Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Juliusz Wolny' _publ_contact_author_address ; Department of Chemistry University of Wroclaw Joliot-Curie 14 Wroclaw 50-383 POLAND ; _publ_contact_author_email WOLNY@PHYSIK.UNI-LUEBECK.DE _publ_section_title ; Strain-induced substitutional lability in a Ru(II) complex o hypodentate polypyridine ligand. ; _publ_requested_category FM loop_ _publ_author_name 'Juliusz Wolny' 'Bjorn Akermark' 'Anna Borje' 'Piotr Chmielewski' 'Ole Simonsen' 'Paul C. Stein' ; H.Toftlund ; data_gorila _database_code_depnum_ccdc_archive 'CCDC 206148' _audit_creation_date 2004-02-04T17:04:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ? _chemical_name_common 'Ru Gorilla' _chemical_formula_moiety 'C33 H35 F6 N7 O8 Ru S2' _chemical_formula_sum 'C33 H35 F6 N7 O8 Ru S2' _chemical_formula_weight 936.87 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall -P_2yn _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.9820(10) _cell_length_b 9.961(3) _cell_length_c 22.6050(10) _cell_angle_alpha 90 _cell_angle_beta 110.3320(10) _cell_angle_gamma 90 _cell_volume 3796.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 37.81 _cell_measurement_theta_max 41.47 _cell_measurement_wavelength 1.54178 _cell_special_details ; ? ; #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_preparation ; A solution in acetone was layered with ligroin and left for several months. ; _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 1.64 _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method ; Flotation in mixture of CCl~4~ and CH~2~BrCl. ; _exptl_crystal_F_000 1904 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.17 0 -1 0 0.17 1 0 -1 0.069 -1 0 1 0.069 1 0 2 0.08 -1 0 -2 0.08 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.169 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; a grid of 8 x 14 x 8 = 896 sampling points was used ; _exptl_absorpt_correction_T_min 0.326 _exptl_absorpt_correction_T_max 0.553 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_UB_11 0.056777 _diffrn_orient_matrix_UB_12 0.000691 _diffrn_orient_matrix_UB_13 0.028375 _diffrn_orient_matrix_UB_21 -0.016961 _diffrn_orient_matrix_UB_22 -0.001399 _diffrn_orient_matrix_UB_23 0.037678 _diffrn_orient_matrix_UB_31 0.000622 _diffrn_orient_matrix_UB_32 -0.100267 _diffrn_orient_matrix_UB_33 -0.000326 _diffrn_measurement_device ; Enraf-Nonius CAD-4F diffractometer ; _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method \w/2\Q _diffrn_standards_number 1 _diffrn_standards_interval_count 30 _diffrn_standards_interval_time 90 _diffrn_standards_decay_% 9 _diffrn_standards_decay_corr_max 1.119 _diffrn_standards_decay_corr_min 0.957 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -7 -5 -8 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_unetI/netI 0.0155 _diffrn_reflns_number 6672 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 65 _diffrn_reflns_theta_full 65 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 6450 _reflns_number_gt 5894 _reflns_threshold_expression 'I > 2.5*sigma(I)' #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Enraf-Nonius CAD-4F