Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global #=============================================================================== _audit_creation_date 7-02-00 # 1. SUBMISSION DETAILS _publ_contact_author 'Dr Nicolas Mercier' _publ_contact_author_address ; Dr Nicolas Mercier Laboratoire Ingenierie Moleculaire et Materiaux Organiques UMR CNRS 6501, Faculte des Sciences, 2 Bd Lavoisier, F-49045 ANGERS, France ; _publ_contact_author_email 'nicolas.mercier@univ-angers.fr' _publ_contact_author_fax '(33)2.41.73.54.05' _publ_contact_author_phone '(33)2.41.73.50.83' _publ_requested_journal 'Chem. Comm.' _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in Acta Crystallographica Section C. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; _publ_requested_category FM #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_Cambridge 182 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name 'Allain, Magali' 'Giffard, Michel' 'Gorgues, Alain' 'Hudhomme, Pietrick' 'Levillain, Eric' 'Mabon, Gilles' 'Mercier, Nicolas' 'Pilet, Guillaume' 'Riou, Amedee' # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=============================================================================== data_gp01_(Bu4N)2TTF(CO2H)2(CO2)2_(1) #=============================================================================== _database_code_CSD 172112 # 5. CHEMICAL DATA _chemical_name_systematic ; (Bu4N)2TTF(CO2H)2(CO2)2 ; _chemical_name_common ? _chemical_formula_moiety 'C42 H74 N2 O8 S4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H74 N2 O8 S4' _chemical_formula_weight 863.32 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 S ? 0.110 0.124 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,-z _cell_length_a 9.442(2) _cell_length_b 10.209(1) _cell_length_c 12.792(2) _cell_angle_alpha 96.77(1) _cell_angle_beta 98.63(1) _cell_angle_gamma 97.72(1) _cell_volume 1196.0(7) _cell_formula_units_Z 1 _cell_measurement_temperature 294 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 14.0 _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.20 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 0.247 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -4 -4 4 -4 3 _diffrn_reflns_number 4195 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4195 _reflns_number_gt 2778 _reflns_threshold_expression >3.0\s(I) _computing_data_collection 'CAD4_(Enraf-Nonius,_1994)' _computing_cell_refinement CAD4_(Enraf-Nonius,_1994) _computing_data_reduction 'process_OpenMoleN_(_1997)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2778 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.083 _refine_ls_R_factor_gt 0.046 _refine_ls_wR_factor_all 0.074 _refine_ls_wR_factor_ref 