Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Tosha M. Barclay' 'Alex McAuley' 'S. Subramanian' _publ_contact_author_name 'Prof Alex McAuley' _publ_contact_author_address ; ? ; _publ_contact_author_email 'amcauley@uvic.ca' _publ_section_title ; Synthesis and Structure of a New Macro-tricyclic Ligand that Encapsulates ; data_for [H2L3](ClO4)2 _database_code_CSD 173092 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H38 Cl2 N4 O8 S2' _chemical_formula_weight 573.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.408(2) _cell_length_b 16.534(5) _cell_length_c 10.412(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.364(6) _cell_angle_gamma 90.00 _cell_volume 1264.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.473 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6459 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.08 _reflns_number_total 2230 _reflns_number_gt 1284 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2230 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0999 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1323 _refine_ls_wR_factor_gt 0.1138 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.36270(13) 0.43619(6) 0.39905(10) 0.0453(3) Uani 1 1 d . . . Cl1 Cl 0.61354(13) 0.35911(6) 0.91173(10) 0.0483(3) Uani 1 1 d . . . O1 O 0.5880(5) 0.43178(18) 0.8407(4) 0.0949(12) Uani 1 1 d . . . O2 O 0.8008(4) 0.3497(2) 0.9593(3) 0.0915(12) Uani 1 1 d . . . O3 O 0.5601(5) 0.29442(18) 0.8275(3) 0.0845(11) Uani 1 1 d . . . O4 O 0.5093(7) 0.3574(3) 1.0128(4) 0.1358(17) Uani 1 1 d . . . N1 N -0.0411(4) 0.43806(18) 0.2864(3) 0.0435(8) Uani 1 1 d . . . HN1 H 0.0232 0.4561 0.3613 0.052 Uiso 1 1 calc R . . N2 N 0.0217(4) 0.37757(17) 0.5435(3) 0.0400(8) Uani 1 1 d . . . C1 C 0.0927(5) 0.4294(3) 0.1897(4) 0.0574(12) Uani 1 1 d . . . H1A H 0.1220 0.4825 0.1585 0.069 Uiso 1 1 calc R . . H1B H 0.0376 0.3981 0.1162 0.069 Uiso 1 1 calc R . . C2 C 0.2665(5) 0.3879(3) 0.2494(4) 0.0604(13) Uani 1 1 d . . . H2A H 0.3549 0.3892 0.1883 0.072 Uiso 1 1 calc R . . H2B H 0.2406 0.3317 0.2664 0.072 Uiso 1 1 calc R . . C3 C 0.3566(5) 0.3583(2) 0.5198(4) 0.0530(11) Uani 1 1 d . . . H3A H 0.4385 0.3154 0.5008 0.064 Uiso 1 1 calc R . . H3B H 0.4049 0.3810 0.6031 0.064 Uiso 1 1 calc R . . C4 C 0.1720(5) 0.3202(2) 0.5335(5) 0.0565(12) Uani 1 1 d . . . H4A H 0.1379 0.2854 0.4594 0.068 Uiso 1 1 calc R . . H4B H 0.1857 0.2862 0.6101 0.068 Uiso 1 1 calc R . . C5 C -0.1461(5) 0.3553(2) 0.4593(4) 0.0533(11) Uani 1 1 d . . . H5A H -0.2433 0.3916 0.4762 