Software' _computing_cell_refinement 'Enraf-Nonius CAD-4F Software' _computing_data_reduction ; Norrestam & Nielsen (1982) and Xtal3.2 ADDREF SORTRF (Hall, Flack & Stewart, 1992) ; _computing_structure_solution 'SHELXS 86 (Sheldrick, 1985)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ' Xtal3.2 ORTEP' _computing_publication_material 'WinGX (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The triflate anion containing C2 and S2 is obviously disordered by rotation around the C2-S2 axis. No acceptable modelling of the disorder could be obtained so very large ADP's have been accepted. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0976P)^2^+7.5145P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6450 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1552 _refine_ls_wR_factor_gt 0.1506 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.25 _refine_diff_density_min -1.58 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.229232(17) 0.51316(3) 0.483433(13) 0.02991(14) Uani 1 1 d . . . N1 N 0.2667(2) 0.5348(4) 0.58096(16) 0.0344(8) Uani 1 1 d . . . N2 N 0.1332(2) 0.5979(4) 0.49065(16) 0.0368(8) Uani 1 1 d . . . N3 N 0.1458(2) 0.5245(4) 0.38195(17) 0.0384(8) Uani 1 1 d . . . N4 N 0.2644(2) 0.6972(4) 0.45615(16) 0.0355(8) Uani 1 1 d . . . N5 N 0.3463(2) 0.4404(4) 0.50480(15) 0.0331(7) Uani 1 1 d . . . N6 N 0.2056(2) 0.3202(4) 0.50757(16) 0.0356(8) Uani 1 1 d . . . N7 N 0.2641(3) 0.5167(4) 0.3185(2) 0.0496(10) Uani 1 1 d . . . C11 C 0.2281(3) 0.6623(5) 0.5909(2) 0.0404(10) Uani 1 1 d . . . H11A H 0.2566 0.7393 0.5832 0.048 Uiso 1 1 calc R . . H11B H 0.229 0.6669 0.634 0.048 Uiso 1 1 calc R . . C12 C 0.2356(3) 0.4221(5) 0.6096(2) 0.0439(10) Uani 1 1 d . . . H12A H 0.2737 0.4018 0.651 0.053 Uiso 1 1 calc R . . H12B H 0.1866 0.4498 0.6148 0.053 Uiso 1 1 calc R . . C13 C 0.3559(3) 0.5383(5) 0.6075(2) 0.0379(9) Uani 1 1 d . . . H13A H 0.3739 0.6307 0.6107 0.046 Uiso 1 1 calc R . . H13B H 0.3742 0.4999 0.6496 0.046 Uiso 1 1 calc R . . C21 C 0.1428(3) 0.6631(5) 0.5450(2) 0.0412(10) Uani 1 1 d . . . C22 C 0.0799(3) 0.7249(5) 0.5548(3) 0.0525(12) Uani 1 1 d . . . H22 H 0.0858 0.7668 0.5929 0.063 Uiso 1 1 calc R . . C23 C 0.0064(3) 0.7229(6) 0.5055(3) 0.0598(15) Uani 1 1 d . . . H23 H -0.0368 0.7668 0.5103 0.072 Uiso 1 1 calc R . . C24 C -0.0023(3) 0.6567(6) 0.4504(3) 0.0540(13) Uani 1 1 d . . . H24 H -0.0512 0.6554 0.4178 0.065 Uiso 1 1 calc R . . C25 C 0.0622(3) 0.5920(5) 0.4436(2) 0.0433(10) Uani 1 1 d . . . C31 C 0.0646(3) 0.5103(5) 0.3886(3) 0.0479(12) Uani 1 1 d . . . H31A H 0.0237 0.5409 0.3503 0.057 Uiso 1 1 calc R . . H31B H 0.0546 0.4167 0.3951 0.057 Uiso 1 1 calc R . . C32 C 0.1441(3) 0.4271(5) 0.3311(2) 0.0437(10) Uani 1 1 d . . . H32A H 0.1053 0.4578 0.2918 0.052 Uiso 1 1 calc R . . H32B H 0.1262 0.341 0.3411 0.052 Uiso 1 1 calc R . . C33 C 0.1505(3) 0.6664(5) 0.3603(2) 0.0430(10) Uani 1 1 d . . . H33A H 0.147 0.6641 0.3165 0.052 Uiso 1 1 calc R . . H33B H 0.1049 0.7158 0.3622 0.052 Uiso 1 1 calc R . . C41 C 0.2233(3) 0.7403(5) 0.39727(19) 0.0393(10) Uani 1 1 d . . . C42 C 0.2457(3) 0.8534(5) 0.3720(2) 0.0554(13) Uani 1 1 d . . . H42 H 0.2157 0.8813 0.3315 0.066 Uiso 1 1 calc R . . C43 C 0.3119(4) 0.9247(6) 0.4065(3) 0.0610(14) Uani 1 1 d . . . H43 H 0.3275 1.0003 0.3897 0.073 Uiso 1 1 calc R . . C44 C 0.3548(3) 0.8811(5) 0.4670(2) 0.0515(12) Uani 1 1 d . . . H44 H 0.3998 0.927 0.4918 0.062 Uiso 1 1 calc R . . C45 C 0.3296(3) 0.7694(5) 0.4892(2) 0.0412(10) Uani 1 1 d . . . H45 H 0.359 0.7407 0.5297 0.049 Uiso 1 1 calc R . . C51 C 0.3906(3) 0.4609(4) 0.5664(2) 0.0345(9) Uani 1 1 d . . . C52 C 0.4683(3) 0.4160(5) 0.5909(2) 0.0431(10) Uani 1 1 d . . . H52 H 0.4981 0.4302 0.6332 0.052 Uiso 1 1 calc R . . C53 C 0.5012(3) 0.3504(6) 0.5525(2) 0.0523(12) Uani 1 1 d . . . H53 H 0.5535 0.3209 0.5685 0.063 Uiso 1 1 calc R . . C54 C 0.4563(3) 0.3287(5) 0.4908(2) 0.0490(12) Uani 1 1 d . . . H54 H 0.4773 0.2836 0.4642 0.059 Uiso 1 1 calc R . . C55 C 0.3791(3) 0.3751(5) 0.4686(2) 0.0386(9) Uani 1 1 d . . . H55 H 0.3486 0.36 0.4265 0.046 Uiso 1 1 calc R . . C61 C 0.2210(3) 0.2996(5) 0.5699(2) 0.0383(9) Uani 1 1 d . . . C62 C 0.2203(3) 0.1720(5) 0.5946(3) 0.0559(13) Uani 1 1 d . . . H62 H 0.2314 0.1602 0.6377 0.067 Uiso 1 1 calc R . . C63 C 0.2028(4) 0.0638(6) 0.5546(3) 0.0682(16) Uani 1 1 d . . . H63 H 0.2015 -0.0223 0.5702 0.082 Uiso 1 1 calc R . . C64 C 0.1873(3) 0.0837(5) 0.4917(3) 0.0590(14) Uani 1 1 d . . . H64 H 0.175 0.0114 0.464 0.071 Uiso 1 1 calc R . . C65 C 0.1900(3) 0.2122(5) 0.4698(2) 0.0454(11) Uani 1 1 d . . . H65 H 0.1807 0.2244 0.427 0.054 Uiso 1 1 calc R . . C71 C 0.2216(3) 0.4070(5) 0.32128(19) 0.0428(10) Uani 1 1 d . . . C72 C 0.2465(3) 0.2785(6) 0.3131(2) 0.0522(12) Uani 1 1 d . . . H72 H 0.216 0.2044 0.315 0.063 Uiso 1 1 calc R . . C73 C 0.3172(3) 0.2615(6) 0.3022(2) 0.0593(14) Uani 1 1 d . . . H73 H 0.3348 0.1762 0.2968 0.071 Uiso 1 1 calc R . . C74 C 0.3607(3) 0.3735(7) 0.2995(2) 0.0575(14) Uani 1 1 d . . . H74 H 0.4085 0.3658 0.2926 0.069 Uiso 1 1 calc R . . C75 C 0.3313(3) 0.4985(6) 0.3075(3) 0.0566(14) Uani 1 1 d . . . H75 H 0.3604 0.574 0.305 0.068 Uiso 1 1 calc R . . S1 S 0.54370(8) 1.10889(14) 0.33503(6) 0.0562(3) Uani 1 1 d . . . F11 F 0.4681(3) 0.8919(7) 0.3417(3) 0.154(3) Uani 1 1 d . . . F12 F 0.5849(4) 0.9052(5) 0.4109(3) 0.130(2) Uani 1 1 d . . . F13 F 0.5659(5) 0.8591(5) 0.3167(4) 0.156(3) Uani 1 1 d . . . O13 O 0.5199(3) 1.1753(6) 0.3810(2) 0.0952(17) Uani 1 1 d . . . O11 O 0.6260(3) 1.1308(5) 0.3451(3) 0.0906(15) Uani 1 1 d . . . O12 O 0.4920(4) 1.1208(6) 0.2724(2) 0.0988(18) Uani 1 1 d . . . C1 C 0.5417(5) 0.9323(8) 0.3530(3) 0.080(2) Uani 1 1 d . . . S2 S 0.49823(11) 0.59422(16) 0.19786(7) 0.0666(4) Uani 1 1 d . . . C2 C 0.5381(7) 0.4597(8) 0.1704(5) 0.104(3) Uani 1 1 d . . . F21 F 0.6049(8) 0.4729(9) 0.1738(12) 0.373(14) Uani 1 1 d . . . F22 F 0.5315(4) 0.3425(5) 0.1896(4) 0.146(2) Uani 1 1 d . . . F23 F 0.5064(16) 0.4504(13) 0.1111(6) 0.401(14) Uani 1 1 d . . . O21 O 0.5225(10) 0.5804(10) 0.2576(3) 0.284(9) Uani 1 1 d . . . O22 O 0.5053(5) 0.7061(5) 0.1657(3) 0.121(2) Uani 1 1 d . . . O23 O 0.4139(6) 0.5562(12) 0.1745(8) 0.255(8) Uani 1 1 d . . . O1 O 0.6942(4) 0.8050(7) 0.2337(3) 0.116(2) Uani 1 1 d . . . O2 O 0.6851(6) 1.0927(8) 0.2400(5) 0.173(4) Uani 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0272(2) 0.0388(2) 