# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Prof Vivian Yam' _publ_contact_author_address ; Department of Chemistry The University of Hong Kong Pokfulam Road Hong Kong ; _publ_contact_author_email WWYAM@HKU.HK _publ_section_title ; Synthesis, Photophysics, Electrochemistry and Metal Ion-Binding Studies of Rhenium(I) Complexes with Crown Ether Pendants: Selective and Specific Binding Properties for Various Metal Ions. ; loop_ _publ_author_name 'Vivian Yam' 'Kung-Kai Cheung.' 'Wei-Ping Li.' 'Keith Man-Chung Wong.' data_kkc364_Yam-RESE_Re1Se1ClO7 _database_code_depnum_ccdc_archive 'CCDC 252682' #------------------------------------------------------------------------------ _audit_creation_date 'Thu Nov 5 09:47:29 2004' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _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 8.669(4) _cell_length_b 12.752(4) _cell_length_c 13.644(4) _cell_angle_alpha 67.57(3) _cell_angle_beta 89.21(3) _cell_angle_gamma 72.56(3) _cell_volume 1321.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 32.2 _cell_measurement_theta_max 37.4 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_meas ? _chemical_formula_weight 741.07 _chemical_formula_analytical ? _chemical_formula_sum 'C23 H24 Cl N2 O7 Re Se ' _chemical_formula_moiety 'C23 H24 Cl N2 O7 Re Se ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 716.00 _exptl_absorpt_coefficient_mu 6.122 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.649 #------------------------------------------------------------------------------ _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 ? _diffrn_measurement_device AFC7R _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% 0.65 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 2 1 3 3 1 2 1 -3 _diffrn_reflns_number 3651 _reflns_number_total 3464 _reflns_number_observed 3037 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 1.48 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 22.52 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.00245 _diffrn_orient_matrix_UB_12 0.07697 _diffrn_orient_matrix_UB_13 0.00440 _diffrn_orient_matrix_UB_21 0.02502 _diffrn_orient_matrix_UB_22 -0.04161 _diffrn_orient_matrix_UB_23 0.07936 _diffrn_orient_matrix_UB_31 -0.11908 _diffrn_orient_matrix_UB_32 0.01881 _diffrn_orient_matrix_UB_33 0.00728 #------------------------------------------------------------------------------ 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 Re 0 2 -1.018 7.231 'International Tables' Se 0 2 -0.093 2.226 'International Tables' Cl 0 2 0.148 0.159 'International Tables' O 0 14 0.011 0.006 'International Tables' C 0 46 0.003 0.002 'International Tables' H 0 48 0.000 0.000 'International Tables' N 0 4 0.006 0.003 '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) 0.18841(3) 0.16319(2) 0.08393(2) 0.04746(9) Uij ? ? Se(1) -0.9477(1) 0.79850(9) -0.49386(10) 0.1226(4) Uij ? ? Cl(1) 0.0344(2) 0.3358(1) 0.1253(1) 0.0606(5) Uij ? ? O(1) -0.0904(6) 0.0568(4) 0.1319(5) 0.088(2) Uij ? ? O(2) 0.3629(7) -0.0487(5) 0.0280(6) 0.105(3) Uij ? ? O(3) 0.3325(8) 0.0055(5) 0.3167(5) 0.100(2) Uij ? ? O(4) -0.3767(5) 0.5698(4) -0.3255(3) 0.056(1) Uij ? ? O(5) -0.6294(6) 0.7740(4) -0.3399(4) 0.076(2) Uij ? ? O(6) -0.7865(6) 0.4307(4) -0.3690(4) 0.077(2) Uij ? ? O(7) -0.4465(6) 0.3950(4) -0.3423(4) 0.069(2) Uij ? ? N(1) 0.3741(6) 0.2508(4) 0.0443(4) 0.046(2) Uij ? ? N(2) 0.1131(6) 0.2956(4) -0.0821(4) 0.048(2) Uij ? ? C(1) 0.0133(9) 0.0986(6) 0.1116(6) 0.063(2) Uij ? ? C(2) 0.3028(8) 0.0323(6) 0.0442(6) 0.063(2) Uij ? ? C(3) 0.2767(9) 0.0656(6) 0.2299(7) 0.065(2) Uij ? ? C(4) 0.5088(8) 0.2282(6) 0.1064(5) 0.054(2) Uij ? ? C(5) 0.6162(8) 0.2918(6) 0.0763(6) 0.059(2) Uij ? ? C(6) 0.5872(8) 0.3822(7) -0.0220(6) 0.066(3) Uij ? ? C(7) 0.4496(9) 0.4088(6) -0.0895(6) 0.067(2) Uij ? ? C(8) 0.3467(8) 0.3417(6) -0.0533(5) 0.053(2) Uij ? ? C(9) 0.2004(8) 0.3623(6) -0.1176(5) 0.055(2) Uij ? ? C(10) -0.0330(7) 0.3188(6) -0.1471(5) 0.050(2) Uij ? ? C(11) -0.1310(7) 0.4374(5) -0.2046(5) 0.046(2) Uij ? ? C(12) -0.2667(7) 0.4577(5) -0.2678(5) 0.047(2) Uij ? ? C(13) -0.3464(8) 0.6697(6) -0.3157(6) 0.063(2) Uij ? ? C(14) -0.4814(9) 0.7799(6) -0.3828(6) 0.065(2) Uij ? ? C(15) -0.7590(10) 0.8844(7) -0.3862(7) 0.090(3) Uij ? ? C(16) -0.915(1) 0.8580(7) -0.3849(7) 0.094(3) Uij ? ? C(17) -0.813(2) 0.626(2) -0.401(1) 0.100(5) Uij ? ? C(17') -0.937(5) 0.622(3) -0.417(3) 0.16(1) Uij ? ? C(18') -0.773(3) 0.570(2) -0.440(2) 0.080(6) Uij ? ? C(18) -0.877(2) 0.546(1) -0.434(1) 0.070(3) Uij ? ? C(19) -0.6666(9) 0.3617(7) -0.4102(6) 0.070(3) Uij ? ? C(20) -0.5072(9) 0.3019(6) -0.3393(6) 0.069(3) Uij ? ? C(21) -0.3064(8) 0.3631(5) -0.2776(5) 0.056(2) Uij ? ? C(22) -0.2060(9) 0.2476(6) -0.2203(6) 0.069(2) Uij ? ? C(23) -0.0714(9) 0.2257(6) -0.1541(6) 0.067(2) Uij ? ? H(1) 0.5304 0.1651 0.1756 0.0611 Uij ? ? H(2) 0.7112 0.2731 0.1226 0.0701 Uij ? ? H(3) 0.6621 0.4264 -0.0456 0.0768 Uij ? ? H(4) 0.4258 0.4707 -0.1596 0.0812 Uij ? ? H(5) 0.1718 0.4261 -0.1859 0.0669 Uij ? ? H(6) -0.1048 0.5027 -0.2000 0.0547 Uij ? ? H(7) -0.3422 0.6601 -0.2436 0.0773 Uij ? ? H(8) -0.2453 0.6764 -0.3418 0.0773 Uij ? ? H(9) -0.4915 0.7849 -0.4534 0.0765 Uij ? ? H(10) -0.4625 0.8487 -0.3821 0.0765 Uij ? ? H(11) -0.7625 0.9315 -0.3472 0.1074 Uij ? ? H(12) -0.7435 0.9260 -0.4585 0.1074 Uij ? ? H(13) -1.0051 0.9286 -0.3972 0.1205 Uij ? ? H(14) -0.9193 0.7984 -0.3169 0.1205 Uij ? ? H(19) -0.7048 0.3018 -0.4165 0.0827 Uij ? ? H(20) -0.6505 0.4126 -0.4782 0.0827 Uij ? ? H(21) -0.4339 0.2495 -0.3647 0.0787 Uij ? ? H(22) -0.5247 0.2588 -0.2680 0.0787 Uij ? ? H(23) -0.2313 0.1822 -0.2259 0.0862 Uij ? ? H(24) -0.0083 0.1457 -0.1127 0.0771 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) 0.0479(2) 0.0379(2) 0.0543(2) -0.0098(1) -0.0015(1) -0.0184(1) Se(1) 0.1271(9) 0.0712(6) 