Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global #------------------------------------------------------------------------------ _journal_coden_Cambridge 186 _publ_requested_journal ' J.Chem. Soc. Dalton Transactions' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Prof. Mike Wolf' _publ_contact_author_address ; Dept. Of Chemistry University of British Columbia 2036 Main Mall Vancouver, B.C., Canada V6T 1Z1 ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' (604) 822-1702 ' _publ_contact_author_fax ' (604) 822-2847 ' _publ_contact_author_email ' mwolf@chem.ubc.ca ' loop_ _publ_author_name 'Patrick, Brian O.' 'Rettig, Steven J.' 'Rogers, Cerrie W.' 'Wolf, Michael' _publ_section_title ; Ligand-assisted O-dealkylation of bis(bipyridyl) Ru(II) phosphine-ether complexes. ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1996-1998). d*TREK. Area Detector Software. Version 4.4. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Altomare, A., Burla, M.C., Cammalli, G., Cascarano, M., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G., Polidori, G., Spagna, A. (1998). SIR97: a new tool for crystal structure determination and refinement. Submitted. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_mw004 _database_code_CSD 153809 #------------------------------------------------------------------------------ _audit_creation_date '2000-03-07' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _computing_data_collection 'd*TREK (MSC, 1996-1998)' _computing_cell_refinement 'd*TREK (MSC, 1996-1998)' _computing_data_reduction 'd*TREK (MSC, 1996-1998)' _computing_structure_solution ; SIR97 (Altomare, et. al. 1998) ; _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 12.0656(4) _cell_length_b 20.2301(5) _cell_length_c 16.9836(6) _cell_angle_alpha 90 _cell_angle_beta 102.651(2) _cell_angle_gamma 90 _cell_volume 4044.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? 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' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 995.69 _chemical_formula_analytical ? _chemical_formula_sum 'C39 H33 F12 N4 O P3 Ru ' _chemical_formula_moiety 'C39 H33 F12 N4 O P3 Ru ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2000.00 _exptl_absorpt_coefficient_mu 0.600 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.7658 _exptl_special_details ; Data were collected in 0.50\% oscillations with 19.0 s exposures. A sweep of data was done using \f oscillations from 0.0 to 190.0\% at \c = -90\% and a second sweep was performed using \w oscillations between -19.0 and 23.0\% at \c = 90.0\%. The crystal-to-detector distance was 40.58 mm. The detector swing angle was -5.55\%. The absorption correction is based on a three-dimensional analysis of symmetry-equivalent data and is performed along with batch scaling in a single step. The resulting transmission factors, therefore, include contributions from absorption, crystal decay, and detectable variations in beam intensity. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_detector_area_resol_mean 11.76 _diffrn_measurement_method 'area detector' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 33540 _reflns_number_total 8759 _reflns_number_gt 7434 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.03762 _diffrn_reflns_av_sigmaI/netI 0.070 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.98 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 156 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 132 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 16 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 4 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 48 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 12 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 4 -1.420 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.54113(1) 0.233937(6) 0.866019(8) 0.01739(4) 1.000 . Uani d ? P(1) 0.55671(4) 0.21474(2) 1.00094(3) 0.0192(1) 1.000 . Uani d ? P(2) 0.14991(5) 0.41138(3) 0.94618(4) 0.0393(2) 1.000 . Uani d ? P(3) 0.87360(5) 0.00879(3) 0.81550(3) 0.0317(1) 1.000 . Uani d ? F(1A) 0.2733(2) 0.3850(2) 0.9786(2) 0.101(1) 0.833 S Uani d ? F(1B) 0.204(3) 0.3362(6) 0.9565(9) 0.170(7) 0.167 S Uani d ? F(2A) 0.2021(3) 0.4798(2) 0.9247(2) 0.090(1) 0.833 S Uani d ? F(2B) 0.262(1) 0.430(1) 0.924(1) 0.093(5) 0.167 S Uani d ? F(3A) 0.0273(2) 0.4420(1) 0.9145(1) 0.0677(7) 0.833 S Uani d ? F(3B) 0.122(2) 0.4821(6) 0.9322(8) 0.109(6) 0.167 S Uani d ? F(4A) 0.0962(3) 0.3442(1) 0.9652(1) 0.0654(7) 0.833 S Uani d ? F(4B) 0.029(1) 0.402(1) 0.9632(6) 0.126(6) 0.167 S Uani d ? F(5A) 0.1479(5) 0.3867(3) 0.8578(3) 0.087(2) 0.750 S Uani d ? F(5B) 0.111(1) 0.3868(8) 0.8502(9) 0.062(3) 0.250 S Uani d ? F(6A) 0.1488(4) 0.4381(2) 1.0349(3) 0.062(1) 0.750 S Uani d ? F(6B) 0.192(1) 0.4215(8) 1.035(1) 0.071(4) 0.250 S Uani d ? F(7) 0.7822(1) -0.04655(7) 0.78095(9) 0.0514(4) 1.000 . Uani d ? F(8) 0.9666(1) 0.06358(8) 0.8493(1) 0.0688(5) 1.000 . Uani d ? F(9) 0.9275(1) -0.03756(7) 0.88974(8) 0.0513(4) 1.000 . Uani d ? F(10) 0.9566(1) -0.02210(9) 0.76397(9) 0.0624(5) 1.000 . Uani d ? F(11) 0.8196(1) 0.05617(8) 0.74217(9) 0.0592(5) 1.000 . Uani d ? F(12) 0.7892(1) 0.03866(8) 0.86611(9) 0.0570(5) 1.000 . Uani d ? O(1) 0.3626(1) 0.22952(6) 0.86968(8) 0.0265(3) 1.000 . Uani d ? N(1) 0.5620(1) 0.33320(7) 0.88880(9) 0.0209(4) 1.000 . Uani d ? N(2) 0.7060(1) 0.24608(7) 0.8598(1) 0.0229(4) 1.000 . Uani d ? N(3) 0.5205(1) 0.13615(7) 0.82474(9) 0.0217(4) 1.000 . Uani d ? N(4) 0.5124(1) 0.24577(7) 0.73956(9) 0.0234(4) 1.000 . Uani d ? C(1) 0.4825(2) 0.37421(9) 0.9058(1) 0.0268(5) 1.000 . Uani d ? C(2) 0.5034(2) 0.44063(9) 0.9211(1) 0.0337(5) 1.000 . Uani d ? C(3) 0.6099(2) 0.46586(9) 0.9208(1) 0.0369(6) 1.000 . Uani d ? C(4) 0.6919(2) 0.42448(9) 0.9033(1) 0.0326(5) 1.000 . Uani d ? C(5) 0.6654(2) 0.35840(9) 0.8865(1) 0.0241(4) 1.000 . Uani d ? C(6) 0.7445(2) 0.30970(9) 0.8651(1) 0.0256(5) 1.000 . Uani d ? C(7) 0.8479(2) 0.3261(1) 0.8490(2) 0.0421(6) 1.000 . Uani d ? C(8) 0.9151(2) 0.2774(1) 0.8269(2) 0.0522(8) 1.000 . Uani d ? C(9) 0.8775(2) 0.2131(1) 0.8223(2) 0.0439(7) 1.000 . Uani d ? C(10) 0.7731(2) 0.1988(1) 0.8389(1) 0.0303(5) 1.000 . Uani d ? C(11) 0.5075(2) 0.08225(9) 0.8682(1) 0.0278(5) 1.000 . Uani d ? C(12) 0.4982(2) 0.0189(1) 0.8364(1) 0.0375(6) 1.000 . Uani d ? C(13) 0.5046(2) 0.0103(1) 0.7574(1) 0.0457(7) 1.000 . Uani d ? C(14) 0.5140(2) 0.0648(1) 0.7110(1) 0.0379(6) 1.000 . Uani d ? C(15) 0.5194(2) 0.12752(9) 0.7452(1) 0.0263(5) 1.000 . Uani d ? C(16) 0.5172(2) 0.18878(9) 0.6983(1) 0.0280(5) 1.000 . Uani d ? C(17) 0.5156(2) 0.1901(1) 0.6163(1) 0.0485(7) 1.000 . Uani d ? C(18) 0.5080(3) 0.2499(1) 0.5763(1) 0.0549(8) 1.000 . Uani d ? C(19) 0.5015(2) 0.3074(1) 0.6179(1) 0.0423(6) 1.000 . Uani d ? C(20) 0.5051(2) 0.30364(9) 0.6996(1) 0.0302(5) 1.000 . Uani d ? C(21) 0.2745(2) 0.2492(1) 0.8019(1) 0.0400(6) 1.000 . Uani d ? C(22) 0.3305(2) 0.19301(9) 0.9307(1) 0.0254(5) 1.000 . Uani d ? C(23) 0.2228(2) 0.1662(1) 0.9216(1) 0.0372(6) 1.000 . Uani d ? C(24) 0.1976(2) 0.1302(1) 0.9851(2) 0.0502(7) 1.000 . Uani d ? C(25) 0.2773(2) 0.1212(1) 1.0554(2) 0.0527(8) 1.000 . Uani d ? C(26) 0.3845(2) 0.1482(1) 1.0633(1) 0.0398(6) 1.000 . Uani d ? C(27) 0.4142(2) 0.18355(9) 1.0007(1) 0.0250(5) 1.000 . Uani d ? C(28) 0.6539(2) 0.15371(9) 1.0582(1) 0.0229(4) 1.000 . Uani d ? C(29) 0.7164(2) 0.1127(1) 1.0182(1) 0.0279(5) 1.000 . Uani d ? C(30) 0.7849(2) 0.0632(1) 1.0596(1) 0.0374(6) 1.000 . Uani d ? C(31) 0.7921(2) 0.0545(1) 1.1412(1) 0.0399(6) 1.000 . Uani d ? C(32) 0.7334(2) 0.0962(1) 1.1823(1) 0.0362(6) 1.000 . Uani d ? C(33) 0.6653(2) 0.1460(1) 1.1414(1) 0.0287(5) 1.000 . Uani d ? C(34) 0.5771(2) 0.28586(9) 1.0684(1) 0.0250(5) 1.000 . Uani d ? C(35) 0.6821(2) 0.3174(1) 1.0828(1) 0.0329(5) 1.000 . Uani d ? C(36) 0.7002(2) 0.3747(1) 1.1292(1) 0.0490(7) 1.000 . Uani d ? C(37) 0.6147(3) 0.3991(1) 1.1629(1) 0.0572(8) 1.000 . Uani d ? C(38) 0.5108(3) 0.3683(1) 1.1497(1) 0.0548(8) 1.000 . Uani d ? C(39) 0.4908(2) 0.3118(1) 1.1020(1) 0.0392(6) 1.000 . Uani d ? H(1) 0.4077 0.3563 0.9078 0.032 1.000 . Uiso c ? H(2) 0.4434 0.4697 0.9320 0.041 1.000 . Uiso c ? H(3) 0.6268 0.5126 0.9327 0.044 1.000 . Uiso c ? H(4) 0.7677 0.4414 0.9028 0.039 1.000 . Uiso c ? H(5) 0.8736 0.3721 0.8526 0.051 1.000 . Uiso c ? H(6) 0.9894 0.2883 0.8160 0.063 1.000 . Uiso c ? H(7) 0.9244 0.1777 0.8073 0.053 1.000 . Uiso c ? H(8) 0.7468 0.1528 0.8354 0.036 1.000 . Uiso c ? H(9) 0.5047 0.0880 0.9250 0.033 1.000 . Uiso c ? H(10) 0.4878 -0.0191 0.8698 0.045 1.000 . Uiso c ? H(11) 0.5017 -0.0342 0.7344 0.055 1.000 . Uiso c ? H(12) 0.5166 0.0594 0.6541 0.045 1.000 . Uiso c ? H(13) 0.5191 0.1488 0.5869 0.058 1.000 . Uiso c ? H(14) 0.5077 0.2514 0.5186 0.066 1.000 . Uiso c ? H(15) 0.4948 0.3503 0.5902 0.051 1.000 . Uiso c ? H(16) 0.5018 0.3446 0.7296 0.036 1.000 . Uiso c ? H(17) 0.3051 0.2808 0.7682 0.050 1.000 . Uiso c ? H(18) 0.2117 0.2700 0.8209 0.050 1.000 . Uiso c ? H(19) 0.2456 0.2102 0.7690 0.050 1.000 . Uiso c ? H(20) 0.1657 0.1724 0.8714 0.044 1.000 . Uiso c ? H(21) 0.1216 0.1110 0.9796 0.060 1.000 . Uiso c ? H(22) 0.2587 0.0955 1.0997 0.064 1.000 . Uiso c ? H(23) 0.4408 0.1422 1.1140 0.048 1.000 . Uiso c ? H(24) 0.7121 0.1189 0.9605 0.034 1.000 . Uiso c ? H(25) 0.8282 0.0345 1.0309 0.045 1.000 . Uiso c ? H(26) 0.8391 0.0189 1.1701 0.048 1.000 . Uiso c ? H(27) 0.7396 0.0905 1.2403 0.044 1.000 . Uiso c ? H(28) 0.6251 0.1758 1.1709 0.034 1.000 . Uiso c ? H(29) 0.7438 0.2994 1.0600 0.040 1.000 . Uiso c ? H(30) 0.7736 0.3974 1.1379 0.059 1.000 . Uiso c ? H(31) 0.6286 0.4391 1.1963 0.068 1.000 . Uiso c ? H(32) 0.4511 0.3860 1.1745 0.066 1.000 . Uiso c ? H(33) 0.4159 0.2905 1.0916 0.046 1.000 . Uiso c ? 