0.0221(2) -0.00075(11) 0.00648(14) 0.00269(11) N1 0.0340(18) 0.0407(19) 0.0279(17) -0.0016(15) 0.0098(15) 0.0017(15) N2 0.0295(17) 0.045(2) 0.0343(18) 0.0030(15) 0.0090(14) 0.0033(15) N3 0.0294(19) 0.051(2) 0.0294(19) 0.0012(16) 0.0036(15) 0.0000(15) N4 0.0341(18) 0.045(2) 0.0270(17) -0.0001(15) 0.0102(14) 0.0055(15) N5 0.0331(17) 0.0397(19) 0.0246(16) 0.0006(14) 0.0076(14) 0.0023(15) N6 0.0290(17) 0.045(2) 0.0328(18) -0.0020(15) 0.0105(14) 0.0014(15) N7 0.043(2) 0.055(3) 0.043(2) 0.0055(18) 0.0064(19) 0.0029(18) C11 0.043(2) 0.045(2) 0.035(2) -0.0068(19) 0.0160(19) 0.002(2) C12 0.053(3) 0.051(3) 0.031(2) 0.003(2) 0.018(2) -0.005(2) C13 0.032(2) 0.051(3) 0.026(2) -0.0017(19) 0.0038(17) 0.0002(19) C21 0.040(2) 0.044(2) 0.044(2) -0.003(2) 0.020(2) 0.0027(19) C22 0.054(3) 0.053(3) 0.059(3) -0.004(2) 0.031(2) 0.005(2) C23 0.046(3) 0.063(3) 0.079(4) 0.006(3) 0.032(3) 0.018(2) C24 0.029(2) 0.064(3) 0.069(3) 0.011(3) 0.017(2) 0.008(2) C25 0.036(2) 0.051(3) 0.043(2) 0.004(2) 0.0124(19) 0.000(2) C31 0.030(2) 0.068(3) 0.041(3) -0.002(2) 0.006(2) -0.001(2) C32 0.038(2) 0.058(3) 0.028(2) -0.002(2) 0.0008(17) -0.001(2) C33 0.038(2) 0.052(3) 0.033(2) 0.009(2) 0.0041(18) 0.005(2) C41 0.044(2) 0.044(2) 0.028(2) 0.0029(18) 0.0106(18) 0.0072(19) C42 0.070(3) 0.053(3) 0.034(2) 0.008(2) 0.007(2) -0.002(3) C43 0.076(4) 0.048(3) 0.054(3) 0.010(2) 0.017(3) -0.012(3) C44 0.050(3) 0.053(3) 0.050(3) -0.002(2) 0.015(2) -0.005(2) C45 0.038(2) 0.048(3) 0.034(2) 0.0013(19) 0.0080(18) -0.0003(19) C51 0.037(2) 0.039(2) 0.027(2) 0.0017(17) 0.0106(17) -0.0026(18) C52 0.030(2) 0.059(3) 0.034(2) 0.002(2) 0.0027(17) 0.000(2) C53 0.037(2) 0.066(3) 0.053(3) 0.007(2) 0.015(2) 0.014(2) C54 0.048(3) 0.056(3) 0.047(3) 0.003(2) 0.022(2) 0.015(2) C55 0.039(2) 0.049(2) 0.029(2) -0.0005(18) 0.0122(17) 0.0057(19) C61 0.035(2) 0.044(2) 0.036(2) 0.0031(19) 0.0132(18) -0.0004(18) C62 0.070(3) 0.049(3) 0.046(3) 0.007(2) 0.017(3) 0.002(3) C63 0.085(4) 0.041(3) 0.077(4) 0.007(3) 0.026(3) -0.001(3) C64 0.066(3) 0.042(3) 0.068(4) -0.013(3) 0.022(3) -0.001(2) C65 0.045(3) 0.048(3) 0.040(2) -0.009(2) 0.011(2) 0.001(2) C71 0.042(2) 0.059(3) 0.0216(19) -0.0024(19) 0.0039(17) 0.001(2) C72 0.064(3) 0.056(3) 0.037(2) -0.011(2) 0.018(2) -0.003(2) C73 0.070(4) 0.068(4) 0.044(3) -0.010(3) 0.025(3) 0.010(3) C74 0.052(3) 0.085(4) 0.036(3) -0.003(3) 0.016(2) 0.010(3) C75 0.046(3) 0.072(4) 0.046(3) 0.008(2) 0.008(2) -0.004(2) S1 0.0594(8) 0.0555(7) 0.0442(7) -0.0063(6) 0.0059(6) -0.0058(6) F11 0.104(4) 0.154(5) 0.176(6) 0.055(5) 0.012(4) -0.065(4) F12 0.158(5) 0.093(3) 0.103(4) 0.035(3) 0.000(3) -0.009(3) F13 0.216(7) 0.072(3) 0.191(6) -0.054(4) 0.086(6) -0.004(4) O13 0.087(3) 0.114(4) 0.075(3) -0.030(3) 0.016(3) 0.025(3) O11 0.069(3) 0.086(3) 0.117(4) -0.021(3) 0.034(3) -0.029(3) O12 0.124(4) 0.091(3) 0.048(2) 0.003(2) -0.012(2) -0.026(3) C1 0.084(5) 0.073(4) 0.069(4) 0.004(4) 0.009(4) -0.017(4) S2 0.0914(11) 0.0673(9) 0.0488(7) 0.0155(7) 0.0340(7) 0.0201(8) C2 0.148(9) 0.065(5) 0.131(8) -0.022(5) 0.090(7) -0.014(5) F21 0.288(14) 0.107(6) 0.92(4) 0.022(13) 0.45(2) 0.038(7) F22 0.173(6) 0.056(3) 0.219(7) 0.015(3) 0.081(5) 0.002(3) F23 0.83(4) 0.199(11) 0.175(10) -0.040(9) 