# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Joydev Dinda' _publ_contact_author_email joydevdinda@gmail.com _publ_section_title ; Synthesis, Structure, Electrochemical Behaviours of Ru(II) and Pt(II)-carbene complexes of NCN-Pincer 1,3-bis(2-pyridylmethyl)-1H Benzimidazolium Chloride ; loop_ _publ_author_name 'Joydev Dinda' 'Sirshendu Dasadhikari' 'Gourisankar Roymahapatra' 'Tapastaru Samanta' 'Frederique Loiseau' ; D.Jouvenot ; 'Santanab Giri' 'P. Chattaraj' # Attachment '- NJ-ART-11-2009-000698.cif' data_Monoclinic_? _database_code_depnum_ccdc_archive 'CCDC 771107' #TrackingRef '- NJ-ART-11-2009-000698.cif' #------------------------------------------------------------------------------ _audit_creation_date 2009-04-09 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; #------------------------------------------------------------------------------ _computing_data_collection 'Enraf-Nonius kappa ccd' _computing_cell_refinement 'Enraf-Nonius kappa ccd' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution 'SIR 92' _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 11.910(1) _cell_length_b 19.351(2) _cell_length_c 21.617(3) _cell_angle_alpha 90 _cell_angle_beta 90.20(1) _cell_angle_gamma 90 _cell_volume 4981.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200.0 _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/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1094.35 _chemical_formula_analytical ? _chemical_formula_sum 'C43 H39.50 F12 N10.50 P2 Ru ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2212.00 _exptl_absorpt_coefficient_mu 0.466 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 200.0 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Bruker Enraf Nonius kappa CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method 'phi and omega scans' _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 28016 _reflns_number_total 7661 _reflns_number_gt 5038 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.12831 _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 -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 10.00 _diffrn_reflns_theta_max 25.00 _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 0 172 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 158 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 42 0.004 0.003 ;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) ; P 0 8 0.090 0.095 ;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) ; #------------------------------------------------------------------------------ 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) 0.75072(3) 0.73933(2) 0.95070(2) 0.02485(9) 1.000 . Uani d ? P(1) 0.8073(1) 0.98137(7) 0.67279(8) 0.0384(4) 1.000 . Uani d ? P(2) 1.3154(1) 0.92931(9) 0.67079(8) 0.0469(4) 1.000 . Uani d ? F(1) 0.8191(5) 1.0623(2) 0.6705(2) 0.087(2) 1.000 . Uani d ? F(2) 0.7982(4) 0.8996(2) 0.6740(2) 0.076(1) 1.000 . Uani d ? F(3) 0.9386(3) 0.9749(2) 0.6638(2) 0.069(1) 1.000 . Uani d ? F(4) 0.6766(3) 0.9877(3) 0.6803(2) 0.088(1) 1.000 . Uani d ? F(5) 0.7920(3) 0.9792(2) 0.5997(2) 0.053(1) 1.000 . Uani d ? F(6) 0.8235(3) 0.9825(2) 0.7455(2) 0.064(1) 1.000 . Uani d ? F(7) 1.3225(4) 0.9729(2) 