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(1) 0.02081(8) 0.01217(7) 0.01976(8) -0.00060(5) 0.00571(5) -0.00239(5) P(1) 0.0212(2) 0.0163(2) 0.0204(2) 0.0005(2) 0.0053(2) -0.0010(2) P(2) 0.0388(3) 0.0408(3) 0.0401(3) -0.0033(3) 0.0124(3) 0.0084(3) P(3) 0.0341(3) 0.0299(3) 0.0330(3) 0.0004(2) 0.0114(2) 0.0048(2) F(1) 0.054(1) 0.129(3) 0.124(2) 0.039(2) 0.032(2) 0.039(2) F(1) 0.35(3) 0.021(5) 0.083(9) 0.07(1) -0.08(1) -0.018(6) F(2) 0.088(2) 0.083(2) 0.091(2) -0.048(2) 0.003(2) 0.031(2) F(2) 0.049(7) 0.12(1) 0.13(1) -0.040(7) 0.052(8) -0.06(1) F(3) 0.052(1) 0.068(1) 0.077(2) 0.007(1) 0.000(1) 0.003(1) F(3) 0.24(2) 0.034(6) 0.064(8) 0.05(1) 0.05(1) 0.010(6) F(4) 0.113(2) 0.040(1) 0.048(1) -0.025(1) 0.028(1) 0.008(1) F(4) 0.080(9) 0.26(2) 0.035(5) -0.11(1) 0.004(6) 0.02(1) F(5) 0.154(6) 0.077(2) 0.047(2) -0.003(3) 0.058(3) -0.004(2) F(5) 0.066(6) 0.057(5) 0.057(5) -0.013(4) -0.004(4) 0.036(4) F(6) 0.074(3) 0.066(2) 0.046(2) -0.006(2) 0.017(2) -0.016(2) F(6) 0.070(9) 0.072(8) 0.060(5) -0.001(5) -0.006(6) -0.008(5) F(7) 0.0513(9) 0.0473(8) 0.0556(8) -0.0149(7) 0.0119(7) -0.0062(7) F(8) 0.070(1) 0.0513(9) 0.078(1) -0.0255(8) -0.0011(9) 0.0012(8) F(9) 0.0563(9) 0.0497(8) 0.0460(8) 0.0094(7) 0.0068(7) 0.0181(7) F(10) 0.0432(9) 0.097(1) 0.0521(8) 0.0107(8) 0.0219(7) -0.0072(8) F(11) 0.0520(9) 0.068(1) 0.0562(9) 0.0014(7) 0.0093(7) 0.0358(8) F(12) 0.071(1) 0.0542(9) 0.0548(8) 0.0176(8) 0.0325(8) -0.0032(7) O(1) 0.0213(7) 0.0312(7) 0.0262(6) 0.0022(5) 0.0036(5) 0.0050(6) N(1) 0.0289(8) 0.0137(7) 0.0205(7) 0.0001(6) 0.0063(6) -0.0027(6) N(2) 0.0245(8) 0.0180(7) 0.0273(7) -0.0008(6) 0.0081(6) -0.0017(6) N(3) 0.0227(8) 0.0158(7) 0.0261(8) -0.0020(6) 0.0044(6) -0.0030(6) N(4) 0.0287(9) 0.0198(7) 0.0226(7) 0.0005(6) 0.0075(6) -0.0027(6) C(1) 0.037(1) 0.0206(9) 0.0242(9) 0.0048(8) 0.0105(8) -0.0019(7) C(2) 0.055(1) 0.0184(9) 0.030(1) 0.0081(9) 0.0129(9) -0.0026(8) C(3) 0.062(1) 0.0154(8) 0.033(1) -0.0041(9) 0.009(1) -0.0055(8) C(4) 0.045(1) 0.0199(9) 0.033(1) -0.0110(8) 0.0079(9) -0.0031(8) C(5) 0.032(1) 0.0176(8) 0.0225(9) -0.0030(7) 0.0049(7) -0.0006(7) C(6) 0.027(1) 0.0214(9) 0.0279(9) -0.0048(7) 0.0046(8) -0.0015(8) C(7) 0.032(1) 0.032(1) 0.065(2) -0.0114(9) 0.017(1) -0.005(1) C(8) 0.031(1) 0.047(1) 0.086(2) -0.009(1) 0.027(1) -0.004(1) C(9) 0.033(1) 0.038(1) 0.066(2) 0.0028(9) 0.022(1) -0.007(1) C(10) 0.029(1) 0.0239(9) 0.041(1) 0.0001(8) 0.0141(9) -0.0040(8) C(11) 0.030(1) 0.0177(8) 0.033(1) -0.0029(7) 0.0024(8) -0.0012(8) C(12) 0.047(1) 0.0168(9) 0.045(1) -0.0060(8) 0.002(1) 0.0001(9) C(13) 0.062(2) 0.0182(9) 0.051(1) -0.000(1) 0.000(1) -0.011(1) C(14) 0.053(1) 0.024(1) 0.036(1) 0.0030(9) 0.008(1) -0.0115(9) C(15) 0.028(1) 0.0210(9) 0.030(1) -0.0006(7) 0.0073(8) -0.0066(8) C(16) 0.035(1) 0.0225(9) 0.029(1) -0.0003(8) 0.0117(8) -0.0057(8) C(17) 0.087(2) 0.033(1) 0.033(1) 0.000(1) 0.028(1) -0.009(1) C(18) 0.101(2) 0.043(1) 0.028(1) 0.001(1) 0.030(1) -0.001(1) C(19) 0.066(2) 0.033(1) 0.031(1) -0.001(1) 0.017(1) 0.0055(9) C(20) 0.044(1) 0.0203(9) 0.0272(9) 0.0013(8) 0.0111(9) -0.0005(8) C(21) 0.029(1) 0.056(1) 0.031(1) 0.005(1) -0.0022(9) 0.008(1) C(22) 0.024(1) 0.0226(9) 0.0316(9) 0.0006(7) 0.0097(8) 0.0017(8) C(23) 0.023(1) 0.040(1) 0.048(1) -0.0039(9) 0.0056(9) 0.001(1) C(24) 0.031(1) 0.053(1) 0.070(2) -0.012(1) 0.017(1) 0.011(1) C(25) 0.042(1) 0.060(2) 0.059(2) -0.010(1) 0.018(1) 0.024(1) C(26) 0.034(1) 0.045(1) 0.040(1) -0.003(1) 0.010(1) 0.014(1) C(27) 0.024(1) 0.0219(9) 0.0304(9) -0.0013(7) 0.0089(8) 0.0018(8) C(28) 0.0229(9) 0.0203(8) 0.0241(9) -0.0006(7) 0.0018(7) -0.0012(7) C(29) 0.028(1) 0.0264(9) 0.0286(9) 0.0045(7) 0.0039(8) -0.0019(8) C(30) 0.033(1) 0.032(1) 0.046(1) 0.0110(9) 0.006(1) -0.003(1) C(31) 0.035(1) 0.034(1) 0.045(1) 0.0084(9) -0.003(1) 0.011(1) C(32) 0.039(1) 0.039(1) 0.027(1) -0.0009(9) -0.0013(9) 0.0079(9) C(33) 0.031(1) 0.0275(9) 0.0261(9) -0.0001(8) 0.0027(8) -0.0029(8) C(34) 0.039(1) 0.0192(8) 0.0176(8) 0.0044(7) 0.0071(8) 0.0004(7) C(35) 0.042(1) 0.0250(9) 0.029(1) -0.0023(9) 0.0007(9) -0.0027(8) C(36) 0.074(2) 0.027(1) 0.036(1) -0.008(1) -0.010(1) -0.005(1) C(37) 0.111(3) 0.024(1) 0.032(1) 0.011(1) 0.005(1) -0.009(1) C(38) 0.098(2) 0.033(1) 0.042(1) 0.024(1) 0.034(1) 0.000(1) C(39) 0.055(1) 0.031(1) 0.038(1) 0.010(1) 0.023(1) -0.0006(9) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 7434 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_all 0.0860 _refine_ls_wR_factor_ref 0.0420 _refine_ls_goodness_of_fit_all 1.466 _refine_ls_goodness_of_fit_ref 1.470 _refine_ls_shift/su_max 0.0500 _refine_ls_shift/su_mean 0.0021 _refine_diff_density_min -0.52 _refine_diff_density_max 0.69 #------------------------------------------------------------------------------ _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(1) P(1) 2.2908(6) . . yes Ru(1) O(1) 2.171(2) . . yes Ru(1) N(1) 2.050(2) . . yes Ru(1) N(2) 2.030(2) . . yes Ru(1) N(3) 2.095(2) . . yes Ru(1) N(4) 2.112(2) . . yes P(1) C(27) 1.831(2) . . yes P(1) C(28) 1.829(2) . . yes P(1) C(34) 1.822(2) . . yes P(2) F(1A) 1.564(3) . . yes P(2) F(2A) 1.595(3) . . yes P(2) F(3A) 1.584(2) . . yes P(2) F(4A) 1.570(2) . . yes P(2) F(5A) 1.577(5) . . yes P(2) F(6A) 1.604(5) . . yes P(2) F(1B) 1.66(1) . . yes P(2) F(2B) 1.53(1) . . yes P(2) F(3B) 1.48(1) . . yes P(2) F(4B) 1.56(1) . . yes P(2) F(5B) 1.67(2) . . yes P(2) F(6B) 1.50(2) . . yes P(3) F(7) 1.591(2) . . yes P(3) F(8) 1.593(2) . . yes P(3) F(9) 1.592(2) . . yes P(3) F(10) 1.595(2) . . yes P(3) F(11) 1.594(2) . . yes P(3) F(12) 1.589(2) . . yes F(1A) F(1B) 1.29(3) . . yes F(1A) F(2B) 1.28(3) . . yes F(1A) F(6B) 1.68(1) . . yes F(2A) F(2B) 1.25(2) . . yes F(2A) F(3B) 1.00(3) . . yes F(3A) F(3B) 1.39(3) . . yes F(3A) F(4B) 1.16(2) . . yes F(4A) F(1B) 1.36(4) . . yes F(4A) F(4B) 1.41(3) . . yes F(5A) F(5B) 0.44(2) . . yes F(6A) F(6B) 0.62(1) . . yes O(1) C(21) 1.441(3) . . yes O(1) C(22) 1.395(3) . . yes N(1) C(1) 1.348(3) . . yes N(1) C(5) 1.356(3) . . yes N(2) C(6) 1.365(3) . . yes N(2) C(10) 1.350(3) . . yes N(3) C(11) 1.344(3) . . yes N(3) C(15) 1.360(3) . . yes N(4) C(16) 1.356(3) . . yes N(4) C(20) 1.347(3) . . yes C(1) C(2) 1.380(3) . . yes C(1) H(1) 0.98 . . no C(2) C(3) 1.385(4) . . yes C(2) H(2) 0.98 . . no C(3) C(4) 1.376(4) . . yes C(3) H(3) 0.98 . . no C(4) C(5) 1.389(3) . . yes C(4) H(4) 0.98 . . no C(5) C(6) 1.471(3) . . yes C(6) C(7) 1.374(3) . . yes C(7) C(8) 1.378(4) . . yes C(7) H(5) 0.98 . . no C(8) C(9) 1.375(4) . . yes C(8) H(6) 0.98 . . no C(9) C(10) 1.380(4) . . yes C(9) H(7) 0.98 . . no C(10) H(8) 0.98 . . no C(11) C(12) 1.385(3) . . yes C(11) H(9) 0.98 . . no C(12) C(13) 1.372(4) . . yes C(12) H(10) 0.98 . . no C(13) C(14) 1.375(4) . . yes C(13) H(11) 0.98 . . no C(14) C(15) 1.391(3) . . yes C(14) H(12) 0.98 . . no C(15) C(16) 1.470(3) . . yes C(16) C(17) 1.390(3) . . yes C(17) C(18) 1.382(4) . . yes C(17) H(13) 0.98 . . no C(18) C(19) 1.372(4) . . yes C(18) H(14) 0.98 . . no C(19) C(20) 1.381(3) . . yes C(19) H(15) 0.98 . . no C(20) H(16) 0.98 . . no C(21) H(17) 0.98 . . no C(21) H(18) 0.98 . . no C(21) H(19) 0.98 . . no C(22) C(23) 1.385(3) . . yes C(22) C(27) 1.394(3) . . yes C(23) C(24) 1.388(4) . . yes C(23) H(20) 0.98 . . no C(24) C(25) 1.373(4) . . yes C(24) H(21) 0.98 . . no C(25) C(26) 1.383(4) . . yes C(25) H(22) 0.98 . . no C(26) C(27) 1.393(3) . . yes C(26) H(23) 0.98 . . no C(28) C(29) 1.393(3) . . yes C(28) C(33) 1.399(3) . . yes C(29) C(30) 1.387(3) . . yes C(29) H(24) 0.98 . . no C(30) C(31) 1.379(4) . . yes C(30) H(25) 0.98 . . no C(31) C(32) 1.384(4) . . yes C(31) H(26) 0.98 . . no C(32) C(33) 1.386(4) . . yes C(32) H(27) 0.98 . . no C(33) H(28) 0.98 . . no C(34) C(35) 1.392(4) . . yes C(34) C(39) 1.396(3) . . yes C(35) C(36) 1.391(4) . . yes C(35) H(29) 0.98 . . no C(36) C(37) 1.375(5) . . yes C(36) H(30) 0.98 . . no C(37) C(38) 1.373(5) . . yes C(37) H(31) 0.98 . . no C(38) C(39) 1.390(4) . . yes C(38) H(32) 0.98 . . no C(39) H(33) 0.98 . . no #------------------------------------------------------------------------------ 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 P(1) Ru(1) O(1) 80.14(4) . . . yes P(1) Ru(1) N(1) 89.85(5) . . . yes P(1) Ru(1) N(2) 101.89(6) . . . yes P(1) Ru(1) N(3) 98.76(5) . . . yes P(1) Ru(1) N(4) 174.40(5) . . . yes O(1) Ru(1) N(1) 96.68(7) . . . yes O(1) Ru(1) N(2) 175.20(7) . . . yes O(1) Ru(1) N(3) 85.70(6) . . . yes O(1) Ru(1) N(4) 95.23(7) . . . yes N(1) Ru(1) N(2) 79.04(7) . . . yes N(1) Ru(1) N(3) 171.35(7) . . . yes N(1) Ru(1) N(4) 93.84(7) . . . yes N(2) Ru(1) N(3) 98.21(7) . . . yes N(2) Ru(1) N(4) 82.97(8) . . . yes N(3) Ru(1) N(4) 77.63(7) . . . yes Ru(1) P(1) C(27) 100.68(7) . . . yes Ru(1) P(1) C(28) 123.26(7) . . . yes Ru(1) P(1) C(34) 117.75(7) . . . yes C(27) P(1) C(28) 105.1(1) . . . yes C(27) P(1) C(34) 105.7(1) . . . yes C(28) P(1) C(34) 102.5(1) . . . yes F(1A) P(2) F(2A) 89.0(2) . . . yes F(1A) P(2) F(3A) 176.9(2) . . . yes F(1A) P(2) F(4A) 92.1(2) . . . yes F(1A) P(2) F(5A) 92.4(3) . . . yes F(1A) P(2) F(6A) 89.3(2) . . . yes F(1A) P(2) F(1B) 47(1) . . . yes F(1A) P(2) F(2B) 49(1) . . . yes F(1A) P(2) F(3B) 123(1) . . . yes F(1A) P(2) F(4B) 138.4(9) . . . yes F(1A) P(2) F(5B) 106.6(7) . . . yes F(1A) P(2) F(6B) 66.7(5) . . . yes F(2A) P(2) F(3A) 88.3(2) . . . yes F(2A) P(2) F(4A) 178.5(2) . . . yes F(2A) P(2) F(5A) 88.9(3) . . . yes F(2A) P(2) F(6A) 90.5(3) . . . yes F(2A) P(2) F(1B) 131(1) . . . yes F(2A) P(2) F(2B) 46.9(9) . . . yes F(2A) P(2) F(3B) 38(1) . . . yes F(2A) P(2) F(4B) 126(1) . . . yes F(2A) P(2) F(5B) 94.4(6) . . . yes F(2A) P(2) F(6B) 92.7(8) . . . yes F(3A) P(2) F(4A) 90.6(2) . . . yes F(3A) P(2) F(5A) 89.0(3) . . . yes F(3A) P(2) F(6A) 89.3(2) . . . yes F(3A) P(2) F(1B) 136(1) . . . yes F(3A) P(2) F(2B) 129(1) . . . yes F(3A) P(2) F(3B) 54(1) . . . yes F(3A) P(2) F(4B) 43.3(9) . . . yes F(3A) P(2) F(5B) 75.0(7) . . . yes F(3A) P(2) F(6B) 112.0(5) . . . yes F(4A) P(2) F(5A) 90.1(3) . . . yes F(4A) P(2) F(6A) 90.6(3) . . . yes F(4A) P(2) F(1B) 50(1) . . . yes F(4A) P(2) F(2B) 134(1) . . . yes F(4A) P(2) F(3B) 142(1) . . . yes F(4A) P(2) F(4B) 54(1) . . . yes F(4A) P(2) F(5B) 84.3(6) . . . yes F(4A) P(2) F(6B) 88.6(8) . . . yes F(5A) P(2) F(6A) 178.2(3) . . . yes F(5A) P(2) F(1B) 74.3(7) . . . yes F(5A) P(2) F(2B) 70.9(7) . . . yes F(5A) P(2) F(3B) 101.5(7) . . . yes F(5A) P(2) F(4B) 108.4(6) . . . yes F(5A) P(2) F(5B) 15.2(9) . . . yes F(5A) P(2) F(6B) 159.0(5) . . . yes F(6A) P(2) F(1B) 107.4(7) . . . yes F(6A) P(2) F(2B) 109.8(6) . . . yes F(6A) P(2) F(3B) 76.9(6) . . . yes F(6A) P(2) F(4B) 70.7(6) . . . yes F(6A) P(2) F(5B) 163.4(7) . . . yes F(6A) P(2) F(6B) 22.8(5) . . . yes F(1B) P(2) F(2B) 84(2) . . . yes F(1B) P(2) F(3B) 168(2) . . . yes F(1B) P(2) F(4B) 103(2) . . . yes F(1B) P(2) F(5B) 81.3(8) . . . yes F(1B) P(2) F(6B) 88.9(8) . . . yes F(2B) P(2) F(3B) 84(1) . . . yes F(2B) P(2) F(4B) 172(2) . . . yes F(2B) P(2) F(5B) 84.9(9) . . . yes F(2B) P(2) F(6B) 95(1) . . . yes F(3B) P(2) F(4B) 88(2) . . . yes F(3B) P(2) F(5B) 97(1) . . . yes F(3B) P(2) F(6B) 92(1) . . . yes F(4B) P(2) F(5B) 93.8(9) . . . yes F(4B) P(2) F(6B) 87.5(8) . . . yes F(5B) P(2) F(6B) 170.1(9) . . . yes F(7) P(3) F(8) 179.0(1) . . . yes F(7) P(3) F(9) 90.5(1) . . . yes F(7) P(3) F(10) 89.4(1) . . . yes F(7) P(3) F(11) 90.2(1) . . . yes F(7) P(3) F(12) 89.6(1) . . . yes F(8) P(3) F(9) 89.5(1) . . . yes F(8) P(3) F(10) 89.6(1) . . . yes F(8) P(3) F(11) 89.9(1) . . . yes F(8) P(3) F(12) 91.4(1) . . . yes F(9) P(3) F(10) 90.4(1) . . . yes F(9) P(3) F(11) 179.0(1) . . . yes F(9) P(3) F(12) 89.7(1) . . . yes F(10) P(3) F(11) 90.3(1) . . . yes F(10) P(3) F(12) 179.0(1) . . . yes F(11) P(3) F(12) 89.6(1) . . . yes P(2) F(1A) F(1B) 70(1) . . . yes P(2) F(1A) F(2B) 64.2(6) . . . yes P(2) F(1A) F(6B) 54.8(6) . . . yes F(1B) F(1A) F(2B) 112(1) . . . yes F(1B) F(1A) F(6B) 95(2) . . . yes F(2B) F(1A) F(6B) 97(1) . . . yes P(2) F(2A) F(2B) 63.8(7) . . . yes P(2) F(2A) F(3B) 64.8(9) . . . yes F(2B) F(2A) F(3B) 128(1) . . . yes P(2) F(3A) F(3B) 59.2(7) . . . yes P(2) F(3A) F(4B) 67(1) . . . yes F(3B) F(3A) F(4B) 111.9(9) . . . yes P(2) F(4A) F(1B) 68.3(7) . . . yes P(2) F(4A) F(4B) 62.8(5) . . . yes F(1B) F(4A) F(4B) 131.0(9) . . . yes P(2) F(5A) F(5B) 94(3) . . . yes P(2) F(6A) F(6B) 69(2) . . . yes Ru(1) O(1) C(21) 121.9(1) . . . yes Ru(1) O(1) C(22) 118.8(1) . . . yes C(21) O(1) C(22) 117.6(2) . . . yes Ru(1) N(1) C(1) 125.4(2) . . . yes Ru(1) N(1) C(5) 116.0(1) . . . yes C(1) N(1) C(5) 118.5(2) . . . yes Ru(1) N(2) C(6) 115.7(1) . . . yes Ru(1) N(2) C(10) 125.3(2) . . . yes C(6) N(2) C(10) 118.1(2) . . . yes Ru(1) N(3) C(11) 127.0(1) . . . yes Ru(1) N(3) C(15) 115.3(1) . . . yes C(11) N(3) C(15) 117.7(2) . . . yes Ru(1) N(4) C(16) 114.4(2) . . . yes Ru(1) N(4) C(20) 126.1(2) . . . yes C(16) N(4) C(20) 118.9(2) . . . yes N(1) C(1) C(2) 122.0(2) . . . yes N(1) C(1) H(1) 119.0 . . . no C(2) C(1) H(1) 119.0 . . . no C(1) C(2) C(3) 