 132.7(2) . . . yes P C(11) C(10) 118.2(2) . . . yes P C(11) C(12) 115.0(1) . . . yes C(10) C(11) C(12) 126.5(2) . . . yes C(11) C(12) C(13) 120.4(2) . . . yes C(11) C(12) C(17) 120.4(2) . . . yes C(13) C(12) C(17) 119.2(2) . . . yes C(12) C(13) C(14) 119.7(3) . . . yes C(13) C(14) C(15) 120.4(3) . . . yes C(14) C(15) C(16) 119.9(3) . . . yes C(15) C(16) C(17) 120.4(3) . . . yes C(12) C(17) C(16) 120.5(3) . . . yes P C(18) C(19) 121.4(2) . . . yes P C(18) C(23) 118.6(2) . . . yes C(19) C(18) C(23) 119.5(2) . . . yes C(18) C(19) C(20) 119.6(3) . . . yes C(19) C(20) C(21) 120.3(3) . . . yes C(20) C(21) C(22) 120.4(3) . . . yes C(21) C(22) C(23) 120.1(3) . . . yes C(18) C(23) C(22) 120.1(3) . . . yes P C(24) C(25) 121.0(2) . . . yes P C(24) C(29) 118.7(2) . . . yes C(25) C(24) C(29) 119.6(2) . . . yes C(24) C(25) C(26) 119.8(3) . . . yes C(25) C(26) C(27) 119.8(3) . . . yes C(26) C(27) C(28) 121.2(3) . . . yes C(27) C(28) C(29) 120.0(3) . . . yes C(24) C(29) C(28) 119.5(2) . . . yes P C(30) C(31) 119.9(2) . . . yes P C(30) C(35) 120.2(2) . . . yes C(31) C(30) C(35) 119.9(2) . . . yes C(30) C(31) C(32) 119.6(3) . . . yes C(31) C(32) C(33) 120.7(3) . . . yes C(32) C(33) C(34) 120.7(3) . . . yes C(33) C(34) C(35) 119.5(3) . . . yes C(30) C(35) C(34) 119.5(3) . . . yes N(3) B(1) N(5) 107.4(2) . . . yes N(3) B(1) N(7) 107.8(2) . . . yes N(5) B(1) N(7) 108.7(2) . . . yes F(1) B(2) F(2) 110.0(3) . . . yes F(1) B(2) F(3) 106.3(4) . . . yes F(1) B(2) F(4) 108.7(4) . . . yes F(2) B(2) F(3) 112.4(4) . . . yes F(2) B(2) F(4) 109.2(4) . . . yes F(3) B(2) F(4) 110.1(4) . . . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ru N(2) N(3) C(3) -172.5(2) . . . . yes Ru N(2) N(3) B(1) 11.6(3) . . . . yes Ru N(2) C(1) C(2) 171.4(2) . . . . yes Ru N(4) N(5) C(6) -176.4(2) . . . . yes Ru N(4) N(5) B(1) 7.1(3) . . . . yes Ru N(4) C(4) C(5) 175.8(2) . . . . yes Ru N(6) N(7) C(9) 177.8(2) . . . . yes Ru N(6) N(7) B(1) 0.7(3) . . . . yes Ru N(6) C(7) C(8) -177.0(2) . . . . yes Ru C(10) C(11) P -170.6(1) . . . . yes Ru C(10) C(11) C(12) 2.2(4) . . . . yes Cl Ru N(1) O 122(1) . . . . yes Cl Ru N(2) N(3) -36.6(5) . . . . yes Cl Ru N(2) C(1) 151.7(3) . . . . yes Cl Ru N(4) N(5) -138.2(2) . . . . yes Cl Ru N(4) C(4) 45.8(2) . . . . yes Cl Ru N(6) N(7) 131.9(2) . . . . yes Cl Ru N(6) C(7) -50.7(2) . . . . yes Cl Ru C(10) C(11) 80.7(2) . . . . yes P C(11) C(12) C(13) -79.2(2) . . . . yes P C(11) C(12) C(17) 100.1(2) . . . . yes P C(18) C(19) C(20) -171.3(3) . . . . yes P C(18) C(23) C(22) 172.8(2) . . . . yes P C(24) C(25) C(26) 172.0(3) . . . . yes P C(24) C(29) C(28) -170.5(2) . . . . yes P C(30) C(31) C(32) -179.0(2) . . . . yes P C(30) C(35) C(34) -178.5(2) . . . . yes O N(1) Ru N(2) -55(1) . . . . yes O N(1) Ru N(4) -9(2) . . . . yes O N(1) Ru N(6) 31(1) . . . . yes O N(1) Ru C(10) -147(1) . . . . yes N(1) Ru N(2) N(3) 126.3(2) . . . . yes N(1) Ru N(2) C(1) -45.4(2) . . . . yes N(1) Ru N(4) N(5) -6.1(10) . . . . yes N(1) Ru N(4) C(4) 177.9(8) . . . . yes N(1) Ru N(6) N(7) -132.5(2) . . . . yes N(1) Ru N(6) C(7) 44.8(2) . . . . yes N(1) Ru C(10) C(11) -14.8(2) . . . . yes N(2) Ru N(4) N(5) 40.0(2) . . . . yes N(2) Ru N(4) C(4) -136.0(2) . . . . yes N(2) Ru N(6) N(7) -40.9(2) . . . . yes N(2) Ru N(6) C(7) 136.5(2) . . . . yes N(2) Ru C(10) C(11) -106.8(2) . . . . yes N(2) N(3) C(3) C(2) -0.7(3) . . . . yes N(2) N(3) B(1) N(5) 50.2(3) . . . . yes N(2) N(3) B(1) N(7) -66.8(3) . . . . yes N(2) C(1) C(2) C(3) 0.7(3) . . . . yes N(3) N(2) Ru N(4) -49.8(2) . . . . yes N(3) N(2) Ru N(6) 33.8(2) . . . . yes N(3) N(2) Ru C(10) -136.2(2) . . . . yes N(3) N(2) C(1) C(2) -1.1(3) . . . . yes N(3) C(3) C(2) C(1) 0.0(3) . . . . yes N(3) B(1) N(5) N(4) -61.2(3) . . . . yes N(3) B(1) N(5) C(6) 123.2(3) . . . . yes N(3) B(1) N(7) N(6) 57.7(3) . . . . yes N(3) B(1) N(7) C(9) -118.6(3) . . . . yes N(4) Ru N(2) C(1) 138.5(2) . . . . yes N(4) Ru N(6) N(7) 43.9(2) . . . . yes N(4) Ru N(6) C(7) -138.7(2) . . . . yes N(4) Ru C(10) C(11) 168.8(2) . . . . yes N(4) N(5) C(6) C(5) -0.2(3) . . . . yes N(4) N(5) B(1) N(7) 55.2(3) . . . . yes N(4) C(4) C(5) C(6) 0.4(3) . . . . yes N(5) N(4) Ru N(6) -47.6(2) . . . . yes N(5) N(4) Ru C(10) 132.3(2) . . . . yes N(5) N(4) C(4) C(5) -0.5(3) . . . . yes N(5) C(6) C(5) C(4) -0.1(3) . . . . yes N(5) B(1) N(3) C(3) -124.6(3) . . . . yes N(5) B(1) N(7) N(6) -58.4(3) . . . . yes N(5) B(1) N(7) C(9) 125.3(3) . . . . yes N(6) Ru N(2) C(1) -137.9(2) . . . . yes N(6) Ru N(4) C(4) 136.4(2) . . . . yes N(6) Ru C(10) C(11) 169.7(4) . . . . yes N(6) N(7) C(9) C(8) -0.3(3) . . . . yes N(6) C(7) C(8) C(9) -0.7(3) . . . . yes N(7) N(6) Ru C(10) 43.0(5) . . . . yes N(7) N(6) C(7) C(8) 0.6(3) . . . . yes N(7) C(9) C(8) C(7) 0.6(3) . . . . yes N(7) B(1) N(3) C(3) 118.4(3) . . . . yes N(7) B(1) N(5) C(6) -120.3(3) . . . . yes C(1) N(2) Ru C(10) 52.1(2) . . . . yes C(1) N(2) N(3) C(3) 1.1(3) . . . . yes C(1) N(2) N(3) B(1) -174.8(2) . . . . yes C(2) C(3) N(3) B(1) 174.6(3) . . . . yes C(4) N(4) Ru C(10) -43.7(2) . . . . yes C(4) N(4) N(5) C(6) 0.5(3) . . . . yes C(4) N(4) N(5) B(1) -176.0(2) . . . . yes C(5) C(6) N(5) B(1) 175.7(3) . . . . yes C(7) N(6) Ru C(10) -139.6(4) . . . . yes C(7) N(6) N(7) C(9) -0.2(3) . . . . yes C(7) N(6) N(7) B(1) -177.3(2) . . . . yes C(8) C(9) N(7) B(1) 176.3(3) . . . . yes C(10) C(11) P C(18) -143.4(2) . . . . yes C(10) C(11) P C(24) 97.0(2) . . . . yes C(10) C(11) P C(30) -19.3(2) . . . . yes C(10) C(11) C(12) C(13) 107.8(3) . . . . yes C(10) C(11) C(12) C(17) -72.9(3) . . . . yes C(11) P C(18) C(19) 96.4(2) . . . . yes C(11) P C(18) C(23) -75.4(2) . . . . yes C(11) P C(24) C(25) 152.2(2) . . . . yes C(11) P C(24) C(29) -37.1(2) . . . . yes C(11) P C(30) C(31) 123.4(2) . . . . yes C(11) P C(30) C(35) -56.3(2) . . . . yes C(11) C(12) C(13) C(14) 179.8(2) . . . . yes C(11) C(12) C(17) C(16) 178.8(2) . . . . yes C(12) C(11) P C(18) 43.0(2) . . . . yes C(12) C(11) P C(24) -76.6(2) . . . . yes C(12) C(11) P C(30) 167.1(2) . . . . yes C(12) C(13) C(14) C(15) 1.4(4) . . . . yes C(12) C(17) C(16) C(15) 1.6(5) . . . . yes C(13) C(12) C(17) C(16) -2.0(4) . . . . yes C(13) C(14) C(15) C(16) -1.7(5) . . . . yes C(14) C(13) C(12) C(17) 0.5(4) . . . . yes C(14) C(15) C(16) C(17) 0.2(5) . . . . yes C(18) P C(24) C(25) 31.5(3) . . . . yes C(18) P C(24) C(29) -157.9(2) . . . . yes C(18) P C(30) C(31) -112.6(2) . . . . yes C(18) P C(30) C(35) 67.8(2) . . . . yes C(18) C(19) C(20) C(21) -0.8(5) . . . . yes C(18) C(23) C(22) C(21) -1.8(4) . . . . yes C(19) C(18) P C(24) -144.6(2) . . . . yes C(19) C(18) P C(30) -27.9(3) . . . . yes C(19) C(18) C(23) C(22) 0.9(4) . . . . yes C(19) C(20) C(21) C(22) -0.1(6) . . . . yes C(20) C(19) C(18) C(23) 0.4(4) . . . . yes C(20) C(21) C(22) C(23) 1.4(5) . . . . yes C(23) C(18) P C(24) 43.7(2) . . . . yes C(23) C(18) P C(30) 160.3(2) . . . . yes C(24) P C(30) C(31) 5.9(2) . . . . yes C(24) P C(30) C(35) -173.8(2) . . . . yes C(24) C(25) C(26) C(27) -2.3(6) . . . . yes C(24) C(29) C(28) C(27) -1.1(5) . . . . yes C(25) C(24) P C(30) -88.2(2) . . . . yes C(25) C(24) C(29) C(28) 0.3(4) . . . . yes C(25) C(26) C(27) C(28) 1.5(7) . . . . yes C(26) C(25) C(24) C(29) 1.4(5) . . . . yes C(26) C(27) C(28) C(29) 0.2(6) . . . . yes C(29) C(24) P C(30) 82.4(2) . . . . yes C(30) C(31) C(32) C(33) -2.2(5) . . . . yes C(30) C(35) C(34) C(33) -2.8(4) . . . . yes C(31) C(30) C(35) C(34) 1.8(4) . . . . yes C(31) C(32) C(33) C(34) 1.2(5) . . . . yes C(32) C(31) C(30) C(35) 0.6(4) . . . . yes C(32) C(33) C(34) C(35) 1.3(5) . . . . yes C(32) C(33) C(34) C(35) 1.3(5) . . . . yes #------------------------------------------------------------------------------ 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 F(1) C(1) 3.092(3) . . ? F(1) C(5) 3.249(3) . 1_545 ? F(1) C(35) 3.258(4) . . ? F(1) C(19) 3.261(3) . . ? F(2) C(35) 3.228(4) . . ? F(2) C(22) 3.322(4) . 4_545 ? F(2) C(34) 3.353(5) . . ? F(3) C(33) 3.189(4) . 2_646 ? F(3) C(5) 3.441(4) . 1_545 ? F(3) C(19) 3.528(4) . . ? F(4) C(6) 3.093(3) . 1_545 ? F(4) C(23) 3.133(3) . 4_545 ? F(4) C(5) 3.274(4) . 1_545 ? F(4) C(2) 3.427(5) . . ? F(4) C(22) 3.520(4) . 4_545 ? F(4) C(25) 3.551(4) . 4_545 ? O N(3) 3.280(3) . 3_655 ? O N(7) 3.304(3) . 3_655 ? O C(3) 3.357(4) . 3_655 ? O C(9) 3.394(3) . 3_655 ? O N(6) 3.473(3) . 3_655 ? N(5) C(8) 3.518(4) . 3_665 ? N(7) C(8) 3.467(3) . 3_665 ? C(1) C(7) 3.589(4) . 3_655 ? C(3) C(28) 3.507(4) . 4_555 ? C(5) B(2) 3.543(5) . 1_565 ? C(6) C(27) 3.445(5) . 4_555 ? C(6) C(8) 3.519(4) . 3_665 ? C(7) C(9) 3.553(4) . 3_665 ? C(8) C(9) 3.507(4) . 3_665 ? C(9) C(14) 3.363(4) . 3_655 ? C(27) C(34) 3.576(4) . 4_455 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_0499c _database_code_depnum_ccdc_archive 'CCDC 252271' _audit_creation_date 'Fri Oct 1 13:18:56 2004' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C32 H31 B2 Cl F4 N7 O P Ru ' _chemical_formula_moiety 'C32 H31 B Cl N7 O P Ru, B F4 ' _chemical_formula_weight 794.75 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 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 13.064(1) _cell_length_b 22.799(2) _cell_length_c 13.2996(2) _cell_angle_alpha 90 _cell_angle_beta 105.2156(4) _cell_angle_gamma 90 _cell_volume 3822.5(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 295.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.300 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.770 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Quantum CCD/Rigaku AFC7' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33079 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9840 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9840 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). Location of BF4 anion were refined as a rigid group. ; _reflns_number_total 8635 _reflns_number_gt 5630 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1335 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 8366 _refine_ls_number_parameters 404 _refine_ls_goodness_of_fit_ref 1.837 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.02000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0009 _refine_diff_density_max 1.54 _refine_diff_density_min -0.78 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru Ru -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.84099(3) -0.03565(2) 0.70311(2) 0.03831(9) Uani 1.00 d . . . Cl Cl 0.8557(1) -0.12548(6) 0.7908(1) 0.0688(4) Uani 1.00 d . . . P P 0.60420(8) -0.16733(5) 0.39103(8) 0.0368(3) Uani 1.00 d . . . F(1) F 0.4326(8) -0.1275(6) 0.8069(10) 0.3256 Uiso 1.00 d G . . F(2) F 0.350(1) -0.0545(5) 0.8635(10) 0.3256 Uiso 1.00 d G . . F(3) F 0.2934(10) -0.1461(5) 0.8683(9) 0.3256 Uiso 1.00 d G . . F(4) F 0.2713(9) -0.1007(6) 0.7165(8) 0.3256 Uiso 1.00 d G . . O O 0.9856(5) -0.0666(3) 0.5843(4) 0.116(2) Uani 1.00 d . . . N(1) N 0.9319(3) -0.0571(2) 0.6265(3) 0.056(1) Uani 1.00 d . . . N(2) N 0.8187(3) 0.0471(2) 0.6374(2) 0.0430(9) Uani 1.00 d . . . N(3) N 0.8289(3) 0.0957(1) 0.7001(2) 0.0388(9) Uani 1.00 d . . . N(4) N 0.7382(3) -0.0068(2) 0.7863(2) 0.0406(9) Uani 1.00 d . . . N(5) N 0.7544(3) 0.0467(2) 0.8345(3) 0.0433(10) Uani 1.00 d . . . N(6) N 0.9638(3) 0.0013(2) 0.8250(2) 0.0403(9) Uani 1.00 d . . . N(7) N 0.9492(3) 0.0555(2) 0.8606(2) 0.0419(9) Uani 1.00 d . . . C(1) C 0.8023(4) 0.0661(2) 0.5403(3) 0.054(1) Uani 1.00 d . . . C(2) C 0.8011(4) 0.1271(3) 0.5394(4) 0.064(2) Uani 1.00 d . . . C(3) C 0.8153(4) 0.1434(2) 0.6396(4) 0.057(1) Uani 1.00 d . . . C(4) C 0.6534(3) -0.0308(2) 0.8087(3) 0.047(1) Uani 1.00 d . . . C(5) C 0.6161(4) 0.0068(3) 0.8736(4) 0.060(2) Uani 1.00 d . . . C(6) C 0.6809(4) 0.0545(2) 0.8879(4) 0.055(1) Uani 1.00 d . . . C(7) C 1.0608(3) -0.0161(2) 0.8739(3) 0.048(1) Uani 1.00 d . . . C(8) C 1.1103(3) 0.0278(2) 0.9435(3) 0.056(1) Uani 1.00 d . . . C(9) C 1.0391(4) 0.0713(2) 0.9336(3) 0.052(1) Uani 1.00 d . . . C(10) C 0.7120(3) -0.0655(2) 0.5975(3) 0.041(1) Uani 1.00 d . . . C(11) C 0.6345(3) -0.0857(2) 0.5391(3) 0.039(1) Uani 1.00 d . . . C(12) C 0.5444(3) -0.1158(2) 0.4686(3) 0.040(1) Uani 1.00 d . . . C(13) C 0.4815(4) -0.1503(2) 0.5317(4) 0.054(1) Uani 1.00 d . . . C(14) C 0.4695(4) -0.0719(2) 0.3962(4) 0.052(1) Uani 1.00 d . . . C(15) C 0.6543(3) -0.2312(2) 0.4674(3) 0.044(1) Uani 1.00 d . . . C(16) C 0.7198(4) -0.2236(2) 0.5676(4) 0.057(1) Uani 1.00 d . . . C(17) C 0.7686(4) -0.2710(3) 0.6248(4) 0.067(2) Uani 1.00 d . . . C(18) C 0.7523(5) -0.3259(3) 0.5827(5) 0.071(2) Uani 1.00 d . . . C(19) C 0.6886(6) -0.3339(2) 0.4857(5) 0.086(2) Uani 1.00 d . . . C(20) C 0.6380(5) -0.2870(2) 0.4259(4) 0.064(2) Uani 1.00 d . . . C(21) C 0.5073(3) -0.1887(2) 0.2738(3) 0.046(1) Uani 1.00 d . . . C(22) C 0.4194(4) -0.2215(3) 0.2781(4) 0.068(2) Uani 1.00 d . . . C(23) C 0.3450(5) -0.2357(3) 0.1875(6) 0.085(2) Uani 1.00 d . . . C(24) C 0.3561(5) -0.2181(3) 0.0917(5) 0.073(2) Uani 1.00 d . . . C(25) C 0.4425(5) -0.1864(3) 0.0859(4) 0.075(2) Uani 1.00 d . . . C(26) C 0.5201(4) -0.1718(2) 0.1776(3) 0.054(1) Uani 1.00 d . . . C(27) C 0.7160(3) -0.1331(2) 0.3597(3) 0.043(1) Uani 1.00 d . . . C(28) C 0.8113(4) -0.1640(3) 0.3788(4) 0.058(1) Uani 1.00 d . . . C(29) C 0.8990(4) -0.1384(3) 0.3590(4) 0.069(2) Uani 1.00 d . . . C(30) C 0.8943(5) -0.0834(3) 0.3208(5) 0.076(2) Uani 1.00 d . . . C(31) C 0.8013(6) -0.0516(3) 0.3015(4) 0.073(2) Uani 1.00 d . . . C(32) C 0.7127(4) -0.0766(2) 0.3217(4) 0.057(1) Uani 1.00 d . . . B(1) B 0.8442(4) 0.0867(2) 0.8197(4) 0.047(1) Uani 1.00 d . . . B(2) B 0.3368(7) -0.1072(4) 0.8138(7) 0.3256 Uiso 1.00 d G . . H(1) H 0.8400 0.1279 0.8504 0.0647 Uiso 1.00 calc . . . H(2) H 0.7926 0.0413 0.4793 0.0642 Uiso 1.00 calc . . . H(3) H 0.7919 0.1525 0.4793 0.0765 Uiso 1.00 calc . . . H(4) H 0.8157 0.1835 0.6640 0.0686 Uiso 1.00 calc . . . H(5) H 0.6227 -0.0685 0.7838 0.0568 Uiso 1.00 calc . . . H(6) H 0.5562 0.0004 0.9026 0.0717 Uiso 1.00 calc . . . H(7) H 0.6752 0.0886 0.9298 0.0658 Uiso 1.00 calc . . . H(8) H 1.0924 -0.0533 0.8634 0.0573 Uiso 1.00 calc . . . H(9) H 1.1815 0.0269 0.9894 0.0673 Uiso 1.00 calc . . . H(10) H 1.0498 0.1079 0.9720 0.0618 Uiso 1.00 calc . . . H(11) H 0.4561 -0.1236 0.5766 0.0647 Uiso 1.00 calc . . . H(12) H 0.4216 -0.1695 0.4844 0.0647 Uiso 1.00 calc . . . H(13) H 0.5271 -0.1796 0.5739 0.0647 Uiso 1.00 calc . . . H(14) H 0.4416 -0.0444 0.4381 0.0625 Uiso 1.00 calc . . . H(15) H 0.5085 -0.0506 0.3551 0.0625 Uiso 1.00 calc . . . H(16) H 0.4113 -0.0930 0.3502 0.0625 Uiso 1.00 calc . . . H(17) H 0.7312 -0.1846 0.5974 0.0689 Uiso 1.00 calc . . . H(18) H 0.8143 -0.2654 0.6944 0.0801 Uiso 1.00 calc . . . H(19) H 0.7865 -0.3594 0.6227 0.0850 Uiso 1.00 calc . . . H(20) H 0.6780 -0.3732 0.4571 0.1031 Uiso 1.00 calc . . . H(21) H 0.5922 -0.2934 0.3565 0.0765 Uiso 1.00 calc . . . H(22) H 0.4105 -0.2345 0.3447 0.0821 Uiso 1.00 calc . . . H(23) H 0.2834 -0.2586 0.1910 0.1022 Uiso 1.00 calc . . . H(24) H 0.3024 -0.2284 0.0286 0.0879 Uiso 1.00 calc . . . H(25) H 0.4506 -0.1738 0.0188 0.0896 Uiso 1.00 calc . . . H(26) H 0.5826 -0.1500 0.1736 0.0648 Uiso 1.00 calc . . . H(27) H 0.8156 -0.2036 0.4061 0.0700 Uiso 1.00 calc . . . H(28) H 0.9650 -0.1601 0.3725 0.0832 Uiso 1.00 calc . . . H(29) H 0.9569 -0.0660 0.3067 0.0908 Uiso 1.00 calc . . . H(30) H 0.7983 -0.0120 0.2741 0.0880 Uiso 1.00 calc . . . H(31) H 0.6473 -0.0543 0.3090 0.0690 Uiso 1.00 calc . . . 