0.6089(2) 0.093(1) 1.000 . Uani d ? F(8) 1.3064(4) 0.8850(3) 0.7312(2) 0.081(1) 1.000 . Uani d ? F(9) 1.3529(7) 0.8636(3) 0.6332(3) 0.140(2) 1.000 . Uani d ? F(10) 1.2829(8) 0.9939(3) 0.7073(3) 0.134(2) 1.000 . Uani d ? F(11) 1.4440(4) 0.9375(4) 0.6807(4) 0.144(2) 1.000 . Uani d ? F(12) 1.1897(4) 0.9172(4) 0.6586(3) 0.126(2) 1.000 . Uani d ? N(1) 0.6990(4) 0.8272(2) 1.0623(2) 0.029(1) 1.000 . Uani d ? N(2) 0.6391(3) 0.7237(2) 1.0755(2) 0.026(1) 1.000 . Uani d ? N(3) 0.8753(3) 0.8144(2) 0.9662(2) 0.024(1) 1.000 . Uani d ? N(4) 0.6215(3) 0.6656(2) 0.9482(2) 0.025(1) 1.000 . Uani d ? N(5) 0.8179(3) 0.7563(2) 0.8164(2) 0.026(1) 1.000 . Uani d ? N(6) 0.8567(3) 0.6543(2) 0.8487(2) 0.026(1) 1.000 . Uani d ? N(7) 0.6432(3) 0.8081(2) 0.9040(2) 0.027(1) 1.000 . Uani d ? N(8) 0.8693(3) 0.6679(2) 0.9865(2) 0.025(1) 1.000 . Uani d ? N(9) 0.2142(6) 0.9683(3) 0.8757(3) 0.065(2) 1.000 . Uani d ? N(10) 0.802(1) 0.9920(5) 0.8973(5) 0.061(3) 0.500 . Uani d ? N(11) 0.812(3) 0.2473(8) 0.650(1) 0.159(8) 0.500 . Uani d ? N(12) 0.649(1) 0.176(1) 0.9542(8) 0.118(6) 0.500 . Uani d ? C(1) 0.6902(4) 0.7643(3) 1.0350(2) 0.028(1) 1.000 . Uani d ? C(2) 0.8115(4) 0.7145(3) 0.8662(2) 0.027(1) 1.000 . Uani d ? C(3) 0.6549(4) 0.8259(3) 1.1218(2) 0.030(1) 1.000 . Uani d ? C(4) 0.6463(5) 0.8751(3) 1.1683(3) 0.038(1) 1.000 . Uani d ? C(5) 0.5961(5) 0.8551(3) 1.2224(3) 0.041(2) 1.000 . Uani d ? C(6) 0.5565(5) 0.7877(3) 1.2303(3) 0.041(2) 1.000 . Uani d ? C(7) 0.5647(5) 0.7386(3) 1.1852(2) 0.037(1) 1.000 . Uani d ? C(8) 0.6148(4) 0.7586(3) 1.1307(2) 0.030(1) 1.000 . Uani d ? C(9) 0.7487(4) 0.8860(3) 1.0303(3) 0.034(1) 1.000 . Uani d ? C(10) 0.8631(5) 0.8700(2) 1.0058(2) 0.031(1) 1.000 . Uani d ? C(11) 0.9526(5) 0.9108(3) 1.0217(3) 0.040(2) 1.000 . Uani d ? C(12) 1.0580(5) 0.8992(3) 0.9985(3) 0.043(2) 1.000 . Uani d ? C(13) 1.0705(5) 0.8441(3) 0.9594(3) 0.040(2) 1.000 . Uani d ? C(14) 0.9804(4) 0.8043(3) 0.9447(3) 0.034(1) 1.000 . Uani d ? C(15) 0.6233(4) 0.6492(3) 1.0623(3) 0.033(1) 1.000 . Uani d ? C(16) 0.5749(4) 0.6372(3) 0.9992(2) 0.030(1) 1.000 . Uani d ? C(17) 0.4844(5) 0.5917(3) 0.9948(3) 0.043(2) 1.000 . Uani d ? C(18) 0.4390(6) 0.5756(4) 0.9390(3) 0.055(2) 1.000 . Uani d ? C(19) 0.4843(5) 0.6057(3) 0.8864(3) 0.048(2) 1.000 . Uani d ? C(20) 0.5733(5) 0.6497(3) 0.8938(2) 0.033(1) 1.000 . Uani d ? C(21) 0.8688(4) 0.7227(2) 0.7669(2) 0.027(1) 1.000 . Uani d ? C(22) 0.8945(5) 0.7422(3) 0.7069(3) 0.037(1) 1.000 . Uani d ? C(23) 0.9475(5) 0.6947(3) 0.6700(3) 0.043(2) 1.000 . Uani d ? C(24) 0.9719(5) 0.6278(3) 0.6911(3) 0.044(2) 1.000 . Uani d ? C(25) 0.9453(5) 0.6082(3) 0.7507(3) 0.035(1) 1.000 . Uani d ? C(26) 0.8927(4) 0.6563(3) 0.7880(2) 0.029(1) 1.000 . Uani d ? C(27) 0.7814(5) 0.8285(2) 0.8201(3) 0.033(1) 1.000 . Uani d ? C(28) 0.6658(4) 0.8368(2) 0.8480(2) 0.030(1) 1.000 . Uani d ? C(29) 0.5893(5) 0.8771(3) 0.8162(3) 0.036(1) 1.000 . Uani d ? C(30) 0.4834(5) 0.8886(3) 0.8417(3) 0.049(2) 1.000 . Uani d ? C(31) 0.4606(5) 0.8594(3) 0.8976(3) 0.045(2) 1.000 . Uani d ? C(32) 0.5385(5) 0.8196(3) 0.9260(3) 0.038(1) 1.000 . Uani d ? C(33) 0.8640(5) 0.5962(3) 0.8923(2) 0.034(1) 1.000 . Uani d ? C(34) 0.9167(5) 0.6163(3) 0.9528(3) 0.034(1) 1.000 . Uani d ? C(35) 