119.3(2) . . . yes C(1) C(2) H(2) 120.4 . . . no C(3) C(2) H(2) 120.3 . . . no C(2) C(3) C(4) 119.2(2) . . . yes C(2) C(3) H(3) 120.4 . . . no C(4) C(3) H(3) 120.4 . . . no C(3) C(4) C(5) 119.1(2) . . . yes C(3) C(4) H(4) 120.5 . . . no C(5) C(4) H(4) 120.5 . . . no N(1) C(5) C(4) 121.8(2) . . . yes N(1) C(5) C(6) 113.9(2) . . . yes C(4) C(5) C(6) 124.2(2) . . . yes N(2) C(6) C(5) 114.7(2) . . . yes N(2) C(6) C(7) 121.6(2) . . . yes C(5) C(6) C(7) 123.7(2) . . . yes C(6) C(7) C(8) 119.8(2) . . . yes C(6) C(7) H(5) 120.1 . . . no C(8) C(7) H(5) 120.1 . . . no C(7) C(8) C(9) 119.0(2) . . . yes C(7) C(8) H(6) 120.5 . . . no C(9) C(8) H(6) 120.5 . . . no C(8) C(9) C(10) 119.4(2) . . . yes C(8) C(9) H(7) 120.2 . . . no C(10) C(9) H(7) 120.3 . . . no N(2) C(10) C(9) 122.0(2) . . . yes N(2) C(10) H(8) 119.0 . . . no C(9) C(10) H(8) 119.0 . . . no N(3) C(11) C(12) 123.1(2) . . . yes N(3) C(11) H(9) 118.5 . . . no C(12) C(11) H(9) 118.5 . . . no C(11) C(12) C(13) 118.8(2) . . . yes C(11) C(12) H(10) 120.6 . . . no C(13) C(12) H(10) 120.6 . . . no C(12) C(13) C(14) 119.2(2) . . . yes C(12) C(13) H(11) 120.4 . . . no C(14) C(13) H(11) 120.5 . . . no C(13) C(14) C(15) 119.7(2) . . . yes C(13) C(14) H(12) 120.2 . . . no C(15) C(14) H(12) 120.2 . . . no N(3) C(15) C(14) 121.4(2) . . . yes N(3) C(15) C(16) 115.1(2) . . . yes C(14) C(15) C(16) 123.3(2) . . . yes N(4) C(16) C(15) 115.8(2) . . . yes N(4) C(16) C(17) 120.6(2) . . . yes C(15) C(16) C(17) 123.6(2) . . . yes C(16) C(17) C(18) 119.6(2) . . . yes C(16) C(17) H(13) 120.2 . . . no C(18) C(17) H(13) 120.2 . . . no C(17) C(18) C(19) 119.7(2) . . . yes C(17) C(18) H(14) 120.2 . . . no C(19) C(18) H(14) 120.2 . . . no C(18) C(19) C(20) 118.6(2) . . . yes C(18) C(19) H(15) 120.7 . . . no C(20) C(19) H(15) 120.7 . . . no N(4) C(20) C(19) 122.6(2) . . . yes N(4) C(20) H(16) 118.7 . . . no C(19) C(20) H(16) 118.7 . . . no O(1) C(21) H(17) 109.5 . . . no O(1) C(21) H(18) 109.5 . . . no O(1) C(21) H(19) 109.5 . . . no H(17) C(21) H(18) 109.5 . . . no H(17) C(21) H(19) 109.5 . . . no H(18) C(21) H(19) 109.4 . . . no O(1) C(22) C(23) 122.0(2) . . . yes O(1) C(22) C(27) 116.1(2) . . . yes C(23) C(22) C(27) 121.9(2) . . . yes C(22) C(23) C(24) 118.6(3) . . . yes C(22) C(23) H(20) 120.7 . . . no C(24) C(23) H(20) 120.8 . . . no C(23) C(24) C(25) 121.0(3) . . . yes C(23) C(24) H(21) 119.5 . . . no C(25) C(24) H(21) 119.5 . . . no C(24) C(25) C(26) 119.6(3) . . . yes C(24) C(25) H(22) 120.2 . . . no C(26) C(25) H(22) 120.2 . . . no C(25) C(26) C(27) 121.4(3) . . . yes C(25) C(26) H(23) 119.3 . . . no C(27) C(26) H(23) 119.4 . . . no P(1) C(27) C(22) 117.3(2) . . . yes P(1) C(27) C(26) 125.0(2) . . . yes C(22) C(27) C(26) 117.6(2) . . . yes P(1) C(28) C(29) 119.7(2) . . . yes P(1) C(28) C(33) 121.5(2) . . . yes C(29) C(28) C(33) 118.7(2) . . . yes C(28) C(29) C(30) 120.6(2) . . . yes C(28) C(29) H(24) 119.7 . . . no C(30) C(29) H(24) 119.7 . . . no C(29) C(30) C(31) 120.1(2) . . . yes C(29) C(30) H(25) 120.0 . . . no C(31) C(30) H(25) 120.0 . . . no C(30) C(31) C(32) 120.1(2) . . . yes C(30) C(31) H(26) 120.0 . . . no C(32) C(31) H(26) 120.0 . . . no C(31) C(32) C(33) 120.2(2) . . . yes C(31) C(32) H(27) 119.9 . . . no C(33) C(32) H(27) 119.9 . . . no C(28) C(33) C(32) 120.3(2) . . . yes C(28) C(33) H(28) 119.9 . . . no C(32) C(33) H(28) 119.9 . . . no P(1) C(34) C(35) 117.7(2) . . . yes P(1) C(34) C(39) 123.0(2) . . . yes C(35) C(34) C(39) 119.2(2) . . . yes C(34) C(35) C(36) 120.3(3) . . . yes C(34) C(35) H(29) 119.8 . . . no C(36) C(35) H(29) 119.9 . . . no C(35) C(36) C(37) 119.8(3) . . . yes C(35) C(36) H(30) 120.0 . . . no C(37) C(36) H(30) 120.2 . . . no C(36) C(37) C(38) 120.6(3) . . . yes C(36) C(37) H(31) 119.7 . . . no C(38) C(37) H(31) 119.7 . . . no C(37) C(38) C(39) 120.3(3) . . . yes C(37) C(38) H(32) 119.8 . . . no C(39) C(38) H(32) 119.9 . . . no C(34) C(39) C(38) 119.8(3) . . . yes C(34) C(39) H(33) 120.1 . . . no C(38) C(39) H(33) 120.1 . . . no P(2) F(1B) F(1A) 62.7(5) . . . yes P(2) F(1B) F(4A) 61.8(9) . . . yes F(1A) F(1B) F(4A) 116(1) . . . yes P(2) F(2B) F(1A) 67.0(8) . . . yes P(2) F(2B) F(2A) 69.3(7) . . . yes F(1A) F(2B) F(2A) 123(1) . . . yes P(2) F(3B) F(2A) 78(1) . . . yes P(2) F(3B) F(3A) 67.0(9) . . . yes F(2A) F(3B) F(3A) 136(1) . . . yes P(2) F(4B) F(3A) 69.5(6) . . . yes P(2) F(4B) F(4A) 64(1) . . . yes F(3A) F(4B) F(4A) 121(2) . . . yes P(2) F(5B) F(5A) 70(3) . . . yes P(2) F(6B) F(1A) 58.5(6) . . . yes P(2) F(6B) F(6A) 88(2) . . . yes F(1A) F(6B) F(6A) 146(3) . . . yes #------------------------------------------------------------------------------ #===END data_mw009/RuPC2OMe _database_code_CSD 153810 #------------------------------------------------------------------------------ _audit_creation_date '2000-10-06' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _computing_data_collection 'd*TREK (MSC, 1996-1998)' _computing_cell_refinement 'd*TREK (MSC, 1996-1998)' _computing_data_reduction 'd*TREK (MSC, 1996-1998)' _computing_structure_solution ; SIR97 (Altomare, et. al. 1998) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 13.2591(4) _cell_length_b 14.2123(5) _cell_length_c 19.930(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3755.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 947.64 _chemical_formula_analytical ? _chemical_formula_sum 'C35 H33 F12 N4 O P3 Ru ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1904.00 _exptl_absorpt_coefficient_mu 0.641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.797 _exptl_special_details ; Data were collected in 0.50\% oscillations with 12.0 s exposures. A sweep of data was done using \f oscillations from 0.0 to 190.0\% at \c = -90\% and a second sweep was performed using \w oscillations between -19.0 and 23.0\% at \c = -90.0\%. The crystal-to-detector distance was 40.48 mm. The detector swing angle was -5.51\%. The absorption correction is based on a three-dimensional analysis of symmetry-equivalent data and is performed along with batch scaling in a single step. The resulting transmission factors, therefore, include contributions from absorption, crystal decay, and detectable variations in beam intensity. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_detector_area_resol_mean 11.76 _diffrn_measurement_method 'area detector' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 32001 _reflns_number_total 8135 _reflns_number_gt 5742 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.05934 _diffrn_reflns_av_sigmaI/netI 0.100 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 140 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 132 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; F 0 48 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 16 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 4 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 12 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 4 -1.420 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.12837(3) -0.00010(3) 0.03274(2) 0.02460(8) 1.000 . Uani d ? P(1) 0.2729(1) -0.02268(8) 0.09315(7) 0.0270(4) 1.000 . Uani d ? P(2) 0.0331(2) 0.4028(1) 0.1122(1) 0.0577(6) 1.000 . Uani d ? P(3) 0.1954(1) 0.6071(1) -0.1130(1) 0.0568(6) 1.000 . Uani d ? F(1) -0.0555(4) 0.4612(5) 0.1388(4) 0.162(3) 1.000 . Uani d ? F(2) -0.0346(5) 0.3398(3) 0.0716(3) 0.120(2) 1.000 . Uani d ? F(3) 0.1192(5) 0.3318(3) 0.0927(3) 0.114(2) 1.000 . Uani d ? F(4) 0.1131(4) 0.4727(3) 0.1439(3) 0.103(2) 1.000 . Uani d ? F(5) 0.0340(7) 0.3476(3) 0.1747(3) 0.160(3) 1.000 . Uani d ? F(6) 0.0496(5) 0.4624(4) 0.0522(4) 0.168(3) 1.000 . Uani d ? F(7) 0.1154(4) 0.6870(4) -0.1157(3) 0.099(2) 1.000 . Uani d ? F(8) 0.1577(5) 0.5583(6) -0.1750(3) 0.161(3) 1.000 . Uani d ? F(9) 0.2803(3) 0.5314(3) -0.1024(2) 0.081(2) 1.000 . Uani d ? F(10) 0.2402(4) 0.6579(3) -0.0457(3) 0.093(2) 1.000 . Uani d ? F(11) 0.1224(4) 0.5509(3) -0.0673(3) 0.091(2) 1.000 . Uani d ? F(12) 0.2683(4) 0.6650(4) -0.1586(3) 0.111(2) 1.000 . Uani d ? O(1) 0.2251(3) -0.0493(2) -0.0480(2) 0.034(1) 1.000 . Uani d ? N(1) 0.1598(4) 0.1326(3) -0.0083(2) 0.033(1) 1.000 . Uani d ? N(2) 0.0009(3) 0.0236(3) -0.0290(2) 0.036(1) 1.000 . Uani d ? N(3) 0.0794(3) -0.1291(3) 0.0662(2) 0.027(1) 1.000 . Uani d ? N(4) 0.0401(3) 0.0387(3) 0.1111(2) 0.031(1) 1.000 . Uani d ? C(1) 0.2441(5) 0.1832(4) -0.0007(3) 0.043(2) 1.000 . Uani d ? C(2) 0.2586(6) 0.2708(4) -0.0310(3) 0.055(2) 1.000 . Uani d ? C(3) 0.1855(7) 0.3071(4) -0.0703(3) 0.058(2) 1.000 . Uani d ? C(4) 0.0992(6) 0.2556(4) -0.0801(4) 0.055(2) 1.000 . Uani d ? C(5) 0.0875(5) 0.1682(4) -0.0496(3) 0.039(2) 1.000 . Uani d ? C(6) -0.0009(5) 0.1079(4) -0.0596(3) 0.043(2) 1.000 . Uani d ? C(7) -0.0816(7) 0.1326(5) -0.1008(5) 0.073(3) 1.000 . Uani d ? C(8) -0.1652(6) 0.0711(7) -0.1064(5) 0.081(3) 1.000 . Uani d ? C(9) -0.1633(5) -0.0108(6) -0.0698(3) 0.055(2) 1.000 . Uani d ? C(10) -0.0808(5) -0.0320(4) -0.0328(3) 0.044(2) 1.000 . Uani d ? C(11) 0.0975(4) -0.2129(3) 0.0384(3) 0.033(1) 1.000 . Uani d ? C(12) 0.0680(4) -0.2963(4) 0.0662(3) 0.037(2) 1.000 . Uani d ? C(13) 0.0192(5) -0.2954(4) 0.1267(3) 0.043(2) 1.000 . Uani d ? C(14) -0.0033(5) -0.2104(4) 0.1570(3) 0.038(2) 1.000 . Uani d ? C(15) 0.0274(5) -0.1263(4) 0.1250(3) 0.030(2) 1.000 . Uani d ? C(16) 0.0028(4) -0.0328(4) 0.1496(3) 0.031(1) 1.000 . Uani d ? C(17) -0.0569(4) -0.0152(4) 0.2039(3) 0.042(2) 1.000 . Uani d ? C(18) -0.0816(5) 0.0761(4) 0.2213(3) 0.048(2) 1.000 . Uani d ? C(19) -0.0464(5) 0.1481(4) 0.1810(3) 0.047(2) 1.000 . Uani d ? C(20) 0.0143(5) 0.1284(4) 0.1257(4) 0.040(2) 1.000 . Uani d ? C(21) 0.3321(5) 0.0668(4) 0.1466(3) 0.034(2) 1.000 . Uani d ? C(22) 0.2756(6) 0.1428(4) 0.1703(3) 0.049(2) 1.000 . Uani d ? C(23) 0.3158(6) 0.2029(5) 0.2176(3) 0.057(2) 1.000 . Uani d ? C(24) 0.4133(8) 0.1872(6) 0.2408(3) 0.070(3) 1.000 . Uani d ? C(25) 0.4666(6) 0.1142(6) 0.2171(4) 0.063(2) 1.000 . Uani d ? C(26) 0.4288(5) 0.0503(5) 0.1701(3) 0.046(2) 1.000 . Uani d ? C(27) 0.2766(4) -0.1212(4) 0.1525(3) 0.030(2) 1.000 . Uani d ? C(28) 0.3149(5) -0.2082(4) 0.1360(3) 0.046(2) 1.000 . Uani d ? C(29) 0.3191(6) -0.2794(4) 0.1831(4) 0.056(2) 1.000 . Uani d ? C(30) 0.2814(6) -0.2648(5) 0.2481(4) 0.053(2) 1.000 . Uani d ? C(31) 0.2412(5) -0.1789(5) 0.2632(3) 0.049(2) 1.000 . Uani d ? C(32) 0.2396(4) -0.1072(4) 0.2165(3) 0.035(2) 1.000 . Uani d ? C(33) 0.3665(4) -0.0485(4) 0.0283(3) 0.040(2) 1.000 . Uani d ? C(34) 0.3172(4) -0.0967(4) -0.0313(3) 0.039(2) 1.000 . Uani d ? C(35) 0.1947(5) -0.0707(4) -0.1138(3) 0.048(2) 1.000 . Uani d ? H(1) 0.2982 0.1576 0.0275 0.052 1.000 . Uiso c ? H(2) 0.3215 0.3057 -0.0239 0.066 1.000 . Uiso c ? H(3) 0.1938 0.3689 -0.0914 0.069 1.000 . Uiso c ? H(4) 0.0453 0.2806 -0.1087 0.066 1.000 . Uiso c ? H(5) -0.0805 0.1921 -0.1255 0.088 1.000 . Uiso c ? H(6) -0.2224 0.0862 -0.1357 0.097 1.000 . Uiso c ? H(7) -0.2214 -0.0535 -0.0704 0.066 1.000 . Uiso c ? H(8) -0.0807 -0.0910 -0.0074 0.053 1.000 . Uiso c ? H(9) 0.1338 -0.2147 -0.0044 0.039 1.000 . Uiso c ? H(10) 0.0817 -0.3559 0.0432 0.044 1.000 . Uiso c ? H(11) 0.0003 -0.3547 0.1485 0.051 1.000 . Uiso c ? H(12) -0.0397 -0.2084 0.1997 0.045 1.000 . Uiso c ? H(13) -0.0824 -0.0677 0.2309 0.050 1.000 . Uiso c ? H(14) -0.1228 0.0894 0.2610 0.057 1.000 . Uiso c ? H(15) -0.0643 0.2134 0.1914 0.056 1.000 . Uiso c ? H(16) 0.0384 0.1799 0.0973 0.048 1.000 . Uiso c ? H(17) 0.2072 0.1533 0.1534 0.059 1.000 . Uiso c ? H(18) 0.2762 0.2560 0.2345 0.068 1.000 . Uiso c ? H(19) 0.4429 0.2293 0.2745 0.083 1.000 . Uiso c ? H(20) 0.5356 0.1053 0.2334 0.076 1.000 . Uiso c ? H(21) 0.4687 -0.0036 0.1546 0.056 1.000 . Uiso c ? H(22) 0.3395 -0.2198 0.0904 0.055 1.000 . Uiso c ? H(23) 0.3483 -0.3404 0.1710 0.068 1.000 . Uiso c ? H(24) 0.2840 -0.3149 0.2818 0.064 1.000 . Uiso c ? H(25) 0.2130 -0.1680 0.3080 0.058 1.000 . Uiso c ? H(26) 0.2118 -0.0456 0.2288 0.042 1.000 . Uiso c ? H(27) 0.3976 0.0104 0.0134 0.047 1.000 . Uiso c ? H(28) 0.4184 -0.0899 0.0470 0.047 1.000 . Uiso c ? H(29) 0.3026 -0.1623 -0.0199 0.047 1.000 . Uiso c ? H(30) 0.3631 -0.0946 -0.0698 0.047 1.000 . Uiso c ? H(31) 0.1324 -0.0366 -0.1242 0.058 1.000 . Uiso c ? H(32) 0.2477 -0.0519 -0.1453 0.058 1.000 . Uiso c ? H(33) 0.1828 -0.1385 -0.1177 0.058 1.000 . Uiso c ? 