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 Ru 0.0336(2) 0.0457(2) 0.0318(2) -0.0005(2) 0.0017(1) -0.0043(1) Cl 0.0774(9) 0.0595(8) 0.0612(7) -0.0016(6) 0.0033(6) 0.0022(6) P 0.0329(5) 0.0368(5) 0.0383(5) -0.0015(4) 0.0052(4) -0.0005(4) O 0.090(4) 0.162(5) 0.102(4) 0.005(3) 0.035(3) -0.045(3) N(1) 0.044(2) 0.073(3) 0.043(2) -0.015(2) -0.002(2) 0.003(2) N(2) 0.032(2) 0.059(2) 0.035(2) -0.004(2) 0.003(1) 0.002(2) N(3) 0.036(2) 0.042(2) 0.036(2) 0.005(1) 0.006(1) 0.006(1) N(4) 0.037(2) 0.048(2) 0.035(2) -0.002(2) 0.005(1) 0.001(1) N(5) 0.039(2) 0.049(2) 0.042(2) 0.003(2) 0.012(1) -0.004(1) N(6) 0.035(2) 0.048(2) 0.033(2) -0.002(1) 0.000(1) 0.000(1) N(7) 0.041(2) 0.048(2) 0.033(2) -0.006(2) 0.002(1) -0.007(1) C(1) 0.040(2) 0.081(4) 0.037(2) -0.004(2) 0.006(2) 0.009(2) C(2) 0.045(3) 0.081(4) 0.062(3) 0.003(2) 0.009(2) 0.036(3) C(3) 0.041(2) 0.056(3) 0.073(3) 0.007(2) 0.012(2) 0.026(2) C(4) 0.040(2) 0.062(3) 0.040(2) -0.006(2) 0.009(2) 0.009(2) C(5) 0.048(3) 0.075(3) 0.064(3) 0.010(3) 0.028(2) 0.019(3) C(6) 0.055(3) 0.064(3) 0.049(2) 0.016(2) 0.020(2) 0.003(2) C(7) 0.034(2) 0.062(3) 0.041(2) -0.001(2) 0.000(2) 0.013(2) C(8) 0.038(2) 0.078(3) 0.041(2) -0.013(2) -0.009(2) 0.012(2) C(9) 0.048(3) 0.064(3) 0.036(2) -0.021(2) -0.001(2) -0.008(2) C(10) 0.040(2) 0.043(2) 0.037(2) 0.001(2) 0.004(2) -0.002(2) C(11) 0.033(2) 0.045(2) 0.037(2) 0.001(2) 0.006(2) -0.003(2) C(12) 0.032(2) 0.043(2) 0.040(2) 0.000(2) 0.003(2) -0.001(2) C(13) 0.044(2) 0.060(3) 0.063(3) -0.010(2) 0.024(2) -0.009(2) C(14) 0.040(2) 0.054(3) 0.054(2) 0.013(2) -0.002(2) -0.002(2) C(15) 0.043(2) 0.038(2) 0.053(2) 0.004(2) 0.017(2) 0.004(2) C(16) 0.060(3) 0.048(3) 0.057(3) 0.002(2) 0.003(2) 0.010(2) C(17) 0.066(3) 0.062(3) 0.070(3) 0.011(3) 0.013(3) 0.020(3) C(18) 0.084(4) 0.056(3) 0.077(4) 0.028(3) 0.029(3) 0.020(3) C(19) 0.132(6) 0.041(3) 0.091(4) 0.024(3) 0.040(4) 0.000(3) C(20) 0.087(4) 0.041(3) 0.062(3) 0.008(2) 0.017(3) -0.005(2) C(21) 0.044(2) 0.044(2) 0.047(2) 0.003(2) 0.003(2) -0.012(2) C(22) 0.063(3) 0.071(3) 0.069(3) -0.022(3) 0.012(2) -0.018(3) C(23) 0.055(3) 0.080(4) 0.108(5) -0.021(3) 0.000(3) -0.036(4) C(24) 0.060(3) 0.070(4) 0.071(4) 0.009(3) -0.016(3) -0.034(3) C(25) 0.079(4) 0.086(4) 0.045(3) 0.029(3) -0.007(2) -0.022(3) C(26) 0.046(2) 0.063(3) 0.046(2) 0.010(2) -0.001(2) -0.009(2) C(27) 0.043(2) 0.047(2) 0.039(2) -0.003(2) 0.012(2) -0.003(2) C(28) 0.040(2) 0.080(4) 0.056(3) 0.000(2) 0.014(2) 0.008(2) C(29) 0.038(3) 0.108(5) 0.065(3) -0.004(3) 0.018(2) 0.012(3) C(30) 0.057(3) 0.106(5) 0.070(3) -0.032(3) 0.028(3) -0.009(3) C(31) 0.096(5) 0.066(4) 0.070(3) -0.028(3) 0.042(3) -0.003(3) C(32) 0.060(3) 0.056(3) 0.061(3) 0.000(2) 0.026(2) 0.007(2) B(1) 0.048(3) 0.046(3) 0.043(2) -0.001(2) 0.007(2) -0.006(2) #------------------------------------------------------------------------------ _computing_data_collection D*TREK _computing_cell_refinement D*TREK _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru Cl 2.340(1) . . yes Ru N(1) 1.823(5) . . yes Ru N(2) 2.067(4) . . yes Ru N(4) 2.059(4) . . yes Ru N(6) 2.132(3) . . yes Ru C(10) 2.008(4) . . yes P C(12) 1.864(4) . . yes P C(15) 1.797(4) . . yes P C(21) 1.799(4) . . yes P C(27) 1.798(5) . . yes O N(1) 1.031(8) . . yes N(2) N(3) 1.371(5) . . yes N(2) C(1) 1.324(6) . . yes N(3) C(3) 1.336(6) . . yes N(3) B(1) 1.564(6) . . yes N(4) N(5) 1.369(5) . . yes N(4) C(4) 1.338(6) . . yes N(5) C(6) 1.347(7) . . yes N(5) B(1) 1.539(7) . . yes N(6) N(7) 1.353(5) . . yes N(6) C(7) 1.324(5) . . yes N(7) C(9) 1.360(5) . . yes N(7) B(1) 1.515(6) . . yes C(1) C(2) 1.390(8) . . yes C(2) C(3) 1.348(8) . . yes C(4) C(5) 1.392(8) . . yes C(5) C(6) 1.361(8) . . yes C(7) C(8) 1.400(7) . . yes C(8) C(9) 1.342(7) . . yes C(10) C(11) 1.195(5) . . yes C(11) C(12) 1.468(5) . . yes C(12) C(13) 1.536(7) . . yes C(12) C(14) 1.548(6) . . yes C(15) C(16) 1.393(6) . . yes C(15) C(20) 1.381(6) . . yes C(16) C(17) 1.378(7) . . yes C(17) C(18) 1.365(8) . . yes C(18) C(19) 1.351(9) . . yes C(19) C(20) 1.392(8) . . yes C(21) C(22) 1.384(8) . . yes C(21) C(26) 1.388(7) . . yes C(22) C(23) 1.373(8) . . yes C(23) C(24) 1.38(1) . . yes C(24) C(25) 1.361(9) . . yes C(25) C(26) 1.405(6) . . yes C(27) C(28) 1.395(7) . . yes C(27) C(32) 1.380(7) . . yes C(28) C(29) 1.370(8) . . yes C(29) C(30) 1.35(1) . . yes C(30) C(31) 1.380(10) . . yes C(31) C(32) 1.379(9) . . yes B(2) F(1) 1.36 . . yes B(2) F(2) 1.36 . . yes B(2) F(3) 1.36 . . yes B(2) F(4) 1.36 . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl Ru N(1) 93.6(1) . . . yes Cl Ru N(2) 173.5(1) . . . yes Cl Ru N(4) 89.5(1) . . . yes Cl Ru N(6) 91.16(10) . . . yes Cl Ru C(10) 89.8(1) . . . yes N(1) Ru N(2) 92.8(2) . . . yes N(1) Ru N(4) 176.8(2) . . . yes N(1) Ru N(6) 93.5(2) . . . yes N(1) Ru C(10) 93.9(2) . . . yes N(2) Ru N(4) 84.0(1) . . . yes N(2) Ru N(6) 87.4(1) . . . yes N(2) Ru C(10) 90.8(1) . . . yes N(4) Ru N(6) 86.1(1) . . . yes N(4) Ru C(10) 86.5(2) . . . yes N(6) Ru C(10) 172.5(2) . . . yes C(12) P C(15) 109.9(2) . . . yes C(12) P C(21) 110.4(2) . . . yes C(12) P C(27) 109.8(2) . . . yes C(15) P C(21) 109.8(2) . . . yes C(15) P C(27) 106.6(2) . . . yes C(21) P C(27) 110.3(2) . . . yes Ru N(1) O 176.2(5) . . . yes Ru N(2) N(3) 120.0(2) . . . yes Ru N(2) C(1) 132.8(3) . . . yes N(3) N(2) C(1) 107.1(4) . . . yes N(2) N(3) C(3) 108.4(3) . . . yes N(2) N(3) B(1) 118.6(3) . . . yes C(3) N(3) B(1) 132.8(4) . . . yes Ru N(4) N(5) 119.6(3) . . . yes Ru N(4) C(4) 133.2(3) . . . yes N(5) N(4) C(4) 107.2(4) . . . yes N(4) N(5) C(6) 108.7(4) . . . yes N(4) N(5) B(1) 119.8(4) . . . yes C(6) N(5) B(1) 131.4(4) . . . yes Ru N(6) N(7) 118.7(2) . . . yes Ru N(6) C(7) 133.4(3) . . . yes N(7) N(6) C(7) 107.8(3) . . . yes N(6) N(7) C(9) 108.5(3) . . . yes N(6) N(7) B(1) 120.0(3) . . . yes C(9) N(7) B(1) 131.5(4) . . . yes N(2) C(1) C(2) 109.5(4) . . . yes C(1) C(2) C(3) 105.6(5) . . . yes N(3) C(3) C(2) 109.4(5) . . . yes N(4) C(4) C(5) 109.3(4) . . . yes C(4) C(5) C(6) 105.9(5) . . . yes N(5) C(6) C(5) 108.9(5) . . . yes N(6) C(7) C(8) 109.1(4) . . . yes C(7) C(8) C(9) 106.0(4) . . . yes N(7) C(9) C(8) 108.7(4) . . . yes Ru C(10) C(11) 176.0(4) . . . yes C(10) C(11) C(12) 174.7(4) . . . yes P C(12) C(11) 105.4(3) . . . yes P C(12) C(13) 110.0(3) . . . yes P C(12) C(14) 110.6(3) . . . yes C(11) C(12) C(13) 110.2(3) . . . yes C(11) C(12) C(14) 111.4(3) . . . yes C(13) C(12) C(14) 109.2(4) . . . yes P C(15) C(16) 118.8(3) . . . yes P C(15) C(20) 121.7(3) . . . yes C(16) C(15) C(20) 119.2(4) . . . yes C(15) C(16) C(17) 120.7(5) . . . yes C(16) C(17) C(18) 119.5(5) . . . yes C(17) C(18) C(19) 120.4(5) . . . yes C(18) C(19) C(20) 121.6(5) . . . yes C(15) C(20) C(19) 118.6(5) . . . yes P C(21) C(22) 120.9(4) . . . yes P C(21) C(26) 119.7(3) . . . yes C(22) C(21) C(26) 119.3(4) . . . yes C(21) C(22) C(23) 119.7(6) . . . yes C(22) C(23) C(24) 121.3(6) . . . yes C(23) C(24) C(25) 119.8(5) . . . yes C(24) C(25) C(26) 119.8(5) . . . yes C(21) C(26) C(25) 120.0(5) . . . yes P C(27) C(28) 118.7(4) . . . yes P C(27) C(32) 122.7(4) . . . yes C(28) C(27) C(32) 118.6(5) . . . yes C(27) C(28) C(29) 120.1(5) . . . yes C(28) C(29) C(30) 120.7(5) . . . yes C(29) C(30) C(31) 120.6(6) . . . yes C(30) C(31) C(32) 119.3(6) . . . yes C(27) C(32) C(31) 120.7(5) . . . yes N(3) B(1) N(5) 108.0(3) . . . yes N(3) B(1) N(7) 106.8(4) . . . yes N(5) B(1) N(7) 108.9(4) . . . yes F(1) B(2) F(2) 109.5(10) . . . yes F(1) B(2) F(3) 109.5(10) . . . yes F(1) B(2) F(4) 109(1) . . . yes F(2) B(2) F(3) 109(1) . . . yes F(2) B(2) F(4) 109.4(9) . . . yes F(3) B(2) F(4) 109.4(9) . . . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ru N(2) N(3) C(3) 177.3(3) . . . . yes Ru N(2) N(3) B(1) -7.1(5) . . . . yes Ru N(2) C(1) C(2) -175.1(3) . . . . yes Ru N(4) N(5) C(6) -176.8(3) . . . . yes Ru N(4) N(5) B(1) 4.4(4) . . . . yes Ru N(4) C(4) C(5) 176.5(3) . . . . yes Ru N(6) N(7) C(9) -176.9(3) . . . . yes Ru N(6) N(7) B(1) 4.5(5) . . . . yes Ru N(6) C(7) C(8) 175.9(3) . . . . yes Ru C(10) C(11) C(12) -58(9) . . . . yes Cl Ru N(1) O -135(6) . . . . yes Cl Ru N(2) N(3) 40.6(9) . . . . yes Cl Ru N(2) C(1) -145.2(7) . . . . yes Cl Ru N(4) N(5) 130.8(2) . . . . yes Cl Ru N(4) C(4) -46.8(3) . . . . yes Cl Ru N(6) N(7) -134.5(3) . . . . yes Cl Ru N(6) C(7) 50.2(4) . . . . yes Cl Ru C(10) C(11) 22(5) . . . . yes P C(12) C(11) C(10) -39(5) . . . . yes P C(15) C(16) C(17) -173.3(5) . . . . yes P C(15) C(20) C(19) 173.1(5) . . . . yes P C(21) C(22) C(23) 178.0(5) . . . . yes P C(21) C(26) C(25) -177.5(4) . . . . yes P C(27) C(28) C(29) -177.9(4) . . . . yes P C(27) C(32) C(31) 178.1(4) . . . . yes O N(1) Ru N(2) 43(6) . . . . yes O N(1) Ru N(4) 37(8) . . . . yes O N(1) Ru N(6) -44(6) . . . . yes O N(1) Ru C(10) 134(6) . . . . yes N(1) Ru N(2) N(3) -130.2(3) . . . . yes N(1) Ru N(2) C(1) 44.0(4) . . . . yes N(1) Ru N(4) N(5) -42(2) . . . . yes N(1) Ru N(4) C(4) 139(2) . . . . yes N(1) Ru N(6) N(7) 131.8(3) . . . . yes N(1) Ru N(6) C(7) -43.4(4) . . . . yes N(1) Ru C(10) C(11) 115(5) . . . . yes N(2) Ru N(4) N(5) -48.2(3) . . . . yes N(2) Ru N(4) C(4) 134.2(3) . . . . yes N(2) Ru N(6) N(7) 39.1(3) . . . . yes N(2) Ru N(6) C(7) -136.1(4) . . . . yes N(2) Ru C(10) C(11) -151(5) . . . . yes N(2) N(3) C(3) C(2) -2.7(5) . . . . yes N(2) N(3) B(1) N(5) -52.8(5) . . . . yes N(2) N(3) B(1) N(7) 64.3(5) . . . . yes N(2) C(1) C(2) C(3) -1.2(5) . . . . yes N(3) N(2) Ru N(4) 49.5(3) . . . . yes N(3) N(2) Ru N(6) -36.8(3) . . . . yes N(3) N(2) Ru C(10) 135.9(3) . . . . yes N(3) N(2) C(1) C(2) -0.4(5) . . . . yes N(3) C(3) C(2) C(1) 2.4(5) . . . . yes N(3) B(1) N(5) N(4) 54.7(5) . . . . yes N(3) B(1) N(5) C(6) -123.8(4) . . . . yes N(3) B(1) N(7) N(6) -62.0(5) . . . . yes N(3) B(1) N(7) C(9) 119.8(5) . . . . yes N(4) Ru N(2) C(1) -136.3(4) . . . . yes N(4) Ru N(6) N(7) -45.0(3) . . . . yes N(4) Ru N(6) C(7) 139.7(4) . . . . yes N(4) Ru C(10) C(11) -67(5) . . . . yes N(4) N(5) C(6) C(5) -0.9(5) . . . . yes N(4) N(5) B(1) N(7) -60.9(4) . . . . yes N(4) C(4) C(5) C(6) 0.7(5) . . . . yes N(5) N(4) Ru N(6) 39.6(3) . . . . yes N(5) N(4) Ru C(10) -139.4(3) . . . . yes N(5) N(4) C(4) C(5) -1.3(4) . . . . yes N(5) C(6) C(5) C(4) 0.1(5) . . . . yes N(5) B(1) N(3) C(3) 121.4(5) . . . . yes N(5) B(1) N(7) N(6) 54.5(5) . . . . yes N(5) B(1) N(7) C(9) -123.8(5) . . . . yes N(6) Ru N(2) C(1) 137.3(4) . . . . yes N(6) Ru N(4) C(4) -138.0(4) . . . . yes N(6) Ru C(10) C(11) -74(5) . . . . yes N(6) N(7) C(9) C(8) 0.5(5) . . . . yes N(6) C(7) C(8) C(9) 0.1(6) . . . . yes N(7) N(6) Ru C(10) -37(1) . . . . yes N(7) N(6) C(7) C(8) 0.2(5) . . . . yes N(7) C(9) C(8) C(7) -0.4(6) . . . . yes N(7) B(1) N(3) C(3) -121.5(5) . . . . yes N(7) B(1) N(5) C(6) 120.6(5) . . . . yes C(1) N(2) Ru C(10) -50.0(4) . . . . yes C(1) N(2) N(3) C(3) 1.9(5) . . . . yes C(1) N(2) N(3) B(1) 177.4(4) . . . . yes C(2) C(3) N(3) B(1) -177.3(4) . . . . yes C(4) N(4) Ru C(10) 43.0(4) . . . . yes C(4) N(4) N(5) C(6) 1.3(4) . . . . yes C(4) N(4) N(5) B(1) -177.4(3) . . . . yes C(5) C(6) N(5) B(1) 177.7(4) . . . . yes C(7) N(6) Ru C(10) 147(1) . . . . yes C(7) N(6) N(7) C(9) -0.5(5) . . . . yes C(7) N(6) N(7) B(1) -179.1(4) . . . . yes C(8) C(9) N(7) B(1) 178.9(5) . . . . yes C(10) C(11) C(12) C(13) 78(5) . . . . yes C(10) C(11) C(12) C(14) -159(4) . . . . yes C(11) C(12) P C(15) 78.3(3) . . . . yes C(11) C(12) P C(21) -160.4(3) . . . . yes C(11) C(12) P C(27) -38.7(3) . . . . yes C(12) P C(15) C(16) -50.0(5) . . . . yes C(12) P C(15) C(20) 136.4(5) . . . . yes C(12) P C(21) C(22) -65.5(5) . . . . yes C(12) P C(21) C(26) 114.1(4) . . . . yes C(12) P C(27) C(28) 130.7(3) . . . . yes C(12) P C(27) C(32) -46.5(4) . . . . yes C(13) C(12) P C(15) -40.5(3) . . . . yes C(13) C(12) P C(21) 80.8(3) . . . . yes C(13) C(12) P C(27) -157.4(3) . . . . yes C(14) C(12) P C(15) -161.2(3) . . . . yes C(14) C(12) P C(21) -39.9(4) . . . . yes C(14) C(12) P C(27) 81.9(3) . . . . yes C(15) P C(21) C(22) 55.8(5) . . . . yes C(15) P C(21) C(26) -124.5(4) . . . . yes C(15) P C(27) C(28) 11.7(4) . . . . yes C(15) P C(27) C(32) -165.5(4) . . . . yes C(15) C(16) C(17) C(18) -0.2(9) . . . . yes C(15) C(20) C(19) C(18) 0(1) . . . . yes C(16) C(15) P C(21) -171.6(4) . . . . yes C(16) C(15) P C(27) 68.9(5) . . . . yes C(16) C(15) C(20) C(19) -0.5(9) . . . . yes C(16) C(17) C(18) C(19) 0(1) . . . . yes C(17) C(16) C(15) C(20) 0.4(8) . . . . yes C(17) C(18) C(19) C(20) 0(1) . . . . yes C(20) C(15) P C(21) 14.8(5) . . . . yes C(20) C(15) P C(27) -104.7(5) . . . . yes C(21) P C(27) C(28) -107.4(4) . . . . yes C(21) P C(27) C(32) 75.4(4) . . . . yes C(21) C(22) C(23) C(24) 0.3(10) . . . . yes C(21) C(26) C(25) C(24) -1.5(9) . . . . yes C(22) C(21) P C(27) 173.0(4) . . . . yes C(22) C(21) C(26) C(25) 2.2(8) . . . . yes C(22) C(23) C(24) C(25) 0(1) . . . . yes C(23) C(22) C(21) C(26) -1.6(8) . . . . yes C(23) C(24) C(25) C(26) 0.2(10) . . . . yes C(26) C(21) P C(27) -7.4(5) . . . . yes C(27) C(28) C(29) C(30) -0.1(8) . . . . yes C(27) C(32) C(31) C(30) -0.6(8) . . . . yes C(28) C(27) C(32) C(31) 0.9(7) . . . . yes C(28) C(29) C(30) C(31) 0.4(9) . . . . yes C(29) C(28) C(27) C(32) -0.5(7) . . . . yes C(29) C(30) C(31) C(32) 0.0(9) . . . . yes C(29) C(30) C(31) C(32) 0.0(9) . . . . yes #------------------------------------------------------------------------------ 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 O C(1) 3.583(8) . 