# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1607 data_triclinic #------------------------------------------------------------------------------ _audit_creation_date '1998-03-18' _audit_creation_method 'by teXsan v1.7' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' J. Chem. Soc., Dalton Trans' _publ_contact_author ; Joseph T. Hupp Department of Chemistry, Northwestern University 2145 Sheridan Road, Evanston, IL 60208, USA ; _publ_contact_letter ; ? ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' (847) 491-3504 ' _publ_contact_author_fax ' (847)491-7713 ' _publ_contact_author_email ' jthupp@chem.nwu.edu ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; A luminescent tricarbonylrhenium(I) complex featuring a flexible "crown ether" ligand. Manipulation of photoexcited state properties via reccognition and binding of small cations. ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. de Meulenaer, J. & Tompa, H. (1965), Acta Cryst. 19, 1014. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1995)' _computing_structure_solution ; 'DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1995)' _computing_publication_material 'teXsan (MSC, 1995)' #------------------------------------------------------------------------------ _cell_length_a 10.312(3) _cell_length_b 12.391(2) _cell_length_c 13.020(3) _cell_angle_alpha 63.94(1) _cell_angle_beta 84.54(2) _cell_angle_gamma 80.56(2) _cell_volume 1474(1) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.9 _cell_measurement_theta_max 11.5 #------------------------------------------------------------------------------ _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 'rectangular' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.34 _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 796.05 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H27 Cl3 N2 O10 Re ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 782.00 _exptl_absorpt_coefficient_mu 4.505 _exptl_absorpt_correction_type ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.383 _exptl_absorpt_correction_T_min 0.205 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 153(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 'scintillation counter' _diffrn_measurement_device 'CAD4' _diffrn_measurement_method \w-\q _diffrn_standards_number 3 _diffrn_standards_interval_count 90 _diffrn_standards_decay_% 0.94 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 -5 -3 4 -2 3 -3 -5 -4 _diffrn_reflns_number 4817 _reflns_number_total 4527 _reflns_number_observed 4527 _reflns_observed_criterion >0.00\s(I) _diffrn_reflns_av_R_equivalents 0.01504 _diffrn_reflns_av_sigmaI/netI 0.020 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 23.95 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01411 _diffrn_orient_matrix_UB_12 0.08318 _diffrn_orient_matrix_UB_13 -0.01322 _diffrn_orient_matrix_UB_21 0.05807 _diffrn_orient_matrix_UB_22 0.00736 _diffrn_orient_matrix_UB_23 -0.06868 _diffrn_orient_matrix_UB_31 -0.08029 _diffrn_orient_matrix_UB_32 0.03538 _diffrn_orient_matrix_UB_33 -0.04921 #------------------------------------------------------------------------------ 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 20 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 4 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 6 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 48 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 54 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ 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_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Re(1) 0.06082(2) 0.36712(2) 0.34284(2) 0.0208(1) 1.000 . Uani d ? Cl(1) -0.0835(2) 0.2640(2) 0.2824(2) 0.0319(5) 1.000 . Uani d ? Cl(2) 0.2000(3) 0.0963(2) 0.1363(3) 0.0630(9) 1.000 . Uani d ? Cl(3A) 0.455(2) 0.137(2) 0.034(2) 0.133(8) 0.500 . Uani d ? Cl(3B) 0.430(2) 0.170(1) -0.017(1) 0.105(5) 0.500 . Uani d ? O(1) 0.4784(6) -0.2031(4) 0.4461(5) 0.034(2) 1.000 . Uani d ? O(2) 0.6087(5) -0.0621(4) 0.3349(5) 0.034(2) 1.000 . Uani d ? O(3) 0.8152(7) -0.0180(5) 