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(1) 0.0336(2) 0.0173(1) 0.0229(2) 0.0026(2) 0.0012(2) -0.0003(2) P(1) 0.0312(7) 0.0253(7) 0.0246(6) -0.0045(5) 0.0020(6) -0.0012(5) P(2) 0.066(1) 0.0390(9) 0.068(1) 0.0059(9) -0.007(1) 0.0070(9) P(3) 0.053(1) 0.0404(9) 0.077(1) -0.0017(8) 0.021(1) 0.0070(9) F(1) 0.048(3) 0.226(8) 0.211(7) 0.055(4) 0.009(4) -0.082(6) F(2) 0.153(6) 0.065(3) 0.142(5) 0.016(3) -0.105(5) -0.030(3) F(3) 0.108(5) 0.076(3) 0.157(6) 0.024(3) -0.003(4) -0.027(4) F(4) 0.120(4) 0.059(3) 0.129(4) -0.034(3) 0.058(4) -0.030(3) F(5) 0.35(1) 0.044(3) 0.089(4) -0.027(4) -0.111(6) 0.015(3) F(6) 0.150(6) 0.100(4) 0.254(9) -0.027(4) -0.026(6) 0.124(5) F(7) 0.103(4) 0.095(3) 0.101(4) 0.039(3) -0.005(4) 0.022(3) F(8) 0.126(5) 0.279(9) 0.079(4) -0.090(5) 0.022(4) -0.066(5) F(9) 0.078(3) 0.067(3) 0.098(3) 0.015(2) 0.029(3) 0.016(2) F(10) 0.095(4) 0.074(3) 0.109(4) 0.012(3) -0.023(3) -0.020(3) F(11) 0.078(3) 0.079(3) 0.115(4) -0.026(3) 0.049(3) 0.007(3) F(12) 0.068(3) 0.113(4) 0.151(5) 0.002(3) 0.024(3) 0.091(4) O(1) 0.048(2) 0.037(2) 0.018(2) 0.014(2) -0.001(2) -0.006(1) N(1) 0.053(3) 0.020(2) 0.025(2) 0.006(2) 0.010(2) 0.001(2) N(2) 0.045(3) 0.038(3) 0.025(2) 0.017(2) -0.003(2) 0.002(2) N(3) 0.027(2) 0.023(2) 0.030(2) 0.000(2) -0.008(2) -0.003(2) N(4) 0.035(3) 0.018(2) 0.039(3) 0.002(2) -0.004(2) -0.002(2) C(1) 0.064(5) 0.028(3) 0.037(3) -0.009(3) 0.014(3) 0.006(2) C(2) 0.088(5) 0.028(3) 0.047(4) -0.018(3) 0.025(4) -0.001(3) C(3) 0.109(7) 0.014(3) 0.050(4) 0.006(3) 0.022(4) 0.007(3) C(4) 0.077(5) 0.029(3) 0.060(5) 0.019(3) 0.012(4) 0.021(3) C(5) 0.066(4) 0.025(3) 0.027(3) 0.017(3) 0.011(3) 0.007(2) C(6) 0.058(4) 0.038(3) 0.033(3) 0.018(3) 0.008(3) 0.012(2) C(7) 0.066(5) 0.063(5) 0.090(6) 0.030(4) -0.007(5) 0.035(5) C(8) 0.054(5) 0.102(7) 0.085(6) 0.025(5) -0.023(5) 0.035(5) C(9) 0.047(3) 0.064(5) 0.054(4) 0.001(4) -0.010(3) -0.003(4) C(10) 0.046(4) 0.045(3) 0.042(3) 0.007(3) -0.006(3) 0.001(3) C(11) 0.035(3) 0.022(2) 0.042(3) 0.001(2) -0.010(3) 0.001(2) C(12) 0.040(4) 0.022(3) 0.048(4) -0.001(2) -0.022(3) 0.007(2) C(13) 0.050(4) 0.026(3) 0.052(4) -0.013(3) -0.020(3) 0.012(3) C(14) 0.044(4) 0.036(3) 0.033(3) -0.012(3) -0.011(3) 0.011(2) C(15) 0.033(3) 0.025(3) 0.032(4) -0.003(2) -0.011(3) 0.004(2) C(16) 0.030(3) 0.034(3) 0.029(3) -0.005(2) 0.001(2) -0.004(2) C(17) 0.041(3) 0.046(4) 0.038(3) -0.011(3) 0.007(2) -0.003(3) C(18) 0.042(4) 0.051(4) 0.050(4) -0.004(3) 0.016(3) -0.013(3) C(19) 0.044(4) 0.048(4) 0.049(4) -0.002(3) 0.013(3) -0.018(3) C(20) 0.037(4) 0.030(3) 0.052(4) 0.014(3) 0.010(3) -0.003(3) C(21) 0.045(3) 0.028(3) 0.030(3) -0.016(2) 0.007(3) 0.001(2) C(22) 0.071(5) 0.041(3) 0.035(4) -0.034(3) 0.015(4) -0.011(3) C(23) 0.090(6) 0.042(4) 0.037(4) -0.029(4) 0.026(4) -0.015(3) C(24) 0.105(7) 0.070(5) 0.033(4) -0.064(5) 0.011(4) -0.011(3) C(25) 0.052(5) 0.094(6) 0.043(4) -0.044(4) 0.005(3) -0.008(4) C(26) 0.042(4) 0.054(4) 0.043(4) -0.023(3) 0.009(3) -0.010(3) C(27) 0.028(3) 0.033(3) 0.030(3) 0.001(2) -0.013(3) -0.001(2) C(28) 0.062(4) 0.044(3) 0.032(3) 0.010(3) -0.015(3) 0.002(3) C(29) 0.073(5) 0.034(3) 0.061(5) 0.011(3) -0.029(4) 0.006(3) C(30) 0.059(5) 0.046(4) 0.055(4) -0.009(3) -0.020(4) 0.015(3) C(31) 0.042(4) 0.053(4) 0.051(4) -0.012(3) -0.003(3) 0.020(3) C(32) 0.030(3) 0.042(3) 0.034(3) -0.002(2) 0.001(3) 0.009(3) C(33) 0.034(3) 0.051(3) 0.034(3) 0.000(3) -0.001(3) -0.008(3) C(34) 0.038(3) 0.049(3) 0.029(3) 0.014(3) 0.004(3) -0.006(3) C(35) 0.066(5) 0.052(4) 0.028(3) 0.006(3) -0.004(3) -0.008(3) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 8135 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.048 _refine_ls_wR_factor_all 0.1191 _refine_ls_wR_factor_ref 0.057 _refine_ls_goodness_of_fit_all 1.336 _refine_ls_goodness_of_fit_ref 1.336 _refine_ls_shift/su_max 0.0360 _refine_ls_shift/su_mean 0.0090 _refine_diff_density_min -1.23 _refine_diff_density_max 1.27 #------------------------------------------------------------------------------ _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(1) P(1) 2.286(2) . . yes Ru(1) O(1) 2.174(3) . . yes Ru(1) N(1) 2.098(4) . . yes Ru(1) N(2) 2.118(4) . . yes Ru(1) N(3) 2.055(4) . . yes Ru(1) N(4) 2.029(5) . . yes P(1) C(21) 1.835(5) . . yes P(1) C(27) 1.833(6) . . yes P(1) C(33) 1.829(6) . . yes P(2) F(1) 1.534(5) . . yes P(2) F(2) 1.504(5) . . yes P(2) F(3) 1.571(5) . . yes P(2) F(4) 1.584(5) . . yes P(2) F(5) 1.472(5) . . yes P(2) F(6) 1.482(7) . . yes P(3) F(7) 1.556(5) . . yes P(3) F(8) 1.502(6) . . yes P(3) F(9) 1.571(4) . . yes P(3) F(10) 1.635(5) . . yes P(3) F(11) 1.551(4) . . yes P(3) F(12) 1.561(5) . . yes O(1) C(34) 1.434(6) . . yes O(1) C(35) 1.405(7) . . yes N(1) C(1) 1.338(8) . . yes N(1) C(5) 1.361(7) . . yes N(2) C(6) 1.344(7) . . yes N(2) C(10) 1.343(7) . . yes N(3) C(11) 1.336(6) . . yes N(3) C(15) 1.361(8) . . yes N(4) C(16) 1.365(6) . . yes N(4) C(20) 1.352(7) . . yes C(1) C(2) 1.398(7) . . yes C(1) H(1) 0.98 . . no C(2) C(3) 1.35(1) . . yes C(2) H(2) 0.98 . . no C(3) C(4) 1.37(1) . . yes C(3) H(3) 0.98 . . no C(4) C(5) 1.391(7) . . yes C(4) H(4) 0.98 . . no C(5) C(6) 1.466(9) . . yes C(6) C(7) 1.39(1) . . yes C(7) C(8) 1.42(1) . . yes C(7) H(5) 0.98 . . no C(8) C(9) 1.37(1) . . yes C(8) H(6) 0.98 . . no C(9) C(10) 1.354(9) . . yes C(9) H(7) 0.98 . . no C(10) H(8) 0.98 . . no C(11) C(12) 1.366(7) . . yes C(11) H(9) 0.98 . . no C(12) C(13) 1.369(9) . . yes C(12) H(10) 0.98 . . no C(13) C(14) 1.383(8) . . yes C(13) H(11) 0.98 . . no C(14) C(15) 1.414(7) . . yes C(14) H(12) 0.98 . . no C(15) C(16) 1.454(7) . . yes C(16) C(17) 1.364(7) . . yes C(17) C(18) 1.383(8) . . yes C(17) H(13) 0.98 . . no C(18) C(19) 1.382(9) . . yes C(18) H(14) 0.98 . . no C(19) C(20) 1.393(9) . . yes C(19) H(15) 0.98 . . no C(20) H(16) 0.98 . . no C(21) C(22) 1.397(9) . . yes C(21) C(26) 1.385(9) . . yes C(22) C(23) 1.379(9) . . yes C(22) H(17) 0.98 . . no C(23) C(24) 1.39(1) . . yes C(23) H(18) 0.98 . . no C(24) C(25) 1.34(1) . . yes C(24) H(19) 0.98 . . no C(25) C(26) 1.397(9) . . yes C(25) H(20) 0.98 . . no C(26) H(21) 0.98 . . no C(27) C(28) 1.378(8) . . yes C(27) C(32) 1.381(8) . . yes C(28) C(29) 1.381(8) . . yes C(28) H(22) 0.98 . . no C(29) C(30) 1.40(1) . . yes C(29) H(23) 0.98 . . no C(30) C(31) 1.37(1) . . yes C(30) H(24) 0.98 . . no C(31) C(32) 1.382(8) . . yes C(31) H(25) 0.98 . . no C(32) H(26) 0.98 . . no C(33) C(34) 1.518(8) . . yes C(33) H(27) 0.98 . . no C(33) H(28) 0.98 . . no C(34) H(29) 0.98 . . no C(34) H(30) 0.98 . . no C(35) H(31) 0.98 . . no C(35) H(32) 0.98 . . no C(35) H(33) 0.98 . . no #------------------------------------------------------------------------------ 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 P(1) Ru(1) O(1) 81.4(1) . . . yes P(1) Ru(1) N(1) 99.5(1) . . . yes P(1) Ru(1) N(2) 176.0(1) . . . yes P(1) Ru(1) N(3) 88.2(1) . . . yes P(1) Ru(1) N(4) 96.7(1) . . . yes O(1) Ru(1) N(1) 83.3(1) . . . yes O(1) Ru(1) N(2) 95.3(2) . . . yes O(1) Ru(1) N(3) 98.0(2) . . . yes O(1) Ru(1) N(4) 176.6(2) . . . yes N(1) Ru(1) N(2) 77.8(2) . . . yes N(1) Ru(1) N(3) 172.3(2) . . . yes N(1) Ru(1) N(4) 99.9(2) . . . yes N(2) Ru(1) N(3) 94.5(2) . . . yes N(2) Ru(1) N(4) 86.8(2) . . . yes N(3) Ru(1) N(4) 79.1(2) . . . yes Ru(1) P(1) C(21) 124.6(2) . . . yes Ru(1) P(1) C(27) 118.0(2) . . . yes Ru(1) P(1) C(33) 103.0(2) . . . yes C(21) P(1) C(27) 98.2(2) . . . yes C(21) P(1) C(33) 105.0(3) . . . yes C(27) P(1) C(33) 106.5(3) . . . yes F(1) P(2) F(2) 92.9(4) . . . yes F(1) P(2) F(3) 171.6(4) . . . yes F(1) P(2) F(4) 92.0(3) . . . yes F(1) P(2) F(5) 90.1(5) . . . yes F(1) P(2) F(6) 94.7(5) . . . yes F(2) P(2) F(3) 85.4(3) . . . yes F(2) P(2) F(4) 170.8(4) . . . yes F(2) P(2) F(5) 98.2(3) . . . yes F(2) P(2) F(6) 89.7(4) . . . yes F(3) P(2) F(4) 90.9(3) . . . yes F(3) P(2) F(5) 82.0(4) . . . yes F(3) P(2) F(6) 93.5(4) . . . yes F(4) P(2) F(5) 89.5(3) . . . yes F(4) P(2) F(6) 82.2(4) . . . yes F(5) P(2) F(6) 170.6(5) . . . yes F(7) P(3) F(8) 94.6(4) . . . yes F(7) P(3) F(9) 173.4(3) . . . yes F(7) P(3) F(10) 87.3(3) . . . yes F(7) P(3) F(11) 88.3(3) . . . yes F(7) P(3) F(12) 91.0(3) . . . yes F(8) P(3) F(9) 92.0(4) . . . yes F(8) P(3) F(10) 178.0(4) . . . yes F(8) P(3) F(11) 92.2(3) . . . yes F(8) P(3) F(12) 88.3(4) . . . yes F(9) P(3) F(10) 86.1(3) . . . yes F(9) P(3) F(11) 90.8(3) . . . yes F(9) P(3) F(12) 89.8(3) . . . yes F(10) P(3) F(11) 88.4(3) . . . yes F(10) P(3) F(12) 91.1(3) . . . yes F(11) P(3) F(12) 179.2(3) . . . yes Ru(1) O(1) C(34) 118.8(3) . . . yes Ru(1) O(1) C(35) 126.2(4) . . . yes C(34) O(1) C(35) 111.1(4) . . . yes Ru(1) N(1) C(1) 127.2(4) . . . yes Ru(1) N(1) C(5) 115.5(4) . . . yes C(1) N(1) C(5) 117.2(5) . . . yes Ru(1) N(2) C(6) 114.8(4) . . . yes Ru(1) N(2) C(10) 125.6(4) . . . yes C(6) N(2) C(10) 119.0(5) . . . yes Ru(1) N(3) C(11) 127.2(4) . . . yes Ru(1) N(3) C(15) 114.4(3) . . . yes C(11) N(3) C(15) 118.3(5) . . . yes Ru(1) N(4) C(16) 116.1(3) . . . yes Ru(1) N(4) C(20) 124.6(4) . . . yes C(16) N(4) C(20) 119.3(5) . . . yes N(1) C(1) C(2) 123.0(6) . . . yes N(1) C(1) H(1) 118.5 . . . no C(2) C(1) H(1) 118.5 . . . no C(1) C(2) C(3) 119.5(6) . . . yes C(1) C(2) H(2) 120.3 . . . no C(3) C(2) H(2) 120.2 . . . no C(2) C(3) C(4) 118.6(5) . . . yes C(2) C(3) H(3) 120.7 . . . no C(4) C(3) H(3) 120.7 . . . no C(3) C(4) C(5) 120.4(7) . . . yes C(3) C(4) H(4) 119.8 . . . no C(5) C(4) H(4) 119.8 . . . no N(1) C(5) C(4) 121.2(6) . . . yes N(1) C(5) C(6) 115.3(5) . . . yes C(4) C(5) C(6) 123.5(6) . . . yes N(2) C(6) C(5) 116.5(5) . . . yes N(2) C(6) C(7) 120.4(7) . . . yes C(5) C(6) C(7) 123.1(6) . . . yes C(6) C(7) C(8) 119.5(6) . . . yes C(6) C(7) H(5) 120.3 . . . no C(8) C(7) H(5) 120.2 . . . no C(7) C(8) C(9) 117.8(6) . . . yes C(7) C(8) H(6) 121.2 . . . no C(9) C(8) H(6) 121.0 . . . no C(8) C(9) C(10) 119.5(7) . . . yes C(8) C(9) H(7) 120.2 . . . no C(10) C(9) H(7) 120.3 . . . no N(2) C(10) C(9) 123.5(6) . . . yes N(2) C(10) H(8) 118.3 . . . no C(9) C(10) H(8) 118.2 . . . no N(3) C(11) C(12) 123.7(6) . . . yes N(3) C(11) H(9) 118.1 . . . no C(12) C(11) H(9) 118.2 . . . no C(11) C(12) C(13) 119.0(5) . . . yes C(11) C(12) H(10) 120.5 . . . no C(13) C(12) H(10) 120.5 . . . no C(12) C(13) C(14) 119.6(5) . . . yes C(12) C(13) H(11) 120.2 . . . no C(14) C(13) H(11) 120.2 . . . no C(13) C(14) C(15) 118.7(6) . . . yes C(13) C(14) H(12) 120.7 . . . no C(15) C(14) H(12) 120.6 . . . no N(3) C(15) C(14) 120.7(5) . . . yes N(3) C(15) C(16) 115.5(5) . . . yes C(14) C(15) C(16) 123.8(6) . . . yes N(4) C(16) C(15) 114.2(5) . . . yes N(4) C(16) C(17) 121.3(5) . . . yes C(15) C(16) C(17) 124.4(5) . . . yes C(16) C(17) C(18) 120.5(5) . . . yes C(16) C(17) H(13) 119.8 . . . no C(18) C(17) H(13) 119.7 . . . no C(17) C(18) C(19) 118.0(6) . . . yes C(17) C(18) H(14) 121.0 . . . no C(19) C(18) H(14) 121.0 . . . no C(18) C(19) C(20) 120.4(6) . . . yes C(18) C(19) H(15) 119.8 . . . no C(20) C(19) H(15) 119.8 . . . no N(4) C(20) C(19) 120.4(6) . . . yes N(4) C(20) H(16) 119.8 . . . no C(19) C(20) H(16) 119.8 . . . no P(1) C(21) C(22) 120.2(5) . . . yes P(1) C(21) C(26) 118.4(5) . . . yes C(22) C(21) C(26) 120.9(6) . . . yes C(21) C(22) C(23) 120.2(8) . . . yes C(21) C(22) H(17) 119.9 . . . no C(23) C(22) H(17) 119.9 . . . no C(22) C(23) C(24) 119.2(7) . . . yes C(22) C(23) H(18) 120.4 . . . no C(24) C(23) H(18) 120.4 . . . no C(23) C(24) C(25) 119.7(6) . . . yes C(23) C(24) H(19) 120.2 . . . no C(25) C(24) H(19) 120.1 . . . no C(24) C(25) C(26) 123.4(7) . . . yes C(24) C(25) H(20) 118.4 . . . no C(26) C(25) H(20) 118.3 . . . no C(21) C(26) C(25) 116.7(7) . . . yes C(21) C(26) H(21) 121.6 . . . no C(25) C(26) H(21) 121.7 . . . no P(1) C(27) C(28) 122.8(5) . . . yes P(1) C(27) C(32) 118.4(4) . . . yes C(28) C(27) C(32) 118.7(5) . . . yes C(27) C(28) C(29) 120.7(6) . . . yes C(27) C(28) H(22) 119.6 . . . no C(29) C(28) H(22) 119.7 . . . no C(28) C(29) C(30) 120.3(6) . . . yes C(28) C(29) H(23) 119.8 . . . no C(30) C(29) H(23) 119.9 . . . no C(29) C(30) C(31) 118.4(6) . . . yes C(29) C(30) H(24) 120.8 . . . no C(31) C(30) H(24) 120.8 . . . no C(30) C(31) C(32) 121.1(6) . . . yes C(30) C(31) H(25) 119.4 . . . no C(32) C(31) H(25) 119.4 . . . no C(27) C(32) C(31) 120.7(6) . . . yes C(27) C(32) H(26) 119.6 . . . no C(31) C(32) H(26) 119.6 . . . no P(1) C(33) C(34) 110.6(4) . . . yes P(1) C(33) H(27) 109.2 . . . no P(1) C(33) H(28) 109.1 . . . no C(34) C(33) H(27) 109.3 . . . no C(34) C(33) H(28) 109.2 . . . no H(27) C(33) H(28) 109.5 . . . no O(1) C(34) C(33) 109.7(4) . . . yes O(1) C(34) H(29) 109.5 . . . no O(1) C(34) H(30) 109.4 . . . no C(33) C(34) H(29) 109.5 . . . no C(33) C(34) H(30) 109.4 . . . no H(29) C(34) H(30) 109.5 . . . no O(1) C(35) H(31) 109.5 . . . no O(1) C(35) H(32) 109.5 . . . no O(1) C(35) H(33) 109.5 . . . no H(31) C(35) H(32) 109.5 . . . no H(31) C(35) H(33) 109.5 . . . no H(32) C(35) H(33) 109.5 . . . no #------------------------------------------------------------------------------ #===END data_mw010/RuPOEt _database_code_CSD 153811 #------------------------------------------------------------------------------ _audit_creation_date '2000-09-07' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ _computing_data_collection 'd*TREK (MSC, 1996-1998)' _computing_cell_refinement 'd*TREK (MSC, 1996-1998)' _computing_data_reduction 'd*TREK (MSC, 1996-1998)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 29.844(1) _cell_length_b 10.7577(6) _cell_length_c 26.255(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8429(1) _cell_formula_units_Z 8 _cell_measurement_temperature 173.2 _cell_measurement_reflns_used 15174 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 25.2 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_Int_Tables_number 33 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y,1/2+z' '1/2-x,1/2+y,1/2+z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'needle' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1009.71 _chemical_formula_analytical ? _chemical_formula_sum 'C40 H35 F12 N4 O P3 Ru ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 4064.00 _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.580 _exptl_special_details ; Data were collected in 0.50\% oscillations with 77.0 s exposures. A sweep of data was done using \f oscillations from 0.0 to 190.0\% at \c = -90\% and a second sweep was performed using \w oscillations between -19.0 and 23.0\% at \c = -90.0\%. The crystal-to-detector distance was 40.50 mm. The detector swing angle was -5.5\%. The absorption correction is based on a three-dimensional analysis of symmetry-equivalent data and is performed along with batch scaling in a single step. The resulting transmission factors, therefore, include contributions from absorption, crystal decay, and detectable variations in beam intensity. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_detector_area_resol_mean 11.76 _diffrn_measurement_method 'area detector' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 35277 _reflns_number_total 12548 _reflns_number_gt 8485 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.11475 _diffrn_reflns_av_sigmaI/netI 0.180 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.13 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 320 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 280 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; F 0 96 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 32 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 8 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 24 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 8 -1.420 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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 Ru1 Ru 0.98877(2) 0.65686(6) -0.01070(3) 0.01425(10) Uani 1 d . . . Ru2 Ru 0.73814(2) 0.89146(6) 0.25720(3) 0.01425(10) Uani 1 d . . . P1 P 0.94090(7) 0.82224(17) -0.00357(8) 0.01361(7) Uani 1 d . . . P2 P 0.68829(8) 0.73325(18) 0.24681(8) 0.0144(4) Uani 1 d . . . P3 P 1.08599(10) 1.4119(3) -0.20569(10) 0.0366(7) Uani 1 d . . . P4 P 0.84206(11) 1.2816(2) 0.04765(11) 0.0274(6) Uani 1 d . . . P5 P 0.59164(12) 1.2668(2) 0.20404(12) 0.0351(7) Uani 1 d . . . P6 P 0.83314(13) 1.0578(3) 0.46432(12) 0.0541(10) Uani 1 d . . . F1 F 1.0624(3) 1.5185(8) -0.2360(3) 0.114(4) Uani 1 d . . . F2 F 1.0416(3) 1.3795(9) -0.1776(3) 0.102(3) Uani 1 d . . . F3 F 1.1113(3) 1.3050(6) -0.1757(3) 0.067(2) Uani 1 d . . . F4 F 1.1321(3) 1.4441(5) -0.2330(3) 0.073(3) Uani 1 d . . . F5 F 1.0755(2) 1.3158(6) -0.2502(3) 0.0568(18) Uani 1 d . . . F6 F 1.0984(3) 1.5088(7) -0.1619(3) 0.079(3) Uani 1 d . . . F7 F 0.8413(2) 1.4083(5) 0.0153(3) 0.054(2) Uani 1 d . . . F8 F 0.8948(3) 1.2925(7) 0.0527(3) 0.075(2) Uani 1 d . . . F9 F 0.8413(3) 1.1556(5) 0.0783(3) 0.054(2) Uani 1 d . . . F10 F 0.7886(2) 1.2753(6) 0.0417(2) 0.0477(17) Uani 1 d . . . F11 F 0.8475(3) 1.2092(5) -0.0051(3) 0.060(2) Uani 1 d . . . F12 F 0.8351(2) 1.3563(5) 0.0992(2) 0.0528(18) Uani 1 d . . . F13 F 0.5945(3) 1.3715(7) 0.1623(3) 0.081(3) Uani 1 d . . . F14 F 0.5400(3) 1.2511(8) 0.1974(4) 0.111(4) Uani 1 d . . . F15 F 0.5894(2) 1.1599(5) 0.2457(3) 0.056(2) Uani 1 d . . . F16 F 0.6424(3) 1.2626(11) 0.2043(5) 0.149(6) Uani 1 d . . . F17 F 0.5949(5) 1.1668(9) 0.1613(4) 0.135(5) Uani 1 d . . . F18 F 0.5875(6) 1.3621(6) 0.2440(4) 0.194(7) Uani 1 d . . . F19 F 0.8564(3) 1.1723(6) 0.4356(3) 0.063(2) Uani 1 d . . . F20 F 0.8816(3) 1.0164(5) 0.4838(3) 0.077(2) Uani 1 d . . . F21 F 0.8124(4) 0.9408(8) 0.4942(3) 0.128(4) Uani 1 d . . . F22 F 0.7861(3) 1.0973(10) 0.4440(4) 0.130(4) Uani 1 d . . . F23 F 0.8395(3) 0.9733(8) 0.4149(3) 0.087(3) Uani 1 d . . . F24 F 0.8274(3) 1.1458(7) 0.5133(3) 0.078(2) Uani 1 d . . . O1 O 1.0274(2) 0.7778(5) 0.0406(2) 0.0205(9) Uani 1 d . . . O2 O 0.7765(2) 0.7678(5) 0.2067(2) 0.0205(9) Uani 1 d . . . N1 N 1.0351(2) 0.5068(6) -0.0091(3) 0.0190(10) Uani 1 d . . . N2 N 0.9710(2) 0.5644(6) 0.0560(3) 0.0167(11) Uani 1 d . . . N3 N 0.9552(2) 0.5502(6) -0.0611(3) 0.0166(10) Uani 1 d . . . N4 N 1.0113(3) 0.7289(6) -0.0789(3) 0.0190(10) Uani 1 d . . . N5 N 0.7853(2) 1.0370(6) 0.2609(3) 0.0190(10) Uani 1 d . . . N6 N 0.7243(3) 0.9915(6) 0.1907(3) 0.0167(11) Uani 1 d . . . N7 N 0.7040(2) 0.9964(6) 0.3074(3) 0.0166(10) Uani 1 d . . . N8 N 0.7585(3) 0.8123(6) 0.3250(3) 0.0190(10) Uani 1 d . . . C1 C 1.0651(3) 0.4808(8) -0.0458(3) 0.0267(15) Uani 1 d . . . H1 H 1.0692 0.5393 -0.0725 0.032 Uiso 1 calc R . . C2 C 1.0905(3) 0.3723(9) -0.0463(4) 0.0365(17) Uani 1 d . . . H2 H 1.1117 0.3566 -0.0726 0.044 Uiso 1 calc R . . C3 C 1.0839(4) 0.2888(9) -0.0077(5) 0.0439(19) Uani 1 d . . . H3 H 1.1004 0.2134 -0.0068 0.053 Uiso 1 calc R . . C4 C 1.0531(4) 0.3146(9) 0.0300(4) 0.0371(18) Uani 1 d . . . H4 H 1.0485 0.2578 0.0572 0.045 Uiso 1 calc R . . C5 C 1.0292(3) 0.4225(8) 0.0278(3) 0.0266(14) Uani 1 d . . . C6 C 0.9953(3) 0.4594(8) 0.0664(3) 0.0217(14) Uani 1 d . . . C7 C 0.9884(4) 0.3895(9) 0.1115(4) 0.0326(15) Uani 1 d . . . H7 H 1.0045 0.3146 0.1172 0.039 Uiso 1 calc R . . C8 C 0.9583(4) 0.4318(9) 0.1464(4) 0.0372(19) Uani 1 d . . . H8 H 0.9537 0.3872 0.1772 0.045 Uiso 1 calc R . . C9 C 0.9347(4) 0.5383(9) 0.1372(3) 0.0296(16) Uani 1 d . . . H9 H 0.9139 0.5695 0.1615 0.036 Uiso 1 calc R . . C10 C 0.9420(3) 0.5997(9) 0.0915(3) 0.0250(14) Uani 1 d . . . H10 H 0.9248 0.6725 0.0851 0.030 Uiso 1 calc R . . C11 C 0.9283(3) 0.4540(8) -0.0493(3) 0.0213(13) Uani 1 d . . . H11 H 0.9218 0.4383 -0.0145 0.026 Uiso 1 calc R . . C12 C 0.9099(3) 0.3773(8) -0.0857(3) 0.0252(14) Uani 1 d . . . H12 H 0.8914 0.3093 -0.0760 0.030 Uiso 1 calc R . . C13 C 0.9186(3) 0.4006(8) -0.1361(3) 0.0259(14) Uani 1 d . . . H13 H 0.9058 0.3488 -0.1615 0.031 Uiso 1 calc R . . C14 C 0.9455(3) 0.4977(8) -0.1502(3) 0.0256(15) Uani 1 d . . . H14 H 0.9514 0.5148 -0.1850 0.031 Uiso 1 calc R . . C15 C 0.9642(3) 0.5713(7) -0.1115(3) 0.0151(13) Uani 1 d . . . C16 C 0.9949(3) 0.6753(7) -0.1208(3) 0.0133(11) Uani 1 d . . . C17 C 1.0061(3) 0.7184(8) -0.1700(3) 0.0247(15) Uani 1 d . . . H17 H 0.9944 0.6795 -0.1996 0.030 Uiso 1 calc R . . C18 C 1.0342(4) 0.8172(8) -0.1735(4) 0.0296(17) Uani 1 d . . . H18 H 1.0414 0.8497 -0.2061 0.036 Uiso 1 calc R . . C19 C 1.0522(3) 0.8709(8) -0.1313(4) 0.0287(15) Uani 1 d . . . H19 H 1.0730 0.9375 -0.1343 0.034 Uiso 1 calc R . . C20 C 1.0396(3) 0.8257(8) -0.0837(3) 0.0216(13) Uani 1 d . . . H20 H 1.0512 0.8641 -0.0539 0.026 Uiso 1 calc R . . C21 C 1.0045(3) 0.8671(7) 0.0695(3) 0.0174(13) Uani 1 d . . . C22 C 1.0245(3) 0.9271(8) 0.1107(3) 0.0314(15) Uani 1 d . . . H22 H 1.0545 0.9103 0.1204 0.038 Uiso 1 calc R . . C23 C 0.9982(4) 1.0132(9) 0.1372(4) 0.0354(17) Uani 1 d . . . H23 H 1.0111 1.0549 0.1655 0.042 Uiso 1 calc R . . C24 C 0.9549(4) 1.0404(9) 0.1245(4) 0.0337(17) Uani 1 d . . . H24 H 0.9378 1.0983 0.1437 0.040 Uiso 1 calc R . . C25 C 0.9368(3) 0.9808(7) 0.0827(3) 0.0227(14) Uani 1 d . . . H25 H 0.9067 0.9985 0.0732 0.027 Uiso 1 calc R . . C26 C 0.9610(3) 0.8959(7) 0.0542(3) 0.0158(11) Uani 1 d . . . C27 C 0.8803(3) 0.8099(6) 0.0027(3) 0.0119(11) Uani 1 d . . . C28 C 0.8606(3) 0.6962(8) 0.0104(3) 0.0216(14) Uani 1 d . . . H28 H 0.8785 0.6233 0.0121 0.026 Uiso 1 calc R . . C29 C 0.8146(3) 0.6884(8) 0.0157(3) 0.0217(14) Uani 1 d . . . H29 H 0.8011 0.6090 0.0201 0.026 Uiso 1 calc R . . C30 C 0.7874(3) 0.7936(8) 0.0147(3) 0.0238(15) Uani 1 d . . . H30 H 0.7558 0.7880 0.0187 0.029 Uiso 1 calc R . . C31 C 0.8085(3) 0.9066(8) 0.0077(3) 0.0245(14) Uani 1 d . . . H31 H 0.7907 0.9798 0.0079 0.029 Uiso 1 calc R . . C32 C 0.8543(3) 0.9190(7) 0.0002(3) 0.0182(13) Uani 1 d . . . H32 H 0.8676 0.9977 -0.0064 0.022 Uiso 1 calc R . . C33 C 0.9483(3) 0.9452(7) -0.0509(3) 0.0175(12) Uani 1 