# ja9829867.cif data_S39f #------------------------------------------------------------------------------ _audit_creation_date '1997-10-26' _audit_creation_method 'by teXsan v1.7' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' ?' _publ_contact_author ; Joseph T. Hupp Department of Chemistry Northwester University 2145 Sheridan Road Evanston, IL 60208 ; _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 ' Suzanne Belanger ' ; Department of Chemistry Northwester University 2145 Sheridan Road Evanston, IL 60208 ; ' Joseph T. Hupp ' ; Department of Chemistry Northwester University 2145 Sheridan Road Evanston, IL 60208 ; ' Charlotte L. Stern ' ; Department of Chemistry Northwester University 2145 Sheridan Road Evanston, IL 60208 ; ' Robert V. Slone ' ; Department of Chemistry Northwester University 2145 Sheridan Road Evanston, IL 60208 ; ' David F. Watson ' ; Department of Chemistry Northwester University 2145 Sheridan Road Evanston, IL 60208 ; ' Tomas M. Carrell ' ; Department of Chemistry Northwester University 2145 Sheridan Road Evanston, IL 60208 ; _publ_section_title ; Thin-Film Molecular Materials Based on Tetrametallic "Squares": Nanoscale Porosity and Size Selective Guest Transport Characteristics. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1995)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1995)' _computing_publication_material 'teXsan (MSC, 1995)' #------------------------------------------------------------------------------ _cell_length_a 22.72(2) _cell_length_b 22.72(2) _cell_length_c 13.54(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6986(6) _cell_formula_units_Z 4 _cell_measurement_temperature 153.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.0 _cell_measurement_theta_max 11.8 #------------------------------------------------------------------------------ _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I -4 ' _symmetry_Int_Tables_number 82 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, +y, +z' ' -x, -y, +z' ' -x, -y, +z' ' +y, -x, -z' ' +y, -x, -z' ' -y, +x, -z' ' -y, +x, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'equidimens' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1847.51 _chemical_formula_analytical ? _chemical_formula_sum 'C52 H32 Cl4 N8 O12 Re4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 3456.00 _exptl_absorpt_coefficient_mu 7.118 _exptl_absorpt_correction_type ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.498 _exptl_absorpt_correction_T_min 0.379 _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 _diffrn_standards_number 3 _diffrn_standards_interval_count 90 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -4 0 -6 5 -6 -5 -2 -11 -1 _diffrn_reflns_number 3385 _reflns_number_total 3266 _reflns_number_observed 2164 _reflns_observed_criterion >3.00\s(I) _diffrn_reflns_av_R_equivalents 0.06711 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.03780 _diffrn_orient_matrix_UB_12 -0.02173 _diffrn_orient_matrix_UB_13 0.01005 _diffrn_orient_matrix_UB_21 0.00620 _diffrn_orient_matrix_UB_22 0.00115 _diffrn_orient_matrix_UB_23 0.07310 _diffrn_orient_matrix_UB_31 -0.02160 _diffrn_orient_matrix_UB_32 0.03830 _diffrn_orient_matrix_UB_33 0.00340 #------------------------------------------------------------------------------ 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 16 -1.018 7.231 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 32 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 208 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 48 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 16 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 128 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) 0.2884(1) 0.58014(4) -0.4778(1) 0.0226(3) 1.00000000 . Uani d ? Re(2) 0.2807(1) 0.62732(4) 0.0352(1) 0.0244(3) 1.00000000 . Uani d ? Cl(1) 0.2172(3) 0.5342(3) -0.595(1) 0.034(2) 1.00000000 . Uani d ? Cl(2) 0.2008(3) 0.6168(3) -0.088(1) 0.035(2) 1.00000000 . Uani d ? O(1) 0.310(1) 0.682(1) -0.620(2) 0.06(1) 1.00000000 . Uani d ? O(2) 0.392(1) 0.508(1) -0.571(2) 0.09(1) 1.00000000 . Uani d ? O(3) 0.377(1) 0.627(1) -0.336(1) 0.04(1) 1.00000000 . Uiso d ? O(4) 0.371(1) 0.574(1) -0.105(2) 0.07(1) 1.00000000 . Uani d ? O(5) 0.312(1) 0.749(1) -0.051(2) 0.07(1) 1.00000000 . Uani d ? O(6) 0.375(1) 0.645(1) 0.190(2) 0.05(1) 1.00000000 . Uani d ? O(7) -0.072469003 0.511146009 -0.018531000 0.18(1) 1.00000000 . Uiso c ? N(1) 0.261(1) 0.510(1) -0.373(2) 0.03(1) 1.00000000 . Uiso d ? N(2) 0.217(1) 0.633(1) -0.409(2) 0.03(1) 1.00000000 . Uiso d ? N(3) 0.253(1) 0.539(1) 0.099(1) 0.02(1) 1.00000000 . Uiso d ? N(4) 0.212(1) 0.661(1) 0.135(1) 0.02(1) 1.00000000 . Uiso d ? C(1) 0.252(1) 0.454(1) -0.404(2) 0.02(1) 1.00000000 . Uiso d ? C(2) 0.228(1) 0.412(1) -0.344(2) 0.02(1) 1.00000000 . Uiso d ? C(3) 0.217(1) 0.423(1) -0.252(2) 0.02(1) 1.00000000 . Uiso d ? C(4) 0.224(1) 0.479(1) -0.215(2) 0.03(1) 1.00000000 . Uiso d ? C(5) 0.250(1) 0.519(1) -0.277(2) 0.03(1) 1.00000000 . Uiso d ? C(6) 0.157(1) 0.617(1) -0.421(2) 0.03(1) 1.00000000 . Uiso d ? C(7) 0.111(1) 0.643(1) -0.373(2) 