3_756 ? N(5) C(8) 3.463(5) . 3_757 ? N(6) C(8) 3.525(6) . 3_757 ? N(6) C(30) 3.546(8) . 3_756 ? N(7) C(8) 3.473(6) . 3_757 ? C(1) F(4) 3.39(1) . 3_656 ? C(2) F(4) 3.34(1) . 3_656 ? C(5) F(2) 3.58(1) . 3_657 ? C(6) F(2) 3.43(1) . 3_657 ? C(6) C(25) 3.471(9) . 3_656 ? C(6) C(8) 3.575(6) . 3_757 ? C(7) C(9) 3.404(7) . 3_757 ? C(17) C(28) 3.596(8) . 4_545 ? C(18) C(26) 3.578(9) . 4_545 ? C(20) F(1) 3.36(1) . 4_544 ? C(22) F(1) 3.46(1) . 4_544 ? C(23) F(1) 3.55(1) . 4_544 ? C(24) F(3) 3.30(1) . 1_554 ? C(25) F(3) 3.17(1) . 1_554 ? C(31) F(2) 3.51(1) . 3_656 ? C(31) F(4) 3.59(1) . 3_656 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_0488a _database_code_depnum_ccdc_archive 'CCDC 252272' _audit_creation_date 'Fri Nov 28 10:29:12 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C42 H35 B2 Cl F4 N7 O P Ru ' _chemical_formula_moiety 'C42 H35 B Cl N7 O P Ru, B F4' _chemical_formula_weight 918.90 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 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 11.1299(5) _cell_length_b 21.586(2) _cell_length_c 17.4043(2) _cell_angle_alpha 90 _cell_angle_beta 91.2394(3) _cell_angle_gamma 90 _cell_volume 4180.4(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.538 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.649 _exptl_absorpt_correction_T_max 0.997 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Quantum CCD/Rigaku AFC7' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36362 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9652 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9652 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). Three fluorine atoms of BF4 anion were disordered with occupancy factors of 0.85 / 0.15. ; _reflns_number_total 9273 _reflns_number_gt 6047 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0904 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 9260 _refine_ls_number_parameters 544 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.02000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0005 _refine_diff_density_max 1.28 _refine_diff_density_min -0.75 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru Ru -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.24597(2) 0.10002(1) 0.31293(1) 0.03711(6) Uani 1.00 d . . . Cl Cl 0.29256(8) 0.14350(4) 0.43481(4) 0.0602(2) Uani 1.00 d . . . P P 0.01470(6) 0.20926(3) 0.32585(4) 0.0356(2) Uani 1.00 d . . . F(1) F -0.1130(2) -0.0273(1) 0.1047(2) 0.113(1) Uani 1.00 d . . . F(2) F -0.2005(5) 0.0579(2) 0.1529(3) 0.155(2) Uani 0.85 d P . . F(2a) F -0.237(2) 0.040(1) 0.102(2) 0.128(7) Uiso 0.15 d P . . F(3) F -0.3033(3) -0.0043(3) 0.0796(2) 0.131(1) Uani 0.85 d P . . F(3a) F -0.301(1) -0.0551(8) 0.133(1) 0.088(4) Uiso 0.15 d P . . F(4) F -0.2457(4) -0.0316(3) 0.1975(2) 0.162(2) Uani 0.85 d P . . F(4a) F -0.158(3) 0.008(2) 0.201(2) 0.159(9) Uiso 0.15 d P . . O O 0.0675(2) 0.0183(1) 0.3722(2) 0.0839(9) Uani 1.00 d . . . N(1) N 0.1314(2) 0.0550(1) 0.3490(1) 0.0492(7) Uani 1.00 d . . . N(2) N 0.2177(2) 0.0624(1) 0.2045(1) 0.0407(6) Uani 1.00 d . . . N(3) N 0.3121(2) 0.0422(1) 0.1635(1) 0.0489(7) Uani 1.00 d . . . N(4) N 0.3979(2) 0.1429(1) 0.2695(1) 0.0399(6) Uani 1.00 d . . . N(5) N 0.4698(2) 0.1104(1) 0.2210(1) 0.0446(7) Uani 1.00 d . . . N(6) N 0.3715(2) 0.0272(1) 0.3339(1) 0.0517(8) Uani 1.00 d . . . N(7) N 0.4399(2) 0.0070(1) 0.2751(2) 0.0516(8) Uani 1.00 d . . . C(1) C 0.1176(3) 0.0495(1) 0.1634(2) 0.0499(9) Uani 1.00 d . . . C(2) C 0.1485(3) 0.0215(2) 0.0952(2) 0.058(1) Uani 1.00 d . . . C(3) C 0.2711(4) 0.0179(2) 0.0969(2) 0.059(1) Uani 1.00 d . . . C(4) C 0.4526(3) 0.1969(1) 0.2851(2) 0.0453(8) Uani 1.00 d . . . C(5) C 0.5592(3) 0.1996(2) 0.2466(2) 0.0542(9) Uani 1.00 d . . . C(6) C 0.5684(3) 0.1450(2) 0.2077(2) 0.0532(9) Uani 1.00 d . . . C(7) C 0.4007(3) -0.0072(2) 0.3946(2) 0.068(1) Uani 1.00 d . . . C(8) C 0.4881(3) -0.0497(2) 0.3765(3) 0.079(1) Uani 1.00 d . . . C(9) C 0.5110(3) -0.0392(2) 0.3006(2) 0.067(1) Uani 1.00 d . . . C(10) C 0.1465(2) 0.1799(1) 0.2801(1) 0.0354(7) Uani 1.00 d . . . C(11) C 0.1789(2) 0.2150(1) 0.2228(1) 0.0368(7) Uani 1.00 d . . . C(12) C 0.2132(2) 0.2517(1) 0.1667(2) 0.0381(7) Uani 1.00 d . . . C(13) C 0.1775(2) 0.2400(1) 0.0850(2) 0.0428(8) Uani 1.00 d . . . C(14) C 0.1666(3) 0.1807(2) 0.0577(2) 0.059(1) Uani 1.00 d . . . C(15) C 0.1307(4) 0.1697(2) -0.0184(2) 0.074(1) Uani 1.00 d . . . C(16) C 0.1086(4) 0.2184(2) -0.0669(2) 0.073(1) Uani 1.00 d . . . C(17) C 0.1200(4) 0.2782(2) -0.0402(2) 0.070(1) Uani 1.00 d . . . C(18) C 0.1549(3) 0.2891(1) 0.0354(2) 0.0546(9) Uani 1.00 d . . . C(19) C 0.2907(3) 0.3060(1) 0.1855(2) 0.0414(8) Uani 1.00 d . . . C(20) C 0.4005(3) 0.3134(2) 0.1507(2) 0.0563(10) Uani 1.00 d . . . C(21) C 0.4768(3) 0.3606(2) 0.1737(3) 0.076(1) Uani 1.00 d . . . C(22) C 0.4449(5) 0.4004(2) 0.2312(3) 0.090(2) Uani 1.00 d . . . C(23) C 0.3339(6) 0.3951(2) 0.2627(3) 0.100(2) Uani 1.00 d . . . C(24) C 0.2576(4) 0.3485(2) 0.2402(2) 0.072(1) Uani 1.00 d . . . C(25) C -0.0772(2) 0.2467(1) 0.2523(2) 0.0393(7) Uani 1.00 d . . . C(26) C -0.0894(3) 0.2188(2) 0.1803(2) 0.0537(9) Uani 1.00 d . . . C(27) C -0.1563(3) 0.2479(2) 0.1227(2) 0.070(1) Uani 1.00 d . . . C(28) C -0.2105(3) 0.3036(2) 0.1365(2) 0.070(1) Uani 1.00 d . . . C(29) C -0.2011(3) 0.3307(2) 0.2071(2) 0.063(1) Uani 1.00 d . . . C(30) C -0.1336(3) 0.3030(1) 0.2652(2) 0.0486(9) Uani 1.00 d . . . C(31) C 0.0509(3) 0.2656(1) 0.3991(1) 0.0421(8) Uani 1.00 d . . . C(32) C 0.1661(3) 0.2903(1) 0.4051(2) 0.0538(9) Uani 1.00 d . . . C(33) C 0.1881(4) 0.3391(2) 0.4556(2) 0.069(1) Uani 1.00 d . . . C(34) C 0.0981(4) 0.3624(2) 0.4994(2) 0.075(1) Uani 1.00 d . . . C(35) C -0.0142(4) 0.3369(2) 0.4954(2) 0.078(1) Uani 1.00 d . . . C(36) C -0.0392(3) 0.2885(2) 0.4458(2) 0.059(1) Uani 1.00 d . . . C(37) C -0.0725(2) 0.1488(1) 0.3688(2) 0.0413(8) Uani 1.00 d . . . C(38) C -0.0578(3) 0.1346(2) 0.4461(2) 0.0573(10) Uani 1.00 d . . . C(39) C -0.1239(4) 0.0864(2) 0.4765(2) 0.080(1) Uani 1.00 d . . . C(40) C -0.2003(4) 0.0527(2) 0.4314(3) 0.090(2) Uani 1.00 d . . . C(41) C -0.2155(4) 0.0664(2) 0.3551(2) 0.083(1) Uani 1.00 d . . . C(42) C -0.1526(3) 0.1145(2) 0.3235(2) 0.061(1) Uani 1.00 d . . . B(1) B 0.4402(3) 0.0434(2) 0.1991(2) 0.052(1) Uani 1.00 d . . . B(2) B -0.2144(4) -0.0038(3) 0.1334(3) 0.074(2) Uani 1.00 d . . . H(1) H 0.5123 0.0243 0.1508 0.0666 Uiso 1.00 calc . . . H(2) H 0.0363 0.0584 0.1790 0.0599 Uiso 1.00 calc . . . H(3) H 0.0943 0.0073 0.0545 0.0701 Uiso 1.00 calc . . . H(4) H 0.3203 0.0006 0.0568 0.0708 Uiso 1.00 calc . . . H(5) H 0.4219 0.2290 0.3184 0.0543 Uiso 1.00 calc . . . H(6) H 0.6163 0.2336 0.2471 0.0650 Uiso 1.00 calc . . . H(7) H 0.6348 0.1330 0.1757 0.0639 Uiso 1.00 calc . . . H(8) H 0.3655 -0.0030 0.4448 0.0815 Uiso 1.00 calc . . . H(9) H 0.5252 -0.0803 0.4102 0.0942 Uiso 1.00 calc . . . H(10) H 0.5689 -0.0616 0.2703 0.0809 Uiso 1.00 calc . . . H(11) H 0.1840 0.1460 0.0916 0.0710 Uiso 1.00 calc . . . H(12) H 0.1213 0.1275 -0.0368 0.0889 Uiso 1.00 calc . . . H(13) H 0.0849 0.2108 -0.1200 0.0877 Uiso 1.00 calc . . . H(14) H 0.1036 0.3127 -0.0744 0.0841 Uiso 1.00 calc . . . H(15) H 0.1636 0.3313 0.0538 0.0656 Uiso 1.00 calc . . . H(16) H 0.4238 0.2853 0.1101 0.0676 Uiso 1.00 calc . . . H(17) H 0.5535 0.3656 0.1491 0.0917 Uiso 1.00 calc . . . H(18) H 0.5005 0.4320 0.2493 0.1085 Uiso 1.00 calc . . . H(19) H 0.3091 0.4247 0.3013 0.1205 Uiso 1.00 calc . . . H(20) H 0.1791 0.3454 0.2631 0.0867 Uiso 1.00 calc . . . H(21) H -0.0514 0.1792 0.1705 0.0645 Uiso 1.00 calc . . . H(22) H -0.1646 0.2288 0.0725 0.0835 Uiso 1.00 calc . . . H(23) H -0.2561 0.3239 0.0957 0.0842 Uiso 1.00 calc . . . H(24) H -0.2420 0.3695 0.2166 0.0755 Uiso 1.00 calc . . . H(25) H -0.1256 0.3229 0.3150 0.0583 Uiso 1.00 calc . . . H(26) H 0.2303 0.2737 0.3744 0.0646 Uiso 1.00 calc . . . H(27) H 0.2680 0.3568 0.4598 0.0826 Uiso 1.00 calc . . . H(28) H 0.1141 0.3971 0.5335 0.0905 Uiso 1.00 calc . . . H(29) H -0.0770 0.3531 0.5276 0.0931 Uiso 1.00 calc . . . H(30) H -0.1190 0.2704 0.4435 0.0707 Uiso 1.00 calc . . . H(31) H -0.0020 0.1580 0.4784 0.0688 Uiso 1.00 calc . . . H(32) H -0.1154 0.0766 0.5308 0.0965 Uiso 1.00 calc . . . H(33) H -0.2446 0.0186 0.4535 0.1074 Uiso 1.00 calc . . . H(34) H -0.2705 0.0421 0.3232 0.0991 Uiso 1.00 calc . . . H(35) H -0.1642 0.1246 0.2696 0.0728 Uiso 1.00 calc . . . 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 Ru 0.0426(1) 0.0404(1) 0.0286(1) 0.0014(1) 0.00725(8) 0.0035(1) Cl 0.0753(5) 0.0754(6) 0.0298(3) 0.0077(4) 0.0003(3) -0.0055(4) P 0.0412(4) 0.0386(4) 0.0272(3) -0.0024(3) 0.0057(3) -0.0018(3) F(1) 0.069(1) 0.129(2) 0.141(2) 0.007(1) 0.023(1) -0.050(2) F(2) 0.200(4) 0.104(3) 0.161(4) 0.036(3) -0.002(3) -0.061(3) F(3) 0.086(2) 0.235(5) 0.072(2) 0.030(3) -0.013(2) -0.025(3) F(4) 0.153(4) 0.230(5) 0.104(3) 0.028(4) 0.042(3) 0.075(3) O 0.089(2) 0.049(1) 0.115(2) -0.006(1) 0.049(2) 0.020(1) N(1) 0.059(2) 0.039(1) 0.050(1) 0.001(1) 0.017(1) 0.007(1) N(2) 0.049(1) 0.038(1) 0.036(1) -0.001(1) 0.005(1) -0.0021(10) N(3) 0.059(2) 0.048(2) 0.040(1) -0.003(1) 0.012(1) -0.011(1) N(4) 0.040(1) 0.045(1) 0.035(1) -0.001(1) 0.0051(10) 0.000(1) N(5) 0.044(1) 0.054(2) 0.037(1) -0.002(1) 0.013(1) 0.000(1) N(6) 0.052(1) 0.055(2) 0.049(1) 0.008(1) 0.010(1) 0.013(1) N(7) 0.048(1) 0.048(2) 0.059(2) 0.010(1) 0.013(1) 0.001(1) C(1) 0.059(2) 0.040(2) 0.050(2) -0.008(1) -0.006(2) 0.001(1) C(2) 0.079(2) 0.050(2) 0.046(2) -0.013(2) -0.008(2) -0.004(1) C(3) 0.092(3) 0.047(2) 0.039(2) -0.007(2) 0.010(2) -0.009(1) C(4) 0.045(2) 0.047(2) 0.043(2) -0.001(1) -0.001(1) 0.002(1) C(5) 0.046(2) 0.063(2) 0.054(2) -0.013(2) 0.003(1) 0.005(2) C(6) 0.041(2) 0.076(2) 0.044(2) -0.005(2) 0.010(1) 0.007(2) C(7) 0.066(2) 0.074(3) 0.065(2) 0.013(2) 0.011(2) 0.028(2) C(8) 0.070(2) 0.065(3) 0.101(3) 0.018(2) 0.005(2) 0.032(2) C(9) 0.055(2) 0.050(2) 0.097(3) 0.013(2) 0.011(2) 0.008(2) C(10) 0.040(1) 0.039(2) 0.027(1) -0.002(1) 0.005(1) -0.002(1) C(11) 0.036(1) 0.042(2) 0.032(1) 0.003(1) 0.005(1) 0.000(1) C(12) 0.043(1) 0.034(1) 0.038(1) 0.006(1) 0.010(1) 0.008(1) C(13) 0.046(2) 0.048(2) 0.035(1) 0.001(1) 0.011(1) 0.007(1) C(14) 0.090(3) 0.048(2) 0.040(2) -0.002(2) 0.009(2) 0.004(1) C(15) 0.113(3) 0.055(2) 0.054(2) -0.004(2) 0.002(2) -0.007(2) C(16) 0.098(3) 0.078(3) 0.042(2) 0.003(2) -0.013(2) 0.002(2) C(17) 0.094(3) 0.065(2) 0.051(2) 0.008(2) -0.014(2) 0.016(2) C(18) 0.069(2) 0.048(2) 0.048(2) 0.004(2) -0.003(2) 0.011(1) C(19) 0.051(2) 0.036(2) 0.037(1) 0.003(1) 0.007(1) 0.009(1) C(20) 0.052(2) 0.055(2) 0.062(2) -0.001(2) 0.007(2) 0.007(2) C(21) 0.054(2) 0.071(3) 0.105(3) -0.012(2) -0.004(2) 0.025(2) C(22) 0.116(4) 0.054(2) 0.100(3) -0.026(3) -0.030(3) 0.003(2) C(23) 0.162(5) 0.053(3) 0.088(3) -0.027(3) 0.028(3) -0.019(2) C(24) 0.102(3) 0.041(2) 0.075(2) -0.005(2) 0.032(2) -0.005(2) C(25) 0.036(1) 0.046(2) 0.036(1) -0.005(1) 0.006(1) 0.003(1) C(26) 0.051(2) 0.073(2) 0.038(2) 0.000(2) 0.001(1) -0.006(1) C(27) 0.057(2) 0.112(3) 0.039(2) -0.003(2) -0.003(2) 0.002(2) C(28) 0.051(2) 0.100(3) 0.060(2) -0.003(2) -0.007(2) 0.030(2) C(29) 0.048(2) 0.058(2) 0.083(3) -0.001(2) -0.006(2) 0.019(2) C(30) 0.044(2) 0.048(2) 0.054(2) -0.004(1) -0.001(1) 0.000(1) C(31) 0.056(2) 0.038(2) 0.032(1) -0.002(1) 0.000(1) -0.002(1) C(32) 0.061(2) 0.049(2) 0.050(2) -0.003(2) -0.005(2) -0.001(1) C(33) 0.086(3) 0.060(2) 0.059(2) -0.020(2) -0.020(2) -0.001(2) C(34) 0.127(4) 0.056(2) 0.043(2) -0.021(2) 0.001(2) -0.012(2) C(35) 0.114(3) 0.067(3) 0.053(2) -0.010(2) 0.027(2) -0.025(2) C(36) 0.075(2) 0.055(2) 0.048(2) -0.010(2) 0.015(2) -0.011(2) C(37) 0.046(2) 0.041(2) 0.038(1) -0.001(1) 0.017(1) -0.003(1) C(38) 0.085(2) 0.049(2) 0.039(2) -0.008(2) 0.018(2) -0.001(1) C(39) 0.131(4) 0.066(3) 0.045(2) -0.018(2) 0.034(2) 0.005(2) C(40) 0.113(3) 0.071(3) 0.086(3) -0.038(3) 0.052(3) 0.001(2) C(41) 0.085(3) 0.084(3) 0.080(3) -0.041(2) 0.020(2) -0.007(2) C(42) 0.060(2) 0.068(2) 0.055(2) -0.018(2) 0.008(2) -0.001(2) B(1) 0.056(2) 0.053(2) 0.048(2) 0.002(2) 0.013(2) -0.005(2) B(2) 0.067(3) 0.100(4) 0.055(2) 0.015(3) 0.004(2) -0.012(3) #------------------------------------------------------------------------------ _computing_data_collection D*TREK _computing_cell_refinement D*TREK _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru Cl 2.3669(7) . . yes Ru N(1) 1.732(3) . . yes Ru N(2) 2.071(2) . . yes Ru N(4) 2.084(2) . . yes Ru N(6) 2.130(2) . . yes Ru C(10) 2.121(3) . . yes P C(10) 1.799(3) . . yes P C(25) 1.811(3) . . yes P C(31) 1.801(3) . . yes P C(37) 1.798(3) . . yes F(1) B(2) 1.343(5) . . yes F(2) F(2a) 1.04(3) . . yes F(2) F(4a) 1.44(3) . . yes F(2) B(2) 1.382(7) . . yes F(2a) F(3) 1.26(3) . . yes F(2a) B(2) 1.12(3) . . yes F(3) F(3a) 1.44(2) . . yes F(3) B(2) 1.347(5) . . yes F(3a) F(4) 1.36(2) . . yes F(3a) B(2) 1.47(2) . . yes F(4) F(4a) 1.30(3) . . yes F(4) B(2) 1.321(6) . . yes F(4a) B(2) 1.35(3) . . yes O N(1) 1.144(3) . . yes N(2) N(3) 1.356(3) . . yes N(2) C(1) 1.341(3) . . yes N(3) C(3) 1.343(4) . . yes N(3) B(1) 1.542(4) . . yes N(4) N(5) 1.369(3) . . yes N(4) C(4) 1.341(4) . . yes N(5) C(6) 1.352(4) . . yes N(5) B(1) 1.529(4) . . yes N(6) N(7) 1.360(3) . . yes N(6) C(7) 1.325(4) . . yes N(7) C(9) 1.343(4) . . yes N(7) B(1) 1.539(4) . . yes C(1) C(2) 1.383(4) . . yes C(2) C(3) 1.367(5) . . yes C(4) C(5) 1.376(4) . . yes C(5) C(6) 1.365(5) . . yes C(7) C(8) 1.378(5) . . yes C(8) C(9) 1.369(6) . . yes C(10) C(11) 1.309(4) . . yes C(11) C(12) 1.320(4) . . yes C(12) C(13) 1.490(4) . . yes C(12) C(19) 1.487(4) . . yes C(13) C(14) 1.371(4) . . yes C(13) C(18) 1.387(4) . . yes C(14) C(15) 1.395(4) . . yes C(15) C(16) 1.367(5) . . yes C(16) C(17) 1.377(5) . . yes