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 'Dalton Transactions' _publ_contact_author ; Dr Kenneth Kam-Wing Lo Department of Biology & Chemistry City University of Hong Kong Tat Chee Avenue Kowloon Hong Kong CHINA ; loop_ _publ_author_name 'Cheung, Kung-Kai' 'Hui, Wai-Ki' 'Lo, Kenneth Kam-Wing' 'Ng, Dominic Chun-Ming' data_afc962_complex_1_18042000 _database_code_CSD 154472 #----------------------------------- _audit_creation_date 'Sat Apr 29 12:55:49 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------- #---- _computing_data_collection 'MSC/AFC DiffractometerControl' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------ #----------- _cell_length_a 11.572(1) _cell_length_b 15.864(1) _cell_length_c 13.054(1) _cell_angle_alpha 90 _cell_angle_beta 91.508(7) _cell_angle_gamma 90 _cell_volume 2395.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 36.3 _cell_measurement_theta_max 38.8 #---------------------------------------------------------------------- #------- _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' #----------------------------------------------------------- #------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.973 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 711.66 _chemical_formula_analytical ? _chemical_formula_sum 'C20 H12 F3 N4 O6 S2 Re' _chemical_formula_moiety '(C19 H12 N4 O3 S Re)+ (CF3SO3)-' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1368.00 _exptl_absorpt_coefficient_mu 5.317 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.721 #--------------------------------------------------------------------- #-------- _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% -2.51 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 4624 _reflns_number_total 4397 _reflns_number_observed 3278 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 1.81 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.00539 _diffrn_orient_matrix_UB_12 0.02683 _diffrn_orient_matrix_UB_13 0.06903 _diffrn_orient_matrix_UB_21 -0.00647 _diffrn_orient_matrix_UB_22 -0.05698 _diffrn_orient_matrix_UB_23 0.03211 _diffrn_orient_matrix_UB_31 0.08603 _diffrn_orient_matrix_UB_32 -0.00260 _diffrn_orient_matrix_UB_33 0.00876 #------------------------------------------------------------------- #---------- 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 80 0.003 0.002 'InternationalTables' H 0 48 0.000 0.000 'International Tables' N 0 16 0.006 0.003 'International Tables' O 0 24 0.011 0.006 'International Tables' F 0 12 0.017 0.010 'International Tables' S 0 8 0.125 0.123 'International Tables' Re 0 4 -1.018 7.231 'International Tables' #------------------------------------------------------------------- #---------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Re(1) 0.15551(3) 0.11807(2) 0.25034(2) 0.0530(1) Uij ? ? S(1) 0.7579(3) -0.1181(2) 