0.03(1) 1.00000000 . Uiso d ? C(8) 0.123(1) 0.690(1) -0.307(2) 0.01(1) 1.00000000 . Uiso d ? C(9) 0.183(1) 0.705(1) -0.301(2) 0.03(1) 1.00000000 . Uiso d ? C(10) 0.227(1) 0.677(1) -0.347(2) 0.02(1) 1.00000000 . Uiso d ? C(11) 0.306(1) 0.644(1) -0.565(2) 0.01(1) 1.00000000 . Uiso d ? C(12) 0.353(1) 0.532(1) -0.534(2) 0.04(1) 1.00000000 . Uiso d ? C(13) 0.344(1) 0.610(1) -0.383(2) 0.05(1) 1.00000000 . Uiso d ? C(14) 0.295(1) 0.507(1) 0.149(2) 0.03(1) 1.00000000 . Uiso d ? C(15) 0.281(1) 0.455(1) 0.197(2) 0.02(1) 1.00000000 . Uiso d ? C(16) 0.221(1) 0.435(1) 0.189(2) 0.02(1) 1.00000000 . Uiso d ? C(17) 0.179(1) 0.467(1) 0.136(2) 0.02(1) 1.00000000 . Uiso d ? C(18) 0.201(1) 0.515(1) 0.094(2) 0.03(1) 1.00000000 . Uiso d ? C(19) 0.200(1) 0.640(1) 0.225(2) 0.02(1) 1.00000000 . Uiso d ? C(20) 0.154(1) 0.662(1) 0.283(2) 0.01(1) 1.00000000 . Uiso d ? C(21) 0.115(1) 0.701(1) 0.253(2) 0.03(1) 1.00000000 . Uiso d ? C(22) 0.128(1) 0.725(1) 0.159(2) 0.02(1) 1.00000000 . Uiso d ? C(23) 0.177(1) 0.704(1) 0.104(2) 0.02(1) 1.00000000 . Uiso d ? C(24) 0.336(1) 0.593(1) -0.048(3) 0.05(1) 1.00000000 . Uiso d ? C(25) 0.298(1) 0.701(1) -0.027(2) 0.03(1) 1.00000000 . Uiso d ? C(26) 0.340(1) 0.640(1) 0.134(2) 0.02(1) 1.00000000 . Uiso d ? C(27) -0.039128002 0.421902001 -0.090415999 0.09(2) 1.00000000 . Uiso c ? C(28) -0.057723999 0.450435996 -0.025339000 0.17(2) 1.00000000 . Uiso c ? C(29) -0.040982001 0.414909989 0.087479003 0.12(2) 1.00000000 . Uiso c ? H(1) 0.263316005 0.443729997 -0.468988001 0.03269433 1.00000000 . Uiso c ? H(2) 0.219027996 0.373519003 -0.370943993 0.02001166 1.00000000 . Uiso c ? H(3) 0.214179993 0.488180012 -0.148306996 0.03656426 1.00000000 . Uiso c ? H(4) 0.259445995 0.557406008 -0.250887007 0.03599894 1.00000000 . Uiso c ? H(5) 0.150068998 0.585820973 -0.464349985 0.02962252 1.00000000 . Uiso c ? H(6) 0.071672998 0.629801989 -0.387145996 0.03134995 1.00000000 . Uiso c ? H(7) 0.193711996 0.736256003 -0.258056015 0.03359033 1.00000000 . Uiso c ? H(8) 0.264432013 0.691284001 -0.341464013 0.03000584 1.00000000 . Uiso c ? H(9) 0.333766013 0.519203007 0.154510006 0.03978940 1.00000000 . Uiso c ? H(10) 0.309067994 0.432143003 0.233330995 0.02191599 1.00000000 . Uiso c ? H(11) 0.140098006 0.454097003 0.131600007 0.02873615 1.00000000 . Uiso c ? H(12) 0.172619000 0.536527991 0.054039001 0.03202887 1.00000000 . Uiso c ? H(13) 0.227026999 0.611509979 0.251915008 0.02410190 1.00000000 . Uiso c ? H(14) 0.150738999 0.645587981 0.346634001 0.01346852 1.00000000 . Uiso c ? H(15) 0.104295000 0.755383015 0.131108001 0.01816617 1.00000000 . Uiso c ? H(16) 0.187803999 0.721717000 0.044047002 0.02397672 1.00000000 . 