0.172(17) 0.192(19) O21 0.57(2) 0.167(8) 0.059(4) -0.001(5) 0.035(8) 0.184(12) O22 0.182(6) 0.069(3) 0.164(6) 0.035(4) 0.126(5) 0.029(4) O23 0.122(7) 0.214(10) 0.47(2) 0.092(14) 0.158(12) 0.008(8) O1 0.129(5) 0.134(5) 0.101(4) -0.010(4) 0.059(4) 0.007(4) O2 0.224(9) 0.132(6) 0.235(10) -0.052(7) 0.173(9) -0.038(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ru N2 1.979(3) . ? Ru N1 2.081(3) . ? Ru N6 2.081(4) . ? Ru N4 2.101(4) . ? Ru N5 2.117(3) . ? Ru N3 2.266(4) . ? N1 C12 1.498(6) . ? N1 C11 1.500(6) . ? N1 C13 1.506(6) . ? N2 C21 1.347(6) . ? N2 C25 1.350(6) . ? N3 C32 1.495(6) . ? N3 C33 1.508(6) . ? N3 C31 1.526(6) . ? N4 C41 1.348(5) . ? N4 C45 1.356(6) . ? N5 C55 1.332(5) . ? N5 C51 1.358(5) . ? N6 C65 1.342(6) . ? N6 C61 1.353(5) . ? N7 C75 1.326(8) . ? N7 C71 1.348(7) . ? C11 C21 1.525(6) . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C12 C61 1.484(6) . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C13 C51 1.500(6) . ? C13 H13A 0.97 . ? C13 H13B 0.97 . ? C21 C22 1.371(7) . ? C22 C23 1.402(8) . ? C22 H22 0.93 . ? C23 C24 1.370(8) . ? C23 H23 0.93 . ? C24 C25 1.381(7) . ? C24 H24 0.93 . ? C25 C31 1.498(7) . ? C31 H31A 0.97 . ? C31 H31B 0.97 . ? C32 C71 1.499(7) . ? C32 H32A 0.97 . ? C32 H32B 0.97 . ? C33 C41 1.482(6) . ? C33 H33A 0.97 . ? C33 H33B 0.97 . ? C41 C42 1.384(7) . ? C42 C43 1.372(8) . ? C42 H42 0.93 . ? C43 C44 1.386(8) . ? C43 H43 0.93 . ? C44 C45 1.361(7) . ? C44 H44 0.93 . ? C45 H45 0.93 . ? C51 C52 1.387(6) . ? C52 C53 1.372(7) . ? C52 H52 0.93 . ? C53 C54 1.365(7) . ? C53 H53 0.93 . ? C54 C55 1.382(6) . ? C54 H54 0.93 . ? C55 H55 0.93 . ? C61 C62 1.391(7) . ? C62 C63 1.371(8) . ? C62 H62 0.93 . ? C63 C64 1.365(9) . ? C63 H63 0.93 . ? C64 C65 1.380(8) . ? C64 H64 0.93 . ? C65 H65 0.93 . ? C71 C72 1.389(7) . ? C72 C73 1.386(8) . ? C72 H72 0.93 . ? C73 C74 1.376(9) . ? C73 H73 0.93 . ? C74 C75 1.388(8) . ? C74 H74 0.93 . ? C75 H75 0.93 . ? S1 O12 1.403(5) . ? S1 O13 1.417(5) . ? S1 O11 1.434(5) . ? S1 C1 1.808(8) . ? F11 C1 1.320(9) . ? F12 C1 1.298(8) . ? F13 C1 1.282(9) . ? S2 O21 1.275(7) . ? S2 O22 1.360(5) . ? S2 O23 1.472(11) . ? S2 C2 1.733(9) . ? C2 F21 1.184(14) . ? C2 F22 1.265(10) . ? C2 F23 1.265(17) . ? 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 N2 Ru N1 80.72(14) . . ? N2 Ru N6 96.24(14) . . ? N1 Ru N6 80.71(14) . . ? N2 Ru N4 90.71(14) . . ? N1 Ru N4 101.58(14) . . ? N6 Ru N4 172.96(13) . . ? N2 Ru N5 162.55(14) . . ? N1 Ru N5 82.17(13) . . ? N6 Ru N5 84.34(14) . . ? N4 Ru N5 89.36(14) . . ? N2 Ru N3 76.84(14) . . ? N1 Ru N3 157.55(15) . . ? N6 Ru N3 100.82(14) . . ? N4 Ru N3 79.65(13) . . ? N5 Ru N3 120.28(13) . . ? C12 N1 C11 108.0(3) . . ? C12 N1 C13 110.5(4) . . ? C11 N1 C13 113.9(4) . . ? C12 N1 Ru 110.4(3) . . ? C11 N1 Ru 104.5(3) . . ? C13 N1 Ru 109.4(3) . . ? C21 N2 C25 121.7(4) . . ? C21 N2 Ru 116.2(3) . . ? C25 N2 Ru 122.0(3) . . ? C32 N3 C33 110.3(4) . . ? C32 N3 C31 104.6(4) . . ? C33 N3 C31 106.4(4) . . ? C32 N3 Ru 125.1(3) . . ? C33 N3 Ru 106.5(3) . . ? C31 N3 Ru 102.4(3) . . ? C41 N4 C45 116.5(4) . . ? C41 N4 Ru 116.7(3) . . ? C45 N4 Ru 126.3(3) . . ? C55 N5 C51 118.4(4) . . ? C55 N5 Ru 130.1(3) . . ? C51 