0.070 _refine_ls_goodness_of_fit_all 1.521 _refine_ls_goodness_of_fit_ref 1.435 _refine_ls_shift/su_max 0.033 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.242 _refine_diff_density_min -0.350 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol C1 1.0305(3) -0.4524(3) 0.5406(2) 0.060(1) Uani ? ? C C2 1.1798(3) -0.2411(3) 0.6574(2) 0.058(1) Uani ? ? C C3 1.0790(3) -0.2849(3) 0.7143(2) 0.059(1) Uani ? ? C C4 1.2953(3) -0.1198(3) 0.6802(3) 0.074(2) Uani ? ? C C5 1.0487(3) -0.2273(3) 0.8216(2) 0.079(2) Uani ? ? C S1 1.18412(8) -0.33717(7) 0.53569(5) 0.0663(4) Uani ? ? S S2 0.96099(8) -0.43124(8) 0.66029(5) 0.0717(4) Uani ? ? S O1 1.3786(2) -0.1101(2) 0.6171(2) 0.097(2) Uani ? ? O O2 1.2951(3) -0.0353(2) 0.7620(2) 0.100(2) Uani ? ? O O3 1.1204(3) -0.1153(3) 0.8657(2) 0.106(2) Uani ? ? O O4 0.9528(3) -0.2917(3) 0.8562(2) 0.107(2) Uani ? ? O N 0.7741(2) 0.1155(2) 0.7683(1) 0.048(1) Uani ? ? N C6 0.7180(3) 0.0333(3) 0.6594(2) 0.058(1) Uani ? ? C C7 0.9241(2) 0.1910(2) 0.7680(2) 0.053(1) Uani ? ? C C8 0.6679(2) 0.2100(3) 0.7911(2) 0.053(1) Uani ? ? C C9 0.7841(3) 0.0259(2) 0.8561(2) 0.055(1) Uani ? ? C C10 0.8020(4) -0.0744(3) 0.6258(3) 0.088(2) Uani ? ? C C11 0.9883(3) 0.2955(3) 0.8619(2) 0.060(1) Uani ? ? C C12 0.6500(3) 0.3141(3) 0.7173(2) 0.067(1) Uani ? ? C C13 0.6469(3) -0.0657(3) 0.8598(2) 0.068(2) Uani ? ? C C14 0.7294(5) -0.1503(4) 0.5166(3) 0.113(3) Uani ? ? C C15 1.1429(3) 0.3504(3) 0.8541(2) 0.066(2) Uani ? ? C C16 0.5471(3) 0.4047(3) 0.7523(2) 0.085(2) Uani ? ? C C17 0.6627(3) -0.1467(3) 0.9496(2) 0.076(2) Uani ? ? C C18 0.8151(7) -0.2015(8) 0.4541(4) 0.195(5) Uani ? ? C C19 1.2075(4) 0.4644(3) 0.9413(3) 0.083(2) Uani ? ? C C20 0.5250(5) 0.5104(4) 0.6801(3) 0.124(3) Uani ? ? C C21 0.5266(4) -0.2368(3) 0.9565(3) 0.090(2) Uani ? ? C H1 0.5440 -0.2852 1.0149 0.1164 Uiso calc C21 H H2 0.4523 -0.1849 0.9667 0.1164 Uiso calc C21 H H3 0.4973 -0.2975 0.8922 0.1164 Uiso calc C21 H H4 0.7581 -0.2460 0.3888 0.2865 Uiso calc C18 H H5 0.8836 -0.1317 0.4396 0.2865 Uiso calc C18 H H6 0.8648 -0.2632 0.4892 0.2865 Uiso calc C18 H H7 1.3042 0.4958 0.9334 0.1159 Uiso calc C19 H H8 1.1515 0.5348 0.9364 0.1159 Uiso calc C19 H H9 1.2076 0.4346 1.0089 0.1159 Uiso calc C19 H H10 0.4596 0.5648 0.7052 0.1554 Uiso calc C20 H H11 0.6154 0.5642 0.6804 0.1554 Uiso calc C20 H H12 0.4862 0.4685 0.6094 0.1554 Uiso calc C20 H H13 1.1440 0.3811 0.7869 0.0885 Uiso calc C15 H H14 1.2001 0.2809 0.8593 0.0885 Uiso calc C15 H H15 0.9874 0.2569 0.9259 0.0803 Uiso calc C11 H H16 0.9322 0.3662 0.8629 0.0803 Uiso calc C11 H H17 0.9189 0.2339 0.7058 0.0703 Uiso calc C7 H H18 0.9883 0.1272 0.7640 0.0703 Uiso calc C7 H H19 0.6799 -0.0904 0.4789 0.1549 Uiso calc