d . . . C34 C 0.9314(3) 0.9250(8) -0.1004(3) 0.0237(15) Uani 1 d . . . H34 H 0.9137 0.8539 -0.1076 0.028 Uiso 1 calc R . . C35 C 0.9411(4) 1.0095(8) -0.1382(4) 0.0317(18) Uani 1 d . . . H35 H 0.9287 0.9981 -0.1712 0.038 Uiso 1 calc R . . C36 C 0.9685(3) 1.1107(9) -0.1291(4) 0.0316(16) Uani 1 d . . . H36 H 0.9762 1.1653 -0.1562 0.038 Uiso 1 calc R . . C37 C 0.9842(3) 1.1316(8) -0.0818(3) 0.0280(17) Uani 1 d . . . H37 H 1.0019 1.2033 -0.0754 0.034 Uiso 1 calc R . . C38 C 0.9749(3) 1.0497(7) -0.0421(3) 0.0211(15) Uani 1 d . . . H38 H 0.9866 1.0651 -0.0090 0.025 Uiso 1 calc R . . C39 C 1.0767(3) 0.7677(9) 0.0456(4) 0.0287(15) Uani 1 d . . . H39A H 1.0896 0.8515 0.0511 0.034 Uiso 1 calc R . . H39B H 1.0894 0.7341 0.0136 0.034 Uiso 1 calc R . . C40 C 1.0896(4) 0.6843(9) 0.0894(4) 0.0402(17) Uani 1 d . . . H40A H 1.0764 0.7162 0.1210 0.060 Uiso 1 calc R . . H40B H 1.1223 0.6826 0.0927 0.060 Uiso 1 calc R . . H40C H 1.0786 0.6000 0.0830 0.060 Uiso 1 calc R . . C41 C 0.8137(3) 1.0597(9) 0.2999(3) 0.0267(15) Uani 1 d . . . H41 H 0.8171 0.9981 0.3255 0.032 Uiso 1 calc R . . C42 C 0.8380(3) 1.1692(9) 0.3042(4) 0.0365(17) Uani 1 d . . . H42 H 0.8567 1.1831 0.3329 0.044 Uiso 1 calc R . . C43 C 0.8349(4) 1.2560(9) 0.2670(5) 0.0439(19) Uani 1 d . . . H43 H 0.8524 1.3296 0.2687 0.053 Uiso 1 calc R . . C44 C 0.8062(4) 1.2369(9) 0.2267(4) 0.0371(18) Uani 1 d . . . H44 H 0.8038 1.2972 0.2004 0.045 Uiso 1 calc R . . C45 C 0.7806(3) 1.1281(8) 0.2248(3) 0.0266(14) Uani 1 d . . . C46 C 0.7491(3) 1.0978(8) 0.1840(3) 0.0217(14) Uani 1 d . . . C47 C 0.7441(4) 1.1718(9) 0.1418(4) 0.0326(15) Uani 1 d . . . H47 H 0.7611 1.2460 0.1391 0.039 Uiso 1 calc R . . C48 C 0.7142(4) 1.1402(9) 0.1024(4) 0.0372(19) Uani 1 d . . . H48 H 0.7110 1.1903 0.0729 0.045 Uiso 1 calc R . . C49 C 0.6898(4) 1.0315(8) 0.1091(3) 0.0296(16) Uani 1 d . . . H49 H 0.6688 1.0055 0.0841 0.036 Uiso 1 calc R . . C50 C 0.6965(3) 0.9607(8) 0.1535(3) 0.0250(14) Uani 1 d . . . H50 H 0.6799 0.8858 0.1570 0.030 Uiso 1 calc R . . C51 C 0.6786(3) 1.0945(8) 0.2954(3) 0.0213(13) Uani 1 d . . . H51 H 0.6746 1.1150 0.2605 0.026 Uiso 1 calc R . . C52 C 0.6578(3) 1.1676(8) 0.3320(3) 0.0252(14) Uani 1 d . . . H52 H 0.6396 1.2358 0.3219 0.030 Uiso 1 calc R . . C53 C 0.6634(3) 1.1413(8) 0.3831(3) 0.0259(14) Uani 1 d . . . H53 H 0.6491 1.1896 0.4087 0.031 Uiso 1 calc R . . C54 C 0.6910(3) 1.0402(8) 0.3956(3) 0.0256(15) Uani 1 d . . . H54 H 0.6964 1.0207 0.4303 0.031 Uiso 1 calc R . . C55 C 0.7102(3) 0.9694(7) 0.3582(3) 0.0151(13) Uani 1 d . . . C56 C 0.7390(3) 0.8631(7) 0.3675(3) 0.0133(11) Uani 1 d . . . C57 C 0.7478(3) 0.8156(8) 0.4154(3) 0.0247(15) Uani 1 d . . . H57 H 0.7349 0.8532 0.4447 0.030 Uiso 1 calc R . . C58 C 0.7753(4) 0.7136(8) 0.4203(4) 0.0296(17) Uani 1 d . . . H58 H 0.7805 0.6775 0.4528 0.036 Uiso 1 calc R . . C59 C 0.7954(3) 0.6641(9) 0.3769(4) 0.0287(15) Uani 1 d . . . H59 H 0.8156 0.5959 0.3791 0.034 Uiso 1 calc R . . C60 C 0.7851(3) 0.7175(8) 0.3306(3) 0.0216(13) Uani 1 d . . . H60 H 0.7982 0.6828 0.3009 0.026 Uiso 1 calc R . . C61 C 0.7528(3) 0.6809(7) 0.1763(3) 0.0174(13) Uani 1 d . . . C62 C 0.7735(3) 0.6138(8) 0.1367(3) 0.0314(15) Uani 1 d . . . H62 H 0.8044 0.6244 0.1291 0.038 Uiso 1 calc R . . C63 C 0.7473(4) 0.5322(8) 0.1092(4) 0.0354(17) Uani 1 d . . . H63 H 0.7607 0.4885 0.0817 0.042 Uiso 1 calc R . . C64 C 0.7025(4) 0.5109(8) 0.1196(4) 0.0337(17) Uani 1 d . . . H64 H 0.6855 0.4547 0.0995 0.040 Uiso 1 calc R . . C65 C 0.6829(4) 0.5740(7) 0.1606(3) 0.0227(14) Uani 1 d . . . H65 H 0.6524 0.5598 0.1689 0.027 Uiso 1 calc R . . C66 C 0.7085(3) 0.6583(7) 0.1891(3) 0.0158(11) Uani 1 d . . . C67 C 0.6282(3) 0.7531(6) 0.2392(3) 0.0119(11) Uani 1 d . . . C68 C 0.6099(3) 0.8702(8) 0.2293(3) 0.0216(14) Uani 1 d . . . H68 H 0.6290 0.9407 0.2271 0.026 Uiso 1 calc R . . C69 C 0.5642(3) 0.8842(8) 0.2226(3) 0.0217(14) Uani 1 d . . . H69 H 0.5520 0.9637 0.2150 0.026 Uiso 1 calc R . . C70 C 0.5366(3) 0.7833(8) 0.2270(3) 0.0238(15) Uani 1 d . . . H70 H 0.5051 0.7941 0.2231 0.029 Uiso 1 calc R . . C71 C 0.5529(3) 0.6682(9) 0.2368(3) 0.0245(14) Uani 1 d . . . H71 H 0.5333 0.5988 0.2393 0.029 Uiso 1 calc R . . C72 C 0.5998(3) 0.6529(8) 0.2433(3) 0.0182(13) Uani 1 d . . . H72 H 0.6116 0.5729 0.2505 0.022 Uiso 1 calc R . . C73 C 0.6922(3) 0.6070(8) 0.2933(3) 0.0175(12) Uani 1 d . . . C74 C 0.7180(3) 0.5025(7) 0.2850(3) 0.0237(15) Uani 1 d . . . H74 H 0.7309 0.4895 0.2523 0.028 Uiso 1 calc R . . C75 C 0.7255(4) 0.4178(8) 0.3224(3) 0.0317(18) Uani 1 d . . . H75 H 0.7424 0.3449 0.3152 0.038 Uiso 1 calc R . . C76 C 0.7085(4) 0.4372(8) 0.3716(4) 0.0316(16) Uani 1 d . . . H76 H 0.7145 0.3795 0.3982 0.038 Uiso 1 calc R . . C77 C 0.6828(3) 0.5421(8) 0.3808(4) 0.0280(17) Uani 1 d . . . H77 H 0.6707 0.5562 0.4138 0.034 Uiso 1 calc R . . C78 C 0.6746(3) 0.6274(7) 0.3415(3) 0.0211(15) Uani 1 d . . . H78 H 0.6569 0.6992 0.3479 0.025 Uiso 1 calc R . . C79 C 0.8250(3) 0.7794(9) 0.2003(4) 0.0287(15) Uani 1 d . . . H79A H 0.8380 0.6958 0.1951 0.034 Uiso 1 calc R . . H79B H 0.8381 0.8146 0.2318 0.034 Uiso 1 calc R . . C80 C 0.8371(4) 0.8615(9) 0.1557(4) 0.0402(17) Uani 1 d . . . H80A H 0.8265 0.8232 0.1241 0.060 Uiso 1 calc R . . H80B H 0.8697 0.8714 0.1542 0.060 Uiso 1 calc R . . H80C H 0.8230 0.9432 0.1599 0.060 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01232(18) 0.01915(18) 0.01128(18) 0.0027(2) 0.0006(3) -0.0002(2) Ru2 0.01232(18) 0.01915(18) 0.01128(18) 0.0027(2) 0.0006(3) -0.0002(2) P1 0.01661(8) 0.01292(18) 0.01130(8) 0.0013(7) -0.0033(7) 0.0015(7) P2 0.0131(7) 0.0170(7) 0.0130(7) -0.0003(9) 0.0026(10) -0.0025(9) P3 0.0287(17) 0.0524(17) 0.0285(14) 0.0019(13) 0.0019(13) 0.0121(14) P4 0.0289(17) 0.0185(12) 0.0348(16) 0.0024(11) 0.0069(13) 0.0026(12) P5 0.0323(19) 0.0290(15) 0.0441(19) 0.0146(13) -0.0104(15) 0.0010(13) P6 0.044(2) 0.086(2) 0.0320(17) -0.0117(17) 0.0012(16) -0.0295(19) F1 0.169(10) 0.131(7) 0.042(5) -0.004(5) -0.014(5) 0.121(7) F2 0.035(5) 0.181(9) 0.089(6) -0.004(6) 0.024(4) -0.011(6) F3 0.053(5) 0.075(5) 0.072(5) 0.014(4) -0.024(4) 0.011(4) F4 0.103(7) 0.056(4) 0.061(5) -0.022(3) 0.046(5) -0.025(4) F5 0.037(4) 0.084(4) 0.050(4) -0.014(4) -0.013(3) -0.001(3) F6 0.110(8) 0.088(5) 0.041(4) -0.022(4) 0.004(4) 0.005(5) F7 0.062(5) 0.019(3) 0.083(5) 0.024(3) 0.022(4) 0.006(3) F8 0.041(6) 0.116(6) 0.068(5) 0.028(4) 0.004(4) 0.000(4) F9 0.069(6) 0.031(3) 0.061(4) 0.015(3) 0.022(4) 0.015(3) F10 0.025(4) 0.079(4) 0.039(4) 0.010(3) -0.010(3) -0.010(3) F11 0.106(6) 0.033(3) 0.041(4) -0.004(3) 0.041(4) 0.001(3) F12 0.056(5) 0.052(4) 0.051(4) -0.021(3) 0.017(3) 0.001(3) F13 0.054(5) 0.090(5) 0.099(6) 0.082(5) 0.005(4) -0.001(4) F14 0.073(8) 0.112(7) 0.149(9) 0.097(6) -0.059(7) -0.040(6) F15 0.038(4) 0.048(4) 0.082(5) 0.045(4) -0.026(4) -0.010(3) F16 0.029(6) 0.224(11) 0.193(12) 0.164(10) -0.033(7) -0.025(7) F17 0.193(15) 0.115(8) 0.097(8) -0.022(6) 0.070(8) -0.026(8) F18 0.45(2) 0.031(4) 0.105(8) -0.036(5) 0.092(10) -0.065(7) F19 0.052(5) 0.075(5) 0.063(5) 0.011(4) -0.001(4) -0.002(4) F20 0.085(6) 0.055(4) 0.090(6) -0.009(4) -0.044(5) -0.008(4) F21 0.179(11) 0.153(7) 0.053(5) -0.020(6) 0.019(6) -0.121(7) F22 0.022(5) 0.196(10) 0.171(10) -0.070(8) -0.033(5) 0.008(6) F23 0.091(7) 0.129(7) 0.041(4) -0.029(4) -0.004(4) -0.053(6) F24 0.051(5) 0.120(6) 0.064(5) -0.039(5) 0.015(4) -0.023(5) O1 0.008(2) 0.033(2) 0.020(2) -0.0044(18) 0.000(2) -0.001(2) O2 0.008(2) 0.033(2) 0.020(2) -0.0044(18) 0.000(2) -0.001(2) N1 0.016(2) 0.028(2) 0.014(2) -0.002(2) 0.000(3) 0.000(2) N2 0.015(3) 0.020(2) 0.016(2) -0.005(2) 0.001(3) 0.001(2) N3 0.013(3) 0.021(2) 0.016(2) 0.008(2) 0.001(2) 0.000(2) N4 0.015(3) 0.024(3) 0.018(2) 0.002(2) 0.003(3) -0.005(3) N5 0.016(2) 0.028(2) 0.014(2) -0.002(2) 0.000(3) 0.000(2) N6 0.015(3) 0.020(2) 0.016(2) -0.005(2) 0.001(3) 0.001(2) N7 0.013(3) 0.021(2) 0.016(2) 0.008(2) 0.001(2) 0.000(2) N8 0.015(3) 0.024(3) 0.018(2) 0.002(2) 0.003(3) -0.005(3) C1 0.018(3) 0.040(4) 0.022(3) 0.007(3) -0.004(3) -0.001(3) C2 0.021(4) 0.051(4) 0.037(4) -0.008(4) 0.000(4) 0.007(4) C3 0.038(4) 0.040(4) 0.053(5) 0.010(4) 0.000(5) 0.001(4) C4 0.048(5) 0.031(4) 0.033(4) 0.010(3) 0.004(4) -0.001(4) C5 0.026(4) 0.033(3) 0.021(3) -0.004(3) -0.002(3) 0.000(3) C6 0.019(4) 0.023(3) 0.023(3) 0.002(3) 0.000(3) -0.005(3) C7 0.042(4) 0.030(3) 0.026(3) 0.014(3) -0.003(4) -0.009(4) C8 0.042(5) 0.046(4) 0.023(4) 0.020(3) 0.007(4) -0.002(4) C9 0.039(4) 0.039(4) 0.011(3) 0.013(3) -0.002(3) -0.006(4) C10 0.028(4) 0.031(3) 0.015(3) 0.001(3) 0.003(3) -0.003(3) C11 0.019(3) 0.029(3) 0.016(3) 0.002(3) 0.000(3) 0.002(3) C12 0.027(4) 0.015(3) 0.033(3) -0.005(3) -0.002(4) -0.002(3) C13 0.029(4) 0.030(3) 0.019(3) -0.011(3) 0.005(3) -0.002(3) C14 0.025(4) 0.040(4) 0.012(3) 0.001(3) -0.002(3) 0.003(3) C15 0.020(3) 0.016(3) 0.009(3) -0.001(2) -0.003(3) 0.002(3) C16 0.012(3) 0.017(3) 0.011(2) 0.001(2) 0.005(3) 0.001(3) C17 0.035(4) 0.031(4) 0.008(3) 0.003(2) 0.000(3) -0.007(3) C18 0.037(5) 0.031(4) 0.020(3) 0.012(3) 0.006(4) -0.001(3) C19 0.019(4) 0.035(4) 0.032(3) 0.017(3) -0.001(4) -0.001(3) C20 0.021(3) 0.028(3) 0.016(3) 0.003(3) -0.003(3) 0.000(3) C21 0.022(3) 0.020(3) 0.010(3) 0.005(2) 0.002(3) -0.001(3) C22 0.027(4) 0.040(4) 0.028(3) -0.005(3) 0.000(4) 0.000(4) C23 0.049(5) 0.034(3) 0.023(3) -0.010(3) 0.000(4) -0.001(4) C24 0.046(5) 0.028(4) 0.027(4) -0.006(3) -0.002(4) -0.001(4) C25 0.032(4) 0.021(3) 0.015(3) -0.005(2) 0.000(3) -0.005(3) C26 0.016(3) 0.022(3) 0.009(3) -0.001(3) -0.002(3) -0.002(3) C27 0.014(3) 0.010(2) 0.012(3) 0.000(2) 0.001(3) -0.001(2) C28 0.029(4) 0.023(3) 0.012(3) 0.000(2) 0.003(3) 0.003(3) C29 0.021(3) 0.023(3) 0.021(3) -0.001(3) -0.006(3) -0.007(3) C30 0.016(3) 0.038(4) 0.017(3) -0.005(3) 0.002(3) 0.004(3) C31 0.017(3) 0.032(3) 0.025(3) -0.005(3) 0.004(3) -0.001(3) C32 0.025(3) 0.019(3) 0.011(3) 0.000(2) -0.001(3) 0.007(3) C33 0.018(3) 0.024(3) 0.010(3) 0.005(2) 0.000(3) -0.003(3) C34 0.021(4) 0.023(4) 0.028(4) 0.000(3) -0.008(3) -0.005(3) C35 0.039(5) 0.029(4) 0.027(4) 0.006(3) -0.002(4) 0.010(3) C36 0.039(5) 0.028(3) 0.028(4) 0.015(3) 0.000(4) 0.003(4) C37 0.033(4) 0.028(4) 0.023(4) 0.007(3) 0.002(3) -0.013(3) C38 0.030(4) 0.012(3) 0.021(3) 0.002(3) -0.003(3) -0.001(3) C39 0.009(3) 0.059(4) 0.019(3) 0.005(3) -0.001(4) 0.005(3) C40 0.028(4) 0.054(4) 0.039(4) 0.003(3) 0.000(4) -0.002(4) C41 0.018(3) 0.040(4) 0.022(3) 0.007(3) -0.004(3) -0.001(3) C42 0.021(4) 0.051(4) 0.037(4) -0.008(4) 0.000(4) 0.007(4) C43 0.038(4) 0.040(4) 0.053(5) 0.010(4) 0.000(5) 0.001(4) C44 0.048(5) 0.031(4) 0.033(4) 0.010(3) 0.004(4) -0.001(4) C45 0.026(4) 0.033(3) 0.021(3) -0.004(3) -0.002(3) 0.000(3) C46 0.019(4) 0.023(3) 0.023(3) 0.002(3) 0.000(3) -0.005(3) C47 0.042(4) 0.030(3) 0.026(3) 0.014(3) -0.003(4) -0.009(4) C48 0.042(5) 0.046(4) 0.023(4) 0.020(3) 0.007(4) -0.002(4) C49 0.039(4) 0.039(4) 0.011(3) 0.013(3) -0.002(3) -0.006(4) C50 0.028(4) 0.031(3) 0.015(3) 0.001(3) 0.003(3) -0.003(3) C51 0.019(3) 0.029(3) 0.016(3) 0.002(3) 0.000(3) 0.002(3) C52 0.027(4) 0.015(3) 0.033(3) -0.005(3) -0.002(4) -0.002(3) C53 0.029(4) 0.030(3) 0.019(3) -0.011(3) 0.005(3) -0.002(3) C54 0.025(4) 0.040(4) 0.012(3) 0.001(3) -0.002(3) 0.003(3) C55 0.020(3) 0.016(3) 0.009(3) -0.001(2) -0.003(3) 0.002(3) C56 0.012(3) 0.017(3) 0.011(2) 0.001(2) 0.005(3) 0.001(3) C57 0.035(4) 0.031(4) 0.008(3) 0.003(2) 0.000(3) -0.007(3) C58 