N5 Ru 111.4(3) . . ? C65 N6 C61 117.6(4) . . ? C65 N6 Ru 126.2(3) . . ? C61 N6 Ru 115.3(3) . . ? C75 N7 C71 117.8(5) . . ? N1 C11 C21 108.1(4) . . ? N1 C11 H11A 110.1 . . ? C21 C11 H11A 110.1 . . ? N1 C11 H11B 110.1 . . ? C21 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? C61 C12 N1 111.7(4) . . ? C61 C12 H12A 109.3 . . ? N1 C12 H12A 109.3 . . ? C61 C12 H12B 109.3 . . ? N1 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C51 C13 N1 110.8(3) . . ? C51 C13 H13A 109.5 . . ? N1 C13 H13A 109.5 . . ? C51 C13 H13B 109.5 . . ? N1 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N2 C21 C22 120.8(4) . . ? N2 C21 C11 113.4(4) . . ? C22 C21 C11 125.8(4) . . ? C21 C22 C23 117.9(5) . . ? C21 C22 H22 121 . . ? C23 C22 H22 121 . . ? C24 C23 C22 120.5(4) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 119.3(5) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? N2 C25 C24 119.6(5) . . ? N2 C25 C31 112.6(4) . . ? C24 C25 C31 127.8(5) . . ? C25 C31 N3 109.7(4) . . ? C25 C31 H31A 109.7 . . ? N3 C31 H31A 109.7 . . ? C25 C31 H31B 109.7 . . ? N3 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? N3 C32 C71 115.5(4) . . ? N3 C32 H32A 108.4 . . ? C71 C32 H32A 108.4 . . ? N3 C32 H32B 108.4 . . ? C71 C32 H32B 108.4 . . ? H32A C32 H32B 107.5 . . ? C41 C33 N3 114.9(4) . . ? C41 C33 H33A 108.6 . . ? N3 C33 H33A 108.6 . . ? C41 C33 H33B 108.6 . . ? N3 C33 H33B 108.6 . . ? H33A C33 H33B 107.5 . . ? N4 C41 C42 121.8(4) . . ? N4 C41 C33 118.2(4) . . ? C42 C41 C33 119.9(4) . . ? C43 C42 C41 120.4(5) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 118.2(5) . . ? C42 C43 H43 120.9 . . ? C44 C43 H43 120.9 . . ? C45 C44 C43 118.5(5) . . ? C45 C44 H44 120.7 . . ? C43 C44 H44 120.7 . . ? N4 C45 C44 124.4(4) . . ? N4 C45 H45 117.8 . . ? C44 C45 H45 117.8 . . ? N5 C51 C52 120.8(4) . . ? N5 C51 C13 119.4(4) . . ? C52 C51 C13 119.7(4) . . ? C53 C52 C51 119.7(4) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C54 C53 C52 119.4(4) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C53 C54 C55 118.7(4) . . ? C53 C54 H54 120.6 . . ? C55 C54 H54 120.6 . . ? N5 C55 C54 122.9(4) . . ? N5 C55 H55 118.5 . . ? C54 C55 H55 118.5 . . ? N6 C61 C62 122.1(4) . . ? N6 C61 C12 115.7(4) . . ? C62 C61 C12 122.1(4) . . ? C63 C62 C61 119.0(5) . . ? C63 C62 H62 120.5 . . ? C61 C62 H62 120.5 . . ? C64 C63 C62 119.3(5) . . ? C64 C63 H63 120.3 . . ? C62 C63 H63 120.3 . . ? C63 C64 C65 119.3(5) . . ? C63 C64 H64 120.3 . . ? C65 C64 H64 120.3 . . ? N6 C65 C64 122.7(5) . . ? N6 C65 H65 118.6 . . ? C64 C65 H65 118.6 . . ? N7 C71 C72 121.7(5) . . ? N7 C71 C32 118.0(4) . . ? C72 C71 C32 120.2(5) . . ? C73 C72 C71 119.6(5) . . ? C73 C72 H72 120.2 . . ? C71 C72 H72 120.2 . . ? C74 C73 C72 118.6(5) . . ? C74 C73 H73 120.7 . . ? C72 C73 H73 120.7 . . ? C73 C74 C75 118.3(5) . . ? C73 C74 H74 120.9 . . ? C75 C74 H74 120.9 . . ? N7 C75 C74 124.0(5) . . ? N7 C75 H75 118 . . ? C74 C75 H75 118 . . ? O12 S1 O13 115.9(4) . . ? O12 S1 O11 115.6(4) . . ? O13 S1 O11 111.8(3) . . ? O12 S1 C1 104.5(3) . . ? O13 S1 C1 104.8(4) . . ? O11 S1 C1 102.3(3) . . ? F13 C1 F12 108.0(8) . . ? F13 C1 F11 104.1(7) . . ? F12 C1 F11 109.8(7) . . ? F13 C1 S1 111.9(6) . . ? F12 C1 S1 112.2(5) . . ? F11 C1 S1 110.5(6) . . ? O21 S2 O22 126.4(7) . . ? O21 S2 O23 106.4(10) . . ? O22 S2 O23 107.2(6) . . ? O21 S2 C2 105.3(6) . . ? O22 S2 C2 108.3(4) . . ? O23 S2 C2 100.1(7) . . ? F21 C2 F22 107.1(11) . . ? F21 C2 F23 98.7(14) . . ? F22 C2 F23 103.5(11) . . ? F21 C2 S2 115.3(9) . . ? F22 C2 S2 119.4(7) . . ? F23 C2 S2 110.2(10) . . ? 