C14 H H20 0.6611 -0.2220 0.5284 0.1549 Uiso calc C14 H H21 0.8055 -0.1347 0.6769 0.1183 Uiso calc C10 H H22 0.8978 -0.0353 0.6216 0.1183 Uiso calc C10 H H23 0.7173 0.0929 0.6077 0.0786 Uiso calc C6 H H24 0.6217 -0.0078 0.6598 0.0786 Uiso calc C6 H H25 0.6910 -0.0874 1.0147 0.0999 Uiso calc C17 H H26 0.7361 -0.2000 0.9401 0.0999 Uiso calc C17 H H27 0.6207 -0.1246 0.7944 0.0890 Uiso calc C13 H H28 0.5723 -0.0134 0.8683 0.0890 Uiso calc C13 H H29 0.8115 0.0818 0.9229 0.0723 Uiso calc C9 H H30 0.8571 -0.0275 0.8456 0.0723 Uiso calc C9 H H31 0.6997 0.2555 0.8616 0.0699 Uiso calc C8 H H32 0.5756 0.1577 0.7870 0.0699 Uiso calc C8 H H33 0.6127 0.2708 0.6468 0.0859 Uiso calc C12 H H34 0.7418 0.3660 0.7184 0.0859 Uiso calc C12 H H35 0.5852 0.4477 0.8228 0.1080 Uiso calc C16 H H36 0.4560 0.3520 0.7517 0.1080 Uiso calc C16 H 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 _atom_site_aniso_type_symbol C1 0.066(1) 0.057(1) 0.056(1) 0.009(1) 0.023(1) 0.012(1) C C2 0.056(1) 0.064(1) 0.054(1) 0.013(1) 0.001(1) 0.011(1) C C3 0.063(1) 0.067(1) 0.048(1) 0.019(1) 0.005(1) 0.009(1) C C4 0.059(2) 0.081(2) 0.083(2) 0.003(1) -0.007(1) 0.009(2) C C5 0.080(2) 0.111(2) 0.056(1) 0.033(2) 0.009(1) 0.003(2) C S1 0.0700(4) 0.0710(4) 0.0587(3) -0.0029(3) 0.0242(3) 0.0086(3) S S2 0.0872(4) 0.0725(4) 0.0582(3) -0.0028(4) 0.0342(3) 0.0076(3) S O1 0.076(1) 0.107(2) 0.110(2) -0.024(1) 0.007(1) 0.015(1) O O2 0.104(2) 0.089(1) 0.110(2) -0.001(1) -0.013(1) -0.024(1) O O3 0.113(2) 0.137(2) 0.078(1) 0.016(2) -0.001(1) -0.045(1) O O4 0.125(2) 0.149(2) 0.066(1) 0.023(2) 0.044(1) 0.005(1) O N 0.047(1) 0.056(1) 0.0432(9) 0.0006(9) 0.0112(8) 0.0062(8) N C6 0.066(2) 0.064(1) 0.046(1) -0.002(1) 0.007(1) 0.003(1) C C7 0.047(1) 0.063(1) 0.052(1) 0.000(1) 0.014(1) 0.008(1) C C8 0.044(1) 0.064(1) 0.055(1) 0.002(1) 0.0159(9) 0.009(1) C C9 0.060(1) 0.059(1) 0.047(1) 0.003(1) 0.009(1) 0.010(1) C C10 0.095(2) 0.098(2) 0.073(2) 0.017(2) 0.014(2) -0.019(2) C C11 0.055(1) 0.066(2) 0.060(1) -0.003(1) 0.011(1) 0.003(1) C C12 0.059(1) 0.075(2) 0.068(1) 0.009(1) 0.017(1) 0.021(1) C C13 0.070(2) 0.064(1) 0.069(2) -0.004(1) 0.010(1) 0.020(1) C C14 0.174(3) 0.108(3) 0.077(2) 0.037(2) 0.029(2) -0.010(2) C C15 0.052(1) 0.074(2) 0.075(2) -0.004(1) 0.011(1) 0.016(1) C C16 0.084(2) 0.093(2) 0.078(2) 0.034(2) 0.011(2) 0.018(2) C C17 0.083(2) 0.079(2) 0.067(2) -0.004(2) 0.013(1) 0.022(1) C C18 0.180(4) 0.381(8) 0.109(3) 0.124(4) 0.023(3) -0.020(5) C C19 0.072(2) 0.074(2) 0.107(2) -0.015(2) 0.002(2) 0.003(2) C C20 0.134(3) 0.109(2) 0.132(3) 0.056(2) 0.020(2) 0.043(2) C C21 0.102(2) 0.078(2) 0.092(2) -0.006(2) 0.035(2) 0.027(2) C # 10. MOLECULAR GEOMETRY 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 C1 S1 