1.0103(5) 0.5823(3) 0.9734(3) 0.039(2) 1.000 . Uani d ? C(36) 1.0560(5) 0.5955(3) 1.0304(3) 0.047(2) 1.000 . Uani d ? C(37) 1.0044(5) 0.6450(3) 1.0669(3) 0.040(2) 1.000 . Uani d ? C(38) 0.9149(4) 0.6791(3) 1.0426(3) 0.031(1) 1.000 . Uani d ? C(39) 0.1497(5) 0.9466(3) 0.8418(3) 0.045(2) 1.000 . Uani d ? C(40) 0.0703(6) 0.9175(4) 0.8010(4) 0.068(2) 1.000 . Uani d ? C(41) 0.738(1) 1.0186(6) 0.8735(6) 0.044(3) 0.500 . Uani d ? C(42) 0.647(1) 1.0531(7) 0.8395(9) 0.076(5) 0.500 . Uani d ? C(43) 0.789(1) 0.2308(6) 0.6952(8) 0.057(4) 0.500 . Uani d ? C(44) 0.762(1) 0.2083(8) 0.7532(8) 0.064(4) 0.500 . Uani d ? C(45) 0.687(1) 0.2260(8) 0.9560(8) 0.066(4) 0.500 . Uani d ? C(46) 0.727(2) 0.279(1) 0.989(1) 0.101(6) 0.500 . Uani d ? H(1) 0.6741 0.9207 1.1629 0.046 1.000 . Uiso c ? H(2) 0.5880 0.8875 1.2551 0.050 1.000 . Uiso c ? H(3) 0.5226 0.7756 1.2685 0.050 1.000 . Uiso c ? H(4) 0.5373 0.6930 1.1911 0.045 1.000 . Uiso c ? H(5) 0.7013 0.8986 0.9968 0.040 1.000 . Uiso c ? H(6) 0.7544 0.9236 1.0584 0.040 1.000 . Uiso c ? H(7) 0.9414 0.9481 1.0496 0.048 1.000 . Uiso c ? H(8) 1.1196 0.9282 1.0091 0.052 1.000 . Uiso c ? H(9) 1.1421 0.8337 0.9426 0.048 1.000 . Uiso c ? H(10) 0.9921 0.7666 0.9172 0.040 1.000 . Uiso c ? H(11) 0.6940 0.6267 1.0650 0.039 1.000 . Uiso c ? H(12) 0.5738 0.6303 1.0922 0.039 1.000 . Uiso c ? H(13) 0.4542 0.5718 1.0313 0.052 1.000 . Uiso c ? H(14) 0.3776 0.5444 0.9360 0.066 1.000 . Uiso c ? H(15) 0.4545 0.5961 0.8465 0.058 1.000 . Uiso c ? H(16) 0.6033 0.6705 0.8577 0.040 1.000 . Uiso c ? H(17) 0.8761 0.7869 0.6919 0.045 1.000 . Uiso c ? H(18) 0.9682 0.7074 0.6292 0.051 1.000 . Uiso c ? H(19) 1.0070 0.5957 0.6642 0.053 1.000 . Uiso c ? H(20) 0.9625 0.5632 0.7656 0.042 1.000 . Uiso c ? H(21) 0.7804 0.8473 0.7796 0.039 1.000 . Uiso c ? H(22) 0.8338 0.8532 0.8449 0.039 1.000 . Uiso c ? H(23) 0.6085 0.8967 0.7774 0.044 1.000 . Uiso c ? H(24) 0.4290 0.9159 0.8208 0.059 1.000 . Uiso c ? H(25) 0.3899 0.8669 0.9166 0.054 1.000 . Uiso c ? H(26) 0.5185 0.7983 0.9639 0.046 1.000 . Uiso c ? H(27) 0.9078 0.5607 0.8741 0.040 1.000 . Uiso c ? H(28) 0.7904 0.5795 0.9000 0.040 1.000 . Uiso c ? H(29) 1.0445 0.5487 0.9476 0.047 1.000 . Uiso c ? H(30) 1.1208 0.5715 1.0445 0.056 1.000 . Uiso c ? H(31) 1.0307 0.6547 1.1075 0.048 1.000 . Uiso c ? H(32) 0.8815 0.7139 1.0675 0.037 1.000 . Uiso c ? H(33) 0.0628 0.8695 0.8095 0.082 1.000 . Uiso c ? H(34) -0.0002 0.9396 0.8065 0.082 1.000 . Uiso c ? H(35) 0.0946 0.9236 0.7596 0.082 1.000 . Uiso c ? H(36) 0.6479 1.1012 0.8485 0.091 0.500 . Uiso d ? H(37) 0.5769 1.0341 0.8516 0.091 0.500 . Uiso d ? H(38) 0.6571 1.0465 0.7963 0.091 0.500 . Uiso d ? H(39) 0.8011 0.2353 0.7831 0.077 0.500 . Uiso d ? H(40) 0.6837 0.2127 0.7593 0.077 0.500 . Uiso d ? H(41) 0.7834 0.1612 0.7576 0.077 0.500 . Uiso d ? H(42) 0.8029 0.2869 0.9782 0.122 0.500 . Uiso d ? H(43) 0.7218 0.2687 1.0317 0.122 0.500 . Uiso d ? H(44) 0.6838 0.3193 0.9801 0.122 0.500 . Uiso d ? 