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 N2 Ru N1 C12 82.1(3) . . . . ? N6 Ru N1 C12 -15.8(3) . . . . ? N4 Ru N1 C12 170.9(3) . . . . ? N5 Ru N1 C12 -101.3(3) . . . . ? N3 Ru N1 C12 80.0(5) . . . . ? N2 Ru N1 C11 -33.8(3) . . . . ? N6 Ru N1 C11 -131.7(3) . . . . ? N4 Ru N1 C11 55.1(3) . . . . ? N5 Ru N1 C11 142.8(3) . . . . ? N3 Ru N1 C11 -35.9(5) . . . . ? N2 Ru N1 C13 -156.1(3) . . . . ? N6 Ru N1 C13 106.0(3) . . . . ? N4 Ru N1 C13 -67.2(3) . . . . ? N5 Ru N1 C13 20.5(3) . . . . ? N3 Ru N1 C13 -158.2(3) . . . . ? N1 Ru N2 C21 19.0(3) . . . . ? N6 Ru N2 C21 98.5(3) . . . . ? N4 Ru N2 C21 -82.6(3) . . . . ? N5 Ru N2 C21 7.5(7) . . . . ? N3 Ru N2 C21 -161.8(4) . . . . ? N1 Ru N2 C25 -161.7(4) . . . . ? N6 Ru N2 C25 -82.2(4) . . . . ? N4 Ru N2 C25 96.7(4) . . . . ? N5 Ru N2 C25 -173.2(4) . . . . ? N3 Ru N2 C25 17.5(4) . . . . ? N2 Ru N3 C32 -149.4(4) . . . . ? N1 Ru N3 C32 -147.2(4) . . . . ? N6 Ru N3 C32 -55.4(4) . . . . ? N4 Ru N3 C32 117.5(4) . . . . ? N5 Ru N3 C32 34.3(4) . . . . ? N2 Ru N3 C33 80.2(3) . . . . ? N1 Ru N3 C33 82.3(5) . . . . ? N6 Ru N3 C33 174.1(3) . . . . ? N4 Ru N3 C33 -13.0(3) . . . . ? N5 Ru N3 C33 -96.1(3) . . . . ? N2 Ru N3 C31 -31.3(3) . . . . ? N1 Ru N3 C31 -29.2(5) . . . . ? N6 Ru N3 C31 62.6(3) . . . . ? N4 Ru N3 C31 -124.5(3) . . . . ? N5 Ru N3 C31 152.3(3) . . . . ? N2 Ru N4 C41 -73.5(3) . . . . ? N1 Ru N4 C41 -154.1(3) . . . . ? N6 Ru N4 C41 97.5(11) . . . . ? N5 Ru N4 C41 124.0(3) . . . . ? N3 Ru N4 C41 3.0(3) . . . . ? N2 Ru N4 C45 114.4(4) . . . . ? N1 Ru N4 C45 33.7(4) . . . . ? N6 Ru N4 C45 -74.6(11) . . . . ? N5 Ru N4 C45 -48.2(4) . . . . ? N3 Ru N4 C45 -169.1(4) . . . . ? N2 Ru N5 C55 178.9(4) . . . . ? N1 Ru N5 C55 167.4(4) . . . . ? N6 Ru N5 C55 86.1(4) . . . . ? N4 Ru N5 C55 -90.8(4) . . . . ? N3 Ru N5 C55 -13.2(4) . . . . ? N2 Ru N5 C51 2.4(7) . . . . ? N1 Ru N5 C51 -9.1(3) . . . . ? N6 Ru N5 C51 -90.4(3) . . . . ? N4 Ru N5 C51 92.7(3) . . . . ? N3 Ru N5 C51 170.3(3) . . . . ? N2 Ru N6 C65 114.7(4) . . . . ? N1 Ru N6 C65 -165.8(4) . . . . ? N4 Ru N6 C65 -56.2(12) . . . . ? N5 Ru N6 C65 -82.9(4) . . . . ? N3 Ru N6 C65 36.9(4) . . . . ? N2 Ru N6 C61 -77.3(3) . . . . ? N1 Ru N6 C61 2.2(3) . . . . ? N4 Ru N6 C61 111.8(10) . . . . ? N5 Ru N6 C61 85.2(3) . . . . ? N3 Ru N6 C61 -155.0(3) . . . . ? C12 N1 C11 C21 -74.8(4) . . . . ? C13 N1 C11 C21 162.0(4) . . . . ? Ru N1 C11 C21 42.7(4) . . . . ? C11 N1 C12 C61 140.2(4) . . . . ? C13 N1 C12 C61 -94.7(4) . . . . ? Ru N1 C12 C61 26.5(5) . . . . ? C12 N1 C13 C51 93.7(4) . . . . ? C11 N1 C13 C51 -144.6(4) . . . . ? Ru N1 C13 C51 -28.1(4) . . . . ? C25 N2 C21 C22 0.9(7) . . . . ? Ru N2 C21 C22 -179.8(4) . . . . ? C25 N2 C21 C11 -177.8(4) . . . . ? Ru N2 C21 C11 1.5(5) . . . . ? N1 C11 C21 N2 -30.8(5) . . . . ? N1 C11 C21 