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) 0.023(1) 0.017(1) 0.028(1) -0.005(1) 0.008(1) -0.001(1) Re(2) 0.025(1) 0.019(1) 0.029(1) 0.003(1) 0.009(1) 0.003(1) Cl(1) 0.038(4) 0.030(4) 0.033(4) -0.003(3) -0.009(3) -0.008(3) Cl(2) 0.05(1) 0.030(4) 0.027(4) 0.011(4) -0.014(3) -0.009(3) O(1) 0.07(2) 0.05(2) 0.06(2) -0.03(1) -0.02(1) 0.02(1) O(2) 0.04(2) 0.08(2) 0.15(3) -0.01(1) 0.03(2) -0.05(2) O(4) 0.05(2) 0.10(2) 0.06(2) 0.02(1) 0.02(1) 0.01(1) O(5) 0.05(1) 0.04(1) 0.11(2) -0.02(1) 0.05(2) 0.02(1) O(6) 0.04(1) 0.04(1) 0.06(1) 0.00(1) 0.01(1) 0.00(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo)] _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.000000007(2) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2164 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1322 _refine_ls_R_factor_obs 0.0587 _refine_ls_wR_factor_all 0.0656 _refine_ls_wR_factor_obs 0.0595 _refine_ls_goodness_of_fit_all 1.822 _refine_ls_goodness_of_fit_obs 2.063 _refine_ls_shift/esd_max 0.1080 _refine_ls_shift/esd_mean 0.0175 _refine_diff_density_min -1.40 _refine_diff_density_max 2.32 #------------------------------------------------------------------------------ _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) 2.49(1) . . yes Re(1) N(1) 2.22(3) . . yes Re(1) N(2) 2.22(3) . . yes Re(1) C(11) 1.91(3) . . yes Re(1) C(12) 1.99(4) . . yes Re(1) C(13) 1.9(1) . . yes Re(2) Cl(2) 2.48(1) . . yes Re(2) N(3) 2.26(3) . . yes Re(2) N(4) 2.20(3) . . yes Re(2) C(24) 1.9(1) . . yes Re(2) C(25) 1.92(4) . . yes Re(2) C(26) 1.92(4) . . yes O(1) C(11) 1.14(4) . . yes O(2) C(12) 1.14(4) . . yes O(3) C(13) 1.0(1) . . yes O(4) C(24) 1.2(1) . . yes O(5) C(25) 1.18(4) . . yes O(6) C(26) 1.10(4) . . yes O(7) C(28) 1.4222(1) . . yes N(1) C(1) 1.36(4) . . yes N(1) C(5) 1.34(4) . . yes N(2) C(6) 1.42(4) . . yes N(2) C(10) 1.31(4) . . yes N(3) C(14) 1.39(4) . . yes N(3) C(18) 1.31(4) . . yes N(4) C(19) 1.33(4) . . yes N(4) C(23) 1.33(4) . . yes C(1) C(2) 1.4(1) . . yes C(1) H(1) 0.95 . . no C(2) C(3) 1.30(4) . . yes C(2) H(2) 0.97 . . no C(3) C(4) 1.4(1) . . yes C(3) C(8) 1.5(1) . 7_454 yes C(4) C(5) 1.4(1) . . yes C(4) H(3) 0.96 . . no C(5) H(4) 0.96 . . no C(6) C(7) 1.4(1) . . yes C(6) H(5) 0.94 . . no C(7) C(8) 1.4(1) . . yes C(7) H(6) 0.96 . . no C(8) C(9) 1.4(1) . . yes C(9) C(10) 1.3(1) . . yes C(9) H(7) 0.95 . . no C(10) H(8) 0.93 . . no C(14) C(15) 1.4(1) . . yes C(14) H(9) 0.92 . . no C(15) C(16) 1.5(1) . . yes C(15) H(10) 0.95 . . no C(16) C(17) 1.4(1) . . yes C(16) C(21) 1.5(1) . 