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) 0.0288(2) 0.0231(2) 0.0226(2) -0.0025(2) -0.0014(2) 0.0010(2) P(1) 0.0357(7) 0.0355(7) 0.0439(9) 0.0013(6) -0.0080(7) 0.0044(7) P(2) 0.0403(8) 0.0519(9) 0.049(1) 0.0083(7) -0.0021(8) 0.0027(8) F(1) 0.140(4) 0.036(2) 0.086(3) -0.005(2) -0.014(3) -0.007(2) F(2) 0.107(3) 0.044(2) 0.075(3) -0.018(2) -0.029(2) 0.024(2) F(3) 0.040(2) 0.104(3) 0.062(2) -0.003(2) -0.009(2) -0.013(2) F(4) 0.038(2) 0.146(4) 0.080(3) 0.014(2) 0.003(2) 0.018(3) F(5) 0.057(2) 0.053(2) 0.048(2) -0.013(2) -0.017(2) 0.006(2) F(6) 0.062(2) 0.085(3) 0.044(2) 0.007(2) -0.008(2) -0.005(2) F(7) 0.100(3) 0.095(3) 0.084(3) 0.054(2) 0.040(2) 0.042(2) F(8) 0.078(3) 0.100(3) 0.063(3) -0.004(2) -0.017(2) 0.032(2) F(9) 0.230(7) 0.082(3) 0.109(4) 0.060(4) 0.045(4) 0.012(3) F(10) 0.226(7) 0.090(3) 0.086(4) 0.023(4) 0.024(4) -0.035(3) F(11) 0.047(3) 0.210(6) 0.175(6) -0.010(3) -0.010(3) 0.059(6) F(12) 0.057(2) 0.240(7) 0.082(3) -0.036(3) -0.031(2) 0.036(4) N(1) 0.036(2) 0.027(2) 0.023(2) -0.002(2) 0.005(2) 0.000(2) N(2) 0.027(2) 0.027(2) 0.024(2) -0.007(2) -0.003(2) 0.000(2) N(3) 0.022(2) 0.030(2) 0.020(2) -0.004(2) -0.005(2) 0.001(2) N(4) 0.021(2) 0.031(2) 0.023(2) -0.006(2) -0.008(2) -0.002(2) N(5) 0.033(2) 0.028(2) 0.018(2) 0.004(2) 0.001(2) 0.006(2) N(6) 0.037(2) 0.020(2) 0.023(2) -0.003(2) 0.000(2) 0.000(2) N(7) 0.028(2) 0.026(2) 0.028(2) -0.001(2) -0.008(2) 0.003(2) N(8) 0.028(2) 0.025(2) 0.022(2) -0.002(2) -0.005(2) 0.001(2) N(9) 0.081(4) 0.049(3) 0.066(4) -0.004(3) 0.020(3) -0.007(3) N(10) 0.104(8) 0.041(5) 0.038(6) -0.002(6) -0.043(6) -0.013(5) N(11) 0.30(3) 0.048(8) 0.13(1) -0.01(1) 0.10(2) 0.010(9) N(12) 0.11(1) 0.17(2) 0.08(1) -0.03(1) 0.054(9) -0.02(1) C(1) 0.027(2) 0.029(2) 0.028(3) 0.005(2) -0.003(2) -0.004(2) C(2) 0.029(2) 0.030(2) 0.022(3) 0.001(2) -0.003(2) 0.000(2) C(3) 0.029(3) 0.031(3) 0.029(3) -0.002(2) 0.001(2) -0.005(2) C(4) 0.042(3) 0.041(3) 0.031(3) -0.007(2) -0.001(3) -0.013(3) C(5) 0.050(3) 0.046(3) 0.029(3) 0.005(3) 0.008(3) -0.007(3) C(6) 0.046(3) 0.058(3) 0.020(3) -0.006(3) -0.002(3) 0.001(3) C(7) 0.046(3) 0.039(3) 0.026(3) -0.008(3) 0.003(2) -0.002(3) C(8) 0.029(2) 0.033(3) 0.027(3) -0.005(2) -0.008(2) 0.000(2) C(9) 0.037(3) 0.025(2) 0.039(3) -0.005(2) 0.007(3) 0.001(2) C(10) 0.042(3) 0.023(2) 0.028(3) -0.006(2) -0.005(2) 0.004(2) C(11) 0.048(3) 0.028(3) 0.043(3) -0.016(2) -0.004(3) -0.004(3) C(12) 0.041(3) 0.043(3) 0.045(3) -0.015(3) -0.010(3) 0.008(3) C(13) 0.036(3) 0.043(3) 0.041(3) -0.007(3) 0.001(3) 0.003(3) C(14) 0.037(3) 0.026(3) 0.038(3) -0.005(2) -0.006(3) 0.001(2) C(15) 0.042(3) 0.026(3) 0.030(3) -0.006(2) 0.000(3) 0.005(2) C(16) 0.032(3) 0.031(3) 0.027(3) -0.003(2) -0.001(2) -0.006(2) C(17) 0.051(3) 0.047(3) 0.031(3) -0.024(3) 0.000(3) 0.003(3) C(18) 0.059(4) 0.063(4) 0.042(4) -0.030(3) 0.003(3) -0.008(3) C(19) 0.052(3) 0.054(3) 0.038(3) -0.020(3) -0.004(3) -0.008(3) C(20) 0.040(3) 0.037(3) 0.023(3) -0.004(2) -0.003(2) 0.004(2) C(21) 0.026(2) 0.033(3) 0.022(3) 0.003(2) 0.000(2) 0.005(2) C(22) 0.042(3) 0.038(3) 0.032(3) 0.009(2) 0.005(2) 0.003(3) C(23) 0.047(3) 0.061(4) 0.020(3) 0.016(3) -0.003(3) 0.003(3) C(24) 0.053(3) 0.048(3) 0.032(3) 0.019(3) 0.005(3) -0.003(3) C(25) 0.041(3) 0.031(3) 0.033(3) 0.005(2) -0.004(3) 0.004(2) C(26) 0.031(3) 0.030(3) 0.026(3) 0.002(2) -0.005(2) -0.002(2) C(27) 0.045(3) 0.023(2) 0.029(3) 0.003(2) 0.003(3) 0.001(2) C(28) 0.035(3) 0.025(2) 0.029(3) -0.002(2) 0.000(2) -0.005(2) C(29) 0.044(3) 0.037(3) 