0.064 Uiso 1 1 calc R . . H5B H -0.1812 0.3009 0.4804 0.064 Uiso 1 1 calc R . . C6 C -0.1241(6) 0.3592(3) 0.3175(4) 0.0584(12) Uani 1 1 d . . . H6A H -0.0470 0.3151 0.2959 0.070 Uiso 1 1 calc R . . H6B H -0.2420 0.3532 0.2659 0.070 Uiso 1 1 calc R . . C7 C -0.1894(5) 0.4992(3) 0.2489(4) 0.0531(11) Uani 1 1 d . . . H7A H -0.2662 0.5022 0.3175 0.064 Uiso 1 1 calc R . . H7B H -0.2643 0.4803 0.1714 0.064 Uiso 1 1 calc R . . C8 C -0.1219(6) 0.5834(3) 0.2237(4) 0.0589(12) Uani 1 1 d . . . H8A H -0.0762 0.5830 0.1405 0.071 Uiso 1 1 calc R . . H8B H -0.2251 0.6199 0.2165 0.071 Uiso 1 1 calc R . . C9 C -0.0248(5) 0.3824(2) 0.6771(4) 0.0512(11) Uani 1 1 d . . . H9A H -0.0548 0.3284 0.7043 0.061 Uiso 1 1 calc R . . H9B H -0.1332 0.4154 0.6764 0.061 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0316(5) 0.0588(7) 0.0454(6) -0.0066(5) 0.0047(4) -0.0023(5) Cl1 0.0455(6) 0.0536(6) 0.0454(6) 0.0017(5) 0.0045(5) -0.0003(5) O1 0.072(2) 0.064(2) 0.148(4) 0.039(2) 0.009(2) 0.0050(17) O2 0.057(2) 0.101(3) 0.105(3) 0.007(2) -0.033(2) -0.0039(19) O3 0.091(3) 0.077(2) 0.076(2) -0.022(2) -0.0255(19) 0.0009(19) O4 0.155(4) 0.182(5) 0.088(3) -0.009(3) 0.083(3) -0.021(3) N1 0.0338(17) 0.063(2) 0.0335(18) -0.0141(16) 0.0024(14) -0.0101(16) N2 0.0333(17) 0.0334(17) 0.054(2) 0.0043(16) 0.0088(15) 0.0013(14) C1 0.040(2) 0.093(3) 0.039(2) -0.024(2) 0.0069(19) -0.006(2) C2 0.042(2) 0.083(3) 0.058(3) -0.030(3) 0.016(2) -0.004(2) C3 0.034(2) 0.056(3) 0.070(3) 0.006(2) 0.011(2) 0.015(2) C4 0.050(3) 0.044(2) 0.077(3) 0.009(2) 0.013(2) 0.008(2) C5 0.039(2) 0.048(2) 0.073(3) 0.002(2) 0.006(2) -0.011(2) C6 0.042(2) 0.055(3) 0.078(3) -0.019(3) 0.005(2) -0.012(2) C7 0.033(2) 0.080(3) 0.044(2) -0.003(2) -0.0042(18) 0.001(2) C8 0.042(3) 0.083(3) 0.051(3) 0.015(2) 0.007(2) 0.004(2) C9 0.043(2) 0.050(2) 0.063(3) 0.016(2) 0.014(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C3 1.804(4) . ? S1 C2 1.814(4) . ? Cl1 O4 1.383(4) . ? Cl1 O3 1.408(3) . ? Cl1 O1 1.411(3) . ? Cl1 O2 1.421(3) . ? N1 C6 1.495(5) . ? N1 C7 1.508(5) . ? N1 C1 1.508(5) . ? N2 C5 1.473(5) . ? N2 C4 1.476(5) . ? N2 C9 1.478(5) . ? C1 C2 1.519(6) . ? C3 C4 1.529(5) . ? C5 C6 1.508(6) . ? C7 C8 1.513(6) . ? C8 C9 1.510(5) 3_566 ? C9 C8 1.510(5) 3_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 S1 C2 104.0(2) . . ? O4 Cl1 O3 108.6(3) . . ? O4 Cl1 O1 111.4(3) . . ? O3 Cl1 O1 108.2(2) . . ? O4 Cl1 O2 110.4(3) . . ? O3 Cl1 O2 108.5(2) . . ? O1 Cl1 O2 109.6(2) . . ? C6 N1 C7 109.6(3) . . ? C6 N1 C1 112.7(3) . . ? C7 N1 C1 114.2(3) . . ? C5 N2 C4 112.6(3) . . ? C5 N2 C9 107.0(3) . . ? C4 N2 C9 111.7(3) . . ? N1 C1 C2 111.4(3) . . ? C1 C2 S1 111.8(3) . . ? C4 C3 S1 117.5(3) . . ? N2 C4 C3 115.7(3) . . ? N2 C5 C6 112.5(3) . . ? N1 C6 C5 110.3(3) . . ? N1 C7 C8 114.6(3) . . ? C9 C8 C7 116.8(3) 3_566 . ? N2 C9 C8 115.5(3) . 