0.037(5) 0.031(4) 0.020(3) 0.012(3) 0.006(4) -0.001(3) C59 0.019(4) 0.035(4) 0.032(3) 0.017(3) -0.001(4) -0.001(3) C60 0.021(3) 0.028(3) 0.016(3) 0.003(3) -0.003(3) 0.000(3) C61 0.022(3) 0.020(3) 0.010(3) 0.005(2) 0.002(3) -0.001(3) C62 0.027(4) 0.040(4) 0.028(3) -0.005(3) 0.000(4) 0.000(4) C63 0.049(5) 0.034(3) 0.023(3) -0.010(3) 0.000(4) -0.001(4) C64 0.046(5) 0.028(4) 0.027(4) -0.006(3) -0.002(4) -0.001(4) C65 0.032(4) 0.021(3) 0.015(3) -0.005(2) 0.000(3) -0.005(3) C66 0.016(3) 0.022(3) 0.009(3) -0.001(3) -0.002(3) -0.002(3) C67 0.014(3) 0.010(2) 0.012(3) 0.000(2) 0.001(3) -0.001(2) C68 0.029(4) 0.023(3) 0.012(3) 0.000(2) 0.003(3) 0.003(3) C69 0.021(3) 0.023(3) 0.021(3) -0.001(3) -0.006(3) -0.007(3) C70 0.016(3) 0.038(4) 0.017(3) -0.005(3) 0.002(3) 0.004(3) C71 0.017(3) 0.032(3) 0.025(3) -0.005(3) 0.004(3) -0.001(3) C72 0.025(3) 0.019(3) 0.011(3) 0.000(2) -0.001(3) 0.007(3) C73 0.018(3) 0.024(3) 0.010(3) 0.005(2) 0.000(3) -0.003(3) C74 0.021(4) 0.023(4) 0.028(4) 0.000(3) -0.008(3) -0.005(3) C75 0.039(5) 0.029(4) 0.027(4) 0.006(3) -0.002(4) 0.010(3) C76 0.039(5) 0.028(3) 0.028(4) 0.015(3) 0.000(4) 0.003(4) C77 0.033(4) 0.028(4) 0.023(4) 0.007(3) 0.002(3) -0.013(3) C78 0.030(4) 0.012(3) 0.021(3) 0.002(3) -0.003(3) -0.001(3) C79 0.009(3) 0.059(4) 0.019(3) 0.005(3) -0.001(4) 0.005(3) C80 0.028(4) 0.054(4) 0.039(4) 0.003(3) 0.000(4) -0.002(4) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)]' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.32(4) _refine_ls_number_reflns 12548 _refine_ls_number_parameters 819 _refine_ls_number_restraints 1 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.919 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.978 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.103 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N3 2.018(7) . ? Ru1 N4 2.064(7) . ? Ru1 N2 2.082(7) . ? Ru1 N1 2.126(6) . ? Ru1 O1 2.199(6) . ? Ru1 P1 2.289(2) . ? Ru2 N7 2.012(7) . ? Ru2 N8 2.064(7) . ? Ru2 N6 2.092(7) . ? Ru2 N5 2.109(6) . ? Ru2 O2 2.200(6) . ? Ru2 P2 2.277(2) . ? P1 C26 1.812(8) . ? P1 C27 1.821(9) . ? P1 C33 1.827(8) . ? P2 C66 1.818(8) . ? P2 C67 1.818(9) . ? P2 C73 1.830(8) . ? P3 F2 1.555(8) . ? P3 F1 1.563(7) . ? P3 F3 1.585(7) . ? P3 F4 1.589(8) . ? P3 F5 1.591(7) . ? P3 F6 1.596(7) . ? P4 F9 1.577(6) . ? P4 F8 1.583(9) . ? P4 F12 1.587(6) . ? P4 F11 1.597(7) . ? P4 F10 1.604(7) . ? P4 F7 1.606(6) . ? P5 F18 1.472(8) . ? P5 F16 1.517(9) . ? P5 F17 1.557(9) . ? P5 F14 1.561(9) . ? P5 F13 1.574(6) . ? P5 F15 1.590(6) . ? P6 F22 1.560(9) . ? P6 F23 1.595(7) . ? P6 F20 1.597(8) . ? P6 F19 1.603(8) . ? P6 F24 1.606(7) . ? P6 F21 1.607(8) . ? O1 C21 1.403(10) . ? O1 C39 1.482(11) . ? O2 C61 1.419(10) . ? O2 C79 1.460(11) . ? N1 C5 1.339(11) . ? N1 C1 1.345(11) . ? N2 C10 1.328(11) . ? N2 C6 1.370(11) . ? N3 C11 1.346(11) . ? N3 C15 1.369(10) . ? N4 C16 1.335(10) . ? N4 C20 1.347(11) . ? N5 C41 1.350(11) . ? N5 C45 1.370(11) . ? N6 C50 1.325(11) . ? N6 C46 1.373(10) . ? N7 C51 1.337(10) . ? N7 C55 1.378(10) . ? N8 C60 1.300(11) . ? N8 C56 1.371(10) . ? C1 C2 1.392(13) . ? C2 C3 1.370(14) . ? C3 C4 1.378(16) . ? C4 C5 1.362(13) . ? C5 C6 1.486(13) . ? C6 C7 1.417(12) . ? C7 C8 1.363(14) . ? C8 C9 1.366(13) . ? C9 C10 1.387(12) . ? C11 C12 1.376(11) . ? C12 C13 1.372(12) . ? C13 C14 1.370(12) . ? C14 C15 1.403(12) . ? C15 C16 1.465(11) . ? C16 C17 1.414(11) . ? C17 C18 1.357(13) . ? C18 C19 1.360(13) . ? C19 C20 1.394(12) . ? C21 C26 1.393(12) . ? C21 C22 1.395(12) . ? C22 C23 1.398(13) . ? C23 C24 1.367(15) . ? C24 C25 1.382(13) . ? C25 C26 1.384(11) . ? C27 C28 1.372(11) . ? C27 C32 1.409(10) . ? C28 C29 1.384(13) . ? C29 C30 1.393(12) . ? C30 C31 1.382(12) . ? C31 C32 1.387(12) . ? C33 C38 1.396(11) . ? C33 C34 1.412(12) . ? C34 C35 1.375(12) . ? C35 C36 1.381(13) . ? C36 C37 1.348(13) . ? C37 C38 1.392(11) . ? C39 C40 1.509(13) . ? C41 C42 1.389(13) . ? C42 C43 1.354(14) . ? C43 C44 1.376(16) . ? C44 C45 1.398(13) . ? C45 C46 1.464(12) . ? C46 C47 1.372(12) . ? C47 C48 1.406(14) . ? C48 C49 1.389(13) . ? C49 C50 1.405(12) . ? C51 C52 1.387(12) . ? C52 C53 1.380(12) . ? C53 C54 1.403(12) . ? C54 C55 1.368(12) . ? C55 C56 1.453(11) . ? C56 C57 1.382(11) . ? C57 C58 1.377(13) . ? C58 C59 1.395(13) . ? C59 C60 1.379(12) . ? C61 C66 1.389(12) . ? C61 C62 1.408(12) . ? C62 C63 1.379(13) . ? C63 C64 1.384(15) . ? C64 C65 1.399(13) . ? C65 C66 1.403(11) . ? C67 C72 1.375(11) . ? C67 C68 1.397(11) . ? C68 C69 1.385(12) . ? C69 C70 1.369(12) . ? C70 C71 1.356(12) . ? C71 C72 1.418(12) . ? C73 C74 1.380(12) . ? C73 C78 1.388(11) . ? C74 C75 1.359(11) . ? C75 C76 1.405(13) . ? C76 C77 1.386(13) . ? C77 C78 1.402(11) . ? C79 C80 1.511(13) . ? #------------------------------------------------------------------------------ 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_3 _geom_angle_publ_flag N3 Ru1 N4 78.8(3) . . ? N3 Ru1 N2 98.8(3) . . ? N4 Ru1 N2 172.7(3) . . ? N3 Ru1 N1 84.5(3) . . ? N4 Ru1 N1 95.2(3) . . ? N2 Ru1 N1 77.7(3) . . ? N3 Ru1 O1 176.8(3) . . ? N4 Ru1 O1 97.9(3) . . ? N2 Ru1 O1 84.3(2) . . ? N1 Ru1 O1 95.5(2) . . ? N3 Ru1 P1 100.7(2) . . ? N4 Ru1 P1 89.0(2) . . ? N2 Ru1 P1 98.25(19) . . ? N1 Ru1 P1 173.9(2) . . ? O1 Ru1 P1 79.48(17) . . ? N7 Ru2 N8 79.4(3) . . ? N7 Ru2 N6 99.1(3) . . ? N8 Ru2 N6 171.7(3) . . ? N7 Ru2 N5 83.8(3) . . ? N8 Ru2 N5 94.0(3) . . ? N6 Ru2 N5 77.7(3) . . ? N7 Ru2 O2 176.0(2) . . ? N8 Ru2 O2 96.7(3) . . ? N6 Ru2 O2 84.9(2) . . ? N5 Ru2 O2 97.4(2) . . ? N7 Ru2 P2 99.6(2) . . ? N8 Ru2 P2 89.3(2) . . ? N6 Ru2 P2 99.0(2) . . ? N5 Ru2 P2 175.7(2) . . ? O2 Ru2 P2 79.41(17) . . ? C26 P1 C27 106.5(4) . . ? C26 P1 C33 102.2(4) . . ? C27 P1 C33 103.5(4) . . ? C26 P1 Ru1 101.6(3) . . ? C27 P1 Ru1 124.8(2) . . ? C33 P1 Ru1 115.6(3) . . ? C66 P2 C67 106.7(4) . . ? C66 P2 C73 101.8(4) . . ? C67 P2 C73 102.9(4) . . ? C66 P2 Ru2 102.4(3) . . ? C67 P2 Ru2 124.8(2) . . ? C73 P2 Ru2 115.6(3) . . ? F2 P3 F1 91.3(6) . . ? F2 P3 F3 90.4(5) . . ? F1 P3 F3 178.2(6) . . ? F2 P3 F4 178.4(5) . . ? F1 P3 F4 90.0(5) . . ? F3 P3 F4 88.3(4) . . ? F2 P3 F5 92.0(5) . . ? F1 P3 F5 90.8(4) . . ? F3 P3 F5 89.2(4) . . ? F4 P3 F5 88.9(4) . . ? F2 P3 F6 90.1(5) . . ? F1 P3 F6 89.5(4) . . ? F3 P3 F6 90.3(4) . . ? F4 P3 F6 89.0(4) . . ? F5 P3 F6 177.9(5) . . ? F9 P4 F8 92.1(4) . . ? F9 P4 F12 89.9(4) . . ? F8 P4 F12 91.1(4) . . ? F9 P4 F11 91.5(3) . . ? F8 P4 F11 90.5(4) . . ? F12 P4 F11 177.8(4) . . ? F9 P4 F10 89.9(4) . . ? F8 P4 F10 178.0(4) . . ? F12 P4 F10 88.5(4) . . ? F11 P4 F10 89.8(4) . . ? F9 P4 F7 178.0(4) . . ? F8 P4 F7 89.7(4) . . ? F12 P4 F7 91.0(3) . . ? F11 P4 F7 87.6(3) . . ? F10 P4 F7 88.3(4) . . ? F18 P5 F16 95.8(8) . . ? F18 P5 F17 178.6(9) . . ? F16 P5 F17 85.5(8) . . ? F18 P5 F14 94.1(8) . . ? F16 P5 F14 170.0(7) . . ? F17 P5 F14 84.6(7) . . ? F18 P5 F13 90.2(5) . . ? F16 P5 F13 88.4(4) . . ? F17 P5 F13 89.4(5) . . ? F14 P5 F13 93.0(4) . . ? F18 P5 F15 90.6(5) . . ? F16 P5 F15 91.0(4) . . ? F17 P5 F15 89.9(5) . . ? F14 P5 F15 87.5(4) . . ? F13 P5 F15 179.1(5) . . ? F22 P6 F23 89.1(5) . . ? F22 P6 F20 178.7(5) . . ? F23 P6 F20 89.7(5) . . ? F22 P6 F19 91.2(6) . . ? F23 P6 F19 90.3(4) . . ? F20 P6 F19 88.4(4) . . ? F22 P6 F24 91.0(5) . . ? F23 P6 F24 178.5(5) . . ? F20 P6 F24 90.2(4) . . ? F19 P6 F24 88.2(4) . . ? F22 P6 F21 91.9(6) . . ? F23 P6 F21 89.8(5) . . ? F20 P6 F21 88.5(5) . . ? F19 P6 F21 176.9(6) . . ? F24 P6 F21 91.7(4) . . ? C21 O1 C39 119.1(7) . . ? C21 O1 Ru1 118.7(5) . . ? C39 O1 Ru1 122.2(5) . . ? C61 O2 C79 119.0(7) . . ? C61 O2 Ru2 118.6(5) . . ? C79 O2 Ru2 122.2(5) . . ? C5 N1 C1 117.7(7) . . ? C5 N1 Ru1 116.3(6) . . ? C1 N1 Ru1 125.2(6) . . ? C10 N2 C6 116.2(8) . . ? C10 N2 Ru1 128.3(6) . . ? C6 N2 Ru1 115.3(6) . . ? C11 N3 C15 117.9(7) . . ? C11 N3 Ru1 125.6(6) . . ? C15 N3 Ru1 116.2(5) . . ? C16 N4 C20 119.2(7) . . ? C16 N4 Ru1 115.6(6) . . ? C20 N4 Ru1 125.2(6) . . ? C41 N5 C45 117.3(7) . . ? C41 N5 Ru2 126.0(6) . . ? C45 N5 Ru2 115.5(6) . . ? C50 N6 C46 116.8(7) . . ? C50 N6 Ru2 127.6(6) . . ? C46 N6 Ru2 115.5(5) . . ? C51 N7 C55 118.0(7) . . ? C51 N7 Ru2 125.2(6) . . ? C55 N7 Ru2 116.6(5) . . ? C60 N8 C56 118.6(7) . . ? C60 N8 Ru2 126.9(6) . . ? C56 N8 Ru2 114.4(6) . . ? N1 C1 C2 123.0(9) . . ? C3 C2 C1 117.6(10) . . ? C2 C3 C4 119.8(10) . . ? C5 C4 C3 119.4(10) . . ? N1 C5 C4 122.6(9) . . ? N1 C5 C6 113.7(8) . . ? C4 C5 C6 123.7(9) . . ? N2 C6 C7 121.8(8) . . ? N2 C6 C5 116.4(7) . . ? C7 C6 C5 121.7(8) . . ? C8 C7 C6 118.7(9) . . ? C7 C8 C9 120.0(9) . . ? C8 C9 C10 118.2(9) . . ? N2 C10 C9 124.9(9) . . ? N3 C11 C12 122.7(8) . . ? C13 C12 C11 119.0(9) . . ? C14 C13 C12 120.7(8) . . ? C13 C14 C15 118.0(8) . . ? N3 C15 C14 121.8(8) . . ? N3 C15 C16 114.2(7) . . ? C14 C15 C16 124.0(8) . . ? N4 C16 C17 121.6(8) . . ? N4 C16 C15 115.0(7) . . ? C17 C16 C15 123.4(8) . . ? C18 C17 C16 117.7(8) . . ? C17 C18 C19 121.5(9) . . ? C18 C19 C20 118.4(9) . . ? N4 C20 C19 121.5(8) . . ? C26 C21 C22 121.3(8) . . ? C26 C21 O1 116.8(7) . . ? C22 C21 O1 121.9(8) . . ? C21 C22 C23 116.9(9) . . ? C24 C23 C22 123.4(9) . . ? C23 C24 C25 117.7(9) . . ? C24 C25 C26 122.1(9) . . ? C25 C26 C21 118.5(8) . . ? C25 C26 P1 124.6(7) . . ? C21 C26 P1 116.9(6) . . ? C28 C27 C32 120.9(9) . . ? C28 C27 P1 120.3(6) . . ? C32 C27 P1 118.8(6) . . ? C27 C28 C29 119.6(8) . . ? C28 C29 C30 121.8(9) . . ? C31 C30 C29 116.9(10) . . ? C30 C31 C32 123.6(9) . . ? C31 C32 C27 117.1(8) . . ? C38 C33 C34 118.6(7) . . ? C38 C33 P1 122.7(6) . . ? C34 C33 P1 118.2(6) . . ? C35 C34 C33 119.2(8) . . ? C34 C35 C36 121.4(9) . . ? C37 C36 C35 119.7(9) . . ? C36 C37 C38 121.0(9) . . ? C37 C38 C33 120.0(8) . . ? O1 C39 C40 111.4(8) . . ? N5 C41 C42 122.9(9) . . ? C43 C42 C41 119.3(10) . . ? C42 C43 C44 119.6(10) . . ? C43 C44 C45 119.5(9) . . ? N5 C45 C44 121.2(9) . . ? N5 C45 C46 114.4(8) . . ? C44 C45 C46 124.3(8) . . ? C47 C46 N6 121.9(8) . . ? C47 C46 C45 122.2(8) . . ? N6 C46 C45 115.9(7) . . ? C46 C47 C48 121.5(9) . . ? C49 C48 C47 116.3(9) . . ? C48 C49 C50 119.1(9) . . ? N6 C50 C49 124.4(9) . . ? N7 C51 C52 122.6(8) . . ? C53 C52 C51 120.2(8) . . ? C52 C53 C54 117.2(8) . . ? C55 C54 C53 120.7(8) . . ? C54 C55 N7 121.4(8) . . ? C54 C55 C56 124.5(8) . . ? N7 C55 C56 114.1(7) . . ? N8 C56 C57 120.9(8) . . ? N8 C56 C55 115.4(7) . . ? C57 C56 C55 123.7(8) . . ? C58 C57 C56 119.5(8) . . ? C57 C58 C59 119.0(9) . . ? C60 C59 C58 117.7(9) . . ? N8 C60 C59 124.3(9) . . ? C66 C61 C62 120.6(8) . . ? C66 C61 O2 117.0(7) . . ? C62 C61 O2 122.4(8) . . ? C63 C62 C61 117.7(9) . . ? C62 C63 C64 123.3(9) . . ? C63 C64 C65 118.5(9) . . ? C64 C65 C66 119.8(10) . . ? C61 C66 C65 120.1(8) . . ? C61 C66 P2 116.2(6) . . ? C65 C66 P2 123.5(7) . . ? C72 C67 C68 118.8(9) . . ? C72 C67 P2 120.5(6) . . ? C68 C67 P2 120.7(6) . . ? C69 C68 C67 120.3(9) . . ? C70 C69 C68 119.8(9) . . ? C71 C70 C69 121.6(10) . . ? C70 C71 C72 118.9(9) . . ? C67 C72 C71 120.5(8) . . ? C74 C73 C78 119.1(8) . . ? C74 C73 P2 122.3(6) . . ? C78 C73 P2 117.8(6) . . ? C75 C74 C73 121.5(9) . . ? C74 C75 C76 120.4(9) . . ? C77 C76 C75 118.8(8) . . ? C76 C77 C78 120.1(9) . . ? C73 C78 C77 120.0(8) . . ? O2 C79 C80 112.1(8) . . ? #------------------------------------------------------------------------------ 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 N3 Ru1 P1 C26 163.7(3) . . . . ? N4 Ru1 P1 C26 -117.8(3) . . . . ? N2 Ru1 P1 C26 63.1(3) . . . . ? N1 Ru1 P1 C26 15.5(18) . . . . ? O1 Ru1 P1 C26 -19.6(3) . . . . ? N3 Ru1 P1 C27 43.9(4) . . . . ? N4 Ru1 P1 C27 122.4(4) . . . . ? N2 Ru1 P1 C27 -56.7(4) . . . . ? N1 Ru1 P1 C27 -104.2(18) . . . . ? O1 Ru1 P1 C27 -139.4(4) . . . . ? N3 Ru1 P1 C33 -86.5(4) . . . . ? N4 Ru1 P1 C33 -8.0(4) . . . . ? N2 Ru1 P1 C33 172.8(4) . . . . ? N1 Ru1 P1 C33 125.3(18) . . . . ? O1 Ru1 P1 C33 90.2(4) . . . . ? N7 Ru2 P2 C66 164.1(3) . . . . ? N8 Ru2 P2 C66 -116.8(3) . . . . ? N6 Ru2 P2 C66 63.2(3) . . . . ? N5 Ru2 P2 C66 23(3) . . . . ? O2 Ru2 P2 C66 -19.8(3) . . . . ? N7 Ru2 P2 C67 43.4(4) . . . . ? N8 Ru2 P2 C67 122.5(4) . . . . ? N6 Ru2 P2 C67 -57.6(4) . . . . ? N5 Ru2 P2 C67 -98(2) . . . . ? O2 Ru2 P2 C67 -140.6(4) . . . . ? N7 Ru2 P2 C73 -86.1(4) . . . . ? N8 Ru2 P2 C73 -7.0(4) . . . . ? N6 Ru2 P2 C73 173.0(4) . . . . ? N5 Ru2 P2 C73 133(2) . . . . ? O2 Ru2 P2 C73 90.0(4) . . . . ? N3 Ru1 O1 C21 117(4) . . . . ? N4 Ru1 O1 C21 110.5(5) . . . . ? N2 Ru1 O1 C21 -76.4(5) . . . . ? N1 Ru1 O1 C21 -153.4(5) . . . . ? P1 Ru1 O1 C21 23.1(5) . . . . ? N3 Ru1 O1 C39 -63(5) . . . . ? N4 Ru1 O1 C39 -69.6(6) . . . . ? N2 Ru1 O1 C39 103.4(6) . . . . ? N1 Ru1 O1 C39 26.4(6) . . . . ? P1 Ru1 O1 C39 -157.1(6) . . . . ? N7 Ru2 O2 C61 99(4) . . . . ? N8 Ru2 O2 C61 110.5(5) . . . . ? N6 Ru2 O2 C61 -77.7(5) . . . . ? N5 Ru2 O2 C61 -154.6(5) . . . . ? P2 Ru2 O2 C61 22.5(5) . . . . ? N7 Ru2 O2 C79 -86(4) . . . . ? N8 Ru2 O2 C79 -74.9(6) . . . . ? N6 Ru2 O2 C79 97.0(6) . . . . ? N5 Ru2 O2 C79 20.1(6) . . . . ? P2 Ru2 O2 C79 -162.9(6) . . . . ? N3 Ru1 N1 C5 -94.3(6) . . . . ? N4 Ru1 N1 C5 -172.6(6) . . . . ? N2 Ru1 N1 C5 6.0(6) . . . . ? O1 Ru1 N1 C5 88.9(6) . . . . ? P1 Ru1 N1 C5 54(2) . . . . ? N3 Ru1 N1 C1 75.7(7) . . . . ? N4 Ru1 N1 C1 -2.6(7) . . . . ? N2 Ru1 N1 C1 176.0(8) . . . . ? O1 Ru1 N1 C1 -101.1(7) . . . . ? P1 Ru1 N1 C1 -135.7(16) . . . . ? N3 Ru1 N2 C10 -105.2(8) . . . . ? N4 Ru1 N2 C10 -176(2) . . . . ? N1 Ru1 N2 C10 172.5(8) . . . . ? O1 Ru1 N2 C10 75.5(8) . . . . ? P1 Ru1 N2 C10 -2.9(8) . . . . ? N3 Ru1 N2 C6 80.9(6) . . . . ? N4 Ru1 N2 C6 10(3) . . . . ? N1 Ru1 N2 C6 -1.4(6) . . . . ? O1 Ru1 N2 C6 -98.4(6) . . . . ? P1 Ru1 N2 C6 -176.8(6) . . . . ? N4 Ru1 N3 C11 176.1(8) . . . . ? N2 Ru1 N3 C11 3.1(7) . . . . ? N1 Ru1 N3 C11 79.7(7) . . . . ? O1 Ru1 N3 C11 170(4) . . . . ? P1 Ru1 N3 C11 -97.1(7) . . . . ? N4 Ru1 N3 C15 2.6(6) . . . . ? N2 Ru1 N3 C15 -170.4(6) . . . . ? N1 Ru1 N3 C15 -93.8(6) . . . . ? O1 Ru1 N3 C15 -4(5) . . . . ? P1 Ru1 N3 C15 89.4(6) . . . . ? N3 Ru1 N4 C16 -0.5(6) . . . . ? N2 Ru1 N4 C16 72(3) . . . . ? N1 Ru1 N4 C16 82.8(6) . . . . ? O1 Ru1 N4 C16 179.1(6) . . . . ? P1 Ru1 N4 C16 -101.6(6) . . . . ? N3 Ru1 N4 C20 177.6(8) . . . . ? N2 Ru1 N4 C20 -110(2) . . . . ? N1 Ru1 N4 C20 -99.1(8) . . . . ? O1 Ru1 N4 C20 -2.8(8) . . . . ? P1 Ru1 N4 C20 76.4(8) . . . . ? N7 Ru2 N5 C41 74.3(7) . . . . ? N8 Ru2 N5 C41 -4.6(8) . . . . ? N6 Ru2 N5 C41 175.1(8) . . . . ? O2 Ru2 N5 C41 -101.9(7) . . . . ? P2 Ru2 N5 C41 -144(2) . . . . ? N7 Ru2 N5 C45 -92.9(6) . . . . ? N8 Ru2 N5 C45 -171.8(6) . . . . ? N6 Ru2 N5 C45 7.8(6) . . . . ? O2 Ru2 N5 C45 90.9(6) . . . . ? P2 Ru2 N5 C45 49(3) . . . . ? N7 Ru2 N6 C50 -105.5(8) . . . . ? N8 Ru2 N6 C50 175.6(17) . . . . ? N5 Ru2 N6 C50 173.0(8) . . . . ? O2 Ru2 N6 C50 74.3(8) . . . . ? P2 Ru2 N6 C50 -4.1(8) . . . . ? N7 Ru2 N6 C46 78.4(6) . . . . ? N8 Ru2 N6 C46 0(2) . . . . ? N5 Ru2 N6 C46 -3.1(6) . . . . ? O2 Ru2 N6 C46 -101.9(6) . . . . ? P2 Ru2 N6 C46 179.7(6) . . . . ? N8 Ru2 N7 C51 175.8(8) . . . . ? N6 Ru2 N7 C51 4.1(8) . . . . ? N5 Ru2 N7 C51 80.5(7) . . . . ? O2 Ru2 N7 C51 -173(3) . . . . ? P2 Ru2 N7 C51 -96.7(7) . . . . ? N8 Ru2 N7 C55 0.6(6) . . . . ? N6 Ru2 N7 C55 -171.1(6) . . . . ? N5 Ru2 N7 C55 -94.7(6) . . . . ? O2 Ru2 N7 C55 12(4) . . . . ? P2 Ru2 N7 C55 88.1(6) . . . . ? N7 Ru2 N8 C60 177.9(9) . . . . ? N6 Ru2 N8 C60 -101.8(19) . . . . ? N5 Ru2 N8 C60 -99.3(8) . . . . ? O2 Ru2 N8 C60 -1.3(8) . . . . ? P2 Ru2 N8 C60 77.9(8) . . . . ? N7 Ru2 N8 C56 2.2(6) . . . . ? N6 Ru2 N8 C56 82(2) . . . . ? N5 Ru2 N8 C56 85.0(6) . . . . ? O2 Ru2 N8 C56 -177.0(6) . . . . ? P2 Ru2 N8 C56 -97.8(6) . . . . ? C5 N1 C1 C2 -1.1(14) . . . . ? Ru1 N1 C1 C2 -171.0(7) . . . . ? N1 C1 C2 C3 0.5(15) . . . . ? C1 C2 C3 C4 -0.3(16) . . . . ? C2 C3 C4 C5 0.8(18) . . . . ? C1 N1 C5 C4 1.6(14) . . . . ? Ru1 N1 C5 C4 172.4(8) . . . . ? C1 N1 C5 C6 -179.8(8) . . . . ? Ru1 N1 C5 C6 -9.0(10) . . . . ? C3 C4 C5 N1 -1.5(16) . . . . ? C3 C4 C5 C6 -180.0(10) . . . . ? C10 N2 C6 C7 2.6(13) . . . . ? Ru1 N2 C6 C7 177.3(7) . . . . ? C10 N2 C6 C5 -177.4(8) . . . . ? Ru1 N2 C6 C5 -2.8(10) . . . . ? N1 C5 C6 N2 7.8(12) . . . . ? C4 C5 C6 N2 -173.6(9) . . . . ? N1 C5 C6 C7 -172.2(8) . . . . ? C4 C5 C6 C7 6.4(15) . . . . ? N2 C6 C7 C8 -3.2(14) . . . . ? C5 C6 C7 C8 176.8(10) . . . . ? C6 C7 C8 C9 1.3(16) . . . . ? C7 C8 C9 C10 0.9(15) . . . . ? C6 N2 C10 C9 -0.2(14) . . . . ? Ru1 N2 C10 C9 -174.0(7) . . . . ? C8 C9 C10 N2 -1.6(15) . . . . ? C15 N3 C11 C12 0.0(13) . . . . ? Ru1 N3 C11 C12 -173.4(7) . . . . ? N3 C11 C12 C13 -1.1(14) . . . . ? C11 C12 C13 C14 0.7(14) . . . . ? C12 C13 C14 C15 0.7(14) . . . . ? C11 N3 C15 C14 1.4(12) . . . . ? Ru1 N3 C15 C14 175.5(7) . . . . ? C11 N3 C15 C16 -178.2(8) . . . . ? Ru1 N3 C15 C16 -4.1(9) . . . . ? C13 C14 C15 N3 -1.8(13) . . . . ? C13 C14 C15 C16 177.8(8) . . . . ? C20 N4 C16 C17 -0.6(13) . . . . ? Ru1 N4 C16 C17 177.6(7) . . . . ? C20 N4 C16 C15 -179.7(8) . . . . ? Ru1 N4 C16 C15 -1.5(10) . . . . ? N3 C15 C16 N4 3.7(11) . . . . ? C14 C15 C16 N4 -175.9(8) . . . . ? N3 C15 C16 C17 -175.4(8) . . . . ? C14 C15 C16 C17 5.0(14) . . . . ? N4 C16 C17 C18 -0.3(14) . . . . ? C15 C16 C17 C18 178.7(9) . . . . ? C16 C17 C18 C19 2.2(15) . . . . ? C17 C18 C19 C20 -3.0(15) . . . . ? C16 N4 C20 C19 -0.2(14) . . . . ? Ru1 N4 C20 C19 -178.2(6) . . . . ? C18 C19 C20 N4 2.0(14) . . . . ? C39 O1 C21 C26 163.5(7) . . . . ? Ru1 O1 C21 C26 -16.7(9) . . . . ? C39 O1 C21 C22 -14.7(11) . . . . ? Ru1 O1 C21 C22 165.1(6) . . . . ? C26 C21 C22 C23 2.8(13) . . . . ? O1 C21 C22 C23 -179.1(8) . . . . ? C21 C22 C23 C24 -0.2(15) . . . . ? C22 C23 C24 C25 -1.2(15) . . . . ? C23 C24 C25 C26 0.1(14) . . . . ? C24 C25 C26 C21 2.3(13) . . . . ? C24 C25 C26 P1 -175.5(7) . . . . ? C22 C21 C26 C25 -3.8(12) . . . . ? O1 C21 C26 C25 178.0(7) . . . . ? C22 C21 C26 P1 174.2(7) . . . . ? O1 C21 C26 P1 -4.0(10) . . . . ? C27 P1 C26 C25 -30.3(8) . . . . ? C33 P1 C26 C25 78.0(8) . . . . ? Ru1 P1 C26 C25 -162.3(7) . . . . ? C27 P1 C26 C21 151.8(6) . . . . ? C33 P1 C26 C21 -99.8(7) . . . . ? Ru1 P1 C26 C21 19.9(7) . . . . ? C26 P1 C27 C28 -108.7(7) . . . . ? C33 P1 C27 C28 143.9(7) . . . . ? Ru1 P1 C27 C28 8.9(8) . . . . ? C26 P1 C27 C32 70.6(7) . . . . ? C33 P1 C27 C32 -36.8(7) . . . . ? Ru1 P1 C27 C32 -171.9(5) . . . . ? C32 C27 C28 C29 0.1(12) . . . . ? P1 C27 C28 C29 179.3(6) . . . . ? C27 C28 C29 C30 -1.7(13) . . . . ? C28 C29 C30 C31 0.7(13) . . . . ? C29 C30 C31 C32 1.9(13) . . . . ? C30 C31 C32 C27 -3.4(12) . . . . ? C28 C27 C32 C31 2.3(12) . . . . ? P1 C27 C32 C31 -176.9(6) . . . . ? C26 P1 C33 C38 15.5(9) . . . . ? C27 P1 C33 C38 126.1(8) . . . . ? Ru1 P1 C33 C38 -93.9(8) . . . . ? C26 P1 C33 C34 -173.4(7) . . . . ? C27 P1 C33 C34 -62.8(8) . . . . ? Ru1 P1 C33 C34 77.2(8) . . . . ? C38 C33 C34 C35 -1.0(14) . . . . ? P1 C33 C34 C35 -172.5(7) . . . . ? C33 C34 C35 C36 2.8(15) . . . . ? C34 C35 C36 C37 -3.7(15) . . . . ? C35 C36 C37 C38 2.8(15) . . . . ? C36 C37 C38 C33 -1.0(14) . . . . ? C34 C33 C38 C37 0.1(14) . . . . ? P1 C33 C38 C37 171.2(7) . . . . ? C21 O1 C39 C40 85.9(10) . . . . ? Ru1 O1 C39 C40 -93.9(8) . . . . ? C45 N5 C41 C42 -0.8(14) . . . . ? Ru2 N5 C41 C42 -167.8(7) . . . . ? N5 C41 C42 C43 -2.5(15) . . . . ? C41 C42 C43 C44 2.8(16) . . . . ? C42 C43 C44 C45 0.1(17) . . . . ? C41 N5 C45 C44 3.8(14) . . . . ? Ru2 N5 C45 C44 172.2(8) . . . . ? C41 N5 C45 C46 -179.4(8) . . . . ? Ru2 N5 C45 C46 -11.0(10) . . . . ? C43 C44 C45 N5 -3.5(16) . . . . ? C43 C44 C45 C46 -180.0(10) . . . . ? C50 N6 C46 C47 2.5(13) . . . . ? Ru2 N6 C46 C47 179.1(7) . . . . ? C50 N6 C46 C45 -178.3(8) . . . . ? Ru2 N6 C46 C45 -1.7(10) . . . . ? N5 C45 C46 C47 -172.4(8) . . . . ? C44 C45 C46 C47 4.3(16) . . . . ? N5 C45 C46 N6 8.4(12) . . . . ? C44 C45 C46 N6 -174.9(9) . . . . ? N6 C46 C47 C48 -2.0(15) . . . . ? C45 C46 C47 C48 178.8(10) . . . . ? C46 C47 C48 C49 1.0(16) . . . . ? C47 C48 C49 C50 -0.7(15) . . . . ? C46 N6 C50 C49 -2.3(14) . . . . ? Ru2 N6 C50 C49 -178.3(7) . . . . ? C48 C49 C50 N6 1.4(16) . . . . ? C55 N7 C51 C52 -1.3(13) . . . . ? Ru2 N7 C51 C52 -176.4(7) . . . . ? N7 C51 C52 C53 0.9(14) . . . . ? C51 C52 C53 C54 0.7(13) . . . . ? C52 C53 C54 C55 -1.9(14) . . . . ? C53 C54 C55 N7 1.6(14) . . . . ? C53 C54 C55 C56 -179.8(9) . . . . ? C51 N7 C55 C54 0.0(12) . . . . ? Ru2 N7 C55 C54 175.6(7) . . . . ? C51 N7 C55 C56 -178.7(8) . . . . ? Ru2 N7 C55 C56 -3.1(9) . . . . ? C60 N8 C56 C57 0.8(13) . . . . ? Ru2 N8 C56 C57 176.9(6) . . . . ? C60 N8 C56 C55 179.4(8) . . . . ? Ru2 N8 C56 C55 -4.5(9) . . . . ? C54 C55 C56 N8 -173.7(8) . . . . ? N7 C55 C56 N8 5.0(11) . . . . ? C54 C55 C56 C57 5.0(14) . . . . ? N7 C55 C56 C57 -176.4(8) . . . . ? N8 C56 C57 C58 -2.1(13) . . . . ? C55 C56 C57 C58 179.3(9) . . . . ? C56 C57 C58 C59 3.0(14) . . . . ? C57 C58 C59 C60 -2.7(14) . . . . ? C56 N8 C60 C59 -0.4(14) . . . . ? Ru2 N8 C60 C59 -176.0(7) . . . . ? C58 C59 C60 N8 1.4(15) . . . . ? C79 O2 C61 C66 169.8(7) . . . . ? Ru2 O2 C61 C66 -15.3(9) . . . . ? C79 O2 C61 C62 -6.3(11) . . . . ? Ru2 O2 C61 C62 168.6(6) . . . . ? C66 C61 C62 C63 4.5(13) . . . . ? O2 C61 C62 C63 -179.6(8) . . . . ? C61 C62 C63 C64 -2.0(15) . . . . ? C62 C63 C64 C65 -0.8(15) . . . . ? C63 C64 C65 C66 1.2(14) . . . . ? C62 C61 C66 C65 -4.2(13) . . . . ? O2 C61 C66 C65 179.7(7) . . . . ? C62 C61 C66 P2 170.9(7) . . . . ? O2 C61 C66 P2 -5.2(10) . . . . ? C64 C65 C66 C61 1.3(13) . . . . ? C64 C65 C66 P2 -173.5(7) . . . . ? C67 P2 C66 C61 153.2(6) . . . . ? C73 P2 C66 C61 -99.2(7) . . . . ? Ru2 P2 C66 C61 20.7(7) . . . . ? C67 P2 C66 C65 -31.8(8) . . . . ? C73 P2 C66 C65 75.7(8) . . . . ? Ru2 P2 C66 C65 -164.3(7) . . . . ? C66 P2 C67 C72 74.2(7) . . . . ? C73 P2 C67 C72 -32.6(7) . . . . ? Ru2 P2 C67 C72 -167.0(5) . . . . ? C66 P2 C67 C68 -106.0(7) . . . . ? C73 P2 C67 C68 147.3(7) . . . . ? Ru2 P2 C67 C68 12.8(8) . . . . ? C72 C67 C68 C69 -1.3(12) . . . . ? P2 C67 C68 C69 178.8(6) . . . . ? C67 C68 C69 C70 1.5(12) . . . . ? C68 C69 C70 C71 -1.3(13) . . . . ? C69 C70 C71 C72 0.8(13) . . . . ? C68 C67 C72 C71 0.8(12) . . . . ? P2 C67 C72 C71 -179.3(6) . . . . ? C70 C71 C72 C67 -0.6(12) . . . . ? C66 P2 C73 C74 17.7(8) . . . . ? C67 P2 C73 C74 128.2(8) . . . . ? Ru2 P2 C73 C74 -92.4(7) . . . . ? C66 P2 C73 C78 -173.0(7) . . . . ? C67 P2 C73 C78 -62.5(8) . . . . ? Ru2 P2 C73 C78 76.9(7) . . . . ? C78 C73 C74 C75 1.7(14) . . . . ? P2 C73 C74 C75 170.9(7) . . . . ? C73 C74 C75 C76 -2.6(15) . . . . ? C74 C75 C76 C77 2.1(15) . . . . ? C75 C76 C77 C78 -0.7(15) . . . . ? C74 C73 C78 C77 -0.4(13) . . . . ? P2 C73 C78 C77 -170.1(7) . . . . ? C76 C77 C78 C73 -0.1(14) . . . . ? C61 O2 C79 C80 81.9(10) . . . . ? Ru2 O2 C79 C80 -92.7(8) . . . . ? #------------------------------------------------------------------------------