0.1530(5) 0.044(2) 1.000 . Uani d ? O(4) 0.7532(5) 0.1843(5) -0.0684(5) 0.034(2) 1.000 . Uani d ? O(5) 0.5886(5) 0.3663(5) -0.2509(4) 0.029(1) 1.000 . Uani d ? O(6) 0.3459(5) 0.5015(5) -0.2147(4) 0.029(1) 1.000 . Uani d ? O(7) 0.4327(6) 0.6438(5) -0.1888(5) 0.035(2) 1.000 . Uani d ? O(8) -0.0880(6) 0.2621(6) 0.5750(5) 0.051(2) 1.000 . Uani d ? O(9) -0.1256(6) 0.6082(5) 0.2776(6) 0.041(2) 1.000 . Uani d ? O(10) 0.2375(6) 0.4654(5) 0.4493(5) 0.041(2) 1.000 . Uani d ? N(1) 0.2094(6) 0.2037(5) 0.3746(5) 0.023(2) 1.000 . Uani d ? N(2) 0.1550(6) 0.4390(5) 0.1656(5) 0.021(2) 1.000 . Uani d ? C(1) 0.3369(7) 0.2172(6) 0.3351(6) 0.024(2) 1.000 . Uani d ? C(2) 0.4319(7) 0.1235(7) 0.3403(6) 0.026(2) 1.000 . Uani d ? C(3) 0.3985(7) 0.0067(6) 0.3927(6) 0.022(2) 1.000 . Uani d ? C(4) 0.2717(8) -0.0106(6) 0.4397(6) 0.027(2) 1.000 . Uani d ? C(5) 0.1793(7) 0.0889(6) 0.4282(6) 0.027(2) 1.000 . Uani d ? C(6) 0.4985(8) -0.0994(7) 0.3956(6) 0.027(2) 1.000 . Uani d ? C(7) 0.7088(9) -0.1537(7) 0.3240(8) 0.036(2) 1.000 . Uani d ? C(8) 0.8316(9) -0.0970(8) 0.2696(7) 0.041(2) 1.000 . Uani d ? C(9) 0.8340(9) 0.1028(8) 0.1208(8) 0.042(3) 1.000 . Uani d ? C(10) 0.8681(9) 0.1614(7) -0.0038(8) 0.041(2) 1.000 . Uani d ? C(11) 0.7857(8) 0.2214(7) -0.1869(7) 0.031(2) 1.000 . Uani d ? C(12) 0.6586(8) 0.2569(7) -0.2513(7) 0.032(2) 1.000 . Uani d ? C(13) 0.4810(8) 0.4140(7) -0.3265(6) 0.031(2) 1.000 . Uani d ? C(14) 0.4149(8) 0.5306(7) -0.3251(6) 0.031(2) 1.000 . Uani d ? C(15) 0.3640(7) 0.5647(7) -0.1589(6) 0.027(2) 1.000 . Uani d ? C(16) 0.2897(7) 0.5198(6) -0.0457(6) 0.022(2) 1.000 . Uani d ? C(17) 0.1965(8) 0.4398(7) -0.0171(7) 0.028(2) 1.000 . Uani d ? C(18) 0.1327(7) 0.4005(7) 0.0896(6) 0.027(2) 1.000 . Uani d ? C(19) 0.2486(8) 0.5156(6) 0.1399(7) 0.029(2) 1.000 . Uani d ? C(20) 0.3140(8) 0.5580(6) 0.0349(6) 0.028(2) 1.000 . Uani d ? C(21) -0.0248(9) 0.2987(7) 0.4887(8) 0.039(2) 1.000 . Uani d ? C(22) -0.0569(8) 0.5149(7) 0.3033(7) 0.029(2) 1.000 . Uani d ? C(23) 0.1769(8) 0.4328(6) 0.4059(6) 0.025(2) 1.000 . Uani d ? C(24) 0.296(1) 0.100(1) 0.018(1) 0.083(5) 1.000 . Uani d ? H(1) 0.3607 0.2966 0.3020 0.029 1.000 . Uiso c ? H(2) 0.5178 0.1381 0.3091 0.031 1.000 . Uiso c ? H(3) 0.2487 -0.0903 0.4794 0.032 1.000 . Uiso c ? H(4) 0.0927 0.0762 0.4586 0.032 1.000 . Uiso c ? H(5) 0.7282 -0.2176 0.3976 0.043 1.000 . Uiso c ? H(6) 0.6780 -0.1849 0.2775 0.043 1.000 . Uiso c ? H(7) 0.9021 -0.1596 0.2766 0.049 1.000 . Uiso c ? H(8) 0.8522 -0.0527 0.3083 0.049 1.000 . Uiso c ? H(9) 0.7554 0.1459 0.1361 0.051 1.000 . Uiso c ? H(10) 0.9035 0.1039 0.1631 0.051 1.000 . Uiso c ? H(11) 0.9344 0.1092 -0.0221 0.049 1.000 . Uiso c ? H(12) 0.8995 0.2359 -0.0223 0.049 1.000 . Uiso c ? H(13) 0.8330 0.2889 -0.2143 0.037 1.000 . Uiso c ? H(14) 0.8381 0.1564 -0.1978 0.037 1.000 . Uiso c ? H(15) 0.6054 0.1937 -0.2154 0.039 1.000 . Uiso c ? H(16) 0.6785 0.2690 -0.3280 0.039 1.000 . Uiso c ? H(17) 0.5124 0.4287 -0.4019 0.037 1.000 . Uiso c ? H(18) 0.4199 0.3574 -0.3023 0.037 1.000 . Uiso c ? H(19) 0.3539 0.5706 -0.3851 0.038 1.000 . Uiso c ? H(20) 0.4788 0.5817 -0.3347 0.038 1.000 . Uiso c ? H(21) 0.1768 0.4124 -0.0707 0.034 1.000 . Uiso c ? H(22) 0.0716 0.3445 0.1084 0.033 1.000 . Uiso c ? H(23) 0.2686 0.5398 0.1958 0.034 1.000 . Uiso c ? H(24) 0.3754 0.6132 0.0180 0.033 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 Re(1) 0.0169(2) 0.0276(2) 0.0139(2) 0.0012(1) 0.0057(1) -0.0080(1) Cl(1) 0.024(1) 0.041(1) 0.028(1) -0.0048(8) 0.0054(8) -0.0130(8) Cl(2) 0.064(2) 0.068(2) 0.068(2) -0.022(1) 0.028(1) -0.040(1) Cl(3A) 0.056(6) 0.24(2) 0.20(2) -0.068(9) 0.06(1) -0.18(2) Cl(3B) 0.11(1) 0.112(7) 0.14(1) -0.083(8) 0.10(1) -0.100(8) O(1) 0.042(3) 0.023(3) 0.030(3) -0.002(2) 0.007(3) -0.008(2) O(2) 0.030(3) 0.027(3) 0.035(3) 0.004(2) 0.010(3) -0.008(2) O(3) 0.063(4) 0.050(3) 0.022(3) -0.019(3) 0.008(3) -0.016(3) O(4) 0.022(3) 0.045(3) 0.030(3) -0.001(2) 0.005(2) -0.013(3) O(5) 0.027(3) 0.039(3) 0.022(3) -0.003(2) 0.006(2) -0.017(2) O(6) 0.034(3) 0.036(3) 0.015(3) -0.007(2) 0.012(2) -0.011(2) O(7) 0.034(3) 0.043(3) 0.027(3) -0.019(3) 0.012(2) -0.011(2) O(8) 