3_566 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.303 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.060 #============END data_Li[HL3](ClO4)2 _database_code_CSD 173093 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H37 Cl2 Li N4 O8 S2' _chemical_formula_weight 579.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3867(16) _cell_length_b 9.057(2) _cell_length_c 10.269(2) _cell_angle_alpha 72.895(4) _cell_angle_beta 80.625(4) _cell_angle_gamma 85.607(4) _cell_volume 647.6(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 306 _exptl_absorpt_coefficient_mu 0.462 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4921 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2280 _reflns_number_gt 1408 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2280 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.36636(12) 0.38447(10) 0.63596(10) 0.0417(3) Uani 1 1 d . . . Cl1 Cl -0.35317(13) 0.19761(11) 1.15072(10) 0.0493(3) Uani 1 1 d . . . O1 O -0.4466(6) 0.2100(6) 1.0436(4) 0.1350(17) Uani 1 1 d . . . O2 O -0.4480(5) 0.1171(5) 1.2740(4) 0.1343(19) Uani 1 1 d . . . O3 O -0.1765(4) 0.1260(4) 1.1294(3) 0.0854(11) Uani 1 1 d . . . O4 O -0.3341(7) 0.3486(5) 1.1530(6) 0.156(2) Uani 1 1 d . . . Li1 Li 0.0000 0.5000 0.5000 0.0341(18) Uani 1 2 d S . . N1 N -0.0431(4) 0.3753(3) 0.7488(3) 0.0392(7) Uani 1 1 d . . . HN1 H 0.0250 0.4105 0.6643 0.047 Uiso 0.50 1 calc PR . . N2 N 0.0384(3) 0.2662(3) 0.5143(3) 0.0345(7) Uani 1 1 d . . . C1 C -0.1458(5) 0.6526(4) 0.7422(4) 0.0475(10) Uani 1 1 d . . . H1A H -0.2546 0.7198 0.7325 0.057 Uiso 1 1 calc R . . H1B H -0.1048 0.6524 0.8273 0.057 Uiso 1 1 calc R . . C2 C -0.2000(5) 0.4900(4) 0.7558(4) 0.0465(10) Uani 1 1 d . . . H2A H -0.2792 0.4523 0.8430 0.056 Uiso 1 1 calc R . . H2B H -0.2712 0.4946 0.6831 0.056 Uiso 1 1 calc R . . C3 C 0.0837(5) 0.3601(5) 0.8527(4) 0.0457(9) Uani 1 1 d . . . H3A H 0.0274 0.2976 0.9420 0.055 Uiso 1 1 calc R . . H3B H 0.1034 0.4615 0.8606 0.055 Uiso 1 1 calc R . . C4 C 0.2674(5) 0.2859(5) 0.8114(4) 0.0493(10) Uani 1 1 d . . . H4A H 0.2505 0.1783 0.8191 0.059 Uiso 1 1 calc R . . H4B H 0.3514 0.2892 0.8738 0.059 Uiso 1 1 calc R . . C5 C 0.3761(5) 0.2412(4) 0.5440(4) 0.0415(9) Uani 