C(17) C(18) 1.384(4) . . yes C(19) C(20) 1.385(4) . . yes C(19) C(24) 1.379(4) . . yes C(20) C(21) 1.380(5) . . yes C(21) C(22) 1.371(6) . . yes C(22) C(23) 1.367(7) . . yes C(23) C(24) 1.368(6) . . yes C(25) C(26) 1.395(4) . . yes C(25) C(30) 1.388(4) . . yes C(26) C(27) 1.386(4) . . yes C(27) C(28) 1.368(6) . . yes C(28) C(29) 1.362(5) . . yes C(29) C(30) 1.384(4) . . yes C(31) C(32) 1.390(4) . . yes C(31) C(36) 1.394(4) . . yes C(32) C(33) 1.391(4) . . yes C(33) C(34) 1.367(6) . . yes C(34) C(35) 1.365(6) . . yes C(35) C(36) 1.380(4) . . yes C(37) C(38) 1.386(4) . . yes C(37) C(42) 1.391(4) . . yes C(38) C(39) 1.386(5) . . yes C(39) C(40) 1.357(6) . . yes C(40) C(41) 1.369(6) . . yes C(41) C(42) 1.374(5) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl Ru N(1) 92.64(9) . . . yes Cl Ru N(2) 176.02(7) . . . yes Cl Ru N(4) 89.15(6) . . . yes Cl Ru N(6) 90.52(7) . . . yes Cl Ru C(10) 91.27(7) . . . yes N(1) Ru N(2) 90.7(1) . . . yes N(1) Ru N(4) 172.0(1) . . . yes N(1) Ru N(6) 90.5(1) . . . yes N(1) Ru C(10) 99.8(1) . . . yes N(2) Ru N(4) 87.24(9) . . . yes N(2) Ru N(6) 87.29(9) . . . yes N(2) Ru C(10) 90.29(9) . . . yes N(4) Ru N(6) 81.69(9) . . . yes N(4) Ru C(10) 87.97(9) . . . yes N(6) Ru C(10) 169.48(10) . . . yes C(10) P C(25) 107.3(1) . . . yes C(10) P C(31) 112.3(1) . . . yes C(10) P C(37) 112.4(1) . . . yes C(25) P C(31) 108.3(1) . . . yes C(25) P C(37) 108.4(1) . . . yes C(31) P C(37) 108.0(1) . . . yes F(2a) F(2) F(4a) 109(2) . . . yes F(2a) F(2) B(2) 52(1) . . . yes F(4a) F(2) B(2) 57(1) . . . yes F(2) F(2a) F(3) 139(2) . . . yes F(2) F(2a) B(2) 79(2) . . . yes F(3) F(2a) B(2) 68(1) . . . yes F(2a) F(3) F(3a) 111(1) . . . yes F(2a) F(3) B(2) 50(1) . . . yes F(3a) F(3) B(2) 63.5(7) . . . yes F(3) F(3a) F(4) 104(1) . . . yes F(3) F(3a) B(2) 55.2(7) . . . yes F(4) F(3a) B(2) 55.5(7) . . . yes F(3a) F(4) F(4a) 127(1) . . . yes F(3a) F(4) B(2) 66.4(8) . . . yes F(4a) F(4) B(2) 62(1) . . . yes F(2) F(4a) F(4) 103(1) . . . yes F(2) F(4a) B(2) 59(1) . . . yes F(4) F(4a) B(2) 59(1) . . . yes Ru N(1) O 169.9(2) . . . yes Ru N(2) N(3) 120.2(2) . . . yes Ru N(2) C(1) 132.5(2) . . . yes N(3) N(2) C(1) 107.2(2) . . . yes N(2) N(3) C(3) 109.2(3) . . . yes N(2) N(3) B(1) 120.1(2) . . . yes C(3) N(3) B(1) 130.4(3) . . . yes Ru N(4) N(5) 119.1(2) . . . yes Ru N(4) C(4) 132.9(2) . . . yes N(5) N(4) C(4) 107.6(2) . . . yes N(4) N(5) C(6) 108.1(2) . . . yes N(4) N(5) B(1) 120.8(2) . . . yes C(6) N(5) B(1) 130.6(3) . . . yes Ru N(6) N(7) 118.9(2) . . . yes Ru N(6) C(7) 134.3(2) . . . yes N(7) N(6) C(7) 106.8(3) . . . yes N(6) N(7) C(9) 108.9(3) . . . yes N(6) N(7) B(1) 119.6(2) . . . yes C(9) N(7) B(1) 130.7(3) . . . yes N(2) C(1) C(2) 109.3(3) . . . yes C(1) C(2) C(3) 105.9(3) . . . yes N(3) C(3) C(2) 108.5(3) . . . yes N(4) C(4) C(5) 109.3(3) . . . yes C(4) C(5) C(6) 106.2(3) . . . yes N(5) C(6) C(5) 108.8(3) . . . yes N(6) C(7) C(8) 110.7(3) . . . yes C(7) C(8) C(9) 104.9(3) . . . yes N(7) C(9) C(8) 108.7(3) . . . yes Ru C(10) P 126.4(1) . . . yes Ru C(10) C(11) 121.7(2) . . . yes P C(10) C(11) 112.0(2) . . . yes C(10) C(11) C(12) 178.1(3) . . . yes C(11) C(12) C(13) 121.9(3) . . . yes C(11) C(12) C(19) 119.1(2) . . . yes C(13) C(12) C(19) 119.0(2) . . . yes C(12) C(13) C(14) 120.6(3) . . . yes C(12) C(13) C(18) 120.4(3) . . . yes C(14) C(13) C(18) 119.0(3) . . . yes C(13) C(14) C(15) 120.6(3) . . . yes C(14) C(15) C(16) 120.0(3) . . . yes C(15) C(16) C(17) 119.8(3) . . . yes C(16) C(17) C(18) 120.2(3) . . . yes C(13) C(18) C(17) 120.3(3) . . . yes C(12) C(19) C(20) 120.5(3) . . . yes C(12) C(19) C(24) 120.9(3) . . . yes C(20) C(19) C(24) 118.5(3) . . . yes C(19) C(20) C(21) 120.1(3) . . . yes C(20) C(21) C(22) 120.4(4) . . . yes C(21) C(22) C(23) 119.5(4) . . . yes C(22) C(23) C(24) 120.5(4) . . . yes C(19) C(24) C(23) 120.9(4) . . . yes P C(25) C(26) 119.0(2) . . . yes P C(25) C(30) 121.8(2) . . . yes C(26) C(25) C(30) 119.2(3) . . . yes C(25) C(26) C(27) 119.6(3) . . . yes C(26) C(27) C(28) 120.3(3) . . . yes C(27) C(28) C(29) 120.7(3) . . . yes C(28) C(29) C(30) 120.2(3) . . . yes C(25) C(30) C(29) 120.0(3) . . . yes P C(31) C(32) 120.3(2) . . . yes P C(31) C(36) 119.9(2) . . . yes C(32) C(31) C(36) 119.6(3) . . . yes C(31) C(32) C(33) 119.2(3) . . . yes C(32) C(33) C(34) 120.6(3) . . . yes C(33) C(34) C(35) 120.3(3) . . . yes C(34) C(35) C(36) 120.6(4) . . . yes C(31) C(36) C(35) 119.7(3) . . . yes P C(37) C(38) 120.8(2) . . . yes P C(37) C(42) 119.7(2) . . . yes C(38) C(37) C(42) 119.5(3) . . . yes C(37) C(38) C(39) 119.0(3) . . . yes C(38) C(39) C(40) 120.9(3) . . . yes C(39) C(40) C(41) 120.5(3) . . . yes C(40) C(41) C(42) 119.9(4) . . . yes C(37) C(42) C(41) 120.1(3) . . . yes N(3) B(1) N(5) 108.0(3) . . . yes N(3) B(1) N(7) 108.5(3) . . . yes N(5) B(1) N(7) 105.9(3) . . . yes F(1) B(2) F(2) 111.4(5) . . . yes F(1) B(2) F(2a) 108(1) . . . yes F(1) B(2) F(3) 110.5(4) . . . yes F(1) B(2) F(3a) 105.9(8) . . . yes F(1) B(2) F(4) 112.5(5) . . . yes F(1) B(2) F(4a) 91(1) . . . yes F(2) B(2) F(2a) 47(1) . . . yes F(2) B(2) F(3) 104.8(5) . . . yes F(2) B(2) F(3a) 142.7(8) . . . yes F(2) B(2) F(4) 105.1(5) . . . yes F(2) B(2) F(4a) 63(1) . . . yes F(2a) B(2) F(3) 60(1) . . . yes F(2a) B(2) F(3a) 119(1) . . . yes F(2a) B(2) F(4) 137(1) . . . yes F(2a) B(2) F(4a) 111(2) . . . yes F(3) B(2) F(3a) 61.4(7) . . . yes F(3) B(2) F(4) 112.3(5) . . . yes F(3) B(2) F(4a) 158(1) . . . yes F(3a) B(2) F(4) 58.1(8) . . . yes F(3a) B(2) F(4a) 115(1) . . . yes F(4) B(2) F(4a) 58(1) . . . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ru N(2) N(3) C(3) 177.7(2) . . . . yes Ru N(2) N(3) B(1) 3.6(3) . . . . yes Ru N(2) C(1) C(2) -176.8(2) . . . . yes Ru N(4) N(5) C(6) -173.2(2) . . . . yes Ru N(4) N(5) B(1) -0.4(3) . . . . yes Ru N(4) C(4) C(5) 172.5(2) . . . . yes Ru N(6) N(7) C(9) -179.2(2) . . . . yes Ru N(6) N(7) B(1) 9.7(3) . . . . yes Ru N(6) C(7) C(8) 178.7(3) . . . . yes Ru C(10) P C(25) -149.2(1) . . . . yes Ru C(10) P C(31) 91.9(2) . . . . yes Ru C(10) P C(37) -30.1(2) . . . . yes Ru C(10) C(11) C(12) -100(8) . . . . yes Cl Ru N(1) O -103(1) . . . . yes Cl Ru N(2) N(3) 14(1) . . . . yes Cl Ru N(2) C(1) -170.1(8) . . . . yes Cl Ru N(4) N(5) 137.4(2) . . . . yes Cl Ru N(4) C(4) -34.0(2) . . . . yes Cl Ru N(6) N(7) -141.1(2) . . . . yes Cl Ru N(6) C(7) 40.5(3) . . . . yes Cl Ru C(10) P -61.5(1) . . . . yes Cl Ru C(10) C(11) 116.7(2) . . . . yes P C(10) Ru N(1) 31.4(2) . . . . yes P C(10) Ru N(2) 122.2(2) . . . . yes P C(10) Ru N(4) -150.6(2) . . . . yes P C(10) Ru N(6) -161.2(4) . . . . yes P C(10) C(11) C(12) 78(8) . . . . yes P C(25) C(26) C(27) -177.9(3) . . . . yes P C(25) C(30) C(29) 178.8(2) . . . . yes P C(31) C(32) C(33) 172.1(2) . . . . yes P C(31) C(36) C(35) -172.1(3) . . . . yes P C(37) C(38) C(39) -177.9(3) . . . . yes P C(37) C(42) C(41) 176.9(3) . . . . yes F(1) B(2) F(2) F(2a) 96(1) . . . . yes F(1) B(2) F(2) F(4a) -80(1) . . . . yes F(1) B(2) F(2a) F(2) -102(1) . . . . yes F(1) B(2) F(2a) F(3) 103.4(9) . . . . yes F(1) B(2) F(3) F(2a) -100(1) . . . . yes F(1) B(2) F(3) F(3a) 97.4(9) . . . . yes F(1) B(2) F(3a) F(3) -105.0(5) . . . . yes F(1) B(2) F(3a) F(4) 106.9(6) . . . . yes F(1) B(2) F(4) F(3a) -95.3(9) . . . . yes F(1) B(2) F(4) F(4a) 76(1) . . . . yes F(1) B(2) F(4a) F(2) 113.4(8) . . . . yes F(1) B(2) F(4a) F(4) -115.9(9) . . . . yes F(2) F(2a) F(3) F(3a) -23(4) . . . . yes F(2) F(2a) F(3) B(2) -40(3) . . . . yes F(2) F(2a) B(2) F(3) 154(2) . . . . yes F(2) F(2a) B(2) F(3a) 136(1) . . . . yes F(2) F(2a) B(2) F(4) 62(2) . . . . yes F(2) F(2a) B(2) F(4a) -3(2) . . . . yes F(2) F(4a) F(4) F(3a) 51(2) . . . . yes F(2) F(4a) F(4) B(2) 42(1) . . . . yes F(2) F(4a) B(2) F(2a) 2(1) . . . . yes F(2) F(4a) B(2) F(3) -60(4) . . . . yes F(2) F(4a) B(2) F(3a) -138.2(10) . . . . yes F(2) F(4a) B(2) F(4) -130(1) . . . . yes F(2) B(2) F(2a) F(3) -154(2) . . . . yes F(2) B(2) F(3) F(2a) 19(1) . . . . yes F(2) B(2) F(3) F(3a) -142.5(9) . . . . yes F(2) B(2) F(3a) F(3) 76(1) . . . . yes F(2) B(2) F(3a) F(4) -71(1) . . . . yes F(2) B(2) F(4) F(3a) 143.4(9) . . . . yes F(2) B(2) F(4) F(4a) -44(1) . . . . yes F(2) B(2) F(4a) F(4) 130(1) . . . . yes F(2a) F(2) F(4a) F(4) -45(2) . . . . yes F(2a) F(2) F(4a) B(2) -2(2) . . . . yes F(2a) F(2) B(2) F(3) -22(1) . . . . yes F(2a) F(2) B(2) F(3a) -84(2) . . . . yes F(2a) F(2) B(2) F(4) -141(1) . . . . yes F(2a) F(2) B(2) F(4a) 176(2) . . . . yes F(2a) F(3) F(3a) F(4) 11(1) . . . . yes F(2a) F(3) F(3a) B(2) -15(1) . . . . yes F(2a) F(3) B(2) F(3a) 161(1) . . . . yes F(2a) F(3) B(2) F(4) 132(1) . . . . yes F(2a) F(3) B(2) F(4a) 73(4) . . . . yes F(2a) B(2) F(2) F(4a) -176(2) . . . . yes F(2a) B(2) F(3) F(3a) -161(1) . . . . yes F(2a) B(2) F(3a) F(3) 18(1) . . . . yes F(2a) B(2) F(3a) F(4) -129(1) . . . . yes F(2a) B(2) F(4) F(3a) 100(2) . . . . yes F(2a) B(2) F(4) F(4a) -87(2) . . . . yes F(2a) B(2) F(4a) F(4) 133(1) . . . . yes F(3) F(2a) F(2) F(4a) 41(4) . . . . yes F(3) F(2a) F(2) B(2) 38(3) . . . . yes F(3) F(2a) B(2) F(3a) -18(1) . . . . yes F(3) F(2a) B(2) F(4) -92(2) . . . . yes F(3) F(2a) B(2) F(4a) -157(1) . . . . yes F(3) F(3a) F(4) F(4a) -35(2) . . . . yes F(3) F(3a) F(4) B(2) -26.6(7) . . . . yes F(3) F(3a) B(2) F(4) 148.1(8) . . . . yes F(3) F(3a) B(2) F(4a) 155(1) . . . . yes F(3) B(2) F(2) F(4a) 160(1) . . . . yes F(3) B(2) F(3a) F(4) -148.1(8) . . . . yes F(3) B(2) F(4) F(3a) 30.1(9) . . . . yes F(3) B(2) F(4) F(4a) -157(1) . . . . yes F(3) B(2) F(4a) F(4) 69(4) . . . . yes F(3a) F(3) F(2a) B(2) 17(1) . . . . yes F(3a) F(3) B(2) F(4) -29.0(9) . . . . yes F(3a) F(3) B(2) F(4a) -88(4) . . . . yes F(3a) F(4) F(4a) B(2) 9(2) . . . . yes F(3a) F(4) B(2) F(4a) -171(1) . . . . yes F(3a) B(2) F(2) F(4a) 98(2) . . . . yes F(3a) B(2) F(4) F(4a) 171(1) . . . . yes F(3a) B(2) F(4a) F(4) -7(1) . . . . yes F(4) F(3a) F(3) B(2) 26.7(7) . . . . yes F(4) F(3a) B(2) F(4a) 7(1) . . . . yes F(4) F(4a) F(2) B(2) -42(1) . . . . yes F(4) B(2) F(2) F(4a) 41(1) . . . . yes F(4a) F(2) F(2a) B(2) 2(2) . . . . yes F(4a) F(4) F(3a) B(2) -8(1) . . . . yes O N(1) Ru N(2) 74(1) . . . . yes O N(1) Ru N(4) 0(2) . . . . yes O N(1) Ru N(6) -12(1) . . . . yes O N(1) Ru C(10) 165(1) . . . . yes N(1) Ru N(2) N(3) -132.9(2) . . . . yes N(1) Ru N(2) C(1) 42.7(3) . . . . yes N(1) Ru N(4) N(5) 34.3(8) . . . . yes N(1) Ru N(4) C(4) -137.1(7) . . . . yes N(1) Ru N(6) N(7) 126.2(2) . . . . yes N(1) Ru N(6) C(7) -52.1(3) . . . . yes N(1) Ru C(10) C(11) -150.4(2) . . . . yes N(2) Ru N(4) N(5) -40.9(2) . . . . yes N(2) Ru N(4) C(4) 147.6(2) . . . . yes N(2) Ru N(6) N(7) 35.6(2) . . . . yes N(2) Ru N(6) C(7) -142.8(3) . . . . yes N(2) Ru C(10) C(11) -59.7(2) . . . . yes N(2) N(3) C(3) C(2) -1.0(4) . . . . yes N(2) N(3) B(1) N(5) -58.7(4) . . . . yes N(2) N(3) B(1) N(7) 55.6(4) . . . . yes N(2) C(1) C(2) C(3) 0.2(4) . . . . yes N(3) N(2) Ru N(4) 39.4(2) . . . . yes N(3) N(2) Ru N(6) -42.4(2) . . . . yes N(3) N(2) Ru C(10) 127.3(2) . . . . yes N(3) N(2) C(1) C(2) -0.7(3) . . . . yes N(3) C(3) C(2) C(1) 0.5(4) . . . . yes N(3) B(1) N(5) N(4) 56.7(3) . . . . yes N(3) B(1) N(5) C(6) -132.4(3) . . . . yes N(3) B(1) N(7) N(6) -62.8(4) . . . . yes N(3) B(1) N(7) C(9) 128.3(3) . . . . yes N(4) Ru N(2) C(1) -145.0(3) . . . . yes N(4) Ru N(6) N(7) -52.0(2) . . . . yes N(4) Ru N(6) C(7) 129.6(3) . . . . yes N(4) Ru C(10) C(11) 27.6(2) . . . . yes N(4) N(5) C(6) C(5) -0.7(3) . . . . yes N(4) N(5) B(1) N(7) -59.4(3) . . . . yes N(4) C(4) C(5) C(6) -0.8(3) . . . . yes N(5) N(4) Ru N(6) 46.8(2) . . . . yes N(5) N(4) Ru C(10) -131.3(2) . . . . yes N(5) N(4) C(4) C(5) 0.3(3) . . . . yes N(5) C(6) C(5) C(4) 0.9(4) . . . . yes N(5) B(1) N(3) C(3) 128.5(3) . . . . yes N(5) B(1) N(7) N(6) 52.9(3) . . . . yes N(5) B(1) N(7) C(9) -116.0(4) . . . . yes N(6) Ru N(2) C(1) 133.2(3) . . . . yes N(6) Ru N(4) C(4) -124.7(3) . . . . yes N(6) Ru C(10) C(11) 16.9(7) . . . . yes N(6) N(7) C(9) C(8) 0.5(4) . . . . yes N(6) C(7) C(8) C(9) 0.1(5) . . . . yes N(7) N(6) Ru C(10) -41.3(6) . . . . yes N(7) N(6) C(7) C(8) 0.2(4) . . . . yes N(7) C(9) C(8) C(7) -0.4(5) . . . . yes N(7) B(1) N(3) C(3) -117.1(3) . . . . yes N(7) B(1) N(5) C(6) 111.6(3) . . . . yes C(1) N(2) Ru C(10) -57.0(3) . . . . yes C(1) N(2) N(3) C(3) 1.1(3) . . . . yes C(1) N(2) N(3) B(1) -173.1(3) . . . . yes C(2) C(3) N(3) B(1) 172.4(3) . . . . yes C(4) N(4) Ru C(10) 57.3(2) . . . . yes C(4) N(4) N(5) C(6) 0.2(3) . . . . yes C(4) N(4) N(5) B(1) 173.0(3) . . . . yes C(5) C(6) N(5) B(1) -172.6(3) . . . . yes C(7) N(6) Ru C(10) 140.3(5) . . . . yes C(7) N(6) N(7) C(9) -0.4(4) . . . . yes C(7) N(6) N(7) B(1) -171.5(3) . . . . yes C(8) C(9) N(7) B(1) 170.3(3) . . . . yes C(10) P C(25) C(26) 41.1(3) . . . . yes C(10) P C(25) C(30) -137.6(2) . . . . yes C(10) P C(31) C(32) 12.1(3) . . . . yes C(10) P C(31) C(36) -173.5(2) . . . . yes C(10) P C(37) C(38) 95.5(3) . . . . yes C(10) P C(37) C(42) -82.2(3) . . . . yes C(10) C(11) C(12) C(13) -173(8) . . . . yes C(10) C(11) C(12) C(19) 7(8) . . . . yes C(11) C(10) P C(25) 32.5(2) . . . . yes C(11) C(10) P C(31) -86.3(2) . . . . yes C(11) C(10) P C(37) 151.6(2) . . . . yes C(11) C(12) C(13) C(14) -34.9(4) . . . . yes C(11) C(12) C(13) C(18) 145.1(3) . . . . yes C(11) C(12) C(19) C(20) 123.7(3) . . . . yes C(11) C(12) C(19) C(24) -53.4(4) . . . . yes C(12) C(13) C(14) C(15) 178.6(3) . . . . yes C(12) C(13) C(18) C(17) -179.0(3) . . . . yes C(12) C(19) C(20) C(21) -173.9(3) . . . . yes C(12) C(19) C(24) C(23) 173.8(4) . . . . yes C(13) C(12) C(19) C(20) -55.7(4) . . . . yes C(13) C(12) C(19) C(24) 127.2(3) . . . . yes C(13) C(14) C(15) C(16) 1.5(6) . . . . yes C(13) C(18) C(17) C(16) -0.6(6) . . . . yes C(14) C(13) C(12) C(19) 144.4(3) . . . . yes C(14) C(13) C(18) C(17) 1.0(5) . . . . yes C(14) C(15) C(16) C(17) -1.1(7) . . . . yes C(15) C(14) C(13) C(18) -1.4(5) . . . . yes C(15) C(16) C(17) C(18) 0.6(7) . . . . yes C(18) C(13) C(12) C(19) -35.6(4) . . . . yes C(19) C(20) C(21) C(22) 0.1(5) . . . . yes C(19) C(24) C(23) C(22) 0.0(7) . . . . yes C(20) C(19) C(24) C(23) -3.4(5) . . . . yes C(20) C(21) C(22) C(23) -3.6(6) . . . . yes C(21) C(20) C(19) C(24) 3.3(5) . . . . yes C(21) C(22) C(23) C(24) 3.5(7) . . . . yes C(25) P C(31) C(32) -106.2(2) . . . . yes C(25) P C(31) C(36) 68.2(3) . . . . yes C(25) P C(37) C(38) -146.1(3) . . . . yes C(25) P C(37) C(42) 36.2(3) . . . . yes C(25) C(26) C(27) C(28) -0.4(5) . . . . yes C(25) C(30) C(29) C(28) -1.4(5) . . . . yes C(26) C(25) P C(31) 162.5(2) . . . . yes C(26) C(25) P C(37) -80.6(3) . . . . yes C(26) C(25) C(30) C(29) 0.1(4) . . . . yes C(26) C(27) C(28) C(29) -0.9(6) . . . . yes C(27) C(26) C(25) C(30) 0.8(5) . . . . yes C(27) C(28) C(29) C(30) 1.8(5) . . . . yes C(30) C(25) P C(31) -16.2(3) . . . . yes C(30) C(25) P C(37) 100.8(2) . . . . yes C(31) P C(37) C(38) -28.9(3) . . . . yes C(31) P C(37) C(42) 153.3(3) . . . . yes C(31) C(32) C(33) C(34) 0.5(5) . . . . yes C(31) C(36) C(35) C(34) -0.4(6) . . . . yes C(32) C(31) P C(37) 136.6(2) . . . . yes C(32) C(31) C(36) C(35) 2.4(5) . . . . yes C(32) C(33) C(34) C(35) 1.5(6) . . . . yes C(33) C(32) C(31) C(36) -2.4(4) . . . . yes C(33) C(34) C(35) C(36) -1.5(6) . . . . yes C(36) C(31) P C(37) -49.0(3) . . . . yes C(37) C(38) C(39) C(40) 1.3(6) . . . . yes C(37) C(42) C(41) C(40) 0.8(6) . . . . yes C(38) C(37) C(42) C(41) -0.8(5) . . . . yes C(38) C(39) C(40) C(41) -1.3(7) . . . . yes C(39) C(38) C(37) C(42) -0.2(5) . . . . yes C(39) C(40) C(41) C(42) 0.2(7) . . . . yes C(39) C(40) C(41) C(42) 0.2(7) . . . . yes #------------------------------------------------------------------------------ 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 F(1) C(2) 3.104(4) . . ? F(1) C(1) 3.205(4) . . ? F(1) C(15) 3.425(4) . 