0.0917(3) 0.109(1) Uij ? ? S(2) 0.6675(4) 0.1710(3) 0.2638(3) 0.122(1) Uij ? ? F(1) 0.712(1) 0.2512(6) 0.0996(7) 0.221(5) Uij ? ? F(2) 0.615(1) 0.3197(7) 0.2033(8) 0.235(6) Uij ? ? F(3) 0.791(1) 0.3002(7) 0.2317(8) 0.200(5) Uij ? ? O(1) 0.0168(6) 0.2550(4) 0.3596(6) 0.089(2) Uij ? ? O(2) 0.2988(7) 0.2579(4) 0.1535(6) 0.100(3) Uij ? ? O(3) -0.0115(7) 0.1343(5) 0.0657(6) 0.097(3) Uij ? ? O(4) 0.668(1) 0.1972(7) 0.3626(8) 0.219(6) Uij ? ? O(5) 0.565(1) 0.1483(10) 0.210(2) 0.282(8) Uij ? ? O(6) 0.769(1) 0.1175(9) 0.229(1) 0.244(9) Uij ? ? N(1) 0.2670(6) 0.0928(4) 0.3832(5) 0.058(2) Uij ? ? N(2) 0.0748(6) 0.0137(4) 0.3282(5) 0.060(2) Uij ? ? N(3) 0.2526(6) 0.0166(4) 0.1724(5) 0.054(2) Uij ? ? N(4) 0.5490(7) -0.0486(5) 0.1332(7) 0.081(3) Uij ? ? C(1) 0.0685(8) 0.2036(6) 0.3188(7) 0.065(3) Uij ? ? C(2) 0.2448(8) 0.2049(6) 0.1880(7) 0.067(3) Uij ? ? C(3) 0.0483(9) 0.1276(5) 0.1340(7) 0.069(3) Uij ? ? C(4) 0.3584(9) 0.1389(6) 0.4118(7) 0.075(3) Uij ? ? C(5) 0.4256(9) 0.1207(8) 0.5009(9) 0.094(4) Uij ? ? C(6) 0.3978(10) 0.0557(8) 0.5588(8) 0.085(4) Uij ? ? C(7) 0.305(1) 0.0063(7) 0.5288(8) 0.084(4) Uij ? ? C(8) 0.2382(8) 0.0240(5) 0.4404(6) 0.063(3) Uij ? ? C(9) 0.1346(8) -0.0205(5) 0.4088(6) 0.061(3) Uij ? ? C(10) 0.094(1) -0.0936(6) 0.4556(7) 0.080(3) Uij ? ? C(11) -0.008(1) -0.1305(6) 0.4215(9) 0.089(4) Uij ? ? C(12) -0.071(1) -0.0930(7) 0.3426(8) 0.086(4) Uij ? ? C(13) -0.0269(8) -0.0231(6) 0.2979(7) 0.073(3) Uij ? ? C(14) 0.1959(8) -0.0401(6) 0.1134(7) 0.070(3) Uij ? ? C(15) 0.2524(10) -0.0985(7) 0.0573(9) 0.090(4) Uij ? ? C(16) 0.371(1) -0.1035(6) 0.0605(8) 0.079(3) Uij ? ? C(17) 0.4289(8) -0.0457(5) 0.1218(6) 0.066(3) Uij ? ? C(18) 0.3684(7) 0.0144(5) 0.1773(6) 0.058(2) Uij ? ? C(19) 0.6357(9) -0.0794(7) 0.1138(7) 0.076(3) Uij ? ? C(20) 0.698(2) 0.263(1) 0.1933(9) 0.128(6) Uij ? ? H(1) 0.3779 0.1856 0.3707 0.0921 Uij ? ? H(2) 0.4919 0.1553 0.5183 0.1112 Uij ? ? H(3) 0.4408 0.0440 0.6201 0.1018 Uij ? ? H(4) 0.2869 -0.0412 0.5695 0.1015 Uij ? ? H(5) 0.1385 -0.1183 0.5108 0.0961 Uij ? ? H(6) -0.0358 -0.1810 0.4519 0.1050 Uij ? ? H(7) -0.1418 -0.1158 0.3204 0.1017 Uij ? ? H(8) -0.0704 0.0010 0.2427 0.0882 Uij ? ? H(9) 0.1147 -0.0392 0.1109 0.0827 Uij ? ? H(10) 0.2077 -0.1366 0.0155 0.1067 Uij ? ? H(11) 0.4122 -0.1443 0.0224 0.0951 Uij ? ? H(12) 0.4088 0.0540 0.2187 0.0689 Uij ? ? 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 Re(1) 0.0583(2) 0.0484(2) 0.0524(2) -0.0002(1) 0.0027(1) 0.0042(1) S(1) 0.085(2) 0.137(3) 0.105(2) 0.034(2) 0.016(2) 0.014(2) S(2) 0.151(3) 0.104(3) 0.113(3) -0.044(2) 0.005(3) 0.007(2) F(1) 0.43(2) 0.138(8) 0.090(6) -0.058(9) 0.037(8) -0.024(5) F(2) 0.32(1) 0.181(10) 0.19(1) 0.13(1) -0.10(1) -0.053(8) F(3) 0.24(1) 0.20(1) 0.157(9) -0.112(10) -0.014(8) 0.013(7) O(1) 0.093(5) 0.074(4) 0.102(5) 0.014(4) 0.023(4) -0.016(4) O(2) 0.116(6) 0.075(5) 