0.1278(10) -0.0155(6) -0.0486(7) -0.0054(6) Cl(1) 0.068(1) 0.0513(10) 0.067(1) -0.0172(8) 0.0090(9) -0.0290(9) O(1) 0.057(3) 0.060(3) 0.149(6) -0.024(3) 0.010(3) -0.040(3) O(2) 0.088(4) 0.086(4) 0.170(7) -0.030(3) 0.041(4) -0.081(5) O(3) 0.120(5) 0.082(4) 0.068(4) -0.033(4) -0.024(4) 0.005(3) O(4) 0.061(3) 0.049(3) 0.054(3) -0.013(2) -0.010(2) -0.019(2) O(5) 0.063(3) 0.063(3) 0.066(3) 0.009(3) -0.005(3) -0.009(3) O(6) 0.083(4) 0.074(3) 0.066(3) -0.014(3) 0.005(3) -0.028(3) O(7) 0.075(3) 0.059(3) 0.069(3) -0.020(3) -0.027(3) -0.021(3) N(1) 0.037(3) 0.046(3) 0.052(3) -0.005(2) 0.000(3) -0.023(3) N(2) 0.055(3) 0.046(3) 0.045(3) -0.010(3) 0.002(3) -0.024(3) C(1) 0.058(5) 0.037(4) 0.087(6) -0.003(3) -0.005(4) -0.027(4) C(2) 0.050(4) 0.050(4) 0.097(6) -0.014(3) 0.006(4) -0.037(4) C(3) 0.073(5) 0.049(4) 0.075(6) -0.026(4) 0.004(4) -0.019(4) C(4) 0.049(4) 0.052(4) 0.055(4) -0.007(3) -0.002(3) -0.022(3) C(5) 0.044(4) 0.068(5) 0.071(5) -0.014(4) 0.001(4) -0.036(4) C(6) 0.058(5) 0.082(5) 0.076(6) -0.038(4) 0.022(4) -0.039(5) C(7) 0.066(5) 0.073(5) 0.057(5) -0.027(4) 0.009(4) -0.015(4) C(8) 0.050(4) 0.062(4) 0.046(4) -0.011(3) 0.005(3) -0.025(4) C(9) 0.060(4) 0.057(4) 0.044(4) -0.021(4) 0.002(3) -0.013(3) C(10) 0.046(4) 0.054(4) 0.048(4) -0.010(3) 0.001(3) -0.023(3) C(11) 0.048(4) 0.041(4) 0.046(4) -0.012(3) 0.001(3) -0.016(3) C(12) 0.051(4) 0.042(4) 0.040(4) -0.008(3) 0.000(3) -0.013(3) C(13) 0.059(4) 0.051(4) 0.076(5) -0.009(3) 0.000(4) -0.030(4) C(14) 0.076(5) 0.049(4) 0.062(5) -0.011(4) 0.000(4) -0.020(4) C(15) 0.064(5) 0.083(6) 0.087(6) 0.016(5) -0.009(5) -0.026(5) C(16) 0.084(6) 0.081(6) 0.070(6) 0.005(5) 0.006(5) -0.005(5) C(19) 0.069(5) 0.074(5) 0.072(5) -0.021(4) -0.007(4) -0.036(4) C(20) 0.076(5) 0.061(4) 0.080(5) -0.023(4) -0.009(4) -0.037(4) C(21) 0.068(5) 0.046(4) 0.053(4) -0.014(3) -0.010(4) -0.021(3) C(22) 0.081(5) 0.054(4) 0.073(5) -0.017(4) -0.019(4) -0.029(4) C(23) 0.081(5) 0.045(4) 0.075(5) -0.010(4) -0.021(4) -0.029(4) #------------------------------------------------------------------------------ _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 ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3037 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0264 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0319 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.496 _refine_ls_shift/esd_max 0.0114 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.58 _refine_diff_density_max 1.16 #------------------------------------------------------------------------------ _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) Cl(1) 2.472(2) ? ? yes Re(1) N(1) 2.174(5) ? ? yes Re(1) N(2) 2.207(5) ? ? yes Re(1) C(1) 1.902(8) ? ? yes Re(1) C(2) 1.937(7) ? ? yes Re(1) C(3) 1.917(8) ? ? yes Se(1) C(16) 1.959(10) ? ? yes Se(1) C(17) 1.96(1) ? ? yes O(1) C(1) 1.157(8) ? ? yes O(2) C(2) 1.111(7) ? ? yes O(3) C(3) 1.149(8) ? ? yes