3_555 ? F(1) C(2) 3.494(4) . 3_555 ? F(2) C(42) 3.246(6) . . ? F(2) C(6) 3.342(5) . 1_455 ? F(2) C(41) 3.531(7) . . ? F(2) C(1) 3.546(6) . . ? F(2a) C(34) 3.30(3) . 4_454 ? F(3) C(3) 3.114(4) . 3_555 ? F(3) C(34) 3.532(6) . 4_454 ? F(3) C(2) 3.548(5) . 3_555 ? F(4) C(9) 3.285(6) . 1_455 ? F(4) C(29) 3.462(6) . 2_445 ? F(4) C(41) 3.474(7) . . ? F(4a) C(41) 3.04(3) . . ? F(4a) C(42) 3.13(3) . . ? F(4a) C(1) 3.28(3) . . ? F(4a) C(22) 3.51(3) . 2_545 ? O C(22) 3.118(5) . 2_545 ? O C(39) 3.515(5) . 3_556 ? O C(21) 3.529(5) . 2_545 ? C(4) C(17) 3.572(4) . 4_555 ? C(4) C(16) 3.577(4) . 4_555 ? C(9) C(29) 3.521(5) . 2_545 ? #------------------------------------------------------------------------------ data_0503b _database_code_depnum_ccdc_archive 'CCDC 252273' _audit_creation_date 'Fri Oct 1 12:50:28 2004' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C30 H29 B2 Cl F4 N7 O2 P Ru ' _chemical_formula_moiety 'C30 H29 B Cl N7 O2 P Ru, B F4 ' _chemical_formula_weight 784.71 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 10.3721(6) _cell_length_b 12.129(1) _cell_length_c 14.712(1) _cell_angle_alpha 77.684(3) _cell_angle_beta 86.322(1) _cell_angle_gamma 70.7225(8) _cell_volume 1706.8(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red-purple _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.601 _exptl_absorpt_correction_T_max 0.824 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Quantum CCD/Rigaku AFC7' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14762 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9287 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9287 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). The oxygen atom of hydroxide is disordered with occupancy factors of 0.8 / 0.2. Three hydrogen atoms of the CH2OH part were not located. ; _reflns_number_total 7261 _reflns_number_gt 5864 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0912 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7179 _refine_ls_number_parameters 437 _refine_ls_goodness_of_fit_ref 1.711 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.02000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0002 _refine_diff_density_max 1.03 _refine_diff_density_min -0.68 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru Ru -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.28095(2) 0.02048(2) 0.31926(2) 0.03432(7) Uani 1.00 d . . . Cl Cl 0.22591(8) -0.02339(8) 0.47835(6) 0.0523(2) Uani 1.00 d . . . P P 0.02730(7) -0.21457(7) 0.25654(6) 0.0376(2) Uani 1.00 d . . . F(1) F 0.5126(4) -0.2840(3) 0.1595(5) 0.201(2) Uani 1.00 d . . . F(2) F 0.5635(5) -0.4435(6) 0.2536(4) 0.219(3) Uani 1.00 d . . . F(3) F 0.5688(5) -0.4312(8) 0.1084(6) 0.284(4) Uani 1.00 d . . . F(4) F 0.7306(2) -0.4059(3) 0.1648(2) 0.110(1) Uani 1.00 d . . . O(1) O 0.5411(3) -0.1650(3) 0.3448(3) 0.091(1) Uani 1.00 d . . . O(2a) O 0.2980(4) -0.3896(3) 0.3548(3) 0.085(1) Uani 0.80 d P . . O(2b) O 0.259(1) -0.285(1) 0.452(1) 0.076(4) Uiso 0.20 d P . . N(1) N 0.4376(3) -0.0954(2) 0.3331(2) 0.0474(8) Uani 1.00 d . . . N(2) N 0.3064(2) 0.0756(2) 0.1778(2) 0.0413(7) Uani 1.00 d . . . N(3) N 0.2856(3) 0.1924(2) 0.1409(2) 0.0449(7) Uani 1.00 d . . . N(4) N 0.0996(2) 0.1637(2) 0.3019(2) 0.0408(7) Uani 1.00 d . . . N(5) N 0.0963(3) 0.2696(2) 0.2458(2) 0.0430(7) Uani 1.00 d . . . N(6) N 0.3651(2) 0.1547(2) 0.3409(2) 0.0392(7) Uani 1.00 d . . . N(7) N 0.3320(3) 0.2609(2) 0.2797(2) 0.0434(7) Uani 1.00 d . . . C(1) C 0.3425(3) 0.0165(4) 0.1083(3) 0.057(1) Uani 1.00 d . . . C(2) C 0.3466(4) 0.0950(4) 0.0265(3) 0.068(1) Uani 1.00 d . . . C(3) C 0.3110(4) 0.2036(4) 0.0494(2) 0.061(1) Uani 1.00 d . . . C(4) C -0.0287(3) 0.1748(4) 0.3310(3) 0.057(1) Uani 1.00 d . . . C(5) C -0.1143(4) 0.2871(4) 0.2926(3) 0.069(1) Uani 1.00 d . . . C(6) C -0.0325(4) 0.3443(3) 0.2396(3) 0.059(1) Uani 1.00 d . . . C(7) C 0.4546(3) 0.1587(3) 0.4000(2) 0.0512(10) Uani 1.00 d . . . C(8) C 0.4814(4) 0.2648(4) 0.3777(3) 0.061(1) Uani 1.00 d . . . C(9) C 0.4024(4) 0.3273(3) 0.3022(3) 0.059(1) Uani 1.00 d . . . C(10) C 0.1644(3) -0.0720(3) 0.2840(2) 0.0443(9) Uani 1.00 d . . . C(11) C 0.1631(3) -0.1820(3) 0.3061(2) 0.0424(9) Uani 1.00 d . . . C(12) C 0.2604(4) -0.2811(3) 0.3750(3) 0.068(1) Uani 1.00 d . . . C(13) C -0.0478(3) -0.2940(3) 0.3491(2) 0.0422(8) Uani 1.00 d . . . C(14) C -0.0687(4) -0.2583(3) 0.4341(3) 0.057(1) Uani 1.00 d . . . C(15) C -0.1339(4) -0.3140(4) 0.5044(3) 0.068(1) Uani 1.00 d . . . C(16) C -0.1782(4) -0.4036(4) 0.4916(3) 0.070(1) Uani 1.00 d . . . C(17) C -0.1587(5) -0.4386(4) 0.4086(3) 0.072(1) Uani 1.00 d . . . C(18) C -0.0925(4) -0.3853(3) 0.3371(3) 0.058(1) Uani 1.00 d . . . C(19) C -0.1032(3) -0.0782(3) 0.2050(2) 0.0411(8) Uani 1.00 d . . . C(20) C -0.0829(4) -0.0150(3) 0.1188(3) 0.064(1) Uani 1.00 d . . . C(21) C -0.1784(5) 0.0898(4) 0.0802(3) 0.079(1) Uani 1.00 d . . . C(22) C -0.2964(5) 0.1345(4) 0.1252(4) 0.085(2) Uani 1.00 d . . . C(23) C -0.3158(5) 0.0742(5) 0.2110(4) 0.106(2) Uani 1.00 d . . . C(24) C -0.2212(4) -0.0311(4) 0.2515(3) 0.077(1) Uani 1.00 d . . . C(25) C 0.0857(3) -0.2939(3) 0.1631(2) 0.0368(8) Uani 1.00 d . . . C(26) C -0.0103(3) -0.3081(3) 0.1086(2) 0.0448(9) Uani 1.00 d . . . C(27) C 0.0327(3) -0.3641(3) 0.0345(2) 0.0508(10) Uani 1.00 d . . . C(28) C 0.1681(3) -0.4045(3) 0.0129(2) 0.0493(9) Uani 1.00 d . . . C(29) C 0.2626(3) -0.3896(3) 0.0659(3) 0.0508(10) Uani 1.00 d . . . C(30) C 0.2224(3) -0.3338(3) 0.1411(2) 0.0438(9) Uani 1.00 d . . . B(1) B 0.2290(4) 0.2864(3) 0.2014(3) 0.047(1) Uani 1.00 d . . . B(2) B 0.5997(5) -0.3873(6) 0.1757(4) 0.077(2) Uani 1.00 d . . . H(1) H 0.2108 0.3721 0.1617 0.0539 Uiso 1.00 calc . . . H(2) H 0.3626 -0.0688 0.1146 0.0688 Uiso 1.00 calc . . . H(3) H 0.3700 0.0765 -0.0347 0.0821 Uiso 1.00 calc . . . H(4) H 0.3048 0.2779 0.0063 0.0732 Uiso 1.00 calc . . . H(5) H -0.0567 0.1133 0.3725 0.0683 Uiso 1.00 calc . . . H(6) H -0.2121 0.3191 0.3012 0.0832 Uiso 1.00 calc . . . H(7) H -0.0628 0.4254 0.2036 0.0705 Uiso 1.00 calc . . . H(8) H 0.4956 0.0948 0.4522 0.0615 Uiso 1.00 calc . . . H(9) H 0.5433 0.2894 0.4092 0.0736 Uiso 1.00 calc . . . H(10) H 0.3972 0.4070 0.2694 0.0712 Uiso 1.00 calc . . . H(11) H 0.0924 -0.0217 0.2401 0.0531 Uiso 1.00 calc . . . H(12) H -0.0375 -0.1945 0.4438 0.0681 Uiso 1.00 calc . . . H(13) H -0.1485 -0.2891 0.5637 0.0819 Uiso 1.00 calc . . . H(14) H -0.2236 -0.4424 0.5417 0.0845 Uiso 1.00 calc . . . H(15) H -0.1917 -0.5016 0.3995 0.0862 Uiso 1.00 calc . . . H(16) H -0.0774 -0.4120 0.2785 0.0695 Uiso 1.00 calc . . . H(17) H 0.0004 -0.0455 0.0852 0.0769 Uiso 1.00 calc . . . H(18) H -0.1618 0.1333 0.0197 0.0948 Uiso 1.00 calc . . . H(19) H -0.3655 0.2079 0.0966 0.1017 Uiso 1.00 calc . . . H(20) H -0.3987 0.1065 0.2444 0.1274 Uiso 1.00 calc . . . H(21) H -0.2374 -0.0725 0.3130 0.0928 Uiso 1.00 calc . . . H(22) H -0.1068 -0.2787 0.1226 0.0537 Uiso 1.00 calc . . . H(23) H -0.0342 -0.3750 -0.0029 0.0610 Uiso 1.00 calc . . . H(24) H 0.1971 -0.4434 -0.0395 0.0591 Uiso 1.00 calc . . . H(25) H 0.3588 -0.4184 0.0507 0.0609 Uiso 1.00 calc . . . H(26) H 0.2900 -0.3229 0.1779 0.0526 Uiso 1.00 calc . . . 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 Ru 0.0361(1) 0.0335(1) 0.0375(1) -0.01560(9) 0.00161(8) -0.00960(9) Cl 0.0600(5) 0.0586(5) 0.0418(5) -0.0275(4) 0.0040(3) -0.0058(4) P 0.0426(4) 0.0410(4) 0.0387(4) -0.0214(3) 0.0070(3) -0.0179(3) F(1) 0.093(3) 0.092(3) 0.378(8) -0.005(2) 0.016(3) -0.011(4) F(2) 0.163(4) 0.262(6) 0.179(5) -0.070(4) 0.053(3) 0.055(5) F(3) 0.108(3) 0.52(1) 0.334(9) -0.111(5) 0.036(4) -0.309(10) F(4) 0.053(2) 0.138(3) 0.136(3) -0.028(1) -0.005(1) -0.022(2) O(1) 0.054(2) 0.069(2) 0.132(3) 0.005(1) -0.008(2) -0.018(2) O(2a) 0.130(3) 0.048(2) 0.076(3) -0.031(2) -0.012(2) -0.007(2) N(1) 0.046(2) 0.045(2) 0.054(2) -0.018(1) 0.004(1) -0.012(1) N(2) 0.044(1) 0.046(1) 0.036(1) -0.015(1) 0.002(1) -0.012(1) N(3) 0.047(1) 0.049(2) 0.036(1) -0.015(1) 0.001(1) -0.004(1) N(4) 0.038(1) 0.044(1) 0.045(2) -0.015(1) 0.001(1) -0.016(1) N(5) 0.048(1) 0.037(1) 0.042(2) -0.008(1) -0.005(1) -0.010(1) N(6) 0.041(1) 0.041(1) 0.041(1) -0.021(1) -0.001(1) -0.007(1) N(7) 0.053(1) 0.034(1) 0.047(2) -0.021(1) -0.002(1) -0.005(1) C(1) 0.053(2) 0.069(2) 0.051(2) -0.011(2) 0.009(2) -0.029(2) C(2) 0.061(2) 0.090(3) 0.041(2) -0.003(2) 0.008(2) -0.020(2) C(3) 0.051(2) 0.082(3) 0.035(2) -0.011(2) 0.001(1) 0.001(2) C(4) 0.043(2) 0.068(2) 0.068(2) -0.021(2) 0.010(2) -0.031(2) C(5) 0.039(2) 0.075(3) 0.092(3) -0.001(2) -0.002(2) -0.039(2) C(6) 0.055(2) 0.051(2) 0.063(2) 0.003(2) -0.011(2) -0.025(2) C(7) 0.048(2) 0.063(2) 0.050(2) -0.030(2) -0.010(1) -0.006(2) C(8) 0.068(2) 0.062(2) 0.069(3) -0.040(2) -0.011(2) -0.012(2) C(9) 0.073(2) 0.046(2) 0.073(3) -0.039(2) 0.007(2) -0.013(2) C(10) 0.048(2) 0.046(2) 0.046(2) -0.021(1) 0.006(1) -0.018(1) C(11) 0.044(2) 0.042(2) 0.045(2) -0.017(1) -0.001(1) -0.013(1) C(12) 0.074(3) 0.047(2) 0.076(3) -0.014(2) -0.029(2) 0.003(2) C(13) 0.049(2) 0.046(2) 0.037(2) -0.019(1) 0.007(1) -0.015(1) C(14) 0.080(2) 0.056(2) 0.046(2) -0.031(2) 0.011(2) -0.023(2) C(15) 0.087(3) 0.076(3) 0.043(2) -0.024(2) 0.022(2) -0.023(2) C(16) 0.086(3) 0.064(2) 0.057(3) -0.027(2) 0.028(2) -0.008(2) C(17) 0.098(3) 0.069(3) 0.065(3) -0.050(2) 0.020(2) -0.016(2) C(18) 0.082(2) 0.061(2) 0.048(2) -0.042(2) 0.016(2) -0.023(2) C(19) 0.045(2) 0.038(2) 0.048(2) -0.019(1) 0.009(1) -0.017(1) C(20) 0.069(2) 0.056(2) 0.050(2) -0.003(2) 0.019(2) -0.008(2) C(21) 0.096(3) 0.061(3) 0.057(3) -0.006(2) 0.018(2) 0.000(2) C(22) 0.074(3) 0.052(2) 0.104(4) -0.002(2) 0.014(2) -0.001(2) C(23) 0.070(3) 0.080(3) 0.129(5) 0.006(2) 0.049(3) 0.001(3) C(24) 0.062(2) 0.063(2) 0.083(3) -0.007(2) 0.033(2) 0.003(2) C(25) 0.039(2) 0.038(2) 0.038(2) -0.015(1) 0.005(1) -0.015(1) C(26) 0.038(2) 0.053(2) 0.047(2) -0.013(1) 0.000(1) -0.022(2) C(27) 0.056(2) 0.053(2) 0.046(2) -0.012(2) -0.007(1) -0.022(2) C(28) 0.061(2) 0.044(2) 0.040(2) -0.009(1) 0.005(1) -0.017(1) C(29) 0.046(2) 0.050(2) 0.053(2) -0.009(1) 0.014(1) -0.018(2) C(30) 0.039(2) 0.047(2) 0.048(2) -0.016(1) 0.002(1) -0.014(1) B(1) 0.055(2) 0.038(2) 0.046(2) -0.015(2) -0.005(2) 0.000(2) B(2) 0.046(3) 0.112(4) 0.066(3) -0.018(3) 0.005(2) -0.016(3) #------------------------------------------------------------------------------ _computing_data_collection D*TREK _computing_cell_refinement D*TREK _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru Cl 2.3633(9) . . yes Ru N(1) 1.752(3) . . yes Ru N(2) 2.074(3) . . yes Ru N(4) 2.083(2) . . yes Ru N(6) 2.170(2) . . yes Ru C(10) 2.053(3) . . yes P C(11) 1.815(3) . . yes P C(13) 1.786(3) . . yes P C(19) 1.806(3) . . yes P C(25) 1.805(3) . . yes F(1) B(2) 1.263(7) . . yes F(2) B(2) 1.304(7) . . yes F(3) B(2) 1.320(7) . . yes F(4) B(2) 1.306(5) . . yes O(1) N(1) 1.122(3) . . yes O(2a) C(12) 1.337(5) . . yes O(2b) C(12) 1.13(2) . . yes N(2) N(3) 1.354(4) . . yes N(2) C(1) 1.336(4) . . yes N(3) C(3) 1.342(4) . . yes N(3) B(1) 1.536(5) . . yes N(4) N(5) 1.362(4) . . yes N(4) C(4) 1.343(4) . . yes N(5) C(6) 1.339(4) . . yes N(5) B(1) 1.541(5) . . yes N(6) N(7) 1.357(3) . . yes N(6) C(7) 1.330(4) . . yes N(7) C(9) 1.350(4) . . yes N(7) B(1) 1.534(5) . . yes C(1) C(2) 1.374(6) . . yes C(2) C(3) 1.356(6) . . yes C(4) C(5) 1.378(6) . . yes C(5) C(6) 1.372(6) . . yes C(7) C(8) 1.373(5) . . yes C(8) C(9) 1.352(6) . . yes C(10) C(11) 1.309(4) . . yes C(11) C(12) 1.517(5) . . yes C(13) C(14) 1.390(4) . . yes C(13) C(18) 1.380(4) . . yes C(14) C(15) 1.378(5) . . yes C(15) C(16) 1.362(6) . . yes C(16) C(17) 1.359(6) . . yes C(17) C(18) 1.381(5) . . yes C(19) C(20) 1.378(5) . . yes C(19) C(24) 1.374(5) . . yes C(20) C(21) 1.360(5) . . yes C(21) C(22) 1.357(6) . . yes C(22) C(23) 1.355(7) . . yes C(23) C(24) 1.368(6) . . yes C(25) C(26) 1.391(4) . . yes C(25) C(30) 1.380(4) . . yes C(26) C(27) 1.379(4) . . yes C(27) C(28) 1.367(5) . . yes C(28) C(29) 1.370(5) . . yes C(29) C(30) 1.389(4) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl Ru N(1) 92.94(9) . . . yes Cl Ru N(2) 172.98(7) . . . yes Cl Ru N(4) 87.93(8) . . . yes Cl Ru N(6) 92.06(7) . . . yes Cl Ru C(10) 91.97(9) . . . yes N(1) Ru N(2) 94.1(1) . . . yes N(1) Ru N(4) 177.4(1) . . . yes N(1) Ru N(6) 94.8(1) . . . yes N(1) Ru C(10) 98.0(1) . . . yes N(2) Ru N(4) 85.06(10) . . . yes N(2) Ru N(6) 87.41(10) . . . yes N(2) Ru C(10) 87.0(1) . . . yes N(4) Ru N(6) 82.75(9) . . . yes N(4) Ru C(10) 84.5(1) . . . yes N(6) Ru C(10) 166.4(1) . . . yes C(11) P C(13) 107.7(1) . . . yes C(11) P C(19) 110.6(1) . . . yes