0.029(3) 0.009(2) -0.006(3) -0.001(3) C(30) 0.035(3) 0.058(4) 0.055(4) 0.007(3) -0.006(3) 0.004(3) C(31) 0.032(3) 0.059(4) 0.044(4) 0.010(3) 0.002(3) 0.001(3) C(32) 0.032(3) 0.040(3) 0.043(3) -0.001(2) 0.002(3) 0.003(3) C(33) 0.050(3) 0.027(2) 0.024(3) 0.000(2) 0.000(3) 0.005(2) C(34) 0.048(3) 0.025(2) 0.029(3) -0.006(2) 0.002(3) 0.009(2) C(35) 0.046(3) 0.031(3) 0.041(3) 0.012(2) -0.001(3) 0.004(3) C(36) 0.056(3) 0.050(3) 0.034(3) 0.014(3) -0.015(3) 0.006(3) C(37) 0.045(3) 0.042(3) 0.032(3) 0.001(3) -0.015(3) 0.002(3) C(38) 0.036(3) 0.027(2) 0.029(3) -0.005(2) -0.007(2) 0.003(2) C(39) 0.046(3) 0.039(3) 0.051(4) 0.005(3) 0.007(3) 0.003(3) C(40) 0.049(4) 0.082(5) 0.074(5) 0.001(4) 0.009(4) 0.021(4) C(41) 0.070(8) 0.023(5) 0.038(7) 0.000(5) -0.007(6) -0.014(5) C(42) 0.09(1) 0.043(7) 0.09(1) 0.019(7) -0.01(1) -0.028(8) C(43) 0.056(7) 0.031(6) 0.08(1) -0.008(5) 0.033(7) 0.014(7) C(44) 0.040(7) 0.070(8) 0.08(1) 0.010(6) -0.006(7) 0.014(9) C(45) 0.036(6) 0.061(9) 0.10(1) 0.009(6) -0.022(7) 0.031(8) C(46) 0.10(1) 0.08(1) 0.12(2) 0.041(9) 0.00(1) 0.04(1) #------------------------------------------------------------------------------ _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) + 0.00010|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 5038 _refine_ls_number_parameters 658 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_all 0.0659 _refine_ls_wR_factor_ref 0.0659 _refine_ls_goodness_of_fit_all 1.948 _refine_ls_goodness_of_fit_ref 1.948 _refine_ls_shift/su_max 0.0089 _refine_ls_shift/su_mean 0.0003 _refine_diff_density_min -0.54 _refine_diff_density_max 0.84 #------------------------------------------------------------------------------ _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 RU1 N3 2.102(4) . . yes RU1 N4 2.099(4) . . yes RU1 N7 2.103(4) . . yes RU1 N8 2.120(4) . . yes RU1 C1 2.020(5) . . yes RU1 C2 2.025(5) . . yes P1 F1 1.572(4) . . yes P1 F2 1.586(4) . . yes P1 F3 1.581(4) . . yes P1 F4 1.571(4) . . yes P1 F5 1.590(4) . . yes P1 F6 1.583(4) . . yes P2 F7 1.584(5) . . yes P2 F8 1.567(5) . . yes P2 F9 1.574(6) . . yes P2 F10 1.528(6) . . yes P2 F11 1.554(5) . . yes P2 F12 1.537(5) . . yes N1 C1 1.356(6) . . yes N1 C3 1.390(7) . . yes N1 C9 1.458(7) . . yes N2 C1 1.327(6) . . yes N2 C8 1.402(7) . . yes N2 C15 1.481(6) . . yes N3 C10 1.382(6) . . yes N3 C14 1.351(7) . . yes N4 C16 1.354(7) . . yes N4 C20 1.342(7) . . yes N5 C2 1.349(6) . . yes N5 C21 1.392(6) . . yes N5 C27 1.464(6) . . yes N6 C2 1.338(6) . . yes N6 C26 1.383(7) . . yes N6 C33 1.469(6) . . yes N7 C28 1.359(7) . . yes N7 C32 1.354(7) . . yes N8 C34 1.360(7) . . yes N8 C38 1.346(7) . . yes N9 C39 1.141(9) . . yes N10 C41 1.05(2) . . yes N11 C43 1.07(2) . . yes N12 C45 1.06(2) . . yes C3 C4 1.390(7) . . yes C3 C8 1.401(7) . . yes C4 C5 1.372(8) . . yes C4 H1 0.95 . . no C5 C6 1.396(9) . . yes C5 H2 0.95 . . no C6 C7 1.366(8) . . yes C6 H3 0.95 . . no C7 C8 1.378(7) . . yes C7 H4 0.95 . . no C9 C10 1.497(8) . . yes C9 H5 0.95 . . no C9 H6 0.95 . . no C10 C11 1.370(8) . . yes C11 C12 1.372(9) . . yes C11 H7 0.95 . . no C12 C13 1.370(8) . . yes C12 H8 0.95 . . no C13 C14 1.358(8) . . yes C13 H9 0.95 . . no C14 H10 0.95 . . no C15 C16 