0.038(4) 0.069(4) 0.021(3) 0.003(3) 0.014(3) -0.004(3) O(9) 0.031(3) 0.039(3) 0.049(4) 0.011(3) -0.001(3) -0.020(3) O(10) 0.050(4) 0.045(3) 0.025(3) -0.011(3) -0.002(3) -0.012(3) N(1) 0.019(3) 0.027(3) 0.022(3) -0.001(2) 0.005(3) -0.011(3) N(2) 0.018(3) 0.025(3) 0.010(3) 0.006(2) -0.005(2) -0.002(2) C(1) 0.020(4) 0.025(3) 0.021(4) -0.003(3) 0.002(3) -0.005(3) C(2) 0.023(4) 0.031(4) 0.020(4) -0.004(3) 0.002(3) -0.009(3) C(3) 0.023(4) 0.028(4) 0.014(3) 0.001(3) -0.003(3) -0.008(3) C(4) 0.031(4) 0.024(3) 0.021(4) -0.006(3) 0.002(3) -0.005(3) C(5) 0.025(4) 0.026(4) 0.020(4) -0.006(3) 0.010(3) -0.004(3) C(6) 0.029(4) 0.034(4) 0.017(4) 0.003(3) -0.004(3) -0.013(3) C(7) 0.032(5) 0.029(4) 0.034(5) 0.013(3) 0.005(4) -0.008(4) C(8) 0.030(5) 0.060(5) 0.024(4) 0.006(4) -0.001(4) -0.015(4) C(9) 0.045(5) 0.049(5) 0.040(5) 0.003(4) -0.009(4) -0.026(4) C(10) 0.031(5) 0.040(4) 0.042(5) -0.004(4) -0.006(4) -0.009(4) C(11) 0.026(4) 0.038(4) 0.025(4) -0.002(3) 0.012(3) -0.013(3) C(12) 0.031(4) 0.041(4) 0.028(4) -0.006(3) 0.013(3) -0.021(4) C(13) 0.026(4) 0.051(5) 0.018(4) -0.008(3) 0.006(3) -0.018(3) C(14) 0.030(4) 0.044(4) 0.010(4) -0.005(3) 0.008(3) -0.005(3) C(15) 0.020(4) 0.032(4) 0.018(4) 0.004(3) 0.003(3) -0.004(3) C(16) 0.019(4) 0.025(3) 0.013(4) 0.002(3) 0.004(3) -0.002(3) C(17) 0.031(4) 0.034(4) 0.022(4) -0.009(3) 0.008(3) -0.014(3) C(18) 0.025(4) 0.036(4) 0.021(4) -0.010(3) 0.012(3) -0.013(3) C(19) 0.030(4) 0.028(4) 0.030(4) -0.009(3) 0.009(3) -0.014(3) C(20) 0.025(4) 0.032(4) 0.022(4) -0.009(3) 0.002(3) -0.007(3) C(21) 0.030(5) 0.038(4) 0.029(5) 0.012(4) -0.002(4) -0.001(4) C(22) 0.022(4) 0.041(4) 0.020(4) 0.001(3) 0.002(3) -0.014(3) C(23) 0.035(4) 0.023(3) 0.008(3) 0.005(3) 0.011(3) -0.004(3) C(24) 0.09(1) 0.096(9) 0.09(1) -0.039(8) 0.053(8) -0.061(8) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00090|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 4527 _refine_ls_number_parameters 0 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1203 _refine_ls_R_factor_obs ? _refine_ls_wR_factor_all 0.1269 _refine_ls_wR_factor_obs ? _refine_ls_goodness_of_fit_all 1.804 _refine_ls_goodness_of_fit_obs 1.804 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -6.04 _refine_diff_density_max 4.76 #------------------------------------------------------------------------------ _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 RE1 CL1 2.489(2) . . yes RE1 N1 2.233(6) . . yes RE1 N2 2.262(6) . . yes RE1 C21 1.901(9) . . yes RE1 C22 1.912(8) . . yes RE1 C23 1.964(9) . . yes CL2 C24 1.74(1) . . yes CL3A CL3B 0.66(3) . . yes CL3A C24 1.83(2) . . yes CL3B C24 1.67(2) . . yes O1 C6 1.202(9) . . yes O2 C6 1.345(9) . . yes O2 C7 1.450(9) . . yes O3 C8 1.41(1) . . yes O3 C9 1.41(1) . . yes O4 C10 1.44(1) . . yes O4 C11 1.43(1) . . yes O5 C12 1.429(9) . . yes O5 C13 1.426(9) . . yes O6 C14 1.462(9) . . yes O6 C15 1.32(1) . . yes O7 C15 1.206(9) . . yes O8 C21 1.18(1) . . yes O9 C22 1.18(1) . . yes O10 C23 1.11(1) . . yes N1 C1 1.37(1) . . yes N1 C5 1.355(9) . . yes N2 C18 1.32(1) . . yes N2 C19 1.38(1) . . yes C1 C2 1.37(1) . . yes C1 H1 0.95 . . no C2 C3 1.39(1) . . yes C2 H2 0.95 . . no C3 C4 1.40(1) . . yes C3 C6 1.52(1) . . yes C4 C5 1.39(1) . . yes C4 H3 0.95 . . no C5 H4 0.95 . . no C7 C8 1.51(1) . . yes C7 H5 0.95 . . no C7 H6 0.95 . . no C8 H7 0.95 . . no C8 H8 0.95 . . no C9 C10 1.49(1) . . yes C9 H9 0.95 . . no C9 H10 0.95 . . no C10 H11 0.95 . . no C10 H12 0.95 . . no C11 C12 1.52(1) . . yes C11 H13 0.95 . . no C11 H14 0.95 . . no C12 H15 0.95 . . no C12 H16 0.95 . . no C13 C14 1.50(1) . . yes C13 H17 0.95 . . no C13 H18 0.95 . . no C14 H19 0.95 . . no C14 H20 0.95 . . no C15 C16 1.51(1) . . yes C16 C17 1.40(1) . . yes C16 C20 1.38(1) . . yes C17 C18 1.39(1) . . yes C17 H21 0.95 . . no C18 H22 0.95 . . no C19 C20 1.38(1) . . yes C19 H23 0.95 . . no C20 H24 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 CL1 RE1 N1 85.4(2) . . . yes CL1 RE1 N2 89.5(2) . . . yes CL1 RE1 C21 86.1(3) . . . yes CL1 RE1 C22 96.1(2) . . . yes CL1 RE1 C23 173.9(2) . . . yes N1 RE1 N2 83.8(2) . . . yes N1 RE1 