C(11) P C(25) 112.6(1) . . . yes C(13) P C(19) 108.2(1) . . . yes C(13) P C(25) 112.6(1) . . . yes C(19) P C(25) 105.1(1) . . . yes Ru N(1) O(1) 175.3(3) . . . yes Ru N(2) N(3) 120.1(2) . . . yes Ru N(2) C(1) 132.5(2) . . . yes N(3) N(2) C(1) 107.4(3) . . . yes N(2) N(3) C(3) 108.2(3) . . . yes N(2) N(3) B(1) 120.3(2) . . . yes C(3) N(3) B(1) 131.3(3) . . . yes Ru N(4) N(5) 119.9(2) . . . yes Ru N(4) C(4) 132.8(2) . . . yes N(5) N(4) C(4) 107.1(3) . . . yes N(4) N(5) C(6) 109.0(3) . . . yes N(4) N(5) B(1) 120.0(2) . . . yes C(6) N(5) B(1) 131.0(3) . . . yes Ru N(6) N(7) 118.7(2) . . . yes Ru N(6) C(7) 135.2(2) . . . yes N(7) N(6) C(7) 105.9(2) . . . yes N(6) N(7) C(9) 108.9(3) . . . yes N(6) N(7) B(1) 119.5(2) . . . yes C(9) N(7) B(1) 131.6(3) . . . yes N(2) C(1) C(2) 109.6(3) . . . yes C(1) C(2) C(3) 105.4(3) . . . yes N(3) C(3) C(2) 109.4(3) . . . yes N(4) C(4) C(5) 109.5(3) . . . yes C(4) C(5) C(6) 105.8(3) . . . yes N(5) C(6) C(5) 108.6(3) . . . yes N(6) C(7) C(8) 111.3(3) . . . yes C(7) C(8) C(9) 104.8(3) . . . yes N(7) C(9) C(8) 109.1(3) . . . yes Ru C(10) C(11) 135.8(3) . . . yes P C(11) C(10) 117.1(2) . . . yes P C(11) C(12) 118.1(2) . . . yes C(10) C(11) C(12) 124.7(3) . . . yes O(2a) C(12) O(2b) 112.3(9) . . . yes O(2a) C(12) C(11) 115.7(4) . . . yes O(2b) C(12) C(11) 123.8(9) . . . yes P C(13) C(14) 118.8(2) . . . yes P C(13) C(18) 121.9(2) . . . yes C(14) C(13) C(18) 119.1(3) . . . yes C(13) C(14) C(15) 119.6(3) . . . yes C(14) C(15) C(16) 120.8(3) . . . yes C(15) C(16) C(17) 120.0(3) . . . yes C(16) C(17) C(18) 120.6(4) . . . yes C(13) C(18) C(17) 119.9(3) . . . yes P C(19) C(20) 120.0(2) . . . yes P C(19) C(24) 121.8(3) . . . yes C(20) C(19) C(24) 118.0(3) . . . yes C(19) C(20) C(21) 120.8(3) . . . yes C(20) C(21) C(22) 121.0(4) . . . yes C(21) C(22) C(23) 118.6(4) . . . yes C(22) C(23) C(24) 121.6(4) . . . yes C(19) C(24) C(23) 120.0(4) . . . yes P C(25) C(26) 119.0(2) . . . yes P C(25) C(30) 121.3(2) . . . yes C(26) C(25) C(30) 119.6(3) . . . yes C(25) C(26) C(27) 119.6(3) . . . yes C(26) C(27) C(28) 120.9(3) . . . yes C(27) C(28) C(29) 119.6(3) . . . yes C(28) C(29) C(30) 120.8(3) . . . yes C(25) C(30) C(29) 119.5(3) . . . yes N(3) B(1) N(5) 107.1(3) . . . yes N(3) B(1) N(7) 108.4(3) . . . yes N(5) B(1) N(7) 108.2(3) . . . yes F(1) B(2) F(2) 106.2(5) . . . yes F(1) B(2) F(3) 100.0(6) . . . yes F(1) B(2) F(4) 122.5(6) . . . yes F(2) B(2) F(3) 106.8(7) . . . yes F(2) B(2) F(4) 115.9(5) . . . yes F(3) B(2) F(4) 103.0(5) . . . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ru N(2) N(3) C(3) 178.9(2) . . . . yes Ru N(2) N(3) B(1) -6.3(3) . . . . yes Ru N(2) C(1) C(2) -179.0(2) . . . . yes Ru N(4) N(5) C(6) 175.0(2) . . . . yes Ru N(4) N(5) B(1) -4.8(4) . . . . yes Ru N(4) C(4) C(5) -174.2(2) . . . . yes Ru N(6) N(7) C(9) -175.7(2) . . . . yes Ru N(6) N(7) B(1) 4.2(4) . . . . yes Ru N(6) C(7) C(8) 174.5(3) . . . . yes Ru C(10) C(11) P 177.1(2) . . . . yes Ru C(10) C(11) C(12) 1.6(6) . . . . yes Cl Ru N(1) O(1) -74(3) . . . . yes Cl Ru N(2) N(3) 49.5(7) . . . . yes Cl Ru N(2) C(1) -130.8(5) . . . . yes Cl Ru N(4) N(5) 139.8(2) . . . . yes Cl Ru N(4) C(4) -45.8(3) . . . . yes Cl Ru N(6) N(7) -135.3(2) . . . . yes Cl Ru N(6) C(7) 50.0(3) . . . . yes Cl Ru C(10) C(11) -59.5(3) . . . . yes P C(11) C(12) O(2a) 39.8(5) . . . . yes P C(11) C(12) O(2b) -106(1) . . . . yes P C(13) C(14) C(15) 176.1(3) . . . . yes P C(13) C(18) C(17) -175.4(3) . . . . yes P C(19) C(20) C(21) -178.0(4) . . . . yes P C(19) C(24) C(23) 178.1(4) . . . . yes P C(25) C(26) C(27) 177.3(3) . . . . yes P C(25) C(30) C(29) -177.0(3) . . . . yes O(1) N(1) Ru N(2) 105(3) . . . . yes O(1) N(1) Ru N(4) 35(5) . . . . yes O(1) N(1) Ru N(6) 18(3) . . . . yes O(1) N(1) Ru C(10) -166(3) . . . . yes O(2a) C(12) C(11) C(10) -144.8(4) . . . . yes O(2b) C(12) C(11) C(10) 69(1) . . . . yes N(1) Ru N(2) N(3) -131.0(2) . . . . yes N(1) Ru N(2) C(1) 48.7(3) . . . . yes N(1) Ru N(4) N(5) 30(2) . . . . yes N(1) Ru N(4) C(4) -155(2) . . . . yes N(1) Ru N(6) N(7) 131.6(2) . . . . yes N(1) Ru N(6) C(7) -43.1(3) . . . . yes N(1) Ru C(10) C(11) 33.7(4) . . . . yes N(2) Ru N(4) N(5) -40.6(2) . . . . yes N(2) Ru N(4) C(4) 133.9(3) . . . . yes N(2) Ru N(6) N(7) 37.7(2) . . . . yes N(2) Ru N(6) C(7) -137.0(3) . . . . yes N(2) Ru C(10) C(11) 127.4(4) . . . . yes N(2) N(3) C(3) C(2) 0.7(4) . . . . yes N(2) N(3) B(1) N(5) -53.5(3) . . . . yes N(2) N(3) B(1) N(7) 63.0(3) . . . . yes N(2) C(1) C(2) C(3) -0.3(4) . . . . yes N(3) N(2) Ru N(4) 46.6(2) . . . . yes N(3) N(2) Ru N(6) -36.4(2) . . . . yes N(3) N(2) Ru C(10) 131.3(2) . . . . yes N(3) N(2) C(1) C(2) 0.7(4) . . . . yes N(3) C(3) C(2) C(1) -0.2(4) . . . . yes N(3) B(1) N(5) N(4) 59.9(4) . . . . yes N(3) B(1) N(5) C(6) -119.8(3) . . . . yes N(3) B(1) N(7) N(6) -60.2(4) . . . . yes N(3) B(1) N(7) C(9) 119.7(4) . . . . yes N(4) Ru N(2) C(1) -133.7(3) . . . . yes N(4) Ru N(6) N(7) -47.6(2) . . . . yes N(4) Ru N(6) C(7) 137.7(3) . . . . yes N(4) Ru C(10) C(11) -147.3(4) . . . . yes N(4) N(5) C(6) C(5) 0.4(4) . . . . yes N(4) N(5) B(1) N(7) -56.8(4) . . . . yes N(4) C(4) C(5) C(6) -0.5(4) . . . . yes N(5) N(4) Ru N(6) 47.5(2) . . . . yes N(5) N(4) Ru C(10) -128.0(2) . . . . yes N(5) N(4) C(4) C(5) 0.8(4) . . . . yes N(5) C(6) C(5) C(4) 0.1(4) . . . . yes N(5) B(1) N(3) C(3) 119.9(4) . . . . yes N(5) B(1) N(7) N(6) 55.6(4) . . . . yes N(5) B(1) N(7) C(9) -124.5(4) . . . . yes N(6) Ru N(2) C(1) 143.3(3) . . . . yes N(6) Ru N(4) C(4) -138.1(3) . . . . yes N(6) Ru C(10) C(11) -166.7(4) . . . . yes N(6) N(7) C(9) C(8) 0.1(4) . . . . yes N(6) C(7) C(8) C(9) 0.8(5) . . . . yes N(7) N(6) Ru C(10) -28.1(6) . . . . yes N(7) N(6) C(7) C(8) -0.7(4) . . . . yes N(7) C(9) C(8) C(7) -0.5(5) . . . . yes N(7) B(1) N(3) C(3) -123.6(3) . . . . yes N(7) B(1) N(5) C(6) 123.5(3) . . . . yes C(1) N(2) Ru C(10) -49.0(3) . . . . yes C(1) N(2) N(3) C(3) -0.8(3) . . . . yes C(1) N(2) N(3) B(1) 173.9(3) . . . . yes C(2) C(3) N(3) B(1) -173.3(3) . . . . yes C(4) N(4) Ru C(10) 46.4(3) . . . . yes C(4) N(4) N(5) C(6) -0.7(3) . . . . yes C(4) N(4) N(5) B(1) 179.5(3) . . . . yes C(5) C(6) N(5) B(1) -179.9(3) . . . . yes C(7) N(6) Ru C(10) 157.2(4) . . . . yes C(7) N(6) N(7) C(9) 0.4(4) . . . . yes C(7) N(6) N(7) B(1) -179.7(3) . . . . yes C(8) C(9) N(7) B(1) -179.9(3) . . . . yes C(10) C(11) P C(13) -130.7(3) . . . . yes C(10) C(11) P C(19) -12.6(3) . . . . yes C(10) C(11) P C(25) 104.7(3) . . . . yes C(11) P C(13) C(14) 40.7(3) . . . . yes C(11) P C(13) C(18) -143.0(3) . . . . yes C(11) P C(19) C(20) 78.5(3) . . . . yes C(11) P C(19) C(24) -98.1(3) . . . . yes C(11) P C(25) C(26) -169.7(3) . . . . yes C(11) P C(25) C(30) 6.1(3) . . . . yes C(12) C(11) P C(13) 45.1(3) . . . . yes C(12) C(11) P C(19) 163.2(3) . . . . yes C(12) C(11) P C(25) -79.6(3) . . . . yes C(13) P C(19) C(20) -163.8(3) . . . . yes C(13) P C(19) C(24) 19.6(4) . . . . yes C(13) P C(25) C(26) 68.3(3) . . . . yes C(13) P C(25) C(30) -115.9(3) . . . . yes C(13) C(14) C(15) C(16) 0.0(6) . . . . yes C(13) C(18) C(17) C(16) -1.3(7) . . . . yes C(14) C(13) P C(19) -78.9(3) . . . . yes C(14) C(13) P C(25) 165.4(3) . . . . yes C(14) C(13) C(18) C(17) 1.0(6) . . . . yes C(14) C(15) C(16) C(17) -0.3(7) . . . . yes C(15) C(14) C(13) C(18) -0.3(6) . . . . yes C(15) C(16) C(17) C(18) 1.0(7) . . . . yes C(18) C(13) P C(19) 97.5(3) . . . . yes C(18) C(13) P C(25) -18.2(3) . . . . yes C(19) P C(25) C(26) -49.3(3) . . . . yes C(19) P C(25) C(30) 126.5(3) . . . . yes C(19) C(20) C(21) C(22) -0.5(8) . . . . yes C(19) C(24) C(23) C(22) 0.0(9) . . . . yes C(20) C(19) P C(25) -43.3(3) . . . . yes C(20) C(19) C(24) C(23) 1.5(7) . . . . yes C(20) C(21) C(22) C(23) 1.9(9) . . . . yes C(21) C(20) C(19) C(24) -1.3(6) . . . . yes C(21) C(22) C(23) C(24) -1.7(10) . . . . yes C(24) C(19) P C(25) 140.1(3) . . . . yes C(25) C(26) C(27) C(28) -1.0(5) . . . . yes C(25) C(30) C(29) C(28) 0.6(5) . . . . yes C(26) C(25) C(30) C(29) -1.2(5) . . . . yes C(26) C(27) C(28) C(29) 0.3(5) . . . . yes C(27) C(26) C(25) C(30) 1.4(5) . . . . yes C(27) C(28) C(29) C(30) -0.1(5) . . . . yes C(27) C(28) C(29) C(30) -0.1(5) . . . . yes #------------------------------------------------------------------------------ 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 Cl C(7) 3.577(3) . 2_656 ? F(1) C(30) 3.297(5) . . ? F(1) O(1) 3.415(8) . . ? F(1) C(1) 3.422(5) . . ? F(1) C(3) 3.595(7) . 2_655 ? F(2) O(2a) 2.988(7) . . ? F(3) C(29) 3.129(5) . . ? F(3) C(30) 3.428(6) . . ? F(3) C(28) 3.451(6) . 2_645 ? F(4) C(6) 3.231(4) . 1_645 ? F(4) C(26) 3.274(4) . 1_655 ? F(4) C(18) 3.319(5) . 1_655 ? F(4) C(3) 3.509(5) . 2_655 ? O(1) C(24) 3.443(5) . 1_655 ? O(2a) C(9) 3.483(5) . 1_545 ? O(2a) C(16) 3.496(6) . 2_546 ? N(6) C(15) 3.575(4) . 2_556 ? C(2) C(2) 3.414(7) . 2_655 ? C(15) C(17) 3.564(7) . 2_546 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_0421 _database_code_depnum_ccdc_archive 'CCDC 252274' _audit_creation_date 'Mon Dec 2 11:48:12 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C61 H52 B3 F8 N7 O P2 Ru ' _chemical_formula_moiety 'C61 H52 B N7 O P2 Ru, B2 F8 ' _chemical_formula_weight 1246.56 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.510(1) _cell_length_b 13.549(3) _cell_length_c 18.814(3) _cell_angle_alpha 99.134(3) _cell_angle_beta 97.113(1) _cell_angle_gamma 93.996(1) _cell_volume 2862.4(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 297.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.405 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.511 _exptl_absorpt_correction_T_max 0.980 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Quantum CCD/Rigaku AFC7' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24502 _diffrn_reflns_av_R_equivalents 0.083 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9123 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9123 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 11985 _reflns_number_gt 5706 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1574 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 11972 _refine_ls_number_parameters 748 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.01000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0001 _refine_diff_density_max 1.36 _refine_diff_density_min -1.45 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru Ru -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.04417(4) 0.08232(3) 0.22145(2) 0.0374(1) Uani 1.00 d . . . P(1) P -0.2739(1) 0.1167(1) 0.36070(7) 0.0468(5) Uani 1.00 d . . . P(2) P 0.0812(1) 0.4259(1) 0.19225(7) 0.0445(4) Uani 1.00 d . . . F(1) F -0.3538(6) -0.2457(6) 0.0167(3) 0.200(3) Uani 1.00 d . . . F(2) F -0.4599(7) -0.2301(7) 0.0949(5) 0.258(5) Uani 1.00 d . . . F(3) F -0.4232(6) -0.1044(4) 0.0508(3) 0.160(3) Uani 1.00 d . . . F(4) F -0.2888(5) -0.1594(4) 0.1247(2) 0.133(2) Uani 1.00 d . . . F(5) F 0.6285(7) 0.5406(6) 0.3226(4) 0.192(3) Uani 1.00 d . . . F(6) F 0.7712(6) 0.4728(5) 0.3838(3) 0.142(2) Uani 1.00 d . . . F(7) F 0.7881(7) 0.6278(6) 0.3648(4) 0.203(4) Uani 1.00 d . . . F(8) F 0.6720(9) 0.5869(6) 0.4385(4) 0.263(5) Uani 1.00 d . . . O O -0.0988(4) 0.0194(3) 0.0825(2) 0.066(1) Uani 1.00 d . . . N(1) N -0.0450(4) 0.0497(3) 0.1385(2) 0.039(1) Uani 1.00 d . . . N(2) N 0.1562(4) 0.1132(3) 0.3209(2) 0.039(1) Uani 1.00 d . . . N(3) N 0.2424(4) 0.0537(3) 0.3355(2) 0.044(1) Uani 1.00 d . . . N(4) N 0.2027(4) 0.0537(3) 0.1761(2) 0.044(1) Uani 1.00 d . . . N(5) N 0.2808(4) -0.0020(4) 0.2076(2) 0.050(1) Uani 1.00 d . . . N(6) N 0.0440(4) -0.0723(3) 0.2404(2) 0.041(1) Uani 1.00 d . . . N(7) N 0.1467(4) -0.1072(3) 0.2649(2) 0.046(1) Uani 1.00 d . . . C(1) C 0.1558(5) 0.1793(4) 0.3819(3) 0.046(2) Uani 1.00 d . . . C(2) C 0.2412(6) 0.1640(5) 0.4358(3) 0.058(2) Uani 1.00 d . . . C(3) C 0.2937(6) 0.0830(5) 0.4046(3) 0.060(2) Uani 1.00 d . . . C(4) C 0.2411(6) 0.0666(5) 0.1133(3) 0.057(2) Uani 1.00 d . . . C(5) C 0.3389(6) 0.0197(5) 0.1038(4) 0.069(2) Uani 1.00 d . . . C(6) C 0.3642(5) -0.0245(5) 0.1642(4) 0.065(2) Uani 1.00 d . . . C(7) C -0.0385(6) -0.1482(4) 0.2300(3) 0.052(2) Uani 1.00 d . . . C(8) C 0.0099(7) -0.2349(4) 0.2481(3) 0.061(2) Uani 1.00 d . . . C(9) C 0.1265(7) -0.2045(4) 0.2698(3) 0.062(2) Uani 1.00 d . . . C(10) C -0.0888(5) 0.0998(4) 0.2866(3) 0.042(2) Uani 1.00 d . . . C(11) C -0.1959(5) 0.1317(4) 0.2841(3) 0.041(2) Uani 1.00 d . . . C(12) C -0.2626(5) 0.1708(4) 0.2234(3) 0.040(2) Uani 1.00 d . . . C(13) C -0.2846(5) 0.2725(4) 0.2313(3) 0.050(2) Uani 1.00 d . . . C(14) C -0.3558(6) 0.3060(5) 0.1772(4) 0.065(2) Uani 1.00 d . . . C(15) C -0.4057(6) 0.2421(6) 0.1156(3) 0.068(2) Uani 1.00 d . . . C(16) C -0.3847(6) 0.1428(5) 0.1069(3) 0.058(2) Uani 1.00 d . . . C(17) C -0.3141(5) 0.1073(4) 0.1608(3) 0.048(2) Uani 1.00 d . . . C(18) C -0.3923(5) 0.1957(4) 0.3665(3) 0.050(2) Uani 1.00 d . . . C(19) C -0.4828(6) 0.1809(5) 0.3081(3) 0.063(2) Uani 1.00 d . . . C(20) C -0.5750(6) 0.2433(7) 0.3079(4) 0.080(3) Uani 1.00 d . . . C(21) C -0.5775(8) 0.3146(7) 0.3663(7) 0.106(4) Uani 1.00 d . . . C(22) C -0.4912(9) 0.3289(6) 0.4260(6) 0.110(4) Uani 1.00 d . . . C(23) C -0.3975(6) 0.2679(5) 0.4258(4) 0.076(2) Uani 1.00 d . . . C(24) C -0.1705(5) 0.1470(5) 0.4426(3) 0.051(2) Uani 1.00 d . . . C(25) C -0.1089(6) 0.2413(5) 0.4592(3) 0.066(2) Uani 1.00 d . . . C(26) C -0.0237(6) 0.2648(5) 0.5197(3) 0.073(2) Uani 1.00 d . . . C(27) C 0.0004(7) 0.1963(7) 0.5635(3) 0.081(3) Uani 1.00 d . . . C(28) C -0.0608(7) 0.1042(7) 0.5486(4) 0.082(3) Uani 1.00 d . . . C(29) C -0.1463(6) 0.0781(5) 0.4877(3) 0.070(2) Uani 1.00 d . . . C(30) C -0.3384(5) -0.0094(4) 0.3534(3) 0.050(2) Uani 1.00 d . . . C(31) C -0.4066(6) -0.0333(5) 0.4057(3) 0.063(2) Uani 1.00 d . . . C(32) C -0.4535(6) -0.1302(6) 0.4034(4) 0.072(3) Uani 1.00 d . . . C(33) C -0.4358(8) -0.2039(6) 0.3488(5) 0.094(3) Uani 1.00 d . . . C(34) C -0.3714(9) -0.1803(6) 0.2956(5) 0.112(4) Uani 1.00 d . . . C(35) C -0.3237(7) -0.0835(5) 0.2983(4) 0.086(3) Uani 1.00 d . . . C(36) C 0.0677(5) 0.2331(4) 0.2189(2) 0.038(2) Uani 1.00 d . . . C(37) C 0.0523(5) 0.2910(4) 0.1678(2) 0.038(1) Uani 1.00 d . . . C(38) C 0.0025(5) 