1.754(3) . . ? C1 S2 1.757(3) . . ? C2 C3 1.344(4) . . ? C2 C4 1.505(4) . . ? C2 S1 1.748(3) . . ? C3 C5 1.511(4) . . ? C3 S2 1.741(2) . . ? C4 O1 1.212(4) . . ? C4 O2 1.276(4) . . ? C5 O3 1.268(4) . . ? C5 O4 1.215(4) . . ? N C6 1.519(3) . . ? N C7 1.520(3) . . ? N C8 1.517(3) . . ? N C9 1.531(3) . . ? C6 C10 1.500(5) . . ? C7 C11 1.502(3) . . ? C8 C12 1.512(4) . . ? C9 C13 1.503(4) . . ? C10 C14 1.529(5) . . ? C11 C15 1.514(4) . . ? C12 C16 1.507(5) . . ? C13 C17 1.493(4) . . ? C14 C18 1.334(8) . . ? C15 C19 1.507(4) . . ? C16 C20 1.516(6) . . ? C17 C21 1.496(5) . . ? 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 ? ? ? ? ? ? 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 S1 C1 S2 114.6(1) . . . ? C3 C2 C4 130.8(2) . . . ? C3 C2 S1 117.4(2) . . . ? C4 C2 S1 111.7(2) . . . ? C2 C3 C3 . . . ? C2 C3 C5 130.4(2) . . . ? C2 C3 S2 117.5(2) . . . ? C3 C3 C5 . . . ? C3 C3 S2 . . . ? C5 C3 S2 112.1(2) . . . ? C2 C4 O1 116.4(3) . . . ? C2 C4 O2 117.7(3) . . . ? O1 C4 O2 125.9(3) . . . ? C3 C5 O3 118.1(3) . . . ? C3 C5 O4 116.1(3) . . . ? O3 C5 O4 125.7(3) . . . ? C1 S1 C2 94.9(1) . . . ? C1 S2 C3 95.1(1) . . . ? C6 N C7 109.1(2) . . . ? C6 N C8 108.5(2) . . . ? C6 N C9 111.0(2) . . . ? C7 N C8 111.5(2) . . . ? C7 N C9 108.9(2) . . . ? C8 N C9 108.0(2) . . . ? N C6 C6 . . . ? N C6 C10 116.7(2) . . . ? C6 C6 C10 . . . ? N C7 C11 117.3(2) . . . ? N C8 C12 116.4(2) . . . ? N C9 C13 115.4(2) . . . ? C6 C10 C14 110.2(3) . . . ? C7 C11 C15 110.2(2) . . . ? C8 C12 C16 110.7(2) . . . ? C9 C13 C17 112.6(2) . . . ? C10 C14 C18 117.2(4) . . . ? C11 C15 C19 112.2(3) . . . ? C12 C16 C20 112.6(3) . . . ? C13 C17 C21 113.7(3) . . . ? #===END #=============================================================================== #=============================================================================== data_(NoName)_(TTF)2[TTF(CO2H)2(CO2)2_(2) #=============================================================================== _database_code_CSD 172113 # 5. CHEMICAL DATA _chemical_name_systematic ; (TTF)2[TTF(CO2H)2(CO2)2] ; _chemical_name_common ? _chemical_formula_moiety 'C22H10O8S12' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C22H10O8S12' _chemical_formula_weight 786.9 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 S ? 0.110 0.124 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,-z _cell_length_a 8.143(1) _cell_length_b 8.203(2) _cell_length_c 10.519(1) _cell_angle_alpha 85.04(1) _cell_angle_beta 82.87(2) _cell_angle_gamma 84.00(1) _cell_volume 691.5(3) _cell_formula_units_z 1 _cell_measurement_temperature 294 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 16.0 _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'BLACK' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.89 