0.111(6) -0.016(4) 0.029(5) 0.027(4) O(3) 0.086(5) 0.124(6) 0.079(5) 0.003(4) -0.021(4) 0.017(4) O(4) 0.43(2) 0.118(8) 0.115(8) -0.07(1) 0.08(1) -0.005(7) O(5) 0.115(8) 0.29(2) 0.45(3) -0.12(1) 0.06(1) -0.22(2) O(6) 0.18(1) 0.24(2) 0.31(2) 0.13(1) 0.03(1) -0.03(1) N(1) 0.061(4) 0.059(4) 0.054(4) 0.001(3) 0.000(3) -0.007(3) N(2) 0.074(4) 0.047(4) 0.060(4) -0.009(3) 0.015(3) -0.001(3) N(3) 0.062(4) 0.056(4) 0.043(3) -0.006(3) 0.000(3) 0.002(3) N(4) 0.059(5) 0.080(5) 0.106(6) 0.005(4) 0.017(5) -0.020(5) C(1) 0.070(6) 0.059(5) 0.068(5) -0.011(4) 0.004(4) 0.006(4) C(2) 0.070(6) 0.061(5) 0.073(6) 0.002(5) 0.014(5) 0.007(4) C(3) 0.068(6) 0.076(6) 0.063(5) 0.009(5) 0.003(5) 0.013(4) C(4) 0.076(7) 0.078(6) 0.070(6) 0.007(5) 0.000(5) -0.005(5) C(5) 0.067(6) 0.14(1) 0.074(7) 0.030(6) -0.021(5) -0.030(7) C(6) 0.085(7) 0.108(8) 0.062(6) 0.033(6) -0.003(5) 0.010(6) C(7) 0.088(7) 0.096(7) 0.068(6) 0.044(6) 0.017(5) 0.020(5) C(8) 0.076(5) 0.066(5) 0.049(5) 0.018(4) 0.015(4) 0.007(4) C(9) 0.080(6) 0.049(5) 0.053(5) 0.006(4) 0.017(4) -0.001(4) C(10) 0.116(9) 0.066(6) 0.060(6) 0.015(6) 0.024(6) 0.011(5) C(11) 0.128(10) 0.058(6) 0.083(7) -0.013(6) 0.035(7) 0.006(5) C(12) 0.106(8) 0.069(6) 0.085(7) -0.031(6) 0.032(6) -0.018(6) C(13) 0.079(6) 0.071(6) 0.071(6) -0.009(5) 0.010(5) -0.012(5) C(14) 0.070(5) 0.059(5) 0.080(6) 0.002(4) -0.013(5) -0.014(4) C(15) 0.088(7) 0.077(7) 0.104(8) 0.015(5) -0.024(6) -0.032(6) C(16) 0.093(8) 0.066(6) 0.077(6) 0.007(5) -0.007(6) -0.015(5) C(17) 0.076(6) 0.065(5) 0.058(5) 0.005(5) 0.003(4) 0.001(4) C(18) 0.059(5) 0.058(5) 0.056(5) 0.000(4) -0.005(4) 0.003(4) C(19) 0.080(6) 0.085(7) 0.062(6) 0.004(5) 0.002(5) 0.003(5) C(20) 0.20(2) 0.12(1) 0.063(8) -0.01(1) -0.018(9) 0.003(7) #-------------------------------------------------------------------------- #--- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3278 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0355 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0537 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.205 _refine_ls_shift/esd_max 0.0540 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.86 _refine_diff_density_max 1.03 #---------------------------------------------------------------------- #------- _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 Re(1) N(1) 2.171(6) ? ? yes Re(1) N(2) 2.167(6) ? ? yes Re(1) N(3) 2.225(6) ? ? yes Re(1) C(1) 1.923(10) ? ? yes Re(1) C(2) 1.916(9) ? ? yes Re(1) C(3) 1.941(10) ? ? yes S(1) C(19) 1.58(1) ? ? yes S(2) O(4) 1.35(1) ? ? yes S(2) O(5) 1.41(1) ? ? yes S(2) O(6) 1.53(1) ? ? yes S(2) C(20) 1.77(1) ? ? yes F(1) C(20) 1.25(1) ? ? yes F(2) C(20) 1.32(2) ? ? yes F(3) C(20) 1.31(2) ? ? yes O(1) C(1) 1.15(1) ? ? yes O(2) C(2) 1.15(1) ? ? yes O(3) C(3) 1.12(1) ? ? yes N(1) C(4) 1.33(1) ? ? yes N(1) C(8) 1.37(1) ? ? yes N(2) C(9) 1.36(1) ? ? yes N(2) C(13) 1.36(1) ? ? yes