0.2583(4) 0.0895(2) 0.043(2) Uani 1.00 d . . . C(39) C 0.0744(5) 0.2482(4) 0.0350(3) 0.051(2) Uani 1.00 d . . . C(40) C 0.0249(7) 0.2202(5) -0.0375(3) 0.063(2) Uani 1.00 d . . . C(41) C -0.0940(7) 0.2002(5) -0.0553(3) 0.064(2) Uani 1.00 d . . . C(42) C -0.1655(6) 0.2115(4) -0.0025(3) 0.059(2) Uani 1.00 d . . . C(43) C -0.1173(6) 0.2409(4) 0.0700(3) 0.052(2) Uani 1.00 d . . . C(44) C -0.0470(5) 0.4837(4) 0.1599(3) 0.047(2) Uani 1.00 d . . . C(45) C -0.0686(6) 0.4890(5) 0.0865(3) 0.059(2) Uani 1.00 d . . . C(46) C -0.1656(7) 0.5325(6) 0.0603(4) 0.073(3) Uani 1.00 d . . . C(47) C -0.2423(7) 0.5685(5) 0.1038(4) 0.077(3) Uani 1.00 d . . . C(48) C -0.2266(7) 0.5610(5) 0.1757(4) 0.076(3) Uani 1.00 d . . . C(49) C -0.1272(6) 0.5188(4) 0.2054(3) 0.059(2) Uani 1.00 d . . . C(50) C 0.2023(5) 0.4737(4) 0.1518(3) 0.046(2) Uani 1.00 d . . . C(51) C 0.2954(6) 0.4173(5) 0.1395(3) 0.063(2) Uani 1.00 d . . . C(52) C 0.3939(7) 0.4603(6) 0.1146(4) 0.087(3) Uani 1.00 d . . . C(53) C 0.3992(7) 0.5579(6) 0.1048(5) 0.090(3) Uani 1.00 d . . . C(54) C 0.3071(7) 0.6156(5) 0.1189(4) 0.079(3) Uani 1.00 d . . . C(55) C 0.2093(6) 0.5739(4) 0.1418(3) 0.058(2) Uani 1.00 d . . . C(56) C 0.1204(6) 0.4633(4) 0.2887(3) 0.057(2) Uani 1.00 d . . . C(57) C 0.0438(7) 0.4378(5) 0.3359(3) 0.074(2) Uani 1.00 d . . . C(58) C 0.080(1) 0.4676(6) 0.4114(4) 0.105(4) Uani 1.00 d . . . C(59) C 0.190(1) 0.5182(7) 0.4371(4) 0.116(4) Uani 1.00 d . . . C(60) C 0.2615(9) 0.5436(6) 0.3908(4) 0.103(3) Uani 1.00 d . . . C(61) C 0.2284(7) 0.5164(5) 0.3159(3) 0.075(2) Uani 1.00 d . . . B(1) B 0.2613(6) -0.0378(5) 0.2780(3) 0.051(2) Uani 1.00 d . . . B(2) B -0.3773(8) -0.1820(6) 0.0707(4) 0.068(3) Uani 1.00 d . . . B(3) B 0.712(2) 0.5557(9) 0.3810(6) 0.117(5) Uani 1.00 d . . . H(1) H 0.3259 -0.0875 0.3129 0.0672 Uiso 1.00 calc . . . H(2) H 0.1022 0.2314 0.3872 0.0550 Uiso 1.00 calc . . . H(3) H 0.2600 0.2016 0.4848 0.0692 Uiso 1.00 calc . . . H(4) H 0.3575 0.0520 0.4285 0.0723 Uiso 1.00 calc . . . H(5) H 0.2033 0.1049 0.0791 0.0681 Uiso 1.00 calc . . . H(6) H 0.3826 0.0175 0.0627 0.0828 Uiso 1.00 calc . . . H(7) H 0.4294 -0.0643 0.1740 0.0775 Uiso 1.00 calc . . . H(8) H -0.1207 -0.1445 0.2124 0.0624 Uiso 1.00 calc . . . H(9) H -0.0302 -0.3010 0.2459 0.0737 Uiso 1.00 calc . . . H(10) H 0.1854 -0.2467 0.2861 0.0743 Uiso 1.00 calc . . . H(11) H -0.0660 0.0783 0.3327 0.0503 Uiso 1.00 calc . . . H(12) H -0.2499 0.3190 0.2746 0.0595 Uiso 1.00 calc . . . H(13) H -0.3708 0.3762 0.1830 0.0782 Uiso 1.00 calc . . . H(14) H -0.4556 0.2670 0.0783 0.0818 Uiso 1.00 calc . . . H(15) H -0.4193 0.0973 0.0631 0.0695 Uiso 1.00 calc . . . H(16) H -0.3006 0.0368 0.1544 0.0579 Uiso 1.00 calc . . . H(17) H -0.4819 0.1272 0.2674 0.0754 Uiso 1.00 calc . . . H(18) H -0.6361 0.2353 0.2665 0.0962 Uiso 1.00 calc . . . H(19) H -0.6418 0.3572 0.3665 0.1277 Uiso 1.00 calc . . . H(20) H -0.4953 0.3805 0.4675 0.1318 Uiso 1.00 calc . . . H(21) H -0.3366 0.2767 0.4674 0.0911 Uiso 1.00 calc . . . H(22) H -0.1255 0.2910 0.4283 0.0788 Uiso 1.00 calc . . . H(23) H 0.0190 0.3309 0.5308 0.0878 Uiso 1.00 calc . . . H(24) H 0.0610 0.2130 0.6052 0.0974 Uiso 1.00 calc . . . H(25) H -0.0448 0.0559 0.5807 0.0980 Uiso 1.00 calc . . . H(26) H -0.1884 0.0118 0.4772 0.0845 Uiso 1.00 calc . . . H(27) H -0.4211 0.0190 0.4442 0.0752 Uiso 1.00 calc . . . H(28) H -0.4993 -0.1459 0.4408 0.0858 Uiso 1.00 calc . . . H(29) H -0.4681 -0.2724 0.3473 0.1128 Uiso 1.00 calc . . . H(30) H -0.3597 -0.2324 0.2560 0.1341 Uiso 1.00 calc . . . H(31) H -0.2789 -0.0680 0.2604 0.1029 Uiso 1.00 calc . . . H(32) H 0.0971 0.2719 0.2664 0.0461 Uiso 1.00 calc . . . H(33) H 0.1591 0.2606 0.0475 0.0611 Uiso 1.00 calc . . . H(34) H 0.0752 0.2148 -0.0754 0.0752 Uiso 1.00 calc . . . H(35) H -0.1277 0.1780 -0.1057 0.0766 Uiso 1.00 calc . . . H(36) H -0.2501 0.1990 -0.0155 0.0710 Uiso 1.00 calc . . . H(37) H -0.1688 0.2491 0.1073 0.0619 Uiso 1.00 calc . . . H(38) H -0.0154 0.4620 0.0537 0.0709 Uiso 1.00 calc . . . H(39) H -0.1790 0.5374 0.0091 0.0881 Uiso 1.00 calc . . . H(40) H -0.3093 0.6001 0.0841 0.0929 Uiso 1.00 calc . . . H(41) H -0.2840 0.5847 0.2064 0.0913 Uiso 1.00 calc . . . H(42) H -0.1149 0.5143 0.2567 0.0712 Uiso 1.00 calc . . . H(43) H 0.2928 0.3485 0.1480 0.0760 Uiso 1.00 calc . . . H(44) H 0.4584 0.4204 0.1042 0.1047 Uiso 1.00 calc . . . H(45) H 0.4678 0.5872 0.0879 0.1081 Uiso 1.00 calc . . . H(46) H 0.3119 0.6854 0.1126 0.0942 Uiso 1.00 calc . . . H(47) H 0.1445 0.6141 0.1510 0.0694 Uiso 1.00 calc . . . H(48) H -0.0320 0.4007 0.3177 0.0893 Uiso 1.00 calc . . . H(49) H 0.0278 0.4525 0.4455 0.1265 Uiso 1.00 calc . . . H(50) H 0.2152 0.5352 0.4891 0.1393 Uiso 1.00 calc . . . H(51) H 0.3368 0.5813 0.4094 0.1239 Uiso 1.00 calc . . . H(52) H 0.2812 0.5346 0.2828 0.0895 Uiso 1.00 calc . . . 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 Ru 0.0421(3) 0.0347(3) 0.0356(2) 0.0061(2) 0.0036(2) 0.0070(2) P(1) 0.0467(10) 0.0508(10) 0.0432(8) 0.0074(8) 0.0083(7) 0.0061(7) P(2) 0.061(1) 0.0325(8) 0.0396(7) 0.0052(7) 0.0031(7) 0.0071(6) F(1) 0.209(7) 0.240(8) 0.114(4) 0.144(6) -0.050(4) -0.075(5) F(2) 0.171(8) 0.26(1) 0.36(1) -0.074(7) 0.062(8) 0.135(9) F(3) 0.227(7) 0.094(4) 0.137(4) 0.052(4) -0.069(4) 0.006(3) F(4) 0.127(5) 0.148(5) 0.103(3) 0.036(4) -0.041(3) -0.011(3) F(5) 0.190(7) 0.204(8) 0.160(6) -0.014(6) -0.038(5) 0.030(5) F(6) 0.207(7) 0.119(5) 0.110(4) 0.047(4) 0.044(4) 0.013(3) F(7) 0.212(8) 0.138(6) 0.237(8) -0.045(6) -0.008(6) 0.024(5) F(8) 0.46(1) 0.274(10) 0.114(5) 0.24(1) 0.127(7) 0.049(5) O 0.091(4) 0.050(3) 0.046(2) 0.009(2) -0.019(2) -0.001(2) N(1) 0.052(3) 0.031(2) 0.038(2) 0.010(2) 0.007(2) 0.014(2) N(2) 0.038(3) 0.041(3) 0.038(2) 0.005(2) 0.003(2) 0.011(2) N(3) 0.043(3) 0.051(3) 0.036(2) 0.010(2) -0.004(2) 0.007(2) N(4) 0.039(3) 0.043(3) 0.050(3) 0.007(2) 0.011(2) 0.006(2) N(5) 0.039(3) 0.061(3) 0.050(3) 0.011(3) 0.011(2) 0.003(2) N(6) 0.038(3) 0.036(3) 0.049(3) 0.002(2) 0.001(2) 0.007(2) N(7) 0.058(3) 0.034(3) 0.048(3) 0.016(2) 0.001(2) 0.010(2) C(1) 0.052(4) 0.049(3) 0.034(3) 0.005(3) 0.003(3) 0.002(2) C(2) 0.064(4) 0.064(4) 0.040(3) 0.006(3) -0.004(3) 0.003(3) C(3) 0.055(4) 0.079(5) 0.046(3) 0.010(4) -0.009(3) 0.020(3) C(4) 0.060(4) 0.062(4) 0.052(4) -0.001(3) 0.022(3) 0.014(3) C(5) 0.047(4) 0.078(5) 0.077(5) 0.005(4) 0.022(4) -0.011(4) C(6) 0.038(4) 0.076(5) 0.075(4) 0.013(3) 0.010(3) -0.008(4) C(7) 0.061(4) 0.047(4) 0.045(3) -0.006(3) 0.010(3) 0.000(3) C(8) 0.082(5) 0.036(4) 0.062(4) -0.004(4) 0.007(4) 0.004(3) C(9) 0.095(6) 0.037(4) 0.056(4) 0.016(4) 0.004(4) 0.015(3) C(10) 0.047(4) 0.038(3) 0.038(3) 0.003(3) -0.002(2) 0.007(2) C(11) 0.041(3) 0.041(3) 0.040(3) 0.012(3) 0.003(2) 0.005(2) C(12) 0.037(3) 0.042(3) 0.042(3) 0.008(3) 0.005(2) 0.004(2) C(13) 0.049(4) 0.044(4) 0.054(3) 0.007(3) 0.001(3) 0.008(3) C(14) 0.068(5) 0.050(4) 0.077(4) 0.019(4) -0.007(4) 0.016(3) C(15) 0.061(5) 0.075(5) 0.071(4) 0.014(4) -0.010(3) 0.031(4) C(16) 0.057(4) 0.065(4) 0.047(3) 0.001(3) -0.006(3) 0.008(3) C(17) 0.044(4) 0.045(3) 0.054(3) 0.005(3) 0.002(3) 0.007(3) C(18) 0.046(4) 0.051(4) 0.053(3) 0.006(3) 0.015(3) 0.006(3) C(19) 0.047(4) 0.073(5) 0.069(4) 0.005(4) 0.006(3) 0.016(3) C(20) 0.041(4) 0.094(6) 0.108(6) 0.009(4) 0.002(4) 0.031(5) C(21) 0.070(6) 0.068(6) 0.185(10) 0.035(5) 0.023(7) 0.018(6) C(22) 0.084(7) 0.078(6) 0.156(9) 0.023(5) 0.033(6) -0.035(6) C(23) 0.072(5) 0.067(5) 0.084(5) 0.020(4) 0.016(4) -0.013(4) C(24) 0.048(4) 0.063(4) 0.045(3) 0.008(3) 0.017(3) 0.009(3) C(25) 0.067(5) 0.070(5) 0.059(4) 0.004(4) 0.011(3) 0.008(3) C(26) 0.074(5) 0.082(5) 0.052(4) -0.004(4) -0.005(3) -0.007(4) C(27) 0.078(6) 0.114(7) 0.046(4) -0.004(5) 0.002(4) 0.010(4) C(28) 0.079(6) 0.108(7) 0.058(4) 0.006(5) -0.008(4) 0.030(4) C(29) 0.070(5) 0.080(5) 0.063(4) 0.007(4) -0.002(4) 0.027(4) C(30) 0.055(4) 0.049(4) 0.046(3) 0.002(3) 0.013(3) 0.012(3) C(31) 0.061(4) 0.069(5) 0.059(4) 0.002(4) 0.007(3) 0.015(3) C(32) 0.061(5) 0.079(6) 0.078(5) -0.003(4) 0.008(4) 0.028(4) C(33) 0.093(7) 0.064(5) 0.131(7) -0.003(5) 0.024(5) 0.035(5) C(34) 0.149(9) 0.046(5) 0.145(8) -0.009(5) 0.072(7) -0.003(5) C(35) 0.114(7) 0.053(5) 0.101(6) 0.004(4) 0.058(5) 0.011(4) C(36) 0.042(3) 0.035(3) 0.038(3) 0.005(3) 0.006(2) 0.002(2) C(37) 0.050(3) 0.031(3) 0.035(3) 0.002(3) 0.008(2) 0.007(2) C(38) 0.066(4) 0.030(3) 0.034(3) -0.001(3) 0.003(3) 0.008(2) C(39) 0.063(4) 0.052(4) 0.039(3) 0.013(3) 0.009(3) 0.006(2) C(40) 0.099(6) 0.053(4) 0.038(3) 0.005(4) 0.019(3) 0.005(3) C(41) 0.099(6) 0.052(4) 0.035(3) 0.004(4) -0.004(3) 0.000(3) C(42) 0.068(5) 0.054(4) 0.050(3) -0.005(3) -0.012(3) 0.012(3) C(43) 0.061(4) 0.049(4) 0.044(3) -0.003(3) 0.010(3) 0.007(3) C(44) 0.051(4) 0.033(3) 0.057(3) 0.001(3) 0.009(3) 0.007(2) C(45) 0.054(4) 0.070(4) 0.058(4) 0.014(3) 0.008(3) 0.023(3) C(46) 0.070(5) 0.085(5) 0.073(4) 0.022(4) 0.004(4) 0.037(4) C(47) 0.071(5) 0.060(5) 0.109(6) 0.019(4) 0.008(4) 0.035(4) C(48) 0.066(5) 0.058(5) 0.108(6) 0.016(4) 0.028(4) 0.010(4) C(49) 0.069(5) 0.039(3) 0.069(4) 0.005(3) 0.012(3) 0.004(3) C(50) 0.043(4) 0.036(3) 0.056(3) 0.002(3) -0.002(3) 0.012(2) C(51) 0.057(5) 0.047(4) 0.085(5) 0.014(3) -0.005(4) 0.016(3) C(52) 0.049(5) 0.082(6) 0.134(7) 0.013(4) 0.013(4) 0.025(5) C(53) 0.058(5) 0.081(6) 0.136(7) -0.002(5) 0.021(5) 0.034(5) C(54) 0.069(5) 0.061(5) 0.113(6) -0.001(4) 0.015(4) 0.035(4) C(55) 0.065(5) 0.045(4) 0.067(4) 0.009(3) 0.013(3) 0.015(3) C(56) 0.090(5) 0.031(3) 0.046(3) 0.010(3) -0.004(3) 0.005(2) C(57) 0.130(7) 0.043(4) 0.051(4) 0.005(4) 0.026(4) 0.003(3) C(58) 0.20(1) 0.065(6) 0.052(5) 0.028(6) 0.026(6) 0.005(4) C(59) 0.21(1) 0.086(7) 0.043(4) 0.028(7) -0.018(6) -0.008(4) C(60) 0.150(9) 0.082(6) 0.059(5) 0.020(6) -0.029(5) -0.017(4) C(61) 0.095(6) 0.063(5) 0.057(4) 0.007(4) -0.012(4) 0.000(3) B(1) 0.053(5) 0.047(4) 0.055(4) 0.017(4) 0.002(3) 0.011(3) B(2) 0.072(6) 0.056(5) 0.067(5) 0.011(5) -0.024(4) 0.000(4) B(3) 0.19(1) 0.067(7) 0.083(7) -0.002(9) -0.009(9) 0.008(6) #------------------------------------------------------------------------------ _computing_data_collection D*TREK _computing_cell_refinement D*TREK _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N(1) 1.734(4) . . yes Ru N(2) 2.102(4) . . yes Ru N(4) 2.141(4) . . yes Ru N(6) 2.180(4) . . yes Ru C(10) 2.079(5) . . yes Ru C(36) 2.051(5) . . yes P(1) C(11) 1.819(5) . . yes P(1) C(18) 1.794(6) . . yes P(1) C(24) 1.800(6) . . yes P(1) C(30) 1.792(6) . . yes P(2) C(37) 1.809(5) . . yes P(2) C(44) 1.803(6) . . yes P(2) C(50) 1.798(6) . . yes P(2) C(56) 1.796(6) . . yes F(1) B(2) 1.293(9) . . yes F(2) B(2) 1.28(1) . . yes F(3) B(2) 1.296(9) . . yes F(4) B(2) 1.328(8) . . yes F(5) B(3) 1.35(1) . . yes F(6) B(3) 1.36(1) . . yes F(7) B(3) 1.36(1) . . yes F(8) B(3) 1.25(1) . . yes O N(1) 1.153(5) . . yes N(2) N(3) 1.350(5) . . yes N(2) C(1) 1.339(6) . . yes N(3) C(3) 1.345(6) . . yes N(3) B(1) 1.557(8) . . yes N(4) N(5) 1.354(6) . . yes N(4) C(4) 1.345(6) . . yes N(5) C(6) 1.355(7) . . yes N(5) B(1) 1.518(7) . . yes N(6) N(7) 1.359(6) . . yes N(6) C(7) 1.323(7) . . yes N(7) C(9) 1.341(7) . . yes N(7) B(1) 1.535(8) . . yes C(1) C(2) 1.374(7) . . yes C(2) C(3) 1.375(8) . . yes C(4) C(5) 1.348(8) . . yes C(5) C(6) 1.377(9) . . yes C(7) C(8) 1.407(8) . . yes C(8) C(9) 1.368(9) . . yes C(10) C(11) 1.333(7) . . yes C(11) C(12) 1.486(7) . . yes C(12) C(13) 1.407(7) . . yes C(12) C(17) 1.383(7) . . yes C(13) C(14) 1.379(8) . . yes C(14) C(15) 1.367(9) . . yes C(15) C(16) 1.372(9) . . yes C(16) C(17) 1.386(7) . . yes C(18) C(19) 1.397(8) . . yes C(18) C(23) 1.372(8) . . yes C(19) C(20) 1.402(9) . . yes C(20) C(21) 1.35(1) . . yes C(21) C(22) 1.38(1) . . yes C(22) C(23) 1.40(1) . . yes C(24) C(25) 1.388(8) . . yes C(24) C(29) 1.377(8) . . yes C(25) C(26) 1.387(9) . . yes C(26) C(27) 1.356(9) . . yes C(27) C(28) 1.36(1) . . yes C(28) C(29) 1.396(9) . . yes C(30) C(31) 1.396(7) . . yes C(30) C(35) 1.360(8) . . yes C(31) C(32) 1.375(9) . . yes C(32) C(33) 1.360(10) . . yes C(33) C(34) 1.38(1) . . yes C(34) C(35) 1.377(10) . . yes C(36) C(37) 1.337(6) . . yes C(37) C(38) 1.497(7) . . yes C(38) C(39) 1.393(7) . . yes C(38) C(43) 1.376(8) . . yes C(39) C(40) 1.393(8) . . yes C(40) C(41) 1.366(9) . . yes C(41) C(42) 1.365(8) . . yes C(42) C(43) 1.392(7) . . yes C(44) C(45) 1.388(7) . . yes C(44) C(49) 1.393(7) . . yes C(45) C(46) 1.372(8) . . yes C(46) C(47) 1.342(9) . . yes C(47) C(48) 1.362(9) . . yes C(48) C(49) 1.407(9) . . yes C(50) C(51) 1.381(8) . . yes C(50) C(55) 1.398(7) . . yes C(51) C(52) 1.405(9) . . yes C(52) C(53) 1.36(1) . . yes C(53) C(54) 1.388(10) . . yes C(54) C(55) 1.372(9) . . yes C(56) C(57) 1.390(8) . . yes C(56) C(61) 1.388(9) . . yes C(57) C(58) 1.416(10) . . yes C(58) C(59) 1.39(1) . . yes C(59) C(60) 1.34(1) . . yes C(60) C(61) 1.396(9) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Ru N(2) 176.5(2) . . . yes N(1) Ru N(4) 93.9(2) . . . yes N(1) Ru N(6) 93.4(2) . . . yes N(1) Ru C(10) 97.5(2) . . . yes N(1) Ru C(36) 96.5(2) . . . yes N(2) Ru N(4) 84.1(2) . . . yes N(2) Ru N(6) 83.5(2) . . . yes N(2) Ru C(10) 84.1(2) . . . yes N(2) Ru C(36) 86.5(2) . . . yes N(4) Ru N(6) 84.8(2) . . . yes N(4) Ru C(10) 166.7(2) . . . yes N(4) Ru C(36) 92.6(2) . . . yes N(6) Ru C(10) 87.7(2) . . . yes N(6) Ru C(36) 169.9(2) . . . yes C(10) Ru C(36) 93.0(2) . . . yes C(11) P(1) C(18) 112.0(2) . . . yes C(11) P(1) C(24) 108.3(2) . . . yes C(11) P(1) C(30) 111.6(2) . . . yes C(18) P(1) C(24) 109.7(3) . . . yes C(18) P(1) C(30) 106.3(3) . . . yes C(24) P(1) C(30) 108.9(3) . . . yes C(37) P(2) C(44) 108.9(3) . . . yes C(37) P(2) C(50) 112.3(2) . . . yes C(37) P(2) C(56) 111.3(2) . . . yes C(44) P(2) C(50) 107.4(2) . . . yes C(44) P(2) C(56) 110.9(3) . . . yes C(50) P(2) C(56) 106.0(3) . . . yes Ru N(1) O 173.3(4) . . . yes Ru N(2) N(3) 120.7(3) . . . yes Ru N(2) C(1) 132.7(4) . . . yes N(3) N(2) C(1) 106.3(4) . . . yes N(2) N(3) C(3) 109.2(4) . . . yes N(2) N(3) B(1) 120.2(4) . . . yes C(3) N(3) B(1) 130.4(5) . . . yes Ru N(4) N(5) 119.9(3) . . . yes Ru N(4) C(4) 134.1(4) . . . yes N(5) N(4) C(4) 105.3(4) . . . yes N(4) N(5) C(6) 110.1(5) . . . yes N(4) N(5) B(1) 120.4(4) . . . yes C(6) N(5) B(1) 