C21 95.0(3) . . . yes N1 RE1 C22 174.7(3) . . . yes N1 RE1 C23 91.1(3) . . . yes N2 RE1 C21 175.5(3) . . . yes N2 RE1 C22 91.1(3) . . . yes N2 RE1 C23 95.1(2) . . . yes C21 RE1 C22 90.2(3) . . . yes C21 RE1 C23 89.3(4) . . . yes C22 RE1 C23 87.9(3) . . . yes CL3B CL3A C24 66(2) . . . yes CL3A CL3B C24 93(2) . . . yes C6 O2 C7 117.5(6) . . . yes C8 O3 C9 115.7(7) . . . yes C10 O4 C11 111.2(6) . . . yes C12 O5 C13 112.0(6) . . . yes C14 O6 C15 117.2(6) . . . yes RE1 N1 C1 120.0(4) . . . yes RE1 N1 C5 123.0(5) . . . yes C1 N1 C5 117.0(6) . . . yes RE1 N2 C18 121.9(5) . . . yes RE1 N2 C19 119.0(5) . . . yes C18 N2 C19 118.8(6) . . . yes N1 C1 C2 124.3(6) . . . yes N1 C1 H1 117.8 . . . no C2 C1 H1 117.8 . . . no C1 C2 C3 117.9(7) . . . yes C1 C2 H2 121.0 . . . no C3 C2 H2 121.0 . . . no C2 C3 C4 119.0(6) . . . yes C2 C3 C6 119.9(7) . . . yes C4 C3 C6 121.1(6) . . . yes C3 C4 C5 119.9(6) . . . yes C3 C4 H3 120.1 . . . no C5 C4 H3 120.1 . . . no N1 C5 C4 121.7(7) . . . yes N1 C5 H4 119.1 . . . no C4 C5 H4 119.1 . . . no O1 C6 O2 125.5(7) . . . yes O1 C6 C3 122.8(7) . . . yes O2 C6 C3 111.7(6) . . . yes O2 C7 C8 109.2(6) . . . yes O2 C7 H5 109.6 . . . no O2 C7 H6 109.6 . . . no C8 C7 H5 109.6 . . . no C8 C7 H6 109.6 . . . no H5 C7 H6 109.5 . . . no O3 C8 C7 111.7(7) . . . yes O3 C8 H7 108.9 . . . no O3 C8 H8 108.9 . . . no C7 C8 H7 108.9 . . . no C7 C8 H8 108.9 . . . no H7 C8 H8 109.5 . . . no O3 C9 C10 109.5(7) . . . yes O3 C9 H9 109.5 . . . no O3 C9 H10 109.5 . . . no C10 C9 H9 109.5 . . . no C10 C9 H10 109.5 . . . no H9 C9 H10 109.5 . . . no O4 C10 C9 109.4(7) . . . yes O4 C10 H11 109.5 . . . no O4 C10 H12 109.5 . . . no C9 C10 H11 109.5 . . . no C9 C10 H12 109.5 . . . no H11 C10 H12 109.5 . . . no O4 C11 C12 108.3(6) . . . yes O4 C11 H13 109.8 . . . no O4 C11 H14 109.8 . . . no C12 C11 H13 109.8 . . . no C12 C11 H14 109.8 . . . no H13 C11 H14 109.5 . . . no O5 C12 C11 110.3(6) . . . yes O5 C12 H15 109.3 . . . no O5 C12 H16 109.3 . . . no C11 C12 H15 109.3 . . . no C11 C12 H16 109.3 . . . no H15 C12 H16 109.5 . . . no O5 C13 C14 109.3(6) . . . yes O5 C13 H17 109.5 . . . no O5 C13 H18 109.5 . . . no C14 C13 H17 109.5 . . . no C14 C13 H18 109.5 . . . no H17 C13 H18 109.5 . . . no O6 C14 C13 108.0(6) . . . yes O6 C14 H19 109.8 . . . no O6 C14 H20 109.8 . . . no C13 C14 H19 109.8 . . . no C13 C14 H20 109.8 . . . no H19 C14 H20 109.5 . . . no O6 C15 O7 127.0(7) . . . yes O6 C15 C16 109.9(6) . . . yes O7 C15 C16 123.1(7) . . . yes C15 C16 C17 123.2(7) . . . yes C15 C16 C20 119.2(6) . . . yes C17 C16 C20 117.6(7) . . . yes C16 C17 C18 120.3(7) . . . yes C16 C17 H21 119.9 . . . no C18 C17 H21 119.9 . . . no N2 C18 C17 121.7(7) . . . yes N2 C18 H22 119.2 . . . no C17 C18 H22 119.2 . . . no N2 C19 C20 121.6(7) . . . yes N2 C19 H23 119.2 . . . no C20 C19 H23 119.2 . . . no C16 C20 C19 119.8(7) . . . yes C16 C20 H24 120.1 . . . no C19 C20 H24 120.1 . . . no RE1 C21 O8 174.2(7) . . . yes RE1 C22 O9 177.6(7) . . . yes RE1 C23 O10 174.6(6) . . . yes CL2 C24 CL3A 106(1) . . . yes CL2 C24 CL3B 119.4(9) . . . yes CL3A C24 CL3B 21(1) . . . yes #------------------------------------------------------------------------------ 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 CL1 C15 3.367(8) . 2_565 no CL1 O6 3.488(6) . 2_565 no CL2 C18 3.502(8) . . no CL3A O4 3.27(2) . . no CL3B O4 3.35(2) . . no CL3B O5 3.42(1) . . no CL3B C12 3.55(2) . . no O1 C12 3.37(1) . 2_655 no O1 C14 3.448(9) . 1_546 no O1 C1 3.501(9) . 2_656 no O1 C13 3.539(9) . 2_655 no O1 C2 3.571(9) . 2_656 no O3 C24 3.19(2) . 2_655 no O4 C20 3.363(9) . 2_665 no O4 C24 3.41(1) . 2_655 no O4 C19 3.411(9) . 2_665 no O5 O10 3.138(8) . 2_665 no O5 C19 3.189(9) . 2_665 no O5 C23 3.571(9) . 2_665 no O6 O9 3.165(8) . 2_565 no O6 C22 3.36(1) . 2_565 no O7 C1 3.137(9) . 2_665 no O7 C2 3.155(9) . 2_665 no O7 C20 3.40(1) . 2_665 no O7 C19 3.50(1) . 2_665 no O8 C11 3.10(1) . 1_456 no O8 C12 3.28(1) . 1_456 no O8 C8 3.30(1) . 2_656 no O8 O10 3.365(9) . 2_566 no O9 O10 3.395(9) . 2_566 no O9 C7 3.42(1) . 1_465 no O9 C14 3.55(1) . 2_565 no O9 C8 3.56(1) . 