1.497(8) . . yes C15 H11 0.95 . . no C15 H12 0.95 . . no C16 C17 1.394(8) . . yes C17 C18 1.356(9) . . yes C17 H13 0.95 . . no C18 C19 1.390(9) . . yes C18 H14 0.95 . . no C19 C20 1.368(8) . . yes C19 H15 0.95 . . no C20 H16 0.95 . . no C21 C22 1.384(7) . . yes C21 C26 1.393(7) . . yes C22 C23 1.373(8) . . yes C22 H17 0.95 . . no C23 C24 1.402(9) . . yes C23 H18 0.95 . . no C24 C25 1.381(8) . . yes C24 H19 0.95 . . no C25 C26 1.383(7) . . yes C25 H20 0.95 . . no C27 C28 1.513(8) . . yes C27 H21 0.95 . . no C27 H22 0.95 . . no C28 C29 1.380(7) . . yes C29 C30 1.397(8) . . yes C29 H23 0.95 . . no C30 C31 1.362(9) . . yes C30 H24 0.95 . . no C31 C32 1.350(8) . . yes C31 H25 0.95 . . no C32 H26 0.95 . . no C33 C34 1.499(8) . . yes C33 H27 0.95 . . no C33 H28 0.95 . . no C34 C35 1.369(8) . . yes C35 C36 1.369(9) . . yes C35 H29 0.95 . . no C36 C37 1.385(9) . . yes C36 H30 0.95 . . no C37 C38 1.357(8) . . yes C37 H31 0.95 . . no C38 H32 0.95 . . no C39 C40 1.41(1) . . yes C40 H33 0.95 . . no C40 H34 0.95 . . no C40 H35 0.95 . . no C41 C42 1.47(2) . . yes C42 H36 0.95 . . no C42 H37 0.95 . . no C42 H38 0.95 . . no C43 C44 1.37(2) . . yes C44 H39 0.95 . . no C44 H40 0.95 . . no C44 H41 0.95 . . no C45 C46 1.34(3) . . yes C46 H42 0.95 . . no C46 H43 0.95 . . no C46 H44 0.95 . . 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 N3 RU1 N4 172.2(2) . . . yes N3 RU1 N7 93.9(2) . . . yes N3 RU1 N8 85.6(1) . . . yes N3 RU1 C1 86.8(2) . . . yes N3 RU1 C2 93.0(2) . . . yes N4 RU1 N7 88.4(2) . . . yes N4 RU1 N8 93.1(2) . . . yes N4 RU1 C1 85.6(2) . . . yes N4 RU1 C2 94.6(2) . . . yes N7 RU1 N8 172.5(2) . . . yes N7 RU1 C1 93.6(2) . . . yes N7 RU1 C2 86.3(2) . . . yes N8 RU1 C1 93.8(2) . . . yes N8 RU1 C2 86.3(2) . . . yes C1 RU1 C2 179.8(2) . . . yes F1 P1 F2 178.5(3) . . . yes F1 P1 F3 89.2(3) . . . yes F1 P1 F4 90.8(3) . . . yes F1 P1 F5 90.3(2) . . . yes F1 P1 F6 90.4(3) . . . yes F2 P1 F3 89.5(3) . . . yes F2 P1 F4 90.4(3) . . . yes F2 P1 F5 89.0(2) . . . yes F2 P1 F6 90.3(2) . . . yes F3 P1 F4 178.9(3) . . . yes F3 P1 F5 89.2(2) . . . yes F3 P1 F6 90.3(2) . . . yes F4 P1 F5 89.7(2) . . . yes F4 P1 F6 90.8(2) . . . yes F5 P1 F6 179.2(2) . . . yes F7 P2 F8 178.6(3) . . . yes F7 P2 F9 88.7(3) . . . yes F7 P2 F10 90.8(3) . . . yes F7 P2 F11 90.3(3) . . . yes F7 P2 F12 89.5(3) . . . yes F8 P2 F9 90.5(3) . . . yes F8 P2 F10 90.0(3) . . . yes F8 P2 F11 90.6(3) . . . yes F8 P2 F12 89.4(3) . . . yes F9 P2 F10 178.1(5) . . . yes F9 P2 F11 82.6(5) . . . yes F9 P2 F12 93.8(5) . . . yes F10 P2 F11 95.6(5) . . . yes F10 P2 F12 88.0(5) . . . yes F11 P2 F12 176.4(5) . . . yes C1 N1 C3 111.0(4) . . . yes C1 N1 C9 121.6(4) . . . yes C3 N1 C9 127.4(4) . . . yes C1 N2 C8 111.9(4) . . . yes C1 N2 C15 120.6(4) . . . yes C8 N2 C15 127.3(4) . . . yes RU1 N3 C10 124.1(3) . . . yes RU1 N3 C14 119.9(3) . . . yes C10 N3 C14 115.2(4) . . . yes RU1 N4 C16 123.9(3) . . . yes RU1 N4 C20 119.4(3) . . . yes C16 N4 C20 116.4(4) . . . yes C2 N5 C21 111.1(4) . . . yes C2 N5 C27 120.6(4) . . . yes C21 N5 C27 128.1(4) . . . yes C2 N6 C26 111.7(4) . . . yes C2 N6 C33 120.6(4) . . . yes C26 N6 C33 127.8(4) . . . yes RU1 N7 C28 124.3(3) . . . yes RU1 N7 C32 119.7(4) . . . yes