O(4) C(12) 1.385(7) ? ? yes O(4) C(13) 1.425(7) ? ? yes O(5) C(14) 1.408(8) ? ? yes O(5) C(15) 1.428(8) ? ? yes O(6) C(18) 1.36(1) ? ? yes O(6) C(19) 1.408(8) ? ? yes O(7) C(20) 1.424(7) ? ? yes O(7) C(21) 1.371(7) ? ? yes N(1) C(4) 1.344(7) ? ? yes N(1) C(8) 1.358(8) ? ? yes N(2) C(9) 1.259(7) ? ? yes N(2) C(10) 1.441(7) ? ? yes C(4) C(5) 1.369(9) ? ? yes C(5) C(6) 1.361(9) ? ? yes C(6) C(7) 1.393(9) ? ? yes C(7) C(8) 1.373(9) ? ? yes C(8) C(9) 1.452(9) ? ? yes C(10) C(11) 1.402(8) ? ? yes C(10) C(23) 1.365(8) ? ? yes C(11) C(12) 1.368(8) ? ? yes C(12) C(21) 1.400(8) ? ? yes C(13) C(14) 1.498(9) ? ? yes C(15) C(16) 1.49(1) ? ? yes C(17) C(18) 1.16(2) ? ? yes C(19) C(20) 1.504(9) ? ? yes C(21) C(22) 1.384(9) ? ? yes C(22) C(23) 1.378(9) ? ? yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Re(1) N(1) 85.4(1) ? ? ? yes Cl(1) Re(1) N(2) 82.6(1) ? ? ? yes Cl(1) Re(1) C(1) 91.5(2) ? ? ? yes Cl(1) Re(1) C(2) 177.1(2) ? ? ? yes Cl(1) Re(1) C(3) 93.2(2) ? ? ? yes N(1) Re(1) N(2) 74.3(2) ? ? ? yes N(1) Re(1) C(1) 175.3(2) ? ? ? yes N(1) Re(1) C(2) 95.0(2) ? ? ? yes N(1) Re(1) C(3) 96.0(2) ? ? ? yes N(2) Re(1) C(1) 101.8(3) ? ? ? yes N(2) Re(1) C(2) 94.7(3) ? ? ? yes N(2) Re(1) C(3) 169.7(2) ? ? ? yes C(1) Re(1) C(2) 87.9(3) ? ? ? yes C(1) Re(1) C(3) 87.8(3) ? ? ? yes C(2) Re(1) C(3) 89.6(3) ? ? ? yes C(16) Se(1) C(17) 98.3(6) ? ? ? yes C(12) O(4) C(13) 117.1(5) ? ? ? yes C(14) O(5) C(15) 113.0(6) ? ? ? yes C(18) O(6) C(19) 116.3(8) ? ? ? yes C(20) O(7) C(21) 117.6(5) ? ? ? yes Re(1) N(1) C(4) 127.6(4) ? ? ? yes Re(1) N(1) C(8) 115.7(4) ? ? ? yes C(4) N(1) C(8) 116.7(5) ? ? ? yes Re(1) N(2) C(9) 115.3(4) ? ? ? yes Re(1) N(2) C(10) 125.8(4) ? ? ? yes C(9) N(2) C(10) 118.6(5) ? ? ? yes Re(1) C(1) O(1) 177.5(7) ? ? ? yes Re(1) C(2) O(2) 174.5(7) ? ? ? yes Re(1) C(3) O(3) 178.6(7) ? ? ? yes N(1) C(4) C(5) 123.4(6) ? ? ? yes C(4) C(5) C(6) 119.0(6) ? ? ? yes C(5) C(6) C(7) 119.6(6) ? ? ? yes C(6) C(7) C(8) 118.0(7) ? ? ? yes N(1) C(8) C(7) 123.2(6) ? ? ? yes N(1) C(8) C(9) 114.5(6) ? ? ? yes C(7) C(8) C(9) 122.3(6) ? ? ? yes N(2) C(9) C(8) 119.9(6) ? ? ? yes N(2) C(10) C(11) 119.6(5) ? ? ? yes N(2) C(10) C(23) 119.7(6) ? ? ? yes C(11) C(10) C(23) 120.7(6) ? ? ? yes C(10) C(11) C(12) 118.6(5) ? ? ? yes O(4) C(12) C(11) 124.4(5) ? ? ? yes O(4) C(12) C(21) 114.2(5) ? ? ? yes C(11) C(12) C(21) 121.4(5) ? ? ? yes O(4) C(13) C(14) 107.7(5) ? ? ? yes O(5) C(14) C(13) 109.2(6) ? ? ? yes O(5) C(15) C(16) 108.4(7) ? ? ? yes Se(1) C(16) C(15) 114.0(6) ? ? ? yes Se(1) C(17) C(18) 126(1) ? ? ? yes O(6) C(18) C(17) 125(1) ? ? ? yes O(6) C(19) C(20) 112.1(6) ? ? ? yes O(7) C(20) C(19) 106.5(6) ? ? ? yes O(7) C(21) C(12) 115.9(5) ? ? ? yes O(7) C(21) C(22) 125.6(6) ? ? ? yes C(12) C(21) C(22) 118.5(6) ? ? ? yes C(21) C(22) C(23) 120.7(6) ? ? ? yes C(10) C(23) C(22) 120.1(6) ? ? ? yes #------------------------------------------------------------------------------