N(3) C(14) 1.343(10) ? ? yes N(3) C(18) 1.339(10) ? ? yes N(4) C(17) 1.39(1) ? ? yes N(4) C(19) 1.15(1) ? ? yes C(4) C(5) 1.41(1) ? ? yes C(5) C(6) 1.32(1) ? ? yes C(6) C(7) 1.38(2) ? ? yes C(7) C(8) 1.40(1) ? ? yes C(8) C(9) 1.44(1) ? ? yes C(9) C(10) 1.40(1) ? ? yes C(10) C(11) 1.38(2) ? ? yes C(11) C(12) 1.38(2) ? ? yes C(12) C(13) 1.36(1) ? ? yes C(14) C(15) 1.36(1) ? ? yes C(15) C(16) 1.37(1) ? ? yes C(16) C(17) 1.38(1) ? ? yes C(17) C(18) 1.40(1) ? ? yes #----------------------------------------------------------------------- #------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Re(1) N(2) 74.8(3) ? ? ? yes N(1) Re(1) N(3) 86.3(2) ? ? ? yes N(1) Re(1) C(1) 93.8(3) ? ? ? yes N(1) Re(1) C(2) 99.0(3) ? ? ? yes N(1) Re(1) C(3) 173.3(3) ? ? ? yes N(2) Re(1) N(3) 83.7(3) ? ? ? yes N(2) Re(1) C(1) 94.8(3) ? ? ? yes N(2) Re(1) C(2) 172.9(3) ? ? ? yes N(2) Re(1) C(3) 98.7(3) ? ? ? yes N(3) Re(1) C(1) 178.5(3) ? ? ? yes N(3) Re(1) C(2) 92.4(3) ? ? ? yes N(3) Re(1) C(3) 91.1(3) ? ? ? yes C(1) Re(1) C(2) 89.1(4) ? ? ? yes C(1) Re(1) C(3) 88.7(4) ? ? ? yes C(2) Re(1) C(3) 87.3(4) ? ? ? yes O(4) S(2) O(5) 122(1) ? ? ? yes O(4) S(2) O(6) 117(1) ? ? ? yes O(4) S(2) C(20) 104.3(6) ? ? ? yes O(5) S(2) O(6) 110.7(9) ? ? ? yes O(5) S(2) C(20) 97.4(10) ? ? ? yes O(6) S(2) C(20) 97.9(9) ? ? ? yes Re(1) N(1) C(4) 125.0(6) ? ? ? yes Re(1) N(1) C(8) 115.8(5) ? ? ? yes C(4) N(1) C(8) 119.2(8) ? ? ? yes Re(1) N(2) C(9) 116.8(5) ? ? ? yes Re(1) N(2) C(13) 124.8(6) ? ? ? yes C(9) N(2) C(13) 118.2(7) ? ? ? yes Re(1) N(3) C(14) 120.1(5) ? ? ? yes Re(1) N(3) C(18) 120.9(5) ? ? ? yes C(14) N(3) C(18) 118.9(7) ? ? ? yes C(17) N(4) C(19) 149.7(10) ? ? ? yes Re(1) C(1) O(1) 179.7(8) ? ? ? yes Re(1) C(2) O(2) 178.0(9) ? ? ? yes Re(1) C(3) O(3) 178.2(9) ? ? ? yes N(1) C(4) C(5) 122.3(10) ? ? ? yes C(4) C(5) C(6) 119(1) ? ? ? yes C(5) C(6) C(7) 118.6(10) ? ? ? yes C(6) C(7) C(8) 122.0(10 ? ? ? yes N(1) C(8) C(7) 118.3(9) ? ? ? yes N(1) C(8) C(9) 116.6(7) ? ? ? yes C(7) C(8) C(9) 125.0(9) ? ? ? yes N(2) C(9) C(8) 115.4(7) ? ? ? yes N(2) C(9) C(10) 119.9(9) ? ? ? yes C(8) C(9) C(10) 124.6(9) ? ? ? yes C(9) C(10) C(11) 120.4(10) ? ? ? yes C(10) C(11) C(12) 119.4(9) ? ? ? yes C(11) C(12) C(13) 118(1) ? ? ? yes N(2) C(13) C(12) 123.8(10) ? ? ? yes N(3) C(14) C(15) 122.0(8) ? ? ? yes C(14) C(15) C(16) 121.1(9) ? ? ? yes C(15) C(16) C(17) 116.7(9) ? ? ? yes N(4) C(17) C(16) 120.5(8) ? ? ? yes N(4) C(17) C(18) 118.7(8) ? ? ? yes C(16) C(17) C(18) 120.7(9) ? ? ? yes N(3) C(18) C(17) 120.5(7) ? ? ? yes S(1) C(19) N(4) 176.8(10) ? ? ? yes S(2) C(20) F(1) 114(1) ? ? ? yes S(2) C(20) F(2) 110(1) ? ? ? yes S(2) C(20) F(3) 110(1) ? ? ? yes F(1) C(20) F(2) 108(1) ? ? ? yes F(1) C(20) F(3) 108(1) ? ? ? yes F(2) C(20) F(3) 104(1) ? ? ? yes #----------------------------------------------------------------------- #------