1_465 no O10 C13 3.41(1) . 2_665 no O10 C12 3.54(1) . 2_665 no C2 C6 3.45(1) . 2_656 no C3 C3 3.58(1) . 2_656 no C8 C21 3.57(1) . 2_656 no C10 C20 3.54(1) . 2_665 no C11 C19 3.53(1) . 2_665 no #------------------------------------------------------------------------------ #=END data_monoclinic #------------------------------------------------------------------------------ _audit_creation_date '1998-12-04' _audit_creation_method 'by teXsan v1.7' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. SMART and SAINT-Pus Versions 5.101. Data collection and processing Software for the SMART system. (1997) Bruker ANalytical X-ray instruments Inc., Madison, Wisconsin, USA. ; #------------------------------------------------------------------------------ _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1995)' _computing_publication_material 'teXsan (MSC, 1995)' #------------------------------------------------------------------------------ _cell_length_a 14.8661(11) _cell_length_b 16.9066(12) _cell_length_c 11.6709(8) _cell_angle_alpha 90 _cell_angle_beta 111.654(1) _cell_angle_gamma 90 _cell_volume 2726.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(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/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 'long plates' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.246 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.036 _exptl_crystal_density_diffrn 1.769 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 726.11 _chemical_formula_analytical ? _chemical_formula_sum 'C23 H24 Cl N2 O11 Re ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1424.00 _exptl_absorpt_coefficient_mu 4.617 _exptl_absorpt_correction_type 'integration' _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD detector' _diffrn_measurement_method 'psi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25150 _reflns_number_total 6757 _reflns_number_observed 6534 _reflns_observed_criterion >0.00\s(I) _diffrn_reflns_av_R_equivalents 0.05612 _diffrn_reflns_av_sigmaI/netI 0.050 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 28.24 _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 92 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 96 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 44 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 4 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Re 0 4 -1.018 7.231 ;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_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Re(1) 0.13453(1) 0.66268(1) 0.16343(2) 0.02722(4) 1.000 . Uani d ? Cl(1a) 0.1127(2) 0.7938(2) 0.2380(2) 0.0343(6) 0.600 . Uani d ? Cl(1b) 0.1387(4) 0.5317(3) 0.0849(5) 0.032(1) 0.400 . Uani d ? O(1) -0.1306(3) 0.5678(2) 0.5486(3) 0.053(1) 1.000 . Uani d ? O(2) -0.2163(3) 0.4986(2) 0.3785(3) 0.049(1) 1.000 . Uani d ? O(3) -0.4228(3) 0.5358(4) 0.2795(5) 0.118(2) 1.000 . Uani d ? O(4) -0.5665(3) 0.5936(3) 0.0582(4) 0.073(1) 1.000 . Uani d ? O(5) -0.5352(3) 0.6644(3) -0.1637(5) 0.081(2) 1.000 . Uani d ? O(6) -0.3625(3) 0.7111(3) -0.2079(3) 0.067(1) 1.000 . Uani d ? O(7) -0.3151(3) 0.6806(3) -0.3657(4) 0.101(2) 1.000 . Uani d ? O(8) 0.3290(2) 0.6329(2) 0.3730(3) 0.0400(9) 1.000 . Uani d ? O(9) 0.2544(2) 0.7408(2) 0.0291(3) 0.040(1) 1.000 . Uani d ? O(10b) 0.1267(6) 0.8321(5) 0.2644(7) 0.031(2) 0.400 D Uiso d ? O(10a) 0.1583(6) 0.5044(4) 0.0576(7) 0.048(2) 0.600 . Uani d ? O(11b) -0.274(1) 0.5715(9) 0.015(2) 0.040(5) 0.200 . Uani d ? O(11a) -0.3364(8) 0.6294(7) 0.126(1) 0.110(5) 0.500 . Uani d ? O(11c) -0.280(1) 0.652(1) 0.203(2) 0.101(7) 0.300 . Uani d ? N(1) 0.0482(3) 0.6123(2) 0.2635(3) 0.030(1) 1.000 . Uani d ? N(2) -0.0105(3) 0.6793(2) 0.0180(3) 0.0306(9) 1.000 . Uani d ? C(1) -0.0235(4) 0.5600(3) 0.2119(4) 0.036(1) 1.000 . Uani d ? C(2) -0.0878(3) 0.5353(3) 0.2663(4) 0.038(1) 1.000 . Uani d ? C(3) -0.0760(3) 0.5635(3) 0.3811(4) 0.032(1) 1.000 . Uani d ? C(4) -0.0009(4) 0.6150(3) 0.4387(4) 0.034(1) 1.000 . Uani d ? C(5) 0.0600(3) 0.6390(3) 0.3787(4) 0.035(1) 1.000 . Uani d ? C(6) -0.1432(4) 0.5442(3) 0.4461(4) 0.038(1) 1.000 . Uani