C22 150.6(5) . . . . ? N2 C21 C22 C23 -2.7(8) . . . . ? C11 C21 C22 C23 175.8(5) . . . . ? C21 C22 C23 C24 2.3(9) . . . . ? C22 C23 C24 C25 -0.1(9) . . . . ? C21 N2 C25 C24 1.4(7) . . . . ? Ru N2 C25 C24 -177.9(4) . . . . ? C21 N2 C25 C31 -177.9(4) . . . . ? Ru N2 C25 C31 2.8(6) . . . . ? C23 C24 C25 N2 -1.8(8) . . . . ? C23 C24 C25 C31 177.5(5) . . . . ? N2 C25 C31 N3 -32.7(6) . . . . ? C24 C25 C31 N3 148.0(5) . . . . ? C32 N3 C31 C25 173.6(4) . . . . ? C33 N3 C31 C25 -69.7(5) . . . . ? Ru N3 C31 C25 41.9(4) . . . . ? C33 N3 C32 C71 74.1(5) . . . . ? C31 N3 C32 C71 -171.8(4) . . . . ? Ru N3 C32 C71 -54.8(5) . . . . ? C32 N3 C33 C41 -117.1(4) . . . . ? C31 N3 C33 C41 130.1(4) . . . . ? Ru N3 C33 C41 21.4(4) . . . . ? C45 N4 C41 C42 -0.9(6) . . . . ? Ru N4 C41 C42 -173.8(4) . . . . ? C45 N4 C41 C33 -178.3(4) . . . . ? Ru N4 C41 C33 8.8(5) . . . . ? N3 C33 C41 N4 -21.4(6) . . . . ? N3 C33 C41 C42 161.1(4) . . . . ? N4 C41 C42 C43 0.9(8) . . . . ? C33 C41 C42 C43 178.3(5) . . . . ? C41 C42 C43 C44 -0.6(9) . . . . ? C42 C43 C44 C45 0.3(9) . . . . ? C41 N4 C45 C44 0.6(7) . . . . ? Ru N4 C45 C44 172.8(4) . . . . ? C43 C44 C45 N4 -0.3(8) . . . . ? C55 N5 C51 C52 0.5(6) . . . . ? Ru N5 C51 C52 177.5(4) . . . . ? C55 N5 C51 C13 177.9(4) . . . . ? Ru N5 C51 C13 -5.1(5) . . . . ? N1 C13 C51 N5 22.6(6) . . . . ? N1 C13 C51 C52 -159.9(4) . . . . ? N5 C51 C52 C53 0.3(7) . . . . ? C13 C51 C52 C53 -177.2(5) . . . . ? C51 C52 C53 C54 -0.9(8) . . . . ? C52 C53 C54 C55 0.7(8) . . . . ? C51 N5 C55 C54 -0.7(7) . . . . ? Ru N5 C55 C54 -177.0(4) . . . . ? C53 C54 C55 N5 0.1(8) . . . . ? C65 N6 C61 C62 -0.7(6) . . . . ? Ru N6 C61 C62 -169.8(4) . . . . ? C65 N6 C61 C12 -178.3(4) . . . . ? Ru N6 C61 C12 12.6(5) . . . . ? N1 C12 C61 N6 -26.1(6) . . . . ? N1 C12 C61 C62 156.3(5) . . . . ? N6 C61 C62 C63 -0.4(8) . . . . ? C12 C61 C62 C63 177.0(5) . . . . ? C61 C62 C63 C64 0.5(9) . . . . ? C62 C63 C64 C65 0.4(10) . . . . ? C61 N6 C65 C64 1.7(7) . . . . ? Ru N6 C65 C64 169.5(4) . . . . ? C63 C64 C65 N6 -1.6(8) . . . . ? C75 N7 C71 C72 0.0(7) . . . . ? C75 N7 C71 C32 -177.7(4) . . . . ? N3 C32 C71 N7 -46.2(6) . . . . ? N3 C32 C71 C72 136.1(4) . . . . ? N7 C71 C72 C73 0.5(7) . . . . ? C32 C71 C72 C73 178.1(4) . . . . ? C71 C72 C73 C74 -0.2(7) . . . . ? C72 C73 C74 C75 -0.4(8) . . . . ? C71 N7 C75 C74 -0.8(8) . . . . ? C73 C74 C75 N7 1.0(8) . . . . ? O12 S1 C1 F13 60.9(7) . . . . ? O13 S1 C1 F13 -176.8(6) . . . . ? O11 S1 C1 F13 -60.0(7) . . . . ? O12 S1 C1 F12 -177.6(6) . . . . ? O13 S1 C1 F12 -55.2(7) . . . . ? O11 S1 C1 F12 61.6(7) . . . . ? O12 S1 C1 F11 -54.7(7) . . . . ? O13 S1 C1 F11 67.7(6) . . . . ? O11 S1 C1 F11 -175.5(6) . . . . ? O21 S2 C2 F21 -81.1(18) . . . . ? O22 S2 C2 F21 56.6(16) . . . . ? O23 S2 C2 F21 168.6(16) . . . . ? O21 S2 C2 F22 48.8(14) . . . . ? O22 S2 C2 F22 -173.5(10) . . . . ? O23 S2 C2 F22 -61.5(12) . . . . ? O21 S2 C2 F23 168.3(16) . . . . ? O22 S2 C2 F23 -54.0(15) . . . . ? O23 S2 C2 F23 58.0(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_A _geom_hbond_distance_DA _geom_hbond_site_symmetry_A O1 O22 3.352(11) . O1 O2 2.877(11) . O2 O11 2.944(9) . O2 O1 2.939(11) 2655 # end of cif