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 398 _exptl_absorpt_coefficient_mu 0.960 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 2 1 -1 -2 -4 3 0 -4 _diffrn_reflns_number 2622 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 24.97 _reflns_number_total 2434 _reflns_number_observed 1604 _reflns_observed_criterion >3.0\s(I) _computing_data_collection 'CAD4_(Enraf-Nonius,_1994)' _computing_cell_refinement CAD4_(Enraf-Nonius,_1994) _computing_data_reduction 'process_MolEN_(Fair,_1990)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ? _computing_publication_material BTABLE_PTABLE_CIF_IN_MolEN_(Fair,_1990) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0036 Fo^4^)' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1604 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.080 _refine_ls_R_factor_obs 0.036 _refine_ls_wR_factor_all 0.072 _refine_ls_wR_factor_obs 0.054 _refine_ls_goodness_of_fit_all 1.848 _refine_ls_goodness_of_fit_obs 1.378 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 1.169 _refine_diff_density_min -1.119 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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 _atom_site_type_symbol S1 0.4335(1) 0.3035(1) 0.3832(1) 0.0293(5) Uij ? ? S S2 0.1906(1) 0.0650(1) 0.4073(1) 0.0341(5) Uij ? ? S S3 0.4902(1) 0.2160(1) 0.6826(1) 0.0313(5) Uij ? ? S S4 0.2455(1) -0.0208(1) 0.7062(1) 0.0332(5) Uij ? ? S S5 0.1615(1) 0.5627(1) 0.6362(1) 0.0278(5) Uij ? ? S S6 -0.1017(1) 0.3363(1) 0.6588(1) 0.0281(5) Uij ? ? S O1 0.3405(4) 0.5775(4) 0.8432(3) 0.046(2) Uij ? ? O O2 0.2124(4) 0.4118(4) 0.9925(3) 0.039(2) Uij ? ? O O3 -0.0060(4) 0.2300(4) 1.0114(3) 0.038(2) Uij ? ? O O4 -0.1846(4) 0.1606(4) 0.8871(3) 0.047(2) Uij ? ? O C1 0.3259(4) 0.1618(4) 0.4823(4) 0.025(2) Uij ? ? C C2 0.3487(4) 0.1250(5) 0.6084(4) 0.025(2) Uij ? ? C C3 0.3377(5) 0.2822(5) 0.2489(4) 0.033(2) Uij ? ? C C4 0.2267(5) 0.1721(6) 0.2613(4) 0.037(2) Uij ? ? C C5 0.4441(5) 0.1168(6) 0.8309(4) 0.038(2) Uij ? ? C C6 0.3299(6) 0.0088(6) 0.8423(4) 0.039(2) Uij ? ? C C7 0.0127(5) 0.4792(5) 0.5606(4) 0.024(2) Uij ? ? C C8 0.1197(5) 0.4520(5) 0.7844(4) 0.025(2) Uij ? ? C C9 -0.0031(5) 0.3499(5) 0.7948(4) 0.024(2) Uij ? ? C C10 0.2320(5) 0.4856(5) 0.8792(4) 0.030(2) Uij ? ? C C11 -0.0699(5) 0.2380(5) 0.9059(4) 0.029(2) Uij ? ? C H1 0.3644 0.3465 0.1691 0.0436 Uiso calc C3 H H2 0.1676 0.1542 0.1910 0.0477 Uiso calc C4 H H3 0.4995 0.1381 0.9029 0.0499 Uiso calc C5 H H4 0.2966 -0.0487 0.9242 0.0525 Uiso calc C6 H 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 _atom_site_aniso_type_symbol S1 0.0297(5) 0.0291(5) 0.0292(5) -0.0113(4) -0.0030(4) 0.0046(4) S