1 1 d . . . H5A H 0.4229 0.2900 0.4482 0.050 Uiso 1 1 calc R . . H5B H 0.4651 0.1612 0.5797 0.050 Uiso 1 1 calc R . . C6 C 0.1983(4) 0.1628(4) 0.5488(4) 0.0407(9) Uani 1 1 d . . . H6A H 0.2215 0.0998 0.4858 0.049 Uiso 1 1 calc R . . H6B H 0.1666 0.0938 0.6408 0.049 Uiso 1 1 calc R . . C7 C -0.0021(5) 0.2780(4) 0.3758(4) 0.0427(9) Uani 1 1 d . . . H7A H -0.1142 0.3398 0.3620 0.051 Uiso 1 1 calc R . . H7B H -0.0250 0.1752 0.3724 0.051 Uiso 1 1 calc R . . C8 C -0.1281(5) 0.2154(4) 0.6125(4) 0.0437(9) Uani 1 1 d . . . H8A H -0.1523 0.1105 0.6158 0.052 Uiso 1 1 calc R . . H8B H -0.2314 0.2809 0.5802 0.052 Uiso 1 1 calc R . . C9 C -0.1137(5) 0.2207(4) 0.7557(4) 0.0453(10) Uani 1 1 d . . . H9A H -0.0307 0.1386 0.7974 0.054 Uiso 1 1 calc R . . H9B H -0.2333 0.2053 0.8122 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0337(5) 0.0473(6) 0.0475(6) -0.0160(4) -0.0088(4) -0.0066(4) Cl1 0.0523(6) 0.0518(6) 0.0407(6) -0.0080(4) -0.0101(5) 0.0029(5) O1 0.098(3) 0.238(5) 0.091(3) -0.063(3) -0.050(2) 0.005(3) O2 0.109(3) 0.133(3) 0.078(3) 0.045(2) 0.051(2) 0.062(3) O3 0.061(2) 0.092(2) 0.075(2) 0.0021(18) 0.0124(17) 0.0202(18) O4 0.157(4) 0.071(3) 0.271(7) -0.073(3) -0.082(4) 0.009(3) Li1 0.035(4) 0.034(4) 0.036(5) -0.009(3) -0.012(4) 0.000(3) N1 0.0369(17) 0.0459(17) 0.0373(17) -0.0138(14) -0.0061(13) -0.0072(14) N2 0.0290(15) 0.0342(15) 0.0433(18) -0.0129(13) -0.0101(13) -0.0010(12) C1 0.051(2) 0.055(2) 0.043(2) -0.0220(19) -0.0132(19) 0.0058(19) C2 0.037(2) 0.058(2) 0.043(2) -0.0135(18) -0.0032(17) -0.0055(18) C3 0.044(2) 0.060(2) 0.034(2) -0.0106(18) -0.0106(17) -0.0078(18) C4 0.043(2) 0.062(2) 0.045(2) -0.0130(19) -0.0174(19) 0.0009(19) C5 0.0324(19) 0.043(2) 0.053(2) -0.0175(18) -0.0132(17) 0.0026(16) C6 0.039(2) 0.0306(18) 0.054(2) -0.0106(17) -0.0146(18) -0.0013(16) C7 0.046(2) 0.040(2) 0.051(2) -0.0208(18) -0.0174(18) -0.0021(17) C8 0.033(2) 0.044(2) 0.058(3) -0.0185(18) -0.0090(18) -0.0050(16) C9 0.044(2) 0.043(2) 0.047(2) -0.0092(17) -0.0020(18) -0.0131(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C5 1.807(4) . ? S1 C4 1.817(4) . ? Cl1 O1 1.365(4) . ? Cl1 O2 1.368(3) . ? Cl1 O4 1.393(4) . ? Cl1 O3 1.426(3) . ? Li1 N2 2.080(3) 2_566 ? Li1 N2 2.080(3) . ? Li1 N1 2.449(3) . ? Li1 N1 2.449(3) 2_566 ? Li1 C8 2.672(3) . ? Li1 C8 2.672(3) 2_566 ? Li1 C7 2.682(3) . ? Li1 C7 2.682(3) 2_566 ? Li1 C2 2.776(4) . ? Li1 C2 2.776(4) 2_566 ? N1 C3 1.501(4) . ? N1 C2 1.503(5) . ? N1 C9 1.510(4) . ? N2 C8 1.467(4) . ? N2 C7 1.472(4) . ? N2 C6 1.473(4) . ? C1 C7 