7_455 yes C(17) C(18) 1.3(1) . . yes C(17) H(11) 0.93 . . no C(18) H(12) 0.97 . . no C(19) C(20) 1.39(4) . . yes C(19) H(13) 0.97 . . no C(20) C(21) 1.3(1) . . yes C(20) H(14) 0.94 . . no C(21) C(22) 1.4(1) . . yes C(22) C(23) 1.43(4) . . yes C(22) H(15) 0.94 . . no C(23) H(16) 0.94 . . no C(27) C(28) 1.1725(1) . . yes C(28) C(29) 1.7688(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 Cl(1) Re(1) N(1) 86(1) . . . yes Cl(1) Re(1) N(2) 91(1) . . . yes Cl(1) Re(1) C(11) 93(1) . . . yes Cl(1) Re(1) C(12) 91(1) . . . yes Cl(1) Re(1) C(13) 176(1) . . . yes N(1) Re(1) N(2) 85(1) . . . yes N(1) Re(1) C(11) 175(1) . . . yes N(1) Re(1) C(12) 93(1) . . . yes N(1) Re(1) C(13) 91(2) . . . yes N(2) Re(1) C(11) 90(1) . . . yes N(2) Re(1) C(12) 178(2) . . . yes N(2) Re(1) C(13) 90(2) . . . yes C(11) Re(1) C(12) 91(2) . . . yes C(11) Re(1) C(13) 91(2) . . . yes C(12) Re(1) C(13) 88(2) . . . yes Cl(2) Re(2) N(3) 88(1) . . . yes Cl(2) Re(2) N(4) 86(1) . . . yes Cl(2) Re(2) C(24) 92(2) . . . yes Cl(2) Re(2) C(25) 86(1) . . . yes Cl(2) Re(2) C(26) 176(1) . . . yes N(3) Re(2) N(4) 83(1) . . . yes N(3) Re(2) C(24) 92(2) . . . yes N(3) Re(2) C(25) 175(1) . . . yes N(3) Re(2) C(26) 93(1) . . . yes N(4) Re(2) C(24) 175(2) . . . yes N(4) Re(2) C(25) 96(1) . . . yes N(4) Re(2) C(26) 91(1) . . . yes C(24) Re(2) C(25) 88(2) . . . yes C(24) Re(2) C(26) 91(2) . . . yes C(25) Re(2) C(26) 92(2) . . . yes Re(1) N(1) C(1) 121(3) . . . yes Re(1) N(1) C(5) 124(3) . . . yes C(1) N(1) C(5) 115(3) . . . yes Re(1) N(2) C(6) 121(3) . . . yes Re(1) N(2) C(10) 124(3) . . . yes C(6) N(2) C(10) 115(3) . . . yes Re(2) N(3) C(14) 118(2) . . . yes Re(2) N(3) C(18) 127(3) . . . yes C(14) N(3) C(18) 115(3) . . . yes Re(2) N(4) C(19) 126(2) . . . yes Re(2) N(4) C(23) 119(2) . . . yes C(19) N(4) C(23) 115(3) . . . yes N(1) C(1) C(2) 122(3) . . . yes N(1) C(1) H(1) 118.7 . . . no C(2) C(1) H(1) 119.0 . . . no C(1) C(2) C(3) 120(4) . . . yes C(1) C(2) H(2) 120.0 . . . no C(3) C(2) H(2) 119.7 . . . no C(2) C(3) C(4) 121(4) . . . yes C(2) C(3) C(8) 117(4) . . 7_454 yes C(4) C(3) C(8) 121(3) . . 