d ? C(7) -0.2874(5) 0.4785(5) 0.4327(6) 0.095(3) 1.000 . Uani d ? C(8) -0.3639(5) 0.5371(6) 0.4073(7) 0.115(3) 1.000 . Uani d ? C(9) -0.5193(4) 0.5318(4) 0.2510(7) 0.074(2) 1.000 . Uani d ? C(10) -0.5764(5) 0.5247(5) 0.1151(8) 0.088(2) 1.000 . Uani d ? C(11) -0.6311(5) 0.5948(4) -0.0696(7) 0.069(2) 1.000 . Uani d ? C(12) -0.6173(4) 0.6680(4) -0.1279(6) 0.067(2) 1.000 . Uani d ? C(13) -0.5242(4) 0.7356(4) -0.2208(6) 0.071(2) 1.000 . Uani d ? C(14) -0.4625(4) 0.7208(5) -0.2931(6) 0.084(2) 1.000 . Uani d ? C(15) -0.2969(4) 0.6931(4) -0.2567(5) 0.067(2) 1.000 . Uani d ? C(16) -0.1969(4) 0.6914(3) -0.1616(4) 0.045(1) 1.000 . Uani d ? C(17) -0.1766(4) 0.7183(3) -0.0430(4) 0.042(1) 1.000 . Uani d ? C(18) -0.0839(3) 0.7125(3) 0.0421(4) 0.038(1) 1.000 . Uani d ? C(19) -0.0310(3) 0.6545(3) -0.0993(4) 0.031(1) 1.000 . Uani d ? C(20) -0.1221(3) 0.6579(3) -0.1904(4) 0.039(1) 1.000 . Uani d ? C(21) 0.2563(3) 0.6453(2) 0.2955(4) 0.030(1) 1.000 . Uani d ? C(22) 0.2079(3) 0.7103(3) 0.0758(4) 0.031(1) 1.000 . Uani d ? C(23a) 0.147(1) 0.5632(7) 0.097(2) 0.038(3) 0.600 . Uani d ? C(23b) 0.128(1) 0.7654(5) 0.225(1) 0.038(4) 0.400 D Uiso d ? H(1) -0.3159 0.4290 0.4002 0.115 1.000 . Uiso c ? H(2) -0.2552 0.4741 0.5193 0.115 1.000 . Uiso c ? H(3) -0.3360 0.5880 0.4293 0.139 1.000 . Uiso c ? H(4) -0.4025 0.5252 0.4543 0.139 1.000 . Uiso c ? H(5) -0.5327 0.4870 0.2910 0.088 1.000 . Uiso c ? H(6) -0.5393 0.5785 0.2800 0.088 1.000 . Uiso c ? H(7) -0.6427 0.5161 0.1017 0.105 1.000 . Uiso c ? H(8) -0.5527 0.4814 0.0826 0.105 1.000 . Uiso c ? H(9) -0.6177 0.5506 -0.1109 0.083 1.000 . Uiso c ? H(10) -0.6962 0.5918 -0.0740 0.083 1.000 . Uiso c ? H(11) -0.6086 0.7103 -0.0715 0.080 1.000 . Uiso c ? H(12) -0.6735 0.6773 -0.1991 0.080 1.000 . Uiso c ? H(13) -0.5860 0.7539 -0.2740 0.086 1.000 . Uiso c ? H(14) -0.4948 0.7745 -0.1598 0.086 1.000 . Uiso c ? H(15) -0.4666 0.7642 -0.3462 0.102 1.000 . Uiso c ? H(16) -0.4834 0.6740 -0.3407 0.102 1.000 . Uiso c ? H(17) -0.0306 0.5385 0.1340 0.043 1.000 . Uiso c ? H(18) -0.1389 0.5000 0.2246 0.045 1.000 . Uiso c ? H(19) 0.0092 0.6341 0.5189 0.041 1.000 . Uiso c ? H(20) 0.1110 0.6750 0.4188 0.041 1.000 . Uiso c ? H(21) -0.2264 0.7402 -0.0204 0.050 1.000 . Uiso c ? H(22) -0.0709 0.7333 0.1221 0.046 1.000 . Uiso c ? H(23) 0.0204 0.6334 -0.1198 0.038 1.000 . Uiso c ? H(24) -0.1334 0.6379 -0.2705 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 Re(1) 0.02385(9) 0.0341(1) 0.02436(8) -0.00136(9) 0.00961(6) -0.00108(9) Cl(1a) 0.033(1) 0.044(1) 0.026(1) -0.004(1) 0.0115(9) -0.001(1) Cl(1b) 0.042(2) 0.030(2) 0.026(2) 0.005(3) 0.014(2) -0.011(2) O(1) 0.049(2) 0.085(3) 0.033(2) 0.005(2) 0.026(2) 0.002(2) O(2) 0.044(2) 0.068(3) 0.039(2) -0.010(2) 0.022(2) 0.004(2) O(3) 0.038(2) 0.248(7) 0.078(3) -0.013(4) 0.031(2) -0.064(4) O(4) 0.053(3) 0.066(3) 0.097(3) 0.010(2) 0.025(2) 0.002(2) O(5) 0.048(3) 0.084(3) 0.127(4) 0.021(3) 0.051(3) 0.024(3) O(6) 0.025(2) 0.124(4) 0.044(2) 0.002(2) 0.005(2) -0.004(2) O(7) 0.053(3) 0.191(6) 0.045(2) 0.023(3) 0.004(2) -0.033(3) O(8) 0.030(2) 0.052(2) 0.035(2) 0.005(2) 0.008(1) 0.007(2) O(9) 0.032(2) 0.057(2) 0.036(2) 0.000(2) 0.019(1) 0.011(2) O(10a) 0.048(5) 0.039(4) 0.044(5) -0.015(4) 0.004(3) -0.016(3) O(11b) 0.018(8) 0.033(9) 0.06(1) 0.001(7) 0.008(8) -0.002(8) O(11a) 0.054(7) 0.094(8) 0.19(1) -0.024(6) 0.061(8) -0.050(9) O(11c) 0.06(1) 0.08(1) 0.14(2) 0.054(9) 0.010(8) 0.04(1) N(1) 0.030(2) 0.038(2) 0.024(2) -0.004(2) 0.012(1) -0.005(1) N(2) 0.023(2) 0.042(2) 0.028(2) -0.005(2) 0.011(1) -0.006(2) C(1) 0.038(3) 0.047(3) 0.024(2) -0.016(2) 0.013(2) -0.013(2) C(2) 0.035(3) 0.052(3) 0.029(2) -0.016(2) 0.014(2) -0.007(2) C(3) 0.031(2) 0.041(3) 0.028(2) 0.000(2) 0.014(2) 0.004(2) C(4) 0.038(3) 0.042(3) 0.025(2) 0.002(2) 0.014(2) -0.004(2) C(5) 0.034(3) 0.046(3) 0.022(2) -0.002(2) 0.008(2) -0.007(2) C(6) 0.040(3) 0.049(3) 0.032(2) 0.006(2) 0.020(2) 0.011(2) C(7) 0.075(5) 0.169(7) 0.065(4) -0.057(4) 0.054(4) 0.001(5) C(8) 0.055(4) 0.23(1) 0.076(3) -0.023(5) 0.046(3) -0.044(6) C(9) 0.041(3) 0.079(5) 0.110(4) 0.004(3) 0.039(3) 0.020(4) C(10) 0.041(4) 0.090(5) 0.114(5) 