C28 N7 C32 115.6(4) . . . yes RU1 N8 C34 124.1(3) . . . yes RU1 N8 C38 119.3(3) . . . yes C34 N8 C38 115.7(4) . . . yes RU1 C1 N1 125.5(4) . . . yes RU1 C1 N2 128.2(4) . . . yes N1 C1 N2 106.2(4) . . . yes RU1 C2 N5 126.8(3) . . . yes RU1 C2 N6 127.3(4) . . . yes N5 C2 N6 105.9(4) . . . yes N1 C3 C4 133.4(5) . . . yes N1 C3 C8 105.9(4) . . . yes C4 C3 C8 120.8(5) . . . yes C3 C4 C5 117.2(5) . . . yes C3 C4 H1 121.4 . . . no C5 C4 H1 121.4 . . . no C4 C5 C6 121.1(5) . . . yes C4 C5 H2 119.4 . . . no C6 C5 H2 119.4 . . . no C5 C6 C7 122.5(5) . . . yes C5 C6 H3 118.7 . . . no C6 C7 C8 116.6(5) . . . yes C6 C7 H4 121.7 . . . no C8 C7 H4 121.7 . . . no N2 C8 C3 105.0(4) . . . yes N2 C8 C7 133.1(5) . . . yes C3 C8 C7 121.8(5) . . . yes N1 C9 C10 112.2(4) . . . yes N1 C9 H5 108.8 . . . no N1 C9 H6 108.8 . . . no C10 C9 H5 108.8 . . . no C10 C9 H6 108.8 . . . no H5 C9 H6 109.5 . . . no N3 C10 C9 118.6(4) . . . yes N3 C10 C11 121.4(5) . . . yes C9 C10 C11 120.0(5) . . . yes C10 C11 C12 121.7(5) . . . yes C10 C11 H7 119.1 . . . no C12 C11 H7 119.1 . . . no C11 C12 C13 117.0(5) . . . yes C11 C12 H8 121.5 . . . no C13 C12 H8 121.5 . . . no C12 C13 C14 120.0(5) . . . yes C12 C13 H9 120.0 . . . no C14 C13 H9 120.0 . . . no N3 C14 C13 124.7(5) . . . yes N3 C14 H10 117.7 . . . no C13 C14 H10 117.7 . . . no N2 C15 C16 112.1(4) . . . yes N2 C15 H11 108.8 . . . no N2 C15 H12 108.8 . . . no C16 C15 H11 108.8 . . . no C16 C15 H12 108.8 . . . no H11 C15 H12 109.5 . . . no N4 C16 C15 121.4(4) . . . yes N4 C16 C17 121.3(5) . . . yes C15 C16 C17 117.1(5) . . . yes C16 C17 C18 120.8(5) . . . yes C16 C17 H13 119.6 . . . no C18 C17 H13 119.6 . . . no C17 C18 C19 118.4(5) . . . yes C17 C18 H14 120.8 . . . no C19 C18 H14 120.8 . . . no C18 C19 C20 118.0(6) . . . yes C18 C19 H15 121.0 . . . no C20 C19 H15 121.0 . . . no N4 C20 C19 125.0(5) . . . yes N4 C20 H16 117.5 . . . no C19 C20 H16 117.5 . . . no N5 C21 C22 133.7(4) . . . yes N5 C21 C26 105.5(4) . . . yes C22 C21 C26 120.8(5) . . . yes C21 C22 C23 117.8(5) . . . yes C21 C22 H17 121.1 . . . no C23 C22 H17 121.1 . . . no C22 C23 C24 121.6(5) . . . yes C22 C23 H18 119.2 . . . no C24 C23 H18 119.2 . . . no C23 C24 C25 120.7(5) . . . yes C23 C24 H19 119.7 . . . no C25 C24 H19 119.7 . . . no C24 C25 C26 117.6(5) . . . yes C24 C25 H20 121.2 . . . no C26 C25 H20 121.2 . . . no N6 C26 C21 105.9(4) . . . yes N6 C26 C25 132.6(5) . . . yes C21 C26 C25 121.5(5) . . . yes N5 C27 C28 113.2(4) . . . yes N5 C27 H21 108.5 . . . no N5 C27 H22 108.5 . . . no C28 C27 H21 108.5 . . . no C28 C27 H22 108.5 . . . no H21 C27 H22 109.5 . . . no N7 C28 C27 119.6(4) . . . yes N7 C28 C29 122.7(5) . . . yes C27 C28 C29 117.5(5) . . . yes C28 C29 C30 119.3(5) . . . yes C28 C29 H23 120.3 . . . no C30 C29 H23 120.3 . . . no C29 C30 C31 117.8(5) . . . yes C29 C30 H24 121.1 . . . no C31 C30 H24 121.1 . . . no C30 C31 C32 120.0(5) . . . yes C30 C31 H25 120.0 . . . no C32 C31 H25 120.0 . . . no N7 C32 C31 124.5(5) . . . yes N7 C32 H26 117.8 . . . no C31 C32 H26 117.8 . . . no N6 C33 C34 112.6(4) . . . yes N6 C33 H27 108.7 . . . no N6 C33 H28 108.7 . . . no C34 C33 H27 108.7 . . . no C34 C33 H28 108.7 . . . no H27 C33 H28 109.5 . . . no N8 C34 C33 118.9(5) . . . yes N8 C34 C35 121.2(5) . . . yes C33 C34 C35 119.8(5) . . . yes C34 C35 C36 121.6(5) . . . yes C34 C35 H29 119.2 . . . no C36 C35 H29 119.2 . . . no C35 C36 C37 117.8(5) . . . yes C35 C36 H30 121.1 . . . no C37 C36 H30 121.1 . . . no C36 C37 C38 117.8(5) . . . yes C36 C37 H31 121.1 . . . no C38 C37 H31 121.1 . . . no N8 C38 C37 125.7(5) . . . yes N8 C38 H32 117.1 . . . no C37 C38 H32 117.1 . . . no N9 C39 C40 177.9(7) . . . yes C39 C40 H33 109.5 . . . no C39 C40 H34 109.5 . . . no C39 C40 H35 109.5 . . . no H33 C40 H34 109.5 . . . no H33 C40 H35 109.5 . . . no H34 C40 H35 109.5 . . . no N10 C41 C42 178(1) . . . yes N10 C41 H36 155.7 . . . no C41 C42 H36 109.5 . . . no C41 C42 H37 109.5 . . . no C41 C42 H38 109.5 . . . no H36 C42 H37 109.5 . . . no H36 C42 H38 109.5 . . . no H37 C42 H38 109.5 . . . no N11 C43 C44 178(2) . . . yes C43 C44 H39 109.5 . . . no C43 C44 H40 109.5 . . . no C43 C44 H41 109.5 . . . no H39 C44 H40 109.5 . . . no H39 C44 H41 109.5 . . . no H40 C44 H41 109.5 . . . no N12 C45 C46 150(2) . . . yes C45 C46 H42 109.5 . . . no C45 C46 H43 109.5 . . . no C45 C46 H44 109.5 . . . no H42 C46 H43 109.5 . . . no H42 C46 H44 109.5 . . . no H43 C46 H44 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F1 C43 3.32(1) . 1_565 no F1 C25 3.395(8) . 2_756 no F1 C44 3.41(2) . 1_565 no F2 C15 3.321(7) . 4_564 no F2 C22 3.332(7) . . no F2 C27 3.453(7) . . no F2 C37 3.489(8) . 4_564 no F2 C38 3.513(7) . 4_564 no F3 F12 3.195(7) . . no F3 C37 3.225(7) . 4_564 no F3 C25 3.457(7) . 2_756 no F3 C36 3.486(7) . 4_564 no F3 C40 3.529(9) . 1_655 no F3 C33 3.540(7) . 2_756 no F4 F11 2.935(7) . 1_455 no F4 C19 3.309(8) . 2_656 no F4 C18 3.379(8) . 2_656 no F5 C15 3.295(6) . 4_564 no F5 C18 3.425(7) . 2_656 no F5 C35 3.470(7) . 2_756 no F5 C37 3.562(7) . 4_564 no F6 C41 3.03(1) . . no F6 C42 3.23(2) . . no F6 N10 3.30(1) . . no F6 C40 3.411(8) . 1_655 no F6 C27 3.427(7) . . no F7 C33 3.261(7) . 2_756 no F7 C17 3.376(7) . 4_664 no F7 C19 3.450(9) . 2_756 no F8 C30 3.181(8) . 1_655 no F8 C40 3.257(9) . 1_655 no F8 C39 3.263(8) . 1_655 no F8 C44 3.53(2) . 2_756 no F8 C43 3.57(1) . 2_756 no F9 C46 3.24(2) . 2_756 no F9 C45 3.32(2) . 2_756 no F9 C7 3.394(9) . 4_664 no F9 C17 3.491(9) . 4_664 no F9 C15 3.580(9) . 4_664 no F10 C33 3.405(9) . 2_756 no F10 C39 3.441(9) . 1_655 no F10 C40 3.57(1) . 1_655 no F10 C5 3.594(9) . 3_777 no F11 C29 3.593(9) . 1_655 no F12 C37 3.197(8) . 4_564 no F12 C36 3.200(8) . 4_564 no F12 C40 3.40(1) . 1_655 no N9 C13 3.465(8) . 1_455 no N9 C9 3.502(8) . 3_677 no N9 C12 3.512(9) . 1_455 no N9 C4 3.584(8) . 3_677 no N10 C10 3.40(1) . . no N10 C12 3.50(1) . 3_777 no N10 C28 3.57(1) . . no N10 C27 3.58(1) . . no N10 C11 3.59(1) . . no N10 C9 3.59(1) . . no N11 C13 3.32(2) . 2_746 no N11 C14 3.40(2) . 2_746 no N12 C32 3.42(2) . 3_667 no N12 C42 3.44(2) . 1_545 no N12 C31 3.53(2) . 3_667 no C13 C39 3.363(9) . 1_655 no C13 C46 3.57(2) . 3_767 no C17 C46 3.56(2) . 3_667 no C17 C17 3.58(1) . 3_667 no C29 C41 3.49(1) . . no C29 C42 3.51(1) . . no C35 C35 3.39(1) . 3_767 no C35 C36 3.530(8) . 3_767 no C36 C46 3.57(2) . 3_767 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------