7_454 yes C(3) C(4) C(5) 117(4) . . . yes C(3) C(4) H(3) 121.8 . . . no C(5) C(4) H(3) 121.6 . . . no N(1) C(5) C(4) 125(4) . . . yes N(1) C(5) H(4) 117.0 . . . no C(4) C(5) H(4) 118.4 . . . no N(2) C(6) C(7) 125(4) . . . yes N(2) C(6) H(5) 114.9 . . . no C(7) C(6) H(5) 120.1 . . . no C(6) C(7) C(8) 118(4) . . . yes C(6) C(7) H(6) 118.6 . . . no C(8) C(7) H(6) 123.4 . . . no C(3) C(8) C(7) 121(4) 8_554 . . yes C(3) C(8) C(9) 125(4) 8_554 . . yes C(7) C(8) C(9) 114(3) . . . yes C(8) C(9) C(10) 125(4) . . . yes C(8) C(9) H(7) 117.3 . . . no C(10) C(9) H(7) 117.6 . . . no N(2) C(10) C(9) 123(4) . . . yes N(2) C(10) H(8) 118.5 . . . no C(9) C(10) H(8) 118.3 . . . no Re(1) C(11) O(1) 173(3) . . . yes Re(1) C(12) O(2) 175(4) . . . yes Re(1) C(13) O(3) 175(4) . . . yes N(3) C(14) C(15) 122(3) . . . yes N(3) C(14) H(9) 122.1 . . . no C(15) C(14) H(9) 116.3 . . . no C(14) C(15) C(16) 117(3) . . . yes C(14) C(15) H(10) 123.8 . . . no C(16) C(15) H(10) 119.4 . . . no C(15) C(16) C(17) 122(4) . . . yes C(15) C(16) C(21) 120(4) . . 7_455 yes C(17) C(16) C(21) 118(4) . . 7_455 yes C(16) C(17) C(18) 113(4) . . . yes C(16) C(17) H(11) 121.8 . . . no C(18) C(17) H(11) 125.5 . . . no N(3) C(18) C(17) 132(4) . . . yes N(3) C(18) H(12) 114.6 . . . no C(17) C(18) H(12) 113.8 . . . no N(4) C(19) C(20) 123(3) . . . yes N(4) C(19) H(13) 117.4 . . . no C(20) C(19) H(13) 119.6 . . . no C(19) C(20) C(21) 125(3) . . . yes C(19) C(20) H(14) 116.5 . . . no C(21) C(20) H(14) 118.8 . . . no C(16) C(21) C(20) 125(4) 8 . . yes C(16) C(21) C(22) 121(4) 8 . . yes C(20) C(21) C(22) 114(4) . . . yes C(21) C(22) C(23) 119(3) . . . yes C(21) C(22) H(15) 122.5 . . . no C(23) C(22) H(15) 118.4 . . . no N(4) C(23) C(22) 124(3) . . . yes N(4) C(23) H(16) 115.8 . . . no C(22) C(23) H(16) 120.6 . . . no Re(2) C(24) O(4) 175(4) . . . yes Re(2) C(25) O(5) 169(4) . . . yes Re(2) C(26) O(6) 177(4) . . . yes O(7) C(28) C(27) 132.038(3) . . . yes O(7) C(28) C(29) 115.921(3) . . . yes C(27) C(28) C(29) 108.61(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 Cl(1) C(29) 3.45(1) . 8_554 no Cl(1) C(19) 3.45(4) . 1_554 no Cl(2) C(9) 3.53(4) . . no Cl(2) C(5) 3.56(4) . . no O(1) O(6) 3.08(4) . 1_554 no O(1) C(2) 3.13(4) . 3_564 no O(1) O(5) 3.32(4) . 6_564 no O(1) C(19) 3.4(1) . 1_554 no O(1) C(26) 3.5(1) . 1_554 no O(1) C(9) 3.6(1) . 6_564 no O(2) O(3) 3.27(4) . 4_654 no O(3) C(15) 3.33(4) . 3_565 no O(3) O(4) 3.35(4) . . no O(3) C(22) 3.36(4) . 6_564 no O(5) C(20) 3.13(4) . 6_564 no O(5) C(21) 3.3(1) . 6_564 no O(5) C(10) 3.4(1) . 6_565 no O(5) N(2) 3.36(4) . 6_565 no O(5) C(16) 3.43(4) . 3_565 no O(5) C(9) 3.5(1) . 6_565 no O(5) C(6) 3.6(1) . 6_565 no O(6) C(3) 3.4(1) . 3_565 no O(7) C(28) 3.085(2) . 2_565 no O(7) C(27) 3.112(2) . 2_565 no O(7) C(7) 3.14(4) . 8_554 no O(7) C(17) 3.24(4) . 2_565 no O(7) O(7) 3.331(2) . 2_565 no O(7) C(18) 3.35(4) . 2_565 no O(7) C(29) 3.395(1) . 2_565 no O(7) C(6) 3.56(4) . 