129.2(5) . . . yes Ru N(6) N(7) 119.4(3) . . . yes Ru N(6) C(7) 133.4(4) . . . yes N(7) N(6) C(7) 107.1(5) . . . yes N(6) N(7) C(9) 109.0(5) . . . yes N(6) N(7) B(1) 119.7(4) . . . yes C(9) N(7) B(1) 131.2(5) . . . yes N(2) C(1) C(2) 111.2(5) . . . yes C(1) C(2) C(3) 104.2(5) . . . yes N(3) C(3) C(2) 109.1(5) . . . yes N(4) C(4) C(5) 111.5(6) . . . yes C(4) C(5) C(6) 106.0(5) . . . yes N(5) C(6) C(5) 107.1(5) . . . yes N(6) C(7) C(8) 110.4(6) . . . yes C(7) C(8) C(9) 104.0(5) . . . yes N(7) C(9) C(8) 109.5(6) . . . yes Ru C(10) C(11) 139.2(4) . . . yes P(1) C(11) C(10) 116.4(4) . . . yes P(1) C(11) C(12) 116.2(4) . . . yes C(10) C(11) C(12) 127.3(5) . . . yes C(11) C(12) C(13) 120.2(5) . . . yes C(11) C(12) C(17) 121.4(5) . . . yes C(13) C(12) C(17) 118.1(5) . . . yes C(12) C(13) C(14) 119.8(5) . . . yes C(13) C(14) C(15) 121.3(6) . . . yes C(14) C(15) C(16) 119.7(5) . . . yes C(15) C(16) C(17) 120.0(6) . . . yes C(12) C(17) C(16) 121.2(5) . . . yes P(1) C(18) C(19) 117.6(4) . . . yes P(1) C(18) C(23) 122.7(5) . . . yes C(19) C(18) C(23) 119.7(6) . . . yes C(18) C(19) C(20) 120.3(6) . . . yes C(19) C(20) C(21) 118.9(7) . . . yes C(20) C(21) C(22) 122.1(7) . . . yes C(21) C(22) C(23) 119.2(7) . . . yes C(18) C(23) C(22) 119.8(7) . . . yes P(1) C(24) C(25) 118.9(5) . . . yes P(1) C(24) C(29) 122.2(5) . . . yes C(25) C(24) C(29) 118.8(6) . . . yes C(24) C(25) C(26) 120.2(6) . . . yes C(25) C(26) C(27) 120.6(7) . . . yes C(26) C(27) C(28) 119.7(7) . . . yes C(27) C(28) C(29) 120.8(7) . . . yes C(24) C(29) C(28) 119.7(7) . . . yes P(1) C(30) C(31) 119.4(4) . . . yes P(1) C(30) C(35) 122.4(4) . . . yes C(31) C(30) C(35) 118.2(6) . . . yes C(30) C(31) C(32) 121.0(6) . . . yes C(31) C(32) C(33) 120.1(6) . . . yes C(32) C(33) C(34) 119.4(7) . . . yes C(33) C(34) C(35) 120.5(7) . . . yes C(30) C(35) C(34) 120.9(6) . . . yes Ru C(36) C(37) 135.6(4) . . . yes P(2) C(37) C(36) 120.0(4) . . . yes P(2) C(37) C(38) 112.7(3) . . . yes C(36) C(37) C(38) 127.2(5) . . . yes C(37) C(38) C(39) 121.5(5) . . . yes C(37) C(38) C(43) 119.9(5) . . . yes C(39) C(38) C(43) 118.6(5) . . . yes C(38) C(39) C(40) 120.1(6) . . . yes C(39) C(40) C(41) 120.3(5) . . . yes C(40) C(41) C(42) 120.1(5) . . . yes C(41) C(42) C(43) 120.1(6) . . . yes C(38) C(43) C(42) 120.8(5) . . . yes P(2) C(44) C(45) 118.5(4) . . . yes P(2) C(44) C(49) 122.3(4) . . . yes C(45) C(44) C(49) 119.2(5) . . . yes C(44) C(45) C(46) 119.8(6) . . . yes C(45) C(46) C(47) 121.6(6) . . . yes C(46) C(47) C(48) 120.3(6) . . . yes C(47) C(48) C(49) 120.2(6) . . . yes C(44) C(49) C(48) 118.8(6) . . . yes P(2) C(50) C(51) 120.8(4) . . . yes P(2) C(50) C(55) 119.2(4) . . . yes C(51) C(50) C(55) 119.5(5) . . . yes C(50) C(51) C(52) 119.5(6) . . . yes C(51) C(52) C(53) 120.3(7) . . . yes C(52) C(53) C(54) 120.4(7) . . . yes C(53) C(54) C(55) 119.9(6) . . . yes C(50) C(55) C(54) 120.4(6) . . . yes P(2) C(56) C(57) 120.2(5) . . . yes P(2) C(56) C(61) 119.6(5) . . . yes C(57) C(56) C(61) 120.1(6) . . . yes C(56) C(57) C(58) 117.7(8) . . . yes C(57) C(58) C(59) 120.9(8) . . . yes C(58) C(59) C(60) 120.4(7) . . . yes C(59) C(60) C(61) 120.5(9) . . . yes C(56) C(61) C(60) 120.3(7) . . . yes N(3) B(1) N(5) 109.3(5) . . . yes N(3) B(1) N(7) 106.2(5) . . . yes N(5) B(1) N(7) 108.8(5) . . . yes F(1) B(2) F(2) 103.3(9) . . . yes F(1) B(2) F(3) 113.0(7) . . . yes F(1) B(2) F(4) 113.4(8) . . . yes F(2) B(2) F(3) 105.3(9) . . . yes F(2) B(2) F(4) 106.8(8) . . . yes F(3) B(2) F(4) 113.9(7) . . . yes F(5) B(3) F(6) 110.6(9) . . . yes F(5) B(3) F(7) 102.1(9) . . . yes F(5) B(3) F(8) 112(1) . . . yes F(6) B(3) F(7) 106(1) . . . yes F(6) B(3) F(8) 113.9(10) . . . yes F(7) B(3) F(8) 110(1) . . . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ru N(2) N(3) C(3) -173.9(4) . . . . yes Ru N(2) N(3) B(1) 1.0(6) . . . . yes Ru N(2) C(1) C(2) 173.5(4) . . . . yes Ru N(4) N(5) C(6) 170.1(4) . . . . yes Ru N(4) N(5) B(1) -4.7(6) . . . . yes Ru N(4) C(4) C(5) -168.4(4) . . . . yes Ru N(6) N(7) C(9) -177.5(3) . . . . yes Ru N(6) N(7) B(1) -0.6(6) . . . . yes Ru N(6) C(7) C(8) 176.9(4) . . . . yes Ru C(10) C(11) P(1) 174.8(4) . . . . yes Ru C(10) C(11) C(12) 0(1) . . . . yes Ru C(36) C(37) P(2) 177.9(3) . . . . yes Ru C(36) C(37) C(38) 3.5(9) . . . . yes P(1) C(11) C(12) C(13) 73.5(6) . . . . yes P(1) C(11) C(12) C(17) -100.2(5) . . . . yes P(1) C(18) C(19) C(20) -177.1(5) . . . . yes P(1) C(18) C(23) C(22) 178.4(6) . . . . yes P(1) C(24) C(25) C(26) -176.3(5) . . . . yes P(1) C(24) C(29) C(28) 176.7(5) . . . . yes P(1) C(30) C(31) C(32) -177.4(5) . . . . yes P(1) C(30) C(35) C(34) 177.9(7) . . . . yes P(2) C(37) C(38) C(39) 82.4(6) . . . . yes P(2) C(37) C(38) C(43) -95.3(5) . . . . yes P(2) C(44) C(45) C(46) 179.9(5) . . . . yes P(2) C(44) C(49) C(48) -178.6(5) . . . . yes P(2) C(50) C(51) C(52) -173.8(5) . . . . yes P(2) C(50) C(55) C(54) 172.5(5) . . . . yes P(2) C(56) C(57) C(58) 178.8(5) . . . . yes P(2) C(56) C(61) C(60) -178.2(5) . . . . yes O N(1) Ru N(2) -4(6) . . . . yes O N(1) Ru N(4) 50(3) . . . . yes O N(1) Ru N(6) -34(3) . . . . yes O N(1) Ru C(10) -122(3) . . . . yes O N(1) Ru C(36) 143(3) . . . . yes N(1) Ru N(2) N(3) 13(3) . . . . yes N(1) Ru N(2) C(1) -159(2) . . . . yes N(1) Ru N(4) N(5) -131.8(4) . . . . yes N(1) Ru N(4) C(4) 36.4(5) . . . . yes N(1) Ru N(6) N(7) 135.0(3) . . . . yes N(1) Ru N(6) C(7) -41.3(5) . . . . yes N(1) Ru C(10) C(11) -35.0(7) . . . . yes N(1) Ru C(36) C(37) -16.5(6) . . . . yes N(2) Ru N(4) N(5) 45.2(4) . . . . yes N(2) Ru N(4) C(4) -146.5(5) . . . . yes N(2) Ru N(6) N(7) -43.3(3) . . . . yes N(2) Ru N(6) C(7) 140.5(5) . . . . yes N(2) Ru C(10) C(11) 148.2(6) . . . . yes N(2) Ru C(36) C(37) 161.6(6) . . . . yes N(2) N(3) C(3) C(2) -0.7(7) . . . . yes N(2) N(3) B(1) N(5) 56.3(7) . . . . yes N(2) N(3) B(1) N(7) -61.0(6) . . . . yes N(2) C(1) C(2) C(3) -0.7(7) . . . . yes N(3) N(2) Ru N(4) -42.7(4) . . . . yes N(3) N(2) Ru N(6) 42.6(4) . . . . yes N(3) N(2) Ru C(10) 131.0(4) . . . . yes N(3) N(2) Ru C(36) -135.7(4) . . . . yes N(3) N(2) C(1) C(2) 0.3(6) . . . . yes N(3) C(3) C(2) C(1) 0.8(7) . . . . yes N(3) B(1) N(5) N(4) -53.3(7) . . . . yes N(3) B(1) N(5) C(6) 133.0(6) . . . . yes N(3) B(1) N(7) N(6) 59.2(6) . . . . yes N(3) B(1) N(7) C(9) -124.7(6) . . . . yes N(4) Ru N(2) C(1) 144.9(5) . . . . yes N(4) Ru N(6) N(7) 41.4(3) . . . . yes N(4) Ru N(6) C(7) -134.9(5) . . . . yes N(4) Ru C(10) C(11) 176.3(6) . . . . yes N(4) Ru C(36) C(37) 77.7(6) . . . . yes N(4) N(5) C(6) C(5) 0.8(7) . . . . yes N(4) N(5) B(1) N(7) 62.3(6) . . . . yes N(4) C(4) C(5) C(6) -0.5(8) . . . . yes N(5) N(4) Ru N(6) -38.7(4) . . . . yes N(5) N(4) Ru C(10) 17(1) . . . . yes N(5) N(4) Ru C(36) 131.5(4) . . . . yes N(5) N(4) C(4) C(5) 1.0(7) . . . . yes N(5) C(6) C(5) C(4) -0.2(8) . . . . yes N(5) B(1) N(3) C(3) -130.0(6) . . . . yes N(5) B(1) N(7) N(6) -58.3(6) . . . . yes N(5) B(1) N(7) C(9) 117.8(6) . . . . yes N(6) Ru N(2) C(1) -129.8(5) . . . . yes N(6) Ru N(4) C(4) 129.5(5) . . . . yes N(6) Ru C(10) C(11) -128.1(6) . . . . yes N(6) Ru C(36) C(37) 152.1(8) . . . . yes N(6) N(7) C(9) C(8) 0.3(6) . . . . yes N(6) C(7) C(8) C(9) -0.1(6) . . . . yes N(7) N(6) Ru C(10) -127.6(4) . . . . yes N(7) N(6) Ru C(36) -33(1) . . . . yes N(7) N(6) C(7) C(8) 0.3(6) . . . . yes N(7) C(9) C(8) C(7) -0.1(7) . . . . yes N(7) B(1) N(3) C(3) 112.8(6) . . . . yes N(7) B(1) N(5) C(6) -111.4(6) . . . . yes C(1) N(2) Ru C(10) -41.4(5) . . . . yes C(1) N(2) Ru C(36) 51.9(5) . . . . yes C(1) N(2) N(3) C(3) 0.2(6) . . . . yes C(1) N(2) N(3) B(1) 175.2(5) . . . . yes C(2) C(3) N(3) B(1) -175.0(6) . . . . yes C(4) N(4) Ru C(10) -174.7(7) . . . . yes C(4) N(4) Ru C(36) -60.3(5) . . . . yes C(4) N(4) N(5) C(6) -1.1(6) . . . . yes C(4) N(4) N(5) B(1) -175.9(5) . . . . yes C(5) C(6) N(5) B(1) 175.0(6) . . . . yes C(7) N(6) Ru C(10) 56.1(5) . . . . yes C(7) N(6) Ru C(36) 150.1(9) . . . . yes C(7) N(6) N(7) C(9) -0.4(6) . . . . yes C(7) N(6) N(7) B(1) 176.5(4) . . . . yes C(8) C(9) N(7) B(1) -176.1(5) . . . . yes C(10) Ru C(36) C(37) -114.4(6) . . . . yes C(10) C(11) P(1) C(18) 161.4(4) . . . . yes C(10) C(11) P(1) C(24) 40.3(5) . . . . yes C(10) C(11) P(1) C(30) -79.6(5) . . . . yes C(10) C(11) C(12) C(13) -111.7(6) . . . . yes C(10) C(11) C(12) C(17) 74.6(8) . . . . yes C(11) P(1) C(18) C(19) 61.3(5) . . . . yes C(11) P(1) C(18) C(23) -119.6(5) . . . . yes C(11) P(1) C(24) C(25) 57.9(5) . . . . yes C(11) P(1) C(24) C(29) -118.9(5) . . . . yes C(11) P(1) C(30) C(31) -176.9(5) . . . . yes C(11) P(1) C(30) C(35) 3.0(7) . . . . yes C(11) C(10) Ru C(36) 62.0(6) . . . . yes C(11) C(12) C(13) C(14) -174.0(5) . . . . yes C(11) C(12) C(17) C(16) 174.3(5) . . . . yes C(12) C(11) P(1) C(18) -23.2(5) . . . . yes C(12) C(11) P(1) C(24) -144.4(4) . . . . yes C(12) C(11) P(1) C(30) 95.8(4) . . . . yes C(12) C(13) C(14) C(15) -0.1(10) . . . . yes C(12) C(17) C(16) C(15) -0.8(9) . . . . yes C(13) C(12) C(17) C(16) 0.5(8) . . . . yes C(13) C(14) C(15) C(16) 0(1) . . . . yes C(14) C(13) C(12) C(17) -0.1(8) . . . . yes C(14) C(15) C(16) C(17) 0(1) . . . . yes C(18) P(1) C(24) C(25) -64.6(5) . . . . yes C(18) P(1) C(24) C(29) 118.5(5) . . . . yes C(18) P(1) C(30) C(31) -54.5(5) . . . . yes C(18) P(1) C(30) C(35) 125.4(6) . . . . yes C(18) C(19) C(20) C(21) -2(1) . . . . yes C(18) C(23) C(22) C(21) 0(1) . . . . yes C(19) C(18) P(1) C(24) -178.4(5) . . . . yes C(19) C(18) P(1) C(30) -60.9(5) . . . . yes C(19) C(18) C(23) C(22) -2(1) . . . . yes C(19) C(20) C(21) C(22) 0(1) . . . . yes C(20) C(19) C(18) C(23) 3.8(10) . . . . yes C(20) C(21) C(22) C(23) 0(1) . . . . yes C(23) C(18) P(1) C(24) 0.7(6) . . . . yes C(23) C(18) P(1) C(30) 118.3(6) . . . . yes C(24) P(1) C(30) C(31) 63.7(6) . . . . yes C(24) P(1) C(30) C(35) -116.4(6) . . . . yes C(24) C(25) C(26) C(27) 0(1) . . . . yes C(24) C(29) C(28) C(27) -1(1) . . . . yes C(25) C(24) P(1) C(30) 179.4(4) . . . . yes C(25) C(24) C(29) C(28) -0.1(10) . . . . yes C(25) C(26) C(27) C(28) -1(1) . . . . yes C(26) C(25) C(24) C(29) 0.7(9) . . . . yes C(26) C(27) C(28) C(29) 1(1) . . . . yes C(29) C(24) P(1) C(30) 2.6(6) . . . . yes C(30) C(31) C(32) C(33) -1(1) . . . . yes C(30) C(35) C(34) C(33) 0(1) . . . . yes C(31) C(30) C(35) C(34) -2(1) . . . . yes C(31) C(32) C(33) C(34) 0(1) . . . . yes C(32) C(31) C(30) C(35) 2(1) . . . . yes C(32) C(33) C(34) C(35) 1(1) . . . . yes C(36) C(37) P(2) C(44) -126.2(4) . . . . yes C(36) C(37) P(2) C(50) 115.0(4) . . . . yes C(36) C(37) P(2) C(56) -3.6(5) . . . . yes C(36) C(37) C(38) C(39) -102.8(7) . . . . yes C(36) C(37) C(38) C(43) 79.5(7) . . . . yes C(37) P(2) C(44) C(45) -76.7(5) . . . . yes C(37) P(2) C(44) C(49) 100.3(5) . . . . yes C(37) P(2) C(50) C(51) -32.3(6) . . . . yes C(37) P(2) C(50) C(55) 156.2(4) . . . . yes C(37) P(2) C(56) C(57) -57.9(6) . . . . yes C(37) P(2) C(56) C(61) 120.9(5) . . . . yes C(37) C(38) C(39) C(40) -178.3(5) . . . . yes C(37) C(38) C(43) C(42) 179.3(5) . . . . yes C(38) C(37) P(2) C(44) 49.0(4) . . . . yes C(38) C(37) P(2) C(50) -69.8(4) . . . . yes C(38) C(37) P(2) C(56) 171.6(4) . . . . yes C(38) C(39) C(40) C(41) -1.5(9) . . . . yes C(38) C(43) C(42) C(41) -0.4(9) . . . . yes C(39) C(38) C(43) C(42) 1.5(8) . . . . yes C(39) C(40) C(41) C(42) 2.6(10) . . . . yes C(40) C(39) C(38) C(43) -0.5(8) . . . . yes C(40) C(41) C(42) C(43) -1.7(9) . . . . yes C(44) P(2) C(50) C(51) -152.0(5) . . . . yes C(44) P(2) C(50) C(55) 36.5(5) . . . . yes C(44) P(2) C(56) C(57) 63.5(5) . . . . yes C(44) P(2) C(56) C(61) -117.7(5) . . . . yes C(44) C(45) C(46) C(47) -1(1) . . . . yes C(44) C(49) C(48) C(47) -1(1) . . . . yes C(45) C(44) P(2) C(50) 45.1(5) . . . . yes C(45) C(44) P(2) C(56) 160.5(5) . . . . yes C(45) C(44) C(49) C(48) -1.6(9) . . . . yes C(45) C(46) C(47) C(48) -1(1) . . . . yes C(46) C(45) C(44) C(49) 2.8(9) . . . . yes C(46) C(47) C(48) C(49) 2(1) . . . . yes C(49) C(44) P(2) C(50) -137.9(5) . . . . yes C(49) C(44) P(2) C(56) -22.5(6) . . . . yes C(50) P(2) C(56) C(57) 179.8(5) . . . . yes C(50) P(2) C(56) C(61) -1.4(6) . . . . yes C(50) C(51) C(52) C(53) 2(1) . . . . yes C(50) C(55) C(54) C(53) 0(1) . . . . yes C(51) C(50) P(2) C(56) 89.4(5) . . . . yes C(51) C(50) C(55) C(54) 0.9(9) . . . . yes C(51) C(52) C(53) C(54) 0(1) . . . . yes C(52) C(51) C(50) C(55) -2.3(9) . . . . yes C(52) C(53) C(54) C(55) 0(1) . . . . yes C(55) C(50) P(2) C(56) -82.1(5) . . . . yes C(56) C(57) C(58) C(59) -1(1) . . . . yes C(56) C(61) C(60) C(59) 0(1) . . . . yes C(57) C(56) C(61) C(60) 0.6(10) . . . . yes C(57) C(58) C(59) C(60) 3(1) . . . . yes C(58) C(57) C(56) C(61) 0.0(9) . . . . yes C(58) C(59) C(60) C(61) -2(1) . . . . yes C(58) C(59) C(60) C(61) -2(1) . . . . yes #------------------------------------------------------------------------------ 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 F(1) C(47) 3.451(9) . 1_545 ? F(1) C(52) 3.47(1) . 2_555 ? F(1) C(39) 3.474(10) . 2_555 ? F(1) C(15) 3.495(8) . 2_455 ? F(2) C(53) 3.24(1) . 1_445 ? F(2) C(54) 3.40(1) . 1_445 ? F(3) C(17) 3.325(8) . . ? F(3) C(16) 3.328(9) . . ? F(3) C(16) 3.418(8) . 2_455 ? F(3) C(5) 3.479(9) . 1_455 ? F(3) C(5) 3.509(10) . 2_555 ? F(3) C(6) 3.556(9) . 1_455 ? F(4) C(7) 3.268(8) . . ? F(4) C(35) 3.347(8) . . ? F(4) O 3.404(8) . . ? F(4) C(34) 3.51(1) . . ? F(5) C(48) 3.44(1) . 1_655 ? F(5) C(33) 3.56(1) . 1_665 ? F(6) C(59) 3.324(9) . 2_666 ? F(6) C(57) 3.414(10) . 1_655 ? F(6) C(23) 3.524(10) . 1_655 ? F(6) C(58) 3.54(1) . 1_655 ? F(6) C(13) 3.583(8) . 1_655 ? F(7) C(27) 3.28(1) . 2_666 ? F(7) C(26) 3.34(1) . 2_666 ? F(7) C(49) 3.41(1) . 1_655 ? F(7) C(48) 3.51(1) . 1_655 ? F(7) C(33) 3.58(1) . 1_665 ? F(8) C(59) 3.24(1) . 2_666 ? F(8) C(22) 3.586(10) . 2_566 ? O C(40) 3.414(7) . 2_555 ? N(2) C(20) 3.507(8) . 1_655 ? N(3) C(20) 3.350(9) . 1_655 ? C(1) C(21) 3.53(1) . 1_655 ? C(2) C(21) 3.34(1) . 1_655 ? C(3) C(20) 3.432(10) . 1_655 ? C(3) C(21) 3.59(1) . 1_655 ? C(5) C(16) 3.476(9) . 1_655 ? C(8) C(49) 3.517(9) . 1_545 ? C(8) C(27) 3.517(8) . 2_556 ? C(28) C(28) 3.58(2) . 2_556 ? C(28) C(29) 3.60(1) . 2_556 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------