S2 0.0287(5) 0.0367(5) 0.0378(6) -0.0141(4) -0.0039(4) -0.0030(5) S S3 0.0280(5) 0.0324(5) 0.0336(5) -0.0099(4) -0.0057(4) -0.0001(5) S S4 0.0310(5) 0.0320(5) 0.0368(6) -0.0123(4) -0.0010(4) 0.0077(5) S S5 0.0290(5) 0.0309(5) 0.0240(5) -0.0153(4) -0.0066(4) 0.0029(4) S S6 0.0281(5) 0.0295(5) 0.0268(5) -0.0149(4) -0.0057(4) 0.0043(4) S O1 0.044(2) 0.062(2) 0.035(2) -0.025(1) -0.006(1) -0.001(1) O O2 0.047(2) 0.052(2) 0.025(1) -0.014(1) -0.012(1) 0.007(1) O O3 0.050(2) 0.044(2) 0.026(1) -0.010(1) -0.006(1) 0.013(1) O O4 0.051(2) 0.053(2) 0.037(2) -0.033(1) -0.000(1) 0.008(1) O C1 0.023(2) 0.022(2) 0.030(2) -0.007(2) 0.000(2) 0.002(2) C C2 0.022(2) 0.022(2) 0.033(2) -0.006(2) 0.000(2) 0.002(2) C C3 0.036(2) 0.037(2) 0.027(2) -0.003(2) -0.006(2) 0.004(2) C C4 0.031(2) 0.047(2) 0.034(2) -0.000(2) -0.010(2) -0.007(2) C C5 0.036(2) 0.046(2) 0.034(2) -0.002(2) -0.009(2) 0.001(2) C C6 0.040(2) 0.049(3) 0.029(2) -0.007(2) 0.001(2) 0.009(2) C C7 0.024(2) 0.023(2) 0.026(2) -0.008(1) -0.003(2) 0.001(2) C C8 0.026(2) 0.027(2) 0.024(2) -0.007(2) -0.000(2) -0.003(2) C C9 0.026(2) 0.026(2) 0.022(2) -0.003(2) -0.002(2) -0.002(2) C C10 0.027(2) 0.039(2) 0.025(2) -0.003(2) -0.006(2) -0.002(2) C C11 0.030(2) 0.031(2) 0.027(2) -0.004(2) 0.001(2) 0.001(2) C # 10. MOLECULAR GEOMETRY 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 S1 C1 1.727(4) . . ? S1 C3 1.727(5) . . ? S2 C1 1.724(4) . . ? S2 C4 1.711(4) . . ? S3 C2 1.731(4) . . ? S3 C5 1.713(4) . . ? S4 C2 1.726(4) . . ? S4 C6 1.710(5) . . ? S5 C7 1.754(4) . . ? S5 C8 1.749(4) . . ? S6 C7 1.757(4) . . ? S6 C9 1.743(4) . . ? O1 C10 1.224(5) . . ? O2 C10 1.288(5) . . ? O3 C11 1.277(5) . . ? O4 C11 1.227(5) . . ? C1 C2 1.366(6) . . ? C3 C4 1.330(6) . . ? C5 C6 1.338(7) . . ? C8 C9 1.359(6) . . ? C8 C10 1.494(6) . . ? C9 C11 1.505(5) . . ? 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 ? ? ? ? ? ? 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 C1 S1 C3 95.7(2) . . . ? C1 S2 C4 95.7(2) . . . ? C2 S3 C5 95.5(2) . . . ? C2 S4 C6 96.0(2) . . . ? C7 S5 C8 95.5(2) . . . ? C7 S6 C9 95.5(2) . . . ? S1 C1 S2 114.3(2) . . . ? S1 C1 C2 123.3(3) . . . ? S2 C1 C2 122.4(3) . . . ? S3 C2 S4 114.0(2) . . . ? S3 C2 C1 122.6(3) . . . ? S4 C2 C1 123.3(3) . . . ? S1 C3 C4 116.4(3) . . . ? S2 C4 C3 117.9(4) . . . ? S3 C5 C6 117.5(4) . . . ? S4 C6 C5 116.8(3) . . . ? S5 C7 S6 114.6(2) . . . ? S5 C8 C9 117.0(3) . . . ? S5 C8 C10 112.2(3) . . . ? C9 C8 C10 130.8(4) . . . ? S6 C9 C8 117.4(3) . . . ? S6 C9 C11 111.7(3) . . . ? C8 C9 C11 130.9(4) . . . ? O1 C10 O2 124.0(4) . . . ? O1 C10 C8 118.0(4) . . . ? O2 C10 C8 118.0(4) . . . ? O3 C11 O4 124.8(4) . . . ? O3 C11 C9 119.1(4) . . . ? O4 C11 C9 116.1(4) . . . ? #===END