8_554 no C(10) C(23) 3.5(1) . 6_564 no C(28) C(28) 3.457(1) . 2_565 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Re(1) N(1) C(1) C(2) . . . . -171(3) no Re(1) N(1) C(5) C(4) . . . . 170(3) no Re(1) N(2) C(6) C(7) . . . . 173(3) no Re(1) N(2) C(10) C(9) . . . . -175(3) no Re(2) N(3) C(14) C(15) . . . . 175(3) no Re(2) N(3) C(18) C(17) . . . . -173(3) no Re(2) N(4) C(19) C(20) . . . . -177(3) no Re(2) N(4) C(23) C(22) . . . . 174(3) no Cl(1) Re(1) N(1) C(1) . . . . 41(3) no Cl(1) Re(1) N(1) C(5) . . . . -137(3) no Cl(1) Re(1) N(2) C(6) . . . . 19(3) no Cl(1) Re(1) N(2) C(10) . . . . -169(3) no Cl(1) Re(1) C(11) O(1) . . . . 37.9(3) no Cl(1) Re(1) C(12) O(2) . . . . 97.4(5) no Cl(1) Re(1) C(13) O(3) . . . . 107.9(5) no Cl(2) Re(2) N(3) C(14) . . . . 154(3) no Cl(2) Re(2) N(3) C(18) . . . . -26(3) no Cl(2) Re(2) N(4) C(19) . . . . 127(3) no Cl(2) Re(2) N(4) C(23) . . . . -52(3) no Cl(2) Re(2) C(24) O(4) . . . . 73.3(5) no Cl(2) Re(2) C(25) O(5) . . . . 157.4(2) no Cl(2) Re(2) C(26) O(6) . . . . 170.1(5) no O(1) C(11) Re(1) N(1) . . . . -39.3(3) no O(1) C(11) Re(1) N(2) . . . . -53.1(3) no O(1) C(11) Re(1) C(12) . . . . 128.5(3) no O(1) C(11) Re(1) C(13) . . . . -143.3(3) no O(2) C(12) Re(1) N(1) . . . . -176.9(5) no O(2) C(12) Re(1) N(2) . . . . -125.2(5) no O(2) C(12) Re(1) C(11) . . . . 4.1(5) no O(2) C(12) Re(1) C(13) . . . . -86.4(5) no O(3) C(13) Re(1) N(1) . . . . 130.2(5) no O(3) C(13) Re(1) N(2) . . . . -144.6(5) no O(3) C(13) Re(1) C(11) . . . . -54.6(5) no O(3) C(13) Re(1) C(12) . . . . 36.8(5) no O(4) C(24) Re(2) N(3) . . . . 161.8(5) no O(4) C(24) Re(2) N(4) . . . . 142.6(4) no O(4) C(24) Re(2) C(25) . . . . -12.9(5) no O(4) C(24) Re(2) C(26) . . . . -104.8(5) no O(5) C(25) Re(2) N(3) . . . . 151.0(1) no O(5) C(25) Re(2) N(4) . . . . 72.1(2) no O(5) C(25) Re(2) C(24) . . . . -110.0(2) no O(5) C(25) Re(2) C(26) . . . . -19.3(2) no O(6) C(26) Re(2) N(3) . . . . 51.9(6) no O(6) C(26) Re(2) N(4) . . . . 134.7(6) no O(6) C(26) Re(2) C(24) . . . . -40.6(6) no O(6) C(26) Re(2) C(25) . . . . -129.0(6) no N(1) Re(1) N(2) C(6) . . . . -66(3) no N(1) Re(1) N(2) C(10) . . . . 105(3) no N(1) C(1) C(2) C(3) . . . . -5(6) no N(1) C(5) C(4) C(3) . . . . 8(6) no N(2) Re(1) N(1) C(1) . . . . 132(3) no N(2) Re(1) N(1) C(5) . . . . -45(3) no N(2) C(6) C(7) C(8) . . . . -1(6) no N(2) C(10) C(9) C(8) . . . . 5(6) no N(3) Re(2) N(4) C(19) . . . . 38(3) no N(3) Re(2) N(4) C(23) . . . . -141(3) no N(3) C(14) C(15) C(16) . . . . 2(6) no N(3) C(18) C(17) C(16) . . . . -5(6) no N(4) Re(2) N(3) C(14) . . . . -120(3) no N(4) Re(2) N(3) C(18) . . . . 60(3) no N(4) C(19) C(20) C(21) . . . . 5(6) no N(4) C(23) C(22) C(21) . . . . 2(5) no C(1) N(1) Re(1) C(11) . . . . 118.3(1) no C(1) N(1) Re(1) C(12) . . . . -50(3) no C(1) N(1) Re(1) C(13) . . . . -138(3) no C(1) N(1) C(5) C(4) . . . . -8(6) no C(1) C(2) C(3) C(4) . . . . 5(6) no C(1) C(2) C(3) C(8) . . . 7_454 179(3) no C(2) C(1) N(1) C(5) . . . . 6(5) no C(2) C(3) C(4) C(5) . . . . -6(6) no C(2) C(3) C(8) C(7) . . 7_454 7_454 -138(4) no C(2) C(3) C(8) C(9) . . 7_454 7_454 40(6) no C(3) C(8) C(7) C(6) . 7_454 7_454 7_454 175(4) no C(3) C(8) C(9) C(10) . 7_454 7_454 7_454 -173(4) no C(4) C(3) C(8) C(7) . . 7_454 7_454 36(6) no C(4) C(3) C(8) C(9) . . 7_454 7_454 -146(4) no C(5) N(1) Re(1) C(11) . . . . -59.0(2) no C(5) N(1) Re(1) C(12) . . . . 133(3) no C(5) N(1) Re(1) C(13) . . . . 45(3) no C(5) C(4) C(3) C(8) . . . 7_454 -180(4) no C(6) N(2) Re(1) C(11) . . . . 112(3) no C(6) N(2) Re(1) C(12) . . . . -118.3(4) no C(6) N(2) Re(1) C(13) . . . . -157(3) no C(6) N(2) C(10) C(9) . . . . -2(6) no C(6) C(7) C(8) C(9) . . . . 3(5) no C(7) C(6) N(2) C(10) . . . . 1(6) no C(7) C(8) C(9) C(10) . . . . -5(6) no C(10) N(2) Re(1) C(11) . . . . -76(3) no C(10) N(2) Re(1) C(12) . . . . 53.4(4) no C(10) N(2) Re(1) C(13) . . . . 15(3) no C(14) N(3) Re(2) C(24) . . . . 62(3) no C(14) N(3) Re(2) C(25) . . . . 160.5(1) no C(14) N(3) Re(2) C(26) . . . . -29(3) no C(14) N(3) C(18) C(17) . . . . 7(6) no C(14) C(15) C(16) C(17) . . . . 0(6) no C(14) C(15) C(16) C(21) . . . 7_455 -173(3) no C(15) C(14) N(3) C(18) . . . . -5(5) no C(15) C(16) C(17) C(18) . . . . 1(6) no C(15) C(16) C(21) C(20) . . 7_455 7_455 -145(4) no C(15) C(16) C(21) C(22) . . 7_455 7_455 31(5) no C(16) C(21) C(20) C(19) . 7_455 7_455 7_455 -176(4) no C(17) C(16) C(21) C(20) . . 7_455 7_455 42(6) no C(17) C(16) C(21) C(22) . . 7_455 7_455 -142(4) no C(18) N(3) Re(2) C(24) . . . . -118(3) no C(18) N(3) Re(2) C(25) . . . . -19.1(2) no C(18) N(3) Re(2) C(26) . . . . 151(3) no C(18) C(17) C(16) C(21) . . . 7_455 174(3) no C(19) N(4) Re(2) C(24) . . . . 57.1(2) no C(19) N(4) Re(2) C(25) . . . . -148(3) no C(19) N(4) Re(2) C(26) . . . . -56(3) no C(19) N(4) C(23) C(22) . . . . -5(5) no C(19) C(20) C(21) C(22) . . . . -7(6) no C(20) C(19) N(4) C(23) . . . . 2(5) no C(20) C(21) C(22) C(23) . . . . 4(5) no C(23) N(4) Re(2) C(24) . . . . -121.9(2) no C(23) N(4) Re(2) C(25) . . . . 33(3) no C(23) N(4) Re(2) C(26) . . . . 126(3) no #------------------------------------------------------------------------------