0.007(4) 0.008(4) 0.040(4) C(11) 0.045(4) 0.072(4) 0.093(4) 0.002(3) 0.031(3) -0.015(3) C(12) 0.047(3) 0.082(4) 0.072(4) 0.005(4) 0.025(3) -0.007(3) C(13) 0.039(4) 0.095(5) 0.077(5) 0.008(4) 0.019(3) 0.011(4) C(14) 0.032(3) 0.144(7) 0.058(4) 0.010(4) -0.006(2) 0.004(4) C(15) 0.031(2) 0.121(6) 0.044(2) -0.002(3) 0.007(2) -0.018(3) C(16) 0.029(2) 0.068(4) 0.034(2) 0.008(2) 0.007(2) 0.000(2) C(17) 0.030(2) 0.062(3) 0.037(2) 0.008(3) 0.015(2) -0.006(2) C(18) 0.027(2) 0.062(3) 0.029(2) -0.001(2) 0.014(2) -0.010(2) C(19) 0.029(2) 0.045(3) 0.026(2) -0.003(2) 0.016(2) -0.004(2) C(20) 0.037(2) 0.055(3) 0.024(2) 0.002(2) 0.011(2) -0.007(2) C(21) 0.031(2) 0.029(2) 0.035(2) 0.004(2) 0.019(1) 0.004(2) C(22) 0.020(2) 0.046(3) 0.024(2) 0.008(2) 0.005(2) -0.001(2) C(23a) 0.038(6) 0.034(6) 0.039(7) 0.007(7) 0.008(5) 0.003(6) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme '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 6534 _refine_ls_number_parameters 0 _refine_ls_number_restraints 2 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_obs ? _refine_ls_wR_factor_all 0.0830 _refine_ls_wR_factor_obs ? _refine_ls_goodness_of_fit_all 1.428 _refine_ls_goodness_of_fit_obs 1.428 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean 0.0220 _refine_diff_density_min -1.46 _refine_diff_density_max 2.05 #------------------------------------------------------------------------------ _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(1a) 2.447(3) . . yes Re(1) Cl(1b) 2.406(5) . . yes Re(1) N(1) 2.203(4) . . yes Re(1) N(2) 2.216(4) . . yes Re(1) C(21) 1.919(6) . . yes Re(1) C(22) 1.927(6) . . yes Re(1) C(23a) 1.89(1) . . yes Re(1) C(23b) 1.896(8) . . yes Cl(1a) O(10b) 0.716(8) . . yes Cl(1a) C(23b) 0.57(1) . . yes Cl(1b) O(10a) 0.685(8) . . yes Cl(1b) C(23a) 0.55(1) . . yes O(1) C(6) 1.210(6) . . yes O(2) C(6) 1.329(7) . . yes O(2) C(7) 1.460(7) . . yes O(3) C(8) 1.43(1) . . yes O(3) C(9) 1.348(8) . . yes O(4) C(10) 1.377(9) . . yes O(4) C(11) 1.447(9) . . yes O(5) C(12) 1.430(8) . . yes O(5) C(13) 1.415(9) . . yes O(6) C(14) 1.461(8) . . yes O(6) C(15) 1.334(8) . . yes O(7) C(15) 1.219(8) . . yes O(8) C(21) 1.145(6) . . yes O(9) C(22) 1.149(6) . . yes O(10b) C(23b) 1.221(8) . . yes O(10a) C(23a) 1.13(1) . . yes O(11a) O(11c) 1.06(2) . . yes N(1) C(1) 1.345(7) . . yes N(1) C(5) 1.369(6) . . yes N(2) C(18) 1.347(7) . . yes N(2) C(19) 1.356(6) . . yes C(1) C(2) 1.392(7) . . yes C(1) H(17) 0.95 . . no C(2) C(3) 1.373(7) . . yes C(2) H(18) 0.95 . . no C(3) C(4) 1.380(8) . . yes C(3) C(6) 1.498(7) . . yes C(4) C(5) 1.394(7) . . yes C(4) H(19) 0.95 . . no C(5) H(20) 0.95 . . no C(7) C(8) 1.45(1) . . yes C(7) H(1) 0.95 . . no C(7) H(2) 0.95 . . no C(8) H(3) 0.95 . . no C(8) H(4) 0.95 . . no C(9) C(10) 1.50(1) . . yes C(9) H(5) 0.95 . . no C(9) H(6) 0.95 . . no C(10) H(7) 0.95 . . no C(10) H(8) 0.95 . . no C(11) C(12) 1.46(1) . . yes C(11) H(9) 0.95 . . no C(11) H(10) 0.95 . . no C(12) H(11) 0.95 . . no C(12) H(12) 0.95 . . no C(13) C(14) 1.48(1) . . yes C(13) H(13) 0.95 . . no C(13) H(14) 0.95 . . no C(14) H(15) 0.95 . . no C(14) H(16) 0.95 . . no C(15) C(16) 1.493(8) . . yes C(16) C(17) 1.383(8) . . yes C(16) C(20) 1.395(8) . . yes C(17) C(18) 1.373(8) . . yes C(17) H(21) 0.95 . . no C(18) H(22) 0.95 . . no C(19) C(20) 1.381(7) . . yes C(19) H(23) 0.95 . . no C(20) H(24) 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 Cl(1a) Re(1) Cl(1b) 174.2(2) . . . yes Cl(1a) Re(1) N(1) 88.9(1) . . . yes Cl(1a) Re(1) N(2) 86.5(1) . . . yes Cl(1a) Re(1) C(21) 93.6(2) . . . yes Cl(1a) Re(1) C(22) 89.2(2) . . . yes Cl(1a) Re(1) C(23a) 176.9(7) . . . yes Cl(1a) Re(1) C(23b) 4.3(7) . . . yes Cl(1b) Re(1) N(1) 87.1(2) . . . yes Cl(1b) Re(1) N(2) 88.8(2) . . . yes Cl(1b) Re(1) C(21) 90.9(2) . . . yes Cl(1b) Re(1) C(22) 94.7(2) . . . yes Cl(1b) Re(1) C(23a) 5.5(7) . . . yes Cl(1b) Re(1) C(23b) 178.5(6) . . . yes N(1) Re(1) N(2) 82.2(2) . . . yes N(1) Re(1) C(21) 94.3(2) . . . yes N(1) Re(1) C(22) 177.9(2) . . . yes N(1) Re(1) C(23a) 92.4(6) . . . yes N(1) Re(1) C(23b) 91.8(6) . . . yes N(2) Re(1) C(21) 176.5(2) . . . yes