1.511(5) 2_566 ? C1 C2 1.517(5) . ? C3 C4 1.521(5) . ? C5 C6 1.527(4) . ? C7 C1 1.511(5) 2_566 ? C8 C9 1.506(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 S1 C4 104.70(18) . . ? O1 Cl1 O2 112.0(3) . . ? O1 Cl1 O4 105.6(3) . . ? O2 Cl1 O4 108.9(3) . . ? O1 Cl1 O3 110.9(3) . . ? O2 Cl1 O3 109.66(19) . . ? O4 Cl1 O3 109.7(3) . . ? N2 Li1 N2 180.0 2_566 . ? N2 Li1 N1 103.31(10) 2_566 . ? N2 Li1 N1 76.69(10) . . ? N2 Li1 N1 76.69(10) 2_566 2_566 ? N2 Li1 N1 103.31(10) . 2_566 ? N1 Li1 N1 180.0 . 2_566 ? N2 Li1 C8 146.92(10) 2_566 . ? N2 Li1 C8 33.08(10) . . ? N1 Li1 C8 57.31(10) . . ? N1 Li1 C8 122.69(10) 2_566 . ? N2 Li1 C8 33.08(10) 2_566 2_566 ? N2 Li1 C8 146.92(10) . 2_566 ? N1 Li1 C8 122.69(10) . 2_566 ? N1 Li1 C8 57.31(10) 2_566 2_566 ? C8 Li1 C8 180.000(1) . 2_566 ? N2 Li1 C7 146.94(10) 2_566 . ? N2 Li1 C7 33.06(10) . . ? N1 Li1 C7 107.37(10) . . ? N1 Li1 C7 72.63(10) 2_566 . ? C8 Li1 C7 52.62(11) . . ? C8 Li1 C7 127.38(11) 2_566 . ? N2 Li1 C7 33.06(10) 2_566 2_566 ? N2 Li1 C7 146.94(10) . 2_566 ? N1 Li1 C7 72.63(10) . 2_566 ? N1 Li1 C7 107.37(10) 2_566 2_566 ? C8 Li1 C7 127.38(11) . 2_566 ? C8 Li1 C7 52.62(11) 2_566 2_566 ? C7 Li1 C7 180.000(1) . 2_566 ? N2 Li1 C2 78.42(11) 2_566 . ? N2 Li1 C2 101.58(11) . . ? N1 Li1 C2 32.68(10) . . ? N1 Li1 C2 147.32(10) 2_566 . ? C8 Li1 C2 72.26(11) . . ? C8 Li1 C2 107.74(11) 2_566 . ? C7 Li1 C2 123.76(11) . . ? C7 Li1 C2 56.24(11) 2_566 . ? N2 Li1 C2 101.58(11) 2_566 2_566 ? N2 Li1 C2 78.42(10) . 2_566 ? N1 Li1 C2 147.32(10) . 2_566 ? N1 Li1 C2 32.68(10) 2_566 2_566 ? C8 Li1 C2 107.74(11) . 2_566 ? C8 Li1 C2 72.26(11) 2_566 2_566 ? C7 Li1 C2 56.24(11) . 2_566 ? C7 Li1 C2 123.76(11) 2_566 2_566 ? C2 Li1 C2 180.0 . 2_566 ? C3 N1 C2 114.5(3) . . ? C3 N1 C9 111.7(3) . . ? C2 N1 C9 110.4(3) . . ? C3 N1 Li1 130.4(2) . . ? C2 N1 Li1 85.70(19) . . ? C9 N1 Li1 101.08(19) . . ? C8 N2 C7 107.7(3) . . ? C8 N2 C6 112.3(3) . . ? C7 N2 C6 112.1(3) . . ? C8 N2 Li1 96.23(19) . . ? C7 N2 Li1 96.54(19) . . ? C6 N2 Li1 129.3(2) . . ? C7 C1 C2 116.4(3) 2_566 . ? N1 C2 C1 115.3(3) . . ? N1 C2 Li1 61.62(16) . . ? C1 C2 Li1 91.2(2) . . ? N1 C3 C4 111.2(3) . . ? C3 C4 S1 111.4(2) . . ? C6 C5 S1 117.8(3) . . ? N2 C6 C5 116.2(3) . . ? N2 C7 C1 115.7(3) . 2_566 ? N2 C7 Li1 50.40(14) . . ? C1 C7 Li1 95.0(2) 2_566 . ? N2 C8 C9 112.9(3) . . ? N2 C8 Li1 50.69(14) . . ? C9 C8 Li1 92.07(19) . . ? C8 C9 N1 109.5(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.447 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.058 #===============END