N(2) Re(1) C(22) 96.9(2) . . . yes N(2) Re(1) C(23a) 90.9(7) . . . yes N(2) Re(1) C(23b) 90.1(6) . . . yes C(21) Re(1) C(22) 86.6(2) . . . yes C(21) Re(1) C(23a) 89.2(7) . . . yes C(21) Re(1) C(23b) 90.1(6) . . . yes C(22) Re(1) C(23a) 89.4(6) . . . yes C(22) Re(1) C(23b) 86.4(6) . . . yes C(23a) Re(1) C(23b) 175.8(8) . . . yes Re(1) Cl(1a) O(10b) 156.7(9) . . . yes Re(1) Cl(1a) C(23b) 15(2) . . . yes O(10b) Cl(1a) C(23b) 142(2) . . . yes Re(1) Cl(1b) O(10a) 151(1) . . . yes Re(1) Cl(1b) C(23a) 19(2) . . . yes O(10a) Cl(1b) C(23a) 132(3) . . . yes C(6) O(2) C(7) 116.2(5) . . . yes C(8) O(3) C(9) 116.5(7) . . . yes C(10) O(4) C(11) 111.3(7) . . . yes C(12) O(5) C(13) 111.2(6) . . . yes C(14) O(6) C(15) 117.0(6) . . . yes Cl(1a) O(10b) C(23b) 17(1) . . . yes Cl(1b) O(10a) C(23a) 21(1) . . . yes Re(1) N(1) C(1) 122.4(3) . . . yes Re(1) N(1) C(5) 120.4(4) . . . yes C(1) N(1) C(5) 116.9(5) . . . yes Re(1) N(2) C(18) 121.7(3) . . . yes Re(1) N(2) C(19) 121.9(3) . . . yes C(18) N(2) C(19) 116.3(5) . . . yes N(1) C(1) C(2) 123.8(5) . . . yes N(1) C(1) H(17) 118.1 . . . no C(2) C(1) H(17) 118.1 . . . no C(1) C(2) C(3) 118.7(5) . . . yes C(1) C(2) H(18) 120.6 . . . no C(3) C(2) H(18) 120.6 . . . no C(2) C(3) C(4) 119.0(5) . . . yes C(2) C(3) C(6) 123.5(5) . . . yes C(4) C(3) C(6) 117.5(5) . . . yes C(3) C(4) C(5) 119.8(5) . . . yes C(3) C(4) H(19) 120.0 . . . no C(5) C(4) H(19) 120.2 . . . no N(1) C(5) C(4) 121.8(5) . . . yes N(1) C(5) H(20) 119.1 . . . no C(4) C(5) H(20) 119.1 . . . no O(1) C(6) O(2) 125.1(6) . . . yes O(1) C(6) C(3) 122.8(6) . . . yes O(2) C(6) C(3) 112.1(5) . . . yes O(2) C(7) C(8) 112.9(8) . . . yes O(2) C(7) H(1) 108.5 . . . no O(2) C(7) H(2) 108.6 . . . no C(8) C(7) H(1) 108.6 . . . no C(8) C(7) H(2) 108.7 . . . no H(1) C(7) H(2) 109.4 . . . no O(3) C(8) C(7) 109.6(8) . . . yes O(3) C(8) H(3) 109.7 . . . no O(3) C(8) H(4) 109.5 . . . no C(7) C(8) H(3) 109.4 . . . no C(7) C(8) H(4) 109.2 . . . no H(3) C(8) H(4) 109.5 . . . no O(3) C(9) C(10) 113.6(7) . . . yes O(3) C(9) H(5) 108.4 . . . no O(3) C(9) H(6) 108.4 . . . no C(10) C(9) H(5) 108.5 . . . no C(10) C(9) H(6) 108.4 . . . no H(5) C(9) H(6) 109.6 . . . no O(4) C(10) C(9) 108.9(8) . . . yes O(4) C(10) H(7) 109.8 . . . no O(4) C(10) H(8) 109.7 . . . no C(9) C(10) H(7) 109.5 . . . no C(9) C(10) H(8) 109.6 . . . no H(7) C(10) H(8) 109.4 . . . no O(4) C(11) C(12) 109.9(7) . . . yes O(4) C(11) H(9) 109.3 . . . no O(4) C(11) H(10) 109.3 . . . no C(12) C(11) H(9) 109.6 . . . no C(12) C(11) H(10) 109.5 . . . no H(9) C(11) H(10) 109.3 . . . no O(5) C(12) C(11) 112.4(6) . . . yes O(5) C(12) H(11) 108.8 . . . no O(5) C(12) H(12) 108.7 . . . no C(11) C(12) H(11) 108.7 . . . no C(11) C(12) H(12) 108.6 . . . no H(11) C(12) H(12) 109.5 . . . no O(5) C(13) C(14) 109.2(7) . . . yes O(5) C(13) H(13) 109.5 . . . no O(5) C(13) H(14) 109.6 . . . no C(14) C(13) H(13) 109.5 . . . no C(14) C(13) H(14) 109.6 . . . no H(13) C(13) H(14) 109.4 . . . no O(6) C(14) C(13) 108.5(6) . . . yes O(6) C(14) H(15) 109.7 . . . no O(6) C(14) H(16) 109.7 . . . no C(13) C(14) H(15) 109.8 . . . no C(13) C(14) H(16) 109.6 . . . no H(15) C(14) H(16) 109.5 . . . no O(6) C(15) O(7) 124.8(6) . . . yes O(6) C(15) C(16) 111.7(6) . . . yes O(7) C(15) C(16) 123.4(7) . . . yes C(15) C(16) C(17) 122.0(6) . . . yes C(15) C(16) C(20) 119.5(6) . . . yes C(17) C(16) C(20) 118.5(5) . . . yes C(16) C(17) C(18) 119.5(5) . . . yes C(16) C(17) H(21) 120.2 . . . no C(18) C(17) H(21) 120.3 . . . no N(2) C(18) C(17) 123.5(5) . . . yes N(2) C(18) H(22) 118.3 . . . no C(17) C(18) H(22) 118.2 . . . no N(2) C(19) C(20) 123.9(5) . . . yes N(2) C(19) H(23) 118.0 . . . no C(20) C(19) H(23) 118.1 . . . no C(16) C(20) C(19) 118.2(5) . . . yes C(16) C(20) H(24) 121.0 . . . no C(19) C(20) H(24) 120.8 . . . no Re(1) C(21) O(8) 178.1(5) . . . yes Re(1) C(22) O(9) 176.4(5) . . . yes Re(1) C(23a) Cl(1b) 155(3) . . . yes Re(1) C(23a) O(10a) 178(2) . . . yes Cl(1b) C(23a) O(10a) 27(2) . . . yes Re(1) C(23b) Cl(1a) 161(3) . . . yes Re